#------------------------------------------------------------------------------ #$Date: 2019-05-22 07:27:21 +0300 (Wed, 22 May 2019) $ #$Revision: 215393 $ #$URL: file:///home/coder/svn-repositories/cod/cif/2/02/16/2021643.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/. The original data for this entry # were provided by IUCr Journals, http://journals.iucr.org/. # # The file may be used within the scientific community so long as # proper attribution is given to the journal article from which the # data were obtained. # data_2021643 loop_ _publ_author_name 'Subramaniyan, Vasudevan' 'Kumar, Ashok' 'Govindaraj, Anbarasu' 'Mani, Ganesan' _publ_section_title ; Crystal structure and DFT analyses of a pentacoordinated PCP pincer nickel(II) complex ; _journal_coeditor_code KY3175 _journal_issue 6 _journal_name_full 'Acta Crystallographica Section C' _journal_page_first ; ; _journal_paper_doi 10.1107/S2053229619006211 _journal_volume 75 _journal_year 2019 _chemical_formula_iupac '[Ni (C9 H9 N1) (C30 H30 Cl N2 P2)] P F6, 0.7H2 O' _chemical_formula_moiety 'C39 H39 Cl N3 Ni P2 +, F6 P -, 0.7(H2 O)' _chemical_formula_sum 'C39 H40.41 Cl F6 N3 Ni O0.7 P3' _chemical_formula_weight 863.42 _chemical_name_systematic ;{1,3-Bis[(diphenylphosphanyl)methyl]hexahydropyrimidin-2-yl-\kN^2^}(2,6-dimethylphenyl isocyanide-\kC)nickel(II) hexafluoridophosphate 0.70-hydrate ; _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_Hall '-P 1' _space_group_name_H-M_alt 'P -1' _symmetry_space_group_name_Hall '-P 1' _symmetry_space_group_name_H-M 'P -1' _atom_sites_solution_hydrogens mixed _atom_sites_solution_primary dual _audit_creation_method ; Olex2 1.2 (compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506) ; _cell_angle_alpha 99.6870(10) _cell_angle_beta 91.5040(10) _cell_angle_gamma 93.4720(10) _cell_formula_units_Z 2 _cell_length_a 9.7632(5) _cell_length_b 10.8846(5) _cell_length_c 18.5771(9) _cell_measurement_reflns_used 24485 _cell_measurement_temperature 100(2) _cell_measurement_theta_max 25.997 _cell_measurement_theta_min 1.902 _cell_volume 1941.11(16) _computing_cell_refinement ; SAINT (Bruker, 2000) ; _computing_data_collection ; SMART (Bruker, 2000) ; _computing_data_reduction ; SAINT (Bruker, 2000) ; _computing_molecular_graphics ; OLEX2 (Dolomanov et al., 2009) ; _computing_publication_material ; OLEX2 (Dolomanov et al., 2009) ; _computing_structure_refinement ; SHELXL2017 (Sheldrick, 2015b) ; _computing_structure_solution ; SHELXT (Sheldrick, 2015a) ; _diffrn_ambient_temperature 100(2) _diffrn_measured_fraction_theta_full 0.987 _diffrn_measured_fraction_theta_max 0.977 _diffrn_measurement_device_type 'Bruker APEXII CCD area detector' _diffrn_measurement_method hemisphere _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0273 _diffrn_reflns_av_unetI/netI 0.0290 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_number 24485 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 25.997 _diffrn_reflns_theta_min 1.902 _diffrn_source 'Fine focused sealed tube' _exptl_absorpt_coefficient_mu 0.757 _exptl_absorpt_correction_T_max 0.827 _exptl_absorpt_correction_T_min 0.761 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; (SADABS; Krause et al., 2015) ; _exptl_crystal_colour brown _exptl_crystal_density_diffrn 1.477 _exptl_crystal_description prism _exptl_crystal_F_000 890 _exptl_crystal_size_max 0.38 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.25 _refine_diff_density_max 0.456 _refine_diff_density_min -0.302 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.068 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 548 _refine_ls_number_reflns 7473 _refine_ls_number_restraints 6 _refine_ls_restrained_S_all 1.067 _refine_ls_R_factor_all 0.0352 _refine_ls_R_factor_gt 0.0299 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0324P)^2^+1.1895P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0714 _refine_ls_wR_factor_ref 0.0753 _reflns_number_gt 6603 _reflns_number_total 7473 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file ky3175sup1.cif _cod_data_source_block I _cod_original_formula_sum 'C39 H40.41 Cl F6 N3 Ni O0.70 P3' _cod_database_code 2021643 _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. ; _shelx_estimated_absorpt_t_min 0.679 _shelx_estimated_absorpt_t_max 0.746 _shelx_hkl_file ; -1 0 0 949.68 21.44 1 0 0 910.57 22.03 1 0 0 897.88 21.43 -2 0 0 1.86 0.40 2 0 0 0.80 0.53 2 0 0 1.73 0.42 2 0 0 -0.11 0.34 2 0 0 1.78 0.68 -3 0 0 355.26 9.02 3 0 0 348.32 10.49 3 0 0 348.59 10.71 -4 0 0 230.99 6.53 4 0 0 239.44 8.44 4 0 0 236.02 8.66 -5 0 0 1442.08 34.18 5 0 0 1428.07 37.65 5 0 0 1414.13 37.18 -6 0 0 443.95 11.59 6 0 0 438.00 14.89 6 0 0 435.98 15.30 7 0 0 0.78 1.62 7 0 0 0.49 1.51 7 0 0 3.81 1.94 8 0 0 294.65 12.89 8 0 0 312.94 13.64 9 0 0 55.50 6.74 9 0 0 59.14 6.61 10 0 0 3.32 3.00 10 0 0 3.36 2.93 10 0 0 1.41 2.91 11 0 0 231.74 14.01 11 0 0 241.67 13.44 12 0 0 155.95 11.52 13 0 0 72.69 9.90 14 0 0 20.18 8.11 14 -1 0 161.71 14.95 13 -1 0 3.66 4.13 12 -1 0 -0.92 4.26 12 -1 0 6.16 3.82 11 -1 0 1.33 3.51 11 -1 0 2.17 3.05 10 -1 0 126.62 8.98 10 -1 0 128.95 9.64 9 -1 0 22.94 4.74 9 -1 0 15.69 3.74 9 -1 0 16.34 4.07 8 -1 0 37.40 4.98 8 -1 0 28.00 4.46 8 -1 0 35.97 5.33 7 -1 0 39.32 4.87 7 -1 0 39.65 5.01 7 -1 0 42.00 4.83 6 -1 0 2444.75 62.61 6 -1 0 2534.82 62.36 -6 1 0 2488.76 59.17 -6 1 0 2441.22 59.25 5 -1 0 311.99 11.18 5 -1 0 306.55 10.83 -5 1 0 313.95 9.13 -5 1 0 304.07 9.17 4 -1 0 147.08 6.10 4 -1 0 124.18 6.09 4 -1 0 153.97 6.43 -4 1 0 154.07 5.12 -4 1 0 147.17 5.13 3 -1 0 329.44 10.03 3 -1 0 328.60 10.21 -3 1 0 332.93 9.31 -3 1 0 344.61 9.39 2 -1 0 25.21 1.85 2 -1 0 23.80 1.67 -2 1 0 27.19 1.62 1 -1 0 664.34 16.54 -1 1 0 674.29 16.52 0 -1 0 796.33 18.62 0 1 0 832.48 18.61 0 1 0 674.43 18.37 -1 -1 0 1795.62 41.76 1 1 0 1804.96 41.75 1 1 0 1791.86 42.59 1 1 0 1787.52 42.62 -2 -1 0 589.46 14.37 2 1 0 611.52 16.01 2 1 0 618.22 16.21 2 1 0 627.39 14.42 2 1 0 591.43 16.01 -3 -1 0 107.53 2.97 -3 -1 0 107.22 2.91 3 1 0 115.58 4.82 3 1 0 117.45 5.07 3 1 0 106.25 4.82 -4 -1 0 4.91 0.52 -4 -1 0 5.12 0.48 4 1 0 4.70 1.51 4 1 0 4.39 1.54 4 1 0 4.29 1.35 5 1 0 674.26 20.38 5 1 0 673.46 20.17 5 1 0 677.37 20.01 6 1 0 482.29 16.10 6 1 0 473.03 16.47 6 1 0 484.51 16.40 7 1 0 37.21 4.90 7 1 0 28.03 4.33 7 1 0 43.67 4.91 8 1 0 60.12 6.73 8 1 0 62.85 6.42 8 1 0 64.10 6.87 9 1 0 649.46 23.02 9 1 0 614.65 22.54 9 1 0 658.96 23.56 10 1 0 84.94 8.93 10 1 0 122.11 9.02 10 1 0 149.41 