# Electronic Supplementary Material (ESI) for Organic Chemistry Frontiers. # This journal is © the Partner Organisations 2015 ####################################################################### # # This file contains crystal structure data downloaded from the # Cambridge Structural Database (CSD) hosted by the Cambridge # Crystallographic Data Centre (CCDC). # # Full information about CCDC data access policies and citation # guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 # # Audit and citation data items may have been added by the CCDC. # Please retain this information to preserve the provenance of # this file and to allow appropriate attribution of the data. # ####################################################################### data_TZ888_2_0m_a _database_code_depnum_ccdc_archive 'CCDC 1423805' _audit_update_record ; 2015-09-11 deposited with the CCDC. 2015-10-15 downloaded from the CCDC. ; _audit_creation_method SHELXL-2014/7 _shelx_SHELXL_version_number 2014/7 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C26 H23 F6 N2 O P2 Rh' _chemical_formula_weight 658.31 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Rh Rh -1.1178 0.9187 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_H-M_alt 'P 21/c' _space_group_name_Hall '-P 2ybc' _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 10.6439(13) _cell_length_b 11.6245(14) _cell_length_c 21.782(3) _cell_angle_alpha 90 _cell_angle_beta 100.416(2) _cell_angle_gamma 90 _cell_volume 2650.7(5) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour 'clear light yellow' _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_density_diffrn 1.650 _exptl_crystal_F_000 1320 _exptl_transmission_factor_min ? _exptl_transmission_factor_max ? _exptl_crystal_size_max 0.389 _exptl_crystal_size_mid 0.319 _exptl_crystal_size_min 0.112 _exptl_absorpt_coefficient_mu 0.831 _shelx_estimated_absorpt_T_min 0.738 _shelx_estimated_absorpt_T_max 0.913 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.59 _exptl_absorpt_correction_T_max 0.91 _exptl_absorpt_process_details 'SADABS V2014/5 (Bruker AXS Inc.)' _exptl_absorpt_special_details ? _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_source ? _diffrn_measurement_device_type 'Bruker ApexII Triumph monochromator sealed tube' _diffrn_measurement_method 'Photon 50 CMOS detector' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 30389 _diffrn_reflns_av_unetI/netI 0.0442 _diffrn_reflns_av_R_equivalents 0.0711 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 2.903 _diffrn_reflns_theta_max 24.997 _diffrn_reflns_theta_full 24.997 _diffrn_measured_fraction_theta_max 0.999 _diffrn_measured_fraction_theta_full 0.999 _diffrn_reflns_Laue_measured_fraction_max 0.999 _diffrn_reflns_Laue_measured_fraction_full 0.999 _diffrn_reflns_point_group_measured_fraction_max 0.999 _diffrn_reflns_point_group_measured_fraction_full 0.999 _reflns_number_total 4661 _reflns_number_gt 3905 _reflns_threshold_expression 'I > 2\s(I)' _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_max . _reflns_Friedel_fraction_full . _reflns_special_details ; Reflections were merged by SHELXL according to the crystal class for the calculation of statistics and refinement. _reflns_Friedel_fraction is defined as the number of unique Friedel pairs measured divided by the number that would be possible theoretically, ignoring centric projections and systematic absences. ; _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement 'SHELXL-2014/7 (Sheldrick, 2014)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ? _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0524P)^2^+5.0183P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary ? _atom_sites_solution_secondary ? _atom_sites_solution_hydrogens mixed _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef . _refine_ls_number_reflns 4661 _refine_ls_number_parameters 346 _refine_ls_number_restraints 334 _refine_ls_R_factor_all 0.0510 _refine_ls_R_factor_gt 0.0382 _refine_ls_wR_factor_ref 0.1062 _refine_ls_wR_factor_gt 0.0948 _refine_ls_goodness_of_fit_ref 1.057 _refine_ls_restrained_S_all 1.038 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Rh1 Rh 0.42179(3) 0.38207(2) 0.32221(2) 0.01866(11) Uani 1 1 d . U . . . P1 P 0.27115(9) 0.42056(8) 0.37710(4) 0.0188(2) Uani 1 1 d . U . . . N1 N 0.2739(3) 0.3091(2) 0.26109(13) 0.0183(6) Uani 1 1 d . U . . . N2 N 0.5289(3) 0.3087(3) 0.25654(14) 0.0216(6) Uani 1 1 d D U . . . H2 H 0.589(3) 0.264(3) 0.2764(18) 0.026 Uiso 1 1 d D U . . . C20 C 0.5469(4) 0.4588(4) 0.37535(18) 0.0275(8) Uani 1 1 d . U . . . O1 O 0.6214(3) 0.5127(3) 0.40771(14) 0.0460(8) Uani 1 1 d . U . . . C1 C 0.4446(4) 0.2236(3) 0.21676(17) 0.0239(8) Uani 1 1 d . U . . . H1A H 0.4642 0.1454 0.2339 0.029 Uiso 1 1 calc R U . . . H1B H 0.4643 0.2251 0.1741 0.029 Uiso 1 1 calc R U . . . C2 C 0.3043(4) 0.2470(3) 0.21316(16) 0.0209(7) Uani 1 1 d . U . . . C3 C 0.2110(4) 0.2037(3) 0.16679(17) 0.0255(8) Uani 1 1 d . U . . . H3 H 0.2337 0.1634 0.1324 0.031 Uiso 1 1 calc R U . . . C4 C 0.0836(4) 0.2196(3) 0.17084(17) 0.0271(8) Uani 1 1 d . U . . . H4 H 0.0180 0.1891 0.1397 0.033 Uiso 1 1 calc R U . . . C5 C 0.0534(4) 0.2804(3) 0.22080(17) 0.0250(8) Uani 1 1 d . U . . . H5 H -0.0333 0.2906 0.2247 0.030 Uiso 1 1 calc R U . . . C6 C 0.1502(3) 0.3264(3) 0.26506(16) 0.0198(7) Uani 1 1 d . U . . . C7 C 0.1257(3) 0.4037(3) 0.31696(16) 0.0219(8) Uani 1 1 d . U . . . H7A H 0.0564 0.3707 0.3363 0.026 Uiso 1 1 calc R U . . . H7B H 0.0973 0.4801 0.2997 0.026 Uiso 1 1 calc R U . . . C8 C 0.2501(3) 0.5598(3) 0.41179(16) 0.0212(7) Uani 1 1 d . U . . . C9 C 0.2070(4) 0.5712(4) 0.46810(18) 0.0312(9) Uani 1 1 d . U . . . H9 H 0.1878 0.5047 0.4900 0.037 Uiso 1 1 calc R U . . . C10 C 0.1919(5) 0.6796(4) 0.49212(19) 0.0371(10) Uani 1 1 d . U . . . H10 H 0.1624 0.6870 0.5306 0.045 Uiso 1 1 calc R U . . . C11 C 0.2193(4) 0.7772(4) 0.4609(2) 0.0344(10) Uani 1 1 d . U . . . H11 H 0.2096 0.8512 0.4780 0.041 Uiso 1 1 calc R U . . . C12 C 0.2612(4) 0.7664(3) 0.40450(18) 0.0299(9) Uani 1 1 d . U . . . H12 H 0.2786 0.8333 0.3824 0.036 Uiso 1 1 calc R U . . . C13 C 0.2776(4) 0.6587(3) 0.38030(17) 0.0258(8) Uani 1 1 d . U . . . H13 H 0.3078 0.6519 0.3420 0.031 Uiso 1 1 calc R U . . . C14 C 0.2671(4) 0.3148(3) 0.43853(16) 0.0212(7) Uani 1 1 d . U . . . C15 C 0.3827(4) 0.2755(4) 0.47228(17) 0.0277(8) Uani 1 1 d . U . . . H15 H 0.4607 0.3062 0.4639 0.033 Uiso 1 1 calc R U . . . C16 C 0.3852(4) 0.1922(4) 0.51799(19) 0.0351(10) Uani 1 1 d . U . . . H16 H 0.4646 0.1669 0.5413 0.042 Uiso 1 1 calc R U . . . C17 C 0.2721(4) 0.1456(4) 0.52965(19) 0.0362(10) Uani 1 1 d . U . . . H17 H 0.2736 0.0872 0.5602 0.043 Uiso 1 1 calc R U . . . C18 C 0.1573(4) 0.1847(4) 0.49662(19) 0.0367(10) Uani 1 1 d . U . . . H18 H 0.0796 0.1536 0.5050 0.044 Uiso 1 1 calc R U . . . C19 C 0.1542(4) 0.2688(4) 0.45131(17) 0.0289(9) Uani 1 1 d . U . . . H19 H 0.0745 0.2951 0.4289 0.035 Uiso 1 1 calc R U . . . C21 C 0.5848(4) 0.3965(3) 0.22225(16) 0.0197(7) Uani 1 1 d . U . . . C22 C 0.5111(4) 0.4527(3) 0.17189(17) 0.0252(8) Uani 1 1 d . U . . . H22 H 0.4228 0.4356 0.1600 0.030 Uiso 1 1 calc R U . . . C23 C 0.5679(4) 0.5337(3) 0.13932(18) 0.0307(9) Uani 1 1 d . U . . . H23 H 0.5181 0.5716 0.1046 0.037 Uiso 1 1 calc R U . . . C24 C 0.6957(4) 0.5604(3) 0.15645(19) 0.0298(9) Uani 1 1 d . U . . . H24 H 0.7344 0.6149 0.1332 0.036 Uiso 1 1 calc R U . . . C25 C 0.7669(4) 0.5069(3) 0.20795(19) 0.0286(9) Uani 1 1 d . U . . . H25 H 0.8546 0.5260 0.2205 0.034 Uiso 1 1 calc R U . . . C26 C 0.7121(4) 0.4255(3) 0.24147(18) 0.0253(8) Uani 1 1 d . U . . . H26 H 0.7612 0.3901 0.2772 0.030 Uiso 1 1 calc R U . . . P2 P 0.16328(9) 0.62625(9) 0.15430(4) 0.0240(2) Uani 1 1 d . U . . . F1 F 0.1174(3) 0.6065(2) 0.08197(11) 0.0432(7) Uani 1 1 d . U . . . F2 F 0.2013(2) 0.4944(2) 0.16359(12) 0.0391(6) Uani 1 1 d . U . . . F3 F 0.2141(3) 0.6503(3) 0.22736(12) 0.0588(8) Uani 1 1 d . U . . . F4 F 0.1281(2) 0.7611(2) 0.14535(11) 0.0371(6) Uani 1 1 d . U . . . F5 F 0.3042(2) 0.6567(2) 0.14267(15) 0.0494(7) Uani 1 1 d . U . . . F6 F 0.0254(3) 0.6017(3) 0.16739(16) 0.0582(8) Uani 1 1 d . U . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Rh1 0.01640(17) 0.02461(18) 0.01559(16) 0.00082(11) 0.00457(11) -0.00127(11) P1 0.0181(5) 0.0252(5) 0.0139(4) 0.0005(3) 0.0045(4) -0.0005(4) N1 0.0200(15) 0.0194(15) 0.0162(13) 0.0023(11) 0.0050(11) -0.0002(12) N2 0.0193(16) 0.0234(16) 0.0228(15) 0.0023(12) 0.0058(12) 0.0034(12) C20 0.024(2) 0.036(2) 0.0232(18) 0.0045(16) 0.0074(15) -0.0053(17) O1 0.0414(19) 0.059(2) 0.0344(16) -0.0041(15) -0.0026(14) -0.0235(16) C1 0.0251(19) 0.0243(19) 0.0242(18) -0.0036(15) 0.0095(15) -0.0028(15) C2 0.0229(18) 0.0198(17) 0.0212(17) 0.0018(13) 0.0075(14) -0.0001(14) C3 0.031(2) 0.028(2) 0.0181(17) -0.0012(14) 0.0070(15) -0.0002(16) C4 0.027(2) 0.030(2) 0.0228(18) -0.0034(15) 0.0004(15) -0.0010(16) C5 0.0180(18) 0.032(2) 0.0245(18) 0.0027(15) 0.0035(14) -0.0004(15) C6 0.0188(17) 0.0244(18) 0.0168(16) 0.0045(13) 0.0047(13) 0.0009(14) C7 0.0172(18) 0.031(2) 0.0179(16) 0.0008(14) 0.0034(14) 0.0019(15) C8 0.0180(18) 0.0289(18) 0.0168(16) -0.0008(14) 0.0030(14) -0.0004(15) C9 0.044(3) 0.032(2) 0.0205(18) 0.0019(15) 0.0126(17) 0.0015(18) C10 0.053(3) 0.036(2) 0.026(2) -0.0060(16) 0.0188(19) 0.0021(19) C11 0.040(3) 0.029(2) 0.035(2) -0.0066(16) 0.0091(19) 0.0012(18) C12 0.035(2) 0.027(2) 0.028(2) 0.0024(15) 0.0085(17) -0.0045(17) C13 0.027(2) 0.0298(19) 0.0223(18) 0.0015(15) 0.0088(16) -0.0014(16) C14 0.0218(18) 0.0271(19) 0.0157(16) -0.0029(14) 0.0061(13) -0.0019(14) C15 0.0229(19) 0.039(2) 0.0213(18) 0.0072(16) 0.0034(15) -0.0024(16) C16 0.033(2) 0.044(2) 0.026(2) 0.0125(18) 0.0001(17) -0.0006(18) C17 0.043(2) 0.042(2) 0.0219(19) 0.0103(17) 0.0015(17) -0.0107(19) C18 0.035(2) 0.049(3) 0.027(2) 0.0075(18) 0.0063(17) -0.0158(19) C19 0.023(2) 0.041(2) 0.0216(18) 0.0063(16) 0.0014(15) -0.0051(17) C21 0.0216(18) 0.0235(18) 0.0161(16) -0.0020(13) 0.0095(14) -0.0007(14) C22 0.0203(19) 0.032(2) 0.0242(18) 0.0025(15) 0.0055(15) 0.0044(15) C23 0.038(2) 0.030(2) 0.0263(19) 0.0066(16) 0.0127(17) 0.0063(17) C24 0.038(2) 0.023(2) 0.033(2) -0.0005(16) 0.0197(17) -0.0026(16) C25 0.025(2) 0.029(2) 0.034(2) -0.0062(16) 0.0121(16) -0.0070(16) C26 0.0248(19) 0.0260(19) 0.0255(18) -0.0048(15) 0.0055(15) -0.0001(15) P2 0.0210(5) 0.0292(5) 0.0222(5) 0.0015(4) 0.0046(4) 0.0011(4) F1 0.0582(18) 0.0428(15) 0.0258(13) -0.0031(10) -0.0001(12) 0.0030(12) F2 0.0426(15) 0.0322(13) 0.0417(14) 0.0095(10) 0.0056(12) 0.0011(11) F3 0.084(2) 0.0581(17) 0.0273(13) -0.0008(12) -0.0083(14) 0.0038(16) F4 0.0365(14) 0.0341(13) 0.0377(13) -0.0033(10) -0.0012(11) 0.0077(10) F5 0.0267(13) 0.0462(15) 0.078(2) 0.0082(14) 0.0156(13) 0.0007(12) F6 0.0390(16) 0.0672(19) 0.077(2) 0.0002(16) 0.0342(15) -0.0070(14) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Rh1 C20 1.831(4) . ? Rh1 N1 2.053(3) . ? Rh1 N2 2.160(3) . ? Rh1 P1 2.2120(9) . ? P1 C8 1.817(4) . ? P1 C14 1.823(4) . ? P1 C7 1.849(4) . ? N1 C6 1.350(5) . ? N1 C2 1.356(5) . ? N2 C21 1.454(5) . ? N2 C1 1.501(5) . ? N2 H2 0.87(3) . ? C20 O1 1.147(5) . ? C1 C2 1.506(5) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 C3 1.377(5) . ? C3 C4 1.387(5) . ? C3 H3 0.9500 . ? C4 C5 1.384(5) . ? C4 H4 0.9500 . ? C5 C6 1.384(5) . ? C5 H5 0.9500 . ? C6 C7 1.503(5) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 C9 1.392(5) . ? C8 C13 1.397(5) . ? C9 C10 1.385(6) . ? C9 H9 0.9500 . ? C10 C11 1.380(6) . ? C10 H10 0.9500 . ? C11 C12 1.386(6) . ? C11 H11 0.9500 . ? C12 C13 1.382(6) . ? C12 H12 0.9500 . ? C13 H13 0.9500 . ? C14 C19 