#------------------------------------------------------------------------------ #$Date: 2016-02-13 14:50:18 +0200 (Sat, 13 Feb 2016) $ #$Revision: 176428 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/03/59/7035948.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_7035948 loop_ _publ_author_name 'Castellanos-Blanco, Nahury' 'Flores-Alamo, Marcos' 'Garc\'ia, Juventino J' _publ_section_title ; Tandem hydrogenation and condensation of fluorinated \a,\b-unsaturated ketones with primary amines, catalyzed by nickel. ; _journal_issue 35 _journal_name_full 'Dalton transactions (Cambridge, England : 2003)' _journal_page_first 15653 _journal_page_last 15663 _journal_paper_doi 10.1039/c5dt02366a _journal_volume 44 _journal_year 2015 _chemical_formula_moiety 'C47 H76 F6 Ni2 O P4' _chemical_formula_sum 'C47 H76 F6 Ni2 O P4' _chemical_formula_weight 1012.37 _chemical_name_systematic ; ? ; _space_group_IT_number 14 _symmetry_cell_setting monoclinic _symmetry_Int_Tables_number 14 _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_space_group_name_H-M 'P 1 21/c 1' _atom_sites_solution_hydrogens geom _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.4.3 _audit_creation_date 2015-06-18T22:17:00-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_update_record ; 2015-06-19 deposited with the CCDC. 2015-07-23 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 98.964(3) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 14.9031(5) _cell_length_b 22.0459(6) _cell_length_c 15.6218(7) _cell_measurement_reflns_used 13147 _cell_measurement_temperature 130(2) _cell_measurement_theta_max 25.9998 _cell_measurement_theta_min 3.3691 _cell_volume 5069.9(3) _computing_cell_refinement ; CrysAlisPro, Agilent Technologies, Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET) (compiled Oct 27 2011,15:02:11) ; _computing_data_collection ; CrysAlisPro, Agilent Technologies, Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET) (compiled Oct 27 2011,15:02:11) ; _computing_data_reduction ; CrysAlisPro, Agilent Technologies, Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET) (compiled Oct 27 2011,15:02:11) ; _computing_structure_refinement 'SHELXL-2013 (Sheldrick, 2013)' _diffrn_ambient_temperature 130(2) _diffrn_detector_area_resol_mean 10.4685 _diffrn_measured_fraction_theta_full 0.997 _diffrn_measured_fraction_theta_max 0.998 _diffrn_measurement_device_type 'Xcalibur, Atlas, Gemini' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_UB_11 -0.0435615 _diffrn_orient_matrix_UB_12 -0.0029513 _diffrn_orient_matrix_UB_13 0.0124068 _diffrn_orient_matrix_UB_21 -0.0152687 _diffrn_orient_matrix_UB_22 -0.0162314 _diffrn_orient_matrix_UB_23 -0.0387569 _diffrn_orient_matrix_UB_31 0.0136537 _diffrn_orient_matrix_UB_32 -0.0276113 _diffrn_orient_matrix_UB_33 0.021493 _diffrn_radiation_monochromator graphite _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0513 _diffrn_reflns_av_unetI/netI 0.1151 _diffrn_reflns_Laue_measured_fraction_full 0.997 _diffrn_reflns_Laue_measured_fraction_max 0.998 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_number 41452 _diffrn_reflns_point_group_measured_fraction_full 0.997 _diffrn_reflns_point_group_measured_fraction_max 0.998 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 26.37 _diffrn_reflns_theta_min 3.376 _exptl_absorpt_coefficient_mu 0.924 _exptl_absorpt_correction_T_max 0.909 _exptl_absorpt_correction_T_min 0.764 _exptl_absorpt_correction_type analytical _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET) (compiled Oct 27 2011,15:02:11) Analytical numeric absorption correction using a multifaceted crystal model based on expressions derived by R.C. Clark & J.S. (Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897) ; _exptl_crystal_colour brown _exptl_crystal_density_diffrn 1.326 _exptl_crystal_description block _exptl_crystal_F_000 2144 _exptl_crystal_size_max 0.37 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.1 _refine_diff_density_max 0.489 _refine_diff_density_min -0.51 _refine_diff_density_rms 0.066 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.047 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 557 _refine_ls_number_reflns 10339 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.047 _refine_ls_R_factor_all 0.0494 _refine_ls_R_factor_gt 0.0345 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0271P)^2^+1.8386P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0707 _refine_ls_wR_factor_ref 0.0794 _reflns_Friedel_coverage 0 _reflns_number_gt 8324 _reflns_number_total 10339 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file c5dt02366a2.cif _cod_data_source_block 2a _cod_depositor_comments 'Adding full bibliography for 7035948--7035950.cif.' _cod_original_sg_symbol_H-M 'P 21/c' _cod_database_code 7035948 #BEGIN Tags that were not found in dictionaries: _shelx_estimated_absorpt_t_min 0.726 _shelx_estimated_absorpt_t_max 