# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_email xlsun@mail.sioc.ac.cn _publ_contact_author_name 'Xiu-Li Sun' loop_ _publ_author_name 'Da-Wei Wan' 'Jun-Fang Li' 'Qi Shen' 'Xiu-Li Sun' 'Yong Tang' data_cd201183 _database_code_depnum_ccdc_archive 'CCDC 847790' #TrackingRef 'cd201183.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C50 H48 Ni O4 P2' _chemical_formula_weight 833.53 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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 41.597(3) _cell_length_b 10.8709(8) _cell_length_c 21.9171(16) _cell_angle_alpha 90.00 _cell_angle_beta 118.4650(10) _cell_angle_gamma 90.00 _cell_volume 8712.7(11) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 2452 _cell_measurement_theta_min 4.446 _cell_measurement_theta_max 38.935 _exptl_crystal_description prismatic _exptl_crystal_colour colorless _exptl_crystal_size_max 0.269 _exptl_crystal_size_mid 0.225 _exptl_crystal_size_min 0.175 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.271 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3504 _exptl_absorpt_coefficient_mu 0.562 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.86809 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 22539 _diffrn_reflns_av_R_equivalents 0.0686 _diffrn_reflns_av_sigmaI/netI 0.1109 _diffrn_reflns_limit_h_min -49 _diffrn_reflns_limit_h_max 50 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.09 _diffrn_reflns_theta_max 25.50 _reflns_number_total 8099 _reflns_number_gt 4199 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0892P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00101(10) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 8099 _refine_ls_number_parameters 518 _refine_ls_number_restraints 25 _refine_ls_R_factor_all 0.1219 _refine_ls_R_factor_gt 0.0659 _refine_ls_wR_factor_ref 0.1902 _refine_ls_wR_factor_gt 0.1602 _refine_ls_goodness_of_fit_ref 0.913 _refine_ls_restrained_S_all 0.933 _refine_ls_shift/su_max 0.042 _refine_ls_shift/su_mean 0.002 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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ni1 Ni 0.121160(16) 0.74289(6) 0.39353(3) 0.0415(2) Uani 1 1 d . . . O1 O 0.15632(9) 0.8407(3) 0.38374(18) 0.0539(10) Uani 1 1 d . . . O2 O 0.11816(18) 0.4990(4) 0.4500(3) 0.1021(17) Uani 1 1 d . . . O3 O 0.14871(11) 1.0228(4) 0.6027(2) 0.0791(13) Uani 1 1 d . . . O4 O 0.06896(10) 0.8207(4) 0.51193(19) 0.0598(10) Uani 1 1 d . . . P1 P 0.12684(4) 0.87533(12) 0.47348(7) 0.0443(4) Uani 1 1 d . . . P2 P 0.12286(3) 0.62404(12) 0.31293(7) 0.0405(4) Uani 1 1 d . . . C1 C 0.16848(13) 0.9420(5) 0.4196(3) 0.0448(13) Uani 1 1 d . . . C2 C 0.15811(13) 0.9767(5) 0.4663(3) 0.0526(14) Uani 1 1 d . . . H2 H 0.1666 1.0480 0.4926 0.063 Uiso 1 1 calc R . . C3 C 0.19488(13) 1.0111(5) 0.4047(3) 0.0514(14) Uani 1 1 d . . . C4 C 0.21352(15) 0.9499(7) 0.3762(3) 0.0713(18) Uani 1 1 d . . . H4 H 0.2091 0.8669 0.3650 0.086 Uiso 1 1 calc R . . C5 C 0.23906(19) 1.0135(9) 0.3642(4) 0.101(3) Uani 1 1 d . . . H5 H 0.2525 0.9731 0.3464 0.121 Uiso 1 1 calc R . . C6 C 0.2441(2) 1.1393(10) 0.3794(4) 0.113(3) Uani 1 1 d . . . H6 H 0.2610 1.1820 0.3709 0.135 Uiso 1 1 calc R . . C7 C 0.2255(2) 1.2004(8) 0.4057(4) 0.100(3) Uani 1 1 d . . . H7 H 0.2290 1.2842 0.4150 0.120 Uiso 1 1 calc R . . C8 C 0.20157(16) 1.1351(6) 0.4182(3) 0.0759(19) Uani 1 1 d . . . H8 H 0.1888 1.1764 0.4371 0.091 Uiso 1 1 calc R . . C9 C 0.08116(19) 0.6575(6) 0.3927(3) 0.0649(18) Uani 1 1 d . . . C10 C 0.04566(15) 0.7159(8) 0.3540(4) 0.097(3) Uani 1 1 d . . . H10 H 0.0429 0.7918 0.3325 0.116 Uiso 1 1 calc R . . C11 C 0.0161(3) 0.6520(10) 0.3510(5) 0.128(3) Uani 1 1 d U . . H11 H -0.0073 0.6855 0.3277 0.154 Uiso 1 1 calc R . . C12 C 0.0211(3) 0.5470(11) 0.3802(5) 0.115(3) Uani 1 1 d U . . H12 H -0.0002 0.5122 0.3766 0.138 Uiso 1 1 calc R . . C13 C 0.0531(3) 0.4718(8) 0.4175(4) 0.125(4) Uani 1 1 d . . . H13 H 0.0543 0.3943 0.4365 0.149 Uiso 1 1 calc R . . C14 C 0.0843(2) 0.5456(9) 0.4195(4) 0.093(2) Uani 1 1 d . . . C15 C 0.1215(3) 0.3769(9) 0.4768(6) 0.175(4) Uani 1 1 d DU . . H15A H 0.1086 0.3191 0.4392 0.210 Uiso 1 1 calc R . . H15B H 0.1110 0.3727 0.5079 0.210 Uiso 1 1 calc R . . C16 C 0.1597(3) 0.3472(11) 0.5135(7) 0.186(6) Uani 1 1 d DU . . H16A H 0.1737 0.4217 0.5278 0.225 Uiso 1 1 calc R . . H16B H 0.1662 0.3015 0.4836 0.225 Uiso 1 1 calc R . . H16C H 0.1646 0.2986 0.5536 0.225 Uiso 1 1 calc R . . C18 C 0.14700(13) 0.8229(5) 0.5630(3) 0.0480(13) Uani 1 1 d . . . C19 C 0.15474(15) 0.7008(6) 0.5759(3) 0.0660(17) Uani 1 1 d . . . H19 H 0.1493 0.6481 0.5388 0.079 Uiso 1 1 calc R . . C20 C 0.1702(2) 0.6532(7) 0.6418(4) 0.091(2) Uani 1 1 d . . . H20 H 0.1747 0.5692 0.6490 0.109 Uiso 1 1 calc R . . C21 C 0.1790(2) 0.7305(8) 0.6967(4) 0.098(2) Uani 1 1 d . . . H21 H 0.1899 0.6992 0.7416 0.118 Uiso 1 1 calc R . . C22 C 0.17161(19) 0.8558(8) 0.6856(4) 0.085(2) Uani 1 1 d . . . H22 H 0.1771 0.9082 0.7228 0.102 Uiso 1 1 calc R . . C23 C 0.15607(15) 0.9020(6) 