1.389(5) . ? C14 C15 1.391(5) . ? C15 C16 1.386(5) . ? C15 H15 0.9500 . ? C16 C17 1.385(6) . ? C16 H16 0.9500 . ? C17 C18 1.378(6) . ? C17 H17 0.9500 . ? C18 C19 1.386(6) . ? C18 H18 0.9500 . ? C19 H19 0.9500 . ? C21 C26 1.386(5) . ? C21 C22 1.390(5) . ? C22 C23 1.382(5) . ? C22 H22 0.9500 . ? C23 C24 1.380(6) . ? C23 H23 0.9500 . ? C24 C25 1.383(6) . ? C24 H24 0.9500 . ? C25 C26 1.386(5) . ? C25 H25 0.9500 . ? C26 H26 0.9500 . ? P2 F6 1.571(3) . ? P2 F1 1.580(3) . ? P2 F2 1.589(3) . ? P2 F5 1.605(3) . ? P2 F3 1.610(3) . ? P2 F4 1.615(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C20 Rh1 N1 175.19(15) . . ? C20 Rh1 N2 101.55(15) . . ? N1 Rh1 N2 80.91(12) . . ? C20 Rh1 P1 94.32(12) . . ? N1 Rh1 P1 83.59(8) . . ? N2 Rh1 P1 163.53(9) . . ? C8 P1 C14 105.92(16) . . ? C8 P1 C7 103.80(17) . . ? C14 P1 C7 108.70(17) . . ? C8 P1 Rh1 124.11(12) . . ? C14 P1 Rh1 112.08(12) . . ? C7 P1 Rh1 101.05(12) . . ? C6 N1 C2 120.0(3) . . ? C6 N1 Rh1 122.6(2) . . ? C2 N1 Rh1 117.2(2) . . ? C21 N2 C1 115.0(3) . . ? C21 N2 Rh1 112.1(2) . . ? C1 N2 Rh1 108.1(2) . . ? C21 N2 H2 110(3) . . ? C1 N2 H2 102(3) . . ? Rh1 N2 H2 109(3) . . ? O1 C20 Rh1 176.0(4) . . ? N2 C1 C2 113.2(3) . . ? N2 C1 H1A 108.9 . . ? C2 C1 H1A 108.9 . . ? N2 C1 H1B 108.9 . . ? C2 C1 H1B 108.9 . . ? H1A C1 H1B 107.7 . . ? N1 C2 C3 121.2(3) . . ? N1 C2 C1 115.4(3) . . ? C3 C2 C1 123.3(3) . . ? C2 C3 C4 119.2(3) . . ? C2 C3 H3 120.4 . . ? C4 C3 H3 120.4 . . ? C5 C4 C3 119.1(4) . . ? C5 C4 H4 120.4 . . ? C3 C4 H4 120.4 . . ? C4 C5 C6 119.7(3) . . ? C4 C5 H5 120.1 . . ? C6 C5 H5 120.1 . . ? N1 C6 C5 120.6(3) . . ? N1 C6 C7 116.2(3) . . ? C5 C6 C7 123.1(3) . . ? C6 C7 P1 111.0(3) . . ? C6 C7 H7A 109.4 . . ? P1 C7 H7A 109.4 . . ? C6 C7 H7B 109.4 . . ? P1 C7 H7B 109.4 . . ? H7A C7 H7B 108.0 . . ? C9 C8 C13 119.1(4) . . ? C9 C8 P1 122.4(3) . . ? C13 C8 P1 118.5(3) . . ? C10 C9 C8 119.9(4) . . ? C10 C9 H9 120.0 . . ? C8 C9 H9 120.0 . . ? C11 C10 C9 120.8(4) . . ? C11 C10 H10 119.6 . . ? C9 C10 H10 119.6 . . ? C10 C11 C12 119.5(4) . . ? C10 C11 H11 120.2 . . ? C12 C11 H11 120.2 . . ? C13 C12 C11 120.2(4) . . ? C13 C12 H12 119.9 . . ? C11 C12 H12 119.9 . . ? C12 C13 C8 120.4(3) . . ? C12 C13 H13 119.8 . . ? C8 C13 H13 119.8 . . ? C19 C14 C15 118.8(3) . . ? C19 C14 P1 122.9(3) . . ? C15 C14 P1 118.2(3) . . ? C16 C15 C14 120.6(4) . . ? C16 C15 H15 119.7 . . ? C14 C15 H15 119.7 . . ? C17 C16 C15 120.0(4) . . ? C17 C16 H16 120.0 . . ? C15 C16 H16 120.0 . . ? C18 C17 C16 119.6(4) . . ? C18 C17 H17 120.2 . . ? C16 C17 H17 120.2 . . ? C17 C18 C19 120.6(4) . . ? C17 C18 H18 119.7 . . ? C19 C18 H18 119.7 . . ? C18 C19 C14 120.3(4) . . ? C18 C19 H19 119.8 . . ? C14 C19 H19 119.8 . . ? C26 C21 C22 120.3(3) . . ? C26 C21 N2 118.9(3) . . ? C22 C21 N2 120.7(3) . . ? C23 C22 C21 119.2(4) . . ? C23 C22 H22 120.4 . . ? C21 C22 H22 120.4 . . ? C24 C23 C22 121.1(4) . . ? C24 C23 H23 119.5 . . ? C22 C23 H23 119.5 . . ? C23 C24 C25 119.1(4) . . ? C23 C24 H24 120.4 . . ? C25 C24 H24 120.4 . . ? C24 C25 C26 120.9(4) . . ? C24 C25 H25 119.6 . . ? C26 C25 H25 119.6 . . ? C21 C26 C25 119.3(4) . . ? C21 C26 H26 120.4 . . ? C25 C26 H26 120.4 . . ? F6 P2 F1 91.39(17) . . ? F6 P2 F2 91.51(16) . . ? F1 P2 F2 90.70(14) . . ? F6 P2 F5 177.39(18) . . ? F1 P2 F5 90.22(16) . . ? F2 P2 F5 90.53(14) . . ? F6 P2 F3 90.58(18) . . ? F1 P2 F3 177.64(18) . . ? F2 P2 F3 90.56(15) . . ? F5 P2 F3 87.77(18) . . ? F6 P2 F4 89.67(15) . . ? F1 P2 F4 89.87(14) . . ? F2 P2 F4 178.68(15) . . ? F5 P2 F4 88.28(14) . . ? F3 P2 F4 88.83(15) . . ? _refine_diff_density_max 1.316 _refine_diff_density_min -0.757 _refine_diff_density_rms 0.104 _shelx_res_file ; TZ888_2_0m_a.res created by SHELXL-2014/7 TITL TZ888_2_0m_a.res in P2(1)/c CELL 0.71073 10.6439 11.6245 21.7819 90.000 100.416 90.000 ZERR 4.000 0.0013 0.0014 0.0025 0.000 0.002 0.000 LATT 1 SYMM -X, 1/2+Y, 1/2-Z SFAC C H N O F P Rh UNIT 104 92 8 4 24 8 4 REM Old TITL TZ888_2_0m in P2(1)/c REM SHELXT solution in P2(1)/c REM R1 0.093, Rweak 0.002, Alpha 0.030, Orientation as input REM Formula found by SHELXT: C26 N O2 F6 P2 Rh L.S. 10 BOND $H FMAP 2 ACTA OMIT 0 1 1 OMIT 1 0 0 OMIT -2 50 PLAN 10 SIZE 0.112 0.319 0.389 DFIX 0.9 0.03 N2 H2 RIGU TEMP -123.140 WGHT 0.052400 5.018300 FVAR 0.28576 RH1 7 0.421785 0.382074 0.322214 11.00000 0.01640 0.02461 = 0.01559 0.00082 0.00457 -0.00127 P1 6 0.271154 0.420558 0.377100 11.00000 0.01806 0.02520 = 0.01389 0.00049 0.00452 -0.00050 N1 3 0.273874 0.309105 0.261087 11.00000 0.02002 0.01943 = 0.01620 0.00227 0.00502 -0.00018 N2 3 0.528942 0.308668 0.256545 11.00000 0.01926 0.02340 = 0.02282 0.00227 0.00584 0.00340 H2 2 0.588666 0.264021 0.276439 11.00000 -1.20000 C20 1 0.546902 0.458786 0.375347 11.00000 0.02415 0.03637 = 0.02316 0.00449 0.00740 -0.00529 O1 4 0.621406 0.512662 0.407710 11.00000 0.04144 0.05859 = 0.03444 -0.00412 -0.00264 -0.02346 C1 1 0.444631 0.223589 0.216761 11.00000 0.02506 0.02428 = 0.02418 -0.00362 0.00952 -0.00279 AFIX 23 H1A 2 0.464178 0.145414 0.233879 11.00000 -1.20000 H1B 2 0.464334 0.225138 0.174056 11.00000 -1.20000 AFIX 0 C2 1 0.304307 0.247004 0.213165 11.00000 0.02294 0.01981 = 0.02117 0.00183 0.00748 -0.00009 C3 1 0.211041 0.203713 0.166793 11.00000 0.03102 0.02823 = 0.01807 -0.00117 0.00701 -0.00019 AFIX 43 H3 2 0.233690 0.163438 0.132438 11.00000 -1.20000 AFIX 0 C4 1 0.083618 0.219611 0.170839 11.00000 0.02654 0.03040 = 0.02284 -0.00343 0.00040 -0.00099 AFIX 43 H4 2 0.017954 0.189125 0.139709 11.00000 -1.20000 AFIX 0 C5 1 0.053415 0.280442 0.220803 11.00000 0.01801 0.03235 = 0.02453 0.00272 0.00349 -0.00040 AFIX 43 H5 2 -0.033340 0.290621 0.224725 11.00000 -1.20000 AFIX 0 C6 1 0.150184 0.326410 0.265056 11.00000 0.01876 0.02445 = 0.01683 0.00452 0.00466 0.00094 C7 1 0.125662 0.403685 0.316959 11.00000 0.01724 0.03078 = 0.01787 0.00078 0.00339 0.00194 AFIX 23 H7A 2 0.056376 0.370735 0.336288 11.00000 -1.20000 H7B 2 0.097330 0.480081 0.299688 11.00000 -1.20000 AFIX 0 C8 1 0.250094 0.559815 0.411788 11.00000 0.01796 0.02888 = 0.01678 -0.00085 0.00303 -0.00038 C9 1 0.206954 0.571226 0.468097 11.00000 0.04377 0.03194 = 0.02052 0.00191 0.01261 0.00150 AFIX 43 H9 2 0.187832 0.504725 0.490034 11.00000 -1.20000 AFIX 0 C10 1 0.191927 0.679650 0.492122 11.00000 0.05348 0.03567 = 0.02643 -0.00603 0.01877 0.00206 AFIX 43 H10 2 0.162381 0.686969 0.530564 11.00000 -1.20000 AFIX 0 C11 1 0.219344 0.777199 0.460908 11.00000 0.04021 0.02940 = 0.03454 -0.00663 0.00914 0.00120 AFIX 43 H11 2 0.209611 0.851196 0.477960 11.00000 -1.20000 AFIX 0 C12 1 0.261183 0.766423 0.404500 11.00000 0.03500 0.02737 = 0.02831 0.00242 0.00854 -0.00447 AFIX 43 H12 2 0.278619 0.833294 0.382411 11.00000 -1.20000 AFIX 0 C13 1 0.277606 0.658720 0.380303 11.00000 0.02699 0.02984 = 0.02226 0.00145 0.00882 -0.00145 AFIX 43 H13 2 0.307806 0.651902 0.342004 11.00000 -1.20000 AFIX 0 C14 1 0.267128 0.314835 0.438526 11.00000 0.02177 0.02715 = 0.01565 -0.00289 0.00614 -0.00193 C15 1 0.382729 0.275548 0.472283 11.00000 0.02291 0.03885 = 0.02126 0.00719 0.00341 -0.00239 AFIX 43 H15 2 0.460669 0.306152 0.463927 11.00000 -1.20000 AFIX 0 C16 1 0.385249 0.192173 0.517992 11.00000 0.03259 0.04435 = 0.02624 0.01248 0.00005 -0.00060 AFIX 43 H16 2 0.464605 0.166943 0.541323 11.00000 -1.20000 AFIX 0 C17 1 0.272087 0.145646 0.529652 11.00000 0.04331 0.04160 = 0.02190 0.01026 0.00149 -0.01069 AFIX 43 H17 2 0.273610 0.087172 0.560246 11.00000 -1.20000 AFIX 0 C18 1 0.157295 0.184664 0.496620 11.00000 0.03494 0.04898 = 0.02652 0.00747 0.00631 -0.01580 AFIX 43 H18 2 0.079570 0.153598 0.504982 11.00000 -1.20000 AFIX 0 C19 1 0.154203 0.268813 0.451310 11.00000 0.02296 0.04112 = 0.02158 0.00631 0.00144 -0.00513 AFIX 43 H19 2 0.074480 0.295150 0.428886 11.00000 -1.20000 AFIX 0 C21 1 0.584755 0.396508 0.222253 11.00000 0.02163 0.02351 = 0.01610 -0.00199 0.00953 -0.00075 C22 1 0.511100 0.452672 0.171893 11.00000 0.02033 0.03153 = 0.02424 0.00255 0.00547 0.00442 AFIX 43 H22 2 0.422771 0.435559 0.160007 11.00000 -1.20000 AFIX 0 C23 1 0.567874 0.533697 0.139317 11.00000 0.03846 0.02989 = 0.02632 0.00662 0.01273 0.00625 AFIX 43 H23 2 0.518072 0.571587 0.104579 11.00000 -1.20000 AFIX 0 C24 1 0.695745 0.560430 0.156450 11.00000 0.03836 0.02304 = 0.03282 -0.00046 0.01970 -0.00257 AFIX 43 H24 2 0.734371 0.614914 0.133177 11.00000 -1.20000 AFIX 0 C25 1 0.766915 0.506851 0.207949 11.00000 0.02527 0.02902 = 0.03413 -0.00617 0.01209 -0.00698 AFIX 43 H25 2 0.854551 0.526042 0.220521 11.00000 -1.20000 AFIX 0 C26 1 0.712076 0.425516 0.241467 11.00000 0.02475 0.02599 = 0.02549 -0.00479 0.00550 -0.00006 AFIX 43 H26 2 0.761233 0.390059 0.277210 11.00000 -1.20000 AFIX 0 P2 6 0.163276 0.626246 0.154301 11.00000 0.02101 0.02924 = 0.02217 0.00153 0.00464 0.00110 F1 5 0.117418 0.606472 0.081966 11.00000 0.05820 0.04282 = 0.02577 -0.00312 -0.00006 0.00300 F2 5 0.201278 0.494358 0.163590 11.00000 0.04255 0.03222 = 0.04167 0.00952 0.00561 0.00106 F3 5 0.214082 0.650345 0.227364 11.00000 0.08421 0.05813 = 0.02733 -0.00076 -0.00830 0.00376 F4 5 0.128086 0.761057 0.145351 11.00000 0.03653 0.03415 = 0.03768 -0.00328 -0.00125 0.00767 F5 5 0.304183 0.656696 0.142675 11.00000 0.02673 0.04618 = 0.07763 0.00824 0.01557 0.00072 F6 5 0.025385 0.601701 0.167391 11.00000 0.03903 0.06715 = 0.07730 0.00016 0.03416 -0.00699 HKLF 4 REM TZ888_2_0m_a.res in P2(1)/c REM R1 = 0.0382 for 3905 Fo > 4sig(Fo) and 0.0510 for all 4661 data REM 346 parameters refined using 334 restraints END WGHT 0.0441 5.5073 REM Highest difference peak 1.316, deepest hole -0.757, 1-sigma level 0.104 Q1 1 0.3987 0.4644 0.3224 11.00000 0.05 1.32 Q2 1 0.4078 0.2976 0.3252 11.00000 0.05 1.14 Q3 1 0.2645 0.8825 0.4677 11.00000 0.05 0.85 Q4 1 0.2593 0.5049 0.3905 11.00000 0.05 0.58 Q5 1 0.2635 0.3394 0.3829 11.00000 0.05 0.58 Q6 1 0.2630 0.6167 0.1096 11.00000 0.05 0.54 Q7 1 0.1070 0.6966 0.1531 11.00000 0.05 0.54 Q8 1 0.2632 0.3810 0.4325 11.00000 0.05 0.48 Q9 1 0.1416 0.6056 0.2280 11.00000 0.05 0.47 Q10 1 0.2814 0.6241 0.2127 11.00000 0.05 0.44 ; _shelx_res_checksum 20373 _shelx_hkl_file ; -1 0 0 -3.90 0.60 1 0 0 -3.50 0.60 -2 0 0 2958.60 231.88 -2 0 0 2700.63 231.88 2 0 0 2716.83 231.98 2 0 0 2987.40 231.88 3 0 0 1526.85 128.39 3 0 0 1638.94 128.29 -3 0 0 1459.15 128.29 -3 0 0 1631.04 128.29 4 0 0 85.49 9.60 -4 0 0 86.49 8.80 4 0 0 89.89 9.10 -4 0 0 92.39 9.50 -5 0 0 421.66 34.60 5 0 0 420.96 34.40 -5 0 0 398.06 34.80 5 0 0 386.96 34.70 -6 0 0 1525.65 129.19 6 0 0 1596.24 128.99 -6 0 0 1526.25 128.99 6 0 0 1619.74 129.39 -7 0 0 2813.32 228.28 -7 0 0 2654.03 227.98 7 0 0 2732.13 228.28 7 0 0 2916.81 227.98 8 0 0 155.28 16.90 -8 0 0 142.99 17.30 8 0 0 163.58 18.20 -8 0 0 178.78 18.10 9 0 0 80.39 12.50 -9 0 0 97.99 13.30 9 0 0 109.19 12.60 -9 0 0 100.99 13.10 10 0 0 -8.30 7.40 -10 0 0 -6.30 9.10 -10 0 0 -8.60 8.20 10 0 0 -7.20 8.80 -11 0 0 30.90 11.60 11 0 0 21.20 10.00 11 0 0 15.20 12.20 -11 0 0 26.30 11.20 -12 0 0 74.39 14.40 12 0 0 82.19 17.30 12 0 0 119.19 15.80 -12 0 0 92.09 17.70 -13 0 0 140.99 21.80 13 0 0 138.39 20.70 13 0 0 181.98 24.40 -13 0 0 217.08 25.20 -14 0 0 203.18 25.40 14 0 0 98.59 29.00 14 0 0 148.89 23.70 0 -1 0 -1.40 0.40 0 1 0 -0.80 0.50 -2 -1 0 2139.99 165.28 2 -1 0 2000.80 165.28 2 -1 0 2232.78 165.28 -2 -1 0 1925.51 165.28 -2 1 0 1980.60 165.28 2 1 0 2037.90 165.18 2 1 0 1898.31 165.28 -2 1 0 1969.30 165.28 3 -1 0 1884.61 148.39 3 -1 0 1748.33 148.39 -3 -1 0 1842.02 148.49 -3 -1 0 1870.81 148.39 3 1 0 1670.53 148.39 -3 1 0 1921.61 148.39 3 1 0 1798.02 148.29 -3 1 0 1768.82 148.39 4 -1 0 98.19 9.40 4 -1 0 91.59 9.90 -4 -1 0 89.99 9.90 -4 -1 0 86.29 9.20 4 1 0 102.69 9.40 -4 1 0 95.19 9.50 -4 1 0 94.59 