#------------------------------------------------------------------------------ #$Date: 2019-11-08 01:51:13 +0200 (Fri, 08 Nov 2019) $ #$Revision: 224592 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/55/04/1550435.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_1550435 loop_ _publ_author_name 'Viertl, Wolfgang' 'Pann, Johann' 'Pehn, Richard' 'Roithmeyer, Helena' 'Bendig, Marvin' 'Rodr\'iguez-Villal\'on, Alba' 'Bereiter, Raphael' 'Heiderscheid, Max' 'M\"uller, Thomas' 'Zhao, Xia' 'Hofer, Thomas S.' 'Thompson, Mark E.' 'Shi, Shuyang' 'Brueggeller, Peter' _publ_section_title ; Performance of enhanced DuBois type water reduction catalysts (WRC) in artificial photosynthesis - effects of various proton relays during catalysis. ; _journal_issue 0 _journal_name_full 'Faraday discussions' _journal_page_first 141 _journal_page_last 161 _journal_paper_doi 10.1039/c8fd00162f _journal_volume 215 _journal_year 2019 _chemical_formula_moiety 'C33 H39 Cl2 N Ni O4 P2, 2(C H Cl3)' _chemical_formula_sum 'C35 H41 Cl8 N Ni O4 P2' _chemical_formula_weight 943.92 _chemical_name_systematic '[NiCl2(PNP-C1-iPr)]' _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_Hall '-P 2ybc' _space_group_name_H-M_alt 'P 1 21/c 1' _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_space_group_name_H-M 'P 1 21/c 1' _atom_sites_solution_hydrogens geom _audit_creation_method SHELXL-2014/7 _audit_update_record ; 2018-10-23 deposited with the CCDC. 2019-01-03 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 101.2322(4) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 11.7989(2) _cell_length_b 15.5485(2) _cell_length_c 23.5593(3) _cell_measurement_reflns_used 9393 _cell_measurement_temperature 173(2) _cell_measurement_theta_max 32.51 _cell_measurement_theta_min 2.19 _cell_volume 4239.29(11) _computing_cell_refinement 'Bruker SAINT-V 8.34A' _computing_data_collection 'Bruker Apex II' _computing_data_reduction 'Bruker SAINT-V 8.34A' _computing_molecular_graphics SHELXLE _computing_publication_material SHELXL-2014/7 _computing_structure_refinement 'SHELXL-2014/7 (Sheldrick, 2014)' _computing_structure_solution 'Bruker Apex II' _diffrn_ambient_temperature 173(2) _diffrn_detector_area_resol_mean 10.4 _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.999 _diffrn_measurement_device_type 'Bruker D8 QUEST PHOTON 100' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0288 _diffrn_reflns_av_unetI/netI 0.0121 _diffrn_reflns_Laue_measured_fraction_full 0.999 _diffrn_reflns_Laue_measured_fraction_max 0.999 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_number 87387 _diffrn_reflns_point_group_measured_fraction_full 0.999 _diffrn_reflns_point_group_measured_fraction_max 0.999 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 25.250 _diffrn_reflns_theta_min 2.194 _diffrn_source 'Incoatec Microfocus' _exptl_absorpt_coefficient_mu 1.075 _exptl_absorpt_correction_T_max 0.815 _exptl_absorpt_correction_T_min 0.815 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'Bruker SADABS-2014/5' _exptl_crystal_colour red _exptl_crystal_density_diffrn 1.479 _exptl_crystal_density_method 'not measured' _exptl_crystal_description prism _exptl_crystal_F_000 1936 _exptl_crystal_size_max 0.180 _exptl_crystal_size_mid 0.180 _exptl_crystal_size_min 0.180 _exptl_transmission_factor_max 0.815 _exptl_transmission_factor_min 0.815 _refine_diff_density_max 0.414 _refine_diff_density_min -0.569 _refine_diff_density_rms 0.049 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.035 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 466 _refine_ls_number_reflns 7578 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.035 _refine_ls_R_factor_all 0.0269 _refine_ls_R_factor_gt 0.0242 