#------------------------------------------------------------------------------ #$Date: 2016-03-26 11:48:58 +0000 (Sat, 26 Mar 2016) $ #$Revision: 180236 $ #$URL: svn://www.crystallography.net/cod/cif/7/11/22/7112260.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_7112260 loop_ _publ_author_name 'Kyle T. Horak' 'Alexandra Velian' 'Michael W. Day' 'Theodor Agapie' _publ_section_title ; Arene non-innocence in dinuclear complexes of Fe, Co, and Ni supported by a para-terphenyl diphosphine ; _journal_name_full Chem.Commun. _journal_page_first 4427 _journal_paper_doi 10.1039/C4CC00838C _journal_volume 50 _journal_year 2014 _chemical_formula_moiety 'C33 H40 Ni2 O3 P2' _chemical_formula_sum 'C33 H40 Ni2 O3 P2' _chemical_formula_weight 664.01 _chemical_name_systematic ; ? ; _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_Hall '-P 2ybc' _space_group_name_H-M_alt 'P 1 21/c 1' _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_space_group_name_H-M 'P 1 21/c 1' _atom_sites_solution_hydrogens geom _audit_creation_method SHELXL-2013 _cell_angle_alpha 90 _cell_angle_beta 115.3799(11) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 14.1146(4) _cell_length_b 15.1785(4) _cell_length_c 15.6000(4) _cell_measurement_reflns_used 9854 _cell_measurement_temperature 100(2) _cell_measurement_theta_max 30.66 _cell_measurement_theta_min 2.64 _cell_volume 3019.56(14) _computing_structure_refinement 'SHELXL-2013 (Sheldrick, 2013)' _diffrn_ambient_temperature 100(2) _diffrn_measured_fraction_theta_full 1.000 _diffrn_measured_fraction_theta_max 0.993 _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 0.0306 _diffrn_reflns_av_unetI/netI 0.0225 _diffrn_reflns_Laue_measured_fraction_full 1.000 _diffrn_reflns_Laue_measured_fraction_max 0.993 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_number 51225 _diffrn_reflns_point_group_measured_fraction_full 1.000 _diffrn_reflns_point_group_measured_fraction_max 0.993 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 30.656 _diffrn_reflns_theta_min 1.972 _exptl_absorpt_coefficient_mu 1.386 _exptl_absorpt_correction_T_max 0.7461 _exptl_absorpt_correction_T_min 0.6891 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details sadabs _exptl_crystal_colour red _exptl_crystal_density_diffrn 1.461 _exptl_crystal_description block _exptl_crystal_F_000 1392 _exptl_crystal_size_max 0.94 _exptl_crystal_size_mid 0.8 _exptl_crystal_size_min 0.7 _refine_diff_density_max 1.939 _refine_diff_density_min -0.466 _refine_diff_density_rms 0.091 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 0.983 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 369 _refine_ls_number_reflns 9272 