#------------------------------------------------------------------------------ #$Date: 2014-12-22 15:52:12 +0200 (Mon, 22 Dec 2014) $ #$Revision: 129001 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/11/60/7116077.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_7116077 loop_ _publ_author_name 'Nicholas D. Staudaher' 'Ryan M. Stolley' 'Janis Louie' _publ_section_title ; Synthesis, mechanism of formation, and catalytic activity of Xantphos nickel pi-complexes ; _journal_name_full Chem.Commun. _journal_page_first 15577 _journal_paper_doi 10.1039/C4cc07590K _journal_volume 50 _journal_year 2014 _chemical_formula_moiety 'C45 H40 Ni O5 P2, 0.5(C6 H6)' _chemical_formula_sum 'C48 H43 Ni O5 P2' _chemical_formula_weight 820.47 _chemical_name_systematic 'Xantphos Ni Dimethylfumarate' _chemical_properties_physical 'Air-sensitive, Moisture-sensitive, Oxygen-sensitive' _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_Hall '-P 1' _space_group_name_H-M_alt 'P -1' _symmetry_space_group_name_Hall '-P 1' _symmetry_space_group_name_H-M 'P -1' _atom_sites_solution_hydrogens geom _audit_creation_method SHELXL-2014 _cell_angle_alpha 73.8372(9) _cell_angle_beta 84.9154(12) _cell_angle_gamma 76.8383(11) _cell_formula_units_Z 2 _cell_length_a 11.8270(2) _cell_length_b 12.1552(2) _cell_length_c 14.8937(3) _cell_measurement_reflns_used 9038 _cell_measurement_temperature 150(1) _cell_measurement_theta_max 27.485 _cell_measurement_theta_min 1.018 _cell_volume 2001.73(6) _computing_cell_refinement DENZO-SMN _computing_data_collection 'Nonius COLLECT' _computing_data_reduction DENZO-SMN _computing_molecular_graphics 'WinGX, Ortep3' _computing_structure_refinement 'SHELXL-2014 (Sheldrick, 2014)' _computing_structure_solution SIR97 _diffrn_ambient_temperature 150(1) _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.996 _diffrn_measurement_device_type 'Nonius KappaCCD Diffractometer' _diffrn_measurement_method 'Phi and Omega scan' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0291 _diffrn_reflns_av_unetI/netI 0.0484 _diffrn_reflns_laue_measured_fraction_full 0.999 _diffrn_reflns_laue_measured_fraction_max 0.996 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_number 17370 _diffrn_reflns_point_group_measured_fraction_full 0.999 _diffrn_reflns_point_group_measured_fraction_max 0.996 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 27.518 _diffrn_reflns_theta_min 2.231 _diffrn_source 'fine-focus sealed tube' _exptl_absorpt_coefficient_mu 0.613 _exptl_absorpt_correction_T_max 0.941 _exptl_absorpt_correction_T_min 0.847 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'DENZO-SMN (Otwinowski & Minor, 1997)' _exptl_crystal_colour orange _exptl_crystal_density_diffrn 1.361 _exptl_crystal_description plate _exptl_crystal_F_000 858 _exptl_crystal_size_max 0.280 _exptl_crystal_size_mid 0.250 _exptl_crystal_size_min 0.100 _refine_diff_density_max 0.539 _refine_diff_density_min -0.650 _refine_diff_density_rms 0.068 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.036 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 505 _refine_ls_number_reflns 9192 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.036 _refine_ls_R_factor_all 0.0665 _refine_ls_R_factor_gt 0.0414 _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^)+(0.0522P)^2^+1.0199P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0971 _refine_ls_wR_factor_ref 0.1088 _reflns_Friedel_coverage 0.000 _reflns_number_gt 6950 _reflns_number_total 9192 _reflns_threshold_expression 'I > 2\s(I)' _[local]_cod_data_source_file c4cc07590k3.cif _[local]_cod_data_source_block jl069 _cod_database_code 7116077 _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 0.847 _shelx_estimated_absorpt_t_max 0.941 _shelxl_version_number 2014-3 _shelx_res_file ; TITL jl069 nds @150K Orange Plate triclinic P-1 6/9/2014 ama SHELXL CELL 0.71073 11.8270 12.1552 14.8937 73.8372 84.9154 76.8383 ZERR 2 0.0002 0.0002 0.0003 0.0009 0.0012 0.0011 LATT 1 SFAC C H O P NI UNIT 96 86 10 4 2 TEMP -123 SIZE 0.28 0.25 0.10 OMIT 0 1 0 OMIT 0 1 1 OMIT 0 0 1 OMIT 1 0 0 FMAP 2 ACTA BOND $H CONF L.S. 28 PLAN -5 WGHT 0.052200 1.019900 FVAR 