0.6187(3) 0.0598(15) Uani 1 1 d . . . C24 C 0.16266(19) 1.1137(7) 0.6563(4) 0.106(3) Uani 1 1 d . . . H24A H 0.1502 1.1913 0.6380 0.127 Uiso 1 1 calc R . . H24B H 0.1581 1.0887 0.6939 0.127 Uiso 1 1 calc R . . C25 C 0.2001(3) 1.1291(8) 0.6813(5) 0.141(4) Uani 1 1 d . . . H25A H 0.2125 1.0537 0.7021 0.212 Uiso 1 1 calc R . . H25B H 0.2089 1.1935 0.7154 0.212 Uiso 1 1 calc R . . H25C H 0.2047 1.1506 0.6436 0.212 Uiso 1 1 calc R . . C27 C 0.08569(13) 0.9622(5) 0.4528(3) 0.0446(13) Uani 1 1 d . . . C28 C 0.05921(14) 0.9201(5) 0.4699(3) 0.0479(13) Uani 1 1 d . . . C29 C 0.02512(15) 0.9796(6) 0.4425(3) 0.0621(16) Uani 1 1 d . . . H29 H 0.0071 0.9490 0.4521 0.075 Uiso 1 1 calc R . . C30 C 0.01813(17) 1.0819(6) 0.4017(3) 0.0720(18) Uani 1 1 d . . . H30 H -0.0042 1.1221 0.3852 0.086 Uiso 1 1 calc R . . C31 C 0.04365(18) 1.1250(6) 0.3852(4) 0.0756(19) Uani 1 1 d . . . H31 H 0.0388 1.1939 0.3570 0.091 Uiso 1 1 calc R . . C32 C 0.07726(16) 1.0644(5) 0.4113(3) 0.0589(15) Uani 1 1 d . . . H32 H 0.0947 1.0947 0.4000 0.071 Uiso 1 1 calc R . . C33 C 0.04276(18) 0.7679(6) 0.5295(4) 0.080(2) Uani 1 1 d . . . H33A H 0.0213 0.7405 0.4880 0.096 Uiso 1 1 calc R . . H33B H 0.0352 0.8283 0.5528 0.096 Uiso 1 1 calc R . . C34 C 0.0609(2) 0.6620(7) 0.5763(4) 0.102(3) Uani 1 1 d . . . H34A H 0.0698 0.6059 0.5540 0.153 Uiso 1 1 calc R . . H34B H 0.0436 0.6205 0.5864 0.153 Uiso 1 1 calc R . . H34C H 0.0810 0.6911 0.6187 0.153 Uiso 1 1 calc R . . C36 C 0.10455(13) 0.4685(4) 0.2932(2) 0.0428(12) Uani 1 1 d . . . C37 C 0.06669(14) 0.4510(5) 0.2676(3) 0.0492(13) Uani 1 1 d . . . H37 H 0.0517 0.5181 0.2621 0.059 Uiso 1 1 calc R . . C38 C 0.05194(16) 0.3346(6) 0.2509(3) 0.0623(16) Uani 1 1 d . . . H38 H 0.0269 0.3240 0.2330 0.075 Uiso 1 1 calc R . . C39 C 0.07374(19) 0.2345(6) 0.2601(3) 0.0702(18) Uani 1 1 d . . . H39 H 0.0635 0.1563 0.2489 0.084 Uiso 1 1 calc R . . C40 C 0.11086(19) 0.2492(5) 0.2859(3) 0.0728(18) Uani 1 1 d . . . H40 H 0.1257 0.1810 0.2925 0.087 Uiso 1 1 calc R . . C41 C 0.12625(16) 0.3666(5) 0.3021(3) 0.0587(15) Uani 1 1 d . . . H41 H 0.1513 0.3764 0.3191 0.070 Uiso 1 1 calc R . . C42 C 0.10095(13) 0.6994(5) 0.2284(3) 0.0466(13) Uani 1 1 d . . . C43 C 0.08862(16) 0.6341(6) 0.1661(3) 0.0670(17) Uani 1 1 d . . . H43 H 0.0915 0.5492 0.1677 0.080 Uiso 1 1 calc R . . C44 C 0.07208(18) 0.6929(8) 0.1018(3) 0.084(2) Uani 1 1 d . . . H44 H 0.0641 0.6476 0.0612 0.100 Uiso 1 1 calc R . . C45 C 0.06780(18) 0.8159(9) 0.0992(4) 0.089(2) Uani 1 1 d . . . H45 H 0.0565 0.8556 0.0564 0.107 Uiso 1 1 calc R . . C46 C 0.07997(19) 0.8827(7) 0.1590(5) 0.094(2) Uani 1 1 d . . . H46 H 0.0777 0.9679 0.1567 0.113 Uiso 1 1 calc R . . C47 C 0.09612(16) 0.8232(6) 0.2249(3) 0.0697(17) Uani 1 1 d . . . H47 H 0.1033 0.8689 0.2652 0.084 Uiso 1 1 calc R . . C48 C 0.17023(13) 0.6048(5) 0.3325(3) 0.0453(13) Uani 1 1 d . . . C49 C 0.18204(15) 0.6016(5) 0.2847(3) 0.0638(17) Uani 1 1 d . . . H49 H 0.1653 0.6067 0.2378 0.077 Uiso 1 1 calc R . . C50 C 0.21951(17) 0.5906(7) 0.3059(4) 0.086(2) Uani 1 1 d . . . H50 H 0.2273 0.5877 0.2726 0.103 Uiso 1 1 calc R . . C51 C 0.24396(18) 0.5843(7) 0.3727(4) 0.090(2) Uani 1 1 d . . . H51 H 0.2687 0.5798 0.3858 0.109 Uiso 1 1 calc R . . C52 C 0.23296(17) 0.5843(7) 0.4219(4) 0.089(2) Uani 1 1 d . . . H52 H 0.2499 0.5775 0.4687 0.107 Uiso 1 1 calc R . . C53 C 0.19640(16) 0.5946(5) 0.4012(3) 0.0684(17) Uani 1 1 d . . . H53 H 0.1889 0.5946 0.4349 0.082 Uiso 1 1 calc R . . 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 0.0401(4) 0.0433(4) 0.0454(4) -0.0046(3) 0.0238(3) -0.0050(3) O1 0.054(2) 0.055(2) 0.064(3) -0.0090(19) 0.038(2) -0.0143(19) O2 0.170(6) 0.047(3) 0.078(4) 0.005(2) 0.050(4) -0.015(3) O3 0.084(3) 0.071(3) 0.072(3) -0.030(2) 0.029(3) -0.008(3) O4 0.056(2) 0.067(3) 0.068(3) 0.007(2) 0.040(2) 0.002(2) P1 0.0407(8) 0.0461(8) 0.0499(9) -0.0086(7) 0.0248(7) -0.0069(6) P2 0.0376(8) 0.0450(8) 0.0393(8) 0.0013(6) 0.0188(7) 0.0024(6) C1 0.033(3) 0.049(3) 0.051(3) 0.006(3) 0.019(3) 0.002(2) C2 0.045(3) 0.049(3) 0.065(4) -0.012(3) 0.027(3) -0.015(3) C3 0.039(3) 0.062(4) 0.047(4) 0.010(3) 0.016(3) -0.009(3) C4 0.059(4) 0.098(5) 0.068(4) -0.006(4) 0.039(4) -0.018(4) C5 0.082(5) 0.151(8) 0.095(6) -0.006(5) 0.063(5) -0.031(5) C6 0.077(6) 0.149(9) 0.100(7) 0.021(6) 0.032(5) -0.060(6) C7 0.080(6) 0.096(6) 0.122(7) 0.020(5) 0.045(5) -0.023(5) C8 0.061(4) 0.062(4) 0.102(5) 0.014(4) 0.036(4) -0.008(3) C9 0.101(5) 0.055(4) 0.060(4) -0.028(3) 0.056(4) -0.034(4) C10 0.021(3) 0.163(7) 0.110(6) -0.099(5) 0.033(4) -0.040(4) C11 0.113(6) 0.148(7) 0.121(7) -0.049(6) 0.053(5) -0.012(6) C12 0.097(6) 0.152(8) 0.102(6) -0.042(6) 0.053(5) -0.033(6) C13 0.237(11) 0.101(7) 0.087(6) -0.055(5) 0.119(8) -0.100(7) C14 0.103(6) 0.113(7) 0.068(5) -0.035(5) 0.047(5) -0.019(6) C15 0.187(8) 0.116(7) 0.170(8) 0.017(6) 0.043(6) 0.001(6) C16 0.164(9) 0.131(8) 0.208(10) -0.025(7) 0.049(7) 0.037(7) C18 0.043(3) 0.055(4) 0.047(4) -0.008(3) 0.022(3) -0.008(3) C19 0.063(4) 0.079(5) 0.045(4) -0.008(3) 