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 0.983 _refine_ls_R_factor_all 0.0409 _refine_ls_R_factor_gt 0.0321 _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^)+(0.1000P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1090 _refine_ls_wR_factor_ref 0.1222 _reflns_Friedel_coverage 0.000 _reflns_number_gt 7834 _reflns_number_total 9272 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file c4cc00838c2.cif _cod_data_source_block kth160 _cod_database_code 7112260 #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. ; _shelxl_version_number 2013-3 _shelx_res_file ; TITL kth16 in P2(1)/c CELL 0.71073 14.11460 15.17850 15.60000 90.0000 115.3799 90.0000 ZERR 4.00 0.00040 0.00040 0.00040 0.0000 0.0011 0.0000 LATT 1 SYMM -X, 0.5+Y, 0.5-Z SFAC C H O P Ni UNIT 132 160 12 8 8 L.S. 64 ACTA BOND FMAP 2 PLAN 20 TEMP 0.000 WGHT 0.100000 FVAR 0.08322 MOLE 1 NI2 5 0.190339 0.778019 0.182245 11.00000 0.00792 0.00795 = 0.00983 0.00010 0.00352 -0.00002 NI1 5 0.345516 0.693502 0.317243 11.00000 0.00824 0.00989 = 0.00901 -0.00015 0.00401 0.00022 P2 4 0.030672 0.770445 0.181388 11.00000 0.00781 0.00839 = 0.00984 -0.00077 0.00345 0.00011 P1 4 0.512988 0.717120 0.351697 11.00000 0.00787 0.01077 = 0.00914 -0.00079 0.00364 -0.00061 C4 1 0.153809 0.664939 0.090419 11.00000 0.00970 0.01002 = 0.00789 -0.00101 0.00352 0.00066 AFIX 43 H4 2 0.103053 0.696087 0.040503 11.00000 -1.20000 AFIX 0 C3 1 0.260964 0.680075 0.116041 11.00000 0.00938 0.00935 = 0.01098 -0.00099 0.00485 -0.00065 AFIX 43 H3 2 0.280783 0.722856 0.084245 11.00000 -1.20000 AFIX 0 C2 1 0.340212 0.630020 0.190958 11.00000 0.00836 0.01103 = 0.01086 -0.00129 0.00490 -0.00006 C5 1 0.123245 0.600875 0.142019 11.00000 0.00901 0.00910 = 0.01080 -0.00216 0.00453 -0.00028 C1 1 0.307437 0.567774 0.240629 11.00000 0.01034 0.00930 = 0.01077 -0.00013 0.00413 0.00043 AFIX 43 H1 2 0.357244 0.536101 0.290711 11.00000 -1.20000 AFIX 0 C6 1 0.198191 0.553438 0.214123 11.00000 0.01074 0.01002 = 0.01325 -0.00015 0.00529 -0.00065 AFIX 43 H6 2 0.177741 0.511400 0.246211 11.00000 -1.20000 AFIX 0 C8 1 0.537584 0.645401 0.269915 11.00000 0.00990 0.01218 = 0.01087 0.00036 0.00513 0.00008 C14 1 -0.043632 0.668173 0.130607 11.00000 0.00880 0.01118 = 0.01000 -0.00182 0.00335 -0.00185 C12 1 0.455877 0.565693 0.121765 11.00000 0.01076 0.01532 = 0.01310 -0.00195 0.00571 -0.00108 AFIX 43 H12 2 0.396094 0.549418 0.068332 11.00000 -1.20000 AFIX 0 C13 1 0.010465 0.593668 0.119592 11.00000 0.00917 0.01162 = 0.00814 0.00061 0.00400 0.00021 C15 1 -0.150336 0.659698 0.108407 11.00000 0.00926 0.01467 = 0.01549 -0.00235 0.00534 -0.00014 AFIX 43 H15 2 -0.187147 0.708230 0.114592 11.00000 -1.20000 AFIX 0 C9 1 0.636333 0.618395 