0.913 _shelx_res_file ; TITL nycb3-b CELL 0.71073 14.9031 22.0459 15.6218 90.000 98.964 90.000 ZERR 4.00 0.0005 0.0006 0.0007 0.000 0.003 0.000 LATT 1 SYMM - X, 1/2 + Y, 1/2 - Z SFAC C H O NI P F UNIT 188 304 4 8 16 24 MERG 2 SHEL 100 0.8 FMAP 2 PLAN 5 SIZE 0.100 0.250 0.370 ACTA BOND BOND $H CONF LIST 4 WPDB -2 L.S. 20 TEMP -153.00 WGHT 0.027100 1.838600 FVAR 1.06043 C1 1 0.498856 0.708254 0.133987 11.00000 0.01265 0.01673 = 0.03196 0.00986 0.00101 -0.00372 C2 1 0.491746 0.681150 0.052066 11.00000 0.02084 0.02828 = 0.03209 0.00677 -0.00079 -0.00343 AFIX 43 H2 2 0.535574 0.651743 0.042143 11.00000 -1.20000 AFIX 0 C3 1 0.422811 0.695868 -0.014965 11.00000 0.03512 0.04148 = 0.03649 0.01337 -0.00922 -0.01402 AFIX 43 H3 2 0.420191 0.676902 -0.069904 11.00000 -1.20000 AFIX 0 C4 1 0.357851 0.738204 -0.001747 11.00000 0.02516 0.04360 = 0.06525 0.02881 -0.01872 -0.00752 AFIX 43 H4 2 0.310326 0.748162 -0.047476 11.00000 -1.20000 AFIX 0 C5 1 0.362141 0.765639 0.077072 11.00000 0.01634 0.03180 = 0.06720 0.02080 -0.00178 0.00013 AFIX 43 H5 2 0.317352 0.794652 0.085919 11.00000 -1.20000 AFIX 0 C6 1 0.431738 0.751519 0.144965 11.00000 0.01281 0.01930 = 0.04895 0.01272 0.00278 -0.00294 C7 1 0.976610 0.602391 0.241859 11.00000 0.01519 0.01363 = 0.02952 0.00298 0.00322 -0.00216 C8 1 0.979500 0.591656 0.153982 11.00000 0.01659 0.02298 = 0.03484 0.00072 0.00289 0.00178 AFIX 43 H8 2 0.937640 0.612477 0.112001 11.00000 -1.20000 AFIX 0 C9 1 1.040740 0.551992 0.125546 11.00000 0.02167 0.02958 = 0.04672 -0.00860 0.01221 -0.00244 AFIX 43 H9 2 1.039682 0.545640 0.065249 11.00000 -1.20000 AFIX 0 C10 1 1.103276 0.521731 0.184979 11.00000 0.02023 0.02042 = 0.06512 -0.00333 0.01491 0.00352 AFIX 43 H10 2 1.145766 0.494649 0.166113 11.00000 -1.20000 AFIX 0 C11 1 1.103096 0.531425 0.272080 11.00000 0.01761 0.01815 = 0.05702 0.00652 0.00323 0.00271 AFIX 43 H11 2 1.146142 0.510767 0.313161 11.00000 -1.20000 AFIX 0 C12 1 1.041355 0.570766 0.301373 11.00000 0.01487 0.01799 = 0.03719 0.00673 0.00072 -0.00052 C13 1 0.432784 0.783807 0.228349 11.00000 0.01892 0.01784 = 0.06815 0.00906 0.01594 0.00407 C14 1 1.045594 0.578354 0.396211 11.00000 0.01987 0.03657 = 0.04278 0.01592 -0.00415 0.00727 C15 1 0.572551 0.690669 0.204118 11.00000 0.01527 0.01157 = 0.02482 0.00241 0.00195 -0.00126 AFIX 13 H15 2 0.579525 0.717589 0.256255 11.00000 -1.20000 AFIX 0 C16 1 0.655808 0.664843 0.185185 11.00000 0.01553 0.01377 = 0.01788 0.00247 0.00180 -0.00233 AFIX 13 H16 2 0.662871 0.661811 0.122712 11.00000 -1.20000 AFIX 0 C17 1 0.740009 0.668877 0.248769 11.00000 0.01679 0.00732 = 0.02028 0.00270 0.00145 -0.00246 C18 1 0.824027 0.655680 0.213275 11.00000 0.01399 0.01156 = 0.02234 0.00257 0.00187 -0.00164 AFIX 13 H18 2 0.815773 0.634671 0.155851 11.00000 -1.20000 AFIX 0 C19 1 0.908682 0.643801 0.269546 11.00000 0.01385 0.01482 = 0.02314 0.00537 0.00380 -0.00011 AFIX 13 H19 2 0.903139 0.640779 0.332379 11.00000 -1.20000 AFIX 0 C20 1 0.721599 0.826450 0.188131 11.00000 0.01747 0.01548 = 0.03524 0.00180 0.00281 0.00224 AFIX 13 H20 2 0.676864 0.792924 0.172420 11.00000 -1.20000 AFIX 0 C21 1 0.732923 0.833375 0.286342 11.00000 0.02684 0.02467 = 0.03734 -0.00219 0.00872 0.00406 AFIX 137 H21A 2 0.772582 0.868040 0.304297 11.00000 -1.50000 H21B 2 0.760085 0.796396 0.313977 11.00000 -1.50000 H21C 2 0.673380 0.840140 0.303872 11.00000 -1.50000 AFIX 0 C22 1 0.680143 0.883386 0.141960 11.00000 0.02757 0.02702 = 0.04970 0.00589 0.00243 0.01086 AFIX 137 H22A 2 0.620624 0.891229 0.158942 11.00000 -1.50000 H22B 2 0.672977 0.877314 0.079117 11.00000 -1.50000 H22C 2 0.720260 0.918100 0.158231 11.00000 -1.50000 AFIX 0 C23 1 0.801817 0.796089 0.034696 11.00000 0.02185 0.02263 = 0.02481 0.00987 0.00116 0.00009 AFIX 13 H23 2 0.778694 0.836393 0.011568 11.00000 -1.20000 AFIX 0 C24 1 0.728469 0.748824 0.006324 11.00000 0.03296 0.03459 = 0.02226 0.00446 0.00072 -0.00633 AFIX 137 H24A 2 0.712810 0.749286 -0.056973 11.00000 -1.50000 H24B 2 0.674345 0.758277 0.032281 11.00000 -1.50000 H24C 2 0.751121 0.708540 0.025434 11.00000 -1.50000 AFIX 0 C25 1 0.887916 0.781556 -0.002810 11.00000 0.02979 0.05162 = 0.02849 0.00500 0.00621 0.00150 AFIX 137 H25A 2 0.915027 0.744116 0.023379 11.00000 -1.50000 H25B 2 0.931313 0.814984 0.009777 11.00000 -1.50000 H25C 2 0.872725 0.776231 -0.065682 11.00000 -1.50000 AFIX 0 C26 1 1.132090 0.759616 0.226065 11.00000 0.01229 0.03090 = 0.05325 0.00449 0.00526 -0.00427 AFIX 13 H26 2 1.173812 0.795407 0.231360 11.00000 -1.20000 AFIX 0 C27 1 1.120512 0.737030 0.132658 11.00000 0.02591 0.04423 = 0.05811 0.00190 0.01650 0.00216 AFIX 137 H27A 2 1.179423 0.723688 0.119076 11.00000 -1.50000 H27B 2 1.096880 0.769957 0.093364 11.00000 -1.50000 H27C 2 1.077795 0.702940 0.125546 11.00000 -1.50000 AFIX 0 C28 1 1.175439 0.710288 0.287917 11.00000 0.01639 0.03495 = 0.06378 0.00200 -0.00141 0.00017 AFIX 137 H28A 2 1.142475 0.672076 0.275115 11.00000 -1.50000 