0.018(3) -0.008(3) C20 0.103(6) 0.085(5) 0.070(5) -0.002(4) 0.028(5) -0.003(4) C21 0.108(6) 0.119(7) 0.058(5) 0.007(5) 0.033(5) -0.011(5) C22 0.095(5) 0.108(6) 0.059(5) -0.025(4) 0.042(4) -0.018(5) C23 0.053(4) 0.074(5) 0.053(4) -0.006(3) 0.026(3) 0.001(3) C24 0.066(5) 0.121(7) 0.120(7) -0.062(5) 0.034(5) -0.011(5) C25 0.180(10) 0.110(7) 0.142(9) -0.035(6) 0.083(8) -0.030(7) C27 0.044(3) 0.045(3) 0.049(3) -0.013(3) 0.025(3) -0.006(2) C28 0.053(4) 0.049(3) 0.043(3) -0.011(3) 0.025(3) -0.005(3) C29 0.047(4) 0.081(5) 0.069(4) -0.013(3) 0.036(3) -0.002(3) C30 0.063(4) 0.075(5) 0.081(5) 0.009(4) 0.037(4) 0.024(4) C31 0.080(5) 0.056(4) 0.100(5) 0.019(4) 0.051(4) 0.023(4) C32 0.068(4) 0.049(4) 0.074(4) 0.000(3) 0.046(4) -0.001(3) C33 0.091(5) 0.091(5) 0.089(5) 0.005(4) 0.069(5) -0.004(4) C34 0.119(6) 0.110(6) 0.109(6) 0.033(5) 0.081(5) 0.004(5) C36 0.046(3) 0.045(3) 0.037(3) 0.001(2) 0.019(3) 0.002(3) C37 0.050(3) 0.052(4) 0.044(3) -0.002(3) 0.021(3) -0.002(3) C38 0.060(4) 0.068(4) 0.060(4) -0.009(3) 0.030(3) -0.013(3) C39 0.082(5) 0.051(4) 0.071(5) -0.008(3) 0.031(4) -0.015(4) C40 0.087(5) 0.049(4) 0.079(5) -0.003(3) 0.036(4) 0.007(4) C41 0.058(4) 0.049(4) 0.062(4) -0.004(3) 0.023(3) 0.001(3) C42 0.038(3) 0.056(4) 0.048(4) 0.009(3) 0.021(3) 0.007(3) C43 0.071(4) 0.074(4) 0.049(4) -0.003(3) 0.023(3) -0.005(3) C44 0.080(5) 0.115(6) 0.049(5) 0.011(4) 0.025(4) -0.009(5) C45 0.065(5) 0.125(7) 0.063(5) 0.032(5) 0.019(4) 0.011(5) C46 0.089(6) 0.074(5) 0.108(7) 0.042(5) 0.037(5) 0.028(4) C47 0.069(4) 0.066(4) 0.066(4) 0.016(3) 0.025(4) 0.017(3) C48 0.041(3) 0.048(3) 0.043(3) 0.000(2) 0.018(3) 0.003(2) C49 0.047(4) 0.090(5) 0.056(4) 0.001(3) 0.027(3) 0.009(3) C50 0.052(4) 0.122(6) 0.092(6) -0.003(5) 0.043(4) 0.014(4) C51 0.039(4) 0.117(6) 0.096(6) -0.005(5) 0.017(4) 0.013(4) C52 0.046(4) 0.124(6) 0.072(5) 0.009(4) 0.007(4) 0.026(4) C53 0.057(4) 0.084(5) 0.062(4) 0.006(3) 0.027(4) 0.011(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ni1 C9 1.898(6) . ? Ni1 O1 1.901(3) . ? Ni1 P1 2.1918(14) . ? Ni1 P2 2.2168(14) . ? O1 C1 1.306(6) . ? O2 C14 1.336(8) . ? O2 C15 1.432(10) . ? O3 C23 1.356(7) . ? O3 C24 1.429(7) . ? O4 C28 1.350(6) . ? O4 C33 1.438(6) . ? P1 C2 1.768(5) . ? P1 C27 1.813(5) . ? P1 C18 1.819(5) . ? P2 C48 1.818(5) . ? P2 C36 1.820(5) . ? P2 C42 1.823(5) . ? C1 C2 1.339(7) . ? C1 C3 1.490(6) . ? C2 H2 0.9300 . ? C3 C4 1.377(7) . ? C3 C8 1.380(8) . ? C4 C5 1.394(8) . ? C4 H4 0.9300 . ? C5 C6 1.399(11) . ? C5 H5 0.9300 . ? C6 C7 1.341(11) . ? C6 H6 0.9300 . ? C7 C8 1.354(8) . ? C7 H7 0.9300 . ? C8 H8 0.9300 . ? C9 C14 1.329(10) . ? C9 C10 1.452(9) . ? C10 C11 1.386(11) . ? C10 H10 0.9300 . ? C11 C12 1.277(12) . ? C11 H11 0.9300 . ? C12 C13 1.440(12) . ? C12 H12 0.9300 . ? C13 C14 1.511(10) . ? C13 H13 0.9300 . ? C15 C16 1.435(11) . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C16 H16A 0.9600 . ? C16 H16B 0.9600 . ? C16 H16C 0.9600 . ? C18 C19 1.363(8) . ? C18 C23 1.390(7) . ? C19 C20 1.371(8) . ? C19 H19 0.9300 . ? C20 C21 1.367(9) . ? C20 H20 0.9300 . ? C21 C22 1.392(9) . ? C21 H21 0.9300 . ? C22 C23 1.384(8) . ? C22 H22 0.9300 . ? C24 C25 1.393(9) . ? C24 H24A 0.9700 . ? C24 H24B 0.9700 . ? C25 H25A 0.9600 . ? C25 H25B 0.9600 . ? C25 H25C 0.9600 . ? C27 C32 1.373(7) . ? C27 C28 1.399(6) . ? C28 C29 1.406(7) . ? C29 C30 1.369(8) . ? C29 H29 0.9300 . ? C30 C31 1.357(8) . ? C30 H30 0.9300 . ? C31 C32 1.397(7) . ? C31 H31 0.9300 . ? C32 H32 0.9300 . ? C33 C34 1.486(8) . ? C33 H33A 0.9700 . ? C33 H33B 0.9700 . ? C34 H34A 0.9600 . ? C34 H34B 0.9600 . ? C34 H34C 0.9600 . ? C36 C41 1.383(7) . ? C36 C37 1.410(6) . ? C37 C38 1.377(7) . ? C37 H37 0.9300 . ? C38 C39 1.369(8) . ? C38 H38 0.9300 . ? C39 C40 1.377(8) . ? C39 H39 0.9300 . ? C40 C41 1.396(7) . ? C40 H40 0.9300 . ? C41 H41 0.9300 . ? C42 C47 1.358(8) . ? C42 C43 1.400(7) . ? C43 C44 1.394(8) . ? C43 H43 0.9300 . ? C44 C45 1.346(10) . ? C44 H44 0.9300 . ? C45 C46 1.369(10) . ? C45 H45 0.9300 . ? C46 C47 1.424(9) . ? C46 H46 0.9300 . ? C47 H47 0.9300 . ? C48 C49 1.352(7) . ? C48 C53 1.379(7) . ? C49 C50 1.404(7) . ? C49 H49 0.9300 . ? C50 C51 1.328(9) . ? C50 H50 0.9300 . ? C51 C52 1.358(9) . ? C51 H51 0.9300 . ? C52 C53 1.369(7) . ? C52 H52 0.9300 . ? C53 H53 0.9300 . ? 