9.70 4 1 0 85.89 10.00 5 -1 0 440.76 35.40 -5 -1 0 414.16 35.80 5 -1 0 394.36 35.50 -5 -1 0 444.16 35.50 5 1 0 431.66 35.40 -5 1 0 399.66 35.60 -5 1 0 424.36 35.50 5 1 0 394.06 35.60 -6 -1 0 16.00 5.10 6 -1 0 20.20 5.70 6 -1 0 15.80 4.60 -6 -1 0 8.80 5.00 -6 1 0 16.00 5.10 6 1 0 8.20 5.60 6 1 0 18.10 4.80 -6 1 0 13.80 4.90 7 -1 0 188.98 18.10 -7 -1 0 156.68 17.60 7 -1 0 173.78 18.30 -7 -1 0 197.78 19.00 7 1 0 191.98 18.50 -7 1 0 198.58 18.60 -7 1 0 199.98 21.20 7 1 0 189.18 18.00 -8 -1 0 292.67 28.50 -8 -1 0 303.97 27.90 8 -1 0 286.87 28.00 8 -1 0 325.07 27.30 8 1 0 301.97 28.70 8 1 0 301.37 27.60 -8 1 0 308.47 28.20 -8 1 0 297.07 28.00 -9 -1 0 175.48 21.00 -9 -1 0 206.58 20.80 9 -1 0 170.68 19.90 9 -1 0 210.98 20.80 -9 1 0 193.98 21.00 9 1 0 191.78 20.00 9 1 0 189.18 20.60 -9 1 0 188.48 19.80 -10 -1 0 35.00 9.90 10 -1 0 46.30 11.60 10 -1 0 32.00 8.40 -10 -1 0 32.40 10.60 -10 1 0 42.00 10.20 -10 1 0 44.10 11.00 10 1 0 23.70 8.30 10 1 0 32.70 10.90 -11 -1 0 132.59 17.00 -11 -1 0 116.09 17.50 11 -1 0 146.79 17.50 11 -1 0 132.89 17.70 -11 1 0 108.99 17.10 11 1 0 143.19 16.90 11 1 0 154.38 18.70 12 -1 0 11.30 10.60 -12 -1 0 27.20 14.00 -12 -1 0 13.10 10.70 12 -1 0 15.10 14.10 -12 1 0 24.40 12.40 -12 1 0 16.10 13.90 12 1 0 10.10 13.20 13 -1 0 5.80 12.80 -13 -1 0 16.30 15.80 13 -1 0 34.50 15.60 -13 -1 0 28.40 13.60 13 1 0 11.20 13.40 -13 1 0 27.00 14.60 -13 1 0 15.50 17.40 13 1 0 20.90 17.20 14 -1 0 2.70 15.10 -14 -1 0 45.10 18.90 14 1 0 31.60 19.40 14 1 0 68.89 20.90 -14 1 0 19.50 18.00 0 -2 0 692.73 54.19 0 2 0 627.64 54.19 1 -2 0 445.26 37.00 -1 -2 0 429.36 37.10 -1 2 0 469.35 37.10 -1 2 0 440.66 37.00 1 2 0 448.96 37.00 1 2 0 468.15 37.10 2 -2 0 53.69 5.80 2 -2 0 57.29 5.50 -2 -2 0 51.49 5.50 -2 -2 0 56.09 5.90 2 2 0 51.09 5.50 -2 2 0 53.49 5.80 -2 2 0 64.89 5.80 2 2 0 50.89 5.90 3 -2 0 18.80 3.50 -3 -2 0 17.60 3.40 -3 -2 0 19.30 3.70 3 -2 0 24.10 3.40 3 2 0 26.10 3.90 3 2 0 20.70 3.30 -3 2 0 19.00 3.40 -3 2 0 25.70 3.60 4 -2 0 77.79 8.40 -4 -2 0 76.79 8.90 -4 -2 0 77.89 8.00 4 -2 0 73.99 8.60 -4 2 0 82.89 8.50 4 2 0 69.79 8.40 4 2 0 72.49 8.30 -4 2 0 85.69 8.60 5 -2 0 138.19 13.10 -5 -2 0 123.79 13.10 -5 -2 0 126.69 12.70 5 -2 0 153.68 13.10 -5 2 0 131.39 13.20 5 2 0 127.09 13.70 5 2 0 141.29 12.90 -5 2 0 124.89 12.70 -6 -2 0 28.10 6.10 6 -2 0 22.30 5.10 6 -2 0 32.10 5.80 -6 -2 0 32.70 5.70 -6 2 0 33.00 5.50 6 2 0 30.60 6.60 -6 2 0 27.10 5.60 6 2 0 20.90 5.00 7 -2 0 -2.00 5.80 -7 -2 0 1.30 4.70 -7 -2 0 5.90 6.00 7 -2 0 7.20 4.60 7 2 0 5.30 6.00 -7 2 0 8.70 5.60 -7 2 0 3.40 4.90 7 2 0 0.30 5.00 8 -2 0 -3.70 6.80 -8 -2 0 -3.80 5.30 8 -2 0 2.30 5.70 -8 -2 0 -10.10 6.10 -8 2 0 -4.20 6.30 8 2 0 -10.60 6.90 8 2 0 -8.20 5.80 -8 2 0 -3.50 6.30 9 -2 0 13.00 7.20 9 -2 0 17.30 8.80 -9 -2 0 12.00 7.70 -9 -2 0 17.70 8.30 -9 2 0 6.10 8.40 9 2 0 7.50 8.70 9 2 0 -2.10 7.00 -9 2 0 8.20 7.70 10 -2 0 6.60 7.90 -10 -2 0 6.40 9.20 -10 -2 0 -3.00 8.60 10 -2 0 -12.00 9.20 10 2 0 -9.00 9.30 -10 2 0 18.60 9.80 10 2 0 6.80 7.80 -10 2 0 8.10 8.80 11 -2 0 -19.60 10.50 -11 -2 0 2.60 10.30 -11 -2 0 -18.10 9.20 -11 2 0 -6.00 10.20 -11 2 0 0.50 11.50 11 2 0 0.30 9.40 11 2 0 4.40 10.70 12 -2 0 12.10 13.90 -12 -2 0 20.30 11.30 12 -2 0 -16.20 10.40 -12 -2 0 -7.70 12.90 12 2 0 17.00 13.80 -12 2 0 27.20 13.80 12 2 0 4.70 11.20 -12 2 0 13.80 12.70 -13 -2 0 17.30 17.20 13 -2 0 33.40 16.60 13 -2 0 49.30 13.70 -13 -2 0 30.60 16.30 13 2 0 43.40 19.00 -13 2 0 57.09 15.40 13 2 0 24.80 14.50 -13 2 0 91.99 22.20 14 -2 0 4.60 15.90 -14 -2 0 16.30 18.00 14 2 0 24.60 17.00 14 2 0 20.90 19.70 -14 2 0 -6.20 18.00 0 -3 0 -2.10 1.60 0 3 0 -0.90 1.60 0 3 0 -0.20 1.60 1 -3 0 9.30 2.20 1 -3 0 9.50 2.00 -1 -3 0 4.90 2.00 -1 -3 0 10.10 2.20 -1 3 0 8.20 2.00 1 3 0 10.70 2.40 -1 3 0 9.70 2.20 1 3 0 11.40 2.10 -2 -3 0 1079.89 95.89 2 -3 0 1270.97 95.89 2 -3 0 1194.28 95.99 -2 3 0 1228.68 95.99 -2 3 0 1130.49 95.89 2 3 0 1138.29 95.99 2 3 0 1148.59 95.79 -3 -3 0 121.19 11.30 3 -3 0 128.79 11.60 -3 -3 0 104.99 11.50 3 -3 0 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163.88 14.70 -2 6 0 156.58 14.30 2 6 0 154.48 14.80 3 -6 0 38.70 5.50 -3 -6 0 43.30 5.60 3 -6 0 47.30 6.30 -3 -6 0 33.00 5.40 -3 6 0 41.30 5.60 3 6 0 48.80 5.60 -3 6 0 63.09 7.20 3 6 0 51.49 6.30 -4 -6 0 30.60 5.20 4 -6 0 31.10 5.00 4 -6 0 21.00 5.30 -4 -6 0 26.70 5.10 -4 6 0 27.40 5.00 -4 6 0 21.10 5.10 4 6 0 34.20 5.80 4 6 0 26.20 4.70 5 -6 0 59.49 7.90 -5 -6 0 49.20 7.30 5 -6 0 51.59 6.80 -5 -6 0 51.79 7.30 -5 6 0 61.99 7.20 -5 6 0 39.30 6.60 5 6 0 44.90 7.40 5 6 0 42.70 6.70 -6 -6 0 231.18 19.90 6 -6 0 195.88 19.20 6 -6 0 181.28 18.70 -6 -6 0 189.18 19.30 -6 6 0 178.28 19.20 6 6 0 215.38 20.20 -6 6 0 196.78 18.90 6 6 0 216.48 19.10 -7 -6 0 217.18 23.00 7 -6 0 220.28 23.20 7 -6 0 227.78 22.00 -7 -6 0 234.18 22.50 7 6 0 256.27 22.90 -7 6 0 243.38 22.50 7 6 0 257.27 22.30 -7 6 0 202.78 21.80 8 -6 0 2.00 7.70 8 -6 0 -1.40 6.10 -8 -6 0 0.20 7.20 -8 -6 0 4.70 7.80 8 6 0 20.30 8.70 -8 6 0 3.90 7.30 -8 6 0 -6.40 8.50 8 6 0 7.90 7.00 -9 -6 0 -7.60 9.20 -9 -6 0 -5.30 7.80 9 -6 0 -0.90 9.40 9 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17.20 10 -7 0 102.39 14.20 -10 -7 0 100.09 15.60 -10 -7 0 114.49 16.30 -10 7 0 78.59 15.30 10 7 0 79.49 14.50 10 7 0 102.89 15.60 -10 7 0 98.69 14.50 -11 -7 0 10.30 11.90 11 -7 0 -13.80 14.00 11 -7 0 17.40 11.30 -11 -7 0 7.60 13.40 11 7 0 -7.10 13.80 11 7 0 18.40 12.60 -11 7 0 32.70 12.50 12 -7 0 9.80 12.20 -12 -7 0 11.50 16.30 12 7 0 3.30 16.20 -12 7 0 -0.70 13.60 12 7 0 -4.00 18.20 0 -8 0 488.55 41.40 0 -8 0 538.05 41.50 0 8 0 444.06 41.10 0 8 0 494.75 41.50 -1 -8 0 49.80 6.50 1 -8 0 50.29 6.50 -1 -8 0 56.29 6.80 1 8 0 41.80 6.50 -1 8 0 50.39 6.50 -1 8 0 52.09 6.30 1 8 0 48.70 6.20 2 -8 0 181.18 17.50 -2 -8 0 160.38 17.30 -2 -8 0 187.98 17.60 2 -8 0 209.28 17.80 2 8 0 202.48 17.70 2 8 0 189.98 17.90 -2 8 0 236.28 18.30 -2 8 0 184.58 17.50 3 -8 0 81.29 10.30 -3 -8 0 75.29 10.00 3 -8 0 91.19 9.60 -3 -8 0 63.99 9.20 3 8 0 78.69 10.10 3 8 0 78.29 9.60 -3 8 0 73.79 9.70 -3 8 0 96.79 10.30 4 -8 0 589.04 49.80 -4 -8 0 627.74 50.19 -4 -8 0 620.14 49.90 4 -8 0 534.75 49.99 -4 8 0 536.95 49.90 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0 -28 112.19 11.30 -3 0 28 3.20 4.00 -3 0 28 -3.50 6.40 3 0 -28 1.30 3.80 3 0 -28 -10.50 6.50 2 0 -28 268.67 21.60 -2 0 28 256.67 21.00 2 0 -28 181.78 19.50 -2 0 28 192.18 19.10 -1 0 28 54.19 7.60 1 0 -28 83.79 10.30 -1 0 28 50.79 9.50 1 0 -28 63.39 8.50 0 0 -28 56.49 10.10 0 0 28 40.70 10.10 0 0 28 32.40 7.30 0 0 -28 50.29 8.40 1 0 28 162.28 17.90 -1 0 -28 162.28 19.00 2 0 28 96.09 16.50 -2 0 -28 151.08 18.50 2 0 28 120.69 15.60 -7 -1 28 1.30 10.70 -7 -1 28 0.70 6.60 7 -1 -28 1.60 8.00 7 -1 -28 -1.10 5.00 7 1 -28 2.70 5.20 -7 1 28 -1.10 6.10 -6 -1 28 7.50 5.80 6 -1 -28 0.10 4.20 6 -1 -28 1.20 6.80 6 1 -28 10.00 5.00 -6 1 28 4.20 5.40 6 1 -28 11.20 8.50 5 -1 -28 12.20 5.90 -5 -1 28 9.60 8.80 5 -1 -28 12.30 3.90 -5 -1 28 11.50 5.40 -5 1 28 12.80 4.90 -5 1 28 18.00 5.50 5 1 -28 4.30 4.50 5 1 -28 -4.80 7.30 4 -1 -28 96.29 10.30 -4 -1 28 104.89 12.50 -4 -1 28 97.59 11.40 4 1 -28 93.79 11.30 -4 1 28 134.19 11.30 3 -1 -28 55.89 7.50 3 -1 -28 41.30 5.80 -3 -1 28 47.70 6.80 -3 -1 28 76.39 9.80 -3 1 28 48.30 6.50 -3 1 28 52.29 6.30 3 1 -28 44.90 6.80 3 1 -28 62.89 9.70 2 -1 -28 116.99 12.30 -2 -1 28 150.18 16.30 2 -1 -28 146.79 13.90 -2 -1 28 107.29 12.40 -2 1 28 112.99 11.30 2 1 -28 123.69 14.00 2 1 -28 94.29 12.80 -2 1 28 118.59 12.70 1 -1 -28 52.09 8.80 1 -1 -28 50.79 7.60 -1 -1 28 43.00 7.10 -1 -1 28 55.39 10.00 -1 1 28 45.60 7.90 -1 1 28 40.30 6.20 1 1 -28 49.00 7.70 0 -1 28 12.00 10.00 0 -1 -28 5.40 8.20 0 -1 -28 0.40 6.60 0 -1 28 -4.10 5.70 0 1 -28 -2.90 6.20 0 1 28 7.80 7.50 0 1 28 -5.00 5.30 0 1 -28 -13.00 9.60 -1 -1 -28 -12.20 9.50 1 -1 28 -4.60 7.00 -1 -1 -28 10.30 7.70 1 -1 28 12.70 11.40 1 1 28 4.20 6.80 -1 1 -28 -10.00 7.10 1 1 28 16.20 9.30 -2 -1 -28 7.10 8.90 2 -1 28 11.80 8.90 2 1 28 5.20 11.50 -2 1 -28 -2.80 8.70 2 1 28 25.20 10.00 -7 -2 28 2.90 12.00 7 -2 -28 1.90 5.30 7 -2 -28 13.00 7.80 7 2 -28 5.80 5.90 6 -2 -28 4.40 4.20 -6 -2 28 3.40 6.20 6 -2 -28 -5.30 5.70 6 2 -28 0.60 5.10 -5 -2 28 33.00 10.20 -5 -2 28 19.00 5.80 5 -2 -28 11.20 5.40 5 -2 -28 14.40 3.90 5 2 -28 11.50 9.10 5 2 -28 12.40 5.10 -4 -2 28 46.70 10.00 4 -2 -28 28.30 4.20 -4 -2 28 38.10 6.40 4 2 -28 26.70 5.80 -3 -2 28 9.60 8.80 -3 -2 28 1.50 5.00 3 -2 -28 5.20 3.00 3 -2 -28 4.70 4.50 3 2 -28 -2.90 4.70 3 2 -28 -9.50 9.00 2 -2 -28 21.40 5.70 -2 -2 28 9.40 5.40 2 -2 -28 14.30 4.40 -2 -2 28 -2.70 9.00 2 2 -28 15.60 5.60 2 2 -28 16.80 9.60 1 -2 -28 7.60 5.40 1 -2 -28 -11.20 6.30 -1 -2 28 -0.90 9.60 -1 -2 28 -8.10 5.30 1 2 -28 4.00 5.80 -1 2 28 4.50 3.40 1 2 -28 24.40 10.00 0 -2 -28 13.90 6.50 0 -2 28 18.70 6.60 0 -2 28 6.60 12.10 0 -2 -28 18.00 8.10 0 2 28 10.80 5.40 0 2 28 14.50 6.50 0 2 -28 4.00 6.70 -1 -2 -28 -7.70 7.60 1 -2 28 -7.40 7.10 -1 -2 -28 16.00 9.60 -1 2 -28 -6.00 7.30 1 2 28 -0.50 7.90 1 2 28 1.50 6.80 2 -2 28 16.50 10.00 -2 -2 -28 22.50 9.20 -2 2 -28 11.00 9.40 2 2 28 15.20 8.80 2 2 28 -6.10 9.80 6 -3 -28 9.20 4.90 -6 -3 28 14.10 6.70 6 -3 -28 18.50 6.20 6 3 -28 6.30 5.90 5 -3 -28 1.50 4.20 5 -3 -28 0.50 3.40 -5 -3 28 4.70 6.10 -5 -3 28 -6.80 12.20 5 3 -28 4.50 5.20 -4 -3 28 139.59 14.60 -4 -3 28 131.69 17.80 4 3 -28 126.29 14.40 -3 -3 28 133.99 14.80 -3 -3 28 155.58 20.60 3 3 -28 129.49 14.70 2 -3 -28 80.99 9.30 2 -3 -28 64.49 7.20 -2 -3 28 61.89 8.90 2 3 -28 53.09 8.60 1 -3 -28 23.80 6.60 1 -3 -28 15.40 5.90 -1 -3 28 18.30 6.20 1 3 -28 17.10 6.70 0 -3 28 29.80 7.80 0 -3 -28 15.00 7.30 0 -3 -28 20.70 8.20 0 3 28 17.00 5.10 0 3 28 17.10 5.70 0 3 -28 28.50 7.50 1 -3 28 -5.50 7.40 -1 -3 -28 26.40 9.30 -1 -3 -28 5.10 7.70 1 3 28 -8.20 6.60 -1 3 -28 8.40 8.00 1 3 28 -7.60 6.70 -5 -4 28 23.40 7.30 5 4 -28 28.50 7.00 -4 -4 28 78.69 9.80 4 4 -28 60.49 9.20 -3 -4 28 1.50 6.20 3 4 -28 0.30 5.70 -2 -4 28 140.19 15.10 2 4 -28 119.99 15.20 1 -4 -28 75.89 8.70 -1 -4 28 52.79 9.60 1 -4 -28 73.29 8.80 1 4 -28 60.39 9.60 0 -4 -28 48.80 9.30 0 -4 28 42.00 9.30 0 -4 -28 49.50 8.80 0 4 -28 45.90 9.00 0 4 28 42.40 6.20 -1 4 -28 103.89 13.80 -4 -5 28 49.70 9.10 4 5 -28 59.49 9.00 -3 -5 28 6.40 7.00 3 5 -28 3.20 6.30 -2 -5 28 6.40 6.90 2 5 -28 -4.70 6.10 1 -5 -28 48.90 6.80 -1 -5 28 43.10 9.20 1 -5 -28 66.89 8.50 1 5 -28 48.00 9.40 6 0 -29 -15.40 7.50 6 0 -29 -5.90 4.50 5 0 -29 -2.50 4.10 -5 0 29 -6.90 6.90 -5 0 29 2.00 5.20 5 0 -29 7.00 7.70 -4 0 29 17.00 4.70 4 0 -29 7.10 4.30 -4 0 29 18.10 7.10 3 0 -29 6.70 7.50 -3 0 29 6.90 4.70 3 0 -29 12.40 4.40 -3 0 29 17.70 6.70 -2 0 29 2.40 7.50 2 0 -29 -0.90 4.60 2 0 -29 2.60 7.80 -2 0 29 -0.50 4.60 1 0 -29 16.10 8.60 -1 0 29 5.70 5.00 1 0 -29 -5.20 5.50 -1 0 29 6.50 8.40 0 0 29 3.60 6.10 0 0 29 1.10 9.10 0 0 -29 -2.90 9.70 0 0 -29 11.20 6.80 5 -1 -29 37.30 7.60 5 -1 -29 25.40 5.10 -5 -1 29 34.70 10.00 -5 -1 29 32.40 6.60 -5 1 29 36.30 6.10 5 1 -29 28.50 5.80 -4 -1 29 7.60 5.20 4 -1 -29 -2.80 3.50 -4 -1 29 -4.20 8.70 4 1 -29 -8.70 8.60 4 1 -29 6.90 4.60 -3 -1 29 222.88 21.20 3 -1 -29 207.68 20.60 3 -1 -29 252.07 22.30 -3 -1 29 289.87 24.50 3 1 -29 217.08 21.50 3 1 -29 278.77 24.50 2 -1 -29 150.68 14.60 2 -1 -29 103.69 12.00 -2 -1 29 99.09 13.50 -2 -1 29 106.69 12.50 2 1 -29 102.49 12.70 2 1 -29 128.19 13.90 -2 1 29 94.79 10.50 -2 1 29 114.29 12.30 -1 -1 29 8.40 9.80 1 -1 -29 -3.00 8.00 -1 -1 29 10.30 5.60 1 -1 -29 8.30 5.90 -1 1 29 5.10 6.60 1 1 -29 8.80 9.70 1 1 -29 12.60 6.20 -1 1 29 0.40 4.30 0 -1 29 14.20 10.80 0 -1 -29 -5.00 9.20 0 -1 -29 -0.10 6.70 0 -1 29 2.80 6.40 0 1 29 -5.70 5.80 0 1 29 4.40 8.30 0 1 -29 6.90 6.70 5 -2 -29 204.18 20.30 5 -2 -29 278.67 21.50 -5 -2 29 229.78 21.80 5 2 -29 