#------------------------------------------------------------------------------ #$Date: 2019-06-04 06:40:31 +0300 (Tue, 04 Jun 2019) $ #$Revision: 215684 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/55/12/1551200.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_1551200 loop_ _publ_author_name 'Tran, Thi V.' 'Nguyen, Yennie H.' 'Do, Loi' _publ_section_title ; Development of Highly Productive Nickel-Sodium Phenoxyphosphine Ethylene Polymerization Catalysts and Their Reaction Temperature Profiles ; _journal_name_full 'Polymer Chemistry' _journal_paper_doi 10.1039/C9PY00610A _journal_year 2019 _chemical_formula_sum 'C39 H54 Ni O3 P2' _chemical_formula_weight 691.47 _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-2018/3 _audit_update_record ; 2019-04-25 deposited with the CCDC. 2019-06-03 downloaded from the CCDC. ; _cell_angle_alpha 72.2620(10) _cell_angle_beta 71.2670(10) _cell_angle_gamma 81.6330(10) _cell_formula_units_Z 2 _cell_length_a 11.0922(13) _cell_length_b 11.6999(14) _cell_length_c 15.9470(19) _cell_measurement_reflns_used 9419 _cell_measurement_temperature 123(2) _cell_measurement_theta_max 27.47 _cell_measurement_theta_min 2.39 _cell_volume 1864.1(4) _computing_cell_refinement 'Bruker SAINT' _computing_data_collection 'Bruker APEX2' _computing_data_reduction 'Bruker SAINT' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _computing_structure_refinement 'SHELXL-2018/3 (Sheldrick, 2018)' _computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2018)' _diffrn_ambient_temperature 123(2) _diffrn_measured_fraction_theta_full 0.973 _diffrn_measured_fraction_theta_max 0.973 _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0106 _diffrn_reflns_av_unetI/netI 0.0214 _diffrn_reflns_Laue_measured_fraction_full 0.973 _diffrn_reflns_Laue_measured_fraction_max 0.973 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_number 9114 _diffrn_reflns_point_group_measured_fraction_full 0.973 _diffrn_reflns_point_group_measured_fraction_max 0.973 _diffrn_reflns_theta_full 25.027 _diffrn_reflns_theta_max 25.027 _diffrn_reflns_theta_min 1.403 _exptl_absorpt_coefficient_mu 0.640 _exptl_absorpt_correction_T_max 0.7456 _exptl_absorpt_correction_T_min 0.6891 _exptl_absorpt_correction_type empirical _exptl_absorpt_process_details sadabs _exptl_crystal_colour yellow _exptl_crystal_density_diffrn 1.232 _exptl_crystal_description Block _exptl_crystal_F_000 740 _exptl_crystal_size_max 0.300 _exptl_crystal_size_mid 0.200 _exptl_crystal_size_min 0.150 _refine_diff_density_max 1.339 _refine_diff_density_min -0.821 _refine_diff_density_rms 0.173 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.085 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 418 _refine_ls_number_reflns 6404 _refine_ls_number_restraints 30 _refine_ls_restrained_S_all 1.096 _refine_ls_R_factor_all 0.0556 _refine_ls_R_factor_gt 0.0466 _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^)+(0.1539P)^2^+2.0173P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1590 _refine_ls_wR_factor_ref 0.2051 _reflns_Friedel_coverage 0.000 _reflns_number_gt 6126 _reflns_number_total 6404 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file c9py00610a2.cif _cod_data_source_block Ni10 _cod_database_code 1551200 _shelx_shelxl_version_number 2018/3 _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; _shelx_estimated_absorpt_t_min 