10.43 11 1 0 1.10 3.28 11 1 0 -0.01 2.82 12 1 0 58.43 8.28 13 1 0 21.24 6.22 14 -2 0 15.37 6.54 13 -2 0 10.96 4.78 12 -2 0 0.05 3.98 12 -2 0 0.82 3.24 11 -2 0 223.64 12.93 11 -2 0 214.98 13.32 10 -2 0 4.88 3.25 10 -2 0 4.52 2.93 9 -2 0 192.53 10.83 9 -2 0 198.09 11.10 9 -2 0 185.38 10.21 8 -2 0 4.14 2.49 8 -2 0 -1.44 1.53 8 -2 0 1.06 2.49 7 -2 0 286.15 11.67 7 -2 0 269.28 11.83 7 -2 0 285.75 12.02 -7 2 0 278.07 9.60 6 -2 0 119.44 6.81 6 -2 0 140.10 6.93 6 -2 0 132.72 7.33 -6 2 0 124.13 5.53 -6 2 0 131.20 5.55 5 -2 0 2271.79 57.62 5 -2 0 2244.36 57.12 5 -2 0 2245.42 56.76 -5 2 0 2320.62 55.38 -5 2 0 2318.30 55.53 4 -2 0 67.84 4.40 4 -2 0 68.48 3.90 4 -2 0 60.86 3.89 -4 2 0 58.32 3.35 -4 2 0 68.97 3.51 3 -2 0 6370.89 147.36 3 -2 0 5711.59 147.88 3 -2 0 6330.12 147.65 -3 2 0 6595.22 147.04 -3 2 0 6486.52 147.12 2 -2 0 172.28 6.08 2 -2 0 175.33 5.94 -2 2 0 178.73 5.96 -2 2 0 173.02 5.99 1 -2 0 1241.88 31.03 1 -2 0 1273.52 31.18 -1 2 0 1299.32 31.09 -1 2 0 1263.90 31.02 -1 2 0 1273.83 31.14 0 -2 0 159.02 5.35 0 2 0 157.97 5.12 0 2 0 161.66 5.34 0 2 0 154.07 5.11 1 2 0 1975.55 48.05 1 2 0 1984.94 47.99 1 2 0 2009.57 47.21 1 2 0 2010.46 47.82 2 2 0 1034.10 26.79 2 2 0 1052.43 25.09 2 2 0 1025.12 26.75 2 2 0 1056.56 26.58 3 2 0 55.04 2.08 3 2 0 54.32 3.60 3 2 0 52.04 3.58 3 2 0 52.74 3.38 4 2 0 20.29 2.89 4 2 0 19.58 2.57 4 2 0 17.85 1.02 4 2 0 18.78 2.77 5 2 0 1227.88 33.85 5 2 0 1240.75 34.10 5 2 0 1267.15 33.86 6 2 0 1018.14 29.87 6 2 0 1037.94 30.14 6 2 0 1042.41 29.67 7 2 0 28.11 4.31 7 2 0 20.52 3.48 7 2 0 21.64 3.95 8 2 0 177.25 9.75 8 2 0 188.43 10.51 8 2 0 174.36 10.27 9 2 0 171.46 10.67 9 2 0 189.58 11.30 9 2 0 176.15 10.25 10 2 0 23.52 5.50 10 2 0 25.63 6.12 10 2 0 21.53 4.82 11 2 0 39.63 6.87 11 2 0 34.05 6.91 12 2 0 9.76 4.71 13 2 0 0.62 3.81 14 -3 0 34.32 7.95 13 -3 0 -0.72 4.03 12 -3 0 67.15 9.38 12 -3 0 68.55 8.93 11 -3 0 119.87 9.48 11 -3 0 121.80 10.23 10 -3 0 369.91 16.21 10 -3 0 374.36 16.81 9 -3 0 67.15 6.84 9 -3 0 66.94 7.56 9 -3 0 61.94 6.99 8 -3 0 320.02 14.06 8 -3 0 336.15 13.65 8 -3 0 315.83 13.84 7 -3 0 63.67 6.19 7 -3 0 64.81 5.09 7 -3 0 61.06 6.31 -7 3 0 61.73 4.23 -7 3 0 52.43 4.11 6 -3 0 843.57 25.57 6 -3 0 840.74 24.92 6 -3 0 874.70 24.77 -6 3 0 821.81 23.11 -6 3 0 824.33 23.32 5 -3 0 343.79 12.58 5 -3 0 367.38 13.29 5 -3 0 366.01 12.41 -5 3 0 350.13 11.61 -5 3 0 376.89 11.99 4 -3 0 128.07 6.77 4 -3 0 137.60 6.41 4 -3 0 148.06 6.32 -4 3 0 137.79 5.96 -4 3 0 138.58 6.07 3 -3 0 209.43 7.74 3 -3 0 222.13 8.06 -3 3 0 221.22 7.77 -3 3 0 216.38 7.86 2 -3 0 155.17 5.91 2 -3 0 146.81 5.63 -2 3 0 137.08 5.72 -2 3 0 141.46 5.68 1 -3 0 105.39 4.53 1 -3 0 104.62 4.36 -1 3 0 99.04 4.43 -1 3 0 103.87 4.62 -1 3 0 106.33 4.63 0 -3 0 337.96 10.38 0 -3 0 345.41 10.23 0 3 0 345.93 10.42 0 3 0 319.13 9.97 0 3 0 329.63 9.93 1 3 0 12.63 1.74 1 3 0 16.53 2.18 1 3 0 9.13 1.39 1 3 0 13.22 1.56 1 3 0 16.31 2.06 2 3 0 671.75 18.35 2 3 0 642.12 18.53 2 3 0 646.09 17.06 2 3 0 644.36 18.56 2 3 0 683.75 17.02 3 3 0 535.07 16.10 3 3 0 556.65 13.99 3 3 0 531.10 16.36 3 3 0 524.85 13.98 3 3 0 543.86 16.52 4 3 0 154.03 7.49 4 3 0 161.28 7.60 4 3 0 161.65 7.37 4 3 0 163.64 5.08 5 3 0 995.82 24.56 5 3 0 1037.02 29.03 5 3 0 997.44 29.29 5 3 0 1054.18 29.51 6 3 0 345.99 13.96 6 3 0 351.84 13.55 6 3 0 353.55 13.95 7 3 0 18.17 3.55 7 3 0 16.98 3.88 7 3 0 23.11 4.34 8 3 0 276.87 13.36 8 3 0 244.95 12.81 8 3 0 248.07 12.24 9 3 0 3.88 3.98 9 3 0 5.98 3.16 9 3 0 9.83 3.44 10 3 0 148.35 10.56 10 3 0 162.87 11.94 10 3 0 169.75 11.84 11 3 0 57.63 8.32 11 3 0 86.24 9.55 12 3 0 128.93 12.61 13 3 0 2.09 4.17 13 -4 0 141.88 13.40 12 -4 0 212.15 16.22 12 -4 0 238.02 13.84 11 -4 0 81.89 9.28 11 -4 0 79.79 8.54 10 -4 0 249.52 12.91 10 -4 0 260.20 13.74 9 -4 0 109.10 7.72 9 -4 0 92.96 7.63 8 -4 0 145.51 8.47 8 -4 0 154.43 9.78 8 -4 0 140.36 8.74 7 -4 0 10.01 2.58 7 -4 0 8.28 2.72 7 -4 0 10.53 3.41 -7 4 0 10.22 2.56 -7 4 0 8.20 2.25 6 -4 0 17.35 2.93 6 -4 0 16.27 3.11 6 -4 0 22.65 4.08 -6 4 0 19.99 2.89 -6 4 0 18.69 2.90 5 -4 0 1133.29 32.56 5 -4 0 1122.73 30.96 5 -4 0 1155.61 31.62 -5 4 0 1114.11 30.54 -5 4 0 1164.01 30.94 4 -4 0 1740.93 43.64 4 -4 0 1715.71 44.00 -4 4 0 1643.22 43.59 -4 4 0 1730.42 43.60 3 -4 0 824.64 22.62 3 -4 0 797.70 22.20 -3 4 0 770.89 22.46 -3 4 0 834.42 22.57 2 -4 0 398.29 12.41 2 -4 0 394.60 12.64 -2 4 0 403.82 12.85 -2 4 0 411.67 12.75 -2 4 0 400.34 12.62 1 -4 0 523.15 15.34 1 -4 0 517.17 15.02 -1 4 0 524.92 15.30 -1 4 0 497.59 15.00 -1 4 0 508.97 15.22 0 -4 0 43.83 3.22 0 -4 0 49.35 3.24 0 4 0 39.07 3.14 0 4 0 38.79 2.89 0 4 0 41.90 3.08 -1 -4 0 37.89 3.79 1 4 0 37.84 2.93 1 4 0 35.78 3.04 2 4 0 1556.94 40.53 2 4 0 1545.24 40.17 2 4 0 1594.47 38.98 2 4 0 1549.56 40.59 2 4 0 1607.54 38.80 3 4 0 464.23 15.12 3 4 0 486.30 13.25 3 4 0 474.16 15.57 3 4 0 474.71 13.31 3 4 0 466.31 15.48 4 4 0 851.59 25.61 4 4 0 877.52 25.65 4 4 0 875.60 22.08 4 4 0 880.24 22.22 4 4 0 860.33 25.21 5 4 0 31.27 4.06 5 4 0 24.36 3.88 5 4 0 34.81 4.67 6 4 0 30.27 4.27 6 4 0 27.50 4.43 6 4 0 21.86 4.06 7 4 0 33.61 5.13 7 4 0 35.71 5.49 7 4 0 32.54 4.88 8 4 0 519.78 19.77 8 4 0 510.65 20.18 8 4 0 491.29 19.88 9 4 0 122.42 9.81 9 4 0 115.10 9.93 9 4 0 111.96 9.00 10 4 0 2.36 4.24 10 4 0 0.54 3.14 10 4 0 1.46 3.74 11 4 0 274.29 15.48 11 4 0 269.28 16.65 12 4 0 475.95 22.57 13 4 0 -1.16 5.01 12 -5 0 0.53 3.97 11 -5 0 12.57 4.52 11 -5 0 -0.24 4.00 10 -5 0 60.01 7.30 10 -5 0 60.24 7.86 9 -5 0 257.16 12.53 9 -5 0 236.09 12.73 8 -5 0 174.55 9.90 8 -5 0 163.64 9.24 8 -5 0 179.19 10.98 -8 5 0 151.15 8.32 -8 5 0 167.96 8.86 7 -5 0 27.23 4.94 7 -5 0 30.31 4.69 7 -5 0 29.44 4.28 -7 5 0 28.86 4.21 -7 5 0 30.94 4.13 6 -5 0 7.03 3.34 6 -5 0 3.55 1.92 6 -5 0 4.12 2.25 -6 5 0 6.54 2.02 -6 5 0 4.64 2.04 5 -5 0 94.09 6.02 5 -5 0 96.89 5.77 -5 5 0 93.87 5.66 -5 5 0 89.71 5.80 4 -5 0 8.69 2.04 4 -5 0 8.83 2.26 -4 5 0 11.35 2.46 -4 5 0 9.32 2.19 3 -5 0 344.76 13.42 3 -5 0 375.78 12.62 3 -5 0 356.66 12.12 -3 5 0 341.91 12.43 -3 5 0 352.37 12.37 2 -5 0 2.72 1.32 2 -5 0 3.35 1.59 -2 5 0 2.35 1.32 -2 5 0 2.23 1.39 -2 5 0 2.78 1.42 1 -5 0 1026.84 28.15 1 -5 0 1046.70 28.63 -1 5 0 1064.70 28.34 -1 5 0 1060.64 28.61 -1 5 0 1044.69 28.54 0 -5 0 362.90 12.00 0 -5 0 336.45 12.04 0 5 0 345.34 12.02 0 5 0 330.72 11.58 0 5 0 345.02 11.52 -1 -5 0 495.96 16.69 1 5 0 509.32 15.64 1 5 0 527.97 16.65 1 5 0 545.30 15.67 1 5 0 537.13 16.31 2 5 0 27.90 3.42 2 5 0 20.55 3.14 2 5 0 24.85 3.55 2 5 0 22.44 2.68 2 5 0 26.91 2.87 3 5 0 64.45 3.80 3 5 0 65.21 4.76 3 5 0 54.59 4.73 