0.26967 NI1 5 0.813341 0.142058 0.253954 11.00000 0.02102 0.01706 = 0.01973 -0.00460 -0.00095 -0.00491 P1 4 0.697595 0.266034 0.144704 11.00000 0.02061 0.01674 = 0.02136 -0.00565 -0.00096 -0.00405 P2 4 0.817235 -0.042120 0.259937 11.00000 0.02163 0.01753 = 0.01922 -0.00426 0.00009 -0.00557 O1 3 0.712124 0.054544 0.081390 11.00000 0.02332 0.01740 = 0.01911 -0.00413 0.00053 -0.00319 O2 3 0.865282 -0.020708 0.502612 11.00000 0.02821 0.02922 = 0.02398 -0.00067 -0.00008 -0.00776 O3 3 0.711906 0.131019 0.468841 11.00000 0.02761 0.03520 = 0.02771 -0.00988 0.00297 -0.00628 O4 3 0.906254 0.429753 0.281409 11.00000 0.05508 0.02268 = 0.04562 -0.00336 -0.01317 -0.01685 O5 3 1.032754 0.277227 0.246882 11.00000 0.03210 0.03820 = 0.04705 0.00065 -0.00140 -0.01398 C1 1 0.704940 0.151549 0.004522 11.00000 0.01998 0.02039 = 0.02149 -0.00225 -0.00149 -0.00504 C2 1 0.687515 0.259895 0.023365 11.00000 0.02038 0.02135 = 0.02358 -0.00523 -0.00197 -0.00448 C3 1 0.675256 0.358292 -0.054615 11.00000 0.02755 0.01832 = 0.02575 -0.00354 -0.00395 -0.00214 AFIX 43 H3 2 0.659101 0.434708 -0.045499 11.00000 -1.20000 AFIX 0 C4 1 0.686494 0.344941 -0.144596 11.00000 0.03083 0.02390 = 0.02474 0.00194 -0.00537 -0.00417 AFIX 43 H4 2 0.677192 0.412364 -0.196490 11.00000 -1.20000 AFIX 0 C5 1 0.711230 0.234013 -0.159862 11.00000 0.02970 0.02943 = 0.01866 -0.00447 -0.00045 -0.00755 AFIX 43 H5 2 0.721855 0.226219 -0.221945 11.00000 -1.20000 AFIX 0 C6 1 0.720515 0.134377 -0.084785 11.00000 0.02378 0.02249 = 0.02229 -0.00658 -0.00117 -0.00573 C7 1 0.750641 0.007351 -0.091036 11.00000 0.03255 0.02429 = 0.02284 -0.00838 -0.00131 -0.00684 C8 1 0.833871 -0.059726 -0.011755 11.00000 0.02583 0.02008 = 0.02392 -0.00654 0.00203 -0.01008 C9 1 0.806453 -0.035245 0.073892 11.00000 0.01954 0.01623 = 0.02526 -0.00606 0.00263 -0.00636 C10 1 0.867829 -0.092657 0.155062 11.00000 0.02189 0.01790 = 0.02327 -0.00494 0.00151 -0.00826 C11 1 0.966248 -0.178584 0.147755 11.00000 0.02399 0.02136 = 0.02848 -0.00630 -0.00115 -0.00687 AFIX 43 H11 2 1.010409 -0.221128 0.201544 11.00000 -1.20000 AFIX 0 C12 1 0.999968 -0.202211 0.062075 11.00000 0.02241 0.02400 = 0.03414 -0.01147 0.00365 -0.00434 AFIX 43 H12 2 1.068768 -0.258904 0.057513 11.00000 -1.20000 AFIX 0 C13 1 0.934720 -0.144288 -0.017040 11.00000 0.02664 0.02534 = 0.02681 -0.01063 0.00622 -0.00826 AFIX 43 H13 2 0.958697 -0.162191 -0.074868 11.00000 -1.20000 AFIX 0 C14 1 0.638722 -0.041791 -0.074013 11.00000 0.03534 0.02797 = 0.03624 -0.00902 -0.00713 -0.01038 AFIX 33 H14A 2 0.603389 -0.034993 -0.013210 11.00000 -1.20000 H14B 2 0.583866 0.002876 -0.123495 11.00000 -1.20000 H14C 2 0.657957 -0.124411 -0.074542 11.00000 -1.20000 AFIX 0 C15 1 0.804752 -0.003762 -0.185898 11.00000 0.05075 0.03406 = 0.02352 -0.01085 -0.00169 -0.00402 AFIX 33 H15A 2 0.749237 0.040155 -0.235072 11.00000 -1.20000 H15B 2 0.875384 0.027963 -0.197553 11.00000 -1.20000 H15C 2 0.824371 -0.086539 -0.185965 11.00000 -1.20000 AFIX 0 C16 1 0.547752 0.276401 0.190485 11.00000 0.02285 0.01763 = 0.02842 -0.00580 0.00015 -0.00708 C17 1 0.528043 0.261296 0.286510 11.00000 0.02684 0.03109 = 0.02778 -0.00459 0.00024 -0.00605 AFIX 43 H17 2 0.591898 0.243175 0.326386 11.00000 -1.20000 AFIX 0 C18 1 0.415988 0.272573 0.323953 11.00000 0.03475 0.04005 = 0.03083 -0.00443 0.00821 -0.00813 AFIX 43 H18 2 0.403461 0.262501 0.389371 11.00000 -1.20000 AFIX 0 C19 1 0.321717 0.298479 0.266739 11.00000 0.02324 0.03440 = 0.04639 -0.00601 0.00672 -0.00769 AFIX 43 H19 2 0.244899 0.306280 0.292668 11.00000 -1.20000 AFIX 0 C20 1 0.340788 0.312798 0.171688 11.00000 0.02346 0.03306 = 0.04526 -0.00911 -0.00485 -0.00736 AFIX 43 H20 2 0.276654 0.330374 0.132183 11.00000 -1.20000 AFIX 0 C21 1 0.452720 0.301735 0.133466 11.00000 0.02758 0.02638 = 0.03046 -0.00711 -0.00376 -0.00635 AFIX 43 H21 2 0.464751 0.311470 0.068046 11.00000 -1.20000 AFIX 0 C22 1 0.715667 0.418257 0.119700 11.00000 0.02409 0.01833 = 0.02027 -0.00193 -0.00522 -0.00521 C23 1 0.822589 0.442340 0.080793 11.00000 0.02562 0.02300 = 0.03130 -0.00730 -0.00014 -0.00463 AFIX 43 H23 2 0.883265 0.380464 0.070561 11.00000 -1.20000 AFIX 0 C24 1 0.840263 0.555550 0.057232 11.00000 