data_refin _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 'C22 H30 B Cl F4 N2 O Pd' _chemical_formula_weight 567.14 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' 'B' 'B' 0.0013 0.0007 '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' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Pd' 'Pd' -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_H-M_alt 'P -1' _space_group_name_Hall '-P 1' _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, -z' _cell_length_a 7.3768(4) _cell_length_b 12.0798(7) _cell_length_c 15.1667(9) _cell_angle_alpha 93.531(3) _cell_angle_beta 89.979(4) _cell_angle_gamma 107.760(3) _cell_volume 1284.41(13) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 101 _cell_measurement_theta_min 6.7018 _cell_measurement_theta_max 22.9845 _exptl_crystal_description block _exptl_crystal_colour 'red' _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_density_diffrn 1.466 _exptl_crystal_F_000 576 _exptl_transmission_factor_min 0.6374 _exptl_transmission_factor_max 0.7465 _exptl_crystal_size_max 0.362 _exptl_crystal_size_mid 0.163 _exptl_crystal_size_min 0.137 _exptl_absorpt_coefficient_mu 0.871 _shelx_estimated_absorpt_T_min 0.743 _shelx_estimated_absorpt_T_max 0.890 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.76 _exptl_absorpt_correction_T_max 0.89 _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 31066 _diffrn_reflns_av_unetI/netI 0.0534 _diffrn_reflns_av_R_equivalents 0.0874 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.900 _diffrn_reflns_theta_max 25.200 _diffrn_reflns_theta_full 25.200 _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 4607 _reflns_number_gt 3779 _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. Structure factors included contributions from the .fab file. _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^)+(0.0263P)^2^+0.9031P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary ? _atom_sites_solution_secondary ? _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef . _refine_ls_number_reflns 4607 _refine_ls_number_parameters 470 _refine_ls_number_restraints 866 _refine_ls_R_factor_all 0.0518 _refine_ls_R_factor_gt 0.0339 _refine_ls_wR_factor_ref 0.0679 _refine_ls_wR_factor_gt 0.0628 _refine_ls_goodness_of_fit_ref 1.015 _refine_ls_restrained_S_all 0.970 _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 Pd1 Pd 0.79883(4) 0.59770(2) 0.43689(2) 0.01649(8) Uani 1 1 d . . . . . Cl1 Cl 0.83236(13) 0.66487(7) 0.58154(5) 0.0272(2) Uani 1 1 d . . . . . C1 C 0.8753(4) 0.7513(3) 0.3050(2) 0.0161(7) Uani 1 1 d . . . . . C2 C 0.9269(4) 0.8538(3) 0.2549(2) 0.0191(7) Uani 1 1 d . . . . . C3 C 0.9172(5) 0.8344(3) 0.1667(2) 0.0276(8) Uani 1 1 d . . . . . H3 H 0.9509 0.9008 0.1326 0.033 Uiso 1 1 calc R U . . . C4 C 0.8598(5) 0.7207(3) 0.1185(2) 0.0242(8) Uani 1 1 d D . . . . C5 C 0.8113(4) 0.6235(3) 0.1630(2) 0.0183(7) Uani 1 1 d . . . . . H5 H 0.7740 0.5491 0.1319 0.022 Uiso 1 1 calc R U . . . C6 C 0.8164(4) 0.6326(3) 0.2578(2) 0.0159(7) Uani 1 1 d . . . . . C7 C 0.7099(5) 0.4207(3) 0.2886(2) 0.0199(7) Uani 1 1 d . . . . . C8 C 0.6810(4) 0.3620(3) 0.3764(2) 0.0192(7) Uani 1 1 d . . . . . C9 C 0.6208(5) 0.2417(3) 0.3783(2) 0.0269(8) Uani 1 1 d . . . . . H9 H 0.5970 0.1942 0.3247 0.032 Uiso 1 1 calc R U . . . C10 C 0.5955(5) 0.1911(3) 0.4581(2) 0.0279(8) Uani 1 1 d . . . . . H10 H 0.5545 0.1087 0.4596 0.033 Uiso 1 1 calc R U . . . C11 C 0.6295(5) 0.2598(3) 0.5355(2) 0.0275(8) Uani 1 1 d . . . . . H11 H 0.6121 0.2258 0.5909 0.033 Uiso 1 1 calc R U . . . C12 C 0.6893(5) 0.3784(3) 0.5310(2) 0.0234(8) Uani 1 1 d . . . . . H12 H 0.7138 0.4264 0.5843 0.028 Uiso 1 1 calc R U . . . C13 C 0.9881(5) 0.9752(3) 0.3034(2) 0.0259(8) Uani 1 1 d . . . . . C14 C 1.1654(5) 0.9912(3) 0.3612(2) 0.0367(9) Uani 1 1 d . . . . . H14A H 1.2697 0.9828 0.3240 0.055 Uiso 1 1 calc R U . . . H14B H 1.1374 0.9321 0.4049 0.055 Uiso 1 1 calc R U . . . H14C H 