233.98 21.50 -4 -2 29 37.80 6.60 4 -2 -29 24.50 4.00 -4 -2 29 27.10 11.10 4 2 -29 30.40 11.60 4 2 -29 29.00 6.00 -3 -2 29 50.69 12.80 -3 -2 29 29.60 6.60 3 -2 -29 23.20 4.10 3 -2 -29 38.20 6.30 3 2 -29 19.80 5.80 3 2 -29 53.19 14.50 2 -2 -29 -5.00 6.00 -2 -2 29 4.50 5.50 2 -2 -29 -1.50 4.20 -2 -2 29 -9.60 9.80 2 2 -29 -4.20 5.30 1 -2 -29 133.49 13.90 -1 -2 29 69.19 9.90 -1 -2 29 84.39 14.10 1 -2 -29 79.79 9.90 1 2 -29 67.99 10.00 0 -2 -29 46.70 9.80 0 -2 -29 41.40 8.20 0 -2 29 36.20 13.70 0 -2 29 29.40 7.90 0 2 29 34.20 7.50 0 2 29 31.00 6.40 0 2 -29 32.70 8.60 -4 -3 29 19.50 12.40 -4 -3 29 7.90 6.40 4 3 -29 19.50 6.10 -3 -3 29 112.09 14.70 -3 -3 29 63.19 9.60 3 3 -29 68.19 9.40 2 -3 -29 44.90 6.50 -2 -3 29 24.20 7.00 2 -3 -29 25.90 5.00 -2 -3 29 42.20 14.00 2 3 -29 19.80 6.80 1 -3 -29 50.29 8.10 1 -3 -29 34.40 6.80 -1 -3 29 28.50 7.80 1 3 -29 20.30 7.60 _computing_structure_solution 'SHELXT 2014/4 (Sheldrick, 2014)' ; _shelx_hkl_checksum 18093 ####################################################################### # # This file contains crystal structure data downloaded from the # Cambridge Structural Database (CSD) hosted by the Cambridge # Crystallographic Data Centre (CCDC). # # Full information about CCDC data access policies and citation # guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 # # Audit and citation data items may have been added by the CCDC. # Please retain this information to preserve the provenance of # this file and to allow appropriate attribution of the data. # ####################################################################### data_TZ814_0m_a _database_code_depnum_ccdc_archive 'CCDC 1423806' _audit_update_record ; 2015-09-11 deposited with the CCDC. 2015-10-15 downloaded from the CCDC. ; _audit_creation_method SHELXL-2014/7 _shelx_SHELXL_version_number 2014/7 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C20 H27 F6 N2 O P2 Rh' _chemical_formula_weight 590.28 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Rh Rh -1.1178 0.9187 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_H-M_alt 'P 21/n' _space_group_name_Hall '-P 2yn' _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; loop_ _space_group_symop_operation_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 13.4021(9) _cell_length_b 10.9937(7) _cell_length_c 15.6906(10) _cell_angle_alpha 90 _cell_angle_beta 97.462(3) _cell_angle_gamma 90 _cell_volume 2292.3(3) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 249 _cell_measurement_theta_min 4.8606 _cell_measurement_theta_max 29.6204 _exptl_crystal_description 'rectangular block' _exptl_crystal_colour 'translucent intense yellow-brown' _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_density_diffrn 1.710 _exptl_crystal_F_000 1192 _exptl_transmission_factor_min ? _exptl_transmission_factor_max ? _exptl_crystal_size_max 0.886 _exptl_crystal_size_mid 0.217 _exptl_crystal_size_min 0.126 _exptl_absorpt_coefficient_mu 0.949 _shelx_estimated_absorpt_T_min ? _shelx_estimated_absorpt_T_max ? _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5796 _exptl_absorpt_correction_T_max 0.7479 _exptl_absorpt_process_details 'SADABS V2014/5 (Bruker AXS Inc.)' _exptl_absorpt_special_details ? _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_source ? _diffrn_measurement_device_type 'Bruker ApexII Triumph monochromator sealed tube' _diffrn_measurement_method 'Photon 50 CMOS detector' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 97401 _diffrn_reflns_av_unetI/netI 0.0436 _diffrn_reflns_av_R_equivalents 0.0669 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 3.406 _diffrn_reflns_theta_max 40.480 _diffrn_reflns_theta_full 25.242 _diffrn_measured_fraction_theta_max 0.998 _diffrn_measured_fraction_theta_full 0.998 _diffrn_reflns_Laue_measured_fraction_max 0.998 _diffrn_reflns_Laue_measured_fraction_full 0.998 _diffrn_reflns_point_group_measured_fraction_max 0.998 _diffrn_reflns_point_group_measured_fraction_full 0.998 _reflns_number_total 14600 _reflns_number_gt 10763 _reflns_threshold_expression 'I > 2\s(I)' _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_max . _reflns_Friedel_fraction_full . _reflns_special_details ; Reflections were merged by SHELXL according to the crystal class for the calculation of statistics and refinement. _reflns_Friedel_fraction is defined as the number of unique Friedel pairs measured divided by the number that would be possible theoretically, ignoring centric projections and systematic absences. ; _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement 'SHELXL-2014/7 (Sheldrick, 2014)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ? _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0405P)^2^+1.5557P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary ? _atom_sites_solution_secondary ? _atom_sites_solution_hydrogens mixed _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef . _refine_ls_number_reflns 14600 _refine_ls_number_parameters 297 _refine_ls_number_restraints 279 _refine_ls_R_factor_all 0.0675 _refine_ls_R_factor_gt 0.0381 _refine_ls_wR_factor_ref 0.0988 _refine_ls_wR_factor_gt 0.0833 _refine_ls_goodness_of_fit_ref 1.079 _refine_ls_restrained_S_all 1.075 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Rh1 Rh 0.70911(2) 0.23653(2) 0.62767(2) 0.01291(3) Uani 1 1 d . U . . . P1 P 0.62332(3) 0.14097(4) 0.71876(2) 0.01362(6) Uani 1 1 d . U . . . N1 N 0.83326(9) 0.18315(11) 0.70917(8) 0.01333(18) Uani 1 1 d . U . . . N2 N 0.82621(10) 0.28100(11) 0.55017(8) 0.0155(2) Uani 1 1 d . U . . . H2 H 0.8148(17) 0.348(2) 0.5270(14) 0.017(5) Uiso 1 1 d . . . . . C20 C 0.59562(12) 0.29066(16) 0.55985(10) 0.0197(3) Uani 1 1 d . U . . . O1 O 0.52458(11) 0.32494(16) 0.51926(10) 0.0351(3) Uani 1 1 d . U . . . C1 C 0.92369(12) 0.28836(15) 0.60672(10) 0.0188(3) Uani 1 1 d . U . . . H1A H 0.9376 0.3743 0.6229 0.023 Uiso 1 1 calc R U . . . H1B H 0.9781 0.2598 0.5746 0.023 Uiso 1 1 calc R U . . . C2 C 0.92453(11) 0.21337(13) 0.68717(9) 0.0155(2) Uani 1 1 d . U . . . C3 C 1.01244(12) 0.18042(16) 0.73788(11) 0.0211(3) Uani 1 1 d . U . . . H3 H 1.0760 0.2010 0.7213 0.025 Uiso 1 1 calc R U . . . C4 C 1.00639(12) 0.11669(17) 0.81356(11) 0.0222(3) Uani 1 1 d . U . . . H4 H 1.0660 0.0931 0.8492 0.027 Uiso 1 1 calc R U . . . C5 C 0.91299(12) 0.08785(15) 0.83666(10) 0.0182(2) Uani 1 1 d . U . . . H5 H 0.9080 0.0459 0.8889 0.022 Uiso 1 1 calc R U . . . C6 C 0.82652(10) 0.12085(13) 0.78264(9) 0.0138(2) Uani 1 1 d . U . . . C7 C 0.72355(11) 0.09076(15) 0.80370(9) 0.0182(3) Uani 1 1 d . U . . . H7A H 0.7135 0.1304 0.8586 0.022 Uiso 1 1 calc R U . . . H7B H 0.7183 0.0017 0.8115 0.022 Uiso 1 1 calc R U . . . C8 C 0.81891(11) 0.18531(13) 0.48609(9) 0.0159(2) Uani 1 1 d . U . . . C9 C 0.86087(14) 0.07117(15) 0.50487(11) 0.0224(3) Uani 1 1 d . U . . . H9 H 0.8969 0.0549 0.5599 0.027 Uiso 1 1 calc R U . . . C10 C 0.84953(16) -0.01884(17) 0.44213(12) 0.0272(3) Uani 1 1 d . U . . . H10 H 0.8771 -0.0974 0.4548 0.033 Uiso 1 1 calc R U . . . C11 C 0.79859(15) 0.00476(19) 0.36139(13) 0.0284(4) Uani 1 1 d . U . . . H11 H 0.7913 -0.0573 0.3189 0.034 Uiso 1 1 calc R U . . . C12 C 0.75838(14) 0.11895(19) 0.34277(12) 0.0267(3) Uani 1 1 d . U . . . H12 H 0.7244 0.1356 0.2870 0.032 Uiso 1 1 calc R U . . . C13 C 0.76724(13) 0.20943(16) 0.40491(10) 0.0208(3) Uani 1 1 d . U . . . H13 H 0.7383 0.2873 0.3922 0.025 Uiso 1 1 calc R U . . . C14 C 0.56577(13) -0.00136(15) 0.67456(11) 0.0211(3) Uani 1 1 d . U . . . H14 H 0.5470 -0.0510 0.7235 0.025 Uiso 1 1 calc R U . . . C15 C 0.46962(15) 0.0247(2) 0.61320(13) 0.0313(4) Uani 1 1 d . U . . . H15A H 0.4855 0.0776 0.5666 0.047 Uiso 1 1 calc R U . . . H15B H 0.4205 0.0651 0.6447 0.047 Uiso 1 1 calc R U . . . H15C H 0.4413 -0.0520 0.5891 0.047 Uiso 1 1 calc R U . . . C16 C 0.64137(16) -0.07428(17) 0.63030(14) 0.0297(4) Uani 1 1 d . U . . . H16A H 0.6100 -0.1502 0.6076 0.045 Uiso 1 1 calc R U . . . H16B H 0.7004 -0.0930 0.6719 0.045 Uiso 1 1 calc R U . . . H16C H 0.6622 -0.0264 0.5830 0.045 Uiso 1 1 calc R U . . . C17 C 0.52806(12) 0.21559(16) 0.77488(10) 0.0196(3) Uani 1 1 d . U . . . H17 H 0.4715 0.2403 0.7303 0.023 Uiso 1 1 calc R U . . . C18 C 0.48396(15) 0.13048(19) 0.83783(13) 0.0286(4) Uani 1 1 d . U . . . H18A H 0.5379 0.1024 0.8816 0.043 Uiso 1 1 calc R U . . . H18B H 0.4525 0.0603 0.8065 0.043 Uiso 1 1 calc R U . . . H18C H 0.4333 0.1744 0.8656 0.043 Uiso 1 1 calc R U . . . C19 C 0.56969(16) 0.33150(17) 0.82026(13) 0.0274(3) Uani 1 1 d . U . . . H19A H 0.5149 0.3758 0.8422 0.041 Uiso 1 1 calc R U . . . H19B H 0.5998 0.3830 0.7795 0.041 Uiso 1 1 calc R U . . . H19C H 0.6210 0.3100 0.8682 0.041 Uiso 1 1 calc R U . . . P2 P 0.75792(3) 0.60278(4) 0.42492(3) 0.01912(7) Uani 1 1 d . U . . . F1 F 0.66380(11) 0.66787(16) 0.37388(10) 0.0463(4) Uani 1 1 d . U . . . F2 F 0.68728(12) 0.51751(14) 0.47480(9) 0.0436(3) Uani 1 1 d . U . . . F3 F 0.85296(11) 0.53291(14) 0.47663(10) 0.0460(4) Uani 1 1 d . U . . . F4 F 0.83189(11) 0.68230(13) 0.37601(9) 0.0399(3) Uani 1 1 d . U . . . F5 F 0.76238(15) 0.70104(13) 0.49911(9) 0.0507(4) Uani 1 1 d . U . . . F6 F 0.75380(12) 0.50190(12) 0.35128(8) 0.0358(3) Uani 1 1 d . U . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Rh1 0.01374(4) 0.01447(4) 0.01042(4) 0.00215(3) 0.00124(3) 0.00073(3) P1 0.01267(14) 0.01611(15) 0.01196(14) 0.00255(11) 0.00109(11) 0.00040(11) N1 0.0137(4) 0.0146(5) 0.0116(4) 0.0006(3) 0.0013(3) -0.0004(4) N2 0.0204(5) 0.0129(5) 0.0135(5) 0.0020(4) 0.0035(4) 0.0006(4) C20 0.0199(6) 0.0221(7) 0.0169(6) 0.0057(5) 0.0022(5) 0.0023(5) O1 0.0239(6) 0.0483(9) 0.0305(7) 0.0154(6) -0.0052(5) 0.0055(6) C1 0.0189(6) 0.0201(6) 0.0178(6) 0.0007(5) 0.0041(5) -0.0051(5) C2 0.0145(5) 0.0170(6) 0.0149(5) -0.0011(4) 0.0016(4) -0.0015(4) C3 0.0142(6) 0.0261(7) 0.0227(7) -0.0006(5) 0.0011(5) -0.0006(5) C4 0.0156(6) 0.0278(8) 0.0214(7) 0.0024(6) -0.0037(5) 0.0023(5) C5 0.0176(6) 0.0201(6) 0.0157(6) 0.0024(5) -0.0026(5) 0.0021(5) C6 0.0149(5) 0.0147(5) 0.0114(5) 0.0002(4) 0.0004(4) 0.0013(4) C7 0.0157(6) 0.0252(7) 0.0133(5) 0.0068(5) 0.0004(4) 0.0005(5) C8 0.0174(6) 0.0161(6) 0.0145(5) 0.0011(4) 0.0036(4) -0.0004(4) C9 0.0301(8) 0.0180(6) 0.0192(6) 0.0005(5) 0.0030(6) 0.0041(6) C10 0.0345(9) 0.0200(7) 0.0275(8) -0.0047(6) 0.0053(7) 0.0048(6) C11 0.0278(8) 0.0300(9) 0.0279(8) -0.0121(7) 0.0050(7) -0.0002(7) C12 0.0269(8) 0.0338(9) 0.0186(7) -0.0050(6) 0.0003(6) 0.0013(7) C13 0.0231(7) 0.0224(7) 0.0165(6) 0.0005(5) 0.0014(5) 0.0018(5) C14 0.0237(7) 0.0196(7) 0.0199(6) 0.0015(5) 0.0024(5) -0.0049(5) C15 0.0252(8) 0.0368(10) 0.0299(9) -0.0049(7) -0.0036(7) -0.0088(7) C16 0.0364(10) 0.0197(7) 0.0334(9) -0.0035(6) 0.0059(8) 0.0003(7) C17 0.0159(6) 0.0244(7) 0.0189(6) 0.0025(5) 0.0037(5) 0.0036(5) C18 0.0269(8) 0.0303(9) 0.0322(9) 0.0054(7) 0.0171(7) 0.0025(7) C19 0.0331(9) 0.0231(8) 0.0270(8) -0.0012(6) 0.0081(7) 0.0033(6) P2 0.02335(18) 0.01861(17) 0.01493(16) 0.00339(13) 0.00065(13) -0.00193(14) F1 0.0358(7) 0.0553(9) 0.0458(8) 0.0118(7) -0.0022(6) 0.0185(7) F2 0.0527(9) 0.0441(8) 0.0380(7) 0.0071(6) 0.0212(6) -0.0147(7) F3 0.0388(7) 0.0447(8) 0.0484(8) 0.0153(6) -0.0175(6) 0.0038(6) F4 0.0429(7) 0.0405(7) 0.0372(7) 0.0083(6) 0.0089(6) -0.0199(6) F5 0.1017(14) 0.0274(6) 0.0228(6) -0.0045(5) 0.0069(7) -0.0050(8) F6 0.0551(8) 0.0275(6) 0.0252(5) -0.0051(4) 0.0065(5) -0.0036(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Rh1 C20 1.8383(16) . ? Rh1 N1 2.0483(12) . ? Rh1 N2 2.1624(13) . ? Rh1 P1 2.2126(4) . ? P1 C17 1.8358(16) . ? P1 C14 1.8399(17) . ? P1 C7 1.8495(15) . ? N1 C6 1.3539(18) . ? N1 C2 1.3549(19) . ? N2 C8 1.450(2) . ? N2 C1 