#------------------------------------------------------------------------------ #$Date: 2016-03-26 14:43:29 +0200 (Sat, 26 Mar 2016) $ #$Revision: 180274 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/11/60/7116078.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_7116078 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 'C53 H42 Ni O P2, C6 H6' _chemical_formula_sum 'C59 H48 Ni O P2' _chemical_formula_weight 893.62 _chemical_name_systematic 'Xantphos Ni Diphenylacetylene' _chemical_properties_physical 'Air-sensitive, Moisture-sensitive, Oxygen-sensitive' _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_Hall '-P 2yn' _space_group_name_H-M_alt 'P 1 21/n 1' _symmetry_space_group_name_Hall '-P 2yn' _symmetry_space_group_name_H-M 'P 1 21/n 1' _atom_sites_solution_hydrogens geom _audit_creation_method SHELXL-2014 _cell_angle_alpha 90 _cell_angle_beta 98.8516(10) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 12.8793(3) _cell_length_b 18.2497(3) _cell_length_c 19.5980(5) _cell_measurement_reflns_used 9768 _cell_measurement_temperature 150(1) _cell_measurement_theta_max 27.485 _cell_measurement_theta_min 1.018 _cell_volume 4551.52(17) _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 0.997 _diffrn_measured_fraction_theta_max 0.992 _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 0.1244 _diffrn_reflns_av_unetI/netI 0.0752 _diffrn_reflns_Laue_measured_fraction_full 0.997 _diffrn_reflns_Laue_measured_fraction_max 0.992 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_number 60117 _diffrn_reflns_point_group_measured_fraction_full 0.997 _diffrn_reflns_point_group_measured_fraction_max 0.992 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 27.001 _diffrn_reflns_theta_min 2.096 _diffrn_source 'fine-focus sealed tube' _exptl_absorpt_coefficient_mu 0.539 _exptl_absorpt_correction_T_max 0.933 _exptl_absorpt_correction_T_min 0.877 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'DENZO-SMN (Otwinowski & Minor, 1997)' _exptl_crystal_colour orange _exptl_crystal_density_diffrn 1.304 _exptl_crystal_description prism _exptl_crystal_F_000 1872 _exptl_crystal_size_max 0.250 _exptl_crystal_size_mid 0.230 _exptl_crystal_size_min 0.130 _refine_diff_density_max 0.366 _refine_diff_density_min -0.433 _refine_diff_density_rms 0.084 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.084 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 568 _refine_ls_number_reflns 9871 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.084 _refine_ls_R_factor_all 0.1186 _refine_ls_R_factor_gt 0.0516 _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^)+(0.0039P)^2^+7.5454P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0755 _refine_ls_wR_factor_ref 0.0950 _reflns_Friedel_coverage 0.000 _reflns_number_gt 6050 _reflns_number_total 9871 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file c4cc07590k3.cif _cod_data_source_block nanny _cod_database_code 7116078 #BEGIN Tags that were not found in dictionaries: _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 0.877 _shelx_estimated_absorpt_t_max 0.933 _shelxl_version_number 2014-3 _shelx_res_file ; TITL jl070 nds @150K Orange Prism Monoclinic P21/n 7/2/2014 ama SHELXL CELL 0.71073 12.8793 18.2497 19.5980 90.0000 98.8516 90.0000 ZERR 4 0.0003 0.0003 0.0005 0.0000 0.0010 0.0000 LATT 1 SYMM 1/2 - X, 1/2 + Y, 1/2 - Z SFAC C H O P Ni UNIT 236 192 4 8 4 TEMP -123 SIZE 0.25 0.23 0.13 OMIT 1 0 1 OMIT 0 0 2 ACTA CONF BOND $H FMAP 2 PLAN -20 L.S. 28 WGHT 0.003900 7.545400 FVAR 0.43696 NI1 5 0.041193 0.048373 0.334676 11.00000 0.01350 0.01383 = 0.01701 0.00158 0.00317 0.00061 P1 4 0.126329 0.144304 0.302467 11.00000 0.01377 0.01368 = 0.01636 0.00157 0.00325 0.00132 P2 4 0.121484 -0.052242 0.308640 11.00000 0.01329 0.01380 = 0.01539 -0.00016 0.00151 0.00020 O1 3 0.298093 0.043342 0.306584 11.00000 0.01602 0.01165 = 0.01797 0.00112 0.00101 0.00087 C1 1 0.336118 0.106742 0.340534 11.00000 0.01735 0.01554 = 0.01529 0.00036 0.00535 -0.00260 C2 1 0.264320 0.163421 0.339322 11.00000 0.01661 0.01602 = 0.01432 0.00300 0.00312 -0.00160 C3 1 0.301521 0.228813 0.371169 11.00000 0.02006 0.01689 = 0.02714 0.00047 0.00545 0.00166 AFIX 43 H3 2 0.256042 0.269881 0.370466 11.00000 -1.20000 AFIX 0 C4 1 0.404965 0.233892 0.403885 11.00000 0.02484 0.01586 = 