1.2028 1.0690 0.3917 0.055 Uiso 1 1 calc R U . . . C15 C 0.8251(5) 0.9912(3) 0.3614(2) 0.0354(9) Uani 1 1 d . . . . . H15A H 0.7953 0.9329 0.4057 0.053 Uiso 1 1 calc R U . . . H15B H 0.7121 0.9816 0.3242 0.053 Uiso 1 1 calc R U . . . H15C H 0.8645 1.0695 0.3911 0.053 Uiso 1 1 calc R U . . . C16 C 1.0363(7) 1.0707(3) 0.2375(3) 0.0491(12) Uani 1 1 d . . . . . H16A H 1.0771 1.1473 0.2698 0.074 Uiso 1 1 calc R U . . . H16B H 0.9234 1.0641 0.2010 0.074 Uiso 1 1 calc R U . . . H16C H 1.1392 1.0619 0.1996 0.074 Uiso 1 1 calc R U . . . C17 C 0.881(3) 0.7182(17) 0.0177(4) 0.037(3) Uani 0.53(3) 1 d D U P A 1 C18 C 0.811(4) 0.5963(17) -0.027(3) 0.040(2) Uani 0.53(3) 1 d D U P A 1 H18A H 0.8897 0.5499 -0.0072 0.060 Uiso 0.53(3) 1 calc R U P A 1 H18B H 0.8203 0.6010 -0.0913 0.060 Uiso 0.53(3) 1 calc R U P A 1 H18C H 0.6782 0.5594 -0.0117 0.060 Uiso 0.53(3) 1 calc R U P A 1 C19 C 0.759(3) 0.7900(14) -0.0177(11) 0.049(3) Uani 0.53(3) 1 d D U P A 1 H19A H 0.7734 0.7935 -0.0819 0.073 Uiso 0.53(3) 1 calc R U P A 1 H19B H 0.8019 0.8691 0.0104 0.073 Uiso 0.53(3) 1 calc R U P A 1 H19C H 0.6253 0.7530 -0.0043 0.073 Uiso 0.53(3) 1 calc R U P A 1 C20 C 1.093(3) 0.7725(17) -0.0059(11) 0.051(4) Uani 0.53(3) 1 d D U P A 1 H20A H 1.1675 0.7249 0.0156 0.077 Uiso 0.53(3) 1 calc R U P A 1 H20B H 1.1403 0.8516 0.0220 0.077 Uiso 0.53(3) 1 calc R U P A 1 H20C H 1.1036 0.7755 -0.0701 0.077 Uiso 0.53(3) 1 calc R U P A 1 C17' C 0.835(3) 0.7185(19) 0.0179(5) 0.034(3) Uani 0.47(3) 1 d D U P A 2 C18' C 0.783(5) 0.5943(19) -0.023(3) 0.040(2) Uani 0.47(3) 1 d D U P A 2 H18D H 0.8765 0.5575 -0.0040 0.060 Uiso 0.47(3) 1 calc R U P A 2 H18E H 0.7818 0.5953 -0.0873 0.060 Uiso 0.47(3) 1 calc R U P A 2 H18F H 0.6562 0.5501 -0.0032 0.060 Uiso 0.47(3) 1 calc R U P A 2 C19' C 0.677(3) 0.7704(18) -0.0060(12) 0.044(4) Uani 0.47(3) 1 d D U P A 2 H19D H 0.6668 0.7708 -0.0704 0.066 Uiso 0.47(3) 1 calc R U P A 2 H19E H 0.7082 0.8503 0.0202 0.066 Uiso 0.47(3) 1 calc R U P A 2 H19F H 0.5559 0.7231 0.0170 0.066 Uiso 0.47(3) 1 calc R U P A 2 C20' C 1.027(3) 0.7902(15) -0.0175(11) 0.044(3) Uani 0.47(3) 1 d D U P A 2 H20D H 1.1276 0.7591 0.0021 0.066 Uiso 0.47(3) 1 calc R U P A 2 H20E H 1.0558 0.8716 0.0049 0.066 Uiso 0.47(3) 1 calc R U P A 2 H20F H 1.0211 0.7856 -0.0823 0.066 Uiso 0.47(3) 1 calc R U P A 2 C21 C 0.8668(5) 0.3868(3) 0.2379(2) 0.0305(9) Uani 1 1 d . . . . . H21A H 0.8862 0.4236 0.1815 0.046 Uiso 1 1 calc R U . . . H21B H 0.8291 0.3019 0.2269 0.046 Uiso 1 1 calc R U . . . H21C H 0.9856 0.4130 0.2730 0.046 Uiso 1 1 calc R U . . . C22 C 0.5199(5) 0.3863(3) 0.2382(2) 0.0308(9) Uani 1 1 d . . . . . H22A H 0.4279 0.4139 0.2726 0.046 Uiso 1 1 calc R U . . . H22B H 0.4720 0.3013 0.2285 0.046 Uiso 1 1 calc R U . . . H22C H 0.5377 0.4216 0.1811 0.046 Uiso 1 1 calc R U . . . N1 N 0.7744(3) 0.5488(2) 0.31173(17) 0.0160(6) Uani 1 1 d . . . . . N2 N 0.7145(4) 0.4293(2) 0.45329(17) 0.0182(6) Uani 1 1 d . . . . . O1 O 0.8790(3) 0.75756(18) 0.38782(14) 0.0208(5) Uani 1 1 d . . . . . B1 B 0.350(3) 0.7033(17) 0.2234(12) 0.047(2) Uani 0.345(3) 1 d D U P B 1 F1 F 0.304(2) 0.6197(10) 0.1582(7) 0.071(3) Uani 0.345(3) 1 d D U P B 1 F2 F 0.506(3) 0.704(2) 0.2738(14) 0.043(3) Uani 0.345(3) 1 d D U P B 1 F3 F 0.201(2) 0.7057(16) 0.2781(10) 0.040(3) Uani 0.345(3) 1 d D U P B 1 F4 F 0.3931(17) 0.8121(9) 0.1827(6) 0.077(3) Uani 0.345(3) 1 d D U P B 1 B1' B 0.346(4) 0.689(3) 0.2205(18) 0.051(3) Uani 0.133(3) 1 d D U P C 2 F1' F 0.382(5) 0.694(3) 0.1340(18) 0.064(4) Uani 0.133(3) 1 d D U P C 2 F2' F 0.508(5) 0.709(5) 0.273(3) 0.049(4) Uani 0.133(3) 1 d D U P C 2 F3' F 0.254(4) 0.7677(19) 0.2502(19) 0.051(4) Uani 0.133(3) 1 d D U P C 2 F4' F 0.224(3) 0.5743(19) 0.2370(15) 0.058(4) Uani 0.133(3) 1 d D U P C 2 B1C B 0.342(3) 0.676(2) 0.2181(15) 0.049(3) Uani 0.244(3) 1 d D U P D 3 F1C F 0.354(3) 0.654(3) 0.1312(12) 0.062(4) Uani 0.244(3) 1 d D U P D 3 F2C F 0.516(2) 0.7478(12) 0.2506(10) 0.051(3) Uani 