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0361P)^2^+1.7555P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0619 _refine_ls_wR_factor_ref 0.0637 _reflns_Friedel_coverage 0.000 _reflns_number_gt 6994 _reflns_number_total 7675 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file c8fd00162f2.cif _cod_data_source_block 5c _cod_depositor_comments 'Adding full bibliography for 1550432--1550436.cif.' _cod_database_code 1550435 _shelx_shelxl_version_number 2014/7 _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 0.815 _shelx_estimated_absorpt_t_max 0.815 _exptl_absorpt_special_details 'Bruker SADABS-2014/5' _shelx_res_file ; pycy.res created by SHELXL-2014/7 TITL pycy_0m_a.res in P2(1)/c REM Old TITL pycy_0m in P2(1)/c REM SHELXT solution in P2(1)/c REM R1 0.168, Rweak 0.005, Alpha 0.041, Orientation as input REM Formula found by SHELXT: C35 N O4 P10 Br CELL 0.71073 11.7986 15.5481 23.5589 90.000 101.232 90.000 ZERR 8.000 0.0005 0.0007 0.0009 0.000 0.001 0.000 LATT 1 SYMM -X, 1/2+Y, 1/2-Z SFAC C H CL N Ni O P UNIT 280 328 64 8 8 32 16 TEMP -100.150 SIZE 0.18 0.18 0.18 OMIT -1 50.5 OMIT -1 3 9 OMIT 0 2 12 OMIT -5 4 6 OMIT 3 2 6 OMIT 4 3 3 OMIT 2 5 0 OMIT 3 0 6 OMIT -4 7 7 OMIT 2 7 5 OMIT -6 2 9 OMIT -2 2 15 OMIT 1 8 2 OMIT 1 6 4 OMIT -6 10 5 OMIT -4 0 12 OMIT 3 1 11 OMIT 0 3 7 OMIT -2 4 10 OMIT -1 13 2 OMIT 0 0 4 OMIT 1 7 1 OMIT 4 22 0 OMIT 2 8 1 OMIT -4 12 1 OMIT -5 11 9 OMIT -2 0 4 OMIT -14 4 23 OMIT 2 8 5 OMIT 2 5 7 OMIT 7 2 0 OMIT 2 9 16 OMIT 0 3 14 OMIT 6 7 29 OMIT -4 3 12 OMIT 17 2 1 OMIT 0 10 10 OMIT 16 1 3 OMIT -4 0 34 OMIT 0 3 6 OMIT 11 12 15 OMIT -1 9 19 OMIT -6 0 2 OMIT -2 12 5 OMIT -5 2 6 OMIT -2 1 16 OMIT -6 4 4 OMIT 2 0 12 OMIT 3 3 7 OMIT -4 9 13 OMIT 1 2 14 OMIT -2 0 12 OMIT -4 4 7 OMIT -3 4 8 OMIT -5 3 11 OMIT -4 1 11 OMIT 4 5 8 OMIT 7 0 6 OMIT 2 4 10 OMIT -3 6 3 OMIT -2 7 4 OMIT -1 7 1 OMIT 1 1 11 OMIT -3 5 7 OMIT 0 8 1 OMIT 5 5 5 OMIT -2 5 6 OMIT 6 1 2 OMIT -4 6 1 OMIT 0 10 5 OMIT -3 6 1 OMIT -1 9 3 OMIT 0 2 0 OMIT -3 5 9 OMIT -3 0 4 OMIT -9 12 6 OMIT 6 7 12 OMIT -7 9 11 OMIT -6 15 3 OMIT 2 5 11 OMIT -6 1 2 OMIT -1 0 16 OMIT -4 2 6 OMIT 0 0 8 OMIT 1 1 1 OMIT -5 13 9 OMIT -5 3 4 OMIT 2 6 4 OMIT -8 10 5 OMIT 0 7 1 OMIT 2 4 2 OMIT 3 5 2 OMIT -5 11 2 OMIT -5 13 3 OMIT 3 0 0 OMIT 2 7 2 OMIT -3 6 7 OMIT -1 5 7 OMIT -6 1 5 OMIT 1 1 2 OMIT -7 8 13 L.S. 10 ACTA CONF BOND $H LIST 6 FMAP 2 PLAN 10 WGHT 0.036100 1.755500 FVAR 0.28527 NI1 5 0.472080 0.321047 0.299221 11.00000 0.01480 0.01908 = 0.01268 -0.00011 0.00099 0.00051 CL1 3 0.451394 0.339731 0.204811 11.00000 0.02432 0.04645 = 0.01378 0.00171 0.00039 0.00348 CL2 3 0.283750 0.318435 0.293287 11.00000 0.01609 0.04671 = 0.02471 -0.00467 0.00103 0.00120 P1 7 0.657573 0.328607 0.302899 11.00000 0.01658 0.01851 = 0.01352 0.00115 0.00275 -0.00008 P2 7 0.487320 0.302573 0.391747 11.00000 0.01603 0.01699 = 0.01393 0.00008 0.00278 -0.00056 O1 6 0.892508 0.400165 0.302670 11.00000 0.02133 0.03864 = 0.04023 0.00797 0.00620 -0.00591 O2 6 0.667883 0.145376 0.295944 11.00000 0.04700 0.02063 = 0.05168 -0.00102 0.01022 -0.00050 O3 6 0.523857 0.486623 0.409069 11.00000 0.03420 0.01942 = 0.02744 -0.00238 0.01048 -0.00463 O4 6 0.463222 0.224439 0.507157 11.00000 0.03880 0.02742 = 0.01658 0.00315 0.00953 0.00018 N1 4 0.706268 0.251134 0.411269 11.00000 0.01718 0.02223 = 0.01698 0.00494 0.00289 0.00300 C1 1 0.760018 0.297296 0.370089 11.00000 0.01542 0.02639 = 0.01842 0.00409 0.00138 0.00002 AFIX 23 H1A 2 0.821486 0.260816 0.359516 11.00000 -1.20000 H1B 2 0.797128 0.349849 0.388896 11.00000 -1.20000 AFIX 0 C2 1 0.632711 0.308261 0.437461 11.00000 0.01894 0.02392 = 0.01419 0.00008 0.00119 -0.00048 AFIX 23 H2A 2 0.662449 0.367922 0.438892 11.00000 -1.20000 H2B 2 0.630606 0.289424 0.477383 11.00000 -1.20000 AFIX 0 C3 1 0.792302 0.201229 0.452725 11.00000 0.02269 0.03670 = 0.02621 0.01370 0.00416 0.00889 AFIX 13 H3 