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 _geom_angle_publ_flag C9 Ni1 O1 172.1(2) . . ? C9 Ni1 P1 95.11(16) . . ? O1 Ni1 P1 85.82(11) . . ? C9 Ni1 P2 93.91(16) . . ? O1 Ni1 P2 85.28(11) . . ? P1 Ni1 P2 170.99(5) . . ? C1 O1 Ni1 120.1(3) . . ? C14 O2 C15 115.4(8) . . ? C23 O3 C24 120.3(5) . . ? C28 O4 C33 118.8(4) . . ? C2 P1 C27 107.5(2) . . ? C2 P1 C18 108.1(2) . . ? C27 P1 C18 109.1(2) . . ? C2 P1 Ni1 98.14(19) . . ? C27 P1 Ni1 114.40(16) . . ? C18 P1 Ni1 118.38(19) . . ? C48 P2 C36 103.5(2) . . ? C48 P2 C42 104.6(2) . . ? C36 P2 C42 103.0(2) . . ? C48 P2 Ni1 108.78(17) . . ? C36 P2 Ni1 124.22(16) . . ? C42 P2 Ni1 110.95(18) . . ? O1 C1 C2 121.6(5) . . ? O1 C1 C3 114.0(5) . . ? C2 C1 C3 124.4(5) . . ? C1 C2 P1 114.3(4) . . ? C1 C2 H2 122.9 . . ? P1 C2 H2 122.9 . . ? C4 C3 C8 118.0(5) . . ? C4 C3 C1 119.3(5) . . ? C8 C3 C1 122.7(5) . . ? C3 C4 C5 119.4(7) . . ? C3 C4 H4 120.3 . . ? C5 C4 H4 120.3 . . ? C4 C5 C6 118.8(7) . . ? C4 C5 H5 120.6 . . ? C6 C5 H5 120.6 . . ? C7 C6 C5 122.2(7) . . ? C7 C6 H6 118.9 . . ? C5 C6 H6 118.9 . . ? C6 C7 C8 117.3(8) . . ? C6 C7 H7 121.3 . . ? C8 C7 H7 121.3 . . ? C7 C8 C3 124.1(7) . . ? C7 C8 H8 117.9 . . ? C3 C8 H8 117.9 . . ? C14 C9 C10 121.2(7) . . ? C14 C9 Ni1 122.7(6) . . ? C10 C9 Ni1 115.7(5) . . ? C11 C10 C9 116.2(9) . . ? C11 C10 H10 121.9 . . ? C9 C10 H10 121.9 . . ? C12 C11 C10 119.7(11) . . ? C12 C11 H11 120.2 . . ? C10 C11 H11 120.2 . . ? C11 C12 C13 132.7(10) . . ? C11 C12 H12 113.6 . . ? C13 C12 H12 113.6 . . ? C12 C13 C14 105.3(8) . . ? C12 C13 H13 127.3 . . ? C14 C13 H13 127.3 . . ? C9 C14 O2 115.3(8) . . ? C9 C14 C13 124.8(9) . . ? O2 C14 C13 119.9(9) . . ? O2 C15 C16 107.6(10) . . ? O2 C15 H15A 110.2 . . ? C16 C15 H15A 110.2 . . ? O2 C15 H15B 110.2 . . ? C16 C15 H15B 110.2 . . ? H15A C15 H15B 108.5 . . ? C15 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C15 C16 H16C 109.4 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C19 C18 C23 118.7(5) . . ? C19 C18 P1 118.1(4) . . ? C23 C18 P1 123.1(5) . . ? C18 C19 C20 122.2(6) . . ? C18 C19 H19 118.9 . . ? C20 C19 H19 118.9 . . ? C21 C20 C19 119.3(7) . . ? C21 C20 H20 120.4 . . ? C19 C20 H20 120.4 . . ? C20 C21 C22 120.2(7) . . ? C20 C21 H21 119.9 . . ? C22 C21 H21 119.9 . . ? C23 C22 C21 119.5(6) . . ? C23 C22 H22 120.2 . . ? C21 C22 H22 120.2 . . ? O3 C23 C22 124.0(6) . . ? O3 C23 C18 116.0(5) . . ? C22 C23 C18 120.0(6) . . ? C25 C24 O3 110.3(6) . . ? C25 C24 H24A 109.6 . . ? O3 C24 H24A 109.6 . . ? C25 C24 H24B 109.6 . . ? O3 C24 H24B 109.6 . . ? H24A C24 H24B 108.1 . . ? C24 C25 H25A 109.5 . . ? C24 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C24 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C32 C27 C28 117.2(5) . . ? C32 C27 P1 120.0(4) . . ? C28 C27 P1 122.2(4) . . ? O4 C28 C27 115.1(5) . . ? O4 C28 C29 125.0(5) . . ? C27 C28 C29 119.8(5) . . ? C30 C29 C28 120.7(5) . . ? C30 C29 H29 119.7 . . ? C28 C29 H29 119.7 . . ? C31 C30 C29 120.3(6) . . ? C31 C30 H30 119.9 . . ? C29 C30 H30 119.9 . . ? C30 C31 C32 119.1(6) . . ? C30 C31 H31 120.5 . . ? C32 C31 H31 120.5 . . ? C27 C32 C31 122.8(5) . . ? C27 C32 H32 118.6 . . ? C31 C32 H32 118.6 . . ? O4 C33 C34 107.1(5) . . ? O4 C33 H33A 110.3 . . ? C34 C33 H33A 110.3 . . ? O4 C33 H33B 110.3 . . ? C34 C33 H33B 110.3 . . ? H33A C33 H33B 108.6 . . ? C33 C34 H34A 109.5 . . ? C33 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C33 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C41 C36 C37 118.6(5) . . ? C41 C36 P2 122.7(4) . . ? C37 C36 P2 118.8(4) . . ? C38 C37 C36 120.1(5) . . ? C38 C37 H37 120.0 . . ? C36 C37 H37 120.0 . . ? C39 C38 C37 120.8(6) . . ? C39 C38 H38 119.6 . . ? C37 C38 H38 119.6 . . ? C38 C39 C40 120.1(6) . . ? C38 C39 H39 119.9 . . ? C40 C39 H39 119.9 . . ? C39 C40 C41 119.9(6) . . ? C39 C40 H40 120.0 . . ? C41 C40 H40 120.0 . . ? C36 C41 C40 120.5(5) . . ? C36 C41 H41 119.8 . . ? C40 C41 H41 119.8 . . ? C47 C42 C43 118.1(5) . . ? C47 C42 P2 119.5(4) . . ? C43 C42 P2 122.4(4) . . ? C44 C43 C42 121.9(6) . . ? C44 C43 H43 119.1 . . ? C42 C43 H43 119.1 . . ? C45 C44 C43 119.4(7) . . ? C45 C44 H44 120.3 . . ? C43 C44 H44 120.3 . . ? C44 C45 C46 120.3(7) . . ? C44 C45 H45 119.8 . . ? C46 C45 H45 119.8 . . ? C45 C46 C47 120.7(7) . . ? C45 C46 H46 119.6 . . ? C47 C46 H46 119.6 . . ? C42 C47 C46 119.6(6) . . ? C42 C47 H47 120.2 . . ? C46 C47 H47 120.2 . . ? C49 C48 C53 117.0(5) . . ? C49 C48 P2 125.0(4) . . ? C53 C48 P2 118.0(4) . . ? C48 C49 C50 120.2(6) . . ? C48 C49 H49 119.9 . . ? C50 C49 H49 119.9 . . ? C51 C50 C49 121.0(6) . . ? C51 C50 H50 119.5 . . ? C49 C50 H50 119.5 . . ? C50 C51 C52 120.3(6) . . ? C50 C51 H51 119.8 . . ? C52 C51 H51 119.8 . . ? C51 C52 C53 118.6(6) . . ? C51 C52 H52 120.7 . . ? C53 C52 H52 120.7 . . ? C52 C53 C48 122.9(6) . . ? C52 C53 H53 118.6 . . ? C48 C53 H53 118.6 . . ? 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_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C9 Ni1 O1 C1 93.6(14) . . . . ? P1 Ni1 O1 C1 -3.4(4) . . . . ? P2 Ni1 O1 C1 178.0(4) . . . . ? C9 Ni1 P1 C2 -169.7(3) . . . . ? O1 Ni1 P1 C2 2.4(2) . . . . ? P2 Ni1 P1 C2 11.4(5) . . . . ? C9 Ni1 P1 C27 -56.3(3) . . . . ? O1 Ni1 P1 C27 115.9(2) . . . . ? P2 Ni1 P1 C27 124.8(4) . . . . ? C9 Ni1 P1 C18 74.5(3) . . . . ? O1 Ni1 P1 C18 -113.3(2) . . . . ? P2 Ni1 P1 C18 -104.4(4) . . . . ? C9 Ni1 P2 C48 -144.7(3) . . . . ? O1 Ni1 P2 C48 43.2(2) . . . . ? P1 Ni1 P2 C48 34.2(4) . . . . ? C9 Ni1 P2 C36 -22.8(3) . . . . ? O1 Ni1 P2 C36 165.1(2) . . . . ? P1 Ni1 P2 C36 156.1(4) . . . . ? C9 Ni1 P2 C42 100.8(3) . . . . ? O1 Ni1 P2 C42 -71.4(2) . . . . ? P1 Ni1 P2 C42 -80.3(4) . . . . ? Ni1 O1 C1 C2 3.3(7) . . . . ? Ni1 O1 C1 C3 -178.0(3) . . . . ? O1 C1 C2 P1 -0.6(7) . . . . ? C3 C1 C2 