1.483(2) . ? N2 H2 0.83(2) . ? C20 O1 1.139(2) . ? C1 C2 1.506(2) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 C3 1.382(2) . ? C3 C4 1.390(2) . ? C3 H3 0.9500 . ? C4 C5 1.384(2) . ? C4 H4 0.9500 . ? C5 C6 1.392(2) . ? C5 H5 0.9500 . ? C6 C7 1.497(2) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 C9 1.391(2) . ? C8 C13 1.394(2) . ? C9 C10 1.390(2) . ? C9 H9 0.9500 . ? C10 C11 1.383(3) . ? C10 H10 0.9500 . ? C11 C12 1.382(3) . ? C11 H11 0.9500 . ? C12 C13 1.387(2) . ? C12 H12 0.9500 . ? C13 H13 0.9500 . ? C14 C16 1.528(3) . ? C14 C15 1.532(3) . ? C14 H14 1.0000 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 C19 1.529(3) . ? C17 C18 1.534(2) . ? C17 H17 1.0000 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? P2 F1 1.5755(14) . ? P2 F5 1.5836(14) . ? P2 F4 1.5917(13) . ? P2 F6 1.5973(13) . ? P2 F2 1.6063(13) . ? P2 F3 1.6132(14) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C20 Rh1 N1 176.44(6) . . ? C20 Rh1 N2 101.98(6) . . ? N1 Rh1 N2 79.97(5) . . ? C20 Rh1 P1 93.86(5) . . ? N1 Rh1 P1 84.77(3) . . ? N2 Rh1 P1 161.18(4) . . ? C17 P1 C14 106.10(8) . . ? C17 P1 C7 105.84(7) . . ? C14 P1 C7 104.33(8) . . ? C17 P1 Rh1 123.35(6) . . ? C14 P1 Rh1 112.83(5) . . ? C7 P1 Rh1 102.56(5) . . ? C6 N1 C2 120.22(12) . . ? C6 N1 Rh1 122.54(9) . . ? C2 N1 Rh1 117.24(10) . . ? C8 N2 C1 115.43(12) . . ? C8 N2 Rh1 103.73(9) . . ? C1 N2 Rh1 108.85(9) . . ? C8 N2 H2 110.4(15) . . ? C1 N2 H2 108.3(16) . . ? Rh1 N2 H2 110.0(16) . . ? O1 C20 Rh1 178.64(17) . . ? N2 C1 C2 112.43(12) . . ? N2 C1 H1A 109.1 . . ? C2 C1 H1A 109.1 . . ? N2 C1 H1B 109.1 . . ? C2 C1 H1B 109.1 . . ? H1A C1 H1B 107.8 . . ? N1 C2 C3 121.30(14) . . ? N1 C2 C1 116.04(13) . . ? C3 C2 C1 122.62(14) . . ? C2 C3 C4 118.96(15) . . ? C2 C3 H3 120.5 . . ? C4 C3 H3 120.5 . . ? C5 C4 C3 119.61(14) . . ? C5 C4 H4 120.2 . . ? C3 C4 H4 120.2 . . ? C4 C5 C6 119.36(14) . . ? C4 C5 H5 120.3 . . ? C6 C5 H5 120.3 . . ? N1 C6 C5 120.53(13) . . ? N1 C6 C7 117.71(12) . . ? C5 C6 C7 121.75(13) . . ? C6 C7 P1 112.27(10) . . ? C6 C7 H7A 109.1 . . ? P1 C7 H7A 109.1 . . ? C6 C7 H7B 109.1 . . ? P1 C7 H7B 109.1 . . ? H7A C7 H7B 107.9 . . ? C9 C8 C13 120.29(15) . . ? C9 C8 N2 121.25(14) . . ? C13 C8 N2 118.45(14) . . ? C10 C9 C8 119.22(16) . . ? C10 C9 H9 120.4 . . ? C8 C9 H9 120.4 . . ? C11 C10 C9 120.70(17) . . ? C11 C10 H10 119.6 . . ? C9 C10 H10 119.6 . . ? C12 C11 C10 119.76(17) . . ? C12 C11 H11 120.1 . . ? C10 C11 H11 120.1 . . ? C11 C12 C13 120.47(17) . . ? C11 C12 H12 119.8 . . ? C13 C12 H12 119.8 . . ? C12 C13 C8 119.53(16) . . ? C12 C13 H13 120.2 . . ? C8 C13 H13 120.2 . . ? C16 C14 C15 111.45(16) . . ? C16 C14 P1 110.32(12) . . ? C15 C14 P1 110.80(13) . . ? C16 C14 H14 108.0 . . ? C15 C14 H14 108.0 . . ? P1 C14 H14 108.0 . . ? C14 C15 H15A 109.5 . . ? C14 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C14 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C14 C16 H16A 109.5 . . ? C14 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C14 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C19 C17 C18 110.87(15) . . ? C19 C17 P1 111.18(12) . . ? C18 C17 P1 112.73(12) . . ? C19 C17 H17 107.2 . . ? C18 C17 H17 107.2 . . ? P1 C17 H17 107.2 . . ? C17 C18 H18A 109.5 . . ? C17 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C17 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C17 C19 H19A 109.5 . . ? C17 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C17 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? F1 P2 F5 90.87(9) . . ? F1 P2 F4 90.75(9) . . ? F5 P2 F4 90.76(9) . . ? F1 P2 F6 89.85(9) . . ? F5 P2 F6 179.03(8) . . ? F4 P2 F6 89.88(8) . . ? F1 P2 F2 91.67(9) . . ? F5 P2 F2 90.47(9) . . ? F4 P2 F2 177.27(9) . . ? F6 P2 F2 88.86(8) . . ? F1 P2 F3 178.58(9) . . ? F5 P2 F3 90.18(9) . . ? F4 P2 F3 90.20(9) . . ? F6 P2 F3 89.09(8) . . ? F2 P2 F3 87.35(9) . . ? _refine_diff_density_max 1.631 _refine_diff_density_min -2.366 _refine_diff_density_rms 0.139 _shelx_res_file ; TZ814_0m_a.res created by SHELXL-2014/7 TITL TZ814_0m_a.res in P2(1)/n CELL 0.71073 13.4021 10.9937 15.6906 90.000 97.462 90.000 ZERR 4.000 0.0009 0.0007 0.0010 0.000 0.003 0.000 LATT 1 SYMM 1/2-X, 1/2+Y, 1/2-Z SFAC C H N O F P Rh UNIT 80 108 8 4 24 8 4 REM Old TITL TZ814_0m in P2(1)/n REM SHELXT solution in P2(1)/n REM R1 0.068, Rweak 0.001, Alpha 0.041, Orientation as input REM Formula found by SHELXT: C20 N2 O F6 P2 Rh L.S. 10 BOND $H ACTA FMAP 2 PLAN 10 TEMP -123.150 DFIX 0.9 0.03 N1 H1 RIGU WGHT 0.040500 1.555700 FVAR 0.44081 RH1 7 0.709110 0.236535 0.627666 11.00000 0.01374 0.01447 = 0.01042 0.00215 0.00124 0.00073 P1 6 0.623317 0.140966 0.718758 11.00000 0.01267 0.01611 = 0.01196 0.00255 0.00109 0.00040 N1 3 0.833259 0.183146 0.709167 11.00000 0.01366 0.01465 = 0.01159 0.00057 0.00126 -0.00041 N2 3 0.826209 0.281004 0.550170 11.00000 0.02036 0.01288 = 0.01352 0.00202 0.00354 0.00064 H2 2 0.814780 0.347883 0.527018 11.00000 0.01749 C20 1 0.595621 0.290660 0.559846 11.00000 0.01994 0.02212 = 0.01693 0.00565 0.00224 0.00231 O1 4 0.524580 0.324940 0.519260 11.00000 0.02395 0.04834 = 0.03054 0.01537 -0.00524 0.00554 C1 1 0.923691 0.288363 0.606719 11.00000 0.01892 0.02014 = 0.01783 0.00065 0.00414 -0.00509 AFIX 23 H1A 2 0.937627 0.374335 0.622866 11.00000 -1.20000 H1B 2 0.978077 0.259782 0.574562 11.00000 -1.20000 AFIX 0 C2 1 0.924533 0.213366 0.687166 11.00000 0.01450 0.01695 = 0.01490 -0.00115 0.00157 -0.00148 C3 1 1.012437 0.180424 0.737882 11.00000 0.01415 0.02607 = 0.02272 -0.00064 0.00107 -0.00058 AFIX 43 H3 2 1.076015 0.201002 0.721300 11.00000 -1.20000 AFIX 0 C4 1 1.006385 0.116690 0.813564 11.00000 0.01563 0.02783 = 0.02144 0.00236 -0.00366 0.00227 AFIX 43 H4 2 1.065991 0.093069 0.849219 11.00000 -1.20000 AFIX 0 C5 1 0.912989 0.087846 0.836664 11.00000 0.01762 0.02013 = 0.01573 0.00238 -0.00258 0.00206 AFIX 43 H5 2 0.907953 0.045935 0.888881 11.00000 -1.20000 AFIX 0 C6 1 0.826518 0.120850 0.782637 11.00000 0.01488 0.01468 = 0.01137 0.00019 0.00043 0.00129 C7 1 0.723550 0.090755 0.803699 11.00000 0.01570 0.02519 = 0.01333 0.00682 0.00039 0.00054 AFIX 23 H7A 2 0.713530 0.130357 0.858615 11.00000 -1.20000 H7B 2 0.718319 0.001733 0.811534 11.00000 -1.20000 AFIX 0 C8 1 0.818908 0.185306 0.486091 11.00000 0.01742 0.01614 = 0.01452 0.00112 0.00361 -0.00041 C9 1 0.860867 0.071173 0.504867 11.00000 0.03011 0.01798 = 0.01918 0.00049 0.00296 0.00414 AFIX 43 H9 2 0.896853 0.054916 0.559920 11.00000 -1.20000 AFIX 0 C10 1 0.849530 -0.018836 0.442128 11.00000 0.03451 0.02001 = 0.02754 -0.00468 0.00527 0.00479 AFIX 43 H10 2 0.877057 -0.097387 0.454834 11.00000 -1.20000 AFIX 0 C11 1 0.798593 0.004762 0.361392 11.00000 0.02776 0.02996 = 0.02791 -0.01212 0.00501 -0.00021 AFIX 43 H11 2 0.791272 -0.057284 0.318897 11.00000 -1.20000 AFIX 0 C12 1 0.758381 0.118948 0.342769 11.00000 0.02687 0.03378 = 0.01862 -0.00499 0.00033 0.00133 AFIX 43 H12 2 0.724434 0.135579 0.287008 11.00000 -1.20000 AFIX 0 C13 1 0.767241 0.209426 0.404914 11.00000 0.02309 0.02236 = 0.01653 0.00054 0.00141 0.00184 AFIX 43 H13 2 0.738301 0.287279 0.392240 11.00000 -1.20000 AFIX 0 C14 1 0.565771 -0.001362 0.674563 11.00000 0.02373 0.01963 = 0.01989 0.00149 0.00243 -0.00486 AFIX 13 H14 2 0.547038 -0.051022 0.723470 11.00000 -1.20000 AFIX 0 C15 1 0.469616 0.024690 0.613198 11.00000 0.02522 0.03681 = 0.02990 -0.00488 -0.00358 -0.00878 AFIX 137 H15A 2 0.485540 0.077635 0.566560 11.00000 -1.50000 H15B 2 0.420461 0.065098 0.644708 11.00000 -1.50000 H15C 2 0.441346 -0.052000 0.589074 11.00000 -1.50000 AFIX 0 C16 1 0.641375 -0.074277 0.630300 11.00000 0.03637 0.01966 = 0.03337 -0.00349 0.00588 0.00034 AFIX 137 H16A 2 0.610030 -0.150178 0.607637 11.00000 -1.50000 H16B 2 0.700404 -0.093046 0.671902 11.00000 -1.50000 H16C 2 0.662184 -0.026376 0.582970 11.00000 -1.50000 AFIX 0 C17 1 0.528062 0.215589 0.774880 11.00000 0.01586 0.02440 = 0.01886 0.00247 0.00371 0.00359 AFIX 13 H17 2 0.471544 0.240336 0.730270 11.00000 -1.20000 AFIX 0 C18 1 0.483958 0.130478 0.837832 11.00000 0.02690 0.03028 = 0.03223 0.00537 0.01707 0.00254 AFIX 137 H18A 2 0.537851 0.102371 0.881624 11.00000 -1.50000 H18B 2 0.452534 0.060321 0.806482 11.00000 -1.50000 H18C 2 0.433308 0.174356 0.865615 11.00000 -1.50000 AFIX 0 C19 1 0.569687 0.331501 0.820257 11.00000 0.03313 0.02312 = 0.02696 -0.00117 0.00812 0.00334 AFIX 137 H19A 2 0.514921 0.375825 0.842203 11.00000 -1.50000 H19B 2 0.599812 0.382979 0.779450 11.00000 -1.50000 H19C 2 0.621002 0.309976 0.868196 11.00000 -1.50000 AFIX 0 P2 6 0.757924 0.602781 0.424919 11.00000 0.02335 0.01861 = 0.01493 0.00339 0.00065 -0.00193 F1 5 0.663803 0.667871 0.373880 11.00000 0.03581 0.05529 = 0.04584 0.01179 -0.00218 0.01850 F2 5 0.687281 0.517509 0.474804 11.00000 0.05274 0.04409 = 0.03796 0.00710 0.02117 -0.01466 F3 5 0.852960 0.532915 0.476635 11.00000 0.03881 0.04474 = 0.04842 0.01530 -0.01752 0.00384 F4 5 0.831888 0.682304 0.376012 11.00000 0.04294 0.04053 = 0.03722 0.00833 0.00892 -0.01985 F5 5 0.762382 0.701042 0.499112 11.00000 0.10166 0.02742 = 0.02277 -0.00453 0.00685 -0.00498 F6 5 0.753799 0.501901 0.351280 11.00000 0.05513 0.02745 = 0.02519 -0.00508 0.00652 -0.00364 HKLF 4 REM TZ814_0m_a.res in P2(1)/n REM R1 = 0.0381 for 10763 Fo > 4sig(Fo) and 0.0675 for all 14600 data REM 297 parameters refined using 279 restraints END WGHT 0.0411 1.4932 REM Highest difference peak 1.631, deepest hole -2.366, 1-sigma level 0.139 Q1 1 0.6265 0.7378 0.3829 11.00000 0.05 1.63 Q2 1 0.6215 0.3336 0.7186 11.00000 0.05 1.61 Q3 1 0.7970 0.1410 0.5369 11.00000 0.05 1.50 Q4 1 0.8407 0.1024 0.6683 11.00000 0.05 0.99 Q5 1 0.8265 0.6003 0.3196 11.00000 0.05 0.74 Q6 1 0.7967 0.3351 0.5392 11.00000 0.05 0.72 Q7 1 0.4558 0.3613 0.5305 11.00000 0.05 0.70 Q8 1 0.7581 -0.1271 0.4251 11.00000 0.05 0.67 Q9 1 0.5866 0.2810 0.7061 11.00000 0.05 0.60 Q10 1 0.6587 0.1593 0.6311 11.00000 0.05 0.58 ; _shelx_res_checksum 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17.20 -16 13 4 24.80 15.00 15 -13 -4 19.30 20.90 -15 -13 4 50.39 13.80 -15 -13 4 44.80 13.10 15 13 -4 54.19 16.30 -15 13 4 15.60 14.40 15 13 -4 62.59 14.20 14 -13 -4 27.60 22.10 -14 -13 4 0.10 12.60 -14 -13 4 -27.00 10.10 14 13 -4 -9.20 11.50 -14 13 4 -8.40 12.40 14 13 -4 -15.90 16.30 13 -13 -4 -23.90 20.70 -13 -13 4 1.20 10.90 -13 -13 4 -0.70 12.30 -13 13 4 6.10 13.00 13 13 -4 5.60 11.50 13 13 -4 18.80 14.60 -12 -13 4 14.90 13.10 -12 -13 4 10.20 10.70 12 -13 -4 19.70 20.50 12 13 -4 28.60 15.90 -12 13 4 19.80 12.60 12 13 -4 13.80 11.00 11 -13 -4 170.78 23.90 -11 -13 4 161.38 20.30 -11 -13 4 148.99 18.10 -11 13 4 171.78 20.70 11 13 -4 151.78 19.90 11 13 -4 155.28 17.80 10 -13 -4 -9.70 22.30 -10 -13 4 -6.50 12.10 10 13 -4 13.40 10.20 10 13 -4 -20.90 14.30 -10 13 4 6.80 12.00 9 -13 -4 252.77 28.10 9 -13 -4 247.48 22.50 -9 -13 4 232.08 29.30 -9 13 4 277.47 23.40 -9 13 4 333.67 27.50 9 13 -4 242.28 24.50 8 -13 -4 12.00 16.50 -8 -13 4 13.30 12.40 8 -13 -4 17.40 13.00 8 13 -4 13.50 10.20 -8 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31.50 9 15 4 344.27 26.80 10 -15 4 26.10 19.50 -10 -15 -4 39.00 13.80 10 15 4 3.20 14.50 10 15 4 8.80 11.50 -10 15 -4 18.00 15.40 -10 15 -4 10.10 13.40 10 15 4 -4.30 16.00 11 -15 4 67.29 21.60 -11 -15 -4 69.89 16.40 -11 15 -4 83.49 18.40 11 15 4 43.30 17.30 11 15 4 38.90 12.70 11 15 4 66.89 16.30 -11 15 -4 30.60 15.60 12 -15 4 -6.60 20.90 -12 -15 -4 -4.10 15.90 -12 15 -4 4.30 16.80 12 15 4 -5.20 12.10 12 15 4 0.10 15.40 -12 15 -4 7.90 15.20 12 15 4 -16.50 15.70 -13 -15 -4 7.80 15.50 13 -15 4 32.90 20.20 13 15 4 9.40 12.90 13 15 4 9.10 15.70 -13 15 -4 9.90 15.90 -13 15 -4 16.20 17.60 13 15 4 -1.10 18.40 14 -15 4 -25.20 23.50 -14 -15 -4 -37.20 16.10 -14 15 -4 -1.60 18.00 14 15 4 -2.90 13.40 14 15 4 14.90 16.00 -14 15 -4 3.00 16.40 -15 -15 -4 4.70 18.10 15 -15 4 -13.40 25.10 15 15 4 -3.70 14.80 15 15 4 -13.40 16.80 -15 15 -4 -21.90 19.50 -15 15 -4 -4.50 18.30 -14 -16 4 39.30 15.00 -14 -16 4 -5.50 15.60 14 -16 -4 -15.60 22.70 -14 16 4 24.10 19.10 14 16 -4 15.20 18.40 14 16 -4 15.80 15.70 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4 -4.70 12.40 -5 -16 4 3.20 14.40 5 -16 -4 16.10 20.90 5 -16 -4 -23.10 15.80 -5 16 4 9.80 12.00 5 16 -4 -9.60 11.80 5 16 -4 -5.90 15.20 -5 16 4 -6.80 15.00 -4 -16 4 30.40 15.20 4 -16 -4 33.00 16.30 -4 16 4 34.60 12.70 4 16 -4 -0.30 13.80 -4 16 4 7.70 14.70 4 16 -4 25.60 12.60 3 -16 -4 140.19 20.40 -3 -16 4 170.68 20.90 -3 16 4 191.88 24.00 -3 16 4 188.58 20.50 3 16 -4 138.99 17.20 3 16 -4 227.38 24.80 -2 -16 4 23.00 14.90 2 -16 -4 -26.40 15.50 -2 16 4 21.10 11.90 2 16 -4 0.10 12.20 2 16 -4 27.20 15.40 1 -16 -4 463.85 34.30 -1 -16 4 428.66 31.40 -1 16 4 436.06 30.50 1 16 -4 465.05 32.50 1 16 -4 521.45 31.80 0 -16 -4 21.80 15.50 0 -16 4 5.70 15.30 0 16 4 13.50 12.10 0 16 -4 7.10 12.00 0 16 4 6.60 14.30 0 16 -4 19.10 15.80 -1 -16 -4 378.26 30.70 1 -16 4 386.46 30.20 -1 16 -4 379.26 31.00 1 16 4 416.96 28.30 -1 16 -4 397.56 28.60 1 16 4 332.97 30.40 2 -16 4 9.40 15.20 -2 -16 -4 37.40 16.50 2 16 4 32.30 12.60 -2 16 -4 8.00 12.50 -2 16 -4 5.60 15.60 2 16 4 32.90 14.80 3 -16 4 7.90 14.90 -3 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14.50 12.50 -10 16 -4 13.30 16.40 11 -16 4 183.98 26.80 -11 -16 -4 165.68 22.00 -11 16 -4 294.67 30.30 -11 16 -4 257.07 27.20 11 16 4 226.58 25.80 11 16 4 195.18 22.00 -12 -16 -4 -10.90 16.80 12 -16 4 -25.70 22.70 12 16 4 9.20 18.80 -12 16 -4 24.90 16.70 -12 16 -4 26.80 18.70 12 16 4 -1.10 12.90 -13 -16 -4 32.40 18.30 13 -16 4 68.89 25.30 13 16 4 87.49 17.00 -13 16 -4 89.39 19.10 -13 16 -4 86.69 21.10 12 -17 -4 17.80 25.90 -12 -17 4 -7.90 16.30 -12 -17 4 -10.90 13.40 -12 17 4 -12.30 17.30 12 17 -4 -22.50 18.00 12 17 -4 -10.20 14.30 -11 -17 4 15.90 13.00 -11 -17 4 0.20 16.10 11 -17 -4 33.00 24.20 11 17 -4 27.20 15.00 11 17 -4 13.40 18.00 -11 17 4 0.60 16.50 -10 -17 4 6.30 15.60 -10 -17 4 7.70 12.80 10 -17 -4 5.50 23.60 10 17 -4 16.60 14.10 -10 17 4 -10.80 14.90 10 17 -4 10.10 17.00 -9 -17 4 85.59 17.20 -9 -17 4 54.49 13.90 9 -17 -4 57.79 24.10 -9 17 4 74.89 17.00 9 17 -4 52.99 18.60 9 17 -4 54.79 14.90 -8 -17 4 -10.40 15.20 8 -17 -4 19.00 23.60 -8 -17 4 -11.00 11.80 8 17 -4 3.40 13.10 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13.90 1 -17 4 57.39 16.80 -1 -17 -4 63.49 17.00 -1 17 -4 38.60 13.90 -1 17 -4 58.69 17.40 1 17 4 55.29 16.50 1 17 4 70.89 14.30 -2 -17 -4 21.40 14.50 2 -17 4 2.30 15.10 -2 17 -4 -17.60 15.30 2 17 4 -13.50 15.60 -2 17 -4 -10.30 13.00 2 17 4 -22.30 10.60 3 -17 4 57.59 17.00 -3 -17 -4 107.79 19.10 -3 17 -4 107.29 16.00 -3 17 -4 100.29 17.80 3 17 4 109.29 18.60 3 17 4 136.09 16.20 -4 -17 -4 -3.10 14.50 4 -17 4 2.50 15.70 -4 17 -4 -15.10 13.30 -4 17 -4 4.50 15.70 4 17 4 -5.50 11.30 4 17 4 -7.90 14.80 5 -17 4 84.99 17.60 -5 -17 -4 83.89 17.00 -5 17 -4 107.99 16.20 5 17 4 133.79 19.00 -5 17 -4 111.09 18.40 5 17 4 123.49 16.00 6 -17 4 -6.00 15.30 -6 -17 -4 12.30 16.30 -6 17 -4 10.40 15.90 6 17 4 -5.00 11.30 6 17 4 -19.20 15.20 -6 17 -4 -2.50 13.70 7 -17 4 168.88 30.10 7 -17 4 186.58 21.40 -7 -17 -4 129.49 19.60 7 17 4 167.08 20.40 7 17 4 134.29 21.00 -7 17 -4 132.39 20.30 -7 17 -4 135.59 18.10 8 -17 4 31.20 22.20 -8 -17 -4 6.80 17.00 8 17 4 19.60 13.10 -8 17 -4 19.40 17.10 -8 17 -4 -5.40 14.90 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204.98 14.20 -9 -4 9 199.18 14.70 9 -4 -9 161.38 16.40 -9 -4 9 167.58 13.00 -9 -4 9 213.88 16.20 9 -4 -9 200.08 19.30 -9 4 9 180.38 14.00 -9 4 9 178.78 15.90 9 4 -9 212.88 21.90 -9 4 9 226.98 14.50 9 4 -9 176.88 15.80 9 4 -9 206.18 17.20 -8 -4 9 81.19 8.20 8 -4 -9 74.79 9.10 -8 -4 9 88.29 9.20 8 -4 -9 113.39 14.20 -8 -4 9 84.19 10.20 -8 4 9 84.69 9.60 8 4 -9 85.29 10.50 8 4 -9 111.99 13.40 -8 4 9 78.19 8.60 -8 4 9 83.79 10.80 7 -4 -9 142.69 15.90 -7 -4 9 98.39 10.70 -7 -4 9 101.89 8.40 -7 -4 9 127.99 11.40 7 -4 -9 100.49 12.10 -7 4 9 105.69 11.20 7 4 -9 107.09 12.40 -7 4 9 109.89 11.00 -7 4 9 117.59 11.70 -7 4 9 111.59 9.70 7 4 -9 99.19 10.50 -6 -4 9 29.60 3.50 -6 -4 9 27.70 4.90 6 -4 -9 25.30 11.10 6 -4 -9 31.70 6.00 -6 4 9 41.40 5.80 -6 4 9 24.50 4.40 6 4 -9 22.10 5.10 -6 4 9 21.80 5.30 -6 4 9 28.30 6.20 5 -4 -9 596.34 32.50 -5 -4 9 578.74 30.80 -5 -4 9 575.64 32.10 -5 -4 9 616.94 31.00 5 4 -9 580.94 32.10 -5 4 9 573.14 32.30 -5 4 9 571.24 31.50 -5 4 9 621.84 32.20 -4 -4 9 1.00 4.00 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561.24 34.60 9 -4 9 544.25 36.30 9 -4 9 635.54 33.30 9 4 9 599.44 34.50 -9 4 -9 648.44 33.50 9 4 9 599.84 34.60 9 4 9 614.64 34.80 9 4 9 567.94 33.10 9 4 9 633.64 34.00 10 -4 9 235.28 19.60 10 -4 9 242.98 20.90 10 -4 9 292.47 17.80 -10 4 -9 290.77 18.30 10 4 9 254.27 19.80 10 4 9 297.77 19.70 10 4 9 250.77 18.00 10 4 9 249.08 19.60 10 4 9 283.87 19.90 11 -4 9 419.06 29.10 11 -4 9 418.46 30.40 11 4 9 465.65 27.50 11 4 9 492.55 28.90 11 4 9 485.45 29.20 11 4 9 490.45 28.80 11 4 9 477.05 28.90 -11 4 -9 485.55 27.50 12 -4 9 206.38 21.00 12 -4 9 199.08 20.40 12 4 9 206.78 16.60 12 4 9 198.48 19.10 12 4 9 216.48 18.50 -12 4 -9 220.78 16.50 12 4 9 208.18 18.70 12 4 9 239.48 19.60 13 -4 9 400.86 32.30 13 -4 9 423.66 29.80 13 4 9 506.85 29.20 13 4 9 503.35 29.70 -13 4 -9 476.55 27.70 13 4 9 468.05 29.30 13 4 9 431.06 27.70 13 4 9 382.86 29.40 14 -4 9 39.10 15.50 14 -4 9 41.40 12.80 -14 4 -9 60.99 9.90 14 4 9 34.70 9.70 14 4 9 47.90 12.40 14 4 9 53.29 12.40 14 4 9 31.80 12.90 15 -4 9 38.20 17.70 15 -4 9 20.50 13.00 -15 4 -9 23.90 10.20 15 4 9 45.90 12.80 15 4 9 15.90 10.30 15 4 9 33.10 12.90 16 -4 9 7.50 13.40 16 -4 9 32.40 17.10 -16 4 -9 29.40 12.80 16 4 9 -24.80 19.90 16 4 9 26.00 10.80 16 4 9 1.40 13.00 17 -4 9 14.50 14.10 -17 -4 -9 50.29 12.10 17 -4 9 23.90 19.40 -17 4 -9 29.00 11.40 17 4 9 38.70 11.30 17 4 9 12.10 15.10 18 -4 9 -4.20 19.20 -18 -4 -9 11.90 11.80 18 -4 9 -21.00 15.80 18 4 9 0.20 15.70 18 4 9 9.80 11.10 -18 4 -9 15.80 12.00 -19 -4 -9 73.59 14.10 19 -4 9 68.69 17.70 19 -4 9 76.49 22.60 19 4 9 92.89 19.20 19 4 9 73.49 13.50 -19 4 -9 86.79 14.20 20 -4 9 21.00 21.10 20 -4 9 -3.20 16.30 20 4 9 -8.30 11.30 20 4 9 20.40 18.10 -20 4 -9 14.80 13.20 21 -4 9 20.80 20.40 21 -4 9 22.30 20.50 21 4 9 21.50 19.10 -21 4 -9 7.60 14.50 -23 -5 9 17.50 15.30 23 -5 -9 -11.50 24.40 23 -5 -9 11.30 21.70 23 5 -9 37.40 20.80 -23 5 9 78.99 19.00 -23 5 9 10.60 12.70 -22 -5 9 31.90 13.90 22 -5 -9 21.20 22.70 22 -5 -9 34.80 19.50 -22 5 9 23.10 12.40 -22 5 9 22.70 16.50 22 5 -9 32.10 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62.69 13.60 -12 -14 14 45.70 16.20 12 -14 -14 60.19 25.60 -12 14 14 58.79 19.60 -12 14 14 57.19 14.90 12 14 -14 41.40 21.90 -11 -14 14 2.60 15.20 11 -14 -14 5.90 23.70 -11 -14 14 8.70 13.40 -11 14 14 -33.50 12.40 11 14 -14 -11.40 20.70 -11 14 14 -3.60 18.10 10 -14 -14 28.20 24.60 -10 -14 14 15.60 11.60 -10 -14 14 -1.70 13.20 10 14 -14 -32.40 19.60 -10 14 14 -27.30 12.10 -10 14 14 -10.00 17.10 9 -14 -14 54.59 18.20 -9 -14 14 6.30 15.00 9 -14 -14 12.00 23.10 -9 -14 14 37.90 12.20 -9 14 14 -7.90 12.50 -9 14 14 32.10 17.40 9 14 -14 -12.30 17.60 8 -14 -14 28.40 17.20 -8 -14 14 -9.30 14.60 8 -14 -14 9.40 23.50 -8 14 14 -17.90 11.60 8 14 -14 6.10 20.20 -8 14 14 4.10 15.10 -7 -14 14 194.48 23.80 7 -14 -14 185.18 22.70 7 -14 -14 193.68 27.80 7 14 -14 204.98 26.30 -7 14 14 207.88 25.30 -7 14 14 194.48 20.90 6 -14 -14 59.59 23.10 -6 -14 14 64.59 16.30 6 14 -14 41.90 20.20 -6 14 14 75.09 16.50 -6 14 14 44.50 12.20 5 -14 -14 331.47 38.40 -5 -14 14 330.57 29.20 -5 14 14 377.26 29.00 -5 14 14 323.67 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23 103.39 15.50 11 3 -23 69.69 24.20 -10 -3 23 -8.60 10.60 -10 -3 23 7.80 10.90 10 -3 -23 3.00 21.60 10 3 -23 -12.20 21.80 -10 3 23 11.00 12.20 -10 3 23 3.50 11.90 9 -3 -23 47.90 25.10 -9 -3 23 52.09 11.80 -9 -3 23 52.09 12.20 -9 3 23 40.60 12.60 -9 3 23 38.60 13.10 9 3 -23 34.90 22.20 -8 -3 23 57.89 12.40 8 -3 -23 50.09 21.80 -8 -3 23 39.70 11.00 -8 3 23 38.00 13.20 8 3 -23 42.90 21.80 -8 3 23 51.29 11.70 -7 -3 23 16.40 9.70 7 -3 -23 -49.00 21.30 -7 -3 23 2.10 10.80 -7 3 23 -16.20 10.40 -7 3 23 -0.70 11.10 7 3 -23 -4.50 20.40 -6 -3 23 20.40 11.30 6 -3 -23 34.00 22.40 -6 -3 23 3.70 9.50 6 3 -23 -9.50 19.80 -6 3 23 17.00 11.20 -6 3 23 10.30 12.10 5 -3 -23 29.70 19.80 -5 -3 23 52.59 12.60 -5 3 23 39.90 12.10 5 3 -23 39.80 18.60 -5 3 23 51.09 13.10 -4 -3 23 15.80 10.00 4 -3 -23 -0.60 18.40 -4 -3 23 20.10 11.60 -4 3 23 53.79 13.20 4 3 -23 6.30 19.80 -4 3 23 15.80 10.80 3 -3 -23 441.56 34.90 -3 -3 23 395.96 28.90 -3 -3 23 486.55 28.30 3 3 -23 436.26 33.80 -3 3 23 419.66 29.30 -3 3 23 403.46 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-27 -23.40 28.10 -9 -3 27 48.50 13.80 -9 -3 27 7.20 14.40 -9 3 27 0.50 14.50 9 3 -27 14.40 27.20 -9 3 27 22.50 15.50 -8 -3 27 -3.00 12.90 8 -3 -27 -20.50 26.20 -8 -3 27 4.80 12.20 8 3 -27 -12.20 25.60 -8 3 27 -10.40 12.80 -8 3 27 9.70 13.90 7 -3 -27 39.10 26.10 -7 -3 27 15.20 12.00 -7 -3 27 12.20 12.10 -7 3 27 -27.50 13.20 7 3 -27 -3.80 25.50 -7 3 27 14.90 13.10 6 -3 -27 35.20 25.10 -6 -3 27 6.80 11.60 6 3 -27 -4.00 24.30 -6 3 27 6.10 14.30 -6 3 27 10.70 12.80 -5 -3 27 12.70 12.80 5 -3 -27 7.60 23.40 -5 3 27 4.50 14.10 5 3 -27 -15.60 22.50 -5 3 27 6.70 12.80 4 -3 -27 116.99 29.00 -4 -3 27 100.49 17.00 -4 3 27 116.19 16.50 -4 3 27 105.39 17.90 4 3 -27 95.49 23.30 3 -3 -27 77.09 26.90 -3 -3 27 86.39 15.20 3 3 -27 124.59 24.10 -3 3 27 95.59 15.60 -3 3 27 97.19 17.00 -2 -3 27 54.69 14.90 2 -3 -27 51.09 23.20 -2 3 27 41.40 15.50 2 3 -27 46.60 22.30 -2 3 27 52.39 13.80 -1 -3 27 246.08 24.70 1 -3 -27 225.08 30.80 1 3 -27 248.98 30.60 -1 3 27 254.97 25.10 -1 3 27 241.98 27.40 0 -3 -27 32.10 21.50 0 -3 27 17.40 12.40 0 3 -27 5.90 23.40 0 3 27 11.20 15.40 0 3 27 8.30 13.10 -1 -3 -27 101.99 25.90 1 -3 27 95.29 15.40 1 3 27 84.49 16.80 1 3 27 147.49 16.70 -2 -3 -27 -45.80 23.00 2 -3 27 13.10 12.30 2 3 27 -4.00 14.50 3 -3 27 4.60 13.70 -3 -3 -27 34.80 25.20 3 3 27 -6.00 15.00 4 -3 27 3.50 14.30 -4 -3 -27 18.70 25.60 4 3 27 32.30 17.50 9 -4 -27 119.09 34.20 -9 -4 27 74.19 17.40 9 4 -27 97.59 29.50 -9 4 27 130.89 18.90 -9 4 27 140.49 20.00 8 -4 -27 -78.89 29.20 -8 -4 27 13.00 13.90 -8 -4 27 -0.30 12.10 -8 4 27 6.00 14.50 -8 4 27 -11.30 14.80 8 4 -27 -14.10 25.80 -7 -4 27 89.79 16.30 7 -4 -27 136.29 32.00 -7 4 27 152.48 18.60 -7 4 27 131.79 19.10 7 4 -27 130.39 28.40 6 -4 -27 -36.10 27.00 -6 -4 27 4.90 12.40 6 4 -27 -26.80 23.60 -6 4 27 11.50 13.40 -6 4 27 10.90 15.40 5 -4 -27 107.49 27.40 -5 -4 27 119.29 16.80 -5 4 27 134.09 19.10 5 4 -27 122.89 26.70 -5 4 27 96.89 16.80 4 -4 -27 -27.30 23.60 -4 -4 27 -7.60 13.30 -4 4 27 13.00 13.50 -4 4 27 -11.70 15.20 4 4 -27 5.30 23.50 -3 -4 27 36.00 14.10 3 -4 -27 27.60 26.40 -3 4 27 22.90 15.70 -3 4 27 11.10 13.30 3 4 -27 31.70 24.10 -2 -4 27 -14.20 13.60 2 -4 -27 15.40 22.70 2 4 -27 -3.80 23.20 -2 4 27 3.50 13.00 -2 4 27 0.10 13.70 1 -4 -27 -17.40 24.40 -1 -4 27 1.70 13.20 -1 4 27 16.40 14.00 1 4 -27 -16.10 23.30 -1 4 27 26.60 17.40 0 -4 -27 -25.60 21.10 0 -4 27 13.00 12.60 0 4 27 2.50 13.50 0 4 -27 8.60 21.40 0 4 27 -22.00 14.40 1 -4 27 180.88 21.30 -1 -4 -27 159.28 27.80 1 4 27 155.38 22.10 1 4 27 157.68 18.60 2 -4 27 -4.70 12.70 -2 -4 -27 -8.40 24.50 2 4 27 7.90 17.60 2 4 27 7.60 13.80 3 -4 27 102.39 17.70 -3 -4 -27 105.39 28.00 3 4 27 129.09 22.20 8 -5 -27 -28.80 29.60 -8 -5 27 5.10 14.30 -8 5 27 13.10 15.30 8 5 -27 18.20 27.10 -8 5 27 -5.20 16.10 7 -5 -27 -13.60 30.00 -7 -5 27 -4.90 12.70 -7 5 27 -1.80 14.80 -7 5 27 -4.90 16.00 7 5 -27 -11.00 25.30 6 -5 -27 -22.10 29.20 -6 -5 27 -13.90 11.90 -6 5 27 1.40 14.20 -6 5 27 6.80 16.30 6 5 -27 -33.80 24.50 -5 -5 27 26.50 14.50 5 -5 -27 -27.70 27.00 -5 5 27 20.60 14.60 5 5 -27 5.50 23.00 -5 5 27 4.20 16.20 -4 -5 27 13.60 14.40 4 -5 -27 33.40 25.10 -4 5 27 -3.50 16.30 -4 5 27 18.60 13.80 4 5 -27 -13.80 20.60 3 -5 -27 37.10 28.00 -3 -5 27 44.40 14.30 -3 5 27 48.70 14.80 3 5 -27 72.09 24.50 -3 5 27 44.40 18.30 2 -5 -27 47.20 24.40 -2 -5 27 33.20 15.30 -2 5 27 35.40 15.00 -2 5 27 17.50 17.00 2 5 -27 50.09 23.60 -1 -5 27 195.38 24.20 1 -5 -27 131.59 30.10 1 5 -27 124.99 24.70 -1 5 27 142.89 18.70 -1 5 27 137.89 21.00 0 -5 -27 30.50 25.50 0 -5 27 11.50 14.50 0 5 27 2.70 14.20 0 5 27 37.80 17.80 1 -5 27 97.89 16.70 -1 -5 -27 83.19 24.80 1 5 27 104.99 17.20 1 5 27 106.79 21.10 -2 -5 -27 -28.00 24.40 2 -5 27 21.50 14.70 2 5 27 8.90 14.90 2 5 27 8.20 18.60 6 -6 -27 -21.20 30.60 -6 -6 27 -1.30 15.60 -6 6 27 -35.10 16.60 -6 6 27 19.90 15.60 6 6 -27 -8.20 25.70 -5 -6 27 75.69 17.20 5 -6 -27 93.99 31.30 -5 6 27 77.39 19.80 -5 6 27 91.99 17.80 5 6 -27 83.19 26.50 -4 -6 27 -1.60 14.50 4 -6 -27 39.50 26.10 -4 6 27 5.00 17.30 4 6 -27 16.20 24.20 -4 6 27 18.20 15.00 3 -6 -27 97.99 31.10 -3 -6 27 60.39 17.00 -3 6 27 64.89 17.20 -3 6 27 73.29 20.50 3 6 -27 136.09 26.80 2 -6 -27 -47.00 25.70 -2 -6 27 13.20 14.00 -2 6 27 13.30 15.10 -2 6 27 15.30 18.30 2 6 -27 46.50 25.00 1 -6 -27 3.90 26.80 -1 -6 27 13.70 15.20 -1 6 27 5.40 17.20 -1 6 27 -3.50 13.90 1 6 -27 42.50 24.80 0 -6 -27 -18.00 27.60 0 -6 27 44.70 16.10 0 6 27 -1.40 19.80 0 6 27 32.40 15.80 -8 0 28 96.99 16.80 8 0 -28 115.89 32.30 -8 0 28 120.49 17.80 7 0 -28 -11.60 25.80 -7 0 28 22.30 13.80 -7 0 28 2.40 14.10 6 0 -28 120.59 28.00 -6 0 28 135.59 17.80 -6 0 28 89.59 15.80 5 0 -28 -9.20 24.20 -5 0 28 27.70 14.10 -5 0 28 -14.20 12.00 4 0 -28 15.10 23.80 -4 0 28 52.99 13.70 -4 0 28 32.80 13.00 -3 0 28 14.50 14.00 3 0 -28 -44.80 25.10 -2 0 28 68.79 16.00 2 0 -28 -14.00 26.00 1 0 -28 -7.80 22.50 -1 0 28 -2.60 14.50 0 0 28 47.40 14.90 0 0 -28 78.09 27.30 1 0 28 -14.80 13.70 -1 0 -28 13.70 23.70 2 0 28 85.79 17.60 -8 -1 28 2.80 14.90 -8 -1 28 38.20 14.80 8 -1 -28 -13.90 30.70 -8 1 28 -2.00 13.70 8 1 -28 -32.80 29.80 -8 1 28 18.50 15.30 -7 -1 28 16.80 14.40 7 -1 -28 -4.60 28.50 -7 -1 28 5.90 13.00 7 1 -28 56.79 28.00 -7 1 28 4.50 13.40 -7 1 28 21.80 15.20 6 -1 -28 64.39 27.30 -6 -1 28 75.69 14.20 -6 -1 28 77.49 16.30 6 1 -28 71.49 27.00 -6 1 28 79.09 15.10 -6 1 28 62.29 15.90 5 -1 -28 -7.70 27.20 -5 -1 28 -0.10 14.00 -5 -1 28 27.50 12.50 -5 1 28 5.00 13.30 5 1 -28 -4.50 24.40 -5 1 28 -0.50 13.80 -4 -1 28 209.08 25.10 4 -1 -28 189.28 32.50 -4 1 28 211.58 25.30 4 1 -28 184.58 28.50 -4 1 28 198.18 23.10 -3 -1 28 13.90 12.70 3 -1 -28 -27.50 26.20 -3 1 28 11.00 14.20 -3 1 28 0.00 12.00 3 1 -28 -7.50 22.20 -2 -1 28 72.79 16.40 2 -1 -28 48.90 23.90 2 1 -28 78.99 27.00 -2 1 28 54.89 16.30 -1 -1 28 26.40 13.20 1 -1 -28 7.60 25.90 -1 1 28 7.40 14.90 1 1 -28 7.50 25.60 0 -1 -28 29.90 24.00 0 -1 28 16.60 14.80 0 1 -28 63.69 26.50 0 1 28 6.40 16.00 -1 -1 -28 19.30 26.70 1 -1 28 -8.60 14.70 -1 1 -28 -12.10 22.70 1 1 28 -13.00 15.50 7 -2 -28 -10.00 30.40 -7 -2 28 24.90 13.10 -7 -2 28 26.10 13.60 -7 2 28 8.00 13.60 7 2 -28 13.80 28.50 -7 2 28 33.30 15.30 -6 -2 28 25.70 15.60 -6 -2 28 53.49 14.50 6 -2 -28 64.99 31.20 6 2 -28 92.89 28.40 -6 2 28 85.79 16.00 -6 2 28 67.59 15.80 5 -2 -28 3.10 29.40 -5 -2 28 8.80 12.00 5 2 -28 -14.40 23.10 -5 2 28 -8.90 13.10 -5 2 28 -1.00 14.00 4 -2 -28 13.10 27.10 -4 -2 28 12.00 14.50 -4 2 28 -7.00 13.20 -4 2 28 18.70 13.80 4 2 -28 6.10 23.40 -3 -2 28 23.10 14.60 3 -2 -28 -10.10 23.80 3 2 -28 -16.90 24.70 -3 2 28 29.50 13.10 -3 2 28 5.30 15.10 2 -2 -28 86.99 28.80 -2 -2 28 64.49 15.80 -2 2 28 63.29 14.50 2 2 -28 73.29 27.00 -2 2 28 50.89 17.20 -1 -2 28 -15.20 13.30 1 -2 -28 18.60 23.70 -1 2 28 13.00 15.50 1 2 -28 22.80 26.20 -1 2 28 19.90 13.50 0 -2 -28 187.88 31.10 0 -2 28 148.49 20.30 0 2 -28 173.38 29.20 0 2 28 147.39 20.20 1 -2 28 14.10 15.10 -1 -2 -28 36.00 26.60 -1 2 -28 3.10 25.70 1 2 28 6.80 17.00 6 -3 -28 122.39 30.40 -6 -3 28 120.39 18.00 6 3 -28 138.59 30.50 -6 3 28 89.59 17.40 -6 3 28 117.79 19.40 5 -3 -28 -0.80 26.00 -5 -3 28 15.50 13.70 5 3 -28 -52.19 25.70 -5 3 28 32.70 14.30 -5 3 28 19.20 16.00 -4 -3 28 44.60 15.10 4 -3 -28 89.49 30.50 -4 3 28 109.19 16.30 4 3 -28 80.89 27.00 -4 3 28 64.99 17.80 3 -3 -28 36.00 28.40 -3 -3 28 9.90 14.70 -3 3 28 33.10 14.40 -3 3 28 -4.90 14.40 3 3 -28 36.60 25.90 2 -3 -28 109.19 27.40 -2 -3 28 120.69 17.70 2 3 -28 162.88 29.80 -2 3 28 124.49 20.40 -2 3 28 95.29 16.90 -1 -3 28 -13.90 13.60 1 -3 -28 -20.90 26.40 1 3 -28 -4.20 25.20 -1 3 28 -2.90 13.40 -1 3 28 4.50 15.90 0 -3 -28 62.19 27.80 0 -3 28 39.20 16.30 0 3 28 64.99 19.30 0 3 -28 70.89 26.80 0 3 28 91.19 16.10 -5 -4 28 15.60 14.80 -4 -4 28 7.80 14.70 4 -4 -28 -47.90 26.40 -4 4 28 7.70 14.30 -4 4 28 19.50 17.60 4 4 -28 -10.10 25.30 -3 -4 28 17.50 15.50 3 -4 -28 -2.90 29.30 3 4 -28 13.90 26.20 -3 4 28 9.50 14.60 -3 4 28 23.30 17.70 2 -4 -28 23.80 26.70 -2 -4 28 21.20 15.10 2 4 -28 37.20 25.50 -2 4 28 22.60 16.40 -2 4 28 -1.00 14.80 _computing_structure_solution 'SHELXT 2014/4 (Sheldrick, 2014)' ; _shelx_hkl_checksum 68807 ####################################################################### # # This file contains crystal structure data downloaded from the # Cambridge Structural Database (CSD) hosted by the Cambridge # Crystallographic Data Centre (CCDC). # # Full information about CCDC data access policies and citation # guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 # # Audit and citation data items may have been added by the CCDC. # Please retain this information to preserve the provenance of # this file and to allow appropriate attribution of the data. # ####################################################################### data_l0476a _database_code_depnum_ccdc_archive 'CCDC 1424620' _audit_update_record ; 2015-09-15 deposited with the CCDC. 2015-10-15 downloaded from the CCDC. ; _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C21 H21 N2 O P Rh, F6 P, C H4 O' _chemical_formula_sum 'C22 H25 F6 N2 O2 P2 Rh' _chemical_formula_weight 628.29 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Rh Rh -1.1178 0.9187 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.70447(19) _cell_length_b 9.77001(15) _cell_length_c 14.1603(3) _cell_angle_alpha 83.358(1) _cell_angle_beta 74.636(1) _cell_angle_gamma 74.636(1) _cell_volume 1246.84(4) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 37776 _cell_measurement_theta_min 2.24 _cell_measurement_theta_max 35.00 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.57 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.674 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 632 _exptl_absorpt_coefficient_mu 0.881 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6669 _exptl_absorpt_correction_T_max 0.7469 _exptl_absorpt_process_details SADABS-2012/1 _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Kappa ApexII' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 41801 _diffrn_reflns_av_R_equivalents 0.0147 _diffrn_reflns_av_sigmaI/netI 0.0138 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.24 _diffrn_reflns_theta_max 35.00 _reflns_number_total 10952 _reflns_number_gt 10239 _reflns_threshold_expression I>2\s(I) _computing_data_collection Apex2 _computing_cell_refinement Peaktref _computing_data_reduction 'Eval15, SADABS-2012/1' _computing_structure_solution 'SHELXT (Sheldrick, 2012)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0265P)^2^+0.5223P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10952 _refine_ls_number_parameters 330 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0243 _refine_ls_R_factor_gt 0.0221 _refine_ls_wR_factor_ref 0.0577 _refine_ls_wR_factor_gt 0.0567 _refine_ls_goodness_of_fit_ref 1.057 _refine_ls_restrained_S_all 1.058 _refine_ls_shift/su_max 0.014 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Rh1 Rh 0.265854(8) 0.519797(8) 0.194368(5) 0.01756(2) Uani 1 1 d . . . P1 P 0.04450(3) 0.64993(3) 0.183102(18) 0.01665(4) Uani 1 1 d . A . O1 O 0.43158(12) 0.67376(13) 0.02784(9) 0.0439(3) Uani 1 1 d . . . N1 N 0.14503(10) 0.42739(9) 0.31413(6) 0.01946(14) Uani 1 1 d . A . N2 N 0.43660(12) 0.36360(15) 0.24304(9) 0.0239(3) Uani 0.884(6) 1 d PD A 1 H2N H 0.439(2) 0.287(2) 0.2173(15) 0.031(5) Uiso 0.884(6) 1 d P A 1 N3 N 0.4375(10) 0.4181(13) 0.2630(7) 0.026(2) Uiso 0.116(6) 1 d PD A 2 H3N H 0.4355 0.4958 0.2960 0.031 Uiso 0.116(6) 1 calc PR A 2 C1 C 0.38332(14) 0.33262(14) 0.34894(9) 0.0307(2) Uani 1 1 d D . . H1A H 0.4060 0.3999 0.3864 0.037 Uiso 0.884(6) 1 calc PR A 1 H1B H 0.4353 0.2352 0.3666 0.037 Uiso 0.884(6) 1 calc PR A 1 H1C H 0.4109 0.3595 0.4054 0.037 Uiso 0.116(6) 1 calc PR A 2 H1D H 0.4345 0.2317 0.3375 0.037 Uiso 0.116(6) 1 calc PR A 2 C2 C 0.22029(13) 0.34496(11) 0.37646(8) 0.02366(18) Uani 1 1 d . A . C3 C 0.14722(16) 0.28381(13) 0.46181(9) 0.0304(2) Uani 1 1 d . . . H3 H 0.2007 0.2233 0.5044 0.036 Uiso 1 1 calc R A . C4 C -0.00524(16) 0.31250(14) 0.48392(9) 0.0309(2) Uani 1 1 d . A . H4 H -0.0572 0.2733 0.5428 0.037 Uiso 1 1 calc R . . C5 C -0.08230(13) 0.39840(12) 0.42017(8) 0.02505(19) Uani 1 1 d . . . H5 H -0.1869 0.4194 0.4352 0.030 Uiso 1 1 calc R A . C6 C -0.00361(11) 0.45291(10) 0.33417(7) 0.01948(16) Uani 1 1 d . A . C7 C -0.07423(11) 0.53651(11) 0.25625(8) 0.02074(17) Uani 1 1 d . . . H7A H -0.1722 0.5964 0.2870 0.025 Uiso 1 1 calc R A . H7B H -0.0881 0.4709 0.2132 0.025 Uiso 1 1 calc R . . C8 C -0.01434(11) 0.81458(10) 0.24660(7) 0.01817(15) Uani 1 1 d . . . C9 C -0.16379(12) 0.88443(12) 0.27273(9) 0.02472(19) Uani 1 1 d . A . H9 H -0.2341 0.8495 0.2533 0.030 Uiso 1 1 calc R . . C10 C -0.20931(13) 1.00486(12) 0.32718(10) 0.0307(2) Uani 1 1 d . . . H10 H -0.3110 1.0512 0.3460 0.037 Uiso 1 1 calc R A . C11 C -0.10660(15) 1.05756(13) 0.35413(10) 0.0310(2) Uani 1 1 d . A . H11 H -0.1382 1.1397 0.3917 0.037 Uiso 1 1 calc R . . C12 C 0.04214(14) 0.99071(12) 0.32645(9) 0.0277(2) Uani 1 1 d . . . H12 H 0.1124 1.0283 0.3439 0.033 Uiso 1 1 calc R A . C13 C 0.08858(12) 0.86870(11) 0.27322(8) 0.02215(17) Uani 1 1 d . A . H13 H 0.1904 0.8223 0.2550 0.027 Uiso 1 1 calc R . . C14 C -0.01884(11) 0.69948(11) 0.07124(7) 0.01991(16) Uani 1 1 d . . . C15 C -0.13649(15) 0.65832(14) 0.05450(9) 0.0307(2) Uani 1 1 d . A . H15 H -0.1859 0.5993 0.1022 0.037 Uiso 1 1 calc R . . C16 C -0.18266(17) 0.70285(16) -0.03163(10) 0.0352(3) Uani 1 1 d . . . H16 H -0.2632 0.6741 -0.0424 0.042 Uiso 1 1 calc R A . C17 C -0.11201(17) 0.78832(15) -0.10123(9) 0.0338(3) Uani 1 1 d . A . H17 H -0.1441 0.8189 -0.1598 0.041 Uiso 1 1 calc R . . C18 C 0.00621(18) 0.82988(18) -0.08580(10) 0.0407(3) Uani 1 1 d . . . H18 H 0.0556 0.8883 -0.1340 0.049 Uiso 1 1 calc R A . C19 C 0.05234(16) 0.78576(16) 0.00035(10) 0.0343(3) Uani 1 1 d . A . H19 H 0.1329 0.8147 0.0108 0.041 Uiso 1 1 calc R . . C20 C 0.36927(12) 0.61208(13) 0.09150(9) 0.0268(2) Uani 1 1 d . A . C21 C 0.58726(14) 0.38515(17) 0.21904(12) 0.0373(3) Uani 1 1 d . . . H21A H 0.6219 0.3990 0.1479 0.056 Uiso 0.88 1 d P A 1 H21B H 0.6533 0.3018 0.2425 0.056 Uiso 0.88 1 d P A 1 H21C H 0.5867 0.4695 0.2509 0.056 Uiso 0.88 1 d P A 1 H21D H 0.6020 0.4069 0.1483 0.056 Uiso 0.12 1 d P A 2 H21E H 0.6285 0.2838 0.2312 0.056 Uiso 0.12 1 d P A 2 H21F H 0.6370 0.4411 0.2461 0.056 Uiso 0.12 1 d P A 2 P2 P 0.45895(3) -0.25455(4) 0.40587(2) 0.02592(6) Uani 1 1 d . . . F1 F 0.53523(12) -0.24161(13) 