0.03340 -0.00843 0.00203 -0.00370 AFIX 43 H4 2 0.429394 0.278555 0.425548 11.00000 -1.20000 AFIX 0 C40 1 -0.191660 0.195101 0.308903 11.00000 0.02273 0.02453 = 0.02536 -0.00099 0.00205 0.00145 AFIX 43 H40 2 -0.174009 0.184765 0.264582 11.00000 -1.20000 AFIX 0 C54 1 0.687405 0.101274 0.053482 11.00000 0.05218 0.07518 = 0.04285 0.01076 0.00986 0.00666 AFIX 43 H54 2 0.671949 0.143495 0.025400 11.00000 -1.20000 AFIX 0 C5 1 0.473146 0.174869 0.405448 11.00000 0.01899 0.02326 = 0.02716 -0.00292 -0.00167 -0.00140 AFIX 43 H5 2 0.543025 0.179199 0.429083 11.00000 -1.20000 AFIX 0 C6 1 0.440169 0.109375 0.372730 11.00000 0.01732 0.01853 = 0.02101 -0.00001 0.00462 -0.00086 C7 1 0.509147 0.041724 0.368299 11.00000 0.01454 0.01803 = 0.02304 -0.00144 0.00157 0.00079 C8 1 0.438904 -0.025022 0.372315 11.00000 0.01154 0.01930 = 0.01625 -0.00371 0.00107 -0.00063 C9 1 0.334007 -0.019954 0.341435 11.00000 0.01969 0.01437 = 0.01265 -0.00147 0.00398 0.00389 C10 1 0.259463 -0.074588 0.343016 11.00000 0.01789 0.01430 = 0.01241 -0.00141 0.00307 0.00192 C11 1 0.294622 -0.140607 0.374814 11.00000 0.01907 0.01592 = 0.01771 -0.00001 0.00373 -0.00027 AFIX 43 H11 2 0.246925 -0.180092 0.376200 11.00000 -1.20000 AFIX 0 C12 1 0.399097 -0.148464 0.404331 11.00000 0.02225 0.01348 = 0.02335 0.00205 0.00033 0.00350 AFIX 43 H12 2 0.422564 -0.193854 0.424898 11.00000 -1.20000 AFIX 0 C13 1 0.469919 -0.091065 0.404301 11.00000 0.01598 0.02309 = 0.02173 -0.00107 0.00006 0.00661 AFIX 43 H13 2 0.540387 -0.097062 0.426420 11.00000 -1.20000 AFIX 0 C14 1 0.548826 0.043385 0.297583 11.00000 0.02079 0.02010 = 0.03646 0.00081 0.01076 0.00077 AFIX 33 H14A 2 0.593830 0.086356 0.295403 11.00000 -1.20000 H14B 2 0.589139 -0.001224 0.292191 11.00000 -1.20000 H14C 2 0.488604 0.046073 0.260428 11.00000 -1.20000 AFIX 0 C15 1 0.604116 0.040126 0.425478 11.00000 0.01415 0.02567 = 0.03797 -0.00260 -0.00330 0.00121 AFIX 33 H15A 2 0.647771 0.083481 0.421705 11.00000 -1.20000 H15B 2 0.580094 0.040064 0.470559 11.00000 -1.20000 H15C 2 0.645444 -0.004192 0.420875 11.00000 -1.20000 AFIX 0 C16 1 0.126436 0.146914 0.208875 11.00000 0.02374 0.01207 = 0.01911 0.00170 0.00301 -0.00145 C17 1 0.216698 0.151894 0.178594 11.00000 0.02787 0.02803 = 0.02402 0.00469 0.00728 0.00447 AFIX 43 H17 2 0.283507 0.154660 0.206823 11.00000 -1.20000 AFIX 0 C18 1 0.209795 0.152856 0.107076 11.00000 0.04123 0.03316 = 0.02886 0.00569 0.01747 0.00083 AFIX 43 H18 2 0.271874 0.155212 0.086521 11.00000 -1.20000 AFIX 0 C19 1 0.112354 0.150375 0.065858 11.00000 0.05957 0.02532 = 0.01788 -0.00137 0.00893 -0.00398 AFIX 43 H19 2 0.107610 0.151512 0.017013 11.00000 -1.20000 AFIX 0 C20 1 0.022743 0.146285 0.095401 11.00000 0.04327 0.03086 = 0.02632 0.00094 -0.00584 -0.01176 AFIX 43 H20 2 -0.044089 0.145479 0.067058 11.00000 -1.20000 AFIX 0 C21 1 0.029591 0.143332 0.166386 11.00000 0.02841 0.03030 = 0.02451 0.00096 0.00215 -0.00963 AFIX 43 H21 2 -0.032713 0.138794 0.186451 11.00000 -1.20000 AFIX 0 C22 1 0.070579 0.234346 0.317753 11.00000 0.00977 0.01594 = 0.02374 0.00015 0.00338 -0.00245 C23 1 0.057484 0.289433 0.268216 11.00000 0.02474 0.02207 = 0.02584 0.00437 0.01071 0.00329 AFIX 43 H23 2 0.073914 0.280038 0.223408 11.00000 -1.20000 AFIX 0 C24 1 0.020783 0.357786 0.283477 11.00000 0.03237 0.02140 = 0.03796 0.01114 0.01105 0.00454 AFIX 43 H24 2 0.011413 0.394793 0.248986 11.00000 -1.20000 AFIX 0 C25 1 -0.002277 0.372483 0.348519 11.00000 0.02765 0.01905 = 0.04611 -0.00200 0.01098 0.00607 AFIX 43 H25 2 -0.026974 0.419605 0.358949 11.00000 -1.20000 AFIX 0 C26 1 0.010756 0.318061 0.398799 11.00000 0.02628 0.02694 = 0.02448 -0.00416 0.00755 0.00235 AFIX 43 H26 2 -0.004772 0.328024 0.443727 11.00000 -1.20000 AFIX 0 C27 1 0.046298 0.249507 0.383368 11.00000 0.01665 0.01423 = 0.02388 0.00112 0.00140 0.00019 AFIX 43 H27 2 0.054301 0.212325 0.417703 11.00000 -1.20000 AFIX 0 C28 1 0.119561 -0.055252 0.215334 11.00000 0.02833 0.01193 = 0.01782 -0.00033 -0.00066 -0.00179 C29 1 0.206824 -0.070241 0.184292 11.00000 0.03529 0.02803 = 0.02005 -0.00270 0.00733 -0.00832 AFIX 43 H29 2 0.272644 -0.079834 0.212002 11.00000 -1.20000 AFIX 0 C30 1 0.198447 -0.071290 0.112994 11.00000 0.06615 0.03633 = 0.02601 -0.00604 0.01865 -0.01835 AFIX 43 H30 2 0.258863 -0.081253 0.092185 11.00000 -1.20000 AFIX 0 C31 1 0.104002 -0.058123 0.072076 