0.278613 11.00000 0.00867 0.01611 = 0.01396 -0.00197 0.00359 -0.00041 AFIX 43 H9 2 0.696625 0.636749 0.330384 11.00000 -1.20000 AFIX 0 C17 1 -0.148581 0.506388 0.067710 11.00000 0.01194 0.01328 = 0.01367 -0.00235 0.00558 -0.00311 AFIX 43 H17 2 -0.183030 0.452844 0.047500 11.00000 -1.20000 AFIX 0 C18 1 -0.042823 0.513962 0.088769 11.00000 0.01311 0.01087 = 0.01291 -0.00236 0.00562 -0.00092 AFIX 43 H18 2 -0.006809 0.465032 0.082221 11.00000 -1.20000 AFIX 0 C7 1 0.446543 0.616477 0.192883 11.00000 0.00996 0.01035 = 0.01167 -0.00092 0.00525 -0.00039 C16 1 -0.202428 0.579724 0.077166 11.00000 0.01002 0.01572 = 0.01606 -0.00240 0.00588 -0.00248 AFIX 43 H16 2 -0.273423 0.575407 0.062601 11.00000 -1.20000 AFIX 0 C11 1 0.554139 0.539608 0.130857 11.00000 0.01543 0.01717 = 0.01492 -0.00070 0.00921 0.00251 AFIX 43 H11 2 0.559635 0.505454 0.083699 11.00000 -1.20000 AFIX 0 C10 1 0.644466 0.564215 0.210051 11.00000 0.01237 0.01667 = 0.01701 0.00187 0.00816 0.00411 AFIX 43 H10 2 0.709809 0.544568 0.217078 11.00000 -1.20000 AFIX 0 C25 1 -0.082693 0.851563 0.005592 11.00000 0.01705 0.01878 = 0.01194 0.00083 0.00281 0.00303 AFIX 137 H25A 2 -0.133340 0.895295 -0.030245 11.00000 -1.50000 H25B 2 -0.108810 0.794108 -0.018892 11.00000 -1.50000 H25C 2 -0.018209 0.862019 0.000519 11.00000 -1.50000 AFIX 0 C29 1 0.027574 0.776733 0.299743 11.00000 0.01146 0.01231 = 0.01154 -0.00059 0.00604 -0.00114 AFIX 13 H29 2 0.076146 0.823739 0.335256 11.00000 -1.20000 AFIX 0 C32 1 0.281422 0.807850 0.309583 11.00000 0.00962 0.01274 = 0.01305 -0.00030 0.00495 -0.00028 C27 1 -0.024258 0.949220 0.150175 11.00000 0.01970 0.00963 = 0.01830 0.00073 0.00762 0.00300 AFIX 137 H27A 2 0.040811 0.961165 0.146727 11.00000 -1.50000 H27B 2 -0.013852 0.952013 0.215098 11.00000 -1.50000 H27C 2 -0.075520 0.992221 0.113550 11.00000 -1.50000 AFIX 0 C33 1 0.200459 0.875684 0.121630 11.00000 0.01073 0.01513 = 0.01256 -0.00132 0.00504 0.00031 C31 1 0.334473 0.655766 0.420940 11.00000 0.01155 0.01588 = 0.01455 0.00000 0.00577 -0.00041 C20 1 0.612423 0.684923 0.471270 11.00000 0.00909 0.01538 = 0.01162 0.00185 0.00219 0.00026 AFIX 13 H20 2 0.682315 0.696919 0.475010 11.00000 -1.20000 AFIX 0 C23 1 0.557932 0.827135 0.331149 11.00000 0.01440 0.01204 = 0.01330 -0.00145 0.00658 -0.00406 AFIX 13 H23 2 0.551243 0.867701 0.377121 11.00000 -1.20000 AFIX 0 C19 1 0.604587 0.586248 0.489116 11.00000 0.02247 0.01816 = 0.01963 0.00593 0.00576 0.00117 AFIX 137 H19A 2 0.658083 0.570697 0.550428 11.00000 -1.50000 H19B 2 0.613895 0.552582 0.441188 11.00000 -1.50000 H19C 2 0.536884 0.573793 0.486884 11.00000 -1.50000 AFIX 0 C28 1 0.072551 0.690435 0.352882 11.00000 0.01758 0.01946 = 0.01573 0.00554 0.00881 