0.03168 0.03067 = 0.03231 -0.00540 0.00068 -0.01377 AFIX 43 H24 2 0.912301 0.571557 0.029528 11.00000 -1.20000 AFIX 0 C25 1 0.752905 0.645877 0.073995 11.00000 0.04184 0.02183 = 0.03143 -0.00444 -0.00390 -0.01336 AFIX 43 H25 2 0.765786 0.723331 0.059492 11.00000 -1.20000 AFIX 0 C26 1 0.647274 0.622791 0.111801 11.00000 0.03553 0.02048 = 0.03641 -0.01157 -0.00222 -0.00177 AFIX 43 H26 2 0.587014 0.684851 0.122298 11.00000 -1.20000 AFIX 0 C27 1 0.628392 0.509220 0.134664 11.00000 0.02694 0.02242 = 0.02832 -0.00868 -0.00014 -0.00538 AFIX 43 H27 2 0.555373 0.494108 0.160618 11.00000 -1.20000 AFIX 0 C28 1 0.675432 -0.081923 0.287701 11.00000 0.02429 0.02133 = 0.02151 -0.00242 0.00003 -0.00712 C29 1 0.607675 -0.040284 0.357262 11.00000 0.02921 0.02976 = 0.03010 -0.01122 0.00541 -0.00950 AFIX 43 H29 2 0.630231 0.016152 0.381041 11.00000 -1.20000 AFIX 0 C30 1 0.507603 -0.080180 0.392302 11.00000 0.03009 0.04284 = 0.03386 -0.01479 0.00768 -0.01222 AFIX 43 H30 2 0.462664 -0.052079 0.440580 11.00000 -1.20000 AFIX 0 C31 1 0.473301 -0.160433 0.357228 11.00000 0.03118 0.05318 = 0.03696 -0.01155 0.00780 -0.02226 AFIX 43 H31 2 0.404952 -0.188170 0.381539 11.00000 -1.20000 AFIX 0 C32 1 0.538463 -0.200816 0.286425 11.00000 0.04259 0.05383 = 0.03869 -0.02147 0.00647 -0.02856 AFIX 43 H32 2 0.514030 -0.255331 0.261561 11.00000 -1.20000 AFIX 0 C33 1 0.639229 -0.161923 0.251731 11.00000 0.03261 0.03950 = 0.02867 -0.01614 0.00557 -0.01590 AFIX 43 H33 2 0.683701 -0.189980 0.203246 11.00000 -1.20000 AFIX 0 C34 1 0.905672 -0.158782 0.349727 11.00000 0.03108 0.01757 = 0.02101 -0.00517 -0.00087 -0.00239 C35 1 0.864735 -0.256997 0.402441 11.00000 0.04461 0.02683 = 0.03713 0.00104 -0.00798 -0.01285 AFIX 43 H35 2 0.789381 -0.265660 0.392446 11.00000 -1.20000 AFIX 0 C36 1 0.934436 -0.341937 0.469486 11.00000 0.06517 0.03188 = 0.04833 0.01089 -0.01618 -0.01465 AFIX 43 H36 2 0.905548 -0.407621 0.506344 11.00000 -1.20000 AFIX 0 C37 1 1.044822 -0.332140 0.483193 11.00000 0.06121 0.03250 = 0.03880 -0.00215 -0.02327 0.00269 AFIX 43 H37 2 1.092115 -0.391308 0.528726 11.00000 -1.20000 AFIX 0 C38 1 1.086584 -0.236559 0.430874 11.00000 0.03694 0.03693 = 0.03587 -0.01562 -0.01157 0.00010 AFIX 43 H38 2 1.163335 -0.230225 0.439216 11.00000 -1.20000 AFIX 0 C39 1 1.015998 -0.149235 0.365715 11.00000 0.02932 0.02509 = 0.02822 -0.00863 -0.00130 -0.00524 AFIX 43 H39 2 1.044045 -0.081797 0.331561 11.00000 -1.20000 AFIX 0 C40 1 0.796179 -0.081132 0.576245 11.00000 0.03838 0.03938 = 0.02684 0.00294 0.00204 -0.01601 AFIX 33 H40A 2 0.843727 -0.156255 0.609649 11.00000 -1.20000 H40B 2 0.767914 -0.033081 0.619934 11.00000 -1.20000 H40C 2 0.729895 -0.095156 0.549234 11.00000 -1.20000 AFIX 0 C41 1 0.810377 0.084460 0.450769 11.00000 0.02776 0.02722 = 0.02102 -0.00911 -0.00246 -0.00985 C42 1 0.884336 0.132697 0.371487 11.00000 0.02466 0.02522 = 0.02093 -0.00765 -0.00101 -0.00773 AFIX 43 H42 2 0.954423 0.085497 0.354984 11.00000 -1.20000 AFIX 0 C43 1 0.847939 0.252228 0.320098 11.00000 0.02768 0.02252 = 0.02551 -0.00742 -0.00601 -0.00674 AFIX 43 H43 2 0.767934 0.288621 0.313402 11.00000 -1.20000 AFIX 0 C44 1 0.938702 0.316780 0.278008 11.00000 0.03643 0.02564 = 0.03029 -0.00280 -0.01033 -0.01079 C45 1 0.993182 0.499644 0.249784 11.00000 0.07532 0.03622 = 0.07255 0.00471 -0.02763 -0.03581 AFIX 33 H45A 2 0.961508 0.579553 0.254939 11.00000 -1.20000 H45B 2 1.061739 0.464961 0.288556 11.00000 -1.20000 H45C 2 1.015231 0.501798 0.184418 11.00000 -1.20000 AFIX 0 C46 1 0.524309 0.502816 0.579063 11.00000 0.48695 0.08906 = 0.21683 -0.00626 -0.23280 -0.07300 AFIX 43 H46 2 0.528890 0.491664 0.644460 11.00000 -1.20000 AFIX 0 C47 1 0.402922 0.517272 0.545473 11.00000 0.32537 0.08896 = 0.15419 -0.06835 -0.01120 0.04081 AFIX 43 H47 2 0.342080 0.545966 0.584542 11.00000 -1.20000 AFIX 0 C48 1 0.367541 0.496789 0.471308 11.00000 0.30964 0.23945 = 0.56280 -0.26307 0.16679 -0.01222 AFIX 43 H48 2 0.295124 0.485646 0.456597 11.00000 -1.20000 AFIX 0 HKLF 4 REM jl069 nds @150K Orange Plate triclinic P-1 6/9/2014 ama SHELXL REM R1 = 0.0414 for 6950 Fo > 4sig(Fo) and 0.0665 for all 9192 data REM 505 parameters refined using 0 restraints END WGHT 0.0522 