3 5 0 68.36 5.08 3 5 0 62.44 3.68 4 5 0 83.64 4.18 4 5 0 90.76 6.42 4 5 0 96.71 6.14 4 5 0 91.25 6.29 4 5 0 83.73 4.28 5 5 0 4.60 2.19 5 5 0 8.70 3.15 5 5 0 8.52 2.82 6 5 0 275.26 12.90 6 5 0 274.75 12.95 6 5 0 246.13 12.03 7 5 0 239.92 12.62 7 5 0 250.72 13.03 7 5 0 261.79 12.53 8 5 0 4.81 3.44 8 5 0 5.07 3.06 8 5 0 2.09 2.60 9 5 0 490.49 21.44 9 5 0 495.75 20.73 9 5 0 541.24 21.88 10 5 0 176.05 12.73 10 5 0 175.62 13.02 10 5 0 183.96 12.13 11 5 0 36.65 8.22 11 5 0 45.76 7.63 12 5 0 -3.12 3.64 11 -6 0 -0.10 2.99 10 -6 0 29.62 5.96 10 -6 0 30.47 5.53 9 -6 0 89.09 8.26 9 -6 0 66.58 7.66 8 -6 0 693.50 26.93 8 -6 0 646.81 23.01 8 -6 0 685.61 22.76 -8 6 0 645.08 21.57 -8 6 0 634.05 21.78 7 -6 0 1306.30 39.27 7 -6 0 1318.71 37.25 7 -6 0 1296.01 37.70 -7 6 0 1310.85 36.74 -7 6 0 1290.97 36.93 6 -6 0 17.04 3.35 6 -6 0 12.79 2.88 6 -6 0 15.07 4.12 -6 6 0 16.28 3.37 -6 6 0 10.39 2.74 5 -6 0 32.64 4.42 5 -6 0 32.26 4.17 -5 6 0 25.05 3.72 -5 6 0 26.15 4.06 4 -6 0 57.38 4.48 4 -6 0 47.62 5.87 4 -6 0 57.51 4.72 -4 6 0 54.59 5.29 -4 6 0 50.38 4.99 3 -6 0 548.60 17.61 3 -6 0 557.97 18.08 -3 6 0 533.94 17.91 -3 6 0 598.92 18.37 -3 6 0 577.54 18.52 2 -6 0 83.74 5.30 2 -6 0 77.07 4.89 -2 6 0 65.03 5.07 -2 6 0 78.88 5.27 -2 6 0 75.16 5.13 1 -6 0 2.43 1.44 1 -6 0 2.56 1.64 -1 6 0 1.94 1.59 -1 6 0 0.92 1.36 -1 6 0 1.42 1.26 0 -6 0 418.74 14.27 0 -6 0 415.06 14.60 0 6 0 401.09 13.70 0 6 0 412.13 14.46 0 6 0 402.40 13.91 -1 -6 0 307.52 11.97 -1 -6 0 300.79 11.51 1 6 0 281.53 10.63 1 6 0 271.32 11.32 1 6 0 279.07 10.40 -2 -6 0 100.56 6.62 2 6 0 92.72 6.23 2 6 0 94.07 5.27 2 6 0 92.96 6.03 2 6 0 103.86 5.60 3 6 0 133.08 7.82 3 6 0 128.63 7.35 3 6 0 120.82 7.44 3 6 0 131.14 6.12 3 6 0 137.82 6.39 4 6 0 1119.65 29.28 4 6 0 1166.56 32.88 4 6 0 1130.86 33.17 4 6 0 1063.25 32.66 4 6 0 1098.03 29.48 5 6 0 951.77 30.50 5 6 0 994.22 30.55 5 6 0 987.40 30.15 6 6 0 87.75 7.49 6 6 0 79.70 8.11 6 6 0 89.72 7.20 7 6 0 158.60 10.57 7 6 0 150.61 10.40 7 6 0 165.47 10.26 8 6 0 313.74 15.48 8 6 0 343.38 16.67 8 6 0 314.90 16.38 9 6 0 463.27 20.41 9 6 0 488.49 21.65 9 6 0 475.47 21.31 10 6 0 0.04 5.32 10 6 0 4.78 3.60 11 6 0 1.73 4.07 12 6 0 7.34 4.93 10 -7 0 134.54 9.73 9 -7 0 1.57 2.33 9 -7 0 -1.15 2.70 8 -7 0 95.38 7.48 8 -7 0 96.57 8.02 -8 7 0 84.55 6.97 -8 7 0 97.66 7.13 7 -7 0 136.68 10.35 7 -7 0 153.87 8.78 7 -7 0 137.35 9.04 -7 7 0 150.84 8.95 -7 7 0 150.00 8.74 6 -7 0 -0.72 2.39 6 -7 0 14.21 3.61 6 -7 0 11.60 3.10 -6 7 0 10.93 3.18 -6 7 0 13.28 3.40 5 -7 0 9.17 3.28 5 -7 0 9.54 2.94 5 -7 0 8.32 2.44 -5 7 0 5.79 2.51 -5 7 0 5.68 2.11 4 -7 0 -0.14 1.59 4 -7 0 -0.51 1.39 4 -7 0 1.00 2.18 -4 7 0 1.70 1.58 -4 7 0 -0.31 1.72 3 -7 0 860.16 26.02 3 -7 0 895.13 25.74 -3 7 0 852.71 26.13 -3 7 0 881.90 26.24 -3 7 0 848.36 26.33 2 -7 0 694.05 21.87 2 -7 0 729.66 21.67 -2 7 0 659.00 21.51 -2 7 0 719.30 22.15 -2 7 0 663.60 21.84 1 -7 0 104.79 6.33 1 -7 0 100.63 6.62 -1 7 0 108.83 6.68 -1 7 0 92.46 6.19 -1 7 0 106.16 6.36 0 -7 0 63.89 5.03 0 -7 0 58.49 5.95 0 7 0 70.65 5.00 0 7 0 56.26 5.37 0 7 0 55.12 5.82 -1 -7 0 766.35 24.49 -1 -7 0 774.54 24.08 1 7 0 777.50 24.37 1 7 0 784.35 23.20 1 7 0 753.10 22.78 -3 -7 0 39.63 5.67 3 7 0 26.95 4.21 3 7 0 24.97 3.37 3 7 0 24.77 4.27 3 7 0 29.69 3.66 4 7 0 282.16 13.21 4 7 0 307.02 14.00 4 7 0 293.68 13.07 4 7 0 288.03 10.91 5 7 0 7.99 3.36 5 7 0 6.60 2.91 5 7 0 6.45 3.46 6 7 0 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7 168.89 13.05 12 3 7 38.45 8.13 11 -4 -7 5.51 6.53 10 -4 -7 263.13 17.10 9 -4 -7 104.98 11.46 8 -4 -7 125.04 10.88 7 -4 -7 83.32 9.47 -7 4 7 81.12 5.68 -7 4 7 79.51 5.83 6 -4 -7 115.30 9.18 -6 4 7 125.15 7.11 -6 4 7 119.93 6.80 5 -4 -7 120.41 8.99 -5 4 7 113.07 6.59 -5 4 7 105.53 6.25 4 -4 -7 11.07 3.48 -4 4 7 15.75 2.90 -4 4 7 12.20 2.63 3 -4 -7 1386.85 33.57 3 -4 -7 1346.91 40.39 -3 4 7 1358.91 37.28 -3 4 7 1430.39 37.26 2 -4 -7 1953.18 53.79 2 -4 -7 1870.27 47.31 2 -4 -7 2043.11 47.34 -2 4 7 2012.75 51.23 -2 4 7 2022.75 50.90 1 -4 -7 962.30 24.72 1 -4 -7 968.55 24.53 -1 4 7 986.80 27.51 -1 4 7 980.61 27.69 0 4 7 264.61 10.42 0 4 7 275.95 8.84 0 4 7 275.17 10.79 0 4 7 279.45 11.11 1 4 7 443.03 15.02 1 4 7 478.57 14.07 1 4 7 464.01 15.73 1 4 7 460.79 14.25 1 4 7 461.00 15.40 2 4 7 1353.87 36.49 2 4 7 1331.55 35.48 2 4 7 1349.60 35.10 2 4 7 1321.42 35.70 2 4 7 1331.56 36.14 3 4 7 106.51 5.93 4 4 7 547.81 17.31 4 4 7 551.72 18.79 4 4 7 552.06 17.57 4 4 7 529.95 18.10 5 4 7 231.51 11.40 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4.05 -3 2 23 24.15 6.64 -2 2 23 5.78 4.45 -1 2 23 0.91 4.10 0 2 23 7.78 4.49 1 2 23 15.40 5.92 2 2 23 1.56 4.67 3 2 23 74.14 10.67 4 2 23 25.28 7.66 5 2 23 117.89 12.99 -5 3 23 4.65 5.25 -4 3 23 5.67 5.01 -3 3 23 127.56 12.91 -2 3 23 78.63 10.29 -1 3 23 27.48 7.24 0 3 23 5.09 4.89 1 3 23 24.29 7.28 2 3 23 72.34 10.42 3 3 23 0.69 4.83 4 3 23 29.73 7.85 -5 4 23 48.90 9.50 -4 4 23 76.91 10.61 -3 4 23 36.39 7.60 -2 4 23 172.64 13.76 -1 4 23 8.66 5.72 0 4 23 25.69 7.12 1 4 23 33.82 8.18 2 4 23 10.61 6.48 3 4 23 296.43 30.94 1 9 -24 101.44 13.67 0 9 -24 165.42 25.53 2 8 -24 62.71 10.99 1 8 -24 -0.58 5.64 0 8 -24 12.03 7.24 -1 8 -24 102.27 13.33 2 7 -24 34.20 8.31 1 7 -24 6.78 6.98 0 7 -24 49.20 9.54 -1 7 -24 -5.59 5.16 -2 7 -24 12.84 6.62 -3 7 -24 64.23 13.80 2 6 -24 35.90 8.36 1 6 -24 79.33 11.05 0 6 -24 107.02 12.78 -1 6 -24 323.02 19.30 -2 6 -24 101.33 12.52 -3 6 -24 11.44 5.97 -4 6 -24 27.17 12.19 3 5 -24 106.13 12.72 2 5 -24 16.86 6.80 1 5 -24 65.61 10.19 0 5 -24 8.22 6.63 -1 5 -24 278.31 18.07 -2 5 -24 1.34 5.44 -3 5 -24 170.10 15.96 -4 5 -24 14.91 6.88 3 4 -24 259.56 17.24 2 4 -24 202.20 15.56 1 4 -24 5.24 5.59 0 4 -24 9.68 5.93 -1 4 -24 9.26 6.53 -2 4 -24 89.55 11.58 -3 4 -24 117.27 13.19 -4 4 -24 -0.85 4.95 -5 4 -24 13.31 8.05 3 3 -24 -1.27 5.52 2 3 -24 245.27 16.75 1 3 -24 74.21 10.41 0 3 -24 57.99 9.54 -1 3 -24 19.65 7.26 -2 3 -24 11.29 6.06 -3 3 -24 219.80 16.16 -4 3 -24 166.29 15.87 -5 3 -24 53.13 9.59 4 2 -24 -3.23 4.95 3 2 -24 102.16 12.24 2 2 -24 149.56 14.48 1 2 -24 97.39 12.02 0 2 -24 58.35 9.25 -1 2 -24 22.94 7.08 -2 2 -24 26.26 7.62 -3 2 -24 64.65 10.02 -4 2 -24 211.31 15.65 -5 2 -24 90.33 11.88 -4 -1 24 21.29 5.94 -3 -1 24 10.41 4.99 -2 -1 24 85.34 10.00 -1 -1 24 74.30 9.51 0 -1 24 66.32 9.37 -2 1 -24 2.57 4.33 -3 1 -24 95.88 11.90 -4 1 -24 5.71 5.03 -5 1 -24 41.51 8.84 -4 0 24 5.56 4.30 -3 0 24 2.75 4.13 -2 0 24 8.28 5.20 -1 0 24 14.22 5.40 0 0 24 0.45 3.78 1 0 24 147.24 13.74 2 0 24 10.68 5.58 -4 0 -24 -2.43 4.32 -5 1 24 127.30 