P1 -179.2(4) . . . . ? C27 P1 C2 C1 -120.5(4) . . . . ? C18 P1 C2 C1 121.8(4) . . . . ? Ni1 P1 C2 C1 -1.7(4) . . . . ? O1 C1 C3 C4 -21.8(7) . . . . ? C2 C1 C3 C4 156.9(6) . . . . ? O1 C1 C3 C8 158.1(5) . . . . ? C2 C1 C3 C8 -23.2(8) . . . . ? C8 C3 C4 C5 2.1(9) . . . . ? C1 C3 C4 C5 -178.0(5) . . . . ? C3 C4 C5 C6 -2.2(10) . . . . ? C4 C5 C6 C7 0.7(13) . . . . ? C5 C6 C7 C8 0.8(13) . . . . ? C6 C7 C8 C3 -0.9(12) . . . . ? C4 C3 C8 C7 -0.6(10) . . . . ? C1 C3 C8 C7 179.6(6) . . . . ? O1 Ni1 C9 C14 156.2(12) . . . . ? P1 Ni1 C9 C14 -107.4(5) . . . . ? P2 Ni1 C9 C14 72.5(5) . . . . ? O1 Ni1 C9 C10 -17.1(17) . . . . ? P1 Ni1 C9 C10 79.3(4) . . . . ? P2 Ni1 C9 C10 -100.9(4) . . . . ? C14 C9 C10 C11 4.2(9) . . . . ? Ni1 C9 C10 C11 177.7(5) . . . . ? C9 C10 C11 C12 -1.3(12) . . . . ? C10 C11 C12 C13 -1.8(17) . . . . ? C11 C12 C13 C14 1.8(14) . . . . ? C10 C9 C14 O2 175.9(5) . . . . ? Ni1 C9 C14 O2 2.9(9) . . . . ? C10 C9 C14 C13 -4.4(10) . . . . ? Ni1 C9 C14 C13 -177.4(5) . . . . ? C15 O2 C14 C9 -178.0(7) . . . . ? C15 O2 C14 C13 2.3(10) . . . . ? C12 C13 C14 C9 1.5(9) . . . . ? C12 C13 C14 O2 -178.8(7) . . . . ? C14 O2 C15 C16 -174.3(9) . . . . ? C2 P1 C18 C19 -116.0(4) . . . . ? C27 P1 C18 C19 127.4(4) . . . . ? Ni1 P1 C18 C19 -5.8(5) . . . . ? C2 P1 C18 C23 61.5(5) . . . . ? C27 P1 C18 C23 -55.1(5) . . . . ? Ni1 P1 C18 C23 171.7(4) . . . . ? C23 C18 C19 C20 1.8(9) . . . . ? P1 C18 C19 C20 179.4(5) . . . . ? C18 C19 C20 C21 -1.4(11) . . . . ? C19 C20 C21 C22 1.1(12) . . . . ? C20 C21 C22 C23 -1.3(11) . . . . ? C24 O3 C23 C22 11.1(9) . . . . ? C24 O3 C23 C18 -169.0(5) . . . . ? C21 C22 C23 O3 -178.3(6) . . . . ? C21 C22 C23 C18 1.7(10) . . . . ? C19 C18 C23 O3 178.1(5) . . . . ? P1 C18 C23 O3 0.6(7) . . . . ? C19 C18 C23 C22 -2.0(8) . . . . ? P1 C18 C23 C22 -179.5(5) . . . . ? C23 O3 C24 C25 73.2(9) . . . . ? C2 P1 C27 C32 25.2(5) . . . . ? C18 P1 C27 C32 142.2(4) . . . . ? Ni1 P1 C27 C32 -82.7(4) . . . . ? C2 P1 C27 C28 -163.6(4) . . . . ? C18 P1 C27 C28 -46.6(5) . . . . ? Ni1 P1 C27 C28 88.6(4) . . . . ? C33 O4 C28 C27 -177.2(5) . . . . ? C33 O4 C28 C29 1.5(8) . . . . ? C32 C27 C28 O4 -178.8(5) . . . . ? P1 C27 C28 O4 9.7(6) . . . . ? C32 C27 C28 C29 2.5(7) . . . . ? P1 C27 C28 C29 -169.0(4) . . . . ? O4 C28 C29 C30 178.3(5) . . . . ? C27 C28 C29 C30 -3.1(8) . . . . ? C28 C29 C30 C31 2.3(9) . . . . ? C29 C30 C31 C32 -0.9(10) . . . . ? C28 C27 C32 C31 -1.1(8) . . . . ? P1 C27 C32 C31 170.5(5) . . . . ? C30 C31 C32 C27 0.3(10) . . . . ? C28 O4 C33 C34 -179.5(5) . . . . ? C48 P2 C36 C41 7.2(5) . . . . ? C42 P2 C36 C41 115.9(4) . . . . ? Ni1 P2 C36 C41 -117.1(4) . . . . ? C48 P2 C36 C37 -172.8(4) . . . . ? C42 P2 C36 C37 -64.0(4) . . . . ? Ni1 P2 C36 C37 62.9(4) . . . . ? C41 C36 C37 C38 -1.3(7) . . . . ? P2 C36 C37 C38 178.6(4) . . . . ? C36 C37 C38 C39 1.5(8) . . . . ? C37 C38 C39 C40 -0.5(9) . . . . ? C38 C39 C40 C41 -0.6(10) . . . . ? C37 C36 C41 C40 0.2(8) . . . . ? P2 C36 C41 C40 -179.7(4) . . . . ? C39 C40 C41 C36 0.7(9) . . . . ? C48 P2 C42 C47 -98.0(5) . . . . ? C36 P2 C42 C47 154.1(4) . . . . ? Ni1 P2 C42 C47 19.1(5) . . . . ? C48 P2 C42 C43 82.2(5) . . . . ? C36 P2 C42 C43 -25.7(5) . . . . ? Ni1 P2 C42 C43 -160.7(4) . . . . ? C47 C42 C43 C44 0.5(9) . . . . ? P2 C42 C43 C44 -179.6(5) . . . . ? C42 C43 C44 C45 0.1(10) . . . . ? C43 C44 C45 C46 0.8(11) . . . . ? C44 C45 C46 C47 -2.3(11) . . . . ? C43 C42 C47 C46 -2.0(8) . . . . ? P2 C42 C47 C46 178.2(5) . . . . ? C45 C46 C47 C42 2.9(10) . . . . ? C36 P2 C48 C49 84.5(5) . . . . ? C42 P2 C48 C49 -23.1(6) . . . . ? Ni1 P2 C48 C49 -141.7(5) . . . . ? C36 P2 C48 C53 -96.6(5) . . . . ? C42 P2 C48 C53 155.8(4) . . . . ? Ni1 P2 C48 C53 37.2(5) . . . . ? C53 C48 C49 C50 -1.2(9) . . . . ? P2 C48 C49 C50 177.8(5) . . . . ? C48 C49 C50 C51 -0.6(11) . . . . ? C49 C50 C51 C52 2.1(12) . . . . ? C50 C51 C52 C53 -1.8(12) . . . . ? C51 C52 C53 C48 0.0(11) . . . . ? C49 C48 C53 C52 1.5(9) . . . . ? P2 C48 C53 C52 -177.5(5) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.50 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.606 _refine_diff_density_min -0.793 _refine_diff_density_rms 0.258 # Attachment 'cd201357.cif' data_cd201357 _database_code_depnum_ccdc_archive 'CCDC 847791' #TrackingRef 'cd201357.