11.00000 0.10185 0.02317 = 0.01323 0.00019 -0.00223 -0.01007 AFIX 43 H31 2 0.099104 -0.058544 0.023212 11.00000 -1.20000 AFIX 0 C32 1 0.016316 -0.044287 0.102294 11.00000 0.07296 0.02877 = 0.02844 -0.00176 -0.02374 0.01026 AFIX 43 H32 2 -0.049597 -0.036167 0.074164 11.00000 -1.20000 AFIX 0 C33 1 0.023801 -0.042154 0.173619 11.00000 0.04331 0.02668 = 0.02927 -0.00383 -0.00883 0.01099 AFIX 43 H33 2 -0.036766 -0.031696 0.194106 11.00000 -1.20000 AFIX 0 C34 1 0.062552 -0.141198 0.324346 11.00000 0.01544 0.01288 = 0.02255 0.00118 -0.00047 0.00182 C35 1 0.041633 -0.155634 0.390469 11.00000 0.01775 0.02614 = 0.02305 0.00443 0.00281 0.00465 AFIX 43 H35 2 0.050663 -0.118142 0.424495 11.00000 -1.20000 AFIX 0 C36 1 0.007593 -0.224607 0.407037 11.00000 0.02479 0.03049 = 0.04505 0.01895 0.01368 0.00624 AFIX 43 H36 2 -0.005879 -0.234203 0.452508 11.00000 -1.20000 AFIX 0 C37 1 -0.006833 -0.279398 0.357868 11.00000 0.02348 0.01905 = 0.06947 0.01222 0.00882 -0.00274 AFIX 43 H37 2 -0.029712 -0.326640 0.369476 11.00000 -1.20000 AFIX 0 C38 1 0.012275 -0.265010 0.291541 11.00000 0.02964 0.01780 = 0.05412 -0.00653 0.00347 -0.00600 AFIX 43 H38 2 0.001037 -0.302252 0.257332 11.00000 -1.20000 AFIX 0 C39 1 0.047786 -0.196432 0.274727 11.00000 0.02163 0.02139 = 0.03382 -0.00107 0.00094 -0.00277 AFIX 43 H39 2 0.062007 -0.187199 0.229362 11.00000 -1.20000 AFIX 0 C41 1 -0.256706 0.253826 0.316836 11.00000 0.02695 0.02914 = 0.04184 0.00638 0.00310 0.00650 AFIX 43 H41 2 -0.285073 0.282442 0.277907 11.00000 -1.20000 AFIX 0 C42 1 -0.280395 0.270838 0.381434 11.00000 0.02633 0.02399 = 0.05845 -0.00344 0.01335 0.00659 AFIX 43 H42 2 -0.324460 0.311443 0.387043 11.00000 -1.20000 AFIX 0 C43 1 -0.239801 0.228614 0.437873 11.00000 0.03219 0.02934 = 0.04180 -0.01000 0.01702 -0.00162 AFIX 43 H43 2 -0.255067 0.240660 0.482434 11.00000 -1.20000 AFIX 0 C44 1 -0.176752 0.168634 0.429404 11.00000 0.02445 0.02331 = 0.02872 -0.00157 0.00451 -0.00200 AFIX 43 H44 2 -0.150356 0.139260 0.468236 11.00000 -1.20000 AFIX 0 C45 1 -0.151606 0.150886 0.364660 11.00000 0.01191 0.01617 = 0.02426 -0.00194 0.00274 -0.00127 C46 1 -0.086359 0.086514 0.357361 11.00000 0.01666 0.02065 = 0.01783 -0.00003 0.00318 0.00019 C47 1 -0.083441 0.017142 0.366267 11.00000 0.01413 0.02252 = 0.01739 0.00115 0.00075 -0.00037 C48 1 -0.142864 -0.044246 0.388905 11.00000 0.01273 0.01947 = 0.02457 0.00372 0.00416 0.00487 C49 1 -0.144097 -0.056365 0.459441 11.00000 0.01944 0.03200 = 0.02597 0.00821 0.00450 0.00507 AFIX 43 H49 2 -0.105240 -0.024848 0.492556 11.00000 -1.20000 AFIX 0 C50 1 -0.200968 -0.113426 0.481386 11.00000 0.02981 0.04244 = 0.03516 0.02244 0.01466 0.01315 AFIX 43 H50 2 -0.201128 -0.120659 0.529374 11.00000 -1.20000 AFIX 0 C51 1 -0.257410 -0.159913 0.434416 11.00000 0.02613 0.02906 = 0.06064 0.02280 0.01992 0.00428 AFIX 43 H51 2 -0.296059 -0.199308 0.449852 11.00000 -1.20000 AFIX 0 C52 1 -0.257612 -0.149017 0.364606 11.00000 0.02749 0.02356 = 0.05419 0.00016 0.00862 -0.00538 AFIX 43 H52 2 -0.297300 -0.180651 0.331995 11.00000 -1.20000 AFIX 0 C53 1 -0.199992 -0.091959 0.341841 11.00000 0.02321 0.02155 = 0.02769 0.00330 0.00668 0.00052 AFIX 43 H53 2 -0.199598 -0.085475 0.293785 11.00000 -1.20000 AFIX 0 C55 1 0.734831 0.108201 0.121058 11.00000 0.03730 0.05579 = 0.04704 -0.00281 0.00196 0.01454 AFIX 43 H55 2 0.752370 0.155433 0.139732 11.00000 -1.20000 AFIX 0 C56 1 0.756855 0.047224 0.161517 11.00000 0.03217 0.05658 = 0.04463 0.00026 -0.00608 0.00144 AFIX 43 H56 2 0.788244 0.052244 0.208423 11.00000 -1.20000 AFIX 0 C57 1 0.733569 -0.020846 0.134250 11.00000 0.04996 0.05839 = 0.05249 0.00673 -0.00258 -0.01246 AFIX 43 H57 2 0.750491 -0.062899 0.162334 11.00000 -1.20000 AFIX 0 C58 1 0.686214 -0.029564 0.067079 11.00000 0.05561 0.07491 = 0.04319 -0.00999 0.01556 -0.03048 AFIX 43 H58 2 0.670071 -0.077049 0.048574 11.00000 -1.20000 AFIX 0 C59 1 0.662508 0.032246 0.026920 11.00000 0.05590 0.10089 = 0.02508 0.00106 0.01400 -0.02235 AFIX 43 H59 2 0.628717 0.027207 -0.019466 11.00000 -1.20000 AFIX 0 HKLF 4 REM jl070 nds @150K Orange Prism Monoclinic P21/n 7/2/2014 ama SHELXL REM R1 = 0.0516 for 6050 Fo > 4sig(Fo) and 0.1186 for all 9871 data REM 568 parameters refined using 0 restraints END WGHT 0.0039 7.5455 REM Highest difference peak 0.366, deepest hole -0.433, 1-sigma level 0.084 