#------------------------------------------------------------------------------ #$Date: 2023-11-16 01:38:50 +0200 (Thu, 16 Nov 2023) $ #$Revision: 287628 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/24/77/7247741.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_7247741 loop_ _publ_author_name 'Srivastava, Devyani' 'Kushwaha, Aparna' 'Kociok-K\"ohn, Gabriele' 'Gosavi, Suresh' 'Chauhan, Ratna' 'Kumar, Abhinav' 'Muddassir, Mohd.' _publ_section_title ; Supramolecular Frameworks and Electrocatalytic Properties of Two New Structurally Diverse Tertiary Phosphane Appended Nickel(II) and Copper(I) Thiosquarates ; _journal_name_full CrystEngComm _journal_paper_doi 10.1039/D3CE00817G _journal_year 2023 _chemical_formula_moiety 'C37.1 H33.25 Cl0.15 Ni O5.55 P2 S1.85, 0.06(C H2 Cl2), 0.09(C H4 O)' _chemical_formula_sum 'C37.25 H33.73 Cl0.27 Ni O5.64 P2 S1.85' _chemical_formula_weight 761.14 _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_Hall '-P 1' _space_group_name_H-M_alt 'P -1' _atom_sites_solution_hydrogens mixed _audit_creation_date 2023-10-10 _audit_creation_method ; Olex2 1.5-dev (compiled 2023.10.06 svn.rcf4196af for OlexSys, GUI svn.r6697) ; _audit_update_record ; 2023-11-01 deposited with the CCDC. 2023-11-15 downloaded from the CCDC. ; _cell_angle_alpha 76.6204(11) _cell_angle_beta 85.3079(11) _cell_angle_gamma 81.3483(10) _cell_formula_units_Z 2 _cell_length_a 9.65800(14) _cell_length_b 10.04345(11) _cell_length_c 18.7630(3) _cell_measurement_reflns_used 17838 _cell_measurement_temperature 150(2) _cell_measurement_theta_max 72.6790 _cell_measurement_theta_min 4.6430 _cell_volume 1748.37(4) _computing_cell_refinement 'CrysAlisPro 1.171.42.56a (Rigaku OD, 2022)' _computing_data_collection 'CrysAlisPro 1.171.42.56a (Rigaku OD, 2022)' _computing_data_reduction 'CrysAlisPro 1.171.42.56a (Rigaku OD, 2022)' _computing_molecular_graphics 'Olex2 1.5-dev (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 1.5-dev (Dolomanov et al., 2009)' _computing_structure_refinement 'SHELXL 2018/3 (Sheldrick, 2015)' _computing_structure_solution ; SHELXT Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122. ; _diffrn_ambient_temperature 150.15 _diffrn_detector_area_resol_mean 8.1150 _diffrn_detector_type EosS2 _diffrn_measured_fraction_theta_full 1.000 _diffrn_measured_fraction_theta_max 0.993 _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'SuperNova, Dual, Cu at home/near, EosS2' _diffrn_measurement_method '\w scans' _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.54184 _diffrn_reflns_av_R_equivalents 0.0363 _diffrn_reflns_av_unetI/netI 0.0251 _diffrn_reflns_Laue_measured_fraction_full 1.000 _diffrn_reflns_Laue_measured_fraction_max 0.993 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_number 35359 _diffrn_reflns_point_group_measured_fraction_full 1.000 _diffrn_reflns_point_group_measured_fraction_max 0.993 _diffrn_reflns_theta_full 67.684 _diffrn_reflns_theta_max 72.868 _diffrn_reflns_theta_min 4.568 _exptl_absorpt_coefficient_mu 3.258 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_correction_T_min 0.446 _exptl_absorpt_correction_type gaussian _exptl_absorpt_process_details ; CrysAlisPro 1.171.42.56a (Rigaku Oxford Diffraction, 2022) Numerical absorption correction based on gaussian integration over a multifaceted crystal model Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour orange _exptl_crystal_colour_primary orange _exptl_crystal_density_diffrn 1.446 _exptl_crystal_description plate _exptl_crystal_F_000 789 _exptl_crystal_size_max 0.287 _exptl_crystal_size_mid 0.107 _exptl_crystal_size_min 0.042 _refine_diff_density_max 0.578 _refine_diff_density_min -0.367 _refine_diff_density_rms 0.057 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.082 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 467 _refine_ls_number_reflns 6914 _refine_ls_number_restraints 5 _refine_ls_restrained_S_all 1.081 _refine_ls_R_factor_all 0.0405 _refine_ls_R_factor_gt 0.0367 _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^)+(0.0418P)^2^+1.4101P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0928 _refine_ls_wR_factor_ref 0.0950 _reflns_Friedel_coverage 0.000 _reflns_number_gt 6347 _reflns_number_total 6914 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d3ce00817g2.cif _cod_data_source_block s23gkk1a _cod_database_code 7247741 _shelx_shelxl_version_number 2018/3 _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_max 0.875 _shelx_estimated_absorpt_t_min 0.455 _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups, All