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C53 H54 Ni O4 P2' _chemical_formula_weight 875.61 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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 17.5838(15) _cell_length_b 13.0885(11) _cell_length_c 20.7174(18) _cell_angle_alpha 90.00 _cell_angle_beta 97.551(2) _cell_angle_gamma 90.00 _cell_volume 4726.7(7) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 2611 _cell_measurement_theta_min 4.505 _cell_measurement_theta_max 38.641 _exptl_crystal_description prismatic _exptl_crystal_colour green _exptl_crystal_size_max 0.223 _exptl_crystal_size_mid 0.215 _exptl_crystal_size_min 0.092 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.230 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1848 _exptl_absorpt_coefficient_mu 0.522 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.68879 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 24458 _diffrn_reflns_av_R_equivalents 0.0916 _diffrn_reflns_av_sigmaI/netI 0.1441 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.85 _diffrn_reflns_theta_max 25.50 _reflns_number_total 8783 _reflns_number_gt 4003 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0509P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8783 _refine_ls_number_parameters 547 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1187 _refine_ls_R_factor_gt 0.0555 _refine_ls_wR_factor_ref 0.1400 _refine_ls_wR_factor_gt 0.1275 _refine_ls_goodness_of_fit_ref 0.864 _refine_ls_restrained_S_all 0.864 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ni1 Ni 0.24815(3) 0.88247(4) 0.22015(3) 0.04640(19) Uani 1 1 d . . . P1 P 0.18236(7) 1.01969(9) 0.23429(5) 0.0482(3) Uani 1 1 d . . . P2 P 0.32101(7) 0.76141(9) 0.18448(6) 0.0507(3) Uani 1 1 d . . . O1 O 0.17138(16) 0.8539(2) 0.14871(13) 0.0596(9) Uani 1 1 d . . . O2 O 0.27028(19) 0.7657(3) 0.33842(14) 0.0646(9) Uani 1 1 d . . . O3 O 0.26709(19) 1.1736(2) 0.32549(16) 0.0769(10) Uani 1 1 d . . . O4 O 0.08427(18) 1.1916(2) 0.26333(15) 0.0682(9) Uani 1 1 d . . . C1 C 0.1124(3) 0.9162(3) 0.1365(2) 0.0483(11) Uani 1 1 d . . . C2 C 0.1063(2) 1.0020(3) 0.17042(19) 0.0520(12) Uani 1 1 d . . . H2 H 0.0660 1.0480 0.1613 0.062 Uiso 1 1 calc R . . C3 C 0.0529(2) 0.8821(3) 0.08261(19) 0.0471(11) Uani 1 1 d . . . C4 C 0.0692(3) 0.8031(4) 0.0419(2) 0.0599(13) Uani 1 1 d . . . H4 H 0.1168 0.7710 0.0491 0.072 Uiso 1 1 calc R . . C5 C 0.0159(3) 0.7711(4) -0.0093(2) 0.0723(15) Uani 1 1 d . . . H5 H 0.0279 0.7184 -0.0363 0.087 Uiso 1 1 calc R . . C6 C -0.0543(3) 0.8170(4) -0.0201(3) 0.0756(16) Uani 1 1 d . . . H6 H -0.0901 0.7955 -0.0544 0.091 Uiso 1 1 calc R . . C7 C -0.0718(3) 0.8945(4) 0.0195(3) 0.0739(15) Uani 1 1 d . . . H7 H -0.1196 0.9258 0.0120 0.089 Uiso 1 1 calc R . . C8 C -0.0190(3) 0.9266(4) 0.0704(2) 0.0641(14) Uani 1 1 d . . . H8 H -0.0319 0.9792 0.0972 0.077 Uiso 1 1 calc R . . C9 C 0.3232(3) 0.9056(3) 0.2920(2) 0.0536(12) Uani 1 1 d . . . C10 C 0.3788(3) 0.9799(4) 0.2956(3) 0.0818(17) Uani 1 1 d . . . H10 H 0.3775 1.0268 0.2617 0.098 Uiso 1 1 calc R . . C11 C 0.4364(4) 0.9878(5) 0.3473(4) 0.125(3) Uani 1 1 d . . . H11 H 0.4745 1.0371 0.3473 0.150 Uiso 1 1 calc R . . C12 C 0.4368(5) 0.9215(7) 0.3988(4) 0.132(3) Uani 1 1 d . . . H12 H 0.4753 0.9262 0.4340 0.159 Uiso 1 1 calc R . . C13 C 0.3804(4) 0.8479(5) 0.3988(3) 0.094(2) Uani 1 1 d . . . H13 H 0.3797 0.8047 0.4343 0.113 Uiso 1 1 calc R . . C14 C 0.3251(3) 0.8396(4) 0.3453(2) 0.0655(14) Uani 1 1 d . . . C15 C 0.2684(4) 0.6900(5) 0.3886(3) 0.0901(19) Uani 1 1 d . . . H15 H 0.3208 0.6693 0.4056 0.108 Uiso 1 1 calc R . . C16 C 0.2253(4) 0.6011(5) 0.3584(3) 0.129(3) Uani 1 1 d . . . H16A H 0.1724 0.6194 0.3471 0.193 Uiso 1 1 calc R . . H16B H 0.2293 0.5452 0.3886 0.193 Uiso 1 1 calc R . . H16C H 0.2464 0.5812 0.3198 0.193 Uiso 1 1 calc R . . C17 C 0.2284(4) 0.7327(5) 0.4438(3) 0.134(3) Uani 1 1 d . . . H17A H 0.2533 0.7946 0.4598 0.201 Uiso 1 1 calc R . . H17B H 0.2309 0.6836 0.4784 0.201 Uiso 1 1 calc R . . H17C H 0.1756 0.7468 0.4278 0.201 Uiso 1 1 calc R . . C18 C 0.2313(2) 1.1375(3) 0.2162(2) 0.0504(12) Uani 1 1 d . . . C19 C 0.2322(3) 1.1618(4) 0.1509(2) 0.0685(14) Uani 1 1 d . . . H19 H 0.2084 1.1183 0.1189 0.082 Uiso 1 1 calc R . . C20 C 0.2677(3) 1.2494(5) 0.1326(3) 0.0874(18) Uani 1 1 d . . . H20 H 0.2683 1.2644 0.0888 0.105 Uiso 1 1 calc R . . C21 C 0.3016(3) 1.3130(5) 0.1794(3) 0.0934(19) Uani 1 1 d . . . H21 H 0.3241 1.3730 0.1671 0.112 Uiso 1 1 calc R . . C22 C 0.3035(3) 1.2918(4) 0.2435(3) 0.0864(18) Uani 1 1 d . . . H22 H 0.3275 1.3366 0.2746 0.104 Uiso 1 1 calc R . . C23 C 0.2696(3) 1.2030(4) 0.2628(3) 0.0629(14) Uani 1 1 d . . . C24 C 0.3039(4) 1.2333(5) 0.3782(3) 0.109(2) Uani 1 1 d . . . H24 H 0.3544 1.2575 0.3697 0.131 Uiso 1 1 calc R . . C25 C 0.3099(4) 1.1598(6) 0.4356(3) 0.155(3) Uani 1 1 d . . . H25A H 0.2594 1.1403 0.4437 0.233 Uiso 1 1 calc R . . H25B H 0.3362 1.1927 0.4736 0.233 Uiso 1 1 calc R . . H25C H 0.3380 1.1001 0.4258 0.233 Uiso 1 1 calc R . . C26 C 0.2547(5) 1.3161(6) 0.3904(4) 0.178(4) Uani 1 1 d . . . H26A H 0.2319 1.3448 0.3498 0.267 Uiso 1 1 calc R . . H26B H 0.2840 1.3676 0.4156 0.267 Uiso 1 1 calc R . . H26C H 0.2150 1.2915 0.4141 0.267 Uiso 1 1 calc R . . C27 C 0.1382(2) 1.0407(3) 0.3075(2) 0.0456(11) Uani 1 1 d . . . C28 C 0.0889(2) 1.1234(4) 0.3134(2) 0.0528(12) Uani 1 1 d . . . C29 C 0.0520(3) 1.1333(4) 0.3676(2) 0.0687(14) Uani 1 1 d . . . H29 H 0.0200 1.1890 0.3713 0.082 Uiso 1 1 calc R . . C30 C 0.0623(3) 1.0613(4) 0.4162(2) 0.0713(15) Uani 1 1 d . . . H30 H 0.0372 1.0684 0.4527 0.086 Uiso 1 1 calc R . . C31 C 0.1095(3) 0.9788(4) 0.4111(2) 0.0663(14) Uani 1 1 d . . . H31 H 0.1159 0.9298 0.4439 0.080 Uiso 1 1 calc R . . C32 C 0.1475(2) 