0.831 _shelx_estimated_absorpt_t_max 0.910 _shelx_res_file ; TITL 2_a.res in P-1 2_a.res created by SHELXL-2018/3 at 13:13:48 on 16-May-2018 REM Old TITL 2 in P-1 REM SHELXT solution in P-1: R1 0.120, Rweak 0.004, Alpha 0.038 REM 0.000 for 0 systematic absences, Orientation as input REM Formula found by SHELXT: C39 O3 P2 Ni CELL 0.71073 11.0922 11.6999 15.9470 72.262 71.267 81.633 ZERR 2.000 0.0013 0.0014 0.0019 0.001 0.001 0.001 LATT 1 SFAC C H O P NI UNIT 78 108 6 4 2 TEMP -150 SIZE 0.15 0.20 0.30 L.S. 30 BOND LIST 6 FMAP 2 PLAN 15 acta SHEL 999 0.84 WGHT 0.153900 2.017300 FVAR 0.56023 0.52881 NI1 5 0.740220 0.480326 0.340793 11.00000 0.02050 0.01144 = 0.01224 -0.00220 -0.00895 0.00124 P1 4 0.708664 0.405464 0.240052 11.00000 0.01690 0.01033 = 0.01087 -0.00182 -0.00476 -0.00162 P2 4 0.759758 0.567810 0.438521 11.00000 0.04086 0.02141 = 0.02347 -0.01115 -0.02361 0.01076 O1 3 0.682008 0.632253 0.274170 11.00000 0.03436 0.01368 = 0.01563 -0.00424 -0.01573 0.00264 O2 3 0.966536 0.476964 0.157338 11.00000 0.02518 0.02484 = 0.02041 -0.00060 -0.00466 -0.01240 O3 3 0.713364 0.150914 0.336529 11.00000 0.02254 0.01422 = 0.02078 0.00059 -0.00621 -0.00151 C1 1 0.656370 0.643744 0.196025 11.00000 0.01592 0.01781 = 0.01261 -0.00299 -0.00584 -0.00161 C2 1 0.659727 0.541906 0.165970 11.00000 0.01679 0.01176 = 0.01310 -0.00102 -0.00599 -0.00226 C3 1 0.633123 0.549930 0.084125 11.00000 0.01779 0.01456 = 0.01601 -0.00556 -0.00465 -0.00378 AFIX 43 H3 2 0.635929 0.479143 0.066031 11.00000 -1.20000 AFIX 0 C4 1 0.603002 0.659499 0.029852 11.00000 0.01769 0.02298 = 0.01324 -0.00315 -0.00674 -0.00422 C5 1 0.600786 0.761707 0.059019 11.00000 0.01797 0.01574 = 0.01420 0.00052 -0.00739 -0.00038 AFIX 43 H5 2 0.580726 0.837722 0.021472 11.00000 -1.20000 AFIX 0 C6 1 0.626262 0.758163 0.139733 11.00000 0.01548 0.01560 = 0.01453 -0.00312 -0.00536 -0.00068 C7 1 0.574499 0.672060 -0.059127 11.00000 0.04186 0.02127 = 0.01853 -0.00146 -0.01817 -0.00370 AFIX 137 H7A 2 0.630686 0.729814 -0.109488 11.00000 -1.50000 H7B 2 0.485440 0.700680 -0.053310 11.00000 -1.50000 H7C 2 0.588883 0.593832 -0.072300 11.00000 -1.50000 AFIX 0 C8 1 0.619247 0.872481 0.168976 11.00000 0.03111 0.01280 = 0.01977 -0.00230 -0.01434 0.00340 C9 1 0.512984 0.862152 0.259976 11.00000 0.04181 0.02279 = 0.02273 -0.01037 -0.01123 0.00748 AFIX 137 H9A 2 0.508536 0.933984 0.280464 11.00000 -1.50000 H9B 2 0.531087 0.790833 0.306707 11.00000 -1.50000 H9C 2 0.431335 0.855030 0.250983 11.00000 -1.50000 AFIX 0 C10 1 0.587698 0.986006 0.098886 11.00000 0.05057 0.01379 = 0.03048 -0.00303 -0.02362 0.00425 AFIX 137 H10A 2 0.655288 0.996393 0.040145 11.00000 -1.50000 H10B 2 0.581294 1.056002 0.121928 11.00000 -1.50000 H10C 2 0.506331 0.978240 0.089753 11.00000 -1.50000 AFIX 0 C11 1 0.748296 0.889458 0.179780 11.00000 0.04144 0.01823 = 0.03445 -0.00660 -0.02208 -0.00350 AFIX 137 H11A 2 0.813175 0.903935 0.119601 11.00000 -1.50000 H11B 2 0.773605 0.816873 0.222214 11.00000 -1.50000 H11C 2 0.740081 0.958351 0.204389 11.00000 -1.50000 AFIX 0 C12 1 0.576433 0.306337 0.282287 11.00000 0.02012 0.01590 = 0.00799 -0.00353 -0.00149 -0.00319 C13 1 0.593549 0.186062 0.331654 11.00000 0.02172 0.01675 = 0.01102 -0.00601 -0.00355 -0.00316 C14 1 0.491691 0.110483 0.369738 11.00000 0.02907 0.01265 = 0.01295 -0.00214 -0.00218 -0.00469 AFIX 43 H14 2 0.503091 0.029528 0.403647 11.00000 -1.20000 AFIX 