Q1 1 0.2442 -0.1597 0.2340 11.00000 0.05 0.37 Q2 1 0.1343 0.1381 0.2492 11.00000 0.05 0.35 Q3 1 0.7935 0.1463 0.0362 11.00000 0.05 0.35 Q4 1 0.0810 -0.1014 0.3170 11.00000 0.05 0.34 Q5 1 0.0290 -0.1435 0.3453 11.00000 0.05 0.33 Q6 1 0.4736 -0.2361 0.3829 11.00000 0.05 0.32 Q7 1 0.2554 0.1573 0.1911 11.00000 0.05 0.32 Q8 1 0.1132 -0.0583 0.2578 11.00000 0.05 0.32 Q9 1 0.7950 -0.0463 0.0213 11.00000 0.05 0.32 Q10 1 -0.0236 0.3608 0.2499 11.00000 0.05 0.31 Q11 1 0.0214 -0.1616 0.2885 11.00000 0.05 0.29 Q12 1 0.6415 -0.0768 0.3089 11.00000 0.05 0.29 Q13 1 0.0935 0.2008 0.3082 11.00000 0.05 0.29 Q14 1 -0.1005 -0.2406 0.2888 11.00000 0.05 0.29 Q15 1 0.2678 0.4598 -0.0034 11.00000 0.05 0.29 Q16 1 0.1981 -0.0946 0.1464 11.00000 0.05 0.29 Q17 1 0.3155 -0.0646 0.1057 11.00000 0.05 0.29 Q18 1 0.2035 -0.0643 0.3168 11.00000 0.05 0.29 Q19 1 -0.1047 -0.1395 0.5109 11.00000 0.05 0.28 Q20 1 0.3041 0.2441 0.1545 11.00000 0.05 0.28 ; _shelx_res_checksum 98767 #END Tags that were not found in dictionaries loop_ _space_group_symop_operation_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -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 0.04119(3) 0.04837(2) 0.33468(2) 0.01469(9) Uani 1 1 d . . P1 P 0.12633(6) 0.14430(4) 0.30247(4) 0.01451(17) Uani 1 1 d . . P2 P 0.12148(5) -0.05224(4) 0.30864(4) 0.01423(16) Uani 1 1 d . . O1 O 0.29809(14) 0.04334(10) 0.30658(9) 0.0154(4) Uani 1 1 d . . C1 C 0.3361(2) 0.10674(15) 0.34053(15) 0.0158(6) Uani 1 1 d . . C2 C 0.2643(2) 0.16342(15) 0.33932(15) 0.0156(6) Uani 1 1 d . . C3 C 0.3015(2) 0.22881(16) 0.37117(16) 0.0212(7) Uani 1 1 d . . H3 H 0.2560 0.2699 0.3705 0.025 Uiso 1 1 calc R U C4 C 0.4050(2) 0.23389(17) 0.40388(17) 0.0250(7) Uani 1 1 d . . H4 H 0.4294 0.2786 0.4255 0.030 Uiso 1 1 calc R U C40 C -0.1917(2) 0.19510(16) 0.30890(17) 0.0244(7) Uani 1 1 d . . H40 H -0.1740 0.1848 0.2646 0.029 Uiso 1 1 calc R U C54 C 0.6874(3) 0.1013(3) 0.0535(2) 0.0565(12) Uani 1 1 d . . H54 H 0.6719 0.1435 0.0254 0.068 Uiso 1 1 calc R U C5 C 0.4731(3) 0.17487(16) 0.40545(16) 0.0237(7) Uani 1 1 d . . H5 H 0.5430 0.1792 0.4291 0.028 Uiso 1 1 calc R U C6 C 0.4402(2) 0.10938(16) 0.37273(15) 0.0188(7) Uani 1 1 d . . C7 C 0.5091(2) 0.04172(16) 0.36830(14) 0.0187(6) Uani 1 1 d . . C8 C 0.4389(2) -0.02502(15) 0.37232(15) 0.0158(6) Uani 1 1 d . . C9 C 0.3340(2) -0.01995(15) 0.34144(14) 0.0154(6) Uani 1 1 d . . C10 C 0.2595(2) -0.07459(15) 0.34302(14) 0.0148(6) Uani 1 1 d . . C11 C 0.2946(2) -0.14061(16) 0.37481(14) 0.0175(6) Uani 1 1 d . . H11 H 0.2469 -0.1801 0.3762 0.021 Uiso 1 1 calc R U C12 C 0.3991(2) -0.14846(16) 0.40433(15) 0.0200(7) Uani 1 1 d . . H12 H 0.4226 -0.1939 0.4249 0.024 Uiso 1 1 calc R U C13 C 0.4699(2) -0.09107(16) 0.40430(15) 0.0206(7) Uani 1 1 d . . H13 H 0.5404 -0.0971 0.4264 0.025 Uiso 1 1 calc R U C14 C 0.5488(2) 0.04339(18) 0.29758(15) 0.0251(7) Uani 1 1 d . . H14A H 0.5938 0.0864 0.2954 0.030 Uiso 1 1 calc R U H14B H 0.5891 -0.0012 0.2922 0.030 Uiso 1 1 calc R U H14C H 0.4886 0.0461 0.2604 0.030 Uiso 1 1 calc R U C15 C 0.6041(2) 0.04013(18) 0.42548(16) 0.0267(7) Uani 1 1 d . . H15A H 0.6478 0.0835 0.4217 0.032 Uiso 1 1 calc R U H15B H 0.5801 0.0401 0.4706 0.032 Uiso 1 1 calc R U H15C H 0.6454 -0.0042 0.4209 0.032 Uiso 1 1 calc R U C16 C 0.1264(2) 0.14691(15) 0.20888(15) 0.0183(7) Uani 1 1 d . . C17 C 0.2167(3) 0.15189(17) 0.17859(16) 0.0263(7) Uani 1 1 d . . H17 H 0.2835 0.1547 0.2068 0.032 Uiso 1 1 calc R U C18 C 0.2098(3) 0.15286(18) 0.10708(18) 0.0331(9) Uani 1 1 d . . H18 H 0.2719 0.1552 0.0865 0.040 Uiso 1 1 calc R U C19 C 0.1124(3) 0.15038(18) 0.06586(18) 0.0339(9) Uani 1 1 d . . H19 H 0.1076 0.1515 0.0170 0.041 Uiso 1 1 calc R U C20 C 0.0227(3) 0.14628(18) 0.09540(17) 0.0347(9) Uani 1 1 d . . H20 H -0.0441 0.1455 0.0671 0.042 Uiso 1 1 calc R U C21 C 0.0296(3) 0.14333(18) 0.16639(16) 0.0279(8) Uani 1 1 d . . H21 H -0.0327 0.1388 0.1865 0.034 Uiso 1 1 calc R U C22 C 0.0706(2) 0.23435(15) 0.31775(15) 0.0164(6) Uani 1 1 d . . C23 C 0.0575(2) 0.28943(16) 0.26822(16) 0.0235(7) Uani 1 1 d . . H23 H 0.0739 0.2800 0.2234 0.028 Uiso 1 1 calc R U C24 C 0.0208(3) 0.35779(17) 0.28348(18) 0.0300(8) Uani 1 1 d . . H24 H 0.0114 0.3948 0.2490 0.036 Uiso 1 1 calc R U C25 C -0.0023(3) 0.37248(18) 0.34852(18) 0.0304(8) Uani 1 1 d . . H25 H -0.0270 0.4196 0.3589 0.036 Uiso 1 1 calc R U