0.244(3) 1 d D U P D 3 F3C F 0.202(3) 0.720(2) 0.2505(13) 0.048(4) Uani 0.244(3) 1 d D U P D 3 F4C F 0.3062(18) 0.5622(10) 0.2509(8) 0.058(3) Uani 0.244(3) 1 d D U P D 3 B1D B 0.349(3) 0.702(2) 0.2174(12) 0.048(3) Uani 0.277(3) 1 d D U P E 4 F1D F 0.302(3) 0.666(2) 0.1328(11) 0.061(4) Uani 0.277(3) 1 d D U P E 4 F2D F 0.479(2) 0.6648(13) 0.2627(12) 0.052(3) Uani 0.277(3) 1 d D U P E 4 F3D F 0.189(3) 0.6688(14) 0.2674(14) 0.047(4) Uani 0.277(3) 1 d D U P E 4 F4D F 0.431(2) 0.8269(11) 0.2193(8) 0.070(3) Uani 0.277(3) 1 d D U P E 4 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 Pd1 0.01845(14) 0.01893(13) 0.01271(13) 0.00375(9) 0.00142(9) 0.00609(10) Cl1 0.0380(5) 0.0272(5) 0.0156(4) 0.0012(3) 0.0004(4) 0.0088(4) C1 0.0086(16) 0.0223(17) 0.0194(18) 0.0034(14) -0.0012(13) 0.0071(14) C2 0.0181(17) 0.0165(16) 0.0244(18) 0.0066(14) 0.0033(14) 0.0069(14) C3 0.039(2) 0.0215(18) 0.0225(19) 0.0056(15) -0.0004(16) 0.0081(16) C4 0.0264(19) 0.0299(19) 0.0166(18) 0.0035(15) 0.0033(15) 0.0085(16) C5 0.0165(17) 0.0201(17) 0.0185(17) 0.0000(14) 0.0006(14) 0.0060(14) C6 0.0090(16) 0.0220(17) 0.0176(17) 0.0015(14) 0.0022(13) 0.0060(13) C7 0.0227(18) 0.0152(16) 0.0199(18) 0.0008(14) -0.0014(14) 0.0030(14) C8 0.0149(17) 0.0228(17) 0.0213(18) 0.0036(14) -0.0006(14) 0.0076(14) C9 0.031(2) 0.0211(18) 0.028(2) 0.0030(15) 0.0014(16) 0.0072(16) C10 0.030(2) 0.0206(18) 0.033(2) 0.0064(16) 0.0024(17) 0.0065(16) C11 0.026(2) 0.0281(19) 0.029(2) 0.0113(16) 0.0030(16) 0.0081(16) C12 0.0226(19) 0.0305(19) 0.0178(17) 0.0053(15) 0.0009(15) 0.0085(16) C13 0.036(2) 0.0209(18) 0.0197(18) 0.0040(14) 0.0007(16) 0.0069(16) C14 0.036(2) 0.030(2) 0.037(2) -0.0041(17) -0.0020(18) -0.0006(17) C15 0.047(2) 0.0263(19) 0.036(2) -0.0004(17) 0.0024(19) 0.0167(18) C16 0.085(3) 0.0201(19) 0.036(2) 0.0087(18) 0.003(2) 0.007(2) C17 0.057(7) 0.037(4) 0.015(4) 0.005(3) 0.000(4) 0.011(5) C18 0.055(6) 0.044(2) 0.018(4) 0.001(2) 0.002(5) 0.012(3) C19 0.069(9) 0.043(5) 0.032(5) 0.012(4) 0.003(6) 0.011(6) C20 0.054(8) 0.065(7) 0.022(5) 0.012(5) 0.019(5) -0.004(5) C17' 0.049(7) 0.035(4) 0.017(4) 0.001(4) 0.005(4) 0.010(5) C18' 0.055(6) 0.044(2) 0.018(4) 0.001(2) 0.002(5) 0.012(3) C19' 0.068(9) 0.055(7) 0.020(6) 0.006(5) -0.010(6) 0.032(7) C20' 0.063(9) 0.044(6) 0.023(5) 0.008(4) 0.003(6) 0.012(6) C21 0.040(2) 0.031(2) 0.026(2) 0.0044(16) 0.0098(17) 0.0195(18) C22 0.029(2) 0.0296(19) 0.028(2) 0.0059(16) -0.0069(16) -0.0018(16) N1 0.0136(14) 0.0174(14) 0.0183(15) 0.0026(12) 0.0014(11) 0.0063(11) N2 0.0162(14) 0.0216(14) 0.0178(15) 0.0065(12) 0.0008(12) 0.0063(12) O1 0.0236(13) 0.0224(12) 0.0148(12) 0.0023(9) 0.0012(10) 0.0046(10) B1 0.036(4) 0.070(5) 0.038(4) -0.006(4) -0.006(4) 0.024(4) F1 0.081(5) 0.072(6) 0.047(5) -0.032(4) 0.002(5) 0.011(5) F2 0.025(4) 0.063(6) 0.045(5) -0.017(5) -0.004(4) 0.025(5) F3 0.016(4) 0.077(7) 0.034(5) -0.007(5) -0.006(4) 0.027(5) F4 0.092(5) 0.078(5) 0.051(5) 0.007(4) -0.020(4) 0.008(4) B1' 0.041(4) 0.072(5) 0.042(4) -0.008(4) -0.007(4) 0.022(4) F1' 0.059(7) 0.082(7) 0.040(6) -0.015(6) -0.005(6) 0.009(7) F2' 0.035(7) 0.069(8) 0.047(7) -0.009(7) -0.008(7) 0.023(7) F3' 0.040(7) 0.070(7) 0.052(7) -0.013(7) -0.009(6) 0.033(6) F4' 0.040(6) 0.075(7) 0.053(6) -0.009(6) -0.008(6) 0.013(6) B1C 0.038(4) 0.072(5) 0.040(4) -0.008(4) -0.007(4) 0.022(4) F1C 0.066(7) 0.069(7) 0.036(6) -0.022(6) 0.005(6) 0.002(7) F2C 0.024(4) 0.078(7) 0.053(6) -0.004(5) -0.011(4) 0.019(5) F3C 0.030(6) 0.073(7) 0.046(6) -0.002(6) -0.005(5) 0.024(5) F4C 0.065(5) 0.063(5) 0.053(5) -0.004(4) -0.022(5) 0.030(5) B1D 0.038(4) 0.070(5) 0.039(4) -0.006(4) -0.006(4) 0.023(4) F1D 0.061(6) 0.079(7) 0.036(5) -0.011(5) -0.004(5) 0.014(6) F2D 0.038(5) 0.076(6) 0.057(5) -0.011(5) -0.006(4) 0.043(5) F3D 0.024(5) 0.071(7) 0.044(6) 0.002(6) 0.001(4) 0.011(5) F4D 0.071(5) 0.073(5) 0.053(5) 0.000(5) -0.026(5) 0.002(5) _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 Pd1 N1 1.945(3) . ? Pd1 