H28B 2 1.172597 0.722355 0.347812 11.00000 -1.50000 H28C 2 1.239021 0.704825 0.280457 11.00000 -1.50000 AFIX 0 C29 1 1.053152 0.811031 0.369229 11.00000 0.02961 0.02708 = 0.03476 0.00187 -0.00444 -0.00627 AFIX 13 H29 2 1.061736 0.774170 0.406924 11.00000 -1.20000 AFIX 0 C30 1 0.974945 0.847129 0.396655 11.00000 0.04408 0.03909 = 0.03653 -0.00463 0.00204 -0.00242 AFIX 137 H30A 2 0.988164 0.855560 0.458941 11.00000 -1.50000 H30B 2 0.918708 0.823531 0.384061 11.00000 -1.50000 H30C 2 0.967763 0.885468 0.364566 11.00000 -1.50000 AFIX 0 C31 1 1.140993 0.848162 0.388444 11.00000 0.03828 0.03778 = 0.05310 -0.00425 -0.01334 -0.01309 AFIX 137 H31A 2 1.133929 0.886046 0.355258 11.00000 -1.50000 H31B 2 1.191441 0.824710 0.371857 11.00000 -1.50000 H31C 2 1.153746 0.857458 0.450497 11.00000 -1.50000 AFIX 0 C32 1 1.001567 0.855352 0.192293 11.00000 0.02187 0.02106 = 0.03914 0.00610 0.00283 -0.00716 AFIX 23 H32A 2 1.033859 0.889109 0.225740 11.00000 -1.20000 H32B 2 1.026868 0.851128 0.137640 11.00000 -1.20000 AFIX 0 C33 1 0.900605 0.870864 0.171007 11.00000 0.02420 0.01514 = 0.03596 0.00719 0.00138 -0.00231 AFIX 23 H33A 2 0.890201 0.896283 0.118146 11.00000 -1.20000 H33B 2 0.882516 0.894750 0.219203 11.00000 -1.20000 AFIX 0 C34 1 0.358621 0.549125 0.220211 11.00000 0.01461 0.02890 = 0.03022 0.00413 0.00207 -0.00542 AFIX 13 H34 2 0.314267 0.537456 0.259220 11.00000 -1.20000 AFIX 0 C35 1 0.320447 0.603694 0.166468 11.00000 0.02085 0.03480 = 0.04733 0.00768 -0.00581 -0.00199 AFIX 137 H35A 2 0.359454 0.612914 0.123124 11.00000 -1.50000 H35B 2 0.318412 0.638826 0.204553 11.00000 -1.50000 H35C 2 0.258951 0.594399 0.137201 11.00000 -1.50000 AFIX 0 C36 1 0.369092 0.495767 0.160842 11.00000 0.02635 0.03419 = 0.04149 -0.00262 -0.00618 -0.00597 AFIX 137 H36A 2 0.310838 0.487623 0.124079 11.00000 -1.50000 H36B 2 0.388227 0.459820 0.195887 11.00000 -1.50000 H36C 2 0.414960 0.505477 0.124307 11.00000 -1.50000 AFIX 0 C37 1 0.430461 0.615290 0.377139 11.00000 0.01835 0.02360 = 0.02892 0.00250 0.00588 0.00088 AFIX 13 H37 2 0.396993 0.651336 0.349465 11.00000 -1.20000 AFIX 0 C38 1 0.366157 0.582653 0.429493 11.00000 0.03611 0.04020 = 0.04100 0.00401 0.02135 -0.00067 AFIX 137 H38A 2 0.396051 0.546284 0.456465 11.00000 -1.50000 H38B 2 0.310606 0.570957 0.390860 11.00000 -1.50000 H38C 2 0.350698 0.609852 0.474629 11.00000 -1.50000 AFIX 0 C39 1 0.513909 0.639308 0.437001 11.00000 0.02958 0.03420 = 0.03243 -0.00628 0.00379 0.00343 AFIX 137 H39A 2 0.494760 0.668858 0.477407 11.00000 -1.50000 H39B 2 0.555034 0.658914 0.402274 11.00000 -1.50000 H39C 2 0.545402 0.605541 0.469680 11.00000 -1.50000 AFIX 0 C40 1 0.677520 0.473197 0.154822 11.00000 0.02696 0.01596 = 0.02823 -0.00305 0.00228 0.00246 AFIX 13 H40 2 0.697587 0.431566 0.174784 11.00000 -1.20000 AFIX 0 C41 1 0.595184 0.467456 0.084144 11.00000 0.03776 0.03563 = 0.03235 -0.01362 0.00062 0.00066 AFIX 137 H41A 2 0.573500 0.507989 0.065241 11.00000 -1.50000 H41B 2 0.546815 0.445482 0.106892 11.00000 -1.50000 H41C 2 0.612245 0.445200 0.034810 11.00000 -1.50000 AFIX 0 C42 1 0.755099 0.503972 0.117933 11.00000 0.03628 0.02782 = 0.03074 -0.00538 0.01113 0.00252 AFIX 137 H42A 2 0.769502 0.480482 0.068574 11.00000 -1.50000 H42B 2 0.808847 0.506092 0.162816 11.00000 -1.50000 H42C 2 0.736684 0.545072 0.098759 11.00000 -1.50000 AFIX 0 C43 1 0.755529 0.515964 0.327799 11.00000 0.02028 0.01540 = 0.02401 0.00050 0.00039 0.00249 AFIX 13 H43 2 0.798843 0.543745 0.304326 11.00000 -1.20000 AFIX 0 C44 1 0.738957 0.542722 0.414070 11.00000 0.02260 0.02359 = 0.02492 -0.00060 -0.00021 0.00106 AFIX 137 H44A 2 0.699870 0.515355 0.441234 11.00000 -1.50000 H44B 2 0.709227 0.582292 0.403979 11.00000 -1.50000 H44C 2 0.797130 0.547700 0.452397 11.00000 -1.50000 AFIX 0 C45 1 0.802369 0.453964 0.341186 11.00000 0.03085 0.02658 = 0.03753 -0.00134 -0.00424 0.01197 AFIX 137 H45A 2 0.859890 0.458320 0.380713 11.00000 -1.50000 H45B 2 0.814301 0.438352 0.285309 11.00000 -1.50000 H45C 2 0.762837 0.425617 0.366087 11.00000 -1.50000 AFIX 0 C46 1 0.573149 0.463905 0.297175 11.00000 0.02532 0.01333 = 0.03193 0.00385 0.00037 -0.00087 AFIX 23 H46A 2 0.537741 0.439196 0.250840 11.00000 -1.20000 H46B 2 0.610409 0.436023 0.337857 11.00000 -1.20000 AFIX 0 C47 1 0.507808 0.499122 0.345706 11.00000 0.02157 0.01905 = 0.02898 0.00871 0.00454 -0.00335 AFIX 23 H47A 2 0.539051 0.509099 0.404674 11.00000 -1.20000 H47B 2 0.454908 0.473168 0.351610 11.00000 -1.20000 AFIX 0 O7 3 0.739716 0.682243 0.325418 11.00000 0.01860 0.02073 = 0.01981 -0.00148 0.00111 0.00062 NI1 4 0.902205 0.728213 0.223271 11.00000 0.01171 0.01358 = 0.02182 0.00238 0.00147 -0.00048 NI2 4 0.580061 0.602465 0.230100 11.00000 0.01259 0.01215 = 0.01919 0.00159 0.00203 -0.00039 P1 5 0.828830 0.801923 0.153486 11.00000 0.01527 0.01453 = 0.02420 0.00391 0.00204 -0.00034 P2 5 1.022109 0.784064 0.255818 11.00000 0.01455 0.01974 = 0.03209 0.00296 0.00038 -0.00343 P3 5 