C(H,H) groups At 1.5 times of: All C(H,H,H) groups, All O(H) groups 2. Restrained distances O10-C40 1.42 with sigma of 0.02 Cl2-C39 \\sim Cl7-C39 with sigma of 0.001 3. Uiso/Uaniso restraints and constraints C39 \\sim Cl7 \\sim Cl2: within 2A with sigma of 0.001 and sigma for terminal atoms of 0.002 within 2A O10 \\sim C40: within 2A with sigma of 0.001 and sigma for terminal atoms of 0.002 within 2A Uanis(Cl1) = Uanis(S1) 4. Others Fixed Sof: O1(0.85) O2(0.85) O3(0.85) S1(0.85) C27(0.85) C28(0.85) C29(0.85) C30(0.85) C31(0.85) H31A(0.85) H31B(0.85) C32(0.85) H32A(0.85) H32B(0.85) H32C(0.85) Cl1(0.15) Cl7(0.06) Cl2(0.06) C39(0.06) H39A(0.06) H39B(0.06) O10(0.09) H10A(0.09) C40(0.09) H40A(0.09) H40B(0.09) H40C(0.09) 5.a Riding coordinates: O10(H10A), C40(H40A,H40B,H40C) 5.b Secondary CH2 refined with riding coordinates: C1(H1A,H1B), C2(H2A,H2B), C31(H31A,H31B), C37(H37A,H37B), C39(H39A,H39B) 5.c Aromatic/amide H refined with riding coordinates: C4(H4), C5(H5), C6(H6), C7(H7), C8(H8), C10(H10), C11(H11), C12(H12), C13(H13), C14(H14), C16(H16), C17(H17), C18(H18), C19(H19), C20(H20), C22(H22), C23(H23), C24(H24), C25(H25), C26(H26) 5.d Idealised Me refined as rotating group: C32(H32A,H32B,H32C), C38(H38A,H38B,H38C) ; _shelx_res_file ; TITL s23gkk1a_auto in P-1 s23gkk1a.res created by SHELXL-2018/3 at 10:58:17 on 10-Oct-2023 REM P-1 (#2 in standard setting) CELL 1.54184 9.658 10.04345 18.763 76.6204 85.3079 81.3483 ZERR 2 0.00014 0.00011 0.0003 0.0011 0.0011 0.001 LATT 1 SFAC C H Cl Ni O P S UNIT 74.5 67.46 0.54 2 11.28 4 3.7 EADP Cl1 S1 SADI 0.001 Cl2 C39 Cl7 C39 SIMU 0.001 0.002 2 C39 Cl7 Cl2 SIMU 0.001 0.002 2 O10 C40 DFIX 1.42 O10 C40 L.S. 12 PLAN 30 SIZE 0.042 0.107 0.287 TEMP -123 CONF BOND $H LIST 4 fmap 2 acta REM REM REM > REM REM > REM > REM REM WGHT 0.041800 1.410100 FVAR 5.29175 NI 4 0.725451 0.442088 0.770892 11.00000 0.01450 0.01347 = 0.02414 -0.00142 -0.00346 -0.00115 P1 6 0.518872 0.374348 0.796137 11.00000 0.01392 0.01633 = 0.02589 -0.00326 -0.00345 -0.00129 P2 6 0.807628 0.238227 0.831909 11.00000 0.01457 0.01414 = 0.02303 -0.00192 -0.00337 -0.00036 S2 7 0.619647 0.648523 0.711242 11.00000 0.02350 0.01593 = 0.02714 -0.00167 -0.00587 0.00063 PART 1 O1 5 0.768672 0.523151 0.581527 10.85000 0.04420 0.06709 = 0.03078 -0.01149 -0.00171 -0.03316 O2 5 1.004246 0.686931 0.476128 10.85000 0.04975 0.06341 = 0.02536 -0.00144 -0.00106 -0.02811 O3 5 1.178124 0.660640 0.624222 10.85000 0.02221 0.03867 = 0.02933 0.00029 -0.00234 -0.00945 PART 0 O4 5 0.709839 0.585282 0.891302 11.00000 0.02945 0.03438 = 0.03506 0.00091 -0.00544 0.00836 O5 5 0.514880 0.862208 0.929434 11.00000 0.03347 0.03783 = 0.04039 -0.01708 -0.00793 0.00073 O6 5 0.417497 0.949244 0.766688 11.00000 0.05719 0.02492 = 0.04782 -0.01213 -0.02358 0.01814 C1 1 0.670551 0.178149 0.900028 11.00000 0.01725 0.02019 = 0.02571 -0.00126 -0.00028 -0.00141 AFIX 23 H1A 2 0.694671 0.078528 0.922015 11.00000 -1.20000 H1B 2 0.660900 0.229531 0.939671 11.00000 -1.20000 AFIX 0 C2 1 0.533844 0.203383 0.860597 11.00000 0.02026 0.01805 = 0.03121 -0.00049 -0.00118 -0.00442 AFIX 23 H2A 2 0.453347 0.200133 0.896898 11.00000 -1.20000 H2B 2 0.532215 0.130231 0.833346 11.00000 -1.20000 AFIX 0 C3 1 0.390414 0.487659 0.838350 11.00000 0.01286 0.01942 = 0.03229 -0.00559 -0.00145 -0.00310 C4 1 0.391578 0.485433 0.912730 11.00000 0.02060 0.02279 = 0.03017 -0.00245 -0.00227 -0.00320 AFIX 43 H4 2 0.453365 0.417182 0.943101 11.00000 -1.20000 AFIX 0 C5 1 0.302915 0.582433 0.942679 11.00000 0.03131 0.03126 = 0.03057 -0.00899 0.00434 -0.00732 AFIX 43 H5 2 0.304653 0.580938 0.993411 11.00000 -1.20000 AFIX 0 C6 1 0.211717 0.681615 0.898761 11.00000 0.02431 0.02729 = 0.04696 -0.01283 0.00503 0.00020 AFIX 43 H6 2 0.152060 0.748874 0.919227 11.00000 -1.20000 AFIX 0 C7 1 0.207659 0.682569 0.825317 11.00000 0.02107 0.02771 = 0.04611 -0.00796 -0.00656 0.00391 AFIX 43 H7 2 0.143900 0.749570 0.795498 11.00000 -1.20000 AFIX 0 C8 1 0.296300 0.586091 0.794772 11.00000 0.01984 0.02493 = 0.03275 -0.00673 -0.00711 -0.00057 AFIX 43 H8 2 0.292914 0.587051 0.744194 11.00000 -1.20000 AFIX 0 C9 1 0.433277 0.353240 0.717486 11.00000 0.02038 0.01830 = 0.03210 -0.00763 -0.00653 0.00117 C10 1 0.301394 0.308898 0.727612 11.00000 0.02022 0.02602 = 0.04144 -0.01129 -0.00315 -0.00202 AFIX 43 H10 2 0.257711 0.288058 0.775364 11.00000 -1.20000 AFIX 0 C11 1 0.234790 0.295522 0.667654 11.00000 0.02518 0.03002 = 0.05699 -0.01901 -0.01388 0.00166 AFIX 43 H11 2 0.145179 0.265051 0.674491 11.00000 -1.20000 AFIX 0 C12 1 0.296603 0.325739 0.598427 11.00000 