0 C15 1 0.373259 0.154981 0.357509 11.00000 0.02198 0.02590 = 0.01878 -0.00676 -0.00130 -0.01149 AFIX 43 H15 2 0.303938 0.103651 0.382472 11.00000 -1.20000 AFIX 0 C16 1 0.355588 0.273520 0.309231 11.00000 0.01931 0.02830 = 0.01928 -0.00709 -0.00497 -0.00331 AFIX 43 H16 2 0.274137 0.303358 0.301950 11.00000 -1.20000 AFIX 0 C17 1 0.456445 0.348347 0.271670 11.00000 0.02346 0.01760 = 0.01143 -0.00348 -0.00426 -0.00079 AFIX 43 H17 2 0.443866 0.429309 0.238245 11.00000 -1.20000 AFIX 0 C18 1 0.738483 0.031972 0.388032 11.00000 0.03121 0.01551 = 0.02338 -0.00103 -0.00981 0.00053 AFIX 137 H18A 2 0.722562 -0.025780 0.359853 11.00000 -1.50000 H18B 2 0.682519 0.017719 0.451464 11.00000 -1.50000 H18C 2 0.827661 0.022095 0.388235 11.00000 -1.50000 AFIX 0 C19 1 0.832866 0.337396 0.160245 11.00000 0.01930 0.01289 = 0.01260 -0.00020 -0.00322 -0.00079 C20 1 0.953698 0.385488 0.124974 11.00000 0.02214 0.01858 = 0.01566 0.00035 -0.00560 -0.00285 C21 1 1.050650 0.340872 0.060434 11.00000 0.02033 0.03274 = 0.02114 -0.00140 0.00156 -0.00322 AFIX 43 H21 2 1.132463 0.373247 0.036887 11.00000 -1.20000 AFIX 0 C22 1 1.026999 0.249233 0.030914 11.00000 0.03304 0.03257 = 0.02313 -0.01028 0.00582 0.00285 AFIX 43 H22 2 1.093392 0.218660 -0.012839 11.00000 -1.20000 AFIX 0 C23 1 0.908011 0.201014 0.064010 11.00000 0.03992 0.02120 = 0.02265 -0.00974 -0.00095 -0.00179 AFIX 43 H23 2 0.892503 0.138343 0.043021 11.00000 -1.20000 AFIX 0 C24 1 0.811928 0.246109 0.128444 11.00000 0.02486 0.01789 = 0.01651 -0.00469 -0.00145 -0.00413 AFIX 43 H24 2 0.730145 0.213773 0.151226 11.00000 -1.20000 AFIX 0 C25 1 1.089906 0.523003 0.128969 11.00000 0.03132 0.04115 = 0.03762 -0.00175 -0.00914 -0.02094 AFIX 137 H25A 2 1.113271 0.564044 0.062899 11.00000 -1.50000 H25B 2 1.152434 0.456600 0.141197 11.00000 -1.50000 H25C 2 1.088747 0.579986 0.163326 11.00000 -1.50000 AFIX 0 C26 1 0.806781 0.336293 0.408519 11.00000 0.02071 0.01258 = 0.01426 -0.00351 -0.00781 0.00151 C27 1 0.937943 0.306244 0.382158 11.00000 0.02091 0.02553 = 0.01939 0.00339 -0.00408 0.00186 AFIX 43 H27 2 0.991394 0.353474 0.326538 11.00000 -1.20000 AFIX 0 C28 1 0.991223 0.207352 0.436858 11.00000 0.02479 0.04006 = 0.03157 -0.00300 -0.00825 0.01536 AFIX 43 H28 2 1.080299 0.188385 0.417669 11.00000 -1.20000 AFIX 0 C29 1 0.916459 0.137377 0.517891 11.00000 0.04133 0.02418 = 0.02515 -0.00470 -0.01719 0.01364 AFIX 43 H29 2 0.953323 0.071482 0.555322 11.00000 -1.20000 AFIX 0 C30 1 0.786815 0.164765 0.543770 11.00000 0.03732 0.01810 = 0.01455 -0.00047 -0.00629 -0.00278 AFIX 43 H30 2 0.733742 0.116758 0.599178 11.00000 -1.20000 AFIX 0 C31 1 0.733163 0.262406 0.489166 11.00000 0.02142 0.02395 = 0.01851 -0.00522 -0.00365 -0.00039 AFIX 43 H31 2 0.643548 0.278738 0.507799 11.00000 -1.20000 AFIX 0 SADI P2 C32 P2 C33 P2 C34 P2 C32a P2 C33a P2 C34a SADI C32 C33 C33 C34 c34 C32 C32a C33a C33a C34a C34a C32a EADP C32 C33 C34 C32a C33a C34a PART 1 C32 1 0.656827 0.698389 0.457460 21.00000 0.09295 0.03128 = 0.05952 -0.01930 -0.05409 0.01561 AFIX 137 H32A 2 0.644373 0.702974 0.520059 21.00000 -1.50000 H32B 2 0.574192 0.691758 0.449734 21.00000 -1.50000 H32C 2 0.696224 0.771083 0.412833 21.00000 -1.50000 AFIX 0 C33 1 0.916873 0.635585 0.382357 21.00000 0.09295 0.03128 = 0.05952 -0.01930 -0.05409 0.01561 AFIX 137 H33A 2 0.984649 0.571705 0.380354 21.00000 -1.50000 H33B 2 0.928040 0.686824 0.417527 21.00000 -1.50000 