2 0.841061 0.169317 0.429473 11.00000 -1.20000 AFIX 0 C4 1 0.732756 0.134195 0.483716 11.00000 0.03831 0.04375 = 0.04844 0.02859 0.01187 0.01155 AFIX 137 H4A 2 0.679431 0.100349 0.455162 11.00000 -1.50000 H4B 2 0.689568 0.162999 0.509817 11.00000 -1.50000 H4C 2 0.790897 0.096039 0.506138 11.00000 -1.50000 AFIX 0 C5 1 0.873586 0.257079 0.495671 11.00000 0.02838 0.06652 = 0.02878 0.01109 -0.00490 0.00172 AFIX 137 H5A 2 0.913812 0.297538 0.474556 11.00000 -1.50000 H5B 2 0.930295 0.220479 0.520463 11.00000 -1.50000 H5C 2 0.828956 0.289158 0.519629 11.00000 -1.50000 AFIX 0 C11 1 0.697592 0.439733 0.292978 11.00000 0.02843 0.02179 = 0.01449 0.00260 0.00395 -0.00276 C12 1 0.813014 0.464539 0.295241 11.00000 0.03051 0.03057 = 0.02007 0.00514 0.00331 -0.00717 C13 1 0.839696 0.551057 0.289766 11.00000 0.04570 0.03742 = 0.02888 0.00670 0.00160 -0.01911 AFIX 43 H13 2 0.917459 0.568105 0.291001 11.00000 -1.20000 AFIX 0 C14 1 0.752873 0.612014 0.282536 11.00000 0.06984 0.02401 = 0.02374 0.00441 0.00290 -0.01229 AFIX 43 H14 2 0.771622 0.670772 0.278243 11.00000 -1.20000 AFIX 0 C15 1 0.639837 0.589269 0.281434 11.00000 0.05955 0.02385 = 0.02015 0.00392 0.00595 0.00420 AFIX 43 H15 2 0.581252 0.632001 0.277314 11.00000 -1.20000 AFIX 0 C16 1 0.612223 0.502837 0.286431 11.00000 0.03604 0.02551 = 0.01643 0.00256 0.00441 0.00259 AFIX 43 H16 2 0.534166 0.486727 0.285359 11.00000 -1.20000 AFIX 0 C17 1 1.012012 0.421820 0.307630 11.00000 0.02320 0.06700 = 0.06242 0.01592 0.00469 -0.01110 AFIX 137 H17A 2 1.023681 0.449221 0.271748 11.00000 -1.50000 H17B 2 1.058899 0.369445 0.314466 11.00000 -1.50000 H17C 2 1.035235 0.461614 0.340071 11.00000 -1.50000 AFIX 0 C21 1 0.704651 0.267414 0.245836 11.00000 0.01707 0.03266 = 0.02038 -0.00684 0.00245 0.00166 C22 1 0.704777 0.177891 0.249131 11.00000 0.02336 0.03509 = 0.03239 -0.01058 0.00187 0.00116 C23 1 0.740641 0.128737 0.206203 11.00000 0.03210 0.04715 = 0.05579 -0.02940 -0.00060 0.00551 AFIX 43 H23 2 0.741775 0.067728 0.208450 11.00000 -1.20000 AFIX 0 C24 1 0.774567 0.170592 0.160239 11.00000 0.02890 0.08872 = 0.03775 -0.03540 0.00405 0.00544 AFIX 43 H24 2 0.800284 0.137589 0.131251 11.00000 -1.20000 AFIX 0 C25 1 0.771805 0.258521 0.155720 11.00000 0.02856 0.08399 = 0.02390 -0.01421 0.00695 -0.00003 AFIX 43 H25 2 0.793963 0.285887 0.123510 11.00000 -1.20000 AFIX 0 C26 1 0.736567 0.307213 0.198326 11.00000 0.02420 0.05247 = 0.02116 -0.00272 0.00391 -0.00028 AFIX 43 H26 2 0.734129 0.368125 0.195158 11.00000 -1.20000 AFIX 0 C27 1 0.687164 0.056587 0.309740 11.00000 0.04960 0.02422 = 0.09212 0.00814 0.00604 -0.00049 AFIX 137 H27A 2 0.643624 0.021312 0.278456 11.00000 -1.50000 H27B 2 0.661346 0.043694 0.345914 11.00000 -1.50000 H27C 2 0.769770 0.043748 0.314328 11.00000 -1.50000 AFIX 0 C31 1 0.395876 0.376945 0.422178 11.00000 0.02073 0.02286 = 0.01373 -0.00092 0.00226 0.00326 C32 1 0.424314 0.464498 0.426415 11.00000 0.02759 0.02384 = 0.01389 0.00030 0.00230 0.00237 C33 1 0.352067 0.522789 0.446855 11.00000 0.04100 0.02399 = 0.02322 -0.00166 0.00422 0.00902 AFIX 43 H33 2 0.372384 0.581927 0.450622 11.00000 -1.20000 AFIX 0 C34 1 0.250606 0.494254 0.461652 11.00000 0.03638 0.03750 = 0.02927 -0.00162 0.00863 0.01660 AFIX 43 H34 2 0.201466 0.534095 0.475620 11.00000 -1.20000 AFIX 0 C35 1 0.219911 0.408264 0.456323 11.00000 0.02386 0.04356 = 0.02946 0.00125 0.00911 0.00749 AFIX 43 H35 2 0.149556 0.389229 0.466009 11.00000 -1.20000 AFIX 0 C36 1 0.292901 0.350065 0.436686 11.00000 0.02227 0.02860 = 0.02303 -0.00015 0.00342 0.00145 AFIX 43 H36 2 0.272083 0.291007 0.433127 11.00000 -1.20000 AFIX 0 C37 1 0.556032 0.575568 0.412299 11.00000 0.05122 0.02141 = 0.02726 -0.00221 0.00777 -0.01067 AFIX 137 H37A 2 0.631907 0.582163 0.401749 11.00000 -1.50000 H37B 2 0.559674 0.596504 0.451850 11.00000 -1.50000 