N2 1.969(2) . ? Pd1 O1 2.028(2) . ? Pd1 Cl1 2.2785(9) . ? C1 O1 1.254(4) . ? C1 C2 1.443(4) . ? C1 C6 1.500(4) . ? C2 C3 1.343(5) . ? C2 C13 1.536(5) . ? C3 C4 1.456(5) . ? C3 H3 0.9500 . ? C4 C5 1.343(4) . ? C4 C17' 1.535(8) . ? C4 C17 1.537(7) . ? C5 C6 1.434(4) . ? C5 H5 0.9500 . ? C6 N1 1.304(4) . ? C7 N1 1.492(4) . ? C7 C22 1.526(4) . ? C7 C8 1.531(4) . ? C7 C21 1.533(4) . ? C8 N2 1.358(4) . ? C8 C9 1.386(4) . ? C9 C10 1.375(5) . ? C9 H9 0.9500 . ? C10 C11 1.372(5) . ? C10 H10 0.9500 . ? C11 C12 1.371(4) . ? C11 H11 0.9500 . ? C12 N2 1.349(4) . ? C12 H12 0.9500 . ? C13 C14 1.530(5) . ? C13 C16 1.534(5) . ? C13 C15 1.541(5) . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? 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 C18 1.520(11) . ? C17 C19 1.544(12) . ? C17 C20 1.547(12) . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C17' C18' 1.520(12) . ? C17' C20' 1.534(13) . ? C17' C19' 1.536(12) . ? C18' H18D 0.9800 . ? C18' H18E 0.9800 . ? C18' H18F 0.9800 . ? C19' H19D 0.9800 . ? C19' H19E 0.9800 . ? C19' H19F 0.9800 . ? C20' H20D 0.9800 . ? C20' H20E 0.9800 . ? C20' H20F 0.9800 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? B1 F1 1.335(13) . ? B1 F2 1.380(14) . ? B1 F3 1.380(14) . ? B1 F4 1.43(2) . ? B1' F1' 1.340(17) . ? B1' F3' 1.377(18) . ? B1' F2' 1.383(17) . ? B1' F4' 1.44(3) . ? B1C F1C 1.337(15) . ? B1C F3C 1.373(16) . ? B1C F2C 1.378(16) . ? B1C F4C 1.44(3) . ? B1D F1D 1.340(15) . ? B1D F3D 1.373(15) . ? B1D F2D 1.377(15) . ? B1D F4D 1.44(2) . ? 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 N1 Pd1 N2 84.16(10) . . ? N1 Pd1 O1 81.60(9) . . ? N2 Pd1 O1 165.76(9) . . ? N1 Pd1 Cl1 177.00(8) . . ? N2 Pd1 Cl1 98.84(8) . . ? O1 Pd1 Cl1 95.40(6) . . ? O1 C1 C2 122.0(3) . . ? O1 C1 C6 118.0(3) . . ? C2 C1 C6 119.9(3) . . ? C3 C2 C1 115.8(3) . . ? C3 C2 C13 124.4(3) . . ? C1 C2 C13 119.8(3) . . ? C2 C3 C4 125.9(3) . . ? C2 C3 H3 117.1 . . ? C4 C3 H3 117.1 . . ? C5 C4 C3 119.8(3) . . ? C5 C4 C17' 122.6(8) . . ? C3 C4 C17' 117.2(8) . . ? C5 C4 C17 122.5(8) . . ? C3 C4 C17 117.3(8) . . ? C4 C5 C6 119.6(3) . . ? C4 C5 H5 120.2 . . ? C6 C5 H5 120.2 . . ? N1 C6 C5 128.3(3) . . ? N1 C6 C1 112.8(3) . . ? C5 C6 C1 118.9(3) . . ? N1 C7 C22 109.9(3) . . ? N1 C7 C8 106.3(2) . . ? C22 C7 C8 108.8(3) . . ? N1 C7 C21 109.3(3) . . ? C22 C7 C21 113.5(3) . . ? C8 C7 C21 108.8(3) . . ? N2 C8 C9 119.8(3) . . ? N2 C8 C7 119.2(3) . . ? C9 C8 C7 121.0(3) . . ? C10 C9 C8 119.9(3) . . ? C10 C9 H9 120.1 . . ? C8 C9 H9 120.1 . . ? C11 C10 C9 120.0(3) . . ? C11 C10 H10 120.0 . . ? C9 C10 H10 120.0 . . ? C12 C11 C10 118.5(3) . . ? C12 C11 H11 120.7 . . ? C10 C11 H11 120.7 . . ? N2 C12 C11 122.2(3) . . ? N2 C12 H12 118.9 . . ? C11 C12 H12 118.9 . . ? C14 C13 C16 107.9(3) . . ? C14 C13 C2 110.4(3) . . ? C16 C13 C2 110.8(3) . . ? C14 C13 C15 109.6(3) . . ? C16 C13 C15 108.0(3) . . ? C2 C13 C15 110.1(3) . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C13 C15 H15A 109.5 . . ? C13 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C13 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C13 C16 H16A 109.5 . . ? C13 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C13 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C18 C17 C4 113(2) . . ? C18 C17 C19 108.1(13) . . ? C4 C17 C19 106.7(11) . . ? C18 C17 C20 108.1(12) . . ? C4 C17 C20 110.1(10) . . ? C19 C17 C20 110.4(10) . . ? 