H33C 2 0.921006 0.684064 0.319492 21.00000 -1.50000 AFIX 0 C34 1 0.771219 0.486885 0.551146 21.00000 0.09295 0.03128 = 0.05952 -0.01930 -0.05409 0.01561 AFIX 137 H34A 2 0.836848 0.421403 0.546346 21.00000 -1.50000 H34B 2 0.688960 0.453518 0.589758 21.00000 -1.50000 H34C 2 0.794113 0.541496 0.578902 21.00000 -1.50000 AFIX 0 part 2 C32A 1 0.624102 0.663444 0.475137 -21.00000 0.09295 0.03128 = 0.05952 -0.01930 -0.05409 0.01561 AFIX 137 H32D 2 0.599315 0.714648 0.421359 -21.00000 -1.50000 H32E 2 0.645575 0.713904 0.506814 -21.00000 -1.50000 H32F 2 0.553108 0.614165 0.517293 -21.00000 -1.50000 AFIX 0 C33A 1 0.888838 0.677161 0.383136 -21.00000 0.09295 0.03128 = 0.05952 -0.01930 -0.05409 0.01561 AFIX 137 H33D 2 0.962268 0.644663 0.406204 -21.00000 -1.50000 H33E 2 0.857165 0.753454 0.397988 -21.00000 -1.50000 H33F 2 0.914704 0.690653 0.316201 -21.00000 -1.50000 AFIX 0 C34A 1 0.807814 0.491391 0.540516 -21.00000 0.09295 0.03128 = 0.05952 -0.01930 -0.05409 0.01561 AFIX 137 H34D 2 0.754396 0.423073 0.576760 -21.00000 -1.50000 H34E 2 0.797845 0.547200 0.577592 -21.00000 -1.50000 H34F 2 0.897280 0.462428 0.522545 -21.00000 -1.50000 AFIX 0 PART 0 C35 1 0.745125 0.291059 0.774279 11.00000 0.07676 0.07277 = 0.05867 0.00356 -0.03074 -0.02723 AFIX 137 H35A 2 0.821126 0.338203 0.750016 11.00000 -1.50000 H35B 2 0.669073 0.343322 0.790828 11.00000 -1.50000 H35C 2 0.738939 0.256280 0.727231 11.00000 -1.50000 AFIX 0 C36 1 0.754706 0.191774 0.858402 11.00000 0.04736 0.06649 = 0.03381 -0.01356 -0.01513 -0.00183 AFIX 23 H36A 2 0.686805 0.135826 0.874241 11.00000 -1.20000 H36B 2 0.736833 0.227544 0.910272 11.00000 -1.20000 AFIX 0 C37 1 0.880716 0.119129 0.851299 11.00000 0.04481 0.06950 = 0.03964 -0.01062 -0.01301 -0.00588 AFIX 23 H37A 2 0.947670 0.173851 0.840493 11.00000 -1.20000 H37B 2 0.874637 0.058903 0.911385 11.00000 -1.20000 AFIX 0 C38 1 0.923191 0.054492 0.777386 11.00000 0.04296 0.06475 = 0.04770 -0.01091 -0.01301 -0.00099 AFIX 23 H38A 2 1.008833 0.015546 0.776609 11.00000 -1.20000 H38B 2 0.931147 0.114464 0.716960 11.00000 -1.20000 AFIX 0 C39 1 0.833970 -0.040949 0.788831 11.00000 0.06303 0.05513 = 0.06197 -0.00203 -0.03074 0.00076 AFIX 137 H39A 2 0.757935 -0.001599 0.771380 11.00000 -1.50000 H39B 2 0.808687 -0.089285 0.853230 11.00000 -1.50000 H39C 2 0.878140 -0.093092 0.749215 11.00000 -1.50000 AFIX 0 HKLF 4 REM 2_a.res in P-1 REM wR2 = 0.2051, GooF = S = 1.085, Restrained GooF = 1.096 for all data REM R1 = 0.0466 for 6126 Fo > 4sig(Fo) and 0.0556 for all 6404 data REM 418 parameters refined using 30 restraints END WGHT 0.1545 1.9823 REM Highest difference peak 1.339, deepest hole -0.821, 1-sigma level 0.173 Q1 1 0.5905 0.5343 0.5294 11.00000 0.05 1.34 Q2 1 0.7604 0.7184 0.4140 11.00000 0.05 1.00 Q3 1 0.8670 0.5149 0.4975 11.00000 0.05 0.85 Q4 1 0.8119 0.1237 0.7924 11.00000 0.05 0.79 Q5 1 0.7054 0.3565 0.8118 11.00000 0.05 0.76 Q6 1 0.7774 0.5603 0.4535 11.00000 0.05 0.76 Q7 1 0.9034 0.5407 0.2396 11.00000 0.05 0.62 Q8 1 0.8753 0.3257 0.4012 11.00000 0.05 0.61 Q9 1 0.7413 0.6848 0.2694 11.00000 0.05 0.58 Q10 1 0.6809 -0.0576 0.3667 11.00000 0.05 0.58 Q11 1 0.7174 0.5398 0.4618 11.00000 0.05 0.56 Q12 1 1.0723 0.2392 0.4431 11.00000 0.05 0.55 Q13 1 0.6816 0.4180 0.3797 11.00000 0.05 0.54 Q14 1 0.9464 0.5586 0.4026 11.00000 0.05 0.53 Q15 1 0.6559 0.3427 0.2686 11.00000 0.05 0.52 ; _shelx_res_checksum 90143 