0.00511 AFIX 137 H28A 2 0.091154 0.698412 0.419219 11.00000 -1.50000 H28B 2 0.133767 0.674210 0.344472 11.00000 -1.50000 H28C 2 0.020869 0.644695 0.328197 11.00000 -1.50000 AFIX 0 C22 1 0.671474 0.832662 0.344446 11.00000 0.01252 0.02142 = 0.01884 0.00369 0.00443 -0.00400 AFIX 137 H22A 2 0.679206 0.799361 0.295510 11.00000 -1.50000 H22B 2 0.717083 0.808999 0.405341 11.00000 -1.50000 H22C 2 0.689490 0.893099 0.340844 11.00000 -1.50000 AFIX 0 C30 1 -0.077927 0.797686 0.301312 11.00000 0.01711 0.01699 = 0.01858 -0.00060 0.01124 0.00148 AFIX 137 H30A 2 -0.126009 0.750149 0.272523 11.00000 -1.50000 H30B 2 -0.105871 0.851059 0.266636 11.00000 -1.50000 H30C 2 -0.067965 0.804969 0.365760 11.00000 -1.50000 AFIX 0 C26 1 -0.063012 0.856798 0.110401 11.00000 0.01143 0.01077 = 0.01266 0.00031 0.00487 0.00212 AFIX 13 H26 2 -0.129826 0.846365 0.113820 11.00000 -1.20000 AFIX 0 C24 1 0.483632 0.860438 0.232218 11.00000 0.01365 0.01839 = 0.01725 0.00468 0.00562 -0.00065 AFIX 137 H24A 2 0.499655 0.920783 0.225473 11.00000 -1.50000 H24B 2 0.412494 0.856142 0.224325 11.00000 -1.50000 H24C 2 0.492214 0.825244 0.184898 11.00000 -1.50000 AFIX 0 C21 1 0.597118 0.740771 0.546174 11.00000 0.01594 0.02775 = 0.01099 -0.00202 0.00537 -0.00517 AFIX 137 H21A 2 0.528933 0.729501 0.543396 11.00000 -1.50000 H21B 2 0.602980 0.802060 0.534025 11.00000 -1.50000 H21C 2 0.649850 0.725750 0.608039 11.00000 -1.50000 AFIX 0 O2 3 0.292280 0.865116 0.363234 11.00000 0.01917 0.01590 = 0.01828 -0.00557 0.00647 0.00021 O3 3 0.204279 0.941545 0.087563 11.00000 0.02573 0.01473 = 0.02762 0.00647 0.01389 0.00137 O1 3 0.337275 0.634973 0.492380 11.00000 0.02451 0.03506 = 0.01763 0.00599 0.01054 -0.00015 HKLF 4 REM kth16 in P2(1)/c REM R1 = 0.0321 for 7834 Fo > 4sig(Fo) and 0.0409 for all 9272 data REM 369 parameters refined using 0 restraints END WGHT 0.0447 2.0978 REM Highest difference peak 1.939, deepest hole -0.466, 1-sigma level 0.091 Q1 1 0.5037 0.5514 0.1303 11.00000 0.05 0.59 Q2 1 0.1906 0.8351 0.1798 11.00000 0.05 0.56 Q3 1 0.2138 0.6671 0.0968 11.00000 0.05 0.55 Q4 1 0.5886 0.6286 0.2769 11.00000 0.05 0.52 Q5 1 0.4951 0.6354 0.2305 11.00000 0.05 0.50 Q6 1 0.2999 0.6498 0.1491 11.00000 0.05 0.50 Q7 1 0.5944 0.5536 0.1688 11.00000 0.05 0.49 Q8 1 0.1228 0.7798 0.1860 11.00000 0.05 0.49 Q9 1 -0.1771 0.6227 0.0886 11.00000 0.05 0.49 Q10 1 -0.1010 0.6630 0.1180 11.00000 0.05 0.49 Q11 1 0.1613 0.5840 0.1791 11.00000 0.05 0.48 Q12 1 -0.1006 0.5121 0.0809 11.00000 0.05 0.47 Q13 1 -0.1762 0.5451 0.0623 11.00000 0.05 0.47 Q14 1 0.1399 0.6288 0.1144 11.00000 0.05 0.46 Q15 1 0.6291 0.5901 0.2368 11.00000 0.05 0.46 Q16 1 -0.0273 0.5575 0.0940 11.00000 0.05 0.46 Q17 1 0.3198 0.5952 0.2076 