H37C 2 0.498530 0.608899 0.385509 11.00000 -1.50000 AFIX 0 C41 1 0.442956 0.194834 0.407465 11.00000 0.01759 0.01882 = 0.02080 0.00218 0.00403 0.00117 C42 1 0.434906 0.166315 0.463224 11.00000 0.01933 0.02437 = 0.02298 0.00330 0.00563 0.00295 C43 1 0.400607 0.082582 0.471486 11.00000 0.02751 0.02798 = 0.03066 0.01113 0.00947 0.00178 AFIX 43 H43 2 0.391883 0.064040 0.508818 11.00000 -1.20000 AFIX 0 C44 1 0.379098 0.026028 0.425034 11.00000 0.03220 0.01970 = 0.04299 0.00667 0.00623 -0.00289 AFIX 43 H44 2 0.354635 -0.030961 0.430837 11.00000 -1.20000 AFIX 0 C45 1 0.392649 0.051188 0.370517 11.00000 0.03226 0.02165 = 0.03554 -0.00321 0.00414 -0.00385 AFIX 43 H45 2 0.381495 0.011281 0.339389 11.00000 -1.20000 AFIX 0 C46 1 0.422866 0.135852 0.362038 11.00000 0.02172 0.02249 = 0.02314 0.00083 0.00325 -0.00211 AFIX 43 H46 2 0.430021 0.154021 0.324396 11.00000 -1.20000 AFIX 0 C47 1 0.464218 0.195272 0.565029 11.00000 0.05207 0.03466 = 0.01982 0.00613 0.01385 0.00742 AFIX 137 H47A 2 0.386763 0.175472 0.568057 11.00000 -1.50000 H47B 2 0.487328 0.242687 0.592229 11.00000 -1.50000 H47C 2 0.519243 0.147733 0.574330 11.00000 -1.50000 AFIX 0 CL3 3 1.184122 0.221032 0.081373 11.00000 0.04488 0.04760 = 0.05737 -0.00769 0.00401 0.00830 CL4 3 1.047128 0.297362 0.156964 11.00000 0.03205 0.07926 = 0.04875 0.00532 0.00842 0.00663 CL5 3 1.159185 0.405106 0.084813 11.00000 0.06089 0.04627 = 0.06228 0.00125 0.01615 0.00547 C6 1 1.169449 0.310013 0.125900 11.00000 0.02600 0.04935 = 0.03850 -0.00380 -0.00060 0.00332 AFIX 13 H6 2 1.239433 0.313497 0.157519 11.00000 -1.20000 AFIX 0 CL6 3 1.077218 0.010738 0.351890 11.00000 0.06808 0.05533 = 0.07658 -0.00594 0.01115 -0.01779 CL7 3 0.998901 0.176147 0.304575 11.00000 0.04193 0.07612 = 0.07239 -0.00589 0.01208 0.01752 CL8 3 1.097542 0.159424 0.426186 11.00000 0.04188 0.10404 = 0.06577 -0.03455 0.01311 -0.01601 C7 1 1.101591 0.122266 0.356291 11.00000 0.02699 0.05125 = 0.06046 -0.01230 0.01294 -0.00504 AFIX 13 H7 2 1.180100 0.134118 0.348036 11.00000 -1.20000 AFIX 0 HKLF 4 REM pycy_0m_a.res in P2(1)/c REM R1 = 0.0242 for 6994 Fo > 4sig(Fo) and 0.0269 for all 7578 data REM 466 parameters refined using 0 restraints END WGHT 0.0362 1.7633 REM Highest difference peak 0.414, deepest hole -0.569, 1-sigma level 0.049 Q1 1 1.0746 0.1078 0.4381 11.00000 0.05 0.41 Q2 1 1.0547 0.2077 0.4133 11.00000 0.05 0.26 Q3 1 1.0638 0.0229 0.3863 11.00000 0.05 0.25 Q4 1 0.7071 0.3160 0.3428 11.00000 0.05 0.24 Q5 1 0.6765 0.2940 0.2667 11.00000 0.05 0.23 Q6 1 0.5691 0.3037 0.4170 11.00000 0.05 0.23 Q7 1 0.9623 0.1345 0.3106 11.00000 0.05 0.23 Q8 1 1.1881 0.2489 0.0503 11.00000 0.05 0.20 Q9 1 0.4596 0.2435 0.4010 11.00000 0.05 0.19 Q10 1 0.4150 0.4180 0.4320 11.00000 0.05 0.19 ; _shelx_res_checksum 70797 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' 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 Ni1 Ni 0.47208(2) 0.32105(2) 0.29922(2) 0.01574(6) Uani 1 1 d . . Cl1 Cl 0.45139(3) 0.33973(3) 0.20481(2) 0.02863(9) Uani 1 1 d . . Cl2 Cl 0.28375(3) 0.31844(3) 0.29329(2) 0.02957(9) Uani 1 1 d . . P1 P 0.65757(3) 0.32861(2) 0.30290(2) 0.01623(8) Uani 1 1 d . . P2 P 0.48732(3) 0.30257(2) 0.39175(2) 0.01566(8) Uani 1 1 d . . O1 O 0.89251(9) 0.40017(8) 0.30267(5) 0.0334(3) Uani 1 1 d . . O2 O 0.66788(11) 0.14538(7) 0.29594(6) 0.0397(3) Uani 1 1 d . . O3 O 0.52386(9) 0.48662(6) 0.40907(4) 0.0264(2) Uani 1 1 d . . O4 O 0.46322(10) 0.22444(7) 0.50716(4) 0.0270(2) Uani 1 1 d . . N1 N 0.70627(10) 0.25113(7) 0.41127(5) 0.0189(2) Uani 1 1 d . . C1 C 0.76002(12) 0.29730(9) 0.37009(6) 0.0203(3) Uani 1 1 d . . H1A H 0.8215 0.2608 0.3595 0.024 Uiso 1 1 calc R U H1B H 0.7971 0.3498 0.3889 0.024 Uiso 1 1 calc R U C2 C 0.63271(12) 0.30826(9) 0.43746(6) 0.0193(3) Uani 1 1 d . . H2A H 0.6624 0.3679 0.4389 0.023 Uiso 1 1 calc