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, -z' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Ni1 Ni 0.74022(3) 0.48033(3) 0.34079(2) 0.01417(19) Uani 1 1 d . . . . . P1 P 0.70866(7) 0.40546(6) 0.24005(5) 0.0127(2) Uani 1 1 d . . . . . P2 P 0.75976(9) 0.56781(7) 0.43852(6) 0.0252(2) Uani 1 1 d D . . . . O1 O 0.6820(2) 0.63225(18) 0.27417(14) 0.0195(5) Uani 1 1 d . . . . . O2 O 0.9665(2) 0.47696(19) 0.15734(14) 0.0241(5) Uani 1 1 d . . . . . O3 O 0.71336(19) 0.15091(18) 0.33653(14) 0.0204(5) Uani 1 1 d . . . . . C1 C 0.6564(3) 0.6437(3) 0.19603(19) 0.0152(6) Uani 1 1 d . . . . . C2 C 0.6597(3) 0.5419(2) 0.16597(19) 0.0139(6) Uani 1 1 d . . . . . C3 C 0.6331(3) 0.5499(2) 0.08412(19) 0.0156(6) Uani 1 1 d . . . . . H3 H 0.635929 0.479143 0.066031 0.019 Uiso 1 1 calc R U . . . C4 C 0.6030(3) 0.6595(3) 0.02985(19) 0.0175(6) Uani 1 1 d . . . . . C5 C 0.6008(3) 0.7617(3) 0.05902(19) 0.0165(6) Uani 1 1 d . . . . . H5 H 0.580726 0.837722 0.021472 0.020 Uiso 1 1 calc R U . . . C6 C 0.6263(3) 0.7582(3) 0.13973(19) 0.0152(6) Uani 1 1 d . . . . . C7 C 0.5745(3) 0.6721(3) -0.0591(2) 0.0256(7) Uani 1 1 d . . . . . H7A H 0.630686 0.729814 -0.109488 0.038 Uiso 1 1 calc R U . . . H7B H 0.485440 0.700680 -0.053310 0.038 Uiso 1 1 calc R U . . . H7C H 0.588883 0.593832 -0.072300 0.038 Uiso 1 1 calc R U . . . C8 C 0.6192(3) 0.8725(3) 0.1690(2) 0.0205(6) Uani 1 1 d . . . . . C9 C 0.5130(3) 0.8622(3) 0.2600(2) 0.0287(7) Uani 1 1 d . . . . . H9A H 0.508536 0.933984 0.280464 0.043 Uiso 1 1 calc R U . . . H9B H 0.531087 0.790833 0.306707 0.043 Uiso 1 1 calc R U . . . H9C H 0.431335 0.855030 0.250983 0.043 Uiso 1 1 calc R U . . . C10 C 0.5877(4) 0.9860(3) 0.0989(2) 0.0301(7) Uani 1 1 d . . . . . H10A H 0.655288 0.996393 0.040145 0.045 Uiso 1 1 calc R U . . . H10B H 0.581294 1.056002 0.121928 0.045 Uiso 1 1 calc R U . . . H10C H 0.506331 0.978240 0.089753 0.045 Uiso 1 1 calc R U . . . C11 C 0.7483(3) 0.8895(3) 0.1798(2) 0.0286(7) Uani 1 1 d . . . . . H11A H 0.813175 0.903935 0.119601 0.043 Uiso 1 1 calc R U . . . H11B H 0.773605 0.816873 0.222214 0.043 Uiso 1 1 calc R U . . . H11C H 0.740081 0.958351 0.204389 0.043 Uiso 1 1 calc R U . . . C12 C 0.5764(3) 0.3063(2) 0.28229(18) 0.0150(6) Uani 1 1 d . . . . . C13 C 0.5935(3) 0.1861(2) 0.33165(18) 0.0161(6) Uani 1 1 d . . . . . C14 C 0.4917(3) 0.1105(2) 0.36974(19) 0.0192(6) Uani 1 1 d . . . . . H14 H 0.503091 0.029528 0.403647 0.023 Uiso 1 1 calc R U . . . C15 C 0.3733(3) 0.1550(3) 0.3575(2) 0.0221(6) Uani 1 1 d . . . . . H15 H 0.303938 0.103651 0.382472 0.027 Uiso 1 1 calc R U . . . C16 C 0.3556(3) 0.2735(3) 0.3092(2) 0.0221(6) Uani 1 1 d . . . . . H16 H 0.274137 0.303358 0.301950 0.027 Uiso 1 1 calc R U . . . C17 C 0.4564(3) 0.3483(3) 0.27167(18) 0.0179(6) Uani 1 1 d . . . . . H17 H 0.443866 0.429309 0.238245 0.021 Uiso 1 1 calc R U . . . C18 C 0.7385(3) 0.0320(3) 0.3880(2) 0.0241(7) Uani 1 1 d . . . . . H18A H 0.722562 -0.025780 0.359853 0.036 Uiso 1 1 calc R U . . . H18B H 0.682519 0.017719 0.451464 0.036 Uiso 1 1 calc R U . . . H18C H 0.827661 0.022095 0.388235 0.036 Uiso 1 1 calc R U . . . C19 C 0.8329(3) 0.3374(2) 0.16025(18) 0.0161(6) Uani 1 1 d . . . . . C20 C 0.9537(3) 0.3855(3) 0.12497(19) 0.0198(6) Uani 1 1 d . . . . . C21 C 1.0506(3) 0.3409(3) 0.0604(2) 0.0279(7) Uani 1 1 d . . . . . H21 H 1.132463 0.373247 0.036887 0.033 Uiso 1 1 calc R U . . . C22 C 1.0270(3) 0.2492(3) 