0.467541 0.570002 0.288843 11.00000 0.01418 0.01743 = 0.02454 0.00392 0.00281 -0.00234 P4 5 0.648738 0.516235 0.248751 11.00000 0.01791 0.01242 = 0.02201 -0.00042 0.00112 0.00048 F1 6 0.431794 0.746432 0.296320 11.00000 0.04830 0.02440 = 0.05472 0.00431 0.02631 0.00680 F2 6 0.506214 0.819542 0.249989 11.00000 0.02200 0.02605 = 0.07088 -0.00578 0.01220 -0.00170 F3 6 0.360561 0.820739 0.229090 11.00000 0.02375 0.02718 = 0.09930 0.00506 0.02039 0.01219 F4 6 1.113336 0.546145 0.442220 11.00000 0.04061 0.07541 = 0.05110 0.02255 -0.00741 0.03030 F5 6 1.059984 0.636116 0.423601 11.00000 0.03041 0.04900 = 0.03799 -0.00318 -0.00048 -0.00163 F6 6 0.969605 0.560929 0.425894 11.00000 0.03066 0.05729 = 0.04641 0.02459 0.00876 0.00100 HKLF 4 REM nycb3-b REM R1 = 0.0345 for 8324 Fo > 4sig(Fo) and 0.0494 for all 10339 data REM 557 parameters refined using 0 restraints END WGHT 0.0272 1.8285 REM Highest difference peak 0.489, deepest hole -0.510, 1-sigma level 0.066 Q1 1 0.8965 0.6784 0.2214 11.00000 0.05 0.49 Q2 1 0.8156 0.7963 0.0981 11.00000 0.05 0.43 Q3 1 0.6265 0.5624 0.2411 11.00000 0.05 0.42 Q4 1 0.8730 0.7676 0.1864 11.00000 0.05 0.41 Q5 1 0.7710 0.8167 0.1695 11.00000 0.05 0.39 ; _shelx_res_checksum 18087 #END Tags that were not found in dictionaries loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' 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 C1 C 0.49886(13) 0.70825(9) 0.13399(16) 0.0207(5) Uani 1 1 d . . C2 C 0.49175(15) 0.68115(10) 0.05207(17) 0.0276(6) Uani 1 1 d . . H2 H 0.5356 0.6517 0.0421 0.033 Uiso 1 1 calc R U C3 C 0.42281(17) 0.69587(12) -0.01497(19) 0.0393(7) Uani 1 1 d . . H3 H 0.4202 0.6769 -0.0699 0.047 Uiso 1 1 calc R U C4 C 0.35785(18) 0.73820(12) -0.0017(2) 0.0474(9) Uani 1 1 d . . H4 H 0.3103 0.7482 -0.0475 0.057 Uiso 1 1 calc R U C5 C 0.36214(16) 0.76564(11) 0.0771(2) 0.0393(7) Uani 1 1 d . . H5 H 0.3174 0.7947 0.0859 0.047 Uiso 1 1 calc R U C6 C 0.43174(14) 0.75152(10) 0.14497(18) 0.0272(6) Uani 1 1 d . . C7 C 0.97661(14) 0.60239(9) 0.24186(16) 0.0195(5) Uani 1 1 d . . C8 C 0.97950(14) 0.59166(9) 0.15398(17) 0.0249(5) Uani 1 1 d . . H8 H 0.9376 0.6125 0.112 0.03 Uiso 1 1 calc R U C9 C 1.04074(15) 0.55199(10) 0.12555(19) 0.0319(6) Uani 1 1 d . . H9 H 1.0397 0.5456 0.0652 0.038 Uiso 1 1 calc R U C10 C 1.10328(15) 0.52173(10) 0.1850(2) 0.0344(7) Uani 1 1 d . . H10 H 1.1458 0.4946 0.1661 0.041 Uiso 1 1 calc R U C11 C 1.10310(15) 0.53142(10) 0.27208(19) 0.0312(6) Uani 1 1 d . . H11 H 1.1461 0.5108 0.3132 0.037 Uiso 1 1 calc R U C12 C 1.04135(14) 0.57077(9) 0.30137(17) 0.0237(5) Uani 1 1 d . . C13 C 0.43278(15) 0.78381(10) 0.2283(2) 0.0340(7) Uani 1 1 d . . C14 C 1.04559(16) 0.57835(11) 0.39621(19) 0.0340(6) Uani 1 1 d . . C15 C 0.57255(13) 0.69067(8) 0.20412(15) 0.0173(5) Uani 1 1 d . . H15 H 0.5795 0.7176 0.2563 0.021 Uiso 1 1 calc R U C16 C 0.65581(13) 0.66484(8) 0.18518(15) 0.0158(4) Uani 1 1 d . . H16 H 0.6629 0.6618 0.1227 0.019 Uiso 1 1 calc R U C17 C 0.74001(13) 0.66888(8) 0.24877(15) 0.0150(4) Uani 1 1 d . . C18 C 0.82403(13) 0.65568(8) 0.21328(15) 0.0161(4) Uani 1 1 d . . H18 H 0.8158 0.6347 0.1559 0.019 Uiso 1 1 calc R U C19 C 0.90868(13) 0.64380(8) 0.26955(15) 0.0172(5) Uani 1 1 d . . H19 H 0.9031 0.6408 0.3324 0.021 Uiso 1 1 calc R U C20 C 0.72160(14) 0.82645(9) 0.18813(16) 0.0229(5) Uani 1 1 d . . H20 H 0.6769 0.7929 0.1724 0.027 Uiso 1 1 calc R U C21 C 0.73292(16) 0.83337(10) 0.28634(17) 0.0292(6) Uani 1 1 d . . H21A H 0.7726 0.868 0.3043 0.044 Uiso 1 1 calc R U H21B H 0.7601 0.7964 0.314 0.044 Uiso 1 1 calc R U H21C H 0.6734 0.8401 0.3039 0.044 Uiso 1 1 calc R U C22 C 0.68014(16) 0.88339(10) 0.14196(19) 0.0351(6) Uani 1 1 d . . H22A H 0.6206 0.8912 0.1589 0.053 Uiso 1 1 calc R U H22B H 0.673 0.8773 0.0791 0.053 Uiso 1 1 calc R U H22C H 0.7203 0.9181 0.1582 0.053 Uiso 1 1 calc R U C23 C 0.80182(14) 0.79609(10) 0.03470(16) 0.0234(5) Uani 1 1 d . . H23 H 0.7787 0.8364 0.0116 0.028 Uiso 1 1 calc R U C24 C 0.72847(16) 0.74882(10) 0.00632(17) 0.0303(6) Uani 1 1 d . . H24A H 0.7128 0.7493 -0.057 0.045 Uiso 1 1 calc R U H24B H 0.6743 0.7583 0.0323 0.045 Uiso 1 1 calc R U H24C H 0.7511 0.7085 0.0254 0.045 Uiso 1 1 calc R U C25 C 0.88792(17) 0.78156(12) -0.00281(18) 0.0365(6) Uani 1 1 d . . H25A H 0.915 0.7441 0.0234 0.055 Uiso 1 1 calc R U H25B H 0.9313 0.815 0.0098 0.055 Uiso 1 1 calc R U H25C H 0.8727 0.7762 -0.0657 0.055 Uiso 1 1 calc R U C26 C 1.13209(15) 0.75962(11) 0.22606(19) 0.0321(6) Uani 1 1 d . . H26 H 1.1738 0.7954 0.2314 0.039 Uiso 1 1 calc R U C27 C 1.12051(17) 0.73703(12) 0.1327(2) 0.0417(7) Uani 1 1 d . . H27A H 1.1794 0.7237 0.1191 0.063 Uiso 1 1 calc R U H27B H 1.0969 0.77 0.0934 0.063 Uiso 1 1 calc R U H27C H 1.0778 0.7029 0.1255 0.063 Uiso 1 1 calc R U C28 C 1.17544(16) 0.71029(11) 0.2879(2) 0.0392(7) Uani 1 1 d . . H28A H 1.1425 0.6721 0.2751 0.059 Uiso 1 1 calc R U H28B H 1.1726 0.7224 0.3478 0.059 Uiso 1 1 calc R U H28C H 1.239 0.7048 0.2805 