R U H2B H 0.6306 0.2894 0.4774 0.023 Uiso 1 1 calc R U C3 C 0.79230(13) 0.20123(11) 0.45273(7) 0.0286(3) Uani 1 1 d . . H3 H 0.8411 0.1693 0.4295 0.034 Uiso 1 1 calc R U C4 C 0.73276(16) 0.13419(12) 0.48372(8) 0.0430(4) Uani 1 1 d . . H4A H 0.6794 0.1003 0.4552 0.065 Uiso 1 1 calc R U H4B H 0.6896 0.1630 0.5098 0.065 Uiso 1 1 calc R U H4C H 0.7909 0.0960 0.5061 0.065 Uiso 1 1 calc R U C5 C 0.87359(15) 0.25708(14) 0.49567(7) 0.0426(4) Uani 1 1 d . . H5A H 0.9138 0.2975 0.4746 0.064 Uiso 1 1 calc R U H5B H 0.9303 0.2205 0.5205 0.064 Uiso 1 1 calc R U H5C H 0.8290 0.2892 0.5196 0.064 Uiso 1 1 calc R U C11 C 0.69759(13) 0.43973(9) 0.29298(6) 0.0216(3) Uani 1 1 d . . C12 C 0.81301(14) 0.46454(10) 0.29524(6) 0.0273(3) Uani 1 1 d . . C13 C 0.83970(16) 0.55106(12) 0.28977(7) 0.0381(4) Uani 1 1 d . . H13 H 0.9175 0.5681 0.2910 0.046 Uiso 1 1 calc R U C14 C 0.75287(18) 0.61201(11) 0.28254(7) 0.0400(4) Uani 1 1 d . . H14 H 0.7716 0.6708 0.2782 0.048 Uiso 1 1 calc R U C15 C 0.63984(17) 0.58927(10) 0.28143(7) 0.0348(4) Uani 1 1 d . . H15 H 0.5813 0.6320 0.2773 0.042 Uiso 1 1 calc R U C16 C 0.61222(14) 0.50284(10) 0.28643(6) 0.0261(3) Uani 1 1 d . . H16 H 0.5342 0.4867 0.2854 0.031 Uiso 1 1 calc R U C17 C 1.01201(15) 0.42182(15) 0.30763(10) 0.0514(5) Uani 1 1 d . . H17A H 1.0237 0.4492 0.2717 0.077 Uiso 1 1 calc R U H17B H 1.0589 0.3694 0.3145 0.077 Uiso 1 1 calc R U H17C H 1.0352 0.4616 0.3401 0.077 Uiso 1 1 calc R U C21 C 0.70465(12) 0.26741(10) 0.24584(6) 0.0235(3) Uani 1 1 d . . C22 C 0.70478(14) 0.17789(11) 0.24913(7) 0.0308(4) Uani 1 1 d . . C23 C 0.74064(15) 0.12874(13) 0.20620(9) 0.0462(5) Uani 1 1 d . . H23 H 0.7418 0.0677 0.2085 0.055 Uiso 1 1 calc R U C24 C 0.77457(16) 0.17059(16) 0.16024(8) 0.0521(6) Uani 1 1 d . . H24 H 0.8003 0.1376 0.1313 0.063 Uiso 1 1 calc R U C25 C 0.77180(15) 0.25852(16) 0.15572(7) 0.0452(5) Uani 1 1 d . . H25 H 0.7940 0.2859 0.1235 0.054 Uiso 1 1 calc R U C26 C 0.73657(14) 0.30721(12) 0.19833(7) 0.0327(4) Uani 1 1 d . . H26 H 0.7341 0.3681 0.1952 0.039 Uiso 1 1 calc R U C27 C 0.68716(19) 0.05659(12) 0.30974(11) 0.0564(6) Uani 1 1 d . . H27A H 0.6436 0.0213 0.2785 0.085 Uiso 1 1 calc R U H27B H 0.6613 0.0437 0.3459 0.085 Uiso 1 1 calc R U H27C H 0.7698 0.0437 0.3143 0.085 Uiso 1 1 calc R U C31 C 0.39588(12) 0.37695(9) 0.42218(6) 0.0193(3) Uani 1 1 d . . C32 C 0.42431(13) 0.46450(9) 0.42641(6) 0.0220(3) Uani 1 1 d . . C33 C 0.35207(15) 0.52279(10) 0.44685(6) 0.0297(3) Uani 1 1 d . . H33 H 0.3724 0.5819 0.4506 0.036 Uiso 1 1 calc R U C34 C 0.25061(15) 0.49425(11) 0.46165(7) 0.0341(4) Uani 1 1 d . . H34 H 0.2015 0.5341 0.4756 0.041 Uiso 1 1 calc R U C35 C 0.21991(14) 0.40826(11) 0.45632(7) 0.0318(4) Uani 1 1 d . . H35 H 0.1496 0.3892 0.4660 0.038 Uiso 1 1 calc R U C36 C 0.29290(13) 0.35006(10) 0.43669(6) 0.0248(3) Uani 1 1 d . . H36 H 0.2721 0.2910 0.4331 0.030 Uiso 1 1 calc R U C37 C 0.55603(16) 0.57557(10) 0.41230(7) 0.0333(4) Uani 1 1 d . . H37A H 0.6319 0.5822 0.4017 0.050 Uiso 1 1 calc R U H37B H 0.5597 0.5965 0.4518 0.050 Uiso 1 1 calc R U H37C H 0.4985 0.6089 0.3855 0.050 Uiso 1 1 calc R U C41 C 0.44296(12) 0.19483(9) 0.40747(6) 0.0190(3) Uani 1 1 d . . C42 C 0.43491(12) 0.16631(9) 0.46322(6) 0.0220(3) Uani 1 1 d . . C43 C 0.40061(13) 0.08258(10) 0.47149(7) 0.0282(3) Uani 1 1 d . . H43 H 0.3919 0.0640 0.5088 0.034 Uiso 1 1 calc R U C44 C 0.37910(14) 0.02603(10) 0.42503(7) 0.0318(4) Uani 1 1 d . . H44 H 0.3546 -0.0310 0.4308 0.038 Uiso 1 1 calc R U C45 C 0.39265(14) 0.05119(10) 0.37052(7) 0.0302(3) Uani 1 1 d . . H45 H 0.3815 0.0113 0.3394 0.036 Uiso 1 1 calc R U C46 C 0.42287(12) 0.13585(9) 0.36204(6) 0.0226(3) Uani 1 1 d . . H46 H 0.4300 0.1540 0.3244 0.027 Uiso 1 1 calc R U C47 C 0.46422(17) 0.19527(11) 0.56503(7) 0.0346(4) Uani 1 1 d . . H47A H 0.3868 0.1755 0.5681 0.052 Uiso 