0.0309(2) 0.0330(8) Uani 1 1 d . . . . . H22 H 1.093392 0.218660 -0.012839 0.040 Uiso 1 1 calc R U . . . C23 C 0.9080(3) 0.2010(3) 0.0640(2) 0.0291(7) Uani 1 1 d . . . . . H23 H 0.892503 0.138343 0.043021 0.035 Uiso 1 1 calc R U . . . C24 C 0.8119(3) 0.2461(3) 0.1284(2) 0.0206(6) Uani 1 1 d . . . . . H24 H 0.730145 0.213773 0.151226 0.025 Uiso 1 1 calc R U . . . C25 C 1.0899(3) 0.5230(4) 0.1290(3) 0.0370(8) Uani 1 1 d . . . . . H25A H 1.113271 0.564044 0.062899 0.056 Uiso 1 1 calc R U . . . H25B H 1.152434 0.456600 0.141197 0.056 Uiso 1 1 calc R U . . . H25C H 1.088747 0.579986 0.163326 0.056 Uiso 1 1 calc R U . . . C26 C 0.8068(3) 0.3363(2) 0.40852(19) 0.0155(6) Uani 1 1 d . . . . . C27 C 0.9379(3) 0.3062(3) 0.3822(2) 0.0250(7) Uani 1 1 d . . . . . H27 H 0.991394 0.353474 0.326538 0.030 Uiso 1 1 calc R U . . . C28 C 0.9912(3) 0.2074(3) 0.4369(2) 0.0356(8) Uani 1 1 d . . . . . H28 H 1.080299 0.188385 0.417669 0.043 Uiso 1 1 calc R U . . . C29 C 0.9165(3) 0.1374(3) 0.5179(2) 0.0305(7) Uani 1 1 d . . . . . H29 H 0.953323 0.071482 0.555322 0.037 Uiso 1 1 calc R U . . . C30 C 0.7868(3) 0.1648(3) 0.5438(2) 0.0245(7) Uani 1 1 d . . . . . H30 H 0.733742 0.116758 0.599178 0.029 Uiso 1 1 calc R U . . . C31 C 0.7332(3) 0.2624(3) 0.4892(2) 0.0221(6) Uani 1 1 d . . . . . H31 H 0.643548 0.278738 0.507799 0.026 Uiso 1 1 calc R U . . . C32 C 0.6568(11) 0.6984(9) 0.4575(8) 0.0538(12) Uani 0.529(15) 1 d D . P A 1 H32A H 0.644373 0.702974 0.520059 0.081 Uiso 0.529(15) 1 calc R U P A 1 H32B H 0.574192 0.691758 0.449734 0.081 Uiso 0.529(15) 1 calc R U P A 1 H32C H 0.696224 0.771083 0.412833 0.081 Uiso 0.529(15) 1 calc R U P A 1 C33 C 0.9169(9) 0.6356(11) 0.3824(6) 0.0538(12) Uani 0.529(15) 1 d D . P A 1 H33A H 0.984649 0.571705 0.380354 0.081 Uiso 0.529(15) 1 calc R U P A 1 H33B H 0.928040 0.686824 0.417527 0.081 Uiso 0.529(15) 1 calc R U P A 1 H33C H 0.921006 0.684064 0.319492 0.081 Uiso 0.529(15) 1 calc R U P A 1 C34 C 0.7712(12) 0.4869(10) 0.5511(7) 0.0538(12) Uani 0.529(15) 1 d D . P A 1 H34A H 0.836848 0.421403 0.546346 0.081 Uiso 0.529(15) 1 calc R U P A 1 H34B H 0.688960 0.453518 0.589758 0.081 Uiso 0.529(15) 1 calc R U P A 1 H34C H 0.794113 0.541496 0.578902 0.081 Uiso 0.529(15) 1 calc R U P A 1 C32A C 0.6241(11) 0.6634(11) 0.4751(8) 0.0538(12) Uani 0.471(15) 1 d D . P A 2 H32D H 0.599315 0.714648 0.421359 0.081 Uiso 0.471(15) 1 calc R U P A 2 H32E H 0.645575 0.713904 0.506814 0.081 Uiso 0.471(15) 1 calc R U P A 2 H32F H 0.553108 0.614165 0.517293 0.081 Uiso 0.471(15) 1 calc R U P A 2 C33A C 0.8888(11) 0.6772(11) 0.3831(7) 0.0538(12) Uani 0.471(15) 1 d D . P A 2 H33D H 0.962268 0.644663 0.406204 0.081 Uiso 0.471(15) 1 calc R U P A 2 H33E H 0.857165 0.753454 0.397988 0.081 Uiso 0.471(15) 1 calc R U P A 2 H33F H 0.914704 0.690653 0.316201 0.081 Uiso 0.471(15) 1 calc R U P A 2 C34A C 0.8078(13) 0.4914(11) 0.5405(8) 0.0538(12) Uani 0.471(15) 1 d D . P A 2 H34D H 0.754396 0.423073 0.576760 0.081 Uiso 0.471(15) 1 calc R U P A 2 H34E H 0.797845 0.547200 0.577592 0.081 Uiso 0.471(15) 1 calc R U P A 2 H34F H 0.897280 0.462428 0.522545 0.081 Uiso 0.471(15) 1 calc R U P A 2 C35 C 0.7451(6) 0.2911(5) 0.7743(4) 0.0693(15) Uani 1 1 d . . . . . H35A H 0.821126 0.338203 0.750016 0.104 Uiso 1 1 calc R U . . . H35B H 0.669073 0.343322 0.790828 0.104 Uiso 1 1 calc R U . . . H35C H 0.738939 0.256280 0.727231 0.104 Uiso 1 1 calc R