12.46 -4 1 24 27.00 7.03 -3 1 24 8.43 5.02 -2 1 24 7.32 5.01 -1 1 24 67.26 9.37 0 1 24 0.88 4.34 1 1 24 4.08 4.92 2 1 24 70.44 10.41 3 1 24 12.24 5.97 -4 2 24 40.88 8.14 -3 2 24 16.38 5.81 -2 2 24 103.17 11.40 -1 2 24 188.38 13.58 0 2 24 115.86 12.00 1 2 24 157.24 14.66 2 2 24 10.34 6.12 3 2 24 0.28 5.54 -4 3 24 37.13 8.10 -3 3 24 2.50 4.72 -2 3 24 23.69 6.79 -1 3 24 108.03 12.03 0 3 24 21.80 6.80 1 3 24 0.91 4.62 1 8 -25 -6.22 8.71 2 7 -25 7.18 7.42 1 7 -25 25.06 8.77 0 7 -25 -1.83 5.62 2 6 -25 18.67 7.14 1 6 -25 8.79 6.82 0 6 -25 0.92 5.31 -1 6 -25 -0.55 6.08 -2 6 -25 81.74 14.97 2 5 -25 18.78 7.81 1 5 -25 61.45 10.68 0 5 -25 -1.17 6.09 -1 5 -25 66.73 10.87 -2 5 -25 -0.97 5.41 3 4 -25 6.35 6.35 2 4 -25 1.68 5.99 1 4 -25 77.75 11.32 0 4 -25 21.15 7.51 -1 4 -25 16.43 6.97 -2 4 -25 125.37 14.06 -3 4 -25 154.22 16.00 3 3 -25 168.52 15.51 2 3 -25 242.10 16.70 1 3 -25 6.20 6.13 0 3 -25 44.14 9.13 -1 3 -25 26.08 7.60 -2 3 -25 4.49 6.30 -3 3 -25 2.86 5.71 3 2 -25 2.84 6.48 2 2 -25 50.04 9.80 1 2 -25 29.25 8.20 0 2 -25 3.69 5.03 -1 2 -25 61.61 10.01 -2 2 -25 11.49 6.35 -3 2 -25 4.81 5.91 -4 -1 25 2.16 5.47 -3 -1 25 -1.63 3.71 -2 -1 25 2.17 4.72 -1 -1 25 36.25 7.91 -1 1 -25 65.00 10.29 -2 1 -25 61.30 9.79 -3 1 -25 13.87 7.13 -4 0 25 9.49 5.51 -3 0 25 18.28 6.21 -2 0 25 146.84 13.53 -1 0 25 348.53 19.07 0 0 25 188.82 14.16 1 0 25 3.94 4.82 2 0 25 115.57 13.02 -5 1 25 27.31 8.97 -4 1 25 20.56 6.81 -3 1 25 10.29 5.91 -2 1 25 3.28 5.07 -1 1 25 30.36 7.40 0 1 25 177.70 13.73 1 1 25 142.88 14.23 -1 2 25 56.33 13.75 2 6 -26 -0.38 8.26 2 5 -26 -0.62 7.19 1 5 -26 3.30 7.21 3 4 -26 550.86 26.75 2 4 -26 190.50 17.21 1 4 -26 6.84 7.02 0 4 -26 4.27 6.99 3 3 -26 26.47 8.90 2 3 -26 30.67 9.17 1 3 -26 5.81 6.25 0 3 -26 48.79 10.11 3 2 -26 -3.10 6.53 2 2 -26 5.57 6.68 1 2 -26 100.72 13.17 0 2 -26 8.53 6.58 0 0 0 0.00 0.00 _exptl_absorpt_process_details ) Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D., J. Appl. Cryst. 48 (2015) 3-10 ) _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_max 0.7462 _exptl_absorpt_correction_T_min 0.6787 _exptl_special_details ) The following wavelength and cell were deduced by SADABS from the direction cosines etc. They are given here for emergency use only: CELL 0.71183 9.825 10.958 18.713 99.687 91.430 93.557 ) _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' ; _shelx_hkl_checksum 19015 _shelx_res_file ; TITL gm_vs_719_0m_a.res in P-1 1.res created by SHELXL-2017/1 at 11:18:53 on 30-Apr-2019 REM Old TITL REM SHELXT solution in P-1 REM R1 0.098, Rweak 0.005, Alpha 0.045, Orientation as input REM Formula found by SHELXT: C39 N4 Ni P4 F6 CELL 0.71073 9.7632 10.8846 18.5771 99.687 91.504 93.472 ZERR 2 0.0005 0.0005 0.0009 0.001 0.001 0.001 LATT 1 SFAC C H Cl F N Ni O P UNIT 78 80.81 2 12 6 2 1.4 6 SADI P3 F6 P3 F6A SADI P3 F5 P3 F5A SADI P3 F3 P3 F3A SADI P3 F2 P3 F2A SADI P3 F4 P3 F4A SADI P3 F1 P3 F1A L.S. 8 PLAN 20 TEMP 23 HTAB O1 Cl1 HTAB C14 O1 HTAB C20 Cl1 HTAB C9 F1 HTAB C9 F1A BOND $H CONF HTAB list 4 fmap 2 53 acta OMIT -2 52 OMIT -2 -4 9 OMIT 2 6 1 OMIT -2 -4 10 OMIT 0 0 1 OMIT 5 6 12 OMIT 6 3 14 OMIT 3 4 7 OMIT 1 -5 15 REM REM REM WGHT 0.032400 1.189500 FVAR 0.51551 0.55093 0.70159 NI1 6 0.552564 0.318712 0.265877 11.00000 0.01062 0.01432 = 0.01261 0.00463 0.00260 0.00193 CL1 3 0.693790 0.480105 0.345663 11.00000 0.01782 0.02664 = 0.01575 0.00054 -0.00200 -0.00350 P1 8 0.363003 0.410890 0.258928 11.00000 0.01127 0.01281 = 0.01160 0.00263 0.00153 0.00111 P2 8 0.699576 0.187565 0.221500 11.00000 0.01188 0.01843 = 0.01724 0.00604 0.00352 0.00412 P3 8 0.089545 -0.277715 0.122128 11.00000 0.02334 0.01529 = 0.02387 0.00427 -0.00619 0.00103 PART 1 F6 4 0.036103 -0.397849 0.064398 21.00000 0.02671 0.02616 = 0.01998 0.00188 0.01159 -0.01507 F5 4 0.108793 -0.187831 0.062758 21.00000 0.03302 0.02304 = 0.03863 0.01336 -0.01934 -0.01115 F3 4 0.087665 -0.369229 0.182030 21.00000 0.02750 0.02515 = 0.02342 0.01099 0.00596 0.01109 F2 4 0.245200 -0.311368 0.105648 21.00000 0.02027 0.04240 = 0.03848 0.02213 -0.00290 0.00251 F4 4 -0.065158 -0.241903 0.136203 21.00000 0.03303 0.04539 = 0.05086 -0.00432 0.00225 0.02146 PART 0 N3 5 0.446059 0.154723 0.368752 11.00000 0.01517 0.01558 = 0.01838 0.00601 0.00224 0.00254 N1 5 0.534573 0.501389 0.172254 11.00000 0.01632 0.01539 = 0.01470 0.00601 0.00404 0.00091 PART 1 F1 4 0.147608 -0.157322 0.178828 21.00000 0.06231 0.02565 = 0.03045 0.00451 -0.01781 -0.00943 PART 0 N2 5 0.713078 0.374488 0.147379 11.00000 0.01354 0.02015 = 0.01657 0.00722 0.00634 0.00168 C32 1 0.389428 0.069710 0.410747 11.00000 0.01284 0.01661 = 0.01883 0.00844 0.00100 0.00075 C1 1 0.269030 0.473850 0.337548 11.00000 0.01577 0.01139 = 0.01459 0.00155 0.00343 -0.00048 C38 1 0.358881 0.114488 0.483072 11.00000 0.01478 0.02073 = 0.02002 0.00645 0.00029 0.00277 C12 1 0.204834 0.360686 0.126679 11.00000 0.01381 0.01850 = 0.01748 0.00299 0.00369 0.00182 AFIX 43 H12 2 0.235275 0.439581 0.118441 11.00000 -1.20000 AFIX 0 C33 1 0.366111 -0.055080 0.377058 11.00000 0.01707 0.01928 = 0.02152 0.00601 -0.00228 0.00219 C2 1 0.335086 0.496867 0.406116 11.00000 0.01994 0.01760 = 0.01729 0.00371 0.00063 0.00303 AFIX 43 H2 2 0.426093 0.478010 0.411243 11.00000 -1.20000 AFIX 0 C7 1 0.241229 0.321909 0.192218 11.00000 0.00935 0.01683 = 0.01400 -0.00043 0.00235 0.00411 C18 1 0.802268 0.283823 0.168588 11.00000 0.01253 0.02282 = 0.02245 0.00642 0.00577 0.00329 AFIX 23 H18A 2 0.880463 0.325815 0.197929 11.00000 -1.20000 H18B 2 0.835727 0.232500 0.125648 11.00000 -1.20000 AFIX 0 C31 1 0.489218 0.220081 0.330200 11.00000 0.01341 0.01593 = 0.01497 0.00056 0.00040 0.00452 C6 1 0.132866 0.504498 0.329941 11.00000 0.01625 0.02293 = 0.02085 -0.00045 0.00058 0.00078 AFIX 43 H6 2 0.088562 0.490372 0.284087 11.00000 -1.20000 AFIX 0 C13 1 0.429235 0.546584 0.221913 11.00000 0.01494 0.01357 = 0.01692 0.00350 0.00215 0.00051 AFIX 23 H13A 2 0.356744 0.580439 0.196048 11.00000 -1.20000 H13B 2 0.467956 0.611237 0.260734 11.00000 -1.20000 AFIX 0 C9 1 0.112358 0.124805 0.150704 11.00000 0.01218 0.01516 = 0.03406 -0.00021 0.00374 0.00122 AFIX 43 H9 2 0.080947 0.045993 0.158656 11.00000 -1.20000 AFIX 0 C17 1 0.603485 0.404474 0.186445 11.00000 0.01264 0.01558 = 0.01254 0.00219 -0.00017 -0.00195 C8 1 0.192034 0.203899 0.204114 11.00000 0.01339 0.01805 = 0.02153 0.00545 0.00190 0.00337 AFIX 43 H8 2 0.212933 0.178289 0.248196 11.00000 -1.20000 AFIX 0 C35 1 0.308089 -0.136706 0.419329 11.00000 0.02318 0.01672 = 0.03129 0.00910 -0.00248 -0.00154 AFIX 43 H35 2 0.289979 -0.220368 0.398939 11.00000 -1.20000 AFIX 0 C11 1 0.123591 0.281880 0.074042 11.00000 0.01414 0.03092 = 0.01383 -0.00080 0.00024 0.00407 AFIX 43 H11 2 0.098397 0.308506 0.030849 11.00000 -1.20000 AFIX 0 C10 1 0.079722 0.163655 0.085438 11.00000 0.01238 0.02668 = 0.02314 -0.00859 0.00091 0.00215 AFIX 43 H10 2 0.028066 0.109994 0.049102 11.00000 -1.20000 AFIX 0 C37 1 0.302144 0.027809 0.522541 11.00000 0.02281 0.02993 = 0.01878 0.01044 0.00506 0.00425 AFIX 43 H37 2 0.280853 0.053574 0.571022 11.00000 -1.20000 AFIX 0 C25 1 0.628373 0.057321 0.154653 11.00000 0.02010 0.01675 = 0.01861 0.00613 0.00624 0.00349 C26 1 0.487101 0.043595 0.141330 11.00000 0.02032 0.01975 = 0.01871 0.00465 0.00495 0.00331 AFIX 43 H26 2 0.431048 0.098797 0.168329 11.00000 -1.20000 AFIX 0 C30 1 0.711806 -0.025392 0.113129 11.00000 0.02186 0.02090 = 0.03472 0.00507 0.01237 0.00448 AFIX 43 H30 2 0.806621 -0.016810 0.121014 11.00000 -1.20000 AFIX 0 C19 1 0.823960 0.132320 0.280806 11.00000 0.01429 0.03547 = 0.02146 0.01240 0.00843 0.01065 C4 1 0.130782 0.576601 0.459009 11.00000 0.02707 0.01694 = 0.02325 -0.00299 0.01417 -0.00513 AFIX 43 H4 2 0.084152 0.610234 0.499969 11.00000 -1.20000 AFIX 0 C3 1 0.265367 0.547912 0.466848 11.00000 0.03092 0.01898 = 0.01539 0.00376 0.00367 0.00052 AFIX 43 H3 2 0.309288 0.562788 0.512807 11.00000 -1.20000 AFIX 0 C36 1 0.276722 -0.096128 0.491070 11.00000 0.02193 0.02770 = 0.03244 0.02009 0.00395 -0.00075 AFIX 43 H36 2 0.238198 -0.152603 0.518431 11.00000 -1.20000 AFIX 0 C14 1 0.581420 0.585122 0.122075 11.00000 0.02722 0.02296 = 0.02561 0.01493 0.00927 0.00341 AFIX 23 H14A 2 0.641321 0.653220 0.148386 11.00000 -1.20000 H14B 2 0.503114 0.620324 0.101877 11.00000 -1.20000 AFIX 0 C39 1 0.384200 0.250028 0.516043 11.00000 0.03968 0.02221 = 0.02325 0.00385 0.00276 0.00397 AFIX 137 H39A 2 0.476880 0.277572 0.507843 11.00000 -1.50000 H39B 2 0.370229 0.260670 0.567623 11.00000 -1.50000 H39C 2 0.321671 0.298462 0.493734 11.00000 -1.50000 AFIX 0 C28 1 0.511843 -0.132575 0.047912 11.00000 0.04128 0.01676 = 0.02338 0.00142 0.00527 -0.00438 AFIX 43 H28 2 0.473117 -0.196220 0.012127 11.00000 -1.20000 AFIX 0 C5 1 0.064270 0.556008 0.391040 11.00000 0.01523 0.02520 = 0.03374 -0.00485 0.00700 -0.00087 AFIX 43 H5 2 -0.026199 0.576635 0.386303 11.00000 -1.20000 AFIX 0 C27 1 0.428848 -0.051178 0.088398 11.00000 0.02491 0.02397 = 0.02480 0.00860 0.00174 -0.00047 AFIX 43 H27 2 0.334121 -0.059979 0.080142 11.00000 -1.20000 AFIX 0 C20 1 0.906678 0.222495 0.327903 11.00000 0.02040 0.04555 = 0.02159 0.00365 0.00186 0.01312 AFIX 43 H20 2 0.895368 0.306770 0.328083 11.00000 -1.20000 AFIX 0 C16 1 0.770896 0.446809 0.093613 11.00000 0.02290 0.03240 = 0.02609 0.01367 0.01360 0.00402 AFIX 23 H16A 2 0.812815 0.391353 0.055220 11.00000 -1.20000 H16B 2 0.841248 0.508151 0.117298 11.00000 -1.20000 AFIX 0 C15 1 0.657981 0.511932 0.061045 11.00000 0.03202 0.03420 = 0.02309 0.01774 0.01204 0.00795 AFIX 23 H15A 2 0.595132 0.450710 0.030908 11.00000 -1.20000 H15B 2 0.697195 0.567956 0.030464 11.00000 -1.20000 AFIX 0 C34 1 0.401827 -0.097611 0.299201 11.00000 0.04994 0.02279 = 0.02479 0.00085 0.00580 0.00069 AFIX 137 H34A 2 0.360008 -0.046466 0.268601 11.00000 -1.50000 H34B 2 0.368621 -0.183124 0.283952 11.00000 -1.50000 H34C 2 0.499716 -0.090470 0.295207 11.00000 -1.50000 AFIX 0 C29 1 0.653062 -0.119557 0.060543 11.00000 0.03760 0.01980 = 0.03471 -0.00017 0.01912 0.00381 AFIX 43 H29 2 0.708560 -0.174920 0.033252 11.00000 -1.20000 AFIX 0 C23 1 0.938679 -0.026483 0.329796 11.00000 0.02966 0.04997 = 0.05402 0.03597 0.01409 0.01676 AFIX 43 H23 2 0.949579 -0.110410 0.331006 11.00000 -1.20000 AFIX 0 C21 1 1.005176 0.187789 0.374247 11.00000 0.02127 0.06481 = 0.02378 0.00638 0.00335 0.01617 AFIX 43 H21 2 1.060609 0.248325 0.404852 11.00000 -1.20000 AFIX 0 C24 1 0.838782 0.006499 0.282041 11.00000 0.02046 0.03875 = 0.04070 0.02345 0.00680 0.00792 AFIX 43 H24 2 0.783558 -0.054714 0.251798 11.00000 -1.20000 AFIX 0 C22 1 1.020363 0.063042 0.374647 11.00000 0.02021 0.07622 = 0.03084 0.02619 0.00503 0.01488 AFIX 43 H22 2 1.086540 0.039324 0.405578 11.00000 -1.20000 AFIX 0 PART 2 F3A 4 0.058038 -0.358614 0.185289 -21.00000 0.02894 0.02524 = 0.02701 0.00683 0.00607 0.01362 F6A 4 0.060452 -0.393195 0.056646 -21.00000 0.02397 0.01826 = 0.01814 0.00106 0.01254 -0.01003 F5A 4 0.099298 -0.196696 0.057358 -21.00000 0.04246 0.03032 = 0.03622 0.02250 -0.02296 -0.01562 F2A 4 0.248660 -0.304911 0.124594 -21.00000 0.01917 0.04772 = 0.04700 0.03231 -0.01652 -0.00829 F4A 4 -0.071688 -0.257642 0.121039 -21.00000 0.03148 0.03862 = 0.03413 0.00575 0.00635 0.01446 F1A 4 0.114929 -0.164512 0.188584 -21.00000 0.08751 0.01639 = 0.03331 -0.00192 -0.01226 -0.01253 PART 0 AFIX 6 O1 7 0.772174 0.708015 0.267180 31.00000 0.06063 0.03897 = 0.05415 0.01967 -0.00048 -0.01336 H1A 2 0.845247 0.690852 0.244737 31.00000 -1.50000 H1B 2 0.756170 0.647324 0.289812 31.00000 -1.50000 AFIX 0 HKLF 4 REM gm_vs_719_0m_a.res in P-1 REM R1 = 0.0299 for 6603 Fo > 4sig(Fo) and 0.0352 for all 7473 data REM 548 parameters refined using 6 restraints END WGHT 0.0323 1.2207 REM Instructions for potential hydrogen bonds HTAB C2 Cl1 EQIV $1 x, y+1, z HTAB C6 F3^a_$1 HTAB C13 F2^a_$1 HTAB C13 F2A^b_$1 HTAB C14 O1 HTAB C20 Cl1 EQIV $2 -x+1, -y, -z HTAB C16 F6A^b_$2 EQIV $3 x+1, y+1, z HTAB C16 F6^a_$3 HTAB C16 F4A^b_$3 EQIV $4 x, y-1, z HTAB C24 O1_$4 REM Highest difference peak 0.456, deepest hole -0.302, 1-sigma level 0.056 Q1 1 0.3999 0.4837 0.2391 11.00000 0.05 0.46 Q2 1 0.6644 0.1227 0.1858 11.00000 0.05 0.43 Q3 1 0.9732 0.1139 0.3666 11.00000 0.05 0.39 Q4 1 0.2986 0.3597 0.2195 11.00000 0.05 0.38 Q5 1 0.8965 -0.0977 0.2999 11.00000 0.05 0.35 Q6 1 0.7576 0.1595 0.2578 11.00000 0.05 0.33 Q7 1 0.5621 0.3340 0.1986 11.00000 0.05 0.32 Q8 1 0.4546 0.3330 0.2411 11.00000 0.05 0.31 Q9 1 0.5838 0.4062 0.2512 11.00000 0.05 0.30 Q10 1 0.6468 0.2368 0.2610 11.00000 0.05 0.29 Q11 1 0.1360 0.1782 0.1799 11.00000 0.05 0.29 Q12 1 0.5343 0.2381 0.2369 11.00000 0.05 0.29 Q13 1 0.3472 0.0973 0.4438 11.00000 0.05 0.29 Q14 1 0.3018 0.5029 0.3702 11.00000 0.05 0.29 Q15 1 0.8709 0.1547 0.3208 11.00000 0.05 0.28 Q16 1 0.7035 0.4058 0.3185 11.00000 0.05 0.28 Q17 1 0.3833 0.1723 0.4996 11.00000 0.05 0.28 Q18 1 0.3187 0.4616 0.3043 11.00000 0.05 0.28 Q19 1 0.7565 0.2257 0.1825 11.00000 0.05 0.28 Q20 1 0.8085 0.0666 0.2750 11.00000 0.05 0.27 ; _shelx_res_checksum 71605 