0.9691(3) 0.3570(2) 0.0532(12) Uani 1 1 d . . . H32 H 0.1798 0.9135 0.3539 0.064 Uiso 1 1 calc R . . C33 C 0.0329(3) 1.2778(4) 0.2601(2) 0.0707(15) Uani 1 1 d . . . H33 H 0.0313 1.3054 0.3038 0.085 Uiso 1 1 calc R . . C34 C -0.0452(4) 1.2392(5) 0.2325(3) 0.136(3) Uani 1 1 d . . . H34A H -0.0486 1.2355 0.1859 0.204 Uiso 1 1 calc R . . H34B H -0.0837 1.2851 0.2442 0.204 Uiso 1 1 calc R . . H34C H -0.0531 1.1725 0.2496 0.204 Uiso 1 1 calc R . . C35 C 0.0617(4) 1.3551(5) 0.2190(4) 0.156(3) Uani 1 1 d . . . H35A H 0.1129 1.3740 0.2369 0.234 Uiso 1 1 calc R . . H35B H 0.0291 1.4141 0.2170 0.234 Uiso 1 1 calc R . . H35C H 0.0621 1.3281 0.1759 0.234 Uiso 1 1 calc R . . C36 C 0.3947(3) 0.6930(4) 0.2377(2) 0.0558(13) Uani 1 1 d . . . C37 C 0.4588(3) 0.7435(4) 0.2677(3) 0.0846(17) Uani 1 1 d . . . H37 H 0.4661 0.8120 0.2582 0.102 Uiso 1 1 calc R . . C38 C 0.5125(3) 0.6936(6) 0.3118(3) 0.108(2) Uani 1 1 d . . . H38 H 0.5556 0.7283 0.3314 0.130 Uiso 1 1 calc R . . C39 C 0.5017(4) 0.5926(7) 0.3265(3) 0.113(3) Uani 1 1 d . . . H39 H 0.5373 0.5588 0.3562 0.135 Uiso 1 1 calc R . . C40 C 0.4391(4) 0.5425(5) 0.2975(3) 0.113(2) Uani 1 1 d . . . H40 H 0.4321 0.4741 0.3074 0.135 Uiso 1 1 calc R . . C41 C 0.3851(3) 0.5911(4) 0.2533(3) 0.0807(16) Uani 1 1 d . . . H41 H 0.3423 0.5554 0.2341 0.097 Uiso 1 1 calc R . . C42 C 0.2664(3) 0.6585(3) 0.1423(2) 0.0539(12) Uani 1 1 d . . . C43 C 0.2003(3) 0.6300(4) 0.1624(3) 0.0751(15) Uani 1 1 d . . . H43 H 0.1829 0.6652 0.1966 0.090 Uiso 1 1 calc R . . C44 C 0.1570(4) 0.5495(5) 0.1337(4) 0.107(2) Uani 1 1 d . . . H44 H 0.1118 0.5300 0.1492 0.129 Uiso 1 1 calc R . . C45 C 0.1815(6) 0.4993(6) 0.0826(4) 0.130(3) Uani 1 1 d . . . H45 H 0.1527 0.4458 0.0626 0.156 Uiso 1 1 calc R . . C46 C 0.2475(5) 0.5276(6) 0.0613(3) 0.119(3) Uani 1 1 d . . . H46 H 0.2639 0.4929 0.0265 0.143 Uiso 1 1 calc R . . C47 C 0.2913(4) 0.6070(4) 0.0900(3) 0.0871(17) Uani 1 1 d . . . H47 H 0.3367 0.6259 0.0747 0.104 Uiso 1 1 calc R . . C48 C 0.3725(3) 0.8176(4) 0.1223(2) 0.0608(13) Uani 1 1 d . . . C49 C 0.4395(3) 0.7788(5) 0.1043(3) 0.103(2) Uani 1 1 d . . . H49 H 0.4639 0.7243 0.1272 0.124 Uiso 1 1 calc R . . C50 C 0.4707(4) 0.8208(7) 0.0522(4) 0.134(3) Uani 1 1 d . . . H50 H 0.5159 0.7939 0.0405 0.161 Uiso 1 1 calc R . . C51 C 0.4363(5) 0.9009(7) 0.0177(3) 0.125(4) Uani 1 1 d . . . H51 H 0.4564 0.9273 -0.0181 0.150 Uiso 1 1 calc R . . C52 C 0.3719(5) 0.9409(5) 0.0371(3) 0.111(2) Uani 1 1 d . . . H52 H 0.3492 0.9978 0.0156 0.133 Uiso 1 1 calc R . . C53 C 0.3392(3) 0.8997(4) 0.0878(3) 0.0775(16) Uani 1 1 d . . . H53 H 0.2941 0.9276 0.0991 0.093 Uiso 1 1 calc R . . 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 0.0519(4) 0.0428(4) 0.0439(3) 0.0036(3) 0.0041(3) 0.0065(3) P1 0.0561(8) 0.0416(7) 0.0468(8) 0.0031(6) 0.0057(6) 0.0064(6) P2 0.0522(8) 0.0487(8) 0.0511(8) 0.0004(6) 0.0064(6) 0.0056(6) O1 0.058(2) 0.055(2) 0.061(2) -0.0075(16) -0.0076(16) 0.0200(17) O2 0.079(2) 0.065(2) 0.051(2) 0.0195(17) 0.0105(17) 0.013(2) O3 0.110(3) 0.068(2) 0.054(2) -0.0057(19) 0.013(2) -0.030(2) O4 0.083(2) 0.058(2) 0.069(2) 0.0191(18) 0.0284(19) 0.0313(19) C1 0.056(3) 0.051(3) 0.039(3) 0.009(2) 0.011(2) 0.007(2) C2 0.057(3) 0.048(3) 0.049(3) 0.002(2) 0.001(2) 0.016(2) C3 0.051(3) 0.050(3) 0.040(3) 0.002(2) 0.004(2) 0.000(3) C4 0.063(3) 0.065(4) 0.050(3) -0.001(3) 0.002(3) 0.009(3) C5 0.082(4) 0.073(4) 0.058(4) -0.011(3) -0.002(3) 0.001(3) C6 0.075(4) 0.080(4) 0.067(4) 0.002(3) -0.011(3) -0.008(3) C7 0.056(3) 0.080(4) 0.080(4) 0.001(3) -0.014(3) 0.007(3) C8 0.062(3) 0.065(4) 0.062(3) 0.002(3) -0.002(3) 0.011(3) C9 0.054(3) 0.043(3) 0.062(3) 0.000(2) 0.000(2) 0.008(2) C10 0.071(4) 0.062(4) 0.108(5) 0.005(3) -0.007(4) 0.004(3) C11 0.087(5) 0.093(6) 0.179(8) -0.027(5) -0.044(6) -0.005(4) C12 0.123(7) 0.127(7) 0.126(7) -0.039(5) -0.065(6) 0.027(6) C13 0.111(5) 0.104(5) 0.059(4) -0.011(3) -0.025(4) 0.013(4) C14 0.071(4) 0.066(4) 0.057(4) -0.005(3) -0.001(3) 0.013(3) C15 0.116(5) 0.092(5) 0.068(4) 0.041(4) 0.034(4) 0.044(4) C16 0.169(7) 0.078(5) 0.151(7) 0.053(5) 0.067(6) 0.015(5) C17 0.177(7) 0.155(7) 0.084(5) 0.050(4) 0.067(5) 0.088(5) C18 0.056(3) 0.050(3) 0.047(3) 0.010(2) 0.011(2) 0.013(2) C19 0.072(3) 0.067(4) 0.067(4) 0.020(3) 0.013(3) 0.010(3) C20 0.093(4) 0.098(5) 0.075(4) 0.044(4) 0.023(4) 0.000(4) C21 0.104(5) 0.074(5) 0.105(6) 0.026(4) 0.027(4) -0.018(4) C22 0.102(5) 0.065(4) 0.094(5) 0.011(3) 0.016(4) -0.030(3) C23 0.068(3) 0.051(3) 0.069(4) 0.005(3) 0.011(3) 0.000(3) C24 0.167(7) 0.095(5) 0.069(5) -0.018(4) 0.022(4) -0.039(5) C25 0.225(8) 0.163(7) 0.072(5) -0.010(5) -0.002(5) -0.060(6) C26 0.264(11) 0.126(7) 0.148(8) -0.063(6) 0.040(7) -0.006(7) C27 0.050(3) 0.041(3) 0.045(3) 0.001(2) 0.005(2) 0.000(2) C28 0.061(3) 0.047(3) 0.051(3) 0.002(3) 0.009(2) 0.004(3) C29 0.081(4) 0.060(4) 0.069(4) 0.004(3) 0.027(3) 0.024(3) C30 0.093(4) 0.067(4) 0.058(4) 0.003(3) 0.027(3) 0.007(3) C31 0.083(4) 0.062(4) 0.055(3) 0.007(3) 0.012(3) -0.004(3) C32 0.059(3) 0.044(3) 0.056(3) 