1 1 calc R U H47B H 0.4873 0.2427 0.5922 0.052 Uiso 1 1 calc R U H47C H 0.5192 0.1477 0.5743 0.052 Uiso 1 1 calc R U Cl3 Cl 1.18412(4) 0.22103(3) 0.08137(2) 0.05075(12) Uani 1 1 d . . Cl4 Cl 1.04713(4) 0.29736(4) 0.15696(2) 0.05328(13) Uani 1 1 d . . Cl5 Cl 1.15919(5) 0.40511(3) 0.08481(2) 0.05592(13) Uani 1 1 d . . C6 C 1.16945(15) 0.31001(12) 0.12590(8) 0.0389(4) Uani 1 1 d . . H6 H 1.2394 0.3135 0.1575 0.047 Uiso 1 1 calc R U Cl6 Cl 1.07722(6) 0.01074(4) 0.35189(3) 0.06706(16) Uani 1 1 d . . Cl7 Cl 0.99890(5) 0.17615(4) 0.30457(3) 0.06335(16) Uani 1 1 d . . Cl8 Cl 1.09754(5) 0.15942(5) 0.42619(3) 0.07021(18) Uani 1 1 d . . C7 C 1.10159(16) 0.12227(13) 0.35629(9) 0.0456(5) Uani 1 1 d . . H7 H 1.1801 0.1341 0.3480 0.055 Uiso 1 1 calc R U loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ni1 0.01480(10) 0.01908(10) 0.01268(9) -0.00011(6) 0.00099(7) 0.00051(6) Cl1 0.02432(18) 0.0465(2) 0.01378(16) 0.00171(14) 0.00039(13) 0.00348(16) Cl2 0.01609(17) 0.0467(2) 0.02471(18) -0.00467(15) 0.00103(14) 0.00120(15) P1 0.01658(17) 0.01851(17) 0.01352(16) 0.00115(12) 0.00275(13) -0.00008(13) P2 0.01603(17) 0.01699(17) 0.01393(16) 0.00008(12) 0.00278(13) -0.00056(13) O1 0.0213(5) 0.0386(6) 0.0402(6) 0.0080(5) 0.0062(5) -0.0059(5) O2 0.0470(7) 0.0206(6) 0.0517(7) -0.0010(5) 0.0102(6) -0.0005(5) O3 0.0342(6) 0.0194(5) 0.0274(5) -0.0024(4) 0.0105(4) -0.0046(4) O4 0.0388(6) 0.0274(5) 0.0166(5) 0.0032(4) 0.0095(4) 0.0002(5) N1 0.0172(6) 0.0222(6) 0.0170(5) 0.0049(5) 0.0029(4) 0.0030(5) C1 0.0154(6) 0.0264(7) 0.0184(7) 0.0041(6) 0.0014(5) 0.0000(5) C2 0.0189(7) 0.0239(7) 0.0142(6) 0.0001(5) 0.0012(5) -0.0005(5) C3 0.0227(7) 0.0367(9) 0.0262(8) 0.0137(7) 0.0042(6) 0.0089(7) C4 0.0383(10) 0.0437(10) 0.0484(10) 0.0286(9) 0.0119(8) 0.0115(8) C5 0.0284(9) 0.0665(13) 0.0288(9) 0.0111(8) -0.0049(7) 0.0017(8) C11 0.0284(7) 0.0218(7) 0.0145(6) 0.0026(5) 0.0039(5) -0.0028(6) C12 0.0305(8) 0.0306(8) 0.0201(7) 0.0051(6) 0.0033(6) -0.0072(6) C13 0.0457(10) 0.0374(10) 0.0289(8) 0.0067(7) 0.0016(7) -0.0191(8) C14 0.0698(13) 0.0240(8) 0.0237(8) 0.0044(6) 0.0029(8) -0.0123(8) C15 0.0596(11) 0.0238(8) 0.0201(7) 0.0039(6) 0.0060(7) 0.0042(8) C16 0.0360(8) 0.0255(8) 0.0164(7) 0.0026(6) 0.0044(6) 0.0026(6) C17 0.0232(9) 0.0670(14) 0.0624(13) 0.0159(11) 0.0047(8) -0.0111(9) C21 0.0171(7) 0.0327(8) 0.0204(7) -0.0068(6) 0.0025(5) 0.0017(6) C22 0.0234(8) 0.0351(9) 0.0324(8) -0.0106(7) 0.0019(7) 0.0012(6) C23 0.0321(9) 0.0471(11) 0.0558(12) -0.0294(9) -0.0006(8) 0.0055(8) C24 0.0289(9) 0.0887(17) 0.0377(10) -0.0354(11) 0.0041(8) 0.0054(10) C25 0.0286(9) 0.0840(16) 0.0239(8) -0.0142(9) 0.0070(7) 0.0000(9) C26 0.0242(8) 0.0525(11) 0.0212(8) -0.0027(7) 0.0039(6) -0.0003(7) C27 0.0496(12) 0.0242(9) 0.0921(17) 0.0081(10) 0.0060(11) -0.0005(8) C31 0.0207(7) 0.0229(7) 0.0137(6) -0.0009(5) 0.0023(5) 0.0033(5) C32 0.0276(8) 0.0238(7) 0.0139(6) 0.0003(5) 0.0023(5) 0.0024(6) C33 0.0410(9) 0.0240(8) 0.0232(7) -0.0017(6) 0.0042(6) 0.0090(7) C34 0.0364(9) 0.0375(9) 0.0293(8) -0.0016(7) 0.0086(7) 0.0166(7) C35 0.0239(8) 0.0436(10) 0.0295(8) 0.0013(7) 0.0091(6) 0.0075(7) C36 0.0223(7) 0.0286(8) 0.0230(7) -0.0001(6) 0.0034(6) 0.0014(6) C37 0.0512(10) 0.0214(8) 0.0273(8) -0.0022(6) 0.0078(7) -0.0107(7) C41 0.0176(7) 0.0188(7) 0.0208(7) 0.0022(5) 0.0040(5) 0.0012(5) C42 0.0193(7) 0.0244(7) 0.0230(7) 0.0033(6) 0.0056(6) 0.0030(6) C43 0.0275(8) 0.0280(8) 0.0307(8) 0.0111(6) 0.0095(6) 0.0018(6) C44 0.0322(8) 0.0197(7) 0.0430(9) 0.0067(7) 0.0062(7) -0.0029(6) C45 0.0323(8) 0.0217(8) 0.0355(8) -0.0032(6) 0.0041(7) -0.0039(6) C46 0.0217(7) 0.0225(7) 0.0231(7) 0.0008(6) 0.0033(6) -0.0021(6) C47 0.0521(11) 0.0347(9) 0.0198(8) 0.0061(6) 0.0139(7) 0.0074(8) Cl3 0.0449(3) 0.0476(3) 0.0574(3) -0.0077(2) 0.0040(2) 0.0083(2) Cl4 0.0320(2) 0.0793(4) 0.0487(3) 0.0053(2) 0.0084(2) 