0.04375 0.03053 = 0.04625 -0.01388 -0.02452 0.00493 AFIX 43 H12 2 0.249679 0.316711 0.557574 11.00000 -1.20000 AFIX 0 C13 1 0.427829 0.369525 0.588187 11.00000 0.05104 0.03228 = 0.02980 -0.00520 -0.00803 -0.00531 AFIX 43 H13 2 0.470864 0.390225 0.540275 11.00000 -1.20000 AFIX 0 C14 1 0.496234 0.383124 0.647672 11.00000 0.03165 0.02591 = 0.03221 -0.00526 -0.00296 -0.00639 AFIX 43 H14 2 0.586175 0.412897 0.640591 11.00000 -1.20000 AFIX 0 C15 1 0.963229 0.218078 0.883519 11.00000 0.01684 0.02101 = 0.02307 0.00042 -0.00344 -0.00160 C16 1 1.069667 0.106228 0.886406 11.00000 0.02165 0.02165 = 0.03629 -0.00373 -0.00710 -0.00034 AFIX 43 H16 2 1.064605 0.039170 0.858693 11.00000 -1.20000 AFIX 0 C17 1 1.182704 0.093305 0.929805 11.00000 0.02129 0.03080 = 0.03872 0.00028 -0.00813 0.00146 AFIX 43 H17 2 1.254656 0.016969 0.931893 11.00000 -1.20000 AFIX 0 C18 1 1.191305 0.190695 0.969991 11.00000 0.01928 0.04103 = 0.02738 0.00212 -0.00612 -0.00719 AFIX 43 H18 2 1.268348 0.180724 1.000077 11.00000 -1.20000 AFIX 0 C19 1 1.087359 0.302883 0.966312 11.00000 0.02590 0.03892 = 0.03034 -0.00981 -0.00393 -0.00873 AFIX 43 H19 2 1.093739 0.370155 0.993690 11.00000 -1.20000 AFIX 0 C20 1 0.974253 0.317713 0.923044 11.00000 0.02079 0.02762 = 0.03012 -0.00662 -0.00290 0.00042 AFIX 43 H20 2 0.904072 0.395687 0.920219 11.00000 -1.20000 AFIX 0 C21 1 0.840736 0.112441 0.774946 11.00000 0.01303 0.01881 = 0.03098 -0.00712 -0.00325 -0.00117 C22 1 0.842832 -0.029341 0.805181 11.00000 0.01859 0.01942 = 0.03724 -0.00432 -0.00050 -0.00282 AFIX 43 H22 2 0.823679 -0.061085 0.856284 11.00000 -1.20000 AFIX 0 C23 1 0.872905 -0.122947 0.760326 11.00000 0.02077 0.01924 = 0.05531 -0.01236 -0.00078 -0.00429 AFIX 43 H23 2 0.874348 -0.218971 0.780678 11.00000 -1.20000 AFIX 0 C24 1 0.900656 -0.076873 0.686369 11.00000 0.03734 0.03665 = 0.05296 -0.02717 0.00291 -0.00442 AFIX 43 H24 2 0.920854 -0.141427 0.655824 11.00000 -1.20000 AFIX 0 C25 1 0.899434 0.062584 0.656039 11.00000 0.05321 0.04027 = 0.03306 -0.01454 0.00372 -0.00749 AFIX 43 H25 2 0.919848 0.093355 0.604982 11.00000 -1.20000 AFIX 0 C26 1 0.868346 0.157634 0.700264 11.00000 0.02902 0.02466 = 0.03122 -0.00611 -0.00169 -0.00433 AFIX 43 H26 2 0.866007 0.253549 0.679341 11.00000 -1.20000 AFIX 0 PART 1 S1 7 0.942648 0.494892 0.747301 10.85000 0.01732 0.02138 = 0.01937 0.00145 -0.00159 -0.00479 C27 1 0.958075 0.559915 0.654605 10.85000 0.01955 0.01798 = 0.02827 -0.00615 -0.00038 -0.00107 C28 1 0.873090 0.562415 0.590520 10.85000 0.02994 0.03473 = 0.02780 -0.00819 0.00405 -0.01275 C29 1 0.986268 0.638073 0.540525 10.85000 0.03198 0.03763 = 0.02342 -0.00565 -0.00227 -0.01229 C30 1 1.060396 0.625005 0.608688 10.85000 0.02127 0.02262 = 0.02512 -0.00425 -0.00307 -0.00237 C31 1 1.263066 0.727583 0.561263 10.85000 0.02762 0.05978 = 0.03765 -0.00114 0.00610 -0.02244 AFIX 23 H31A 2 1.258486 0.684262 0.519333 10.85000 -1.20000 H31B 2 1.362209 0.715100 0.574270 10.85000 -1.20000 AFIX 0 C32 1 1.209593 0.878091 0.540043 10.85000 0.06101 0.05974 = 0.04216 0.00256 -0.00669 -0.02972 AFIX 137 H32A 2 1.269188 0.922915 0.499502 10.85000 -1.50000 H32B 2 1.211315 0.920004 0.582167 10.85000 -1.50000 H32C 2 1.113187 0.890115 0.524535 10.85000 -1.50000 AFIX 0 PART 2 CL1 3 0.942215 0.504543 0.734061 10.15000 0.01732 0.02138 = 0.01937 0.00145 -0.00159 -0.00479 PART 0 C33 1 0.581669 0.723853 0.783981 11.00000 0.02026 0.01644 = 0.03199 -0.00261 -0.00532 -0.00398 C34 1 0.630366 0.681690 0.859276 11.00000 0.01878 0.02239 = 0.03240 -0.00361 -0.00278 -0.00286 C35 1 0.541201 0.810302 0.876996 11.00000 0.02230 0.02406 = 0.03570 -0.00783 -0.00624 -0.00442 C36 1 0.502139 0.842233 0.800489 11.00000 0.02611 0.01872 = 0.03884 -0.00665 -0.00998 0.00097 C37 1 0.388681 0.949791 0.691030 11.00000 0.06005 0.03073 = 0.05007 -0.00586 -0.02163 0.01214 AFIX 23 H37A 2 0.378245 0.855163 0.687207 11.00000 -1.20000 H37B 2 0.299866 1.010414 0.677186 11.00000 -1.20000 AFIX 0 C38 1 0.503612 0.999546 0.641250 11.00000 0.07291 0.03501 = 0.08006 -0.00130 -0.02036 0.00328 AFIX 137 H38A 2 0.479163 1.009574 0.590429 11.00000 -1.50000 H38B 2 0.588927 0.933184 0.651207 11.00000 -1.50000 H38C 2 0.519820 1.089248 0.648730 11.00000 -1.50000 AFIX 0 PART 2 CL7 3 1.229239 0.726648 0.575587 10.06000 0.06499 CL2 3 0.957118 0.754190 0.521310 10.06000 0.06500 C39 1 1.098563 0.652959 0.556310 10.06000 0.06487 AFIX 23 H39A 2 1.068273 0.590518 0.602037 10.06000 -1.20000 H39B 2 1.136298 0.594467 0.521452 10.06000 -1.20000 AFIX 0 PART 3 O10 5 0.899853 0.575219 0.578322 10.09000 0.07427 AFIX 3 H10A 2 0.844163 0.636749 0.552812 