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, -z' loop_ _atom_site_type_symbol _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Ni Ni1 0.55256(2) 0.31871(2) 0.26588(2) 0.01216(7) Uani d 1 . . Cl Cl1 0.69379(5) 0.48010(4) 0.34566(2) 0.02068(11) Uani d 1 . . P P1 0.36300(5) 0.41089(4) 0.25893(2) 0.01180(10) Uani d 1 . . P P2 0.69958(5) 0.18756(4) 0.22150(3) 0.01532(11) Uani d 1 . . P P3 0.08955(5) -0.27772(4) 0.12213(3) 0.02086(12) Uani d 1 . . F F6 0.036(2) -0.3978(15) 0.0644(9) 0.025(2) Uani d 0.55(5) A 1 F F5 0.109(3) -0.188(3) 0.0628(15) 0.032(3) Uani d 0.55(5) A 1 F F3 0.088(2) -0.3692(17) 0.1820(9) 0.0241(19) Uani d 0.55(5) A 1 F F2 0.2452(11) -0.3114(18) 0.1056(10) 0.032(2) Uani d 0.55(5) A 1 F F4 -0.0652(11) -0.2419(18) 0.1362(12) 0.044(3) Uani d 0.55(5) A 1 N N3 0.44606(16) 0.15472(14) 0.36875(9) 0.0159(3) Uani d 1 . . N N1 0.53457(16) 0.50139(13) 0.17225(8) 0.0150(3) Uani d 1 . . F F1 0.1476(19) -0.1573(11) 0.1788(8) 0.040(2) Uani d 0.55(5) A 1 N N2 0.71308(16) 0.37449(14) 0.14738(8) 0.0162(3) Uani d 1 . . C C32 0.38943(18) 0.06971(16) 0.41075(10) 0.0155(4) Uani d 1 . . C C1 0.26903(19) 0.47385(15) 0.33755(10) 0.0140(4) Uani d 1 . . C C38 0.35888(19) 0.11449(17) 0.48307(11) 0.0181(4) Uani d 1 . . C C12 0.20483(19) 0.36069(17) 0.12668(10) 0.0165(4) Uani d 1 . . H H12 0.235275 0.439581 0.118441 0.020 Uiso calc 1 . . C C33 0.3661(2) -0.05508(17) 0.37706(11) 0.0190(4) Uani d 1 . . C C2 0.3351(2) 0.49687(17) 0.40612(10) 0.0181(4) Uani d 1 . . H H2 0.426093 0.478010 0.411243 0.022 Uiso calc 1 . . C C7 0.24123(18) 0.32191(16) 0.19222(10) 0.0136(4) Uani d 1 . . C C18 0.80227(19) 0.28382(18) 0.16859(11) 0.0188(4) Uani d 1 . . H H18A 0.880463 0.325815 0.197929 0.023 Uiso calc 1 . . H H18B 0.835727 0.232500 0.125648 0.023 Uiso calc 1 . . C C31 0.48922(18) 0.22008(16) 0.33020(10) 0.0149(4) Uani d 1 . . C C6 0.1329(2) 0.50450(18) 0.32994(11) 0.0205(4) Uani d 1 . . H H6 0.088562 0.490372 0.284087 0.025 Uiso calc 1 . . C C13 0.42924(19) 0.54658(16) 0.22191(10) 0.0150(4) Uani d 1 . . H H13A 0.356744 0.580439 0.196048 0.018 Uiso calc 1 . . H H13B 0.467956 0.611237 0.260734 0.018 Uiso calc 1 . . C C9 0.11236(19) 0.12481(17) 0.15070(11) 0.0209(4) Uani d 1 . . H H9 0.080947 0.045993 0.158656 0.025 Uiso calc 1 . . C C17 0.60348(18) 0.40447(16) 0.18644(10) 0.0137(4) Uani d 1 . . C C8 0.19203(19) 0.20390(17) 0.20411(11) 0.0173(4) Uani d 1 . . H H8 0.212933 0.178289 0.248196 0.021 Uiso calc 1 . . C C35 0.3081(2) -0.13671(18) 0.41933(12) 0.0233(4) Uani d 1 . . H H35 0.289979 -0.220368 0.398939 0.028 Uiso calc 1 . . C C11 0.12359(19) 0.28188(18) 0.07404(10) 0.0201(4) Uani d 1 . . H H11 0.098397 0.308506 0.030849 0.024 Uiso calc 1 . . C C10 0.07972(19) 0.16365(18) 0.08544(11) 0.0222(4) Uani d 1 . . H H10 0.028066 0.109994 0.049102 0.027 Uiso calc 1 . . C C37 0.3021(2) 0.02781(19) 0.52254(11) 0.0229(4) Uani d 1 . . H H37 0.280853 0.053574 0.571022 0.028 Uiso calc 1 . . C C25 0.6284(2) 0.05732(17) 0.15465(10) 0.0179(4) Uani d 1 . . C C26 0.4871(2) 0.04360(17) 0.14133(11) 0.0193(4) Uani d 1 . . H H26 0.431048 0.098797 0.168329 0.023 Uiso calc 1 . . C C30 0.7118(2) -0.02539(18) 0.11313(12) 0.0255(5) Uani d 1 . . H H30 0.806621 -0.016810 0.121014 0.031 Uiso calc 1 . . C C19 0.8240(2) 0.13232(19) 0.28081(11) 0.0224(4) Uani d 1 . . C C4 0.1308(2) 0.57660(17) 0.45901(11) 0.0232(4) Uani d 1 . . H H4 0.084152 0.610234 0.499969 0.028 Uiso calc 1 . . C C3 0.2654(2) 0.54791(17) 0.46685(11) 0.0217(4) Uani d 1 . . H H3 0.309288 0.562788 0.512807 0.026 Uiso calc 1 . . C C36 0.2767(2) -0.09613(19) 0.49107(12) 0.0257(5) Uani d 1 . . H H36 0.238198 -0.152603 0.518431 0.031 Uiso calc 1 . . C C14 0.5814(2) 0.58512(18) 0.12208(11) 0.0238(4) Uani d 1 . . H H14A 0.641321 0.653220 0.148386 0.029 Uiso calc 1 . . H H14B 0.503114 0.620324 0.101877 0.029 Uiso calc 1 . . C C39 0.3842(2) 0.25003(18) 0.51604(12) 0.0283(5) Uani d 1 . . H H39A 0.476880 0.277572 0.507843 0.042 Uiso calc 1 . . H H39B 0.370229 0.260670 0.567623 0.042 Uiso calc 1 . . H H39C 0.321671 0.298462 0.493734 0.042 Uiso calc 1 . . C C28 0.5118(2) -0.13257(18) 0.04791(12) 0.0276(5) Uani d 1 . . H H28 0.473117 -0.196220 0.012127 0.033 Uiso calc 1 . . C C5 0.0643(2) 0.55601(19) 0.39104(12) 0.0258(5) Uani d 1 . . H H5 -0.026199 0.576635 0.386303 0.031 Uiso calc 1 . . C C27 0.4288(2) -0.05118(18) 0.08840(11) 0.0241(4) Uani d 1 . . H H27 0.334121 -0.059979 0.080142 0.029 Uiso calc 1 . . C C20 0.9067(2) 0.2225(2) 0.32790(11) 0.0289(5) Uani d 1 . . H H20 0.895368 0.306770 0.328083 0.035 Uiso calc 1 . . C C16 0.7709(2) 0.4468(2) 0.09361(12) 0.0258(5) Uani d 1 . . H H16A 0.812815 0.391353 0.055220 0.031 Uiso calc 1 . . H H16B 0.841248 0.508151 0.117298 0.031 Uiso calc 1 . . C C15 0.6580(2) 0.5119(2) 0.06104(12) 0.0278(5) Uani d 1 . . H H15A 0.595132 0.450710 0.030908 0.033 Uiso calc 1 . . H H15B 0.697195 0.567956 0.030464 0.033 Uiso calc 1 . . C C34 0.4018(3) -0.0976(2) 0.29920(12) 0.0329(5) Uani d 1 . . H H34A 0.360008 -0.046466 0.268601 0.049 Uiso calc 1 . . H H34B 0.368621 -0.183124 0.283952 0.049 Uiso calc 1 . . H H34C 0.499716 -0.090470 0.295207 0.049 Uiso calc 1 . . C C29 0.6531(2) -0.11956(19) 0.06054(13) 0.0309(5) Uani d 1 . . H H29 0.708560 -0.174920 0.033252 0.037 Uiso calc 1 . . C C23 0.9387(2) -0.0265(2) 0.32980(15) 0.0406(6) Uani d 1 . . H H23 0.949579 -0.110410 0.331006 0.049 Uiso calc 1 . . C C21 1.0052(2) 0.1878(3) 0.37425(12) 0.0362(6) Uani d 1 . . H H21 1.060609 0.248325 0.404852 0.043 Uiso calc 1 . . C C24 0.8388(2) 0.0065(2) 0.28204(13) 0.0310(5) Uani d 1 . . H H24 0.783558 -0.054714 0.251798 0.037 Uiso calc 1 . . C C22 1.0204(2) 0.0630(3) 0.37465(13) 0.0399(6) Uani d 1 . . H H22 1.086540 0.039324 0.405578 0.048 Uiso calc 1 . . F F3A 0.058(2) -0.359(2) 0.1853(11) 0.026(2) Uani d 0.45(5) A 2 F F6A 0.060(3) -0.3932(17) 0.0566(11) 0.021(2) Uani d 0.45(5) A 2 F F5A 0.099(4) -0.197(3) 0.0574(18) 0.036(5) Uani d 0.45(5) A 2 F F2A 0.2487(12) -0.305(2) 0.1246(13) 0.036(3) Uani d 0.45(5) A 2 F F4A -0.0717(12) -0.258(2) 0.1210(13) 0.034(3) Uani d 0.45(5) A 2 F F1A 0.115(3) -0.1645(14) 0.1886(10) 0.047(4) Uani d 0.45(5) A 2 O O1 0.7722(3) 0.7080(2) 0.26718(16) 0.0506(10) Uani d 0.702(6) . . H H1A 0.845247 0.690852 0.244737 0.076 Uiso d 0.702(6) . . H H1B 0.756170 0.647324 0.289812 0.076 Uiso d 0.702(6) . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Ni1 0.01062(12) 0.01432(12) 0.01261(13) 0.00193(9) 0.00260(9) 0.00463(9) Cl1 0.0178(2) 0.0266(2) 0.0157(2) -0.00350(18) -0.00200(18) 0.00054(18) P1 0.0113(2) 0.0128(2) 0.0116(2) 0.00111(17) 0.00153(18) 0.00263(17) P2 0.0119(2) 0.0184(2) 0.0172(2) 0.00412(18) 0.00352(19) 0.00604(19) P3 0.0233(3) 0.0153(2) 0.0239(3) 0.0010(2) -0.0062(2) 0.0043(2) F6 0.027(5) 0.026(2) 0.020(3) -0.015(2) 0.012(3) 0.002(2) F5 0.033(4) 0.023(3) 0.039(5) -0.011(4) -0.019(4) 0.013(3) F3 0.028(5) 0.025(3) 0.023(2) 0.011(3) 0.006(3) 0.011(2) F2 0.020(2) 0.042(2) 0.038(5) 0.003(2) -0.003(2) 0.022(4) F4 0.033(3) 0.045(4) 0.051(8) 0.021(2) 0.002(3) -0.004(4) N3 0.0152(8) 0.0156(7) 0.0184(8) 0.0025(6) 0.0022(7) 0.0060(7) N1 0.0163(8) 0.0154(7) 0.0147(8) 0.0009(6) 0.0040(6) 0.0060(6) F1 0.062(5) 0.026(3) 0.030(3) -0.009(2) -0.018(3) 0.005(2) N2 0.0135(8) 0.0202(8) 0.0166(8) 0.0017(6) 0.0063(6) 0.0072(6) C32 0.0128(9) 0.0166(9) 0.0188(10) 0.0008(7) 0.0010(7) 0.0084(7) C1 0.0158(9) 0.0114(8) 0.0146(9) -0.0005(7) 0.0034(7) 0.0015(7) C38 0.0148(10) 0.0207(9) 0.0200(10) 0.0028(7) 0.0003(8) 0.0065(8) C12 0.0138(9) 0.0185(9) 0.0175(10) 0.0018(7) 0.0037(8) 0.0030(7) C33 0.0171(10) 0.0193(9) 0.0215(10) 0.0022(7) -0.0023(8) 0.0060(8) C2 0.0199(10) 0.0176(9) 0.0173(10) 0.0030(7) 0.0006(8) 0.0037(7) C7 0.0093(9) 0.0168(8) 0.0140(9) 0.0041(7) 0.0023(7) -0.0004(7) C18 0.0125(9) 0.0228(9) 0.0224(10) 0.0033(7) 0.0058(8) 0.0064(8) C31 0.0134(9) 0.0159(9) 0.0150(9) 0.0045(7) 0.0004(7) 0.0006(7) C6 0.0162(10) 0.0229(10) 0.0209(10) 0.0008(8) 0.0006(8) -0.0005(8) C13 0.0149(9) 0.0136(8) 0.0169(9) 0.0005(7) 0.0021(8) 0.0035(7) C9 0.0122(9) 0.0152(9) 0.0341(12) 0.0012(7) 0.0037(8) -0.0002(8) C17 0.0126(9) 0.0156(8) 0.0125(9) -0.0019(7) -0.0002(7) 0.0022(7) C8 0.0134(9) 0.0180(9) 0.0215(10) 0.0034(7) 0.0019(8) 0.0055(8) C35 0.0232(11) 0.0167(9) 0.0313(12) -0.0015(8) -0.0025(9) 0.0091(8) C11 0.0141(10) 0.0309(11) 0.0138(9) 0.0041(8) 0.0002(8) -0.0008(8) C10 0.0124(10) 0.0267(10) 0.0231(11) 0.0022(8) 0.0009(8) -0.0086(8) C37 0.0228(11) 0.0299(11) 0.0188(10) 0.0042(8) 0.0051(8) 0.0104(8) C25 0.0201(10) 0.0167(9) 0.0186(10) 0.0035(7) 0.0062(8) 0.0061(7) C26 0.0203(10) 0.0198(9) 0.0187(10) 0.0033(8) 0.0050(8) 0.0047(8) C30 0.0219(11) 0.0209(10) 0.0347(12) 0.0045(8) 0.0124(9) 0.0051(9) C19 0.0143(10) 0.0355(11) 0.0215(10) 0.0107(8) 0.0084(8) 0.0124(9) C4 0.0271(11) 0.0169(9) 0.0233(11) -0.0051(8) 0.0142(9) -0.0030(8) C3 0.0309(12) 0.0190(9) 0.0154(10) 0.0005(8) 0.0037(8) 0.0038(8) C36 0.0219(11) 0.0277(11) 0.0324(12) -0.0007(8) 0.0039(9) 0.0201(9) C14 0.0272(11) 0.0230(10) 0.0256(11) 0.0034(8) 0.0093(9) 0.0149(9) C39 0.0397(13) 0.0222(10) 0.0233(11) 0.0040(9) 0.0028(10) 0.0038(9) C28 0.0413(13) 0.0168(9) 0.0234(11) -0.0044(9) 0.0053(10) 0.0014(8) C5 0.0152(10) 0.0252(10) 0.0337(12) -0.0009(8) 0.0070(9) -0.0048(9) C27 0.0249(11) 0.0240(10) 0.0248(11) -0.0005(8) 0.0017(9) 0.0086(8) C20 0.0204(11) 0.0455(13) 0.0216(11) 0.0131(10) 0.0019(9) 0.0036(10) C16 0.0229(11) 0.0324(11) 0.0261(11) 0.0040(9) 0.0136(9) 0.0137(9) C15 0.0320(12) 0.0342(11) 0.0231(11) 0.0079(9) 0.0120(9) 0.0177(9) C34 0.0499(15) 0.0228(11) 0.0248(12) 0.0007(10) 0.0058(11) 0.0009(9) C29 0.0376(13) 0.0198(10) 0.0347(13) 0.0038(9) 0.0191(11) -0.0002(9) C23 0.0297(13) 0.0500(15) 0.0540(16) 0.0168(11) 0.0141(12) 0.0360(13) C21 0.0213(12) 0.0648(17) 0.0238(12) 0.0162(11) 0.0034(9) 0.0064(11) C24 0.0205(11) 0.0388(12) 0.0407(14) 0.0079(9) 0.0068(10) 0.0234(11) C22 0.0202(12) 0.0762(19) 0.0308(13) 0.0149(12) 0.0050(10) 0.0262(13) F3A 0.029(7) 0.025(3) 0.027(3) 0.014(4) 0.006(4) 0.007(2) F6A 0.024(6) 0.018(3) 0.018(3) -0.010(3) 0.013(3) 0.001(2) F5A 0.042(8) 0.030(7) 0.036(5) -0.016(4) -0.023(4) 0.023(7) F2A 0.019(3) 0.048(4) 0.047(8) -0.008(2) -0.017(3) 0.032(6) F4A 0.031(3) 0.039(5) 0.034(6) 0.014(2) 0.006(3) 0.006(5) F1A 0.088(10) 0.016(3) 0.033(4) -0.013(4) -0.012(5) -0.002(3) O1 0.061(2) 0.0390(16) 0.054(2) -0.0134(13) -0.0005(14) 0.0197(13) 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' Cl Cl 0.1484 0.1585 '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' Ni Ni 0.3393 1.1124 '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' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_publ_flag P1 Ni1 Cl1 100.968(19) y P2 Ni1 Cl1 103.29(2) y P2 Ni1 P1 152.21(2) y C31 Ni1 Cl1 101.89(6) y C31 Ni1 P1 94.89(6) y C31 Ni1 P2 93.19(6) y C31 Ni1 C17 171.10(8) y C17 Ni1 Cl1 87.02(5) y C17 Ni1 P1 83.42(5) y C17 Ni1 P2 84.51(5) y C1 P1 Ni1 123.61(6) ? C1 P1 C7 107.69(8) ? C1 P1 C13 105.08(8) ? C7 P1 Ni1 112.12(6) ? C7 P1 C13 107.81(8) ? C13 P1 Ni1 98.98(6) ? C18 P2 Ni1 100.44(6) ? C25 P2 Ni1 114.87(6) ? C25 P2 C18 104.57(9) ? C25 P2 C19 109.27(9) ? C19 P2 Ni1 120.87(7) ? C19 P2 C18 104.45(9) ? F6 P3 F5 95.0(17) ? F6 P3 F3 86.3(11) ? F6 P3 F2 89.4(9) ? F6 P3 F4 90.5(9) ? F6 P3 F1 178.2(8) ? F5 P3 F3 173.9(14) ? F5 P3 F2 85.4(12) ? F5 P3 F1 84.2(16) ? F2 P3 F3 88.7(7) ? F4 P3 F5 92.7(12) ? F4 P3 F3 93.2(8) ? F4 P3 F2 178.1(8) ? F4 P3 F1 91.2(9) ? F1 P3 F3 94.3(10) ? F1 P3 F2 89.0(8) ? F3A P3 F5A 172.4(18) ? F6A P3 F3A 94.6(13) ? F6A P3 F5A 84(2) ? F6A P3 F4A 88.4(11) ? F2A P3 F3A 91.5(9) ? F2A P3 F6A 90.3(11) ? F2A P3 F5A 96.0(17) ? F2A P3 F4A 176.9(11) ? F4A P3 F3A 85.8(10) ? F4A P3 F5A 86.7(16) ? F1A P3 F3A 84.0(13) ? F1A P3 F6A 178.3(10) ? F1A P3 F5A 97.3(19) ? F1A P3 F2A 90.7(10) ? F1A P3 F4A 90.5(11) ? C31 N3 C32 175.71(18) y C13 N1 C14 116.07(14) ? C17 N1 C13 118.15(15) ? C17 N1 C14 123.79(16) ? C18 N2 C16 114.51(15) ? C17 N2 C18 119.58(15) ? C17 N2 C16 124.39(15) ? C38 C32 N3 118.38(16) ? C38 C32 C33 123.96(17) ? C33 C32 N3 117.66(17) ? C2 C1 P1 119.25(14) ? C2 C1 C6 119.76(17) ? C6 C1 P1 120.93(14) ? C32 C38 C39 121.63(17) ? C37 C38 C32 116.62(17) ? C37 C38 C39 121.75(18) ? C7 C12 H12 119.9 ? C11 C12 H12 119.9 ? C11 C12 C7 120.13(17) ? C32 C33 C34 121.45(17) ? C35 C33 C32 116.53(18) ? C35 C33 C34 122.02(18) ? C1 C2 H2 120.0 ? C3 C2 C1 120.01(18) ? C3 C2 H2 120.0 ? C12 C7 P1 122.88(14) ? C12 C7 C8 119.00(17) ? C8 C7 P1 117.83(14) ? P2 C18 H18A 110.4 ? P2 C18 H18B 110.4 ? N2 C18 P2 106.75(12) ? N2 C18 H18A 110.4 ? N2 C18 H18B 110.4 ? H18A C18 H18B 108.6 ? N3 C31 Ni1 177.33(17) y C1 C6 H6 120.1 ? C5 C6 C1 119.74(18) ? C5 C6 H6 120.1 ? P1 C13 H13A 110.6 ? P1 C13 H13B 110.6 ? N1 C13 P1 105.48(11) ? N1 C13 H13A 110.6 ? N1 C13 H13B 110.6 ? H13A C13 H13B 108.8 ? C8 C9 H9 120.1 ? C10 C9 H9 120.1 ? C10 C9 C8 119.72(18) ? N1 C17 Ni1 120.68(13) ? N2 C17 Ni1 121.04(13) ? N2 C17 N1 118.13(16) ? C7 C8 H8 119.7 ? C9 C8 C7 120.51(18) ? C9 C8 H8 119.7 ? C33 C35 H35 119.4 ? C36 C35 C33 121.26(18) ? C36 C35 H35 119.4 ? C12 C11 H11 119.9 ? C10 C11 C12 120.25(18) ? C10 C11 H11 119.9 ? C9 C10 H10 119.8 ? C11 C10 C9 120.33(18) ? C11 C10 H10 119.8 ? C38 C37 H37 119.4 ? C36 C37 C38 121.15(19) ? C36 C37 H37 119.4 ? C26 C25 P2 118.84(14) ? C26 C25 C30 119.10(18) ? C30 C25 P2 121.95(16) ? C25 C26 H26 119.6 ? C27 C26 C25 120.79(18) ? C27 C26 H26 119.6 ? C25 C30 H30 120.1 ? C29 C30 C25 119.8(2) ? C29 C30 H30 120.1 ? C20 C19 P2 117.36(15) ? C24 C19 P2 123.23(17) ? C24 C19 C20 119.40(19) ? C3 C4 H4 119.6 ? C3 C4 C5 120.83(19) ? C5 C4 H4 119.6 ? C2 C3 H3 120.1 ? C4 C3 C2 119.87(19) ? C4 C3 H3 120.1 ? C35 C36 C37 120.48(18) ? C35 C36 H36 119.8 ? C37 C36 H36 119.8 ? N1 C14 H14A 109.8 ? N1 C14 H14B 109.8 ? N1 C14 C15 109.24(15) ? H14A C14 H14B 108.3 ? C15 C14 H14A 109.8 ? C15 C14 H14B 109.8 ? C38 C39 H39A 109.5 ? C38 C39 H39B 109.5 ? C38 C39 H39C 109.5 ? H39A C39 H39B 109.5 ? H39A C39 H39C 109.5 ? H39B C39 H39C 109.5 ? C27 C28 H28 120.0 ? C27 C28 C29 120.0(2) ? C29 C28 H28 120.0 ? C6 C5 H5 120.1 ? C4 C5 C6 119.78(19) ? C4 C5 H5 120.1 ? C26 C27 H27 120.1 ? C28 C27 C26 119.7(2) ? C28 C27 H27 120.1 ? C19 C20 H20 119.6 ? C21 C20 C19 120.8(2) ? C21 C20 H20 119.6 ? N2 C16 H16A 109.8 ? N2 C16 H16B 109.8 ? N2 C16 C15 109.58(16) ? H16A C16 H16B 108.2 ? C15 C16 H16A 109.8 ? C15 C16 H16B 109.8 ? C14 C15 H15A 109.8 ? C14 C15 H15B 109.8 ? C16 C15 C14 109.25(17) ? C16 C15 H15A 109.8 ? C16 C15 H15B 109.8 ? H15A C15 H15B 108.3 ? C33 C34 H34A 109.5 ? C33 C34 H34B 109.5 ? C33 C34 H34C 109.5 ? H34A C34 H34B 109.5 ? H34A C34 H34C 109.5 ? H34B C34 H34C 109.5 ? C30 C29 C28 120.59(19) ? C30 C29 H29 119.7 ? C28 C29 H29 119.7 ? C24 C23 H23 119.5 ? C22 C23 H23 119.5 ? C22 C23 C24 121.0(2) ? C20 C21 H21 120.3 ? C22 C21 C20 119.5(2) ? C22 C21 H21 120.3 ? C19 C24 C23 118.8(2) ? C19 C24 H24 120.6 ? C23 C24 H24 120.6 ? C23 C22 C21 120.5(2) ? C23 C22 H22 119.8 ? C21 C22 H22 119.8 ? H1A O1 H1B 104.4 ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_publ_flag Ni1 Cl1 2.4305(5) y Ni1 P1 2.1690(5) y Ni1 P2 2.1660(5) y Ni1 C31 1.8311(19) y Ni1 C17 1.9344(18) y P1 C1 1.8039(19) ? P1 C7 1.8074(18) ? P1 C13 1.8226(18) ? P2 C18 1.8276(19) ? P2 C25 1.811(2) ? P2 C19 1.814(2) ? P3 F6 1.596(9) ? P3 F5 1.600(9) ? P3 F3 1.613(8) ? P3 F2 1.610(8) ? P3 F4 1.600(9) ? P3 F1 1.601(8) ? P3 F3A 1.606(11) ? P3 F6A 1.601(11) ? P3 F5A 1.609(11) ? P3 F2A 1.600(11) ? P3 F4A 1.602(11) ? P3 F1A 1.593(10) ? N3 C32 1.405(2) ? N1 C13 1.452(2) y N1 C17 1.344(2) y N1 C14 1.472(2) ? N2 C17 1.335(2) y N2 C18 1.451(2) y N2 C16 1.475(2) ? N3 C31 1.161(2) y C32 C38 1.396(3) ? C32 C33 1.399(3) ? C1 C2 1.390(3) ? C1 C6 1.399(3) ? C38 C37 1.388(3) ? C38 C39 1.502(3) ? C12 H12 0.9300 ? C12 C7 1.398(3) ? C12 C11 1.384(3) ? C33 C35 1.387(3) ? C33 C34 1.500(3) ? C2 H2 0.9300 ? C2 C3 1.386(3) ? C7 C8 1.399(3) ? C18 H18A 0.9700 ? C18 H18B 0.9700 ? C6 H6 0.9300 ? C6 C5 1.387(3) ? C13 H13A 0.9700 ? C13 H13B 0.9700 ? C9 H9 0.9300 ? C9 C8 1.386(3) ? C9 C10 1.385(3) ? C8 H8 0.9300 ? C35 H35 0.9300 ? C35 C36 1.380(3) ? C11 H11 0.9300 ? C11 C10 1.383(3) ? C10 H10 0.9300 ? C37 H37 0.9300 ? C37 C36 1.382(3) ? C25 C26 1.389(3) ? C25 C30 1.399(3) ? C26 H26 0.9300 ? C26 C27 1.383(3) ? C30 H30 0.9300 ? C30 C29 1.377(3) ? C19 C20 1.400(3) ? C19 C24 1.390(3) ? C4 H4 0.9300 ? C4 C3 1.378(3) ? C4 C5 1.382(3) ? C3 H3 0.9300 ? C36 H36 0.9300 ? C14 H14A 0.9700 ? C14 H14B 0.9700 ? C14 C15 1.514(3) ? C39 H39A 0.9600 ? C39 H39B 0.9600 ? C39 H39C 0.9600 ? C28 H28 0.9300 ? C28 C27 1.379(3) ? C28 C29 1.387(3) ? C5 H5 0.9300 ? C27 H27 0.9300 ? C20 H20 0.9300 ? C20 C21 1.385(3) ? C16 H16A 0.9700 ? C16 H16B 0.9700 ? C16 C15 1.513(3) ? C15 H15A 0.9700 ? C15 H15B 0.9700 ? C34 H34A 0.9600 ? C34 H34B 0.9600 ? C34 H34C 0.9600 ? C29 H29 0.9300 ? C23 H23 0.9300 ? C23 C24 1.404(3) ? C23 C22 1.370(4) ? C21 H21 0.9300 ? C21 C22 1.376(4) ? C24 H24 0.9300 ? C22 H22 0.9300 ? O1 H1A 0.8504 ? O1 H1B 0.8497 ? 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_publ_flag C9 H9 F1 0.93 2.43 3.237(15) 145.3 yes C9 H9 F1A 0.93 2.49 3.342(19) 153.1 yes C14 H14A O1 0.97 2.48 3.278(4) 138.8 yes C20 H20 Cl1 0.93 2.80 3.567(2) 141.0 yes O1 H1B Cl1 0.85 2.30 3.148(3) 174.8 yes 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 Ni1 P1 C1 C2 18.36(17) Ni1 P1 C1 C6 -164.32(12) Ni1 P1 C7 C12 -110.89(14) Ni1 P1 C7 C8 62.89(15) Ni1 P1 C13 N1 36.09(12) Ni1 P2 C18 N2 -27.67(13) Ni1 P2 C25 C26 -5.68(17) Ni1 P2 C25 C30 170.53(14) Ni1 P2 C19 C20 -53.86(18) Ni1 P2 C19 C24 125.23(16) P1 C1 C2 C3 178.51(14) P1 C1 C6 C5 -178.20(15) P1 C7 C8 C9 -171.79(14) P2 C25 C26 C27 177.05(14) P2 C25 C30 C29 -176.95(16) P2 C19 C20 C21 -179.24(17) P2 C19 C24 C23 179.73(17) N3 C32 C38 C37 179.53(16) N3 C32 C38 C39 0.4(3) N3 C32 C33 C35 -178.99(16) N3 C32 C33 C34 0.8(3) N1 C14 C15 C16 -53.8(2) N2 C16 C15 C14 52.2(2) C32 C38 C37 C36 -0.5(3) C32 C33 C35 C36 -0.6(3) C1 P1 C7 C12 109.92(16) C1 P1 C7 C8 -76.30(15) C1 P1 C13 N1 164.62(12) C1 C2 C3 C4 -0.5(3) C1 C6 C5 C4 -0.1(3) C38 C32 C33 C35 0.5(3) C38 C32 C33 C34 -179.68(19) C38 C37 C36 C35 0.3(3) C12 C7 C8 C9 2.2(3) C12 C11 C10 C9 2.4(3) C33 C32 C38 C37 0.0(3) C33 C32 C38 C39 -179.05(18) C33 C35 C36 C37 0.3(3) C2 C1 C6 C5 -0.9(3) C7 P1 C1 C2 151.72(14) C7 P1 C1 C6 -30.96(17) C7 P1 C13 N1 -80.73(13) C7 C12 C11 C10 -1.0(3) C18 P2 C25 C26 -114.76(15) C18 P2 C25 C30 61.46(18) C18 P2 C19 C20 57.98(18) C18 P2 C19 C24 -122.93(18) C18 N2 C17 Ni1 -5.4(2) C18 N2 C17 N1 170.37(16) C18 N2 C16 C15 165.17(17) C6 C1 C2 C3 1.2(3) C13 P1 C1 C2 -93.55(15) C13 P1 C1 C6 83.77(16) C13 P1 C7 C12 -2.98(18) C13 P1 C7 C8 170.80(14) C13 N1 C17 Ni1 5.3(2) C13 N1 C17 N2 -170.45(16) C13 N1 C14 C15 -163.90(17) C17 N1 C13 P1 -29.47(19) C17 N1 C14 C15 32.5(3) C17 N2 C18 P2 23.4(2) C17 N2 C16 C15 -29.0(3) C8 C9 C10 C11 -1.5(3) C11 C12 C7 P1 172.42(14) C11 C12 C7 C8 -1.3(3) C10 C9 C8 C7 -0.9(3) C25 P2 C18 N2 91.66(14) C25 P2 C19 C20 169.40(15) C25 P2 C19 C24 -11.5(2) C25 C26 C27 C28 -0.5(3) C25 C30 C29 C28 0.5(3) C26 C25 C30 C29 -0.7(3) C30 C25 C26 C27 0.7(3) C19 P2 C18 N2 -153.56(13) C19 P2 C25 C26 133.90(15) C19 P2 C25 C30 -49.89(19) C19 C20 C21 C22 -0.9(3) C3 C4 C5 C6 0.8(3) C14 N1 C13 P1 165.93(13) C14 N1 C17 Ni1 168.61(14) C14 N1 C17 N2 -7.1(3) C39 C38 C37 C36 178.63(19) C5 C4 C3 C2 -0.5(3) C27 C28 C29 C30 -0.3(3) C20 C19 C24 C23 -1.2(3) C20 C21 C22 C23 -0.2(4) C16 N2 C18 P2 -170.03(14) C16 N2 C17 Ni1 -170.47(14) C16 N2 C17 N1 5.2(3) C34 C33 C35 C36 179.6(2) C29 C28 C27 C26 0.3(3) C24 C19 C20 C21 1.6(3) C24 C23 C22 C21 0.6(4) C22 C23 C24 C19 0.1(3) _cod_database_fobs_code 2021643