0.001(2) 0.006(3) 0.001(2) C33 0.077(4) 0.063(4) 0.074(4) 0.013(3) 0.021(3) 0.032(3) C34 0.106(6) 0.134(7) 0.169(7) 0.044(5) 0.024(5) 0.042(5) C35 0.145(6) 0.087(5) 0.252(9) 0.089(6) 0.088(6) 0.043(4) C36 0.052(3) 0.061(4) 0.054(3) -0.005(3) 0.005(2) 0.016(3) C37 0.061(4) 0.089(4) 0.100(5) 0.002(4) -0.007(3) 0.011(3) C38 0.068(4) 0.142(7) 0.108(6) 0.007(5) -0.013(4) 0.019(5) C39 0.083(5) 0.161(8) 0.088(5) 0.012(5) -0.016(4) 0.053(5) C40 0.115(6) 0.094(5) 0.119(6) 0.029(4) -0.020(5) 0.037(5) C41 0.078(4) 0.069(4) 0.091(4) 0.008(3) -0.004(3) 0.018(3) C42 0.054(3) 0.049(3) 0.057(3) 0.002(2) -0.001(3) 0.010(3) C43 0.090(4) 0.045(3) 0.087(4) 0.003(3) 0.002(3) -0.006(3) C44 0.090(5) 0.080(5) 0.144(7) 0.029(5) -0.019(5) -0.019(4) C45 0.177(9) 0.065(5) 0.123(8) 0.019(5) -0.070(7) -0.025(6) C46 0.192(8) 0.083(6) 0.081(5) -0.022(4) 0.015(6) -0.009(6) C47 0.128(5) 0.064(4) 0.072(4) -0.010(3) 0.021(4) -0.010(4) C48 0.060(3) 0.064(4) 0.058(3) -0.007(3) 0.008(3) -0.013(3) C49 0.076(4) 0.142(6) 0.100(5) -0.008(4) 0.040(4) -0.007(4) C50 0.101(6) 0.213(10) 0.101(7) -0.027(6) 0.057(5) -0.051(6) C51 0.153(9) 0.167(9) 0.056(5) -0.011(5) 0.020(5) -0.100(7) C52 0.154(7) 0.105(6) 0.071(5) 0.011(4) 0.006(5) -0.064(5) C53 0.095(4) 0.068(4) 0.069(4) 0.005(3) 0.006(3) -0.023(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ni1 C9 1.881(5) . ? Ni1 O1 1.905(3) . ? Ni1 P1 2.1768(13) . ? Ni1 P2 2.2243(13) . ? P1 C2 1.768(4) . ? P1 C27 1.812(4) . ? P1 C18 1.828(5) . ? P2 C42 1.811(5) . ? P2 C36 1.822(5) . ? P2 C48 1.824(5) . ? O1 C1 1.317(4) . ? O2 C14 1.361(5) . ? O2 C15 1.440(5) . ? O3 C23 1.360(5) . ? O3 C24 1.426(6) . ? O4 C28 1.362(5) . ? O4 C33 1.441(5) . ? C1 C2 1.337(5) . ? C1 C3 1.494(6) . ? C2 H2 0.9300 . ? C3 C8 1.386(5) . ? C3 C4 1.388(6) . ? C4 C5 1.384(6) . ? C4 H4 0.9300 . ? C5 C6 1.364(6) . ? C5 H5 0.9300 . ? C6 C7 1.365(6) . ? C6 H6 0.9300 . ? C7 C8 1.376(6) . ? C7 H7 0.9300 . ? C8 H8 0.9300 . ? C9 C10 1.374(6) . ? C9 C14 1.398(6) . ? C10 C11 1.378(8) . ? C10 H10 0.9300 . ? C11 C12 1.375(9) . ? C11 H11 0.9300 . ? C12 C13 1.382(9) . ? C12 H12 0.9300 . ? C13 C14 1.378(6) . ? C13 H13 0.9300 . ? C15 C16 1.481(8) . ? C15 C17 1.524(7) . ? C15 H15 0.9800 . ? C16 H16A 0.9600 . ? C16 H16B 0.9600 . ? C16 H16C 0.9600 . ? C17 H17A 0.9600 . ? C17 H17B 0.9600 . ? C17 H17C 0.9600 . ? C18 C19 1.393(6) . ? C18 C23 1.397(6) . ? C19 C20 1.381(6) . ? C19 H19 0.9300 . ? C20 C21 1.357(7) . ? C20 H20 0.9300 . ? C21 C22 1.352(7) . ? C21 H21 0.9300 . ? C22 C23 1.389(6) . ? C22 H22 0.9300 . ? C24 C26 1.430(8) . ? C24 C25 1.523(8) . ? C24 H24 0.9800 . ? C25 H25A 0.9600 . ? C25 H25B 0.9600 . ? C25 H25C 0.9600 . ? C26 H26A 0.9600 . ? C26 H26B 0.9600 . ? C26 H26C 0.9600 . ? C27 C32 1.384(5) . ? C27 C28 1.403(5) . ? C28 C29 1.374(6) . ? C29 C30 1.374(6) . ? C29 H29 0.9300 . ? C30 C31 1.374(6) . ? C30 H30 0.9300 . ? C31 C32 1.384(5) . ? C31 H31 0.9300 . ? C32 H32 0.9300 . ? C33 C35 1.455(7) . ? C33 C34 1.503(7) . ? C33 H33 0.9800 . ? C34 H34A 0.9600 . ? C34 H34B 0.9600 . ? C34 H34C 0.9600 . ? C35 H35A 0.9600 . ? C35 H35B 0.9600 . ? C35 H35C 0.9600 . ? C36 C37 1.382(6) . ? C36 C41 1.388(6) . ? C37 C38 1.389(7) . ? C37 H37 0.9300 . ? C38 C39 1.376(8) . ? C38 H38 0.9300 . ? C39 C40 1.353(8) . ? C39 H39 0.9300 . ? C40 C41 1.383(7) . ? C40 H40 0.9300 . ? C41 H41 0.9300 . ? C42 C43 1.339(6) . ? C42 C47 1.393(6) . ? C43 C44 1.387(7) . ? C43 H43 0.9300 . ? C44 C45 1.362(9) . ? C44 H44 0.9300 . ? C45 C46 1.347(9) . ? C45 H45 0.9300 . ? C46 C47 1.382(8) . ? C46 H46 0.9300 . ? C47 H47 0.9300 . ? C48 C53 1.378(6) . ? C48 C49 1.379(6) . ? C49 C50 1.388(8) . ? C49 H49 0.9300 . ? C50 C51 1.365(10) . ? C50 H50 0.9300 . ? C51 C52 1.356(9) . ? C51 H51 0.9300 . ? C52 C53 1.372(7) . ? C52 H52 0.9300 . ? C53 H53 0.9300 . ? 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 _geom_angle_publ_flag C9 Ni1 O1 177.76(18) . . ? C9 Ni1 P1 95.20(13) . . ? O1 Ni1 P1 86.07(9) . . ? C9 Ni1 P2 90.17(13) . . ? O1 Ni1 P2 88.99(9) . . ? P1 Ni1 P2 166.40(5) . . ? C2 P1 C27 106.32(19) . . ? C2 P1 C18 106.7(2) . . ? C27 P1 C18 107.9(2) . . ? C2 P1 Ni1 98.89(15) . . ? C27 P1 Ni1 122.09(15) . . ? C18 P1 Ni1 113.29(14) . . ? C42 P2 C36 102.5(2) . . ? C42 P2 C48 103.8(2) . . ? C36 P2 C48 104.2(2) . . ? C42 P2 Ni1 113.49(16) . . ? C36 P2 Ni1 122.97(15) . . ? C48 P2 Ni1 107.99(18) . . ? C1 O1 Ni1 119.2(3) . . ? C14 O2 C15 119.8(4) . . ? C23 O3 C24 120.5(4) . . ? C28 O4 C33 121.5(3) . . ? O1 C1 C2 122.3(4) . . ? O1 C1 C3 114.5(4) . . ? C2 C1 C3 123.2(4) . . ? C1 C2 P1 113.5(3) . . ? C1 C2 H2 123.3 . . ? P1 C2 H2 123.3 . . ? C8 C3 C4 117.3(4) . . ? C8 C3 C1 122.9(4) . . ? C4 C3 C1 119.8(4) . . ? C5 C4 C3 121.2(4) . . ? C5 C4 H4 119.4 . . ? C3 C4 H4 119.4 . . ? C6 C5 C4 119.9(5) . . ? C6 C5 H5 120.0 . . ? C4 C5 H5 120.0 . . ? C5 C6 C7 120.0(5) . . ? C5 C6 H6 120.0 . . ? C7 C6 H6 120.0 . . ? C6 C7 C8 120.3(5) . . ? C6 C7 H7 119.8 . . ? C8 C7 H7 119.8 . . ? C7 C8 C3 121.2(5) . . ? C7 C8 H8 119.4 . . ? C3 C8 H8 119.4 . . ? C10 C9 C14 116.9(