1.0199 REM Highest difference peak 0.539, deepest hole -0.650, 1-sigma level 0.068 Q1 1 0.7876 0.2997 0.3548 11.00000 0.05 0.54 Q2 1 0.3374 0.4713 0.5139 11.00000 0.05 0.50 Q3 1 0.5974 0.4917 0.5409 11.00000 0.05 0.49 Q4 1 0.9793 0.1036 0.3840 11.00000 0.05 0.46 Q5 1 0.6828 0.4739 0.5906 11.00000 0.05 0.44 ; _shelx_res_checksum 69165 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 Ni1 Ni 0.81334(2) 0.14206(2) 0.25395(2) 0.01916(8) Uani 1 1 d . . P1 P 0.69760(5) 0.26603(5) 0.14470(4) 0.01941(12) Uani 1 1 d . . P2 P 0.81724(5) -0.04212(5) 0.25994(4) 0.01939(12) Uani 1 1 d . . O1 O 0.71212(12) 0.05454(12) 0.08139(10) 0.0203(3) Uani 1 1 d . . O2 O 0.86528(13) -0.02071(14) 0.50261(11) 0.0282(4) Uani 1 1 d . . O3 O 0.71191(14) 0.13102(15) 0.46884(11) 0.0302(4) Uani 1 1 d . . O4 O 0.90625(17) 0.42975(15) 0.28141(13) 0.0401(4) Uani 1 1 d . . O5 O 1.03275(15) 0.27723(16) 0.24688(13) 0.0405(4) Uani 1 1 d . . C1 C 0.70494(18) 0.15155(18) 0.00452(15) 0.0211(4) Uani 1 1 d . . C2 C 0.68752(18) 0.25990(19) 0.02337(15) 0.0218(4) Uani 1 1 d . . C3 C 0.67526(19) 0.35829(19) -0.05462(16) 0.0246(5) Uani 1 1 d . . H3 H 0.6591 0.4347 -0.0455 0.030 Uiso 1 1 calc R U C4 C 0.6865(2) 0.3449(2) -0.14460(16) 0.0282(5) Uani 1 1 d . . H4 H 0.6772 0.4124 -0.1965 0.034 Uiso 1 1 calc R U C5 C 0.71123(19) 0.2340(2) -0.15986(16) 0.0261(5) Uani 1 1 d . . H5 H 0.7219 0.2262 -0.2219 0.031 Uiso 1 1 calc R U C6 C 0.72051(18) 0.13438(19) -0.08479(15) 0.0226(4) Uani 1 1 d . . C7 C 0.7506(2) 0.0074(2) -0.09104(16) 0.0260(5) Uani 1 1 d . . C8 C 0.83387(19) -0.05973(18) -0.01175(15) 0.0224(5) Uani 1 1 d . . C9 C 0.80645(17) -0.03525(18) 0.07389(15) 0.0200(4) Uani 1 1 d . . C10 C 0.86783(18) -0.09266(18) 0.15506(15) 0.0206(4) Uani 1 1 d . . C11 C 0.96625(19) -0.17858(19) 0.14776(16) 0.0243(5) Uani 1 1 d . . H11 H 1.0104 -0.2211 0.2015 0.029 Uiso 1 1 calc R U C12 C 0.99997(19) -0.2022(2) 0.06208(16) 0.0265(5) Uani 1 1 d . . H12 H 1.0688 -0.2589 0.0575 0.032 Uiso 1 1 calc R U C13 C 0.93472(19) -0.14429(19) -0.01704(16) 0.0255(5) Uani 1 1 d . . H13 H 0.9587 -0.1622 -0.0749 0.031 Uiso 1 1 calc R U C14 C 0.6387(2) -0.0418(2) -0.07401(18) 0.0321(5) Uani 1 1 d . . H14A H 0.6034 -0.0350 -0.0132 0.039 Uiso 1 1 calc R U H14B H 0.5839 0.0029 -0.1235 0.039 Uiso 1 1 calc R U H14C H 0.6580 -0.1244 -0.0745 0.039 Uiso 1 1 calc R U C15 C 0.8048(2) -0.0038(2) -0.18590(17) 0.0362(6) Uani 1 1 d . . H15A H 0.7492 0.0402 -0.2351 0.043 Uiso 1 1 calc R U H15B H 0.8754 0.0280 -0.1976 0.043 Uiso 1 1 calc R U H15C H 0.8244 -0.0865 -0.1860 0.043 Uiso 1 1 calc R U C16 C 0.54775(18) 0.27640(18) 0.19049(16) 0.0226(5) Uani 1 1 d . . C17 C 0.5280(2) 0.2613(2) 0.28651(17) 0.0293(5) Uani 1 1 d . . H17 H 0.5919 0.2432 0.3264 0.035 Uiso 1 1 calc R U C18 C 0.4160(2) 0.2726(2) 0.32395(18) 0.0368(6) Uani 1 1 d . . H18 H 0.4035 0.2625 0.3894 0.044 Uiso 1 1 calc R U C19 C 0.3217(2) 0.2985(2) 0.26674(19) 0.0359(6) Uani 1 1 d . . H19 H 0.2449 0.3063 0.2927 0.043 Uiso 1 1 calc R U C20 C 0.3408(2) 0.3128(2) 0.17169(19) 0.0337(6) Uani 1 1 d . . H20 H 0.2767 0.3304 0.1322 0.040 Uiso 1 1 calc R U C21 C 0.45272(19) 0.3017(2) 0.13347(17) 0.0279(5) Uani 1 1 d . . H21 H 0.4648 0.3115 0.0680 0.034 Uiso 1 1 calc R U C22 C 0.71567(18) 0.41826(18) 0.11970(15) 0.0211(4) Uani 1 1 d . . C23 C 0.82259(19) 0.4423(2) 0.08079(16) 0.0268(5) Uani 1 1 d . . H23 H 0.8833 0.3805 0.0706 0.032 Uiso 1 1 calc R U C24 C 0.8403(2) 0.5556(2) 0.05723(17) 0.0311(5) Uani 1 1 d . . H24 H 0.9123 0.5716 0.0295 0.037 Uiso 1 1 calc R U C25 C 0.7529(2) 0.6459(2) 0.07399(17) 0.0310(5) Uani 1 1 d . . H25 H 0.7658 0.7233 0.0595 0.037 Uiso 1 1 calc R U C26 C 0.6473(2) 0.6228(2) 0.11180(17) 0.0306(5) Uani 1 1 d . . H26 H 0.5870 0.6849 0.1223 0.037 Uiso 1 1 calc R U C27 C 0.6284(2) 0.50922(19) 0.13466(16) 0.0255(5) Uani 1 1 d . . H27 H 0.5554 0.4941 0.1606 0.031 Uiso 1 1 calc R U C28 C 0.67543(19) -0.08192(19) 0.28770(15) 0.0227(4) Uani 1 1 d . . C29 C 0.6077(2) -0.0403(2) 0.35726(17) 0.0289(5) Uani 1 1 d . . H29 H 0.6302 0.0162 0.3810 0.035 Uiso 1 1 calc R U C30 C 0.5076(2) -0.0802(2) 0.39230(18) 0.0344(6) Uani 1 1 d . . H30 H 0.4627 -0.0521 0.4406 0.041 Uiso 1 1 calc R U C31 C 