10.09000 -1.50000 AFIX 0 C40 1 1.029794 0.632144 0.568327 10.09000 0.07445 AFIX 3 H40A 2 1.021774 0.709104 0.593057 10.09000 -1.50000 H40B 2 1.062194 0.662844 0.517077 10.09000 -1.50000 H40C 2 1.097184 0.555894 0.593057 10.09000 -1.50000 AFIX 0 HKLF 4 REM s23gkk1a_auto in P-1 REM wR2 = 0.0950, GooF = S = 1.082, Restrained GooF = 1.081 for all data REM R1 = 0.0367 for 6347 Fo > 4sig(Fo) and 0.0405 for all 6914 data REM 467 parameters refined using 5 restraints END WGHT 0.0418 1.4100 REM Highest difference peak 0.578, deepest hole -0.367, 1-sigma level 0.057 Q1 1 0.7486 0.4553 0.7151 11.00000 0.05 0.58 Q2 1 0.7190 0.4185 0.8279 11.00000 0.05 0.51 Q3 1 0.9622 0.5167 0.6907 11.00000 0.05 0.43 Q4 1 0.5006 0.9801 0.7572 11.00000 0.05 0.43 Q5 1 0.5143 0.3823 0.7467 11.00000 0.05 0.42 Q6 1 0.4858 0.3614 0.7536 11.00000 0.05 0.40 Q7 1 0.4684 0.9988 0.6925 11.00000 0.05 0.38 Q8 1 0.6333 0.6740 0.6552 11.00000 0.05 0.36 Q9 1 0.9368 0.4840 0.7967 11.00000 0.05 0.34 Q10 1 0.5971 0.6598 0.7583 11.00000 0.05 0.34 Q11 1 0.9005 0.2266 0.8598 11.00000 0.05 0.32 Q12 1 0.8318 0.1623 0.8007 11.00000 0.05 0.32 Q13 1 1.0429 0.7855 0.5277 11.00000 0.05 0.32 Q14 1 0.7831 0.2206 0.8869 11.00000 0.05 0.31 Q15 1 0.7274 0.2055 0.8694 11.00000 0.05 0.30 Q16 1 0.6216 0.3935 0.8044 11.00000 0.05 0.29 Q17 1 0.9539 0.2417 0.9184 11.00000 0.05 0.29 Q18 1 1.0847 0.6522 0.4880 11.00000 0.05 0.28 Q19 1 0.5894 0.7394 0.8773 11.00000 0.05 0.27 Q20 1 0.3241 0.9345 0.6509 11.00000 0.05 0.27 Q21 1 0.5587 0.6418 0.6724 11.00000 0.05 0.27 Q22 1 0.6495 0.4271 0.7467 11.00000 0.05 0.26 Q23 1 0.8547 0.0551 0.7843 11.00000 0.05 0.26 Q24 1 0.8617 0.4524 0.7515 11.00000 0.05 0.26 Q25 1 0.3796 0.4797 0.8760 11.00000 0.05 0.26 Q26 1 0.4579 0.3697 0.6851 11.00000 0.05 0.26 Q27 1 0.6369 0.7067 0.8113 11.00000 0.05 0.25 Q28 1 0.5122 0.8400 0.8411 11.00000 0.05 0.25 Q29 1 0.9071 0.5392 0.6371 11.00000 0.05 0.24 Q30 1 0.5485 0.7847 0.7837 11.00000 0.05 0.24 ; _shelx_res_checksum 71707 _olex2_submission_special_instructions 'No special instructions were received' _oxdiff_exptl_absorpt_empirical_details ; Empirical correction (ABSPACK) includes: - Absorption correction using spherical harmonics - Frame scaling ; loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, -z' 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 Ni Ni 0.72545(3) 0.44209(3) 0.77089(2) 0.01776(9) Uani 1 1 d . . . . . P1 P 0.51887(5) 0.37435(5) 0.79614(3) 0.01889(11) Uani 1 1 d . . . . . P2 P 0.80763(5) 0.23823(5) 0.83191(3) 0.01764(11) Uani 1 1 d . . . . . S2 S 0.61965(5) 0.64852(5) 0.71124(3) 0.02279(11) Uani 1 1 d . . . . . O1 O 0.7687(2) 0.5232(3) 0.58153(11) 0.0446(5) Uani 0.85 1 d . . P A 1 O2 O 1.0042(2) 0.6869(2) 0.47613(11) 0.0455(5) Uani 0.85 1 d . . P A 1 O3 O 1.17812(19) 0.6606(2) 0.62422(10) 0.0307(4) Uani 0.85 1 d . . P A 1 O4 O 0.70984(17) 0.58528(17) 0.89130(9) 0.0355(4) Uani 1 1 d . . . . . O5 O 0.51488(18) 0.86221(17) 0.92943(9) 0.0361(4) Uani 1 1 d . . . . . O6 O 0.4175(2) 0.94924(17) 0.76669(10) 0.0440(5) Uani 1 1 d . . . . . C1 C 0.6706(2) 0.1781(2) 0.90003(11) 0.0218(4) Uani 1 1 d . . . . . H1A H 0.694671 0.078528 0.922015 0.026 Uiso 1 1 calc R U . . . H1B H 0.660900 0.229531 0.939671 0.026 Uiso 1 1 calc R U . . . C2 C 0.5338(2) 0.2034(2) 0.86060(11) 0.0238(4) Uani 1 1 d . . . . . H2A H 0.453347 0.200133 0.896898 0.029 Uiso 1 1 calc R U . . . H2B H 0.532215 0.130231 0.833346 0.029 Uiso 1 1 calc R U . . . C3 C 0.3904(2) 0.4877(2) 0.83835(11) 0.0214(4) Uani 1 1 d . . . . . C4 C 0.3916(2) 0.4854(2) 0.91273(12) 0.0250(4) Uani 1 1 d . . . . . H4 H 0.453365 0.417182 0.943101 0.030 Uiso 1 1 calc R U . . . C5 C 0.3029(2) 0.5824(2) 0.94268(13) 0.0307(5) Uani 1 1 d . . . . . H5 H 0.304653 0.580938 0.993411 0.037 Uiso 1 1 calc R U . . . C6 C 0.2117(2) 0.6816(2) 0.89876(14) 0.0329(5) Uani 1 1 d . . . . . H6 H 0.152060 0.748874 0.919227 0.039 Uiso 1 1 calc R U . . . C7 C 0.2077(2) 0.6826(2) 0.82532(14) 0.0322(5) Uani 1 1 d . . . . . H7 H 0.143900 0.749570 0.795498 0.039 Uiso 1 1 calc R U . . . C8 C 0.2963(2) 0.5861(2) 0.79477(12) 0.0257(4) Uani 1 1 d . . . . . H8 H 0.292914 0.587051 0.744194 0.031 Uiso 1 1 calc R U . . . C9 C 0.4333(2) 0.3532(2) 0.71749(12) 0.0234(4) Uani 1 1 d . . . . . C10 C 0.3014(2) 0.3089(2) 0.72761(13) 0.0286(5) Uani 1 1 d . . . . . H10 H 0.257711 0.288058 0.775364 0.034 Uiso 1 1 calc R U . . . C11 C 0.2348(3) 0.2955(2) 0.66765(15) 0.0358(5) Uani 1 1 d . . . . . H11 H 0.145179 0.265051 0.674491 0.043 Uiso 1 1 calc R U . . . C12 C 0.2966(3) 0.3257(2) 0.59843(14) 0.0391(6) Uani 1 1 d . . . . . H12 H 0.249679 