C26 C 0.0108(2) 0.31806(17) 0.39880(17) 0.0255(7) Uani 1 1 d . . H26 H -0.0048 0.3280 0.4437 0.031 Uiso 1 1 calc R U C27 C 0.0463(2) 0.24951(15) 0.38337(16) 0.0184(7) Uani 1 1 d . . H27 H 0.0543 0.2123 0.4177 0.022 Uiso 1 1 calc R U C28 C 0.1196(2) -0.05525(16) 0.21533(14) 0.0198(6) Uani 1 1 d . . C29 C 0.2068(3) -0.07024(17) 0.18429(16) 0.0275(8) Uani 1 1 d . . H29 H 0.2726 -0.0798 0.2120 0.033 Uiso 1 1 calc R U C30 C 0.1984(3) -0.07129(19) 0.11299(18) 0.0416(10) Uani 1 1 d . . H30 H 0.2589 -0.0813 0.0922 0.050 Uiso 1 1 calc R U C31 C 0.1040(4) -0.05812(19) 0.07208(18) 0.0472(11) Uani 1 1 d . . H31 H 0.0991 -0.0585 0.0232 0.057 Uiso 1 1 calc R U C32 C 0.0163(3) -0.0443(2) 0.10229(18) 0.0467(11) Uani 1 1 d . . H32 H -0.0496 -0.0362 0.0742 0.056 Uiso 1 1 calc R U C33 C 0.0238(3) -0.04215(19) 0.17362(17) 0.0346(8) Uani 1 1 d . . H33 H -0.0368 -0.0317 0.1941 0.042 Uiso 1 1 calc R U C34 C 0.0626(2) -0.14120(15) 0.32435(15) 0.0173(7) Uani 1 1 d . . C35 C 0.0416(2) -0.15563(17) 0.39047(16) 0.0223(7) Uani 1 1 d . . H35 H 0.0507 -0.1181 0.4245 0.027 Uiso 1 1 calc R U C36 C 0.0076(3) -0.22461(18) 0.40704(19) 0.0326(9) Uani 1 1 d . . H36 H -0.0059 -0.2342 0.4525 0.039 Uiso 1 1 calc R U C37 C -0.0068(3) -0.27940(19) 0.3579(2) 0.0372(9) Uani 1 1 d . . H37 H -0.0297 -0.3266 0.3695 0.045 Uiso 1 1 calc R U C38 C 0.0123(3) -0.26501(17) 0.2915(2) 0.0342(9) Uani 1 1 d . . H38 H 0.0010 -0.3023 0.2573 0.041 Uiso 1 1 calc R U C39 C 0.0478(2) -0.19643(17) 0.27473(18) 0.0260(8) Uani 1 1 d . . H39 H 0.0620 -0.1872 0.2294 0.031 Uiso 1 1 calc R U C41 C -0.2567(3) 0.25383(18) 0.31684(19) 0.0329(8) Uani 1 1 d . . H41 H -0.2851 0.2824 0.2779 0.039 Uiso 1 1 calc R U C42 C -0.2804(3) 0.27084(18) 0.3814(2) 0.0355(9) Uani 1 1 d . . H42 H -0.3245 0.3114 0.3870 0.043 Uiso 1 1 calc R U C43 C -0.2398(3) 0.22861(18) 0.43787(19) 0.0332(8) Uani 1 1 d . . H43 H -0.2551 0.2407 0.4824 0.040 Uiso 1 1 calc R U C44 C -0.1768(2) 0.16863(17) 0.42940(17) 0.0254(7) Uani 1 1 d . . H44 H -0.1504 0.1393 0.4682 0.031 Uiso 1 1 calc R U C45 C -0.1516(2) 0.15089(15) 0.36466(15) 0.0175(6) Uani 1 1 d . . C46 C -0.0864(2) 0.08651(16) 0.35736(15) 0.0183(7) Uani 1 1 d . . C47 C -0.0834(2) 0.01714(16) 0.36627(15) 0.0182(7) Uani 1 1 d . . C48 C -0.1429(2) -0.04425(17) 0.38890(14) 0.0188(6) Uani 1 1 d . . C49 C -0.1441(2) -0.05636(18) 0.45944(16) 0.0257(7) Uani 1 1 d . . H49 H -0.1052 -0.0248 0.4926 0.031 Uiso 1 1 calc R U C50 C -0.2010(3) -0.1134(2) 0.48139(19) 0.0348(9) Uani 1 1 d . . H50 H -0.2011 -0.1207 0.5294 0.042 Uiso 1 1 calc R U C51 C -0.2574(3) -0.15991(19) 0.4344(2) 0.0372(9) Uani 1 1 d . . H51 H -0.2961 -0.1993 0.4499 0.045 Uiso 1 1 calc R U C52 C -0.2576(3) -0.14902(18) 0.3646(2) 0.0348(9) Uani 1 1 d . . H52 H -0.2973 -0.1807 0.3320 0.042 Uiso 1 1 calc R U C53 C -0.2000(2) -0.09196(16) 0.34184(17) 0.0239(7) Uani 1 1 d . . H53 H -0.1996 -0.0855 0.2938 0.029 Uiso 1 1 calc R U C55 C 0.7348(3) 0.1082(2) 0.1211(2) 0.0472(10) Uani 1 1 d . . H55 H 0.7524 0.1554 0.1397 0.057 Uiso 1 1 calc R U C56 C 0.7569(3) 0.0472(2) 0.1615(2) 0.0457(9) Uani 1 1 d . . H56 H 0.7882 0.0522 0.2084 0.055 Uiso 1 1 calc R U C57 C 0.7336(3) -0.0208(2) 0.1342(2) 0.0547(12) Uani 1 1 d . . H57 H 0.7505 -0.0629 0.1623 0.066 Uiso 1 1 calc R U C58 C 0.6862(3) -0.0296(3) 0.0671(2) 0.0571(13) Uani 1 1 d . . H58 H 0.6701 -0.0770 0.0486 0.068 Uiso 1 1 calc R U C59 C 0.6625(3) 0.0322(3) 0.0269(2) 0.0598(13) Uani 1 1 d . . H59 H 0.6287 0.0272 -0.0195 0.072 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 0.01350(18) 0.01383(18) 0.01701(19) 0.00158(17) 0.00317(14) 0.00061(18) P1 0.0138(4) 0.0137(4) 0.0164(4) 0.0016(3) 0.0033(3) 0.0013(3) P2 0.0133(4) 0.0138(4) 0.0154(4) -0.0002(3) 0.0015(3) 0.0002(3) O1 0.0160(9) 0.0117(9) 0.0180(10) 0.0011(9) 0.0010(8) 0.0009(9) C1 0.0173(16) 0.0155(15) 0.0153(16) 0.0004(12) 0.0054(13) -0.0026(12) C2 0.0166(16) 0.0160(15) 0.0143(16) 0.0030(12) 0.0031(12) -0.0016(12) C3 0.0201(17) 0.0169(16) 0.0271(19) 0.0005(13) 0.0054(14) 0.0017(13) C4 0.0248(18) 0.0159(16) 0.033(2) -0.0084(14) 0.0020(15) -0.0037(14) C40 0.0227(18) 0.0245(17) 0.0254(18) -0.0010(14) 0.0020(14) 0.0015(14) C54 0.052(3) 0.075(3) 0.043(3) 0.011(2) 0.010(2) 0.007(2) C5 0.0190(17) 0.0233(17) 0.0272(19) -0.0029(13) -0.0017(14) -0.0014(14) C6 0.0173(16) 0.0185(16) 0.0210(17) 0.0000(12) 0.0046(13) -0.0009(13) C7 