U . . . C36 C 0.7547(4) 0.1918(4) 0.8584(3) 0.0486(10) Uani 1 1 d . . . . . H36A H 0.686805 0.135826 0.874241 0.058 Uiso 1 1 calc R U . . . H36B H 0.736833 0.227544 0.910272 0.058 Uiso 1 1 calc R U . . . C37 C 0.8807(4) 0.1191(5) 0.8513(3) 0.0519(11) Uani 1 1 d . . . . . H37A H 0.947670 0.173851 0.840493 0.062 Uiso 1 1 calc R U . . . H37B H 0.874637 0.058903 0.911385 0.062 Uiso 1 1 calc R U . . . C38 C 0.9232(4) 0.0545(5) 0.7774(3) 0.0532(11) Uani 1 1 d . . . . . H38A H 1.008833 0.015546 0.776609 0.064 Uiso 1 1 calc R U . . . H38B H 0.931147 0.114464 0.716960 0.064 Uiso 1 1 calc R U . . . C39 C 0.8340(5) -0.0409(5) 0.7888(4) 0.0607(13) Uani 1 1 d . . . . . H39A H 0.757935 -0.001599 0.771380 0.091 Uiso 1 1 calc R U . . . H39B H 0.808687 -0.089285 0.853230 0.091 Uiso 1 1 calc R U . . . H39C H 0.878140 -0.093092 0.749215 0.091 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 0.0205(3) 0.0114(3) 0.0122(3) -0.00220(17) -0.00895(18) 0.00124(17) P1 0.0169(4) 0.0103(4) 0.0109(4) -0.0018(3) -0.0048(3) -0.0016(3) P2 0.0409(5) 0.0214(4) 0.0235(5) -0.0112(3) -0.0236(4) 0.0108(4) O1 0.0344(12) 0.0137(10) 0.0156(10) -0.0042(8) -0.0157(9) 0.0026(8) O2 0.0252(11) 0.0248(11) 0.0204(11) -0.0006(9) -0.0047(9) -0.0124(9) O3 0.0225(10) 0.0142(10) 0.0208(10) 0.0006(8) -0.0062(8) -0.0015(8) C1 0.0159(13) 0.0178(14) 0.0126(13) -0.0030(11) -0.0058(10) -0.0016(10) C2 0.0168(13) 0.0118(13) 0.0131(13) -0.0010(10) -0.0060(10) -0.0023(10) C3 0.0178(13) 0.0146(13) 0.0160(13) -0.0056(11) -0.0047(11) -0.0038(10) C4 0.0177(13) 0.0230(15) 0.0132(13) -0.0032(11) -0.0067(11) -0.0042(11) C5 0.0180(13) 0.0157(14) 0.0142(13) 0.0005(11) -0.0074(11) -0.0004(11) C6 0.0155(13) 0.0156(14) 0.0145(13) -0.0031(11) -0.0054(10) -0.0007(10) C7 0.0419(18) 0.0213(16) 0.0185(15) -0.0015(12) -0.0182(13) -0.0037(13) C8 0.0311(16) 0.0128(14) 0.0198(14) -0.0023(11) -0.0143(12) 0.0034(11) C9 0.0418(19) 0.0228(16) 0.0227(16) -0.0104(13) -0.0112(14) 0.0075(14) C10 0.051(2) 0.0138(15) 0.0305(17) -0.0030(13) -0.0236(16) 0.0043(14) C11 0.0414(19) 0.0182(15) 0.0344(18) -0.0066(13) -0.0221(15) -0.0035(13) C12 0.0201(14) 0.0159(13) 0.0080(12) -0.0035(10) -0.0015(10) -0.0032(11) C13 0.0217(14) 0.0167(13) 0.0110(13) -0.0060(10) -0.0035(10) -0.0032(11) C14 0.0291(15) 0.0126(13) 0.0129(13) -0.0021(10) -0.0022(11) -0.0047(11) C15 0.0220(14) 0.0259(16) 0.0188(14) -0.0068(12) -0.0013(11) -0.0115(12) C16 0.0193(14) 0.0283(16) 0.0193(14) -0.0071(12) -0.0050(11) -0.0033(12) C17 0.0235(14) 0.0176(14) 0.0114(13) -0.0035(10) -0.0043(11) -0.0008(11) C18 0.0312(16) 0.0155(14) 0.0234(15) -0.0010(12) -0.0098(13) 0.0005(12) C19 0.0193(13) 0.0129(13) 0.0126(13) -0.0002(10) -0.0032(11) -0.0008(10) C20 0.0221(14) 0.0186(14) 0.0157(14) 0.0004(11) -0.0056(11) -0.0029(11) C21 0.0203(15) 0.0327(17) 0.0211(15) -0.0014(13) 0.0016(12) -0.0032(13) C22 0.0330(18) 0.0326(18) 0.0231(17) -0.0103(14) 0.0058(14) 0.0029(14) C23 0.0399(18) 0.0212(16) 0.0226(16) -0.0097(13) -0.0009(14) -0.0018(13) C24 0.0249(15) 0.0179(14) 0.0165(14) -0.0047(11) -0.0015(11) -0.0041(11) C25 0.0313(18) 0.041(2) 0.038(2) -0.0018(16) -0.0091(15) -0.0209(16) C26 0.0207(14) 0.0126(13) 0.0143(13) -0.0035(11) -0.0078(11) 0.0015(11) C27 0.0209(15) 0.0255(16) 0.0194(15) 0.0034(12) -0.0041(12) 0.0019(12) C28 0.0248(16) 0.040(2) 0.0316(18) -0.0030(15) -0.0083(14) 0.0154(15) C29 0.0413(19) 0.0242(16) 0.0251(16) -0.0047(13) -0.0172(14) 