11.00000 0.05 0.45 Q18 1 0.3367 0.7549 0.3189 11.00000 0.05 0.44 Q19 1 -0.0169 0.7868 0.3006 11.00000 0.05 0.44 Q20 1 0.5666 0.7044 0.4189 11.00000 0.05 0.43 ; _shelx_res_checksum 94685 #END Tags that were not found in dictionaries loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp Ni2 Ni 0.19034(2) 0.77802(2) 0.18225(2) 0.00867(7) Uani 1 1 d . . Ni1 Ni 0.34552(2) 0.69350(2) 0.31724(2) 0.00894(7) Uani 1 1 d . . P2 P 0.03067(3) 0.77044(2) 0.18139(3) 0.00879(9) Uani 1 1 d . . P1 P 0.51299(3) 0.71712(3) 0.35170(3) 0.00927(9) Uani 1 1 d . . C4 C 0.15381(12) 0.66494(9) 0.09042(10) 0.0093(3) Uani 1 1 d . . H4 H 0.1031 0.6961 0.0405 0.011 Uiso 1 1 calc R U C3 C 0.26096(12) 0.68007(10) 0.11604(11) 0.0097(3) Uani 1 1 d . . H3 H 0.2808 0.7229 0.0842 0.012 Uiso 1 1 calc R U C2 C 0.34021(12) 0.63002(10) 0.19096(10) 0.0098(3) Uani 1 1 d . . C5 C 0.12325(12) 0.60087(9) 0.14202(10) 0.0095(3) Uani 1 1 d . . C1 C 0.30744(12) 0.56777(10) 0.24063(11) 0.0103(3) Uani 1 1 d . . H1 H 0.3572 0.5361 0.2907 0.012 Uiso 1 1 calc R U C6 C 0.19819(12) 0.55344(10) 0.21412(11) 0.0113(3) Uani 1 1 d . . H6 H 0.1777 0.5114 0.2462 0.014 Uiso 1 1 calc R U C8 C 0.53758(12) 0.64540(10) 0.26991(11) 0.0107(3) Uani 1 1 d . . C14 C -0.04363(12) 0.66817(10) 0.13061(11) 0.0102(3) Uani 1 1 d . . C12 C 0.45588(12) 0.56569(10) 0.12176(11) 0.0129(3) Uani 1 1 d . . H12 H 0.3961 0.5494 0.0683 0.015 Uiso 1 1 calc R U C13 C 0.01046(12) 0.59367(10) 0.11959(10) 0.0095(3) Uani 1 1 d . . C15 C -0.15034(12) 0.65970(11) 0.10841(11) 0.0131(3) Uani 1 1 d . . H15 H -0.1871 0.7082 0.1146 0.016 Uiso 1 1 calc R U C9 C 0.63633(12) 0.61839(11) 0.27861(11) 0.0134(3) Uani 1 1 d . . H9 H 0.6966 0.6367 0.3304 0.016 Uiso 1 1 calc R U C17 C -0.14858(12) 0.50639(11) 0.06771(11) 0.0129(3) Uani 1 1 d . . H17 H -0.1830 0.4528 0.0475 0.016 Uiso 1 1 calc R U C18 C -0.04282(13) 0.51396(10) 0.08877(11) 0.0123(3) Uani 1 1 d . . H18 H -0.0068 0.4650 0.0822 0.015 Uiso 1 1 calc R U C7 C 0.44654(12) 0.61648(10) 0.19288(11) 0.0104(3) Uani 1 1 d . . C16 C -0.20243(12) 0.57972(11) 0.07717(12) 0.0138(3) Uani 1 1 d . . H16 H -0.2734 0.5754 0.0626 0.017 Uiso 1 1 calc R U C11 C 0.55414(13) 0.53961(11) 0.13086(12) 0.0149(3) Uani 1 1 d . . H11 H 0.5596 0.5055 0.0837 0.018 Uiso 1 1 calc R U C10 C 0.64447(13) 0.56421(11) 0.21005(12) 0.0147(3) Uani 1 1 d . . H10 H 0.7098 0.5446 0.2171 0.018 Uiso 1 1 calc R U C25 C -0.08269(14) 0.85156(12) 0.00559(11) 0.0171(3) Uani 1 1 d . . H25A H -0.1333 0.8953 -0.0302 0.026 Uiso 1 1 calc R U H25B H -0.1088 0.7941 -0.0189 0.026 Uiso 1 1 calc R U H25C H -0.0182 0.8620 0.0005 0.026 Uiso 1 1 calc R U C29 C 0.02757(13) 0.77673(10) 0.29974(11) 0.0114(3) Uani 1 1 d . . H29 H 0.0761 