0.0145(14) 0.0180(15) 0.0230(16) -0.0014(13) 0.0016(12) 0.0008(13) C8 0.0115(15) 0.0193(16) 0.0162(16) -0.0037(11) 0.0011(12) -0.0006(12) C9 0.0197(16) 0.0144(14) 0.0127(15) -0.0015(11) 0.0040(13) 0.0039(12) C10 0.0179(16) 0.0143(14) 0.0124(15) -0.0014(11) 0.0031(12) 0.0019(12) C11 0.0191(16) 0.0159(15) 0.0177(16) 0.0000(12) 0.0037(13) -0.0003(13) C12 0.0222(17) 0.0135(15) 0.0233(17) 0.0020(12) 0.0003(14) 0.0035(13) C13 0.0160(16) 0.0231(17) 0.0217(18) -0.0011(13) 0.0001(13) 0.0066(13) C14 0.0208(15) 0.0201(16) 0.0365(18) 0.0008(15) 0.0108(13) 0.0008(14) C15 0.0141(15) 0.0257(18) 0.0380(19) -0.0026(15) -0.0033(13) 0.0012(14) C16 0.0237(17) 0.0121(15) 0.0191(16) 0.0017(12) 0.0030(13) -0.0014(13) C17 0.0279(19) 0.0280(18) 0.0240(19) 0.0047(14) 0.0073(15) 0.0045(15) C18 0.041(2) 0.033(2) 0.029(2) 0.0057(15) 0.0175(17) 0.0008(17) C19 0.060(3) 0.0253(19) 0.0179(18) -0.0014(14) 0.0089(18) -0.0040(18) C20 0.043(2) 0.031(2) 0.026(2) 0.0009(15) -0.0058(17) -0.0118(17) C21 0.0284(19) 0.0303(19) 0.0245(19) 0.0010(15) 0.0021(15) -0.0096(15) C22 0.0098(14) 0.0159(15) 0.0237(17) 0.0002(12) 0.0034(12) -0.0024(12) C23 0.0247(18) 0.0221(17) 0.0258(18) 0.0044(13) 0.0107(14) 0.0033(14) C24 0.032(2) 0.0214(17) 0.038(2) 0.0111(15) 0.0111(16) 0.0045(15) C25 0.0276(19) 0.0191(18) 0.046(2) -0.0020(15) 0.0110(17) 0.0061(15) C26 0.0263(19) 0.0269(18) 0.0245(19) -0.0042(14) 0.0076(15) 0.0024(14) C27 0.0167(16) 0.0142(15) 0.0239(17) 0.0011(12) 0.0014(13) 0.0002(12) C28 0.0283(17) 0.0119(15) 0.0178(15) -0.0003(13) -0.0007(13) -0.0018(14) C29 0.035(2) 0.0280(18) 0.0201(17) -0.0027(13) 0.0073(15) -0.0083(15) C30 0.066(3) 0.036(2) 0.026(2) -0.0060(16) 0.019(2) -0.0184(19) C31 0.102(4) 0.023(2) 0.0132(18) 0.0002(15) -0.002(2) -0.010(2) C32 0.073(3) 0.029(2) 0.028(2) -0.0018(18) -0.024(2) 0.010(2) C33 0.043(2) 0.0267(18) 0.0293(19) -0.0038(16) -0.0088(16) 0.0110(18) C34 0.0154(16) 0.0129(14) 0.0226(17) 0.0012(12) -0.0005(13) 0.0018(12) C35 0.0177(17) 0.0261(18) 0.0231(18) 0.0044(13) 0.0028(14) 0.0046(14) C36 0.0248(19) 0.030(2) 0.045(2) 0.0189(17) 0.0137(17) 0.0062(15) C37 0.0235(19) 0.0191(18) 0.069(3) 0.0122(18) 0.0088(19) -0.0027(15) C38 0.030(2) 0.0178(17) 0.054(3) -0.0065(16) 0.0035(18) -0.0060(15) C39 0.0216(18) 0.0214(17) 0.034(2) -0.0011(14) 0.0009(15) -0.0028(14) C41 0.0270(19) 0.0291(19) 0.042(2) 0.0064(16) 0.0031(16) 0.0065(15) C42 0.026(2) 0.0240(18) 0.058(3) -0.0034(17) 0.0133(18) 0.0066(15) C43 0.032(2) 0.0293(19) 0.042(2) -0.0100(16) 0.0170(17) -0.0016(16) C44 0.0245(18) 0.0233(17) 0.0287(19) -0.0016(14) 0.0045(15) -0.0020(14) C45 0.0119(15) 0.0162(15) 0.0243(17) -0.0019(12) 0.0027(13) -0.0013(12) C46 0.0167(16) 0.0207(17) 0.0178(16) 0.0000(12) 0.0032(13) 0.0002(13) C47 0.0141(15) 0.0225(17) 0.0174(16) 0.0011(12) 0.0008(13) -0.0004(13) C48 0.0127(14) 0.0195(15) 0.0246(16) 0.0037(14) 0.0042(12) 0.0049(14) C49 0.0194(16) 0.0320(19) 0.0260(17) 0.0082(15) 0.0045(13) 0.0051(15) C50 0.030(2) 0.042(2) 0.035(2) 0.0224(17) 0.0147(17) 0.0132(17) C51 0.026(2) 0.029(2) 0.061(3) 0.0228(18) 0.0199(19) 0.0043(16) C52 0.0275(19) 0.0236(18) 0.054(3) 0.0002(16) 0.0086(17) -0.0054(15) C53 0.0232(17) 0.0216(17) 0.0277(19) 0.0033(14) 0.0067(14) 0.0005(14) C55 0.037(2) 0.056(3) 0.047(3) -0.003(2) 0.002(2) 0.015(2) C56 0.032(2) 0.057(2) 0.045(2) 0.000(2) -0.0061(17) 0.001(2) C57 0.050(3) 0.058(3) 0.052(3) 0.007(2) -0.003(2) -0.012(2) C58 0.056(3) 0.075(3) 0.043(3) -0.010(2) 0.016(2) -0.030(2) C59 0.056(3) 0.101(4) 0.025(2) 0.001(2) 0.0140(19) -0.022(3) 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 C47 Ni1 C46 39.36(12) C47 Ni1 P2 106.03(9) C46 Ni1 P2 144.36(9) C47 Ni1 P1 144.54(9) C46 Ni1 P1 105.17(9) P2 Ni1 P1 108.83(3) C16 P1 C22 101.55(13) C16 P1 C2 103.74(13) C22 P1 C2 98.29(13) C16 P1 Ni1 112.52(10) C22 P1 Ni1 116.03(9) C2 P1 Ni1 121.90(9) C28 P2 C34 101.47(13) C28 P2 C10 102.87(13) C34 P2 C10 98.21(13) C28 P2 Ni1 108.80(10) C34 P2 Ni1 118.44(9) C10 P2 Ni1 123.96(9) C9 O1 C1 113.15(19) C2 C1 O1 115.4(2) C2 C1 C6 125.2(3) O1 C1 C6 119.4(2) C1 C2 C3 116.6(3) C1 C2 P1 117.7(2) C3 C2 P1 125.4(2) C4 C3 C2 120.1(3) C4 C3 H3 119.9 C2 C3 H3 119.9 C5 C4 C3 121.1(3) C5 C4 H4 119.4 C3 C4 H4 119.4 C41 C40 C45 121.2(3) C41 C40 H40 119.4 C45 C40 H40 119.4 C55 C54 C59 119.3(4) C55 C54 H54 120.4 C59 C54 H54 120.4 C4 C5 C6 120.6(3) C4 C5 