0.4733(2) -0.1604(2) 0.35723(19) 0.0389(6) Uani 1 1 d . . H31 H 0.4050 -0.1882 0.3815 0.047 Uiso 1 1 calc R U C32 C 0.5385(2) -0.2008(3) 0.28642(19) 0.0406(7) Uani 1 1 d . . H32 H 0.5140 -0.2553 0.2616 0.049 Uiso 1 1 calc R U C33 C 0.6392(2) -0.1619(2) 0.25173(17) 0.0312(5) Uani 1 1 d . . H33 H 0.6837 -0.1900 0.2032 0.037 Uiso 1 1 calc R U C34 C 0.90567(19) -0.15878(19) 0.34973(15) 0.0237(5) Uani 1 1 d . . C35 C 0.8647(2) -0.2570(2) 0.40244(18) 0.0368(6) Uani 1 1 d . . H35 H 0.7894 -0.2657 0.3924 0.044 Uiso 1 1 calc R U C36 C 0.9344(3) -0.3419(3) 0.4695(2) 0.0513(8) Uani 1 1 d . . H36 H 0.9055 -0.4076 0.5063 0.062 Uiso 1 1 calc R U C37 C 1.0448(3) -0.3321(2) 0.4832(2) 0.0464(7) Uani 1 1 d . . H37 H 1.0921 -0.3913 0.5287 0.056 Uiso 1 1 calc R U C38 C 1.0866(2) -0.2366(2) 0.43087(18) 0.0360(6) Uani 1 1 d . . H38 H 1.1633 -0.2302 0.4392 0.043 Uiso 1 1 calc R U C39 C 1.0160(2) -0.1492(2) 0.36572(16) 0.0273(5) Uani 1 1 d . . H39 H 1.0440 -0.0818 0.3316 0.033 Uiso 1 1 calc R U C40 C 0.7962(2) -0.0811(2) 0.57625(17) 0.0362(6) Uani 1 1 d . . H40A H 0.8437 -0.1563 0.6096 0.043 Uiso 1 1 calc R U H40B H 0.7679 -0.0331 0.6199 0.043 Uiso 1 1 calc R U H40C H 0.7299 -0.0952 0.5492 0.043 Uiso 1 1 calc R U C41 C 0.81038(19) 0.0845(2) 0.45077(15) 0.0240(5) Uani 1 1 d . . C42 C 0.88434(19) 0.13270(19) 0.37149(15) 0.0229(5) Uani 1 1 d . . H42 H 0.9544 0.0855 0.3550 0.027 Uiso 1 1 calc R U C43 C 0.8479(2) 0.25223(19) 0.32010(16) 0.0245(5) Uani 1 1 d . . H43 H 0.7679 0.2886 0.3134 0.029 Uiso 1 1 calc R U C44 C 0.9387(2) 0.3168(2) 0.27801(17) 0.0304(5) Uani 1 1 d . . C45 C 0.9932(3) 0.4996(3) 0.2498(2) 0.0597(9) Uani 1 1 d . . H45A H 0.9615 0.5796 0.2549 0.072 Uiso 1 1 calc R U H45B H 1.0617 0.4650 0.2886 0.072 Uiso 1 1 calc R U H45C H 1.0152 0.5018 0.1844 0.072 Uiso 1 1 calc R U C46 C 0.5243(17) 0.5028(7) 0.5791(8) 0.255(8) Uani 1 1 d . . H46 H 0.5289 0.4917 0.6445 0.306 Uiso 1 1 calc R U C47 C 0.4029(11) 0.5173(7) 0.5455(7) 0.196(5) Uani 1 1 d . . H47 H 0.3421 0.5460 0.5845 0.235 Uiso 1 1 calc R U C48 C 0.3675(14) 0.4968(13) 0.4713(15) 0.357(14) Uani 1 1 d . . H48 H 0.2951 0.4856 0.4566 0.429 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 0.02102(14) 0.01706(15) 0.01973(15) -0.00460(11) -0.00095(11) -0.00491(10) P1 0.0206(3) 0.0167(3) 0.0214(3) -0.0056(2) -0.0010(2) -0.0041(2) P2 0.0216(3) 0.0175(3) 0.0192(3) -0.0043(2) 0.0001(2) -0.0056(2) O1 0.0233(7) 0.0174(7) 0.0191(7) -0.0041(6) 0.0005(6) -0.0032(6) O2 0.0282(8) 0.0292(9) 0.0240(8) -0.0007(7) -0.0001(7) -0.0078(7) O3 0.0276(9) 0.0352(9) 0.0277(9) -0.0099(7) 0.0030(7) -0.0063(7) O4 0.0551(11) 0.0227(9) 0.0456(11) -0.0034(8) -0.0132(9) -0.0169(8) O5 0.0321(10) 0.0382(11) 0.0470(11) 0.0006(9) -0.0014(8) -0.0140(8) C1 0.0200(10) 0.0204(11) 0.0215(11) -0.0023(9) -0.0015(8) -0.0050(8) C2 0.0204(10) 0.0214(11) 0.0236(11) -0.0052(9) -0.0020(9) -0.0045(8) C3 0.0276(11) 0.0183(11) 0.0258(12) -0.0035(9) -0.0040(9) -0.0021(9) C4 0.0308(12) 0.0239(12) 0.0247(12) 0.0019(9) -0.0054(10) -0.0042(9) C5 0.0297(12) 0.0294(12) 0.0187(11) -0.0045(9) -0.0004(9) -0.0076(10) C6 0.0238(11) 0.0225(11) 0.0223(11) -0.0066(9) -0.0012(9) -0.0057(9) C7 0.0325(12) 0.0243(12) 0.0228(11) -0.0084(9) -0.0013(9) -0.0068(9) C8 0.0258(11) 0.0201(11) 0.0239(11) -0.0065(9) 0.0020(9) -0.0101(9) C9 0.0195(10) 0.0162(10) 0.0253(11) -0.0061(9) 0.0026(8) -0.0064(8) C10 0.0219(10) 0.0179(10) 0.0233(11) -0.0049(8) 0.0015(9) -0.0083(8) C11 0.0240(11) 0.0214(11) 0.0285(12) -0.0063(9) -0.0011(9) -0.0069(9) C12 0.0224(11) 0.0240(12) 0.0341(13) -0.0115(10) 0.0036(10) -0.0043(9) C13 0.0266(11) 0.0253(12) 0.0268(12) -0.0106(9) 0.0062(9) -0.0083(9) C14 0.0353(13) 0.0280(13) 0.0362(14) -0.0090(11) -0.0071(11) -0.0104(10) C15 0.0508(16) 0.0341(14) 0.0235(12) -0.0108(11) -0.0017(11) -0.0040(12) C16 0.0228(10) 0.0176(11) 0.0284(12) -0.0058(9) 0.0002(9) -0.0071(8) C17 0.0268(12) 0.0311(13) 0.0278(12) -0.0046(10) 0.0002(10) -0.0060(10) C18 0.0347(14) 0.0400(15) 0.0308(14) -0.0044(11) 0.0082(11) -0.0081(11) C19 0.0232(12) 0.0344(14) 0.0464(16) -0.0060(12) 0.0067(11) -0.0077(10) C20 0.0235(11) 0.0331(14) 0.0453(15) -0.0091(11) -0.0048(11) -0.0074(10) C21 0.0276(12) 0.0264(12) 