0.316711 0.557574 0.047 Uiso 1 1 calc R U . . . C13 C 0.4278(3) 0.3695(2) 0.58819(13) 0.0377(6) Uani 1 1 d . . . . . H13 H 0.470864 0.390225 0.540275 0.045 Uiso 1 1 calc R U . . . C14 C 0.4962(3) 0.3831(2) 0.64767(12) 0.0298(5) Uani 1 1 d . . . . . H14 H 0.586175 0.412897 0.640591 0.036 Uiso 1 1 calc R U . . . C15 C 0.9632(2) 0.2181(2) 0.88352(11) 0.0211(4) Uani 1 1 d . . . . . C16 C 1.0697(2) 0.1062(2) 0.88641(12) 0.0269(4) Uani 1 1 d . . . . . H16 H 1.064605 0.039170 0.858693 0.032 Uiso 1 1 calc R U . . . C17 C 1.1827(2) 0.0933(2) 0.92980(13) 0.0317(5) Uani 1 1 d . . . . . H17 H 1.254656 0.016969 0.931893 0.038 Uiso 1 1 calc R U . . . C18 C 1.1913(2) 0.1907(2) 0.96999(12) 0.0302(5) Uani 1 1 d . . . . . H18 H 1.268348 0.180724 1.000077 0.036 Uiso 1 1 calc R U . . . C19 C 1.0874(2) 0.3029(2) 0.96631(12) 0.0308(5) Uani 1 1 d . . . . . H19 H 1.093739 0.370155 0.993690 0.037 Uiso 1 1 calc R U . . . C20 C 0.9743(2) 0.3177(2) 0.92304(12) 0.0264(4) Uani 1 1 d . . . . . H20 H 0.904072 0.395687 0.920219 0.032 Uiso 1 1 calc R U . . . C21 C 0.8407(2) 0.11244(19) 0.77495(11) 0.0207(4) Uani 1 1 d . . . . . C22 C 0.8428(2) -0.0293(2) 0.80518(12) 0.0254(4) Uani 1 1 d . . . . . H22 H 0.823679 -0.061085 0.856284 0.031 Uiso 1 1 calc R U . . . C23 C 0.8729(2) -0.1229(2) 0.76033(14) 0.0310(5) Uani 1 1 d . . . . . H23 H 0.874348 -0.218971 0.780678 0.037 Uiso 1 1 calc R U . . . C24 C 0.9007(3) -0.0769(3) 0.68637(15) 0.0398(6) Uani 1 1 d . . . . . H24 H 0.920854 -0.141427 0.655824 0.048 Uiso 1 1 calc R U . . . C25 C 0.8994(3) 0.0626(3) 0.65604(14) 0.0413(6) Uani 1 1 d . . . . . H25 H 0.919848 0.093355 0.604982 0.050 Uiso 1 1 calc R U . . . C26 C 0.8683(2) 0.1576(2) 0.70026(12) 0.0282(4) Uani 1 1 d . . . . . H26 H 0.866007 0.253549 0.679341 0.034 Uiso 1 1 calc R U . . . S1 S 0.9426(3) 0.4949(2) 0.74730(7) 0.0201(3) Uani 0.85 1 d . . P A 1 C27 C 0.9581(2) 0.5599(2) 0.65460(13) 0.0220(5) Uani 0.85 1 d . . P A 1 C28 C 0.8731(4) 0.5624(4) 0.5905(2) 0.0300(8) Uani 0.85 1 d . . P A 1 C29 C 0.9863(3) 0.6381(3) 0.54052(15) 0.0303(6) Uani 0.85 1 d . . P A 1 C30 C 1.0604(3) 0.6250(2) 0.60869(14) 0.0231(5) Uani 0.85 1 d . . P A 1 C31 C 1.2631(4) 0.7276(5) 0.5613(2) 0.0420(10) Uani 0.85 1 d . . P A 1 H31A H 1.258486 0.684262 0.519333 0.050 Uiso 0.85 1 calc R U P A 1 H31B H 1.362209 0.715100 0.574270 0.050 Uiso 0.85 1 calc R U P A 1 C32 C 1.2096(4) 0.8781(4) 0.54004(19) 0.0541(9) Uani 0.85 1 d . . P A 1 H32A H 1.269188 0.922915 0.499502 0.081 Uiso 0.85 1 calc R U P A 1 H32B H 1.211315 0.920004 0.582167 0.081 Uiso 0.85 1 calc R U P A 1 H32C H 1.113187 0.890115 0.524535 0.081 Uiso 0.85 1 calc R U P A 1 Cl1 Cl 0.9422(16) 0.5045(15) 0.7341(6) 0.0201(3) Uani 0.15 1 d . . P A 2 C33 C 0.5817(2) 0.72385(19) 0.78398(12) 0.0230(4) Uani 1 1 d . . . . . C34 C 0.6304(2) 0.6817(2) 0.85928(12) 0.0248(4) Uani 1 1 d . . . . . C35 C 0.5412(2) 0.8103(2) 0.87700(12) 0.0268(4) Uani 1 1 d . . . . . C36 C 0.5021(2) 0.8422(2) 0.80049(13) 0.0278(5) Uani 1 1 d . . . . . C37 C 0.3887(3) 0.9498(3) 0.69103(16) 0.0483(7) Uani 1 1 d . . . . . H37A H 0.378245 0.855163 0.687207 0.058 Uiso 1 1 calc R U . . . H37B H 0.299866 1.010414 0.677186 0.058 Uiso 1 1 calc R U . . . C38 C 0.5036(4) 0.9995(3) 0.6413(2) 0.0647(9) Uani 1 1 d . . . . . H38A H 0.479163 1.009574 0.590429 0.097 Uiso 1 1 calc R U . . . H38B H 0.588927 0.933184 0.651207 0.097 Uiso 1 1 calc R U . . . H38C H 0.519820 1.089248 0.648730 0.097 Uiso 1 1 calc R U . . . Cl7 Cl 1.229(2) 0.727(2) 0.5756(13) 0.065(4) Uiso 0.06 1 d D U P B 2 Cl2 Cl 0.9571(15) 0.7542(15) 0.5213(8) 0.065(3) Uiso 0.06 1 d D U P B 2 C39 C 1.0986(18) 0.653(6) 0.556(2) 0.065(3) Uiso 0.06 1 d D U P B 2 H39A H 1.068273 0.590518 0.602037 0.078 Uiso 0.06 1 calc R U P B 2 H39B H 1.136298 0.594467 0.521452 0.078 Uiso 0.06 1 calc R U P B 2 O10 O 0.900(5) 0.575(5) 0.578(3) 0.074(11) Uiso 0.09 1 d D U P C 3 H10A H 0.844163 0.636749 0.552812 0.111 Uiso 0.09 1 d R U P C 3 C40 C 1.030(5) 0.632(6) 0.568(3) 0.074(11) Uiso 0.09 1 d D U P C 3 H40A H 1.021774 0.709104 0.593057 0.112 Uiso 0.09 1 d R U P C 3 H40B H 1.062194 0.662844 0.517077 0.112 Uiso 0.09 1 d R U P C 3 H40C H 1.097184 0.555894 0.593057 0.112 Uiso 0.09 1 d R U P C 3 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 Ni 0.01450(17) 0.01347(16) 0.02414(18) -0.00142(12) -0.00346(13) -0.00115(12) P1 0.0139(2) 0.0163(2) 0.0259(2) -0.00326(18) -0.00345(18) -0.00129(17) P2 0.0146(2) 0.0141(2) 0.0230(2) -0.00192(17) -0.00337(17) -0.00036(17) S2 0.0235(3) 0.0159(2) 0.0271(2) -0.00167(17) -0.00587(19) 0.00063(18) O1 0.0442(13) 0.0671(15) 