0.059 Uiso 1 1 calc R U C29 C 1.05315(16) 0.81103(10) 0.36923(17) 0.0315(6) Uani 1 1 d . . H29 H 1.0617 0.7742 0.4069 0.038 Uiso 1 1 calc R U C30 C 0.97494(18) 0.84713(12) 0.39665(19) 0.0404(7) Uani 1 1 d . . H30A H 0.9882 0.8556 0.4589 0.061 Uiso 1 1 calc R U H30B H 0.9187 0.8235 0.3841 0.061 Uiso 1 1 calc R U H30C H 0.9678 0.8855 0.3646 0.061 Uiso 1 1 calc R U C31 C 1.14099(18) 0.84816(12) 0.3884(2) 0.0452(8) Uani 1 1 d . . H31A H 1.1339 0.886 0.3553 0.068 Uiso 1 1 calc R U H31B H 1.1914 0.8247 0.3719 0.068 Uiso 1 1 calc R U H31C H 1.1537 0.8575 0.4505 0.068 Uiso 1 1 calc R U C32 C 1.00157(15) 0.85535(10) 0.19229(17) 0.0276(6) Uani 1 1 d . . H32A H 1.0339 0.8891 0.2257 0.033 Uiso 1 1 calc R U H32B H 1.0269 0.8511 0.1376 0.033 Uiso 1 1 calc R U C33 C 0.90061(14) 0.87086(9) 0.17101(17) 0.0255(5) Uani 1 1 d . . H33A H 0.8902 0.8963 0.1181 0.031 Uiso 1 1 calc R U H33B H 0.8825 0.8947 0.2192 0.031 Uiso 1 1 calc R U C34 C 0.35862(14) 0.54912(10) 0.22021(16) 0.0247(5) Uani 1 1 d . . H34 H 0.3143 0.5375 0.2592 0.03 Uiso 1 1 calc R U C35 C 0.32045(16) 0.60369(11) 0.16647(19) 0.0355(6) Uani 1 1 d . . H35A H 0.3595 0.6129 0.1231 0.053 Uiso 1 1 calc R U H35B H 0.3184 0.6388 0.2046 0.053 Uiso 1 1 calc R U H35C H 0.259 0.5944 0.1372 0.053 Uiso 1 1 calc R U C36 C 0.36909(17) 0.49577(11) 0.16084(18) 0.0352(6) Uani 1 1 d . . H36A H 0.3108 0.4876 0.1241 0.053 Uiso 1 1 calc R U H36B H 0.3882 0.4598 0.1959 0.053 Uiso 1 1 calc R U H36C H 0.415 0.5055 0.1243 0.053 Uiso 1 1 calc R U C37 C 0.43046(14) 0.61529(10) 0.37714(16) 0.0234(5) Uani 1 1 d . . H37 H 0.397 0.6513 0.3495 0.028 Uiso 1 1 calc R U C38 C 0.36616(18) 0.58265(11) 0.42949(19) 0.0375(6) Uani 1 1 d . . H38A H 0.3961 0.5463 0.4565 0.056 Uiso 1 1 calc R U H38B H 0.3106 0.571 0.3909 0.056 Uiso 1 1 calc R U H38C H 0.3507 0.6099 0.4746 0.056 Uiso 1 1 calc R U C39 C 0.51391(16) 0.63931(11) 0.43700(17) 0.0322(6) Uani 1 1 d . . H39A H 0.4948 0.6689 0.4774 0.048 Uiso 1 1 calc R U H39B H 0.555 0.6589 0.4023 0.048 Uiso 1 1 calc R U H39C H 0.5454 0.6055 0.4697 0.048 Uiso 1 1 calc R U C40 C 0.67752(15) 0.47320(9) 0.15482(16) 0.0239(5) Uani 1 1 d . . H40 H 0.6976 0.4316 0.1748 0.029 Uiso 1 1 calc R U C41 C 0.59518(17) 0.46746(11) 0.08414(18) 0.0358(6) Uani 1 1 d . . H41A H 0.5735 0.508 0.0652 0.054 Uiso 1 1 calc R U H41B H 0.5468 0.4455 0.1069 0.054 Uiso 1 1 calc R U H41C H 0.6122 0.4452 0.0348 0.054 Uiso 1 1 calc R U C42 C 0.75510(17) 0.50397(10) 0.11793(17) 0.0310(6) Uani 1 1 d . . H42A H 0.7695 0.4805 0.0686 0.046 Uiso 1 1 calc R U H42B H 0.8088 0.5061 0.1628 0.046 Uiso 1 1 calc R U H42C H 0.7367 0.5451 0.0988 0.046 Uiso 1 1 calc R U C43 C 0.75553(14) 0.51596(9) 0.32780(15) 0.0202(5) Uani 1 1 d . . H43 H 0.7988 0.5437 0.3043 0.024 Uiso 1 1 calc R U C44 C 0.73896(15) 0.54272(10) 0.41407(15) 0.0241(5) Uani 1 1 d . . H44A H 0.6999 0.5154 0.4412 0.036 Uiso 1 1 calc R U H44B H 0.7092 0.5823 0.404 0.036 Uiso 1 1 calc R U H44C H 0.7971 0.5477 0.4524 0.036 Uiso 1 1 calc R U C45 C 0.80237(16) 0.45396(10) 0.34119(18) 0.0327(6) Uani 1 1 d . . H45A H 0.8599 0.4583 0.3807 0.049 Uiso 1 1 calc R U H45B H 0.8143 0.4384 0.2853 0.049 Uiso 1 1 calc R U H45C H 0.7628 0.4256 0.3661 0.049 Uiso 1 1 calc R U C46 C 0.57315(15) 0.46390(9) 0.29718(16) 0.0240(5) Uani 1 1 d . . H46A H 0.5377 0.4392 0.2508 0.029 Uiso 1 1 calc R U H46B H 0.6104 0.436 0.3379 0.029 Uiso 1 1 calc R U C47 C 0.50781(15) 0.49912(9) 0.34571(16) 0.0231(5) Uani 1 1 d . . H47A H 0.5391 0.5091 0.4047 0.028 Uiso 1 1 calc R U H47B H 0.4549 0.4732 0.3516 0.028 Uiso 1 1 calc R U O7 O 0.73972(9) 0.68224(6) 0.32542(10) 0.0199(3) Uani 1 1 d . . Ni1 Ni 0.90221(2) 0.72821(2) 0.22327(2) 0.01583(7) Uani 1 1 d . . Ni2 Ni 0.58006(2) 0.60246(2) 0.23010(2) 0.01469(7) Uani 1 1 d . . P1 P 0.82883(4) 0.80192(2) 0.15349(4) 0.01811(13) Uani 1 1 d . . P2 P 1.02211(4) 0.78406(2) 0.25582(4) 0.02247(14) Uani 1 1 d . . P3 P 0.46754(4) 0.57000(2) 0.28884(4) 0.01874(13) Uani 1 1 d . . P4 P 0.64874(4) 0.51623(2) 0.24875(4) 0.01766(13) Uani 1 1 d . . F1 F 0.43179(10) 0.74643(6) 0.29632(11) 0.0405(4) Uani 1 1 d . . F2 F 0.50621(9) 0.81954(6) 0.24999(11) 0.0391(4) Uani 1 1 d . . F3 F 0.36056(9) 0.82074(6) 0.22909(12) 0.0489(5) Uani 1 1 d . . F4 F 1.11334(10) 0.54614(8) 0.44222(11) 0.0573(5) Uani 1 1 d . . F5 F 1.05998(9) 0.63612(7) 0.42360(10) 0.0398(4) Uani 1 1 d . . F6 F 0.96961(9) 0.56093(7) 0.42589(11) 0.0445(4) Uani 1 1 d . . 