0.0305(13) -0.0071(10) -0.0038(10) -0.0063(9) C22 0.0241(10) 0.0183(10) 0.0203(11) -0.0019(8) -0.0052(9) -0.0052(8) C23 0.0256(11) 0.0230(12) 0.0313(13) -0.0073(10) -0.0001(10) -0.0046(9) C24 0.0317(12) 0.0307(13) 0.0323(13) -0.0054(10) 0.0007(10) -0.0138(10) C25 0.0418(14) 0.0218(12) 0.0314(13) -0.0044(10) -0.0039(11) -0.0134(10) C26 0.0355(13) 0.0205(12) 0.0364(14) -0.0116(10) -0.0022(11) -0.0018(10) C27 0.0269(11) 0.0224(12) 0.0283(12) -0.0087(9) -0.0001(9) -0.0054(9) C28 0.0243(11) 0.0213(11) 0.0215(11) -0.0024(9) 0.0000(9) -0.0071(9) C29 0.0292(12) 0.0298(13) 0.0301(13) -0.0112(10) 0.0054(10) -0.0095(10) C30 0.0301(13) 0.0428(15) 0.0339(14) -0.0148(12) 0.0077(11) -0.0122(11) C31 0.0312(13) 0.0532(17) 0.0370(14) -0.0115(13) 0.0078(11) -0.0223(12) C32 0.0426(15) 0.0538(17) 0.0387(15) -0.0215(13) 0.0065(12) -0.0286(13) C33 0.0326(12) 0.0395(14) 0.0287(13) -0.0161(11) 0.0056(10) -0.0159(11) C34 0.0311(12) 0.0176(11) 0.0210(11) -0.0052(9) -0.0009(9) -0.0024(9) C35 0.0446(15) 0.0268(13) 0.0371(14) 0.0010(11) -0.0080(12) -0.0128(11) C36 0.065(2) 0.0319(15) 0.0483(18) 0.0109(13) -0.0162(15) -0.0147(14) C37 0.0612(19) 0.0325(15) 0.0388(16) -0.0021(12) -0.0233(14) 0.0027(13) C38 0.0369(14) 0.0369(15) 0.0359(14) -0.0156(12) -0.0116(11) 0.0001(11) C39 0.0293(12) 0.0251(12) 0.0282(12) -0.0086(10) -0.0013(10) -0.0052(9) C40 0.0384(14) 0.0394(15) 0.0268(13) 0.0029(11) 0.0020(11) -0.0160(11) C41 0.0278(12) 0.0272(12) 0.0210(11) -0.0091(9) -0.0025(9) -0.0099(9) C42 0.0247(11) 0.0252(12) 0.0209(11) -0.0077(9) -0.0010(9) -0.0077(9) C43 0.0277(11) 0.0225(11) 0.0255(12) -0.0074(9) -0.0060(9) -0.0067(9) C44 0.0364(13) 0.0256(12) 0.0303(13) -0.0028(10) -0.0103(11) -0.0108(10) C45 0.075(2) 0.0362(17) 0.073(2) 0.0047(15) -0.0276(18) -0.0358(16) C46 0.49(2) 0.089(5) 0.217(11) -0.006(6) -0.233(14) -0.073(9) C47 0.325(15) 0.089(5) 0.154(7) -0.068(5) -0.011(8) 0.041(7) C48 0.310(19) 0.239(14) 0.56(3) -0.263(18) 0.17(2) -0.012(12) 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' 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' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 C42 Ni1 C43 42.14(9) . . C42 Ni1 P2 104.10(7) . . C43 Ni1 P2 146.20(7) . . C42 Ni1 P1 141.15(7) . . C43 Ni1 P1 100.37(7) . . P2 Ni1 P1 112.11(2) . . C16 P1 C22 102.51(10) . . C16 P1 C2 103.78(10) . . C22 P1 C2 98.43(10) . . C16 P1 Ni1 108.16(7) . . C22 P1 Ni1 113.44(7) . . C2 P1 Ni1 127.58(7) . . C28 P2 C10 103.58(10) . . C28 P2 C34 100.09(10) . . C10 P2 C34 100.48(10) . . C28 P2 Ni1 113.51(7) . . C10 P2 Ni1 118.10(7) . . C34 P2 Ni1 118.43(7) . . C1 O1 C9 112.32(15) . . C41 O2 C40 115.76(18) . . C44 O4 C45 115.7(2) . . C2 C1 O1 116.47(19) . . C2 C1 C6 124.5(2) . . O1 C1 C6 118.93(19) . . C1 C2 C3 116.3(2) . . C1 C2 P1 119.25(16) . . C3 C2 P1 124.11(17) . . C4 C3 C2 120.7(2) . . C4 C3 H3 119.7 . . C2 C3 H3 119.7 . . C3 C4 C5 120.8(2) . . C3 C4 H4 119.6 . . C5 C4 H4 119.6 . . C4 C5 C6 120.4(2) . . C4 C5 H5 119.8 . . C6 C5 H5 119.8 . . C5 C6 C1 117.1(2) . . C5 C6 C7 126.0(2) . . C1 C6 C7 116.87(19) . . C15 C7 C8 111.57(19) . . C15 C7 C6 112.47(19) . . C8 C7 C6 105.64(18) . . C15 C7 C14 108.9(2) . . C8 C7 C14 109.16(18) . . C6 C7 C14 108.98(19) . . C9 C8 C13 116.7(2) . . C9 C8 C7 116.92(19) . . C13 C8 C7 126.3(2) . . C8 C9 C10 124.9(2) . . C8 C9 O1 119.20(19) . . C10 C9 O1 115.91(18) . . C9 C10 C11 116.7(2) . . C9 C10 P2 117.06(16) . . C11 C10 P2 126.07(17) . . C12 C11 C10 120.2(2) . . C12 C11 H11 119.9 . . C10 C11 H11 119.9 . . C13 C12 C11 121.1(2) . . C13 C12 H12 119.4 . . C11 C12 H12 119.4 . . C12 C13 C8 120.2(2) . . C12 C13 H13 119.9 . . C8 C13 H13 119.9 . . C7 C14 H14A 109.5 . . C7 C14 H14B 109.5 . . H14A C14 H14B 109.5 . . C7 C14 H14C 109.5 . . H14A C14 H14C 109.5 . . H14B C14 H14C 109.5 . . C7 C15 H15A 109.5 . . C7 C15 H15B 109.5 . . H15A C15 H15B 109.5 . . C7 C15 H15C 109.5 . . H15A C15 H15C 109.5 . . H15B C15 H15C 109.5 . . C21 C16 C17 118.8(2) . . C21 C16 P1 122.95(17) . . C17 C16 P1 118.24(17) . . C18 C17 C16 120.4(2) . . C18 C17 H17 119.8 . . C16 C17 H17 119.8 . . C17 C18 C19 120.6(2) . . C17 C18 H18 119.7 . . C19 C18 H18 119.7 . . C20 C19 C18 119.3(2) . . C20 C19 H19 120.3 . . C18 C19 H19 120.3 . . C19 