H5 119.7 C6 C5 H5 119.7 C1 C6 C5 116.3(3) C1 C6 C7 118.2(3) C5 C6 C7 125.5(3) C8 C7 C15 111.2(2) C8 C7 C6 106.7(2) C15 C7 C6 112.3(2) C8 C7 C14 110.0(2) C15 C7 C14 108.6(2) C6 C7 C14 108.0(2) C13 C8 C9 116.4(3) C13 C8 C7 125.8(3) C9 C8 C7 117.8(2) O1 C9 C10 115.5(2) O1 C9 C8 119.8(2) C10 C9 C8 124.7(3) C9 C10 C11 116.8(3) C9 C10 P2 117.6(2) C11 C10 P2 125.4(2) C12 C11 C10 120.1(3) C12 C11 H11 120.0 C10 C11 H11 120.0 C11 C12 C13 121.1(3) C11 C12 H12 119.5 C13 C12 H12 119.5 C8 C13 C12 120.8(3) C8 C13 H13 119.6 C12 C13 H13 119.6 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 C17 C16 C21 118.7(3) C17 C16 P1 124.0(2) C21 C16 P1 117.3(2) C16 C17 C18 120.3(3) C16 C17 H17 119.9 C18 C17 H17 119.9 C19 C18 C17 119.9(3) C19 C18 H18 120.0 C17 C18 H18 120.0 C20 C19 C18 120.1(3) C20 C19 H19 119.9 C18 C19 H19 119.9 C19 C20 C21 120.0(3) C19 C20 H20 120.0 C21 C20 H20 120.0 C20 C21 C16 120.9(3) C20 C21 H21 119.5 C16 C21 H21 119.5 C23 C22 C27 118.7(3) C23 C22 P1 122.8(2) C27 C22 P1 118.4(2) C24 C23 C22 120.7(3) C24 C23 H23 119.7 C22 C23 H23 119.7 C25 C24 C23 120.3(3) C25 C24 H24 119.8 C23 C24 H24 119.8 C24 C25 C26 119.8(3) C24 C25 H25 120.1 C26 C25 H25 120.1 C27 C26 C25 120.0(3) C27 C26 H26 120.0 C25 C26 H26 120.0 C26 C27 C22 120.6(3) C26 C27 H27 119.7 C22 C27 H27 119.7 C29 C28 C33 118.8(3) C29 C28 P2 124.0(2) C33 C28 P2 117.2(2) C30 C29 C28 120.2(3) C30 C29 H29 119.9 C28 C29 H29 119.9 C31 C30 C29 120.8(4) C31 C30 H30 119.6 C29 C30 H30 119.6 C30 C31 C32 119.5(3) C30 C31 H31 120.2 C32 C31 H31 120.2 C31 C32 C33 120.3(3) C31 C32 H32 119.9 C33 C32 H32 119.9 C32 C33 C28 120.3(3) C32 C33 H33 119.8 C28 C33 H33 119.8 C35 C34 C39 119.3(3) C35 C34 P2 117.9(2) C39 C34 P2 122.5(2) C36 C35 C34 120.3(3) C36 C35 H35 119.9 C34 C35 H35 119.9 C37 C36 C35 120.5(3) C37 C36 H36 119.8 C35 C36 H36 119.8 C36 C37 C38 119.6(3) C36 C37 H37 120.2 C38 C37 H37 120.2 C37 C38 C39 120.4(3) C37 C38 H38 119.8 C39 C38 H38 119.8 C38 C39 C34 120.0(3) C38 C39 H39 120.0 C34 C39 H39 120.0 C42 C41 C40 120.0(3) C42 C41 H41 120.0 C40 C41 H41 120.0 C41 C42 C43 119.9(3) C41 C42 H42 120.1 C43 C42 H42 120.1 C42 C43 C44 120.0(3) C42 C43 H43 120.0 C44 C43 H43 120.0 C43 C44 C45 120.9(3) C43 C44 H44 119.5 C45 C44 H44 119.5 C40 C45 C44 118.0(3) C40 C45 C46 122.5(3) C44 C45 C46 119.5(3) C47 C46 C45 141.9(3) C47 C46 Ni1 70.15(19) C45 C46 Ni1 147.9(2) C46 C47 C48 142.6(3) C46 C47 Ni1 70.5(2) C48 C47 Ni1 146.9(2) C53 C48 C49 118.0(3) C53 C48 C47 121.7(3) C49 C48 C47 120.3(3) C50 C49 C48 120.9(3) C50 C49 H49 119.6 C48 C49 H49 119.6 C51 C50 C49 120.6(3) C51 C50 H50 119.7 C49 C50 H50 119.7 C50 C51 C52 119.6(3) C50 C51 H51 120.2 C52 C51 H51 120.2 C51 C52 C53 120.3(3) C51 C52 H52 119.8 C53 C52 H52 119.8 C52 C53 C48 120.6(3) C52 C53 H53 119.7 C48 C53 H53 119.7 C56 C55 C54 120.3(4) C56 C55 H55 119.9 C54 C55 H55 119.9 C57 C56 C55 119.9(4) C57 C56 H56 120.1 C55 C56 H56 120.1 C56 C57 C58 121.2(4) C56 C57 H57 119.4 C58 C57 H57 119.4 C57 C58 C59 118.6(4) C57 C58 H58 120.7 C59 C58 H58 120.7 C54 C59 C58 120.7(4) C54 C59 H59 119.6 C58 C59 H59 119.6 loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance Ni1 C47 1.895(3) Ni1 C46 1.899(3) Ni1 P2 2.2054(8) Ni1 P1 2.2088(8) P1 C16 1.835(3) P1 C22 1.836(3) P1 C2 1.846(3) P2 C28 1.826(3) P2 C34 1.838(3) P2 C10 1.847(3) O1 C9 1.385(3) O1 C1 1.386(3) C1 C2 1.385(4) C1 C6 1.391(4) C2 C3 1.397(4) C3 C4 1.390(4) C3 H3 0.9500 C4 C5 1.387(4) C4 H4 0.9500 C40 C41 1.384(4) C40 C45 1.392(4) C40 H40 0.9500 C54 C55 1.376(5) C54 C59 1.382(6) C54 H54 0.9500 C5 C6 1.392(4) C5 H5 0.9500 C6 C7 1.531(4) C7 C8 1.527(4) C7 C15 1.527(4) C7 C14 1.549(4) C8 C13 1.389(4) C8 C9 1.396(4) C9 C10 1.388(4) C10 C11 1.399(4) C11 C12 1.388(4) C11 H11 0.9500 C12 C13 1.389(4) 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 C17 1.387(4) C16 C21 1.391(4) C17 C18 1.391(4) C17 H17 0.9500 C18 C19 1.385(5) C18 H18 0.9500 C19 C20 1.371(5) C19 H19 0.9500 C20 C21 1.381(4) C20 H20 0.9500 C21 H21 0.9500 C22 C23 1.390(4) C22 C27 1.397(4) C23 C24 1.383(4) C23 H23 0.9500 C24 C25 1.379(5) C24 H24 0.9500 C25 C26 1.391(4) C25 H25 0.9500 C26 C27 1.382(4) C26 H26 0.9500 C27 H27 0.9500 C28 C29 1.385(4) C28 C33 1.392(4) C29 C30 1.385(4) C29 H29 0.9500 C30 C31 1.371(5) C30 H30 0.9500 C31 C32 1.377(6) C31 H31 0.9500 C32 C33 1.387(5) C32 H32 0.9500 C33 H33 0.9500 C34 C35 1.389(4) C34 C39 