0.0066(2) Cl5 0.0609(3) 0.0463(3) 0.0623(3) 0.0013(2) 0.0162(3) 0.0055(2) C6 0.0260(9) 0.0493(11) 0.0385(10) -0.0038(8) -0.0006(7) 0.0033(7) Cl6 0.0681(4) 0.0553(3) 0.0766(4) -0.0059(3) 0.0111(3) -0.0178(3) Cl7 0.0419(3) 0.0761(4) 0.0724(4) -0.0059(3) 0.0121(3) 0.0175(3) Cl8 0.0419(3) 0.1040(5) 0.0658(4) -0.0345(3) 0.0131(3) -0.0160(3) C7 0.0270(9) 0.0513(11) 0.0605(12) -0.0123(9) 0.0129(8) -0.0050(8) 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' 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 P2 Ni1 P1 94.657(14) P2 Ni1 Cl2 86.931(14) P1 Ni1 Cl2 177.565(16) P2 Ni1 Cl1 178.438(15) P1 Ni1 Cl1 86.905(14) Cl2 Ni1 Cl1 91.507(15) C11 P1 C21 106.12(7) C11 P1 C1 102.48(7) C21 P1 C1 104.51(7) C11 P1 Ni1 109.30(5) C21 P1 Ni1 113.05(5) C1 P1 Ni1 120.10(5) C41 P2 C31 106.81(6) C41 P2 C2 101.41(6) C31 P2 C2 107.16(6) C41 P2 Ni1 110.87(5) C31 P2 Ni1 111.82(4) C2 P2 Ni1 117.80(5) C12 O1 C17 118.75(14) C22 O2 C27 118.86(15) C32 O3 C37 117.61(12) C42 O4 C47 117.81(12) C1 N1 C2 110.82(11) C1 N1 C3 111.56(11) C2 N1 C3 115.27(11) N1 C1 P1 113.77(9) N1 C1 H1A 108.8 P1 C1 H1A 108.8 N1 C1 H1B 108.8 P1 C1 H1B 108.8 H1A C1 H1B 107.7 N1 C2 P2 106.64(9) N1 C2 H2A 110.4 P2 C2 H2A 110.4 N1 C2 H2B 110.4 P2 C2 H2B 110.4 H2A C2 H2B 108.6 N1 C3 C4 110.72(13) N1 C3 C5 113.63(14) C4 C3 C5 111.21(14) N1 C3 H3 107.0 C4 C3 H3 107.0 C5 C3 H3 107.0 C3 C4 H4A 109.5 C3 C4 H4B 109.5 H4A C4 H4B 109.5 C3 C4 H4C 109.5 H4A C4 H4C 109.5 H4B C4 H4C 109.5 C3 C5 H5A 109.5 C3 C5 H5B 109.5 H5A C5 H5B 109.5 C3 C5 H5C 109.5 H5A C5 H5C 109.5 H5B C5 H5C 109.5 C16 C11 C12 119.01(14) C16 C11 P1 118.90(11) C12 C11 P1 121.97(12) O1 C12 C13 124.06(15) O1 C12 C11 116.21(13) C13 C12 C11 119.73(16) C14 C13 C12 119.89(17) C14 C13 H13 120.1 C12 C13 H13 120.1 C15 C14 C13 121.27(15) C15 C14 H14 119.4 C13 C14 H14 119.4 C14 C15 C16 119.23(16) C14 C15 H15 120.4 C16 C15 H15 120.4 C11 C16 C15 120.85(16) C11 C16 H16 119.6 C15 C16 H16 119.6 O1 C17 H17A 109.5 O1 C17 H17B 109.5 H17A C17 H17B 109.5 O1 C17 H17C 109.5 H17A C17 H17C 109.5 H17B C17 H17C 109.5 C26 C21 C22 119.38(14) C26 C21 P1 122.03(13) C22 C21 P1 118.56(12) O2 C22 C21 114.80(13) O2 C22 C23 125.01(17) C21 C22 C23 120.20(17) C24 C23 C22 118.84(19) C24 C23 H23 120.6 C22 C23 H23 120.6 C25 C24 C23 121.48(17) C25 C24 H24 119.3 C23 C24 H24 119.3 C24 C25 C26 119.67(19) C24 C25 H25 120.2 C26 C25 H25 120.2 C25 C26 C21 120.39(18) C25 C26 H26 119.8 C21 C26 H26 119.8 O2 C27 H27A 109.5 O2 C27 H27B 109.5 H27A C27 H27B 109.5 O2 C27 H27C 109.5 H27A C27 H27C 109.5 H27B C27 H27C 109.5 C36 C31 C32 118.93(13) C36 C31 P2 121.30(11) C32 C31 P2 119.54(11) O3 C32 C33 124.16(14) O3 C32 C31 115.66(12) C33 C32 C31 120.18(14) C34 C33 C32 119.76(15) C34 C33 H33 120.1 C32 C33 H33 120.1 C33 C34 C35 120.71(14) C33 C34 H34 119.6 C35 C34 H34 119.6 C34 C35 C36 119.41(15) C34 C35 H35 120.3 C36 C35 H35 120.3 C31 C36 C35 120.97(15) C31 C36 H36 119.5 C35 C36 H36 119.5 O3 C37 H37A 109.5 O3 C37 H37B 109.5 H37A C37 H37B 109.5 O3 C37 H37C 109.5 H37A C37 H37C 109.5 H37B C37 H37C 109.5 C46 C41 C42 118.49(13) C46 C41 P2 117.60(11) C42 C41 P2 123.78(11) O4 C42 C43 123.32(13) O4 C42 C41 116.62(12) C43 C42 C41 120.06(14) C42 C43 C44 119.80(14) C42 C43 H43 120.1 C44 C43 H43 120.1 C45 C44 C43 121.14(14) C45 C44 H44 119.4 C43 C44 H44 119.4 C44 C45 C46 118.80(15) C44 C45 H45 120.6 C46 C45 H45 120.6 C45 C46 C41 121.55(14) C45 C46 H46 119.2 C41 C46 H46 119.2 O4 C47 H47A 109.5 O4 C47 H47B 109.5 H47A C47 H47B 109.5 O4 C47 H47C 109.5 H47A C47 H47C 109.5 H47B C47 H47C 109.5 Cl4 C6 Cl5 110.51(10) Cl4 C6 Cl3 110.15(10) Cl5 C6 Cl3 109.64(10) Cl4 C6 H6 108.8 Cl5 C6 H6 108.8 Cl3 C6 H6 108.8 Cl8 C7 Cl7 110.68(11) Cl8 C7 Cl6 110.26(12) Cl7 C7 Cl6 110.31(11) Cl8 C7 H7 108.5 Cl7 C7 H7 108.5 Cl6 C7 H7 108.5 loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance Ni1 P2 