C20 C21 120.6(2) . . C19 C20 H20 119.7 . . C21 C20 H20 119.7 . . C20 C21 C16 120.4(2) . . C20 C21 H21 119.8 . . C16 C21 H21 119.8 . . C27 C22 C23 119.1(2) . . C27 C22 P1 123.32(16) . . C23 C22 P1 117.54(16) . . C24 C23 C22 120.4(2) . . C24 C23 H23 119.8 . . C22 C23 H23 119.8 . . C23 C24 C25 120.1(2) . . C23 C24 H24 120.0 . . C25 C24 H24 120.0 . . C26 C25 C24 119.8(2) . . C26 C25 H25 120.1 . . C24 C25 H25 120.1 . . C25 C26 C27 120.5(2) . . C25 C26 H26 119.8 . . C27 C26 H26 119.8 . . C22 C27 C26 120.2(2) . . C22 C27 H27 119.9 . . C26 C27 H27 119.9 . . C29 C28 C33 118.8(2) . . C29 C28 P2 117.06(17) . . C33 C28 P2 123.59(17) . . C30 C29 C28 120.7(2) . . C30 C29 H29 119.6 . . C28 C29 H29 119.6 . . C31 C30 C29 120.0(2) . . C31 C30 H30 120.0 . . C29 C30 H30 120.0 . . C30 C31 C32 120.0(2) . . C30 C31 H31 120.0 . . C32 C31 H31 120.0 . . C31 C32 C33 120.2(2) . . C31 C32 H32 119.9 . . C33 C32 H32 119.9 . . C32 C33 C28 120.2(2) . . C32 C33 H33 119.9 . . C28 C33 H33 119.9 . . C39 C34 C35 118.6(2) . . C39 C34 P2 119.33(17) . . C35 C34 P2 122.08(18) . . C36 C35 C34 119.8(2) . . C36 C35 H35 120.1 . . C34 C35 H35 120.1 . . C37 C36 C35 120.8(3) . . C37 C36 H36 119.6 . . C35 C36 H36 119.6 . . C38 C37 C36 119.9(3) . . C38 C37 H37 120.1 . . C36 C37 H37 120.1 . . C37 C38 C39 119.7(2) . . C37 C38 H38 120.2 . . C39 C38 H38 120.2 . . C34 C39 C38 121.2(2) . . C34 C39 H39 119.4 . . C38 C39 H39 119.4 . . O2 C40 H40A 109.5 . . O2 C40 H40B 109.5 . . H40A C40 H40B 109.5 . . O2 C40 H40C 109.5 . . H40A C40 H40C 109.5 . . H40B C40 H40C 109.5 . . O3 C41 O2 122.8(2) . . O3 C41 C42 125.8(2) . . O2 C41 C42 111.39(19) . . C43 C42 C41 118.2(2) . . C43 C42 Ni1 69.86(13) . . C41 C42 Ni1 108.87(14) . . C43 C42 H42 120.9 . . C41 C42 H42 120.9 . . Ni1 C42 H42 91.2 . . C42 C43 C44 117.5(2) . . C42 C43 Ni1 68.00(12) . . C44 C43 Ni1 116.91(16) . . C42 C43 H43 121.3 . . C44 C43 H43 121.3 . . Ni1 C43 H43 85.7 . . O5 C44 O4 122.6(2) . . O5 C44 C43 126.8(2) . . O4 C44 C43 110.6(2) . . O4 C45 H45A 109.5 . . O4 C45 H45B 109.5 . . H45A C45 H45B 109.5 . . O4 C45 H45C 109.5 . . H45A C45 H45C 109.5 . . H45B C45 H45C 109.5 . . C48 C46 C47 130.7(13) 2_666 . C48 C46 C47 40.4(10) 2_666 2_666 C47 C46 C47 91.8(7) . 2_666 C48 C46 H46 114.7 2_666 . C47 C46 H46 114.7 . . C47 C46 H46 151.1 2_666 . C48 C47 C46 131.0(11) . . C48 C47 C46 44.4(8) . 2_666 C46 C47 C46 88.2(7) . 2_666 C48 C47 H47 114.5 . . C46 C47 H47 114.5 . . C46 C47 H47 154.0 2_666 . C47 C48 C46 95.3(15) . 2_666 C47 C48 H48 132.4 . . C46 C48 H48 132.4 2_666 . loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 Ni1 C42 1.972(2) . Ni1 C43 1.997(2) . Ni1 P2 2.2056(6) . Ni1 P1 2.2097(6) . P1 C16 1.831(2) . P1 C22 1.841(2) . P1 C2 1.845(2) . P2 C28 1.831(2) . P2 C10 1.837(2) . P2 C34 1.847(2) . O1 C1 1.389(2) . O1 C9 1.393(2) . O2 C41 1.347(3) . O2 C40 1.441(3) . O3 C41 1.216(3) . O4 C44 1.353(3) . O4 C45 1.446(3) . O5 C44 1.213(3) . C1 C2 1.388(3) . C1 C6 1.393(3) . C2 C3 1.406(3) . C3 C4 1.386(3) . C3 H3 0.9500 . C4 C5 1.391(3) . C4 H4 0.9500 . C5 C6 1.392(3) . C5 H5 0.9500 . C6 C7 1.531(3) . C7 C15 1.527(3) . C7 C8 1.527(3) . C7 C14 1.546(3) . C8 C9 1.384(3) . C8 C13 1.398(3) . C9 C10 1.389(3) . C10 C11 1.395(3) . C11 C12 1.390(3) . C11 H11 0.9500 . C12 C13 1.390(3) . C12 H12 0.9500 . C13 H13 0.9500 . C14 H14A 0.9800 . C14 H14B 0.9800 . C14 H14C 0.9800 . C15 H15A 0.9800 . C15 H15B 0.9800 . C15 H15C 0.9800 . C16 C21 1.395(3) . C16 C17 1.396(3) . C17 C18 1.384(3) . C17 H17 0.9500 . C18 C19 1.388(4) . C18 H18 0.9500 . C19 C20 1.382(4) . C19 H19 0.9500 . C20 C21 1.387(3) . C20 H20 0.9500 . C21 H21 0.9500 . C22 C27 1.384(3) . C22 C23 1.402(3) . C23 C24 1.382(3) . C23 H23 0.9500 . C24 C25 1.388(3) . C24 H24 0.9500 . C25 C26 1.380(3) . C25 H25 0.9500 . C26 C27 1.392(3) . C26 H26 0.9500 . C27 H27 0.9500 . C28 C29 1.390(3) . C28 C33 1.391(3) . C29 C30 1.385(3) . C29 H29 0.9500 . C30 C31 1.375(4) . C30 H30 0.9500 . C31 C32 1.385(4) . C31 H31 0.9500 . C32 C33 1.386(3) . C32 H32 0.9500 . C33 H33 0.9500 . C34 C39 1.383(3) . C34 C35 1.396(3) . C35 C36 1.388(4) . C35 H35 0.9500 . C36 C37 1.375(4) . C36 H36 0.9500 . C37 C38 1.375(4) . C37 H37 0.9500 . C38 C39 1.390(3) . C38 H38 0.9500 . C39 H39 0.9500 . C40 H40A 0.9800 . C40 H40B 0.9800 . C40 H40C 0.9800 . C41 C42 1.472(3) . C42 C43 1.427(3) . C42 H42 0.9500 . C43 C44 1.467(3) . C43 H43 0.9500 . C45 H45A 0.9800 . C45 H45B 0.9800 . C45 H45C 0.9800 . C46 C48 1.42(2) 2_666 C46 C47 1.518(16) . C46 C47 2.028(16) 2_666 C46 H46 0.9500 . C47 C48 1.32(2) . C47 C46 2.028(16) 2_666 C47 H47 0.9500 . C48 C46 1.42(2) 2_666 C48 H48 0.9500 . 