0.0308(10) -0.0115(10) -0.0017(9) -0.0332(11) O2 0.0498(13) 0.0634(14) 0.0254(10) -0.0014(9) -0.0011(9) -0.0281(11) O3 0.0222(9) 0.0387(10) 0.0293(9) 0.0003(8) -0.0023(7) -0.0094(8) O4 0.0295(9) 0.0344(8) 0.0351(9) 0.0009(7) -0.0054(7) 0.0084(7) O5 0.0335(9) 0.0378(9) 0.0404(9) -0.0171(7) -0.0079(7) 0.0007(7) O6 0.0572(12) 0.0249(8) 0.0478(10) -0.0121(7) -0.0236(9) 0.0181(8) C1 0.0172(9) 0.0202(9) 0.0257(10) -0.0013(7) -0.0003(7) -0.0014(7) C2 0.0203(10) 0.0180(9) 0.0312(10) -0.0005(8) -0.0012(8) -0.0044(7) C3 0.0129(9) 0.0194(9) 0.0323(10) -0.0056(8) -0.0015(8) -0.0031(7) C4 0.0206(10) 0.0228(10) 0.0302(10) -0.0025(8) -0.0023(8) -0.0032(8) C5 0.0313(12) 0.0313(11) 0.0306(11) -0.0090(9) 0.0043(9) -0.0073(9) C6 0.0243(11) 0.0273(11) 0.0470(13) -0.0128(10) 0.0050(10) 0.0002(9) C7 0.0211(11) 0.0277(11) 0.0461(13) -0.0080(9) -0.0066(9) 0.0039(9) C8 0.0198(10) 0.0249(10) 0.0328(11) -0.0067(8) -0.0071(8) -0.0006(8) C9 0.0204(10) 0.0183(9) 0.0321(11) -0.0076(8) -0.0065(8) 0.0012(7) C10 0.0202(10) 0.0260(10) 0.0414(12) -0.0113(9) -0.0031(9) -0.0020(8) C11 0.0252(12) 0.0300(11) 0.0570(15) -0.0190(11) -0.0139(11) 0.0017(9) C12 0.0438(15) 0.0305(12) 0.0463(14) -0.0139(10) -0.0245(12) 0.0049(10) C13 0.0510(16) 0.0323(12) 0.0298(12) -0.0052(9) -0.0080(11) -0.0053(11) C14 0.0317(12) 0.0259(10) 0.0322(11) -0.0053(8) -0.0030(9) -0.0064(9) C15 0.0168(9) 0.0210(9) 0.0231(9) 0.0004(7) -0.0034(7) -0.0016(7) C16 0.0216(10) 0.0217(10) 0.0363(11) -0.0037(8) -0.0071(9) -0.0003(8) C17 0.0213(11) 0.0308(11) 0.0387(12) 0.0003(9) -0.0081(9) 0.0015(9) C18 0.0193(10) 0.0410(12) 0.0274(11) 0.0021(9) -0.0061(8) -0.0072(9) C19 0.0259(11) 0.0389(12) 0.0303(11) -0.0098(9) -0.0039(9) -0.0087(9) C20 0.0208(10) 0.0276(10) 0.0301(11) -0.0066(8) -0.0029(8) 0.0004(8) C21 0.0130(9) 0.0188(9) 0.0310(10) -0.0071(8) -0.0032(7) -0.0012(7) C22 0.0186(10) 0.0194(9) 0.0372(11) -0.0043(8) -0.0005(8) -0.0028(8) C23 0.0208(11) 0.0192(10) 0.0553(14) -0.0124(9) -0.0008(10) -0.0043(8) C24 0.0373(14) 0.0366(13) 0.0530(15) -0.0272(11) 0.0029(11) -0.0044(11) C25 0.0532(16) 0.0403(13) 0.0331(12) -0.0145(10) 0.0037(11) -0.0075(12) C26 0.0290(12) 0.0247(10) 0.0312(11) -0.0061(8) -0.0017(9) -0.0043(8) S1 0.0173(2) 0.0214(5) 0.0194(7) 0.0015(5) -0.0016(6) -0.0048(3) C27 0.0196(12) 0.0180(10) 0.0283(12) -0.0062(9) -0.0004(9) -0.0011(9) C28 0.0299(18) 0.0347(16) 0.0278(16) -0.0082(12) 0.0040(12) -0.0128(13) C29 0.0320(15) 0.0376(15) 0.0234(13) -0.0056(11) -0.0023(12) -0.0123(12) C30 0.0213(12) 0.0226(11) 0.0251(12) -0.0042(9) -0.0031(10) -0.0024(9) C31 0.0276(19) 0.060(2) 0.038(2) -0.0011(16) 0.0061(14) -0.0224(17) C32 0.061(2) 0.060(2) 0.0422(18) 0.0026(15) -0.0067(16) -0.0297(18) Cl1 0.0173(2) 0.0214(5) 0.0194(7) 0.0015(5) -0.0016(6) -0.0048(3) C33 0.0203(10) 0.0164(9) 0.0320(11) -0.0026(8) -0.0053(8) -0.0040(7) C34 0.0188(10) 0.0224(10) 0.0324(11) -0.0036(8) -0.0028(8) -0.0029(8) C35 0.0223(11) 0.0241(10) 0.0357(12) -0.0078(9) -0.0062(9) -0.0044(8) C36 0.0261(11) 0.0187(9) 0.0388(12) -0.0067(8) -0.0100(9) 0.0010(8) C37 0.0601(18) 0.0307(12) 0.0501(16) -0.0059(11) -0.0216(14) 0.0121(12) C38 0.073(2) 0.0350(15) 0.080(2) -0.0013(15) -0.0204(19) 0.0033(15) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni -3.0029 0.5091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist 0 -1 -12 0.0056 0 0 12 0.0275 -6 -2 0 0.1281 1 1 12 0.0540 0 6 5 0.0230 0 -6 -5 0.0642 6 0 -4 0.1235 5 4 -1 0.1148 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 P1 Ni S2 88.52(2) . . y P1 Ni S1 175.80(6) . . y P1 Ni Cl1 174.2(3) . . y P2 Ni P1 86.08(2) . . y P2 Ni S2 174.55(2) . . y P2 Ni S1 89.91(5) . . y P2 Ni Cl1 93.9(3) . . y S2 Ni Cl1 91.5(3) . . y S1 Ni S2 95.50(5) . . y C2 P1 Ni 110.00(7) . . ? C3 P1 Ni 115.14(7) . . ? C3 P1 C2 106.25(9) . . ? C3 P1 C9 104.35(9) . . ? C9 P1 Ni 114.73(7) . . ? C9 P1 C2 105.58(9) . . ? C1 P2 Ni 107.23(6) . . ? C15 P2 Ni 119.18(7) . . ? C15 P2 C1 105.15(9) . . ? C21 P2 Ni 112.41(7) . . ? C21 P2 C1 105.36(9) . . ? C21 P2 C15 106.48(9) . . ? C33 S2 Ni 98.48(7) . . ? C30 O3 C31 115.9(2) . . ? C36 O6 C37 115.91(18) . . ? P2 C1 H1A 110.2 . . ? P2 C1 H1B 110.2 . . ? H1A C1 H1B 108.5 . . ? C2 C1 P2 107.47(14) . . ? C2 C1 H1A 110.2 . . ? C2 C1 H1B 110.2 . . ? P1 C2 H2A 109.7 . . ? P1 C2 H2B 109.7 . . ? C1 C2 P1 109.64(14) . . ? C1 C2 H2A 109.7 . . ? C1 C2 H2B 109.7 . . ? H2A C2 H2B 108.2 . . ? C4 C3 P1 120.84(15) . . ? C4 C3 C8 119.27(18) . . ? C8 C3 P1 119.69(16) . . ? C3 C4 H4 119.9 . . ? C5 C4 C3 120.25(19) . . ? C5 C4 H4 119.9 . . ? C4 C5 H5 119.9 . . ? C4 C5 C6 120.1(2) . . ? C6 C5 H5 119.9 . . ? C5 C6 H6 120.0 . . ? C7 C6 C5 120.0(2) . . ? C7 C6 H6 120.0 . . ? C6 C7 H7 119.8 . . ? C6 C7 C8 120.3(2) . . ? C8 C7 H7 119.8 . . ? C3 C8 H8 120.0 . . ? C7 C8 C3 120.0(2) . . ? C7 C8 H8 120.0 . . ? C10 C9 P1 119.43(17) . . ? C14 C9 P1 120.75(17) . . ? C14 C9 C10 119.8(2) . . ? C9 C10 H10 120.2 . . ? C11 C10 C9 119.5(2) . . ? C11 C10 H10 120.2 . . ? C10 C11 H11 119.6 . . ? C12 C11 C10 120.8(2) . . ? C12 C11 H11 119.6 . . ? C11 C12 H12 120.1 . . ? C11 C12 C13 119.9(2) . . ? C13 C12 H12 120.1 . . ? C12 C13 H13 119.9 . . ? C14 C13 C12 120.2(2) . . ? C14 C13 H13 119.9 . . ? C9 C14 C13 119.9(2) . . ? C9 C14 H14 120.1 . . ? C13 C14 H14 120.1 . . ? C16 C15 P2 122.77(16) . . ? C20 C15 P2 117.94(15) . . ? C20 C15 C16 119.28(19) . . ? C15 C16 H16 120.0 . . ? C17 C16 C15 119.9(2) . . ? C17 C16 H16 120.0 . . ? C16 C17 H17 119.8 . . ? C18 C17 C16 120.4(2) . . ? C18 C17 H17 119.8 . . ? C17 C18 H18 120.1 . . ? C17 C18 C19 119.8(2) . . ? C19 C18 H18 120.1 . . ? C18 C19 H19 119.8 . . ? C20 C19 C18 120.5(2) . . ? C20 C19 H19 119.8 . . ? C15 C20 H20 120.0 . . ? C19 C20 C15 120.0(2) . . ? C19 C20 H20 120.0 . . ? C22 C21 P2 121.41(16) . . ? C26 C21 P2 118.99(15) . . ? C26 C21 C22 119.58(19) . . ? C21 C22 H22 120.1 . . ? C23 C22 C21 119.9(2) . . ? C23 C22 H22 120.1 . . ? C22 C23 H23 120.0 . . ? C24 C23 C22 120.0(2) . . ? C24 C23 H23 120.0 . . ? C23 C24 H24 119.7 . . ? C23 C24 C25 120.6(2) . . ? C25 C24 H24 119.7 . . ? C24 C25 H25 120.0 . . ? C24 C25 C26 120.0(2) . . ? C26 C25 H25 120.0 . . ? C21 C26 C25 120.0(2) . . ? C21 C26 H26 120.0 . . ? C25 C26 H26 120.0 . . ? C27 S1 Ni 106.18(13) . . ? C28 C27 S1 134.8(2) . . ? C30 C27 S1 133.4(2) . . ? C30 C27 C28 91.7(2) . . ? O1 C28 C27 136.7(3) . . ? O1 C28 C29 135.8(4) . . ? C27 C28 C29 87.5(2) . . ? O2 C29 C28 136.6(3) . . ? O2 C29 C30 136.9(3) . . ? C30 C29 C28 86.4(2) . . ? O3 C30 C27 130.4(2) . . ? O3 C30 C29 135.3(2) . . ? C27 C30 C29 94.3(2) . . ? O3 C31 H31A 109.7 . . ? O3 C31 H31B 109.7 . . ? O3 C31 C32 109.8(3) . . ? H31A C31 H31B 108.2 . . ? C32 C31 H31A 109.7 . . ? C32 C31 H31B 109.7 . . ? C31 C32 H32A 109.5 . . ? C31 C32 H32B 109.5 . . ? C31 C32 H32C 109.5 . . ? H32A C32 H32B 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C34 C33 S2 130.87(15) . . ? C36 C33 S2 138.77(17) . . ? C36 C33 C34 90.35(17) . . ? O4 C34 C33 133.9(2) . . ? O4 C34 C35 136.9(2) . . ? O4 C34 C36 177.0(2) . . ? C33 C34 C35 89.16(16) . . ? C33 C34 C36 43.36(11) . . ? C35 C34 C36 45.80(11) . . ? O5 C35 C34 137.4(2) . . ? O5 C35 C36 136.9(2) . . ? C36 C35 C34 85.73(16) . . ? O6 C36 C33 137.7(2) . . ? O6 C36 C34 176.02(19) . . ? O6 C36 C35 127.6(2) . . ? C33 C36 C34 46.29(12) . . ? C33 C36 C35 94.74(17) . . ? C35 C36 C34 48.46(12) . . ? O6 C37 H37A 109.7 . . ? O6 C37 H37B 109.7 . . ? H37A C37 H37B 108.2 . . ? C38 C37 O6 109.8(3) . . ? C38 C37 H37A 109.7 . . ? C38 C37 H37B 109.7 . . ? C37 C38 H38A 109.5 . . ? C37 C38 H38B 109.5 . . ? C37 C38 H38C 109.5 . . ? H38A C38 H38B 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? Cl7 C39 Cl2 118(4) . . ? Cl7 C39 H39A 107.7 . . ? Cl7 C39 H39B 107.7 . . ? Cl2 C39 H39A 107.7 . . ? Cl2 C39 H39B 107.7 . . ? H39A C39 H39B 107.1 . . ? C40 O10 H10A 104.0 . . ? O10 C40 H40A 109.6 . . ? O10 C40 H40B 114.8 . . ? O10 C40 H40C 103.8 . . ? H40A C40 H40B 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? 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 Ni P1 2.1846(6) . y Ni P2 2.1697(5) . y Ni S2 2.2520(5) . y Ni S1 2.225(2) . y Ni Cl1 2.283(15) . y P1 C2 1.851(2) . ? P1 C3 1.815(2) . ? P1 C9 1.817(2) . ? P2 C1 1.832(2) . ? P2 C15 1.815(2) . ? P2 C21 1.8133(19) . ? S2 C33 1.698(2) . ? O1 C28 1.174(4) . ? O2 C29 1.203(3) . ? O3 C30 1.316(3) . ? O3 C31 1.470(4) . ? O4 C34 1.213(3) . ? O5 C35 1.209(3) . ? O6 C36 1.316(3) . ? O6 C37 1.467(3) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C1 C2 1.526(3) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 C4 1.392(3) . ? C3 C8 1.396(3) . ? C4 H4 0.9500 . ? C4 C5 1.386(3) . ? C5 H5 0.9500 . ? C5 C6 1.386(3) . ? C6 H6 0.9500 . ? C6 C7 1.380(3) . ? C7 H7 0.9500 . ? C7 C8 1.388(3) . ? C8 H8 0.9500 . ? C9 C10 1.396(3) . ? C9 C14 1.385(3) . ? C10 H10 0.9500 . ? C10 C11 1.383(3) . ? C11 H11 0.9500 . ? C11 C12 1.371(4) . ? C12 H12 0.9500 . ? C12 C13 1.388(4) . ? C13 H13 0.9500 . ? C13 C14 1.385(3) . ? C14 H14 0.9500 . ? C15 C16 1.398(3) . ? C15 C20 1.397(3) . ? C16 H16 0.9500 . ? C16 C17 1.388(3) . ? C17 H17 0.9500 . ? C17 C18 1.381(3) . ? C18 H18 0.9500 . ? C18 C19 1.385(3) . ? C19 H19 0.9500 . ? C19 C20 1.384(3) . ? C20 H20 0.9500 . ? C21 C22 1.403(3) . ? C21 C26 1.386(3) . ? C22 H22 0.9500 . ? C22 C23 1.386(3) . ? C23 H23 0.9500 . ? C23 C24 1.375(4) . ? C24 H24 0.9500 . ? C24 C25 1.383(4) . ? C25 H25 0.9500 . ? C25 C26 1.389(3) . ? C26 H26 0.9500 . ? S1 C27 1.713(3) . ? C27 C28 1.504(5) . ? C27 C30 1.393(3) . ? C28 C29 1.551(4) . ? C29 C30 1.486(3) . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? C31 C32 1.493(6) . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C33 C34 1.473(3) . ? C33 C36 1.399(3) . ? C34 C35 1.529(3) . ? C34 C36 2.037(3) . ? C35 C36 1.465(3) . ? C37 H37A 0.9900 . ? C37 H37B 0.9900 . ? C37 C38 1.461(5) . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C38 H38C 0.9800 . ? Cl7 C39 1.66(3) . ? Cl2 C39 1.66(3) . ? C39 H39A 0.9900 . ? C39 H39B 0.9900 . ? O10 H10A 0.8399 . ? O10 C40 1.44(2) . ? C40 H40A 0.9802 . ? C40 H40B 0.9799 . ? C40 H40C 0.9800 . ? 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 Ni P1 C2 C1 20.24(16) . . . . ? Ni P1 C3 C4 -78.97(17) . . . . ? Ni P1 C3 C8 95.82(17) . . . . ? Ni P1 C9 C10 179.34(14) . . . . ? Ni P1 C9 C14 -1.89(19) . . . . ? Ni P2 C1 C2 47.81(14) . . . . ? Ni P2 C15 C16 -139.88(16) . . . . ? Ni P2 C15 C20 41.55(19) . . . . ? Ni P2 C21 C22 -155.88(15) . . . . ? Ni P2 C21 C26 25.94(18) . . . . ? Ni S2 C33 C34 12.5(2) . . . . ? Ni S2 C33 C36 -169.2(2) . . . . ? Ni S1 C27 C28 -13.4(3) . . . . ? Ni S1 C27 C30 171.0(2) . . . . ? P1 C3 C4 C5 173.02(17) . . . . ? P1 C3 C8 C7 -173.25(17) . . . . ? P1 C9 C10 C11 178.66(16) . . . . ? P1 C9 C14 C13 -178.46(17) . . . . ? P2 C1 C2 P1 -41.86(16) . . . . ? P2 C15 C16 C17 -176.82(17) . . . . ? P2 C15 C20 C19 176.58(17) . . . . ? P2 C21 C22 C23 -177.94(16) . . . . ? P2 C21 C26 C25 177.47(19) . . . . ? S2 C33 C34 O4 0.7(4) . . . . ? S2 C33 C34 C35 179.74(18) . . . . ? S2 C33 C34 C36 178.9(3) . . . . ? S2 C33 C36 O6 1.5(5) . . . . ? S2 C33 C36 C34 -178.8(3) . . . . ? S2 C33 C36 C35 -179.6(2) . . . . ? O1 C28 C29 O2 3.3(8) . . . . ? O1 C28 C29 C30 -177.8(5) . . . . ? O2 C29 C30 O3 -1.7(6) . . . . ? O2 C29 C30 C27 177.6(4) . . . . ? O4 C34 C35 O5 -1.7(5) . . . . ? O4 C34 C35 C36 178.2(3) . . . . ? O5 C35 C36 O6 -0.2(5) . . . . ? O5 C35 C36 C33 -179.3(3) . . . . ? O5 C35 C36 C34 179.9(4) . . . . ? C1 P2 C15 C16 99.95(19) . . . . ? C1 P2 C15 C20 -78.62(18) . . . . ? C1 P2 C21 C22 -39.43(18) . . . . ? C1 P2 C21 C26 142.39(17) . . . . ? C2 P1 C3 C4 43.06(19) . . . . ? C2 P1 C3 C8 -142.15(17) . . . . ? C2 P1 C9 C10 58.05(18) . . . . ? C2 P1 C9 C14 -123.17(17) . . . . ? C3 P1 C2 C1 -105.00(15) . . . . ? C3 P1 C9 C10 -53.74(18) . . . . ? C3 P1 C9 C14 125.03(17) . . . . ? C3 C4 C5 C6 0.5(3) . . . . ? C4 C3 C8 C7 1.6(3) . . . . ? C4 C5 C6 C7 1.0(4) . . . . ? C5 C6 C7 C8 -1.1(4) . . . . ? C6 C7 C8 C3 -0.2(4) . . . . ? C8 C3 C4 C5 -1.8(3) . . . . ? C9 P1 C2 C1 144.55(14) . . . . ? C9 P1 C3 C4 154.38(17) . . . . ? C9 P1 C3 C8 -30.83(19) . . . . ? C9 C10 C11 C12 -0.2(3) . . . . ? C10 C9 C14 C13 0.3(3) . . . . ? C10 C11 C12 C13 0.4(3) . . . . ? C11 C12 C13 C14 -0.2(4) . . . . ? C12 C13 C14 C9 -0.2(3) . . . . ? C14 C9 C10 C11 -0.1(3) . . . . ? C15 P2 C1 C2 175.60(13) . . . . ? C15 P2 C21 C22 71.90(18) . . . . ? C15 P2 C21 C26 -106.28(17) . . . . ? C15 C16 C17 C18 -0.3(3) . . . . ? C16 C15 C20 C19 -2.0(3) . . . . ? C16 C17 C18 C19 -0.8(3) . . . . ? C17 C18 C19 C20 0.5(3) . . . . ? C18 C19 C20 C15 1.0(3) . . . . ? C20 C15 C16 C17 1.7(3) . . . . ? C21 P2 C1 C2 -72.12(14) . . . . ? C21 P2 C15 C16 -11.5(2) . . . . ? C21 P2 C15 C20 169.91(16) . . . . ? C21 C22 C23 C24 0.0(3) . . . . ? C22 C21 C26 C25 -0.7(3) . . . . ? C22 C23 C24 C25 0.2(4) . . . . ? C23 C24 C25 C26 -0.8(4) . . . . ? C24 C25 C26 C21 1.0(4) . . . . ? C26 C21 C22 C23 0.2(3) . . . . ? S1 C27 C28 O1 0.9(7) . . . . ? S1 C27 C28 C29 -178.1(2) . . . . ? S1 C27 C30 O3 -2.4(4) . . . . ? S1 C27 C30 C29 178.3(2) . . . . ? C27 C28 C29 O2 -177.7(4) . . . . ? C27 C28 C29 C30 1.2(2) . . . . ? C28 C27 C30 O3 -179.3(3) . . . . ? C28 C27 C30 C29 1.4(2) . . . . ? C28 C29 C30 O3 179.4(3) . . . . ? C28 C29 C30 C27 -1.3(2) . . . . ? C30 O3 C31 C32 83.0(4) . . . . ? C30 C27 C28 O1 177.7(5) . . . . ? C30 C27 C28 C29 -1.3(2) . . . . ? C31 O3 C30 C27 179.5(3) . . . . ? C31 O3 C30 C29 -1.5(4) . . . . ? C33 C34 C35 O5 179.3(3) . . . . ? C33 C34 C35 C36 -0.79(16) . . . . ? C34 C33 C36 O6 -179.7(3) . . . . ? C34 C33 C36 C35 -0.87(18) . . . . ? C34 C35 C36 O6 179.9(3) . . . . ? C34 C35 C36 C33 0.84(17) . . . . ? C36 O6 C37 C38 -81.3(3) . . . . ? C36 C33 C34 O4 -178.2(3) . . . . ? C36 C33 C34 C35 0.83(17) . . . . ? C36 C34 C35 O5 -179.9(4) . . . . ? C37 O6 C36 C33 3.1(4) . . . . ? C37 O6 C36 C35 -175.5(2) . . . . ?