0.8237 0.3353 0.014 Uiso 1 1 calc R U C32 C 0.28142(12) 0.80785(10) 0.30958(11) 0.0118(3) Uani 1 1 d . . C27 C -0.02426(14) 0.94922(10) 0.15018(12) 0.0161(3) Uani 1 1 d . . H27A H 0.0408 0.9612 0.1467 0.024 Uiso 1 1 calc R U H27B H -0.0139 0.9520 0.2151 0.024 Uiso 1 1 calc R U H27C H -0.0755 0.9922 0.1135 0.024 Uiso 1 1 calc R U C33 C 0.20046(12) 0.87568(10) 0.12163(11) 0.0128(3) Uani 1 1 d . . C31 C 0.33447(13) 0.65577(11) 0.42094(11) 0.0139(3) Uani 1 1 d . . C20 C 0.61242(12) 0.68492(10) 0.47127(11) 0.0128(3) Uani 1 1 d . . H20 H 0.6823 0.6969 0.4750 0.015 Uiso 1 1 calc R U C23 C 0.55793(13) 0.82713(10) 0.33115(11) 0.0130(3) Uani 1 1 d . . H23 H 0.5512 0.8677 0.3771 0.016 Uiso 1 1 calc R U C19 C 0.60459(15) 0.58625(12) 0.48912(13) 0.0212(4) Uani 1 1 d . . H19A H 0.6581 0.5707 0.5504 0.032 Uiso 1 1 calc R U H19B H 0.6139 0.5526 0.4412 0.032 Uiso 1 1 calc R U H19C H 0.5369 0.5738 0.4869 0.032 Uiso 1 1 calc R U C28 C 0.07255(14) 0.69043(11) 0.35288(12) 0.0170(3) Uani 1 1 d . . H28A H 0.0912 0.6984 0.4192 0.026 Uiso 1 1 calc R U H28B H 0.1338 0.6742 0.3445 0.026 Uiso 1 1 calc R U H28C H 0.0209 0.6447 0.3282 0.026 Uiso 1 1 calc R U C22 C 0.67147(13) 0.83266(12) 0.34445(13) 0.0184(3) Uani 1 1 d . . H22A H 0.6792 0.7994 0.2955 0.028 Uiso 1 1 calc R U H22B H 0.7171 0.8090 0.4053 0.028 Uiso 1 1 calc R U H22C H 0.6895 0.8931 0.3408 0.028 Uiso 1 1 calc R U C30 C -0.07793(14) 0.79769(11) 0.30131(12) 0.0163(3) Uani 1 1 d . . H30A H -0.1260 0.7501 0.2725 0.024 Uiso 1 1 calc R U H30B H -0.1059 0.8511 0.2666 0.024 Uiso 1 1 calc R U H30C H -0.0680 0.8050 0.3658 0.024 Uiso 1 1 calc R U C26 C -0.06301(12) 0.85680(10) 0.11040(11) 0.0117(3) Uani 1 1 d . . H26 H -0.1298 0.8464 0.1138 0.014 Uiso 1 1 calc R U C24 C 0.48363(13) 0.86044(11) 0.23222(12) 0.0168(3) Uani 1 1 d . . H24A H 0.4997 0.9208 0.2255 0.025 Uiso 1 1 calc R U H24B H 0.4125 0.8561 0.2243 0.025 Uiso 1 1 calc R U H24C H 0.4922 0.8252 0.1849 0.025 Uiso 1 1 calc R U C21 C 0.59712(14) 0.74077(12) 0.54617(12) 0.0184(3) Uani 1 1 d . . H21A H 0.5289 0.7295 0.5434 0.028 Uiso 1 1 calc R U H21B H 0.6030 0.8021 0.5340 0.028 Uiso 1 1 calc R U H21C H 0.6498 0.7257 0.6080 0.028 Uiso 1 1 calc R U O2 O 0.29228(10) 0.86512(8) 0.36323(9) 0.0183(2) Uani 1 1 d . . O3 O 0.20428(11) 0.94155(8) 0.08756(10) 0.0218(3) Uani 1 1 d . . O1 O 0.33728(11) 0.63497(10) 0.49238(9) 0.0252(3) Uani 1 1 d . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ni2 0.00792(11) 0.00795(11) 0.00983(11) 0.00010(6) 0.00352(8) -0.00002(6) Ni1 0.00824(11) 0.00989(11) 0.00901(11) -0.00015(6) 0.00401(8) 0.00022(7) P2 0.00781(18) 0.00839(17) 0.00984(18) -0.00077(12) 0.00345(14) 0.00011(13) P1 0.00787(18) 0.01077(18) 0.00914(18) -0.00079(13) 0.00364(15) -0.00061(13) C4 0.0097(6) 0.0100(6) 0.0079(6) -0.0010(5) 0.0035(5) 0.0007(5) C3 0.0094(6) 0.0093(6) 0.0110(6) -0.0010(5) 0.0048(5) -0.0006(5) C2 0.0084(6) 0.0110(6) 0.0109(6) -0.0013(5) 0.0049(5) -0.0001(5) C5 0.0090(6) 0.0091(6) 0.0108(6) -0.0022(5) 0.0045(5) -0.0003(5) C1 0.0103(6) 0.0093(6) 0.0108(6) -0.0001(5) 0.0041(5) 0.0004(5) C6 0.0107(7) 0.0100(6) 0.0132(7) -0.0001(5) 0.0053(6) -0.0007(5) C8 0.0099(6) 0.0122(6) 0.0109(6) 0.0004(5) 0.0051(5) 0.0001(5) C14 0.0088(6) 0.0112(6) 0.0100(6) -0.0018(5) 0.0034(5) -0.0018(5) C12 0.0108(7) 0.0153(7) 0.0131(7) -0.0020(5) 0.0057(6) -0.0011(6) C13 0.0092(6) 0.0116(6) 0.0081(6) 0.0006(5) 0.0040(5) 0.0002(5) C15 0.0093(7) 0.0147(7) 0.0155(7) -0.0023(6) 0.0053(6) -0.0001(6) C9 0.0087(7) 0.0161(7) 0.0140(7) -0.0020(6) 0.0036(6) -0.0004(6) C17 0.0119(7) 0.0133(7) 0.0137(7) -0.0023(5) 0.0056(6) -0.0031(6) C18 0.0131(7) 0.0109(6) 0.0129(7) -0.0024(5) 0.0056(6) -0.0009(6) C7 0.0100(6) 0.0103(6) 0.0117(7) -0.0009(5) 0.0053(6) -0.0004(5) C16 0.0100(7) 0.0157(7) 0.0161(7) -0.0024(6) 0.0059(6) -0.0025(6) C11 0.0154(7) 0.0172(7) 0.0149(7) -0.0007(6) 0.0092(6) 0.0025(6) C10 0.0124(7) 0.0167(7) 0.0170(7) 0.0019(6) 0.0082(6) 0.0041(6) C25 0.0170(8) 0.0188(7) 0.0119(7) 0.0008(6) 0.0028(6) 0.0030(6) C29 0.0115(7) 0.0123(7) 0.0115(7) -0.0006(5) 0.0060(6) -0.0011(5) C32 0.0096(7) 0.0127(7) 0.0130(7) -0.0003(5) 0.0050(6) -0.0003(5) C27 0.0197(8) 0.0096(7) 0.0183(8) 0.0007(6) 0.0076(7) 0.0030(6) C33 0.0107(7) 0.0151(7) 0.0126(7) -0.0013(5) 0.0050(6) 0.0003(6) C31 0.0116(7) 0.0159(7) 0.0146(7) 0.0000(6) 0.0058(6) -0.0004(6) C20 0.0091(7) 0.0154(7) 0.0116(7) 0.0019(5) 0.0022(6) 0.0003(6) C23 0.0144(7) 0.0120(6) 0.0133(7) -0.0015(5) 0.0066(6) -0.0041(6) C19 0.0225(9) 0.0182(8) 0.0196(8) 0.0059(6) 0.0058(7) 0.0012(7) C28 0.0176(8) 0.0195(8) 0.0157(8) 0.0055(6) 0.0088(7) 0.0051(6) C22 0.0125(7) 0.0214(8) 0.0188(8) 0.0037(6) 0.0044(6) -0.0040(6) C30 0.0171(8) 0.0170(7) 0.0186(8) -0.0006(6) 0.0112(7) 0.0015(6) C26 0.0114(7) 0.0108(6) 0.0127(7) 0.0003(5) 0.0049(6) 0.0021(5) C24 0.0136(7) 0.0184(8) 0.0172(8) 0.0047(6) 0.0056(6) -0.0007(6) C21 0.0159(8) 0.0277(9) 0.0110(7) -0.0020(6) 0.0054(6) -0.0052(7) O2 0.0192(6) 0.0159(6) 0.0183(6) -0.0056(4) 0.0065(5) 0.0002(5) O3 0.0257(7) 0.0147(6) 0.0276(7) 0.0065(5) 0.0139(6) 0.0014(5) O1 0.0245(7) 0.0351(8) 0.0176(6) 0.0060(5) 0.0105(5) -0.0002(6) 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 C33 Ni2 C32 100.53(7) C33 Ni2 C4 110.99(6) C32 Ni2 C4 138.35(6) C33 Ni2 P2 110.14(5) C32 Ni2 P2 104.20(5) C4 Ni2 P2 90.10(4) C33 Ni2 C3 98.71(6) C32 Ni2 C3 113.53(6) C4 Ni2 C3 37.01(5) P2 Ni2 C3 126.70(4) C33 Ni2 Ni1 126.64(5) C32 Ni2 Ni1 47.29(5) C4 Ni2 Ni1 