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_4 C9 O1 C1 C2 -132.51(19) . . C9 O1 C1 C6 44.7(2) . . O1 C1 C2 C3 -177.34(18) . . C6 C1 C2 C3 5.6(3) . . O1 C1 C2 P1 9.2(3) . . C6 C1 C2 P1 -167.81(17) . . C16 P1 C2 C1 -92.46(18) . . C22 P1 C2 C1 162.36(17) . . Ni1 P1 C2 C1 33.9(2) . . C16 P1 C2 C3 94.6(2) . . C22 P1 C2 C3 -10.6(2) . . Ni1 P1 C2 C3 -138.97(16) . . C1 C2 C3 C4 -3.3(3) . . P1 C2 C3 C4 169.81(17) . . C2 C3 C4 C5 -0.6(3) . . C3 C4 C5 C6 2.6(3) . . C4 C5 C6 C1 -0.5(3) . . C4 C5 C6 C7 -178.1(2) . . C2 C1 C6 C5 -3.8(3) . . O1 C1 C6 C5 179.25(18) . . C2 C1 C6 C7 174.0(2) . . O1 C1 C6 C7 -2.9(3) . . C5 C6 C7 C15 16.8(3) . . C1 C6 C7 C15 -160.8(2) . . C5 C6 C7 C8 138.7(2) . . C1 C6 C7 C8 -38.9(2) . . C5 C6 C7 C14 -104.1(3) . . C1 C6 C7 C14 78.3(2) . . C15 C7 C8 C9 165.65(19) . . C6 C7 C8 C9 43.1(2) . . C14 C7 C8 C9 -73.9(2) . . C15 C7 C8 C13 -14.9(3) . . C6 C7 C8 C13 -137.4(2) . . C14 C7 C8 C13 105.5(2) . . C13 C8 C9 C10 -3.7(3) . . C7 C8 C9 C10 175.81(19) . . C13 C8 C9 O1 175.06(17) . . C7 C8 C9 O1 -5.5(3) . . C1 O1 C9 C8 -40.3(2) . . C1 O1 C9 C10 138.56(18) . . C8 C9 C10 C11 2.1(3) . . O1 C9 C10 C11 -176.67(17) . . C8 C9 C10 P2 178.39(16) . . O1 C9 C10 P2 -0.4(2) . . C28 P2 C10 C9 66.98(17) . . C34 P2 C10 C9 170.16(16) . . Ni1 P2 C10 C9 -59.48(17) . . C28 P2 C10 C11 -117.13(19) . . C34 P2 C10 C11 -14.0(2) . . Ni1 P2 C10 C11 116.41(17) . . C9 C10 C11 C12 1.0(3) . . P2 C10 C11 C12 -174.92(16) . . C10 C11 C12 C13 -2.3(3) . . C11 C12 C13 C8 0.7(3) . . C9 C8 C13 C12 2.2(3) . . C7 C8 C13 C12 -177.2(2) . . C22 P1 C16 C21 88.9(2) . . C2 P1 C16 C21 -13.2(2) . . Ni1 P1 C16 C21 -151.03(17) . . C22 P1 C16 C17 -89.36(19) . . C2 P1 C16 C17 168.57(18) . . Ni1 P1 C16 C17 30.74(19) . . C21 C16 C17 C18 -0.7(3) . . P1 C16 C17 C18 177.63(19) . . C16 C17 C18 C19 0.3(4) . . C17 C18 C19 C20 0.1(4) . . C18 C19 C20 C21 -0.1(4) . . C19 C20 C21 C16 -0.2(4) . . C17 C16 C21 C20 0.6(3) . . P1 C16 C21 C20 -177.58(18) . . C16 P1 C22 C27 -0.6(2) . . C2 P1 C22 C27 105.6(2) . . Ni1 P1 C22 C27 -117.00(18) . . C16 P1 C22 C23 -178.55(18) . . C2 P1 C22 C23 -72.32(19) . . Ni1 P1 C22 C23 65.08(19) . . C27 C22 C23 C24 -0.4(3) . . P1 C22 C23 C24 177.64(18) . . C22 C23 C24 C25 1.5(4) . . C23 C24 C25 C26 -1.8(4) . . C24 C25 C26 C27 1.1(4) . . C23 C22 C27 C26 -0.4(3) . . P1 C22 C27 C26 -178.29(18) . . C25 C26 C27 C22 0.1(4) . . C10 P2 C28 C29 -171.47(18) . . C34 P2 C28 C29 85.05(19) . . Ni1 P2 C28 C29 -42.2(2) . . C10 P2 C28 C33 16.7(2) . . C34 P2 C28 C33 -86.7(2) . . Ni1 P2 C28 C33 146.04(19) . . C33 C28 C29 C30 1.9(4) . . P2 C28 C29 C30 -170.3(2) . . C28 C29 C30 C31 -1.1(4) . . C29 C30 C31 C32 -0.4(4) . . C30 C31 C32 C33 1.0(5) . . C31 C32 C33 C28 -0.1(4) . . C29 C28 C33 C32 -1.3(4) . . P2 C28 C33 C32 170.3(2) . . C28 P2 C34 C39 -167.65(18) . . C10 P2 C34 C39 86.36(19) . . Ni1 P2 C34 C39 -43.8(2) . . C28 P2 C34 C35 12.3(2) . . C10 P2 C34 C35 -93.7(2) . . Ni1 P2 C34 C35 136.20(18) . . C39 C34 C35 C36 0.3(4) . . P2 C34 C35 C36 -179.6(2) . . C34 C35 C36 C37 -1.6(5) . . C35 C36 C37 C38 0.8(5) . . C36 C37 C38 C39 1.3(4) . . C35 C34 C39 C38 1.8(3) . . P2 C34 C39 C38 -178.26(18) . . C37 C38 C39 C34 -2.6(4) . . C40 O2 C41 O3 5.9(3) . . C40 O2 C41 C42 -173.75(19) . . O3 C41 C42 C43 11.8(3) . . O2 C41 C42 C43 -168.54(19) . . O3 C41 C42 Ni1 -64.9(3) . . O2 C41 C42 Ni1 114.73(17) . . C41 C42 C43 C44 148.9(2) . . Ni1 C42 C43 C44 -109.9(2) . . C41 C42 C43 Ni1 -101.18(19) . . C45 O4 C44 O5 -3.0(4) . . C45 O4 C44 C43 174.5(2) . . C42 C43 C44 O5 33.3(4) . . Ni1 C43 C44 O5 -44.6(3) . . C42 C43 C44 O4 -144.1(2) . . Ni1 C43 C44 O4 138.02(17) . . C48 C46 C47 C48 25(3) 2_666 . C47 C46 C47 C48 13.0(15) 2_666 . C48 C46 C47 C46 12.0(12) 2_666 2_666 C47 C46 C47 C46 0.000(2) 2_666 2_666 C46 C47 C48 C46 -19(2) . 2_666