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 . . ? C17 C20 H20A 109.5 . . ? C17 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C17 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C18' C17' C20' 109.6(14) . . ? C18' C17' C4 111(2) . . ? C20' C17' C4 106.8(11) . . ? C18' C17' C19' 108.3(13) . . ? C20' C17' C19' 110.8(11) . . ? C4 C17' C19' 110.6(11) . . ? C17' C18' H18D 109.5 . . ? C17' C18' H18E 109.5 . . ? H18D C18' H18E 109.5 . . ? C17' C18' H18F 109.5 . . ? H18D C18' H18F 109.5 . . ? H18E C18' H18F 109.5 . . ? C17' C19' H19D 109.5 . . ? C17' C19' H19E 109.5 . . ? H19D C19' H19E 109.5 . . ? C17' C19' H19F 109.5 . . ? H19D C19' H19F 109.5 . . ? H19E C19' H19F 109.5 . . ? C17' C20' H20D 109.5 . . ? C17' C20' H20E 109.5 . . ? H20D C20' H20E 109.5 . . ? C17' C20' H20F 109.5 . . ? H20D C20' H20F 109.5 . . ? H20E C20' H20F 109.5 . . ? C7 C21 H21A 109.5 . . ? C7 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C7 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C7 C22 H22A 109.5 . . ? C7 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C7 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C6 N1 C7 127.7(3) . . ? C6 N1 Pd1 115.7(2) . . ? C7 N1 Pd1 116.63(19) . . ? C12 N2 C8 119.7(3) . . ? C12 N2 Pd1 126.6(2) . . ? C8 N2 Pd1 113.8(2) . . ? C1 O1 Pd1 111.87(19) . . ? F1 B1 F2 114.2(15) . . ? F1 B1 F3 114.3(14) . . ? F2 B1 F3 109.6(15) . . ? F1 B1 F4 106.6(15) . . ? F2 B1 F4 108.1(16) . . ? F3 B1 F4 103.2(14) . . ? F1' B1' F3' 113(2) . . ? F1' B1' F2' 113(2) . . ? F3' B1' F2' 108(2) . . ? F1' B1' F4' 109(2) . . ? F3' B1' F4' 107(2) . . ? F2' B1' F4' 107(3) . . ? F1C B1C F3C 120.4(19) . . ? F1C B1C F2C 109.2(18) . . ? F3C B1C F2C 108.7(17) . . ? F1C B1C F4C 102.0(19) . . ? F3C B1C F4C 106.7(18) . . ? F2C B1C F4C 109.3(18) . . ? F1D B1D F3D 108.8(18) . . ? F1D B1D F2D 121.2(18) . . ? F3D B1D F2D 103.4(16) . . ? F1D B1D F4D 106.3(18) . . ? F3D B1D F4D 112.4(16) . . ? F2D B1D F4D 104.8(16) . . ? 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 O1 C1 C2 C3 179.8(3) . . . . ? C6 C1 C2 C3 0.2(4) . . . . ? O1 C1 C2 C13 -0.1(5) . . . . ? C6 C1 C2 C13 -179.7(3) . . . . ? C1 C2 C3 C4 0.1(5) . . . . ? C13 C2 C3 C4 -179.9(3) . . . . ? C2 C3 C4 C5 -0.3(6) . . . . ? C2 C3 C4 C17' 172.7(9) . . . . ? C2 C3 C4 C17 -173.0(9) . . . . ? C3 C4 C5 C6 0.1(5) . . . . ? C17' C4 C5 C6 -172.5(9) . . . . ? C17 C4 C5 C6 172.4(9) . . . . ? C4 C5 C6 N1 179.9(3) . . . . ? C4 C5 C6 C1 0.2(4) . . . . ? O1 C1 C6 N1 0.3(4) . . . . ? C2 C1 C6 N1 179.9(3) . . . . ? O1 C1 C6 C5 -180.0(3) . . . . ? C2 C1 C6 C5 -0.4(4) . . . . ? N1 C7 C8 N2 0.3(4) . . . . ? C22 C7 C8 N2 -118.0(3) . . . . ? C21 C7 C8 N2 117.9(3) . . . . ? N1 C7 C8 C9 -179.9(3) . . . . ? C22 C7 C8 C9 61.8(4) . . . . ? C21 C7 C8 C9 -62.3(4) . . . . ? N2 C8 C9 C10 -0.1(5) . . . . ? C7 C8 C9 C10 -179.9(3) . . . . ? C8 C9 C10 C11 0.1(5) . . . . ? C9 C10 C11 C12 -0.2(5) . . . . ? C10 C11 C12 N2 0.3(5) . . . . ? C3 C2 C13 C14 -119.4(4) . . . . ? C1 C2 C13 C14 60.5(4) . . . . ? C3 C2 C13 C16 0.0(5) . . . . ? C1 C2 C13 C16 180.0(3) . . . . ? C3 C2 C13 C15 119.4(4) . . . . ? C1 C2 C13 C15 -60.7(4) . . . . ? C5 C4 C17 C18 9.6(15) . . . . ? C3 C4 C17 C18 -177.9(12) . . . . ? C5 C4 C17 C19 128.5(10) . . . . ? C3 C4 C17 C19 -59.0(11) . . . . ? C5 C4 C17 C20 -111.7(12) . . . . ? C3 C4 C17 C20 60.8(13) . . . . ? C5 C4 C17' C18' -9.4(15) . . . . ? C3 C4 C17' C18' 177.8(12) . . . . ? C5 C4 C17' C20' -128.7(11) . . . . ? C3 C4 C17' C20' 58.5(13) . . . . ? C5 C4 C17' C19' 110.7(13) . . . . ? C3 C4 C17' C19' -62.1(13) . . . . ? C5 C6 N1 C7 0.0(5) . . . . ? C1 C6 N1 C7 179.7(3) . . . . ? C5 C6 N1 Pd1 -179.8(2) . . . . ? C1 C6 N1 Pd1 -0.1(3) . . . . ? C22 C7 N1 C6 -62.5(4) . . . . ? C8 C7 N1 C6 179.9(3) . . . . ? C21 C7 N1 C6 62.7(4) . . . . ? C22 C7 N1 Pd1 117.4(2) . . . . ? C8 C7 N1 Pd1 -0.3(3) . . . . ? C21 C7 N1 Pd1 -117.5(2) . . . . ? C11 C12 N2 C8 -0.3(5) . . . . ? C11 C12 N2 Pd1 179.9(2) . . . . ? C9 C8 N2 C12 0.2(4) . . . . ? C7 C8 N2 C12 179.9(3) . . . . ? C9 C8 N2 Pd1 180.0(2) . . . . ? C7 C8 N2 Pd1 -0.2(4) . . . . ? C2 C1 O1 Pd1 -179.9(2) . . . . ? C6 C1 O1 Pd1 -0.3(3) . . . . ? _refine_diff_density_max 0.491 _refine_diff_density_min -0.396 _refine_diff_density_rms 0.084 _shelx_res_file ; refin.res created by SHELXL-2014/7 TITL KvL016_0m_a.res in P-1 CELL 0.71073 7.3768 12.0798 15.1667 93.531 89.979 107.760 ZERR 2.000 0.0004 0.0007 0.0009 0.003 0.004 0.003 LATT 1 SFAC C H B N O F Cl Pd UNIT 44 60 2 4 2 8 2 2 