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 C1 0.0126(10) 0.0167(10) 0.0320(15) 0.0099(9) 0.0010(9) -0.0037(8) C2 0.0208(12) 0.0283(12) 0.0321(16) 0.0068(10) -0.0008(10) -0.0034(10) C3 0.0351(15) 0.0415(15) 0.0365(18) 0.0134(12) -0.0092(12) -0.0140(12) C4 0.0252(14) 0.0436(16) 0.065(2) 0.0288(16) -0.0187(14) -0.0075(12) C5 0.0163(12) 0.0318(14) 0.067(2) 0.0208(14) -0.0018(13) 0.0001(10) C6 0.0128(11) 0.0193(11) 0.0490(18) 0.0127(11) 0.0028(11) -0.0029(9) C7 0.0152(10) 0.0136(10) 0.0295(14) 0.0030(9) 0.0032(9) -0.0022(8) C8 0.0166(11) 0.0230(11) 0.0348(16) 0.0007(10) 0.0029(10) 0.0018(9) C9 0.0217(12) 0.0296(13) 0.0467(18) -0.0086(12) 0.0122(12) -0.0024(10) C10 0.0202(12) 0.0204(12) 0.065(2) -0.0033(12) 0.0149(13) 0.0035(10) C11 0.0176(12) 0.0181(11) 0.057(2) 0.0065(11) 0.0032(12) 0.0027(9) C12 0.0149(11) 0.0180(11) 0.0372(16) 0.0067(10) 0.0007(10) -0.0005(9) C13 0.0189(12) 0.0178(11) 0.068(2) 0.0091(12) 0.0159(12) 0.0041(9) C14 0.0199(12) 0.0366(14) 0.0428(18) 0.0159(12) -0.0042(11) 0.0073(10) C15 0.0153(10) 0.0116(9) 0.0248(13) 0.0024(8) 0.0019(9) -0.0013(8) C16 0.0155(10) 0.0138(10) 0.0179(13) 0.0025(8) 0.0018(9) -0.0023(8) C17 0.0168(10) 0.0073(9) 0.0203(13) 0.0027(8) 0.0014(9) -0.0025(8) C18 0.0140(10) 0.0116(9) 0.0223(13) 0.0026(8) 0.0019(9) -0.0016(8) C19 0.0139(10) 0.0148(10) 0.0231(13) 0.0054(9) 0.0038(9) -0.0001(8) C20 0.0175(11) 0.0155(10) 0.0352(16) 0.0018(9) 0.0028(10) 0.0022(8) C21 0.0268(12) 0.0247(12) 0.0373(17) -0.0022(10) 0.0087(11) 0.0041(10) C22 0.0276(13) 0.0270(12) 0.0497(19) 0.0059(12) 0.0024(12) 0.0109(10) C23 0.0219(11) 0.0226(11) 0.0248(14) 0.0099(9) 0.0012(10) 0.0001(9) C24 0.0330(14) 0.0346(13) 0.0223(15) 0.0045(10) 0.0007(11) -0.0063(11) C25 0.0298(14) 0.0516(16) 0.0285(16) 0.0050(12) 0.0062(11) 0.0015(12) C26 0.0123(11) 0.0309(13) 0.0533(19) 0.0045(12) 0.0053(11) -0.0043(9) C27 0.0259(13) 0.0442(16) 0.058(2) 0.0019(14) 0.0165(13) 0.0022(12) C28 0.0164(12) 0.0350(14) 0.064(2) 0.0020(13) -0.0014(12) 0.0002(10) C29 0.0296(13) 0.0271(12) 0.0348(16) 0.0019(11) -0.0044(11) -0.0063(10) C30 0.0441(16) 0.0391(15) 0.0365(18) -0.0046(12) 0.0020(13) -0.0024(12) C31 0.0383(15) 0.0378(15) 0.053(2) -0.0042(13) -0.0133(14) -0.0131(12) C32 0.0219(12) 0.0211(11) 0.0391(16) 0.0061(10) 0.0028(11) -0.0072(9) C33 0.0242(12) 0.0151(10) 0.0360(16) 0.0072(10) 0.0014(11) -0.0023(9) C34 0.0146(11) 0.0289(12) 0.0302(15) 0.0041(10) 0.0021(10) -0.0054(9) C35 0.0208(12) 0.0348(14) 0.0473(19) 0.0077(12) -0.0058(12) -0.0020(10) C36 0.0264(13) 0.0342(13) 0.0415(18) -0.0026(12) -0.0062(12) -0.0060(11) C37 0.0183(11) 0.0236(11) 0.0289(15) 0.0025(10) 0.0059(10) 0.0009(9) C38 0.0361(14) 0.0402(14) 0.0410(18) 0.0040(12) 0.0214(13) -0.0007(12) C39 0.0296(13) 0.0342(13) 0.0324(16) -0.0063(11) 0.0038(11) 0.0034(11) C40 0.0270(12) 0.0160(10) 0.0282(15) -0.0031(9) 0.0023(10) 0.0025(9) C41 0.0378(15) 0.0356(14) 0.0324(17) -0.0136(11) 0.0006(12) 0.0007(11) C42 0.0363(14) 0.0278(12) 0.0307(16) -0.0054(11) 0.0111(12) 0.0025(11) C43 0.0203(11) 0.0154(10) 0.0240(14) 0.0005(9) 0.0004(9) 0.0025(8) C44 0.0226(12) 0.0236(11) 0.0249(14) -0.0006(9) -0.0002(10) 0.0011(9) C45 0.0309(13) 0.0266(12) 0.0375(17) -0.0013(11) -0.0042(12) 0.0120(10) C46 0.0253(12) 0.0133(10) 0.0319(15) 0.0039(9) 0.0004(10) -0.0009(9) C47 0.0216(11) 0.0191(11) 0.0290(15) 0.0087(9) 0.0045(10) -0.0034(9) O7 0.0186(8) 0.0207(7) 0.0198(10) -0.0015(6) 0.0011(6) 0.0006(6) Ni1 0.01171(13) 0.01358(13) 0.02182(17) 0.00238(11) 0.00147(11) -0.00048(10) Ni2 0.01259(13) 0.01215(13) 0.01919(17) 0.00159(10) 0.00203(11) -0.00039(10) P1 0.0153(3) 0.0145(3) 0.0242(4) 0.0039(2) 0.0020(2) -0.0003(2) P2 0.0145(3) 0.0197(3) 0.0321(4) 0.0030(2) 0.0004(2) -0.0034(2) P3 0.0142(3) 0.0174(3) 0.0245(4) 0.0039(2) 0.0028(2) -0.0023(2) P4 0.0179(3) 0.0124(3) 0.0220(3) -0.0004(2) 0.0011(2) 0.0005(2) F1 0.0483(9) 0.0244(7) 0.0547(11) 0.0043(7) 0.0263(8) 0.0068(6) F2 0.0220(7) 0.0261(7) 0.0709(12) -0.0058(7) 0.0122(7) -0.0017(6) F3 0.0238(7) 0.0272(7) 0.0993(15) 0.0051(8) 0.0204(8) 0.0122(6) F4 0.0406(9) 0.0754(12) 0.0511(12) 0.0225(9) -0.0074(8) 0.0303(8) F5 0.0304(8) 0.0490(9) 0.0380(10) -0.0032(7) -0.0005(7) -0.0016(7) F6 0.0307(8) 0.0573(10) 0.0464(11) 0.0246(8) 0.0088(7) 0.0010(7) 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 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.006 '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' P P 0.1023 0.0942 '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' loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist 1 -26 12 0.0881 0 26 -12 0.1395 -20 6 9 0.1702 20 -6 -9 0.1702 5 23 13 0.0516 -5 -23 -13 0.0516 8 -6 18 0.0676 -5 26 -10 0.1478 loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle C2 C1 C6 116.4(2) C2 C1 C15 120.5(2) C6 C1 C15 123.1(2) C3 C2 C1 122.1(2) C3 C2 H2 118.9 C1 C2 H2 118.9 C4 C3 C2 119.9(3) C4 C3 H3 120 C2 C3 H3 120 C5 C4 C3 119.9(2) C5 C4 H4 120.1 C3 C4 H4 120.1 C4 C5 C6 120.7(3) C4 C5 H5 119.6 C6 C5 H5 119.6 C5 C6 C1 120.9(3) C5 C6 C13 117.7(2) C1 C6 C13 121.4(2) C8 C7 C12 116.0(2) C8 C7 C19 121.24(19) C12 C7 C19 122.7(2) C9 C8 C7 122.9(2) C9 C8 H8 118.6 C7 C8 H8 118.6 C10 C9 C8 119.9(3) C10 C9 H9 120 C8 C9 H9 120 C11 C10 C9 119.0(2) C11 C10 H10 120.5 C9 C10 H10 120.5 C10 C11 C12 121.6(2) C10 C11 H11 119.2 C12 C11 H11 119.2 C11 C12 C7 120.6(2) C11 C12 C14 118.1(2) C7 C12 C14 121.3(2) F1 C13 F2 105.6(2) F1 C13 F3 104.8(2) F2 C13 F3 105.21(17) F1 C13 C6 113.54(19) F2 C13 C6 113.5(2) F3 C13 C6 