1.393(4) C35 C36 1.388(4) C35 H35 0.9500 C36 C37 1.381(5) C36 H36 0.9500 C37 C38 1.385(5) C37 H37 0.9500 C38 C39 1.389(4) C38 H38 0.9500 C39 H39 0.9500 C41 C42 1.382(5) C41 H41 0.9500 C42 C43 1.383(5) C42 H42 0.9500 C43 C44 1.388(4) C43 H43 0.9500 C44 C45 1.395(4) C44 H44 0.9500 C45 C46 1.464(4) C46 C47 1.278(4) C47 C48 1.464(4) C48 C53 1.393(4) C48 C49 1.402(4) C49 C50 1.379(4) C49 H49 0.9500 C50 C51 1.375(5) C50 H50 0.9500 C51 C52 1.382(5) C51 H51 0.9500 C52 C53 1.391(4) C52 H52 0.9500 C53 H53 0.9500 C55 C56 1.371(5) C55 H55 0.9500 C56 C57 1.367(6) C56 H56 0.9500 C57 C58 1.372(5) C57 H57 0.9500 C58 C59 1.382(6) C58 H58 0.9500 C59 H59 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 C9 O1 C1 C2 -139.8(3) C9 O1 C1 C6 40.1(3) O1 C1 C2 C3 -177.9(2) C6 C1 C2 C3 2.3(4) O1 C1 C2 P1 6.9(3) C6 C1 C2 P1 -172.9(2) C16 P1 C2 C1 -78.1(2) C22 P1 C2 C1 177.8(2) Ni1 P1 C2 C1 50.0(3) C16 P1 C2 C3 107.2(3) C22 P1 C2 C3 3.1(3) Ni1 P1 C2 C3 -124.8(2) C1 C2 C3 C4 -2.0(4) P1 C2 C3 C4 172.7(2) C2 C3 C4 C5 0.3(5) C3 C4 C5 C6 1.5(5) C2 C1 C6 C5 -0.6(5) O1 C1 C6 C5 179.6(2) C2 C1 C6 C7 -179.4(3) O1 C1 C6 C7 0.8(4) C4 C5 C6 C1 -1.4(5) C4 C5 C6 C7 177.3(3) C1 C6 C7 C8 -36.7(3) C5 C6 C7 C8 144.7(3) C1 C6 C7 C15 -158.7(3) C5 C6 C7 C15 22.6(4) C1 C6 C7 C14 81.5(3) C5 C6 C7 C14 -97.2(3) C15 C7 C8 C13 -22.1(4) C6 C7 C8 C13 -144.9(3) C14 C7 C8 C13 98.3(3) C15 C7 C8 C9 157.8(3) C6 C7 C8 C9 35.0(3) C14 C7 C8 C9 -81.8(3) C1 O1 C9 C10 137.8(3) C1 O1 C9 C8 -41.8(3) C13 C8 C9 O1 -177.9(2) C7 C8 C9 O1 2.2(4) C13 C8 C9 C10 2.6(4) C7 C8 C9 C10 -177.3(3) O1 C9 C10 C11 176.8(2) C8 C9 C10 C11 -3.6(4) O1 C9 C10 P2 -7.2(3) C8 C9 C10 P2 172.3(2) C28 P2 C10 C9 76.5(2) C34 P2 C10 C9 -179.6(2) Ni1 P2 C10 C9 -47.0(3) C28 P2 C10 C11 -107.9(3) C34 P2 C10 C11 -4.1(3) Ni1 P2 C10 C11 128.5(2) C9 C10 C11 C12 1.5(4) P2 C10 C11 C12 -174.0(2) C10 C11 C12 C13 1.4(4) C9 C8 C13 C12 0.6(4) C7 C8 C13 C12 -179.6(3) C11 C12 C13 C8 -2.5(5) C22 P1 C16 C17 109.7(3) C2 P1 C16 C17 8.1(3) Ni1 P1 C16 C17 -125.6(2) C22 P1 C16 C21 -70.6(3) C2 P1 C16 C21 -172.2(2) Ni1 P1 C16 C21 54.1(3) C21 C16 C17 C18 -0.3(5) P1 C16 C17 C18 179.4(2) C16 C17 C18 C19 1.3(5) C17 C18 C19 C20 -0.6(5) C18 C19 C20 C21 -1.1(5) C19 C20 C21 C16 2.2(5) C17 C16 C21 C20 -1.4(5) P1 C16 C21 C20 178.8(2) C16 P1 C22 C23 -11.5(3) C2 P1 C22 C23 94.5(3) Ni1 P1 C22 C23 -133.8(2) C16 P1 C22 C27 172.5(2) C2 P1 C22 C27 -81.6(2) Ni1 P1 C22 C27 50.2(3) C27 C22 C23 C24 -0.2(5) P1 C22 C23 C24 -176.2(2) C22 C23 C24 C25 0.7(5) C23 C24 C25 C26 -0.5(5) C24 C25 C26 C27 -0.3(5) C25 C26 C27 C22 0.7(5) C23 C22 C27 C26 -0.5(4) P1 C22 C27 C26 175.7(2) C34 P2 C28 C29 -102.2(3) C10 P2 C28 C29 -0.9(3) Ni1 P2 C28 C29 132.2(2) C34 P2 C28 C33 77.2(3) C10 P2 C28 C33 178.5(2) Ni1 P2 C28 C33 -48.4(3) C33 C28 C29 C30 0.7(5) P2 C28 C29 C30 -179.9(2) C28 C29 C30 C31 -0.5(5) C29 C30 C31 C32 -0.5(5) C30 C31 C32 C33 1.3(6) C31 C32 C33 C28 -1.1(5) C29 C28 C33 C32 0.1(5) P2 C28 C33 C32 -179.4(3) C28 P2 C34 C35 -173.9(2) C10 P2 C34 C35 81.1(2) Ni1 P2 C34 C35 -55.0(3) C28 P2 C34 C39 12.4(3) C10 P2 C34 C39 -92.6(3) Ni1 P2 C34 C39 131.3(2) C39 C34 C35 C36 0.8(4) P2 C34 C35 C36 -173.2(2) C34 C35 C36 C37 -0.6(5) C35 C36 C37 C38 -0.4(5) C36 C37 C38 C39 1.3(5) C37 C38 C39 C34 -1.2(5) C35 C34 C39 C38 0.1(5) P2 C34 C39 C38 173.8(2) C45 C40 C41 C42 2.0(5) C40 C41 C42 C43 -0.6(5) C41 C42 C43 C44 -1.0(5) C42 C43 C44 C45 1.3(5) C41 C40 C45 C44 -1.6(5) C41 C40 C45 C46 177.3(3) C43 C44 C45 C40 0.0(4) C43 C44 C45 C46 -179.0(3) C40 C45 C46 C47 -119.8(5) C44 C45 C46 C47 59.1(6) C40 C45 C46 Ni1 63.9(5) C44 C45 C46 Ni1 -117.2(4) P2 Ni1 C46 C47 17.6(3) P1 Ni1 C46 C47 179.83(17) C47 Ni1 C46 C45 177.6(6) P2 Ni1 C46 C45 -164.8(3) P1 Ni1 C46 C45 -2.6(4) C45 C46 C47 C48 0.7(8) Ni1 C46 C47 C48 178.7(5) C45 C46 C47 Ni1 -177.9(5) P2 Ni1 C47 C46 -169.44(17) P1 Ni1 C47 C46 -0.3(3) C46 Ni1 C47 C48 -178.5(5) P2 Ni1 C47 C48 12.0(4) P1 Ni1 C47 C48 -178.8(3) C46 C47 C48 C53 102.3(5) Ni1 C47 C48 C53 -80.0(5) C46 C47 C48 C49 -77.4(6) Ni1 C47 C48 C49 100.4(4) C53 C48 C49 C50 -0.6(4) C47 C48 C49 C50 179.1(3) C48 C49 C50 C51 0.3(5) C49 C50 C51 C52 -0.4(5) C50 C51 C52 C53 0.8(5) C51 C52 C53 C48 -1.2(5) C49 C48 C53 C52 1.0(4) C47 C48 C53 C52 -178.7(3) C59 C54 C55 C56 -0.1(6) C54 C55 C56 C57 1.3(6) C55 C56 C57 C58 -1.4(6) C56 C57 C58 C59 0.2(6) C55 C54 C59 C58 -1.0(6) C57 C58 C59 C54 1.0(6)