TEMP -123.150 ACTA HTAB BOND BOND $H CONF WPDB L.S. 10 FMAP 2 PLAN 10 OMIT -2 50.4 ABIN WGHT 0.026300 0.903100 FVAR 0.34405 0.52709 0.34539 0.13350 0.24434 0.27678 PART 0 PD1 8 0.798830 0.597700 0.436888 11.00000 0.01845 0.01893 = 0.01271 0.00375 0.00142 0.00609 CL1 7 0.832363 0.664867 0.581543 11.00000 0.03804 0.02717 = 0.01560 0.00122 0.00044 0.00881 C1 1 0.875337 0.751253 0.304957 11.00000 0.00862 0.02226 = 0.01936 0.00338 -0.00116 0.00715 C2 1 0.926905 0.853757 0.254933 11.00000 0.01808 0.01654 = 0.02437 0.00661 0.00326 0.00691 C3 1 0.917224 0.834367 0.166687 11.00000 0.03860 0.02154 = 0.02249 0.00562 -0.00037 0.00808 AFIX 43 H3 2 0.950907 0.900804 0.132597 11.00000 -1.20000 AFIX 0 C4 1 0.859782 0.720748 0.118525 11.00000 0.02637 0.02991 = 0.01662 0.00350 0.00326 0.00851 C5 1 0.811350 0.623506 0.163040 11.00000 0.01650 0.02009 = 0.01852 0.00004 0.00059 0.00597 AFIX 43 H5 2 0.773982 0.549135 0.131930 11.00000 -1.20000 AFIX 0 C6 1 0.816378 0.632606 0.257778 11.00000 0.00904 0.02198 = 0.01758 0.00151 0.00223 0.00598 C7 1 0.709898 0.420723 0.288635 11.00000 0.02275 0.01515 = 0.01991 0.00081 -0.00136 0.00303 C8 1 0.680968 0.361974 0.376396 11.00000 0.01491 0.02283 = 0.02127 0.00360 -0.00065 0.00761 C9 1 0.620757 0.241653 0.378332 11.00000 0.03124 0.02110 = 0.02791 0.00299 0.00145 0.00721 AFIX 43 H9 2 0.596999 0.194206 0.324691 11.00000 -1.20000 AFIX 0 C10 1 0.595498 0.191138 0.458077 11.00000 0.02993 0.02056 = 0.03299 0.00641 0.00235 0.00650 AFIX 43 H10 2 0.554468 0.108708 0.459562 11.00000 -1.20000 AFIX 0 C11 1 0.629540 0.259759 0.535464 11.00000 0.02647 0.02814 = 0.02905 0.01129 0.00303 0.00807 AFIX 43 H11 2 0.612102 0.225836 0.590935 11.00000 -1.20000 AFIX 0 C12 1 0.689317 0.378439 0.530973 11.00000 0.02260 0.03050 = 0.01779 0.00525 0.00085 0.00850 AFIX 43 H12 2 0.713809 0.426436 0.584347 11.00000 -1.20000 AFIX 0 C13 1 0.988077 0.975153 0.303447 11.00000 0.03630 0.02088 = 0.01966 0.00403 0.00067 0.00693 C14 1 1.165423 0.991181 0.361212 11.00000 0.03554 0.02975 = 0.03681 -0.00408 -0.00196 -0.00055 AFIX 137 H14A 2 1.269700 0.982767 0.324029 11.00000 -1.50000 H14B 2 1.137351 0.932089 0.404944 11.00000 -1.50000 H14C 2 1.202787 1.068952 0.391653 11.00000 -1.50000 AFIX 0 C15 1 0.825146 0.991243 0.361398 11.00000 0.04732 0.02627 = 0.03584 -0.00041 0.00236 0.01668 AFIX 137 H15A 2 0.795280 0.932936 0.405736 11.00000 -1.50000 H15B 2 0.712080 0.981563 0.324198 11.00000 -1.50000 H15C 2 0.864483 1.069462 0.391109 11.00000 -1.50000 AFIX 0 C16 1 1.036305 1.070745 0.237499 11.00000 0.08511 0.02014 = 0.03636 0.00865 0.00299 0.00650 AFIX 137 H16A 2 1.077100 1.147313 0.269790 11.00000 -1.50000 H16B 2 0.923401 1.064073 0.201005 11.00000 -1.50000 H16C 2 1.139233 1.061937 0.199557 11.00000 -1.50000 AFIX 0 rem restraints SADI 0.01 C4 C17 C4 C17' SIMU 0.01 C17 > C20' PART 1 C17 1 0.881172 0.718166 0.017675 21.00000 0.05673 0.03657 = 0.01487 0.00517 -0.00030 0.01133 C18 1 0.811118 0.596256 -0.027121 21.00000 0.05534 0.04390 = 0.01818 0.00123 0.00199 0.01202 AFIX 137 H18A 2 0.889674 0.549853 -0.007205 21.00000 -1.50000 H18B 2 0.820286 0.600960 -0.091323 21.00000 -1.50000 H18C 2 0.678226 0.559350 -0.011716 21.00000 -1.50000 AFIX 0 C19 1 0.759310 0.789980 -0.017746 21.00000 0.06890 0.04273 = 0.03210 0.01158 0.00253 0.01141 AFIX 137 H19A 2 0.773354 0.793515 -0.081858 21.00000 -1.50000 H19B 2 0.801908 0.869063 0.010407 21.00000 -1.50000 H19C 2 0.625302 0.752954 -0.004275 21.00000 -1.50000 AFIX 0 C20 1 1.092503 0.772516 -0.005877 21.00000 0.05375 0.06499 = 0.02168 0.01157 0.01930 -0.00378 AFIX 137 H20A 2 1.167483 0.724883 0.015591 21.00000 -1.50000 H20B 2 1.140327 0.851591 0.021997 21.00000 -1.50000 H20C 2 1.103579 0.775504 -0.070140 21.00000 -1.50000 AFIX 0 rem constraints EADP C18 C18' rem restraints ISOR 0.01 C20 PART 2 SAME C17 > C20 C17' 1 0.835298 0.718457 0.017874 -21.00000 0.04867 0.03521 = 0.01659 0.00060 0.00521 0.00952 C18' 1 0.782794 