0.29038(7) 0.0494(2) Uani 1 1 d . . . F2 F 0.34648(15) -0.10420(11) 0.39672(10) 0.0610(3) Uani 1 1 d . . . F3 F 0.38357(9) -0.26928(10) 0.52000(6) 0.03630(17) Uani 1 1 d . . . F4 F 0.57151(12) -0.40387(13) 0.41281(8) 0.0620(3) Uani 1 1 d . . . F5 F 0.56942(14) -0.17787(17) 0.43004(9) 0.0687(4) Uani 1 1 d . . . F6 F 0.34667(11) -0.33017(12) 0.38137(8) 0.0469(2) Uani 1 1 d . . . O2 O 0.4360(2) 0.07198(15) 0.21298(11) 0.0631(4) Uani 1 1 d . . . H2O H 0.436(4) -0.001(4) 0.258(3) 0.117(12) Uiso 1 1 d . . . C22 C 0.5009(4) 0.0048(2) 0.12469(16) 0.0801(9) Uani 1 1 d . . . H22A H 0.5105 0.0766 0.0706 0.120 Uiso 1 1 calc R . . H22B H 0.4390 -0.0542 0.1147 0.120 Uiso 1 1 calc R . . H22C H 0.5986 -0.0551 0.1268 0.120 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Rh1 0.01478(3) 0.01842(3) 0.01807(3) -0.00071(2) -0.00363(2) -0.00212(2) P1 0.01512(9) 0.01645(9) 0.01748(10) 0.00094(8) -0.00349(8) -0.00360(8) O1 0.0348(5) 0.0441(6) 0.0430(6) 0.0094(5) 0.0058(4) -0.0132(4) N1 0.0212(4) 0.0181(3) 0.0187(3) 0.0007(3) -0.0055(3) -0.0042(3) N2 0.0205(5) 0.0229(6) 0.0274(5) -0.0020(4) -0.0090(4) -0.0005(4) C1 0.0282(5) 0.0337(6) 0.0301(5) 0.0048(4) -0.0143(4) -0.0030(4) C2 0.0290(5) 0.0209(4) 0.0223(4) 0.0013(3) -0.0108(4) -0.0046(4) C3 0.0419(6) 0.0283(5) 0.0242(5) 0.0074(4) -0.0142(5) -0.0113(5) C4 0.0420(6) 0.0315(5) 0.0219(5) 0.0072(4) -0.0075(4) -0.0177(5) C5 0.0291(5) 0.0247(5) 0.0225(4) 0.0022(4) -0.0034(4) -0.0128(4) C6 0.0221(4) 0.0163(4) 0.0199(4) 0.0001(3) -0.0040(3) -0.0060(3) C7 0.0186(4) 0.0198(4) 0.0236(4) 0.0030(3) -0.0049(3) -0.0062(3) C8 0.0180(4) 0.0171(4) 0.0182(4) 0.0010(3) -0.0036(3) -0.0039(3) C9 0.0185(4) 0.0209(4) 0.0326(5) -0.0024(4) -0.0022(4) -0.0046(3) C10 0.0235(5) 0.0215(5) 0.0409(6) -0.0057(4) 0.0023(4) -0.0033(4) C11 0.0357(6) 0.0215(5) 0.0327(6) -0.0070(4) -0.0016(5) -0.0060(4) C12 0.0322(5) 0.0237(5) 0.0303(5) -0.0034(4) -0.0113(4) -0.0073(4) C13 0.0222(4) 0.0211(4) 0.0244(4) -0.0004(3) -0.0089(3) -0.0044(3) C14 0.0197(4) 0.0202(4) 0.0192(4) 0.0002(3) -0.0054(3) -0.0036(3) C15 0.0342(6) 0.0364(6) 0.0290(5) 0.0070(4) -0.0149(5) -0.0179(5) C16 0.0411(7) 0.0415(7) 0.0329(6) 0.0030(5) -0.0212(5) -0.0166(6) C17 0.0422(7) 0.0377(6) 0.0244(5) 0.0018(4) -0.0160(5) -0.0082(5) C18 0.0451(8) 0.0535(8) 0.0288(6) 0.0178(6) -0.0156(5) -0.0227(7) C19 0.0347(6) 0.0454(7) 0.0295(6) 0.0147(5) -0.0146(5) -0.0215(5) C20 0.0194(4) 0.0284(5) 0.0287(5) -0.0006(4) -0.0016(4) -0.0040(4) C21 0.0202(5) 0.0457(7) 0.0437(7) 0.0024(6) -0.0110(5) -0.0027(5) P2 0.01852(11) 0.03430(15) 0.02659(13) 0.00155(11) -0.00777(10) -0.00831(10) F1 0.0480(5) 0.0746(7) 0.0266(4) 0.0088(4) -0.0079(4) -0.0226(5) F2 0.0674(7) 0.0356(5) 0.0718(8) 0.0051(5) -0.0232(6) 0.0043(5) F3 0.0276(4) 0.0508(5) 0.0288(4) -0.0051(3) -0.0010(3) -0.0114(3) F4 0.0420(5) 0.0668(7) 0.0464(6) 0.0077(5) -0.0002(4) 0.0244(5) F5 0.0649(7) 0.1205(11) 0.0489(6) 0.0096(6) -0.0200(5) -0.0702(8) F6 0.0471(5) 0.0601(6) 0.0469(5) -0.0035(4) -0.0180(4) -0.0292(5) O2 0.1049(13) 0.0349(6) 0.0487(7) 0.0020(5) -0.0214(8) -0.0147(7) C22 0.150(3) 0.0405(9) 0.0444(10) 0.0003(8) -0.0307(13) -0.0088(13) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Rh1 C20 1.8283(12) . ? Rh1 N1 2.0540(9) . ? Rh1 N3 2.113(9) . ? Rh1 N2 2.1381(10) . ? Rh1 P1 2.2234(3) . ? P1 C8 1.8160(10) . ? P1 C14 1.8172(10) . ? P1 C7 1.8458(10) . ? O1 C20 1.1489(15) . ? N1 C2 1.3515(13) . ? N1 C6 1.3536(13) . ? N2 C1 1.4747(17) . ? N2 C21 1.4768(18) . ? N2 H2N 0.86(2) . ? N3 C21 1.387(9) . ? N3 C1 1.453(7) . ? N3 H3N 0.9300 . ? C1 C2 1.5008(17) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C1 H1C 0.9900 . ? C1 H1D 0.9900 . ? C2 C3 1.3871(17) . ? C3 C4 1.386(2) . ? C3 H3 0.9500 . ? C4 C5 1.3886(17) . ? C4 H4 0.9500 . ? C5 C6 1.3865(14) . ? C5 H5 0.9500 . ? C6 C7 1.4999(14) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 C13 1.3945(14) . ? C8 C9 1.3985(14) . ? C9 C10 1.3884(16) . ? C9 H9 0.9500 . ? C10 C11 1.3868(19) . ? C10 H10 0.9500 . ? C11 C12 1.3870(18) . ? C11 H11 0.9500 . ? C12 C13 1.3912(16) . ? C12 H12 0.9500 . ? C13 H13 0.9500 . ? C14 C15 1.3893(16) . ? C14 C19 1.3931(16) . ? C15 C16 1.3933(17) . ? C15 H15 0.9500 . ? C16 C17 1.376(2) . ? C16 H16 0.9500 . ? C17 C18 1.389(2) . ? C17 H17 0.9500 . ? C18 C19 1.3927(18) . ? C18 H18 0.9500 . ? C19 H19 0.9500 . ? C21 H21A 0.9800 . ? C21 H21B 0.9791 . ? C21 H21C 0.9821 . ? C21 H21D 0.9799 . ? C21 H21E 0.9787 . ? C21 H21F 0.9823 . ? P2 F5 1.5835(10) . ? P2 F4 1.5844(10) . ? P2 F6 1.5936(9) . ? P2 F3 1.5947(9) . ? P2 F2 1.5960(11) . ? P2 F1 1.6120(10) . ? O2 C22 1.394(3) . ? O2 H2O 0.89(4) . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C20 Rh1 N1 176.57(4) . . ? C20 Rh1 N3 99.3(2) . . ? N1 Rh1 N3 81.3(2) . . ? C20 Rh1 N2 102.62(5) . . ? N1 Rh1 N2 78.97(4) . . ? N3 Rh1 N2 17.1(4) . . ? C20 Rh1 P1 95.60(4) . . ? N1 Rh1 P1 82.83(2) . . ? N3 Rh1 P1 157.2(3) . . ? N2 Rh1 P1 161.78(3) . . ? C8 P1 C14 103.69(5) . . ? C8 P1 C7 105.05(5) . . ? C14 P1 C7 104.86(5) . . ? C8 P1 Rh1 113.89(3) . . ? C14 P1 Rh1 126.30(3) . . ? C7 P1 Rh1 100.89(3) . . ? C2 N1 C6 120.60(9) . . ? C2 N1 Rh1 116.69(7) . . ? C6 N1 Rh1 122.60(7) . . ? C1 N2 C21 111.54(11) . . ? C1 N2 Rh1 108.30(8) . . ? C21 N2 Rh1 119.67(9) . . ? C1 N2 H2N 103.1(13) . . ? C21 N2 H2N 108.7(13) . . ? Rh1 N2 H2N 104.0(13) . . ? C21 N3 C1 118.4(6) . . ? C21 N3 Rh1 126.6(5) . . ? C1 N3 Rh1 110.5(5) . . ? C21 N3 H3N 97.0 . . ? C1 N3 H3N 97.0 . . ? Rh1 N3 H3N 97.0 . . ? N3 C1 C2 115.9(4) . . ? N2 C1 C2 111.23(9) . . ? N2 C1 H1A 109.4 . . ? C2 C1 H1A 109.4 . . ? N2 C1 H1B 109.4 . . ? C2 C1 H1B 109.4 . . ? H1A C1 H1B 108.0 . . ? N3 C1 H1C 108.3 . . ? C2 C1 H1C 108.3 . . ? N3 C1 H1D 108.3 . . ? C2 C1 H1D 108.3 . . ? H1C C1 H1D 107.4 . . ? N1 C2 C3 120.81(11) . . ? N1 C2 C1 115.29(10) . . ? C3 C2 C1 123.82(10) . . ? C4 C3 C2 118.82(11) . . ? C4 C3 H3 120.6 . . ? C2 C3 H3 120.6 . . ? C3 C4 C5 120.18(11) . . ? C3 C4 H4 119.9 . . ? C5 C4 H4 119.9 . . ? C6 C5 C4 118.69(11) . . ? C6 C5 H5 120.7 . . ? C4 C5 H5 120.7 . . ? N1 C6 C5 120.85(10) . . ? N1 C6 C7 115.90(9) . . ? C5 C6 C7 123.20(10) . . ? C6 C7 P1 109.37(7) . . ? C6 C7 H7A 109.8 . . ? P1 C7 H7A 109.8 . . ? C6 C7 H7B 109.8 . . ? P1 C7 H7B 109.8 . . ? H7A C7 H7B 108.2 . . ? C13 C8 C9 119.67(9) . . ? C13 C8 P1 120.12(7) . . ? C9 C8 P1 120.15(8) . . ? C10 C9 C8 119.92(11) . . ? C10 C9 H9 120.0 . . ? C8 C9 H9 120.0 . . ? C11 C10 C9 120.15(11) . . ? C11 C10 H10 119.9 . . ? C9 C10 H10 119.9 . . ? C10 C11 C12 120.20(11) . . ? C10 C11 H11 119.9 . . ? C12 C11 H11 119.9 . . ? C11 C12 C13 120.06(11) . . ? C11 C12 H12 120.0 . . ? C13 C12 H12 120.0 . . ? C12 C13 C8 119.97(10) . . ? C12 C13 H13 120.0 . . ? C8 C13 H13 120.0 . . ? C15 C14 C19 118.87(10) . . ? C15 C14 P1 123.13(8) . . ? C19 C14 P1 117.98(8) . . ? C14 C15 C16 120.54(12) . . ? C14 C15 H15 119.7 . . ? C16 C15 H15 119.7 . . ? C17 C16 C15 120.26(12) . . ? C17 C16 H16 119.9 . . ? C15 C16 H16 119.9 . . ? C16 C17 C18 119.90(11) . . ? C16 C17 H17 120.0 . . ? C18 C17 H17 120.0 . . ? C17 C18 C19 119.94(13) . . ? C17 C18 H18 120.0 . . ? C19 C18 H18 120.0 . . ? C18 C19 C14 120.49(12) . . ? C18 C19 H19 119.8 . . ? C14 C19 H19 119.8 . . ? O1 C20 Rh1 178.01(12) . . ? N2 C21 H21A 109.5 . . ? N2 C21 H21B 109.5 . . ? H21A C21 H21B 109.6 . . ? N2 C21 H21C 109.5 . . ? H21A C21 H21C 109.3 . . ? H21B C21 H21C 109.4 . . ? N3 C21 H21D 109.1 . . ? N3 C21 H21E 109.1 . . ? H21D C21 H21E 109.6 . . ? N3 C21 H21F 110.2 . . ? H21D C21 H21F 109.3 . . ? H21E C21 H21F 109.5 . . ? F5 P2 F4 90.18(8) . . ? F5 P2 F6 179.41(8) . . ? F4 P2 F6 90.41(7) . . ? F5 P2 F3 89.95(6) . . ? F4 P2 F3 90.34(5) . . ? F6 P2 F3 90.10(5) . . ? F5 P2 F2 90.05(8) . . ? F4 P2 F2 178.94(7) . . ? F6 P2 F2 89.36(7) . . ? F3 P2 F2 90.70(6) . . ? F5 P2 F1 90.51(6) . . ? F4 P2 F1 89.16(6) . . ? F6 P2 F1 89.45(6) . . ? F3 P2 F1 179.32(6) . . ? F2 P2 F1 89.80(7) . . ? C22 O2 H2O 103(2) . . ? O2 C22 H22A 109.5 . . ? O2 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? O2 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C20 Rh1 P1 C8 -84.83(5) . . . . ? N1 Rh1 P1 C8 92.10(4) . . . . ? N3 Rh1 P1 C8 45.9(8) . . . . ? N2 Rh1 P1 C8 94.67(14) . . . . ? C20 Rh1 P1 C14 45.44(6) . . . . ? N1 Rh1 P1 C14 -137.63(5) . . . . ? N3 Rh1 P1 C14 176.2(8) . . . . ? N2 Rh1 P1 C14 -135.05(14) . . . . ? C20 Rh1 P1 C7 163.18(5) . . . . ? N1 Rh1 P1 C7 -19.89(4) . . . . ? N3 Rh1 P1 C7 -66.1(8) . . . . ? N2 Rh1 P1 C7 -17.32(14) . . . . ? N3 Rh1 N1 C2 -2.5(4) . . . . ? N2 Rh1 N1 C2 14.69(8) . . . . ? P1 Rh1 N1 C2 -166.13(8) . . . . ? N3 Rh1 N1 C6 173.7(4) . . . . ? N2 Rh1 N1 C6 -169.10(9) . . . . ? P1 Rh1 N1 C6 10.08(8) . . . . ? C20 Rh1 N2 C1 151.22(10) . . . . ? N1 Rh1 N2 C1 -25.67(10) . . . . ? N3 Rh1 N2 C1 70.7(7) . . . . ? P1 Rh1 N2 C1 -28.3(2) . . . . ? C20 Rh1 N2 C21 21.91(13) . . . . ? N1 Rh1 N2 C21 -154.97(12) . . . . ? N3 Rh1 N2 C21 -58.6(7) . . . . ? P1 Rh1 N2 C21 -157.58(9) . . . . ? C20 Rh1 N3 C21 -23.5(11) . . . . ? N1 Rh1 N3 C21 160.0(11) . . . . ? N2 Rh1 N3 C21 79.3(13) . . . . ? P1 Rh1 N3 C21 -153.6(4) . . . . ? C20 Rh1 N3 C1 -179.0(7) . . . . ? N1 Rh1 N3 C1 4.4(7) . . . . ? N2 Rh1 N3 C1 -76.2(8) . . . . ? P1 Rh1 N3 C1 50.9(14) . . . . ? C21 N3 C1 N2 -78.7(12) . . . . ? Rh1 N3 C1 N2 79.1(9) . . . . ? C21 N3 C1 C2 -163.6(7) . . . . ? Rh1 N3 C1 C2 -5.8(9) . . . . ? C21 N2 C1 N3 60.5(9) . . . . ? Rh1 N2 C1 N3 -73.2(9) . . . . ? C21 N2 C1 C2 166.54(12) . . . . ? Rh1 N2 C1 C2 32.83(14) . . . . ? C6 N1 C2 C3 0.53(16) . . . . ? Rh1 N1 C2 C3 176.82(9) . . . . ? C6 N1 C2 C1 -176.27(10) . . . . ? Rh1 N1 C2 C1 0.02(13) . . . . ? N3 C1 C2 N1 4.0(7) . . . . ? N2 C1 C2 N1 -22.81(16) . . . . ? N3 C1 C2 C3 -172.7(6) . . . . ? N2 C1 C2 C3 160.49(12) . . . . ? N1 C2 C3 C4 -2.13(18) . . . . ? C1 C2 C3 C4 174.39(12) . . . . ? C2 C3 C4 C5 1.48(19) . . . . ? C3 C4 C5 C6 0.71(18) . . . . ? C2 N1 C6 C5 1.75(15) . . . . ? Rh1 N1 C6 C5 -174.31(8) . . . . ? C2 N1 C6 C7 -175.51(9) . . . . ? Rh1 N1 C6 C7 8.43(12) . . . . ? C4 C5 C6 N1 -2.35(16) . . . . ? C4 C5 C6 C7 174.71(11) . . . . ? N1 C6 C7 P1 -26.35(11) . . . . ? C5 C6 C7 P1 156.46(9) . . . . ? C8 P1 C7 C6 -88.76(8) . . . . ? C14 P1 C7 C6 162.29(7) . . . . ? Rh1 P1 C7 C6 29.85(7) . . . . ? C14 P1 C8 C13 -123.28(8) . . . . ? C7 P1 C8 C13 126.92(8) . . . . ? Rh1 P1 C8 C13 17.46(9) . . . . ? C14 P1 C8 C9 59.46(9) . . . . ? C7 P1 C8 C9 -50.34(9) . . . . ? Rh1 P1 C8 C9 -159.80(8) . . . . ? C13 C8 C9 C10 -1.72(16) . . . . ? P1 C8 C9 C10 175.55(9) . . . . ? C8 C9 C10 C11 1.21(19) . . . . ? C9 C10 C11 C12 0.3(2) . . . . ? C10 C11 C12 C13 -1.33(19) . . . . ? C11 C12 C13 C8 0.81(17) . . . . ? C9 C8 C13 C12 0.71(16) . . . . ? P1 C8 C13 C12 -176.56(9) . . . . ? C8 P1 C14 C15 -107.86(10) . . . . ? C7 P1 C14 C15 2.08(11) . . . . ? Rh1 P1 C14 C15 118.03(10) . . . . ? C8 P1 C14 C19 70.52(11) . . . . ? C7 P1 C14 C19 -179.54(10) . . . . ? Rh1 P1 C14 C19 -63.60(11) . . . . ? C19 C14 C15 C16 -0.1(2) . . . . ? P1 C14 C15 C16 178.23(11) . . . . ? C14 C15 C16 C17 0.0(2) . . . . ? C15 C16 C17 C18 0.3(2) . . . . ? C16 C17 C18 C19 -0.4(3) . . . . ? C17 C18 C19 C14 0.3(3) . . . . ? C15 C14 C19 C18 0.0(2) . . . . ? P1 C14 C19 C18 -178.46(13) . . . . ? C1 N3 C21 N2 75.2(10) . . . . ? Rh1 N3 C21 N2 -78.6(11) . . . . ? C1 N2 C21 N3 -64.3(7) . . . . ? Rh1 N2 C21 N3 63.5(7) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N2 H2N O2 0.86(2) 2.11(2) 2.931(2) 157.4(18) . O2 H2O F1 0.89(4) 2.34(4) 3.1201(18) 146(3) . O2 H2O F2 0.89(4) 2.18(4) 3.0076(19) 154(3) . _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 35.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.610 _refine_diff_density_min -0.533 _refine_diff_density_rms 0.062 #===END