113.4(2) F6 C14 F4 105.5(2) F6 C14 F5 105.1(2) F4 C14 F5 105.0(2) F6 C14 C12 113.9(2) F4 C14 C12 112.7(2) F5 C14 C12 113.8(2) C16 C15 C1 121.2(2) C16 C15 Ni2 68.36(10) C1 C15 Ni2 114.85(14) C16 C15 H15 114.8 C1 C15 H15 114.8 Ni2 C15 H15 114.8 C15 C16 C17 120.5(2) C15 C16 Ni2 69.10(11) C17 C16 Ni2 106.00(14) C15 C16 H16 116.9 C17 C16 H16 116.9 Ni2 C16 H16 116.9 O7 C17 C18 122.92(18) O7 C17 C16 122.41(19) C18 C17 C16 114.67(19) C19 C18 C17 121.3(2) C19 C18 Ni1 69.47(11) C17 C18 Ni1 109.65(13) C19 C18 H18 115.8 C17 C18 H18 115.8 Ni1 C18 H18 115.8 C18 C19 C7 120.5(2) C18 C19 Ni1 67.78(10) C7 C19 Ni1 117.87(15) C18 C19 H19 114.3 C7 C19 H19 114.3 Ni1 C19 H19 114.3 C21 C20 C22 111.45(19) C21 C20 P1 111.05(15) C22 C20 P1 114.00(17) C21 C20 H20 106.6 C22 C20 H20 106.6 P1 C20 H20 106.6 C20 C21 H21A 109.5 C20 C21 H21B 109.5 H21A C21 H21B 109.5 C20 C21 H21C 109.5 H21A C21 H21C 109.5 H21B C21 H21C 109.5 C20 C22 H22A 109.5 C20 C22 H22B 109.5 H22A C22 H22B 109.5 C20 C22 H22C 109.5 H22A C22 H22C 109.5 H22B C22 H22C 109.5 C25 C23 C24 110.6(2) C25 C23 P1 109.69(16) C24 C23 P1 112.02(16) C25 C23 H23 108.1 C24 C23 H23 108.1 P1 C23 H23 108.1 C23 C24 H24A 109.5 C23 C24 H24B 109.5 H24A C24 H24B 109.5 C23 C24 H24C 109.5 H24A C24 H24C 109.5 H24B C24 H24C 109.5 C23 C25 H25A 109.5 C23 C25 H25B 109.5 H25A C25 H25B 109.5 C23 C25 H25C 109.5 H25A C25 H25C 109.5 H25B C25 H25C 109.5 C27 C26 C28 110.2(2) C27 C26 P2 111.24(16) C28 C26 P2 110.58(18) C27 C26 H26 108.2 C28 C26 H26 108.2 P2 C26 H26 108.2 C26 C27 H27A 109.5 C26 C27 H27B 109.5 H27A C27 H27B 109.5 C26 C27 H27C 109.5 H27A C27 H27C 109.5 H27B C27 H27C 109.5 C26 C28 H28A 109.5 C26 C28 H28B 109.5 H28A C28 H28B 109.5 C26 C28 H28C 109.5 H28A C28 H28C 109.5 H28B C28 H28C 109.5 C30 C29 C31 109.4(2) C30 C29 P2 110.30(17) C31 C29 P2 115.8(2) C30 C29 H29 107 C31 C29 H29 107 P2 C29 H29 107 C29 C30 H30A 109.5 C29 C30 H30B 109.5 H30A C30 H30B 109.5 C29 C30 H30C 109.5 H30A C30 H30C 109.5 H30B C30 H30C 109.5 C29 C31 H31A 109.5 C29 C31 H31B 109.5 H31A C31 H31B 109.5 C29 C31 H31C 109.5 H31A C31 H31C 109.5 H31B C31 H31C 109.5 C33 C32 P2 112.34(15) C33 C32 H32A 109.1 P2 C32 H32A 109.1 C33 C32 H32B 109.1 P2 C32 H32B 109.1 H32A C32 H32B 107.9 C32 C33 P1 111.99(14) C32 C33 H33A 109.2 P1 C33 H33A 109.2 C32 C33 H33B 109.2 P1 C33 H33B 109.2 H33A C33 H33B 107.9 C36 C34 C35 109.8(2) C36 C34 P3 112.33(16) C35 C34 P3 109.85(15) C36 C34 H34 108.2 C35 C34 H34 108.2 P3 C34 H34 108.2 C34 C35 H35A 109.5 C34 C35 H35B 109.5 H35A C35 H35B 109.5 C34 C35 H35C 109.5 H35A C35 H35C 109.5 H35B C35 H35C 109.5 C34 C36 H36A 109.5 C34 C36 H36B 109.5 H36A C36 H36B 109.5 C34 C36 H36C 109.5 H36A C36 H36C 109.5 H36B C36 H36C 109.5 C39 C37 C38 110.7(2) C39 C37 P3 109.44(15) C38 C37 P3 115.31(16) C39 C37 H37 107 C38 C37 H37 107 P3 C37 H37 107 C37 C38 H38A 109.5 C37 C38 H38B 109.5 H38A C38 H38B 109.5 C37 C38 H38C 109.5 H38A C38 H38C 109.5 H38B C38 H38C 109.5 C37 C39 H39A 109.5 C37 C39 H39B 109.5 H39A C39 H39B 109.5 C37 C39 H39C 109.5 H39A C39 H39C 109.5 H39B C39 H39C 109.5 C41 C40 C42 109.6(2) C41 C40 P4 110.91(16) C42 C40 P4 110.69(15) C41 C40 H40 108.5 C42 C40 H40 108.5 P4 C40 H40 108.5 C40 C41 H41A 109.5 C40 C41 H41B 109.5 H41A C41 H41B 109.5 C40 C41 H41C 109.5 H41A C41 H41C 109.5 H41B C41 H41C 109.5 C40 C42 H42A 109.5 C40 C42 H42B 109.5 H42A C42 H42B 109.5 C40 C42 H42C 109.5 H42A C42 H42C 109.5 H42B C42 H42C 109.5 C44 C43 C45 110.90(19) C44 C43 P4 110.26(14) C45 C43 P4 114.73(15) C44 C43 H43 106.8 C45 C43 H43 106.8 P4 C43 H43 106.8 C43 C44 H44A 109.5 C43 C44 H44B 109.5 H44A C44 H44B 109.5 C43 C44 H44C 109.5 H44A C44 H44C 109.5 H44B C44 H44C 109.5 C43 C45 H45A 109.5 C43 C45 H45B 109.5 H45A C45 H45B 109.5 C43 C45 H45C 109.5 H45A C45 H45C 109.5 H45B C45 H45C 109.5 C47 C46 P4 111.06(14) C47 C46 H46A 109.4 P4 C46 H46A 109.4 C47 C46 H46B 109.4 P4 C46 H46B 109.4 H46A C46 H46B 108 C46 C47 P3 111.92(16) C46 C47 H47A 109.2 P3 C47 H47A 109.2 C46 C47 H47B 109.2 P3 C47 H47B 109.2 H47A C47 H47B 107.9 C18 Ni1 C19 42.75(8) C18 Ni1 P1 108.93(6) C19 Ni1 P1 151.48(6) C18 Ni1 P2 159.50(6) C19 Ni1 P2 117.02(6) P1 Ni1 P2 91.44(2) C16 Ni2 C15 42.54(8) C16 Ni2 P3 155.18(6) C15 Ni2 P3 112.91(6) C16 Ni2 P4 112.08(6) C15 Ni2 P4 154.27(6) P3 Ni2 P4 91.96(2) C23 P1 C20 104.63(11) C23 P1 C33 103.68(11) C20 P1 C33 102.85(10) C23 P1 Ni1 118.08(7) C20 P1 Ni1 117.79(8) C33 P1 Ni1 107.91(7) C26 P2 C29 103.52(12) C26 P2 C32 100.99(11) C29 P2 C32 103.56(11) C26 P2 Ni1 120.40(8) C29 P2 Ni1 118.68(8) C32 P2 Ni1 107.12(7) C47 P3 C37 102.09(11) C47 P3 C34 104.87(10) C37 P3 C34 103.16(10) C47 P3 Ni2 105.61(7) C37 P3 Ni2 118.65(7) C34 P3 Ni2 120.27(8) C40 P4 C46 103.58(10) C40 P4 C43 104.18(10) C46 P4 C43 103.83(10) C40 P4 Ni2 120.52(8) C46 P4 Ni2 107.32(7) C43 P4 Ni2 115.61(7) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance C1 C2 1.401(3) C1 C6 1.412(3) C1 C15 1.477(3) C2 C3 1.386(3) C2 H2 0.95 C3 C4 1.383(4) C3 H3 0.95 C4 C5 1.364(4) C4 H4 0.95 C5 C6 