2.1711(4) Ni1 P1 2.1765(4) Ni1 Cl2 2.1995(4) Ni1 Cl1 2.2090(4) P1 C11 1.8182(14) P1 C21 1.8199(14) P1 C1 1.8596(14) P2 C41 1.8146(14) P2 C31 1.8211(14) P2 C2 1.8414(14) O1 C12 1.359(2) O1 C17 1.432(2) O2 C22 1.360(2) O2 C27 1.426(2) O3 C32 1.3608(18) O3 C37 1.4322(18) O4 C42 1.3656(18) O4 C47 1.4347(18) N1 C1 1.4485(18) N1 C2 1.4600(18) N1 C3 1.4833(18) C1 H1A 0.9900 C1 H1B 0.9900 C2 H2A 0.9900 C2 H2B 0.9900 C3 C4 1.521(2) C3 C5 1.523(3) C3 H3 1.0000 C4 H4A 0.9800 C4 H4B 0.9800 C4 H4C 0.9800 C5 H5A 0.9800 C5 H5B 0.9800 C5 H5C 0.9800 C11 C16 1.393(2) C11 C12 1.406(2) C12 C13 1.393(2) C13 C14 1.382(3) C13 H13 0.9500 C14 C15 1.375(3) C14 H14 0.9500 C15 C16 1.393(2) C15 H15 0.9500 C16 H16 0.9500 C17 H17A 0.9800 C17 H17B 0.9800 C17 H17C 0.9800 C21 C26 1.393(2) C21 C22 1.394(2) C22 C23 1.397(2) C23 C24 1.387(3) C23 H23 0.9500 C24 C25 1.371(3) C24 H24 0.9500 C25 C26 1.384(2) C25 H25 0.9500 C26 H26 0.9500 C27 H27A 0.9800 C27 H27B 0.9800 C27 H27C 0.9800 C31 C36 1.389(2) C31 C32 1.401(2) C32 C33 1.393(2) C33 C34 1.383(2) C33 H33 0.9500 C34 C35 1.384(3) C34 H34 0.9500 C35 C36 1.389(2) C35 H35 0.9500 C36 H36 0.9500 C37 H37A 0.9800 C37 H37B 0.9800 C37 H37C 0.9800 C41 C46 1.394(2) C41 C42 1.407(2) C42 C43 1.388(2) C43 C44 1.388(2) C43 H43 0.9500 C44 C45 1.381(2) C44 H44 0.9500 C45 C46 1.388(2) C45 H45 0.9500 C46 H46 0.9500 C47 H47A 0.9800 C47 H47B 0.9800 C47 H47C 0.9800 Cl3 C6 1.7650(19) Cl4 C6 1.7517(19) Cl5 C6 1.758(2) C6 H6 1.0000 Cl6 C7 1.757(2) Cl7 C7 1.755(2) Cl8 C7 1.754(2) C7 H7 1.0000 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 C2 N1 C1 P1 -70.60(13) C3 N1 C1 P1 159.51(10) C11 P1 C1 N1 134.69(10) C21 P1 C1 N1 -114.77(11) Ni1 P1 C1 N1 13.38(12) C1 N1 C2 P2 90.63(11) C3 N1 C2 P2 -141.47(10) C41 P2 C2 N1 70.52(10) C31 P2 C2 N1 -177.69(9) Ni1 P2 C2 N1 -50.63(10) C1 N1 C3 C4 -163.62(14) C2 N1 C3 C4 68.85(18) C1 N1 C3 C5 70.38(16) C2 N1 C3 C5 -57.14(17) C21 P1 C11 C16 124.01(11) C1 P1 C11 C16 -126.65(11) Ni1 P1 C11 C16 1.80(12) C21 P1 C11 C12 -59.94(13) C1 P1 C11 C12 49.40(13) Ni1 P1 C11 C12 177.85(10) C17 O1 C12 C13 2.7(2) C17 O1 C12 C11 -177.53(15) C16 C11 C12 O1 178.91(12) P1 C11 C12 O1 2.86(18) C16 C11 C12 C13 -1.3(2) P1 C11 C12 C13 -177.33(12) O1 C12 C13 C14 -179.78(15) C11 C12 C13 C14 0.4(2) C12 C13 C14 C15 1.0(2) C13 C14 C15 C16 -1.4(2) C12 C11 C16 C15 0.8(2) P1 C11 C16 C15 176.97(11) C14 C15 C16 C11 0.5(2) C11 P1 C21 C26 -14.07(14) C1 P1 C21 C26 -121.97(13) Ni1 P1 C21 C26 105.72(12) C11 P1 C21 C22 168.13(12) C1 P1 C21 C22 60.24(13) Ni1 P1 C21 C22 -72.08(12) C27 O2 C22 C21 -167.12(15) C27 O2 C22 C23 13.1(2) C26 C21 C22 O2 -177.48(14) P1 C21 C22 O2 0.38(19) C26 C21 C22 C23 2.3(2) P1 C21 C22 C23 -179.83(12) O2 C22 C23 C24 179.03(16) C21 C22 C23 C24 -0.7(2) C22 C23 C24 C25 -1.1(3) C23 C24 C25 C26 1.2(3) C24 C25 C26 C21 0.4(3) C22 C21 C26 C25 -2.1(2) P1 C21 C26 C25 -179.92(12) C41 P2 C31 C36 -17.72(13) C2 P2 C31 C36 -125.76(12) Ni1 P2 C31 C36 103.74(11) C41 P2 C31 C32 167.95(11) C2 P2 C31 C32 59.91(12) Ni1 P2 C31 C32 -70.59(11) C37 O3 C32 C33 0.2(2) C37 O3 C32 C31 179.62(12) C36 C31 C32 O3 -177.19(12) P2 C31 C32 O3 -2.73(16) C36 C31 C32 C33 2.3(2) P2 C31 C32 C33 176.74(11) O3 C32 C33 C34 177.85(14) C31 C32 C33 C34 -1.6(2) C32 C33 C34 C35 -0.1(2) C33 C34 C35 C36 0.9(2) C32 C31 C36 C35 -1.4(2) P2 C31 C36 C35 -175.75(11) C34 C35 C36 C31 -0.2(2) C31 P2 C41 C46 131.37(11) C2 P2 C41 C46 -116.57(11) Ni1 P2 C41 C46 9.31(12) C31 P2 C41 C42 -52.79(13) C2 P2 C41 C42 59.27(13) Ni1 P2 C41 C42 -174.84(11) C47 O4 C42 C43 4.0(2) C47 O4 C42 C41 -175.41(13) C46 C41 C42 O4 175.48(12) P2 C41 C42 O4 -0.33(19) C46 C41 C42 C43 -3.9(2) P2 C41 C42 C43 -179.75(11) O4 C42 C43 C44 -176.62(14) C41 C42 C43 C44 2.8(2) C42 C43 C44 C45 0.9(2) C43 C44 C45 C46 -3.2(2) C44 C45 C46 C41 1.9(2) C42 C41 C46 C45 1.6(2) P2 C41 C46 C45 177.68(12)