0.594347 -0.022751 -21.00000 0.05534 0.04390 = 0.01818 0.00123 0.00199 0.01202 AFIX 137 H18D 2 0.876506 0.557519 -0.003960 -21.00000 -1.50000 H18E 2 0.781819 0.595339 -0.087309 -21.00000 -1.50000 H18F 2 0.656198 0.550149 -0.003181 -21.00000 -1.50000 AFIX 0 C19' 1 0.677243 0.770362 -0.005990 -21.00000 0.06762 0.05464 = 0.01997 0.00575 -0.00987 0.03235 AFIX 137 H19D 2 0.666756 0.770778 -0.070372 -21.00000 -1.50000 H19E 2 0.708159 0.850293 0.020184 -21.00000 -1.50000 H19F 2 0.555941 0.723142 0.016989 -21.00000 -1.50000 AFIX 0 C20' 1 1.027272 0.790183 -0.017544 -21.00000 0.06329 0.04401 = 0.02303 0.00818 0.00340 0.01229 AFIX 137 H20D 2 1.127586 0.759118 0.002088 -21.00000 -1.50000 H20E 2 1.055774 0.871613 0.004913 -21.00000 -1.50000 H20F 2 1.021103 0.785643 -0.082262 -21.00000 -1.50000 AFIX 0 PART 0 C21 1 0.866842 0.386753 0.237915 11.00000 0.04027 0.03132 = 0.02612 0.00439 0.00981 0.01954 AFIX 137 H21A 2 0.886204 0.423641 0.181452 11.00000 -1.50000 H21B 2 0.829084 0.301923 0.226894 11.00000 -1.50000 H21C 2 0.985552 0.412983 0.272980 11.00000 -1.50000 AFIX 0 C22 1 0.519880 0.386314 0.238198 11.00000 0.02855 0.02963 = 0.02755 0.00595 -0.00689 -0.00179 AFIX 137 H22A 2 0.427902 0.413902 0.272630 11.00000 -1.50000 H22B 2 0.472034 0.301336 0.228482 11.00000 -1.50000 H22C 2 0.537681 0.421607 0.181092 11.00000 -1.50000 AFIX 0 N1 4 0.774432 0.548785 0.311733 11.00000 0.01356 0.01738 = 0.01825 0.00257 0.00141 0.00634 N2 4 0.714486 0.429277 0.453286 11.00000 0.01624 0.02163 = 0.01784 0.00653 0.00081 0.00632 O1 5 0.878955 0.757560 0.387815 11.00000 0.02360 0.02238 = 0.01481 0.00227 0.00120 0.00461 rem restraints SIMU 0.01 B1 > F4D SUMP 1 0 1 3 1 4 1 5 1 6 PART 1 B1 3 0.349937 0.703286 0.223448 31.00000 0.03606 0.07019 = 0.03797 -0.00613 -0.00608 0.02375 F1 6 0.303990 0.619740 0.158196 31.00000 0.08129 0.07176 = 0.04749 -0.03164 0.00230 0.01133 F2 6 0.506187 0.704256 0.273839 31.00000 0.02512 0.06323 = 0.04479 -0.01732 -0.00357 0.02524 F3 6 0.201331 0.705694 0.278067 31.00000 0.01581 0.07718 = 0.03385 -0.00660 -0.00628 0.02684 F4 6 0.393116 0.812096 0.182702 31.00000 0.09187 0.07807 = 0.05105 0.00689 -0.01981 0.00837 PART 2 SAME B1 > F4 B1' 3 0.346454 0.689416 0.220531 41.00000 0.04056 0.07163 = 0.04150 -0.00764 -0.00668 0.02167 F1' 6 0.381959 0.693946 0.133982 41.00000 0.05900 0.08245 = 0.03963 -0.01458 -0.00531 0.00871 F2' 6 0.508165 0.709076 0.272805 41.00000 0.03536 0.06894 = 0.04706 -0.00898 -0.00795 0.02299 F3' 6 0.254328 0.767659 0.250244 41.00000 0.03994 0.06984 = 0.05221 -0.01273 -0.00859 0.03275 F4' 6 0.224271 0.574297 0.237033 41.00000 0.03956 0.07531 = 0.05291 -0.00879 -0.00769 0.01280 PART 3 SAME B1 > F4 B1C 3 0.342276 0.676489 0.218069 51.00000 0.03848 0.07156 = 0.04033 -0.00758 -0.00651 0.02228 F1C 6 0.354497 0.654455 0.131182 51.00000 0.06586 0.06851 = 0.03594 -0.02172 0.00467 0.00215 F2C 6 0.515746 0.747755 0.250621 51.00000 0.02365 0.07803 = 0.05345 -0.00378 -0.01081 0.01923 F3C 6 0.201948 0.719715 0.250489 51.00000 0.03035 0.07310 = 0.04578 -0.00189 -0.00501 0.02365 F4C 6 0.306200 0.562216 0.250916 51.00000 0.06474 0.06271 = 0.05312 -0.00356 -0.02219 0.03036 PART 4 SAME B1 > F4 B1D 3 0.349193 0.702357 0.217437 61.00000 0.03785 0.07049 = 0.03929 -0.00647 -0.00567 0.02272 F1D 6 0.301860 0.666325 0.132827 61.00000 0.06117 0.07871 = 0.03624 -0.01133 -0.00409 0.01372 F2D 6 0.478851 0.664774 0.262697 61.00000 0.03806 0.07600 = 0.05718 -0.01085 -0.00553 0.04282 F3D 6 0.188525 0.668825 0.267356 61.00000 0.02442 0.07050 = 0.04449 0.00238 0.00108 0.01051 F4D 6 0.430762 0.826899 0.219321 61.00000 0.07081 0.07281 = 0.05329 0.00032 -0.02641 0.00152 HKLF 4 REM KvL016_0m_a.res in P-1 REM R1 = 0.0339 for 3779 Fo > 4sig(Fo) and 0.0518 for all 4607 data REM 470 parameters refined using 866 restraints END WGHT 0.0263 0.9032 REM Instructions for potential hydrogen bonds EQIV $1 -x+1, -y+1, -z+1 HTAB C11 F2_$1 HTAB C11 F3_$1 HTAB C11 F3'_$1 