0.0136(14) C30 0.0373(17) 0.0181(14) 0.0145(14) -0.0005(11) -0.0063(12) -0.0028(13) C31 0.0214(14) 0.0240(15) 0.0185(14) -0.0052(12) -0.0036(12) -0.0004(12) C32 0.093(3) 0.0313(19) 0.060(2) -0.0193(17) -0.054(2) 0.016(2) C33 0.093(3) 0.0313(19) 0.060(2) -0.0193(17) -0.054(2) 0.016(2) C34 0.093(3) 0.0313(19) 0.060(2) -0.0193(17) -0.054(2) 0.016(2) C32A 0.093(3) 0.0313(19) 0.060(2) -0.0193(17) -0.054(2) 0.016(2) C33A 0.093(3) 0.0313(19) 0.060(2) -0.0193(17) -0.054(2) 0.016(2) C34A 0.093(3) 0.0313(19) 0.060(2) -0.0193(17) -0.054(2) 0.016(2) C35 0.077(4) 0.073(4) 0.059(3) 0.004(3) -0.031(3) -0.027(3) C36 0.047(2) 0.066(3) 0.034(2) -0.014(2) -0.0151(18) -0.002(2) C37 0.045(2) 0.069(3) 0.040(2) -0.011(2) -0.0130(18) -0.006(2) C38 0.043(2) 0.065(3) 0.048(2) -0.011(2) -0.0130(19) -0.001(2) C39 0.063(3) 0.055(3) 0.062(3) -0.002(2) -0.031(2) 0.001(2) 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 C26 Ni1 O1 175.58(10) C26 Ni1 P2 87.83(9) O1 Ni1 P2 88.64(7) C26 Ni1 P1 96.81(9) O1 Ni1 P1 86.80(6) P2 Ni1 P1 175.03(3) C2 P1 C19 103.48(13) C2 P1 C12 106.16(13) C19 P1 C12 104.49(13) C2 P1 Ni1 99.12(9) C19 P1 Ni1 125.01(10) C12 P1 Ni1 116.20(9) C32A P2 C34A 105.5(5) C34 P2 C32 103.6(4) C34 P2 C33 102.2(4) C32 P2 C33 101.0(4) C32A P2 C33A 101.4(4) C34A P2 C33A 97.4(5) C32A P2 Ni1 113.2(4) C34 P2 Ni1 123.2(4) C34A P2 Ni1 124.7(5) C32 P2 Ni1 119.2(3) C33 P2 Ni1 104.1(3) C33A P2 Ni1 111.3(3) C1 O1 Ni1 120.68(18) C20 O2 C25 117.7(3) C13 O3 C18 119.3(2) O1 C1 C2 120.2(3) O1 C1 C6 121.9(3) C2 C1 C6 118.0(3) C3 C2 C1 122.0(3) C3 C2 P1 124.9(2) C1 C2 P1 113.0(2) C4 C3 C2 120.5(3) C3 C4 C5 117.8(3) C3 C4 C7 122.1(3) C5 C4 C7 120.1(3) C6 C5 C4 123.8(3) C5 C6 C1 118.0(3) C5 C6 C8 121.3(3) C1 C6 C8 120.7(2) C6 C8 C9 108.4(2) C6 C8 C10 112.8(2) C9 C8 C10 107.4(3) C6 C8 C11 110.3(2) C9 C8 C11 110.7(3) C10 C8 C11 107.1(3) C17 C12 C13 118.9(2) C17 C12 P1 121.8(2) C13 C12 P1 119.3(2) O3 C13 C14 124.1(3) O3 C13 C12 115.4(2) C14 C13 C12 120.4(3) C15 C14 C13 119.3(3) C16 C15 C14 120.6(3) C17 C16 C15 120.0(3) C16 C17 C12 120.8(3) C24 C19 C20 118.6(3) C24 C19 P1 123.5(2) C20 C19 P1 117.8(2) O2 C20 C21 124.1(3) O2 C20 C19 115.5(3) C21 C20 C19 120.3(3) C22 C21 C20 119.6(3) C21 C22 C23 121.2(3) C22 C23 C24 118.8(3) C19 C24 C23 121.5(3) C31 C26 C27 117.0(3) C31 C26 Ni1 122.9(2) C27 C26 Ni1 119.9(2) C26 C27 C28 120.8(3) C29 C28 C27 121.0(3) C28 C29 C30 118.7(3) C29 C30 C31 120.5(3) C26 C31 C30 121.9(3) C35 C36 C37 116.7(4) C38 C37 C36 116.2(4) C37 C38 C39 114.5(4) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance Ni1 C26 1.895(3) Ni1 O1 1.913(2) Ni1 P2 2.1856(8) Ni1 P1 2.1860(8) P1 C2 1.803(3) P1 C19 1.823(3) P1 C12 1.826(3) P2 C32A 1.789(8) P2 C34 1.793(8) P2 C34A 1.806(8) P2 C32 1.811(7) P2 C33 1.853(8) P2 C33A 1.871(9) O1 C1 1.329(4) O2 C20 1.364(4) O2 C25 1.427(4) O3 C13 1.352(4) O3 C18 1.424(3) C1 C2 1.405(4) C1 C6 1.428(4) C2 C3 1.401(4) C3 C4 1.374(4) C4 C5 1.404(4) C4 C7 1.511(4) C5 C6 1.391(4) C6 C8 1.529(4) C8 C9 1.532(4) C8 C10 1.532(4) C8 C11 1.543(4) C12 C17 1.395(4) C12 C13 1.407(4) C13 C14 1.396(4) C14 C15 1.392(5) C15 C16 1.386(4) C16 C17 1.383(4) C19 C24 1.389(4) C19 C20 1.404(4) C20 C21 1.393(4) C21 C22 1.382(5) C22 C23 1.388(5) C23 C24 1.390(4) C26 C31 1.386(4) C26 C27 1.402(4) C27 C28 1.402(5) C28 C29 1.376(5) C29 C30 1.381(5) C30 C31 1.395(4) C35 C36 1.505(7) C36 C37 1.517(6) C37 C38 1.505(7) C38 C39 1.530(7)