1.398(3) C5 H5 0.95 C6 C13 1.482(4) C7 C8 1.400(3) C7 C12 1.415(3) C7 C19 1.477(3) C8 C9 1.386(3) C8 H8 0.95 C9 C10 1.381(4) C9 H9 0.95 C10 C11 1.378(4) C10 H10 0.95 C11 C12 1.393(3) C11 H11 0.95 C12 C14 1.483(4) C13 F1 1.346(3) C13 F2 1.348(3) C13 F3 1.351(3) C14 F6 1.345(3) C14 F4 1.347(3) C14 F5 1.350(3) C15 C16 1.437(3) C15 Ni2 1.9860(19) C15 H15 1 C16 C17 1.477(3) C16 Ni2 1.9760(19) C16 H16 1 C17 O7 1.234(3) C17 C18 1.475(3) C18 C19 1.445(3) C18 Ni1 1.9703(18) C18 H18 1 C19 Ni1 1.9933(19) C19 H19 1 C20 C21 1.525(4) C20 C22 1.529(3) C20 P1 1.846(2) C20 H20 1 C21 H21A 0.98 C21 H21B 0.98 C21 H21C 0.98 C22 H22A 0.98 C22 H22B 0.98 C22 H22C 0.98 C23 C25 1.525(3) C23 C24 1.525(3) C23 P1 1.841(2) C23 H23 1 C24 H24A 0.98 C24 H24B 0.98 C24 H24C 0.98 C25 H25A 0.98 C25 H25B 0.98 C25 H25C 0.98 C26 C27 1.526(4) C26 C28 1.529(3) C26 P2 1.852(2) C26 H26 1 C27 H27A 0.98 C27 H27B 0.98 C27 H27C 0.98 C28 H28A 0.98 C28 H28B 0.98 C28 H28C 0.98 C29 C30 1.527(4) C29 C31 1.533(3) C29 P2 1.858(3) C29 H29 1 C30 H30A 0.98 C30 H30B 0.98 C30 H30C 0.98 C31 H31A 0.98 C31 H31B 0.98 C31 H31C 0.98 C32 C33 1.528(3) C32 P2 1.858(2) C32 H32A 0.99 C32 H32B 0.99 C33 P1 1.854(2) C33 H33A 0.99 C33 H33B 0.99 C34 C36 1.521(3) C34 C35 1.525(3) C34 P3 1.858(2) C34 H34 1 C35 H35A 0.98 C35 H35B 0.98 C35 H35C 0.98 C36 H36A 0.98 C36 H36B 0.98 C36 H36C 0.98 C37 C39 1.529(3) C37 C38 1.533(3) C37 P3 1.855(2) C37 H37 1 C38 H38A 0.98 C38 H38B 0.98 C38 H38C 0.98 C39 H39A 0.98 C39 H39B 0.98 C39 H39C 0.98 C40 C41 1.523(3) C40 C42 1.529(3) C40 P4 1.853(2) C40 H40 1 C41 H41A 0.98 C41 H41B 0.98 C41 H41C 0.98 C42 H42A 0.98 C42 H42B 0.98 C42 H42C 0.98 C43 C44 1.526(3) C43 C45 1.534(3) C43 P4 1.856(2) C43 H43 1 C44 H44A 0.98 C44 H44B 0.98 C44 H44C 0.98 C45 H45A 0.98 C45 H45B 0.98 C45 H45C 0.98 C46 C47 1.535(3) C46 P4 1.854(2) C46 H46A 0.99 C46 H46B 0.99 C47 P3 1.851(2) C47 H47A 0.99 C47 H47B 0.99 Ni1 P1 2.1572(6) Ni1 P2 2.1644(6) Ni2 P3 2.1554(6) Ni2 P4 2.1572(6) 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 C6 C1 C2 C3 0.1(3) C15 C1 C2 C3 179.1(2) C1 C2 C3 C4 -0.5(4) C2 C3 C4 C5 0.4(4) C3 C4 C5 C6 0.1(4) C4 C5 C6 C1 -0.5(3) C4 C5 C6 C13 179.1(2) C2 C1 C6 C5 0.4(3) C15 C1 C6 C5 -178.6(2) C2 C1 C6 C13 -179.2(2) C15 C1 C6 C13 1.8(3) C12 C7 C8 C9 0.8(3) C19 C7 C8 C9 -178.36(19) C7 C8 C9 C10 -0.9(3) C8 C9 C10 C11 0.4(3) C9 C10 C11 C12 0.2(3) C10 C11 C12 C7 -0.2(3) C10 C11 C12 C14 179.7(2) C8 C7 C12 C11 -0.3(3) C19 C7 C12 C11 178.93(19) C8 C7 C12 C14 179.8(2) C19 C7 C12 C14 -1.0(3) C5 C6 C13 F1 123.8(2) C1 C6 C13 F1 -56.6(3) C5 C6 C13 F2 -115.7(2) C1 C6 C13 F2 63.9(3) C5 C6 C13 F3 4.3(3) C1 C6 C13 F3 -176.13(18) C11 C12 C14 F6 -118.1(2) C7 C12 C14 F6 61.9(3) C11 C12 C14 F4 2.0(3) C7 C12 C14 F4 -178.00(19) C11 C12 C14 F5 121.5(2) C7 C12 C14 F5 -58.6(3) C2 C1 C15 C16 23.9(3) C6 C1 C15 C16 -157.19(19) C2 C1 C15 Ni2 -54.9(2) C6 C1 C15 Ni2 124.05(18) C1 C15 C16 C17 156.49(18) Ni2 C15 C16 C17 -96.74(17) C1 C15 C16 Ni2 -106.77(18) C15 C16 C17 O7 15.6(3) Ni2 C16 C17 O7 -59.3(2) C15 C16 C17 C18 -164.43(17) Ni2 C16 C17 C18 120.74(15) O7 C17 C18 C19 14.6(3) C16 C17 C18 C19 -165.39(17) O7 C17 C18 Ni1 -62.8(2) C16 C17 C18 Ni1 117.25(15) C17 C18 C19 C7 148.68(18) Ni1 C18 C19 C7 -110.21(18) C17 C18 C19 Ni1 -101.11(17) C8 C7 C19 C18 24.3(3) C12 C7 C19 C18 -154.86(19) C8 C7 C19 Ni1 -55.0(2) C12 C7 C19 Ni1 125.81(19) P2 C32 C33 P1 -33.7(2) P4 C46 C47 P3 37.9(2) C25 C23 P1 C20 174.89(16) C24 C23 P1 C20 -61.84(18) C25 C23 P1 C33 67.42(17) C24 C23 P1 C33 -169.31(16) C25 C23 P1 Ni1 -51.84(17) C24 C23 P1 Ni1 71.44(17) C21 C20 P1 C23 179.93(15) C22 C20 P1 C23 -53.19(19) C21 C20 P1 C33 -71.99(17) C22 C20 P1 C33 54.9(2) C21 C20 P1 Ni1 46.49(17) C22 C20 P1 Ni1 173.37(14) C32 C33 P1 C23 -100.77(19) C32 C33 P1 C20 150.43(18) C32 C33 P1 Ni1 25.2(2) C27 C26 P2 C29 -178.62(17) C28 C26 P2 C29 58.53(19) C27 C26 P2 C32 -71.63(19) C28 C26 P2 C32 165.53(18) C27 C26 P2 Ni1 45.9(2) C28 C26 P2 Ni1 -76.97(19) C30 C29 P2 C26 166.08(17) C31 C29 P2 C26 41.1(2) C30 C29 P2 C32 61.02(19) C31 C29 P2 C32 -63.9(2) C30 C29 P2 Ni1 -57.47(19) C31 C29 P2 Ni1 177.57(15) C33 C32 P2 C26 154.25(18) C33 C32 P2 C29 -98.78(19) C33 C32 P2 Ni1 27.4(2) C46 C47 P3 C37 -158.95(16) C46 C47 P3 C34 93.73(17) C46 C47 P3 Ni2 -34.28(17) C39 C37 P3 C47 74.73(17) C38 C37 P3 C47 -50.77(19) C39 C37 P3 C34 -176.64(16) C38 C37 P3 C34 57.86(19) C39 C37 P3 Ni2 -40.78(18) C38 C37 P3 Ni2 -166.27(15) C36 C34 P3 C47 -54.9(2) C35 C34 P3 C47 -177.45(18) C36 C34 P3 C37 -161.42(17) C35 C34 P3 C37 76.02(19) C36 C34 P3 Ni2 63.62(18) C35 C34 P3 Ni2 -58.93(19) C41 C40 P4 C46 69.91(18) C42 C40 P4 C46 -168.25(16) C41 C40 P4 C43 178.25(17) C42 C40 P4 C43 -59.91(18) C41 C40 P4 Ni2 -49.96(19) C42 C40 P4 Ni2 71.88(17) C47 C46 P4 C40 -153.07(16) C47 C46 P4 C43 98.33(17) C47 C46 P4 Ni2 -24.56(18) C44 C43 P4 C40 -172.47(15) C45 C43 P4 C40 -46.4(2) C44 C43 P4 C46 -64.32(16) C45 C43 P4 C46 61.7(2) C44 C43 P4 Ni2 52.95(16) C45 C43 P4 Ni2 179.01(15)