HTAB C11 F2C_$1 HTAB C11 F3D_$1 HTAB C12 Cl1 HTAB C12 F4C_$1 EQIV $2 -x+2, -y+1, -z+1 HTAB C21 Cl1_$2 EQIV $3 x+1, y, z HTAB C21 F4'_$3 HTAB C21 F4C_$3 HTAB C22 Cl1_$1 HTAB C22 F4C REM Highest difference peak 0.491, deepest hole -0.396, 1-sigma level 0.084 Q1 1 0.4103 0.5882 0.2238 11.00000 0.05 0.49 Q2 1 0.4649 0.9009 0.1454 11.00000 0.05 0.47 Q3 1 0.7279 0.5014 0.4463 11.00000 0.05 0.46 Q4 1 0.8430 0.6685 0.4169 11.00000 0.05 0.45 Q5 1 0.5061 0.8023 0.1933 11.00000 0.05 0.43 Q6 1 0.3000 0.7639 0.1566 11.00000 0.05 0.36 Q7 1 0.9496 0.7779 0.1401 11.00000 0.05 0.35 Q8 1 0.8196 0.5986 0.5400 11.00000 0.05 0.34 Q9 1 0.6741 0.5788 0.5013 11.00000 0.05 0.33 Q10 1 0.7323 0.3945 0.4182 11.00000 0.05 0.32 ; _shelx_res_checksum 44796 _shelx_hkl_file ; -1 0 0 393.86 16.70 1 0 0 418.46 16.30 -2 0 0 1470.75 52.19 -2 0 0 1439.16 52.89 -2 0 0 1468.55 52.19 2 0 0 1523.65 52.69 2 0 0 1477.45 53.19 2 0 0 1473.15 52.19 2 0 0 1456.35 52.29 2 0 0 1417.06 52.29 -3 0 0 1306.67 49.40 -3 0 0 1320.97 50.89 -3 0 0 1357.36 49.60 3 0 0 1321.77 49.80 3 0 0 1396.06 50.29 3 0 0 1306.07 49.80 3 0 0 1358.16 51.19 -4 0 0 6.20 4.90 -4 0 0 -4.60 6.70 -4 0 0 2.00 6.60 -4 0 0 4.00 6.60 4 0 0 -1.90 7.60 4 0 0 9.50 6.70 4 0 0 -11.50 6.10 4 0 0 -3.30 6.40 -5 0 0 205.18 16.60 -5 0 0 211.88 16.90 -5 0 0 224.18 12.60 -5 0 0 236.58 18.60 5 0 0 230.58 19.20 5 0 0 205.78 16.50 5 0 0 233.88 15.80 5 0 0 212.48 16.80 -6 0 0 171.98 11.80 -6 0 0 176.18 26.10 -6 0 0 168.58 16.30 6 0 0 146.29 17.80 6 0 0 110.89 15.60 6 0 0 127.29 19.00 6 0 0 174.38 18.70 -7 0 0 85.89 16.10 -7 0 0 61.29 15.70 -7 0 0 77.39 18.60 -7 0 0 84.69 10.00 7 0 0 56.89 17.90 7 0 0 54.19 14.50 7 0 0 85.19 16.50 -8 0 0 87.39 20.10 -8 0 0 73.39 19.00 8 0 0 53.39 18.10 8 0 0 63.29 18.20 8 0 0 67.39 18.70 -9 0 0 15.80 22.50 9 0 0 -8.60 22.70 9 0 0 25.80 23.00 9 0 0 -5.40 20.80 -10 0 0 49.10 33.10 10 0 0 40.30 31.30 10 -1 0 24.20 28.10 10 -1 0 26.10 26.70 -10 1 0 5.00 26.00 9 -1 0 36.00 20.50 9 -1 0 -17.60 19.30 9 -1 0 15.20 23.40 -9 1 0 12.00 26.60 -9 1 0 15.60 19.50 8 -1 0 12.70 18.40 8 -1 0 26.20 18.10 8 -1 0 -1.70 16.10 -8 1 0 32.00 15.60 -8 1 0 8.70 17.70 7 -1 0 129.29 19.90 7 -1 0 135.39 19.90 7 -1 0 117.69 17.80 7 -1 0 132.79 18.90 -7 1 0 162.58 21.20 -7 1 0 145.89 19.00 -7 1 0 145.49 20.30 -7 1 0 93.09 13.50 6 -1 0 -4.40 9.20 6 -1 0 18.00 11.40 6 -1 0 -4.70 9.40 6 -1 0 11.20 11.30 -6 1 0 13.00 7.30 -6 1 0 -3.70 10.10 -6 1 0 -13.00 10.10 -6 1 0 5.30 10.40 5 -1 0 162.18 14.90 5 -1 0 194.38 15.70 5 -1 0 149.19 14.20 5 -1 0 171.38 15.10 -5 1 0 194.38 12.50 -5 1 0 190.38 15.30 -5 1 0 177.88 14.80 -5 1 0 189.48 16.20 4 -1 0 650.33 28.10 4 -1 0 609.54 27.80 4 -1 0 596.04 29.00 4 -1 0 598.24 27.30 -4 1 0 605.64 28.20 -4 1 0 623.14 26.70 -4 1 0 656.63 25.30 -4 1 0 576.54 28.10 3 -1 0 136.69 11.30 3 -1 0 131.79 10.40 3 -1 0 147.59 10.30 3 -1 0 120.09 10.00 -3 1 0 137.59 9.00 -3 1 0 133.99 9.10 -3 1 0 134.59 10.00 -3 1 0 127.29 10.40 2 -1 0 9632.94 314.17 2 -1 0 9250.27 313.77 2 -1 0 9174.68 313.67 2 -1 0 8920.41 313.67 2 -1 0 9537.05 314.67 2 -1 0 9999.00 314.27 -2 1 0 8918.81 313.77 -2 1 0 9117.49 313.77 -2 1 0 9223.38 313.07 -1 1 0 419.56 16.80 -1 -1 0 207.88 10.00 -1 -1 0 201.18 9.40 -1 -1 0 217.08 9.70 -1 -1 0 215.68 9.80 1 1 0 210.18 9.40 1 1 0 229.58 10.30 1 1 0 209.28 11.20 1 1 0 215.18 9.20 1 1 0 199.28 9.80 -2 -1 0 35.60 5.50 -2 -1 0 29.10 6.00 -2 -1 0 36.10 6.00 2 1 0 33.30 5.50 2 1 0 42.20 6.40 2 1 0 32.40 6.60 2 1 0 38.00 5.20 2 1 0 33.80 5.00 -3 -1 0 562.24 24.40 -3 -1 0 578.84 26.40 -3 -1 0 565.94 24.40 3 1 0 539.15 24.70 3 1 0 568.34 24.90 3 1 0 572.74 25.50 3 1 0 584.04 24.80 -4 -1 0 73.89 10.60 -4 -1 0 83.79 11.70 -4 -1 0 75.49 9.80 4 1 0 78.89 10.60 4 1 0 78.99 10.90 4 1 0 56.19 9.30 4 1 0 88.19 11.80 -5 -1 0 64.29 10.00 -5 -1 0 66.19 9.00 -5 -1 0 73.79 12.90 -5 -1 0 59.39 11.90 5 1 0 55.79 10.30 5 1 0 70.69 12.40 5 1 0 69.59 12.30 5 1 0 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