91.36(4) P2 Ni2 Ni1 117.884(13) C3 Ni2 Ni1 70.59(4) C31 Ni1 C32 97.10(7) C31 Ni1 C2 134.38(7) C32 Ni1 C2 120.63(6) C31 Ni1 C1 96.81(7) C32 Ni1 C1 138.35(6) C2 Ni1 C1 38.00(5) C31 Ni1 P1 109.29(5) C32 Ni1 P1 106.93(5) C2 Ni1 P1 84.84(4) C1 Ni1 P1 105.05(4) C31 Ni1 Ni2 121.05(5) C32 Ni1 Ni2 46.16(5) C2 Ni1 Ni2 78.26(4) C1 Ni1 Ni2 93.59(4) P1 Ni1 Ni2 123.395(14) C14 P2 C26 102.07(7) C14 P2 C29 102.53(7) C26 P2 C29 103.97(7) C14 P2 Ni2 115.32(5) C26 P2 Ni2 115.05(5) C29 P2 Ni2 116.04(5) C8 P1 C20 104.94(7) C8 P1 C23 103.55(7) C20 P1 C23 104.03(7) C8 P1 Ni1 103.72(5) C20 P1 Ni1 118.00(5) C23 P1 Ni1 120.64(5) C3 C4 C5 119.59(13) C3 C4 Ni2 76.06(9) C5 C4 Ni2 102.12(9) C4 C3 C2 120.70(13) C4 C3 Ni2 66.93(8) C2 C3 Ni2 108.43(10) C1 C2 C3 118.21(13) C1 C2 C7 117.04(13) C3 C2 C7 120.68(13) C1 C2 Ni1 72.05(8) C3 C2 Ni1 102.45(10) C7 C2 Ni1 113.46(10) C6 C5 C4 120.12(14) C6 C5 C13 121.88(13) C4 C5 C13 117.83(13) C2 C1 C6 120.42(14) C2 C1 Ni1 69.95(8) C6 C1 Ni1 105.77(10) C5 C6 C1 120.90(14) C7 C8 C9 119.96(14) C7 C8 P1 114.09(11) C9 C8 P1 125.96(12) C15 C14 C13 118.42(14) C15 C14 P2 122.38(12) C13 C14 P2 119.07(11) C11 C12 C7 120.25(15) C18 C13 C14 119.66(14) C18 C13 C5 120.75(13) C14 C13 C5 119.58(13) C16 C15 C14 121.13(14) C10 C9 C8 120.27(15) C18 C17 C16 119.30(15) C17 C18 C13 121.25(14) C8 C7 C12 119.20(14) C8 C7 C2 121.01(13) C12 C7 C2 119.41(13) C17 C16 C15 120.23(15) C12 C11 C10 120.53(15) C9 C10 C11 119.61(15) C30 C29 C28 110.38(13) C30 C29 P2 117.44(12) C28 C29 P2 108.11(11) O2 C32 Ni2 138.31(13) O2 C32 Ni1 134.98(13) Ni2 C32 Ni1 86.55(6) O3 C33 Ni2 174.58(14) O1 C31 Ni1 173.12(15) C21 C20 C19 110.89(14) C21 C20 P1 109.14(11) C19 C20 P1 110.90(11) C22 C23 C24 110.11(13) C22 C23 P1 116.16(12) C24 C23 P1 109.42(11) C27 C26 C25 110.31(13) C27 C26 P2 111.40(11) C25 C26 P2 110.85(11) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance Ni2 C33 1.7966(16) Ni2 C32 1.9012(16) Ni2 C4 2.1519(14) Ni2 P2 2.2509(4) Ni2 C3 2.2700(15) Ni2 Ni1 2.6313(3) Ni1 C31 1.7848(16) Ni1 C32 1.9371(15) Ni1 C2 2.1653(15) Ni1 C1 2.1928(15) Ni1 P1 2.2172(4) P2 C14 1.8507(15) P2 C26 1.8541(16) P2 C29 1.8680(16) P1 C8 1.8201(16) P1 C20 1.8558(16) P1 C23 1.8622(16) C4 C3 1.408(2) C4 C5 1.441(2) C3 C2 1.440(2) C2 C1 1.419(2) C2 C7 1.502(2) C5 C6 1.372(2) C5 C13 1.480(2) C1 C6 1.432(2) C8 C7 1.402(2) C8 C9 1.403(2) C14 C15 1.399(2) C14 C13 1.416(2) C12 C11 1.390(2) C12 C7 1.403(2) C13 C18 1.397(2) C15 C16 1.394(2) C9 C10 1.392(2) C17 C18 1.389(2) C17 C16 1.391(2) C11 C10 1.393(2) C25 C26 1.539(2) C29 C30 1.533(2) C29 C28 1.535(2) C32 O2 1.1703(19) C27 C26 1.537(2) C33 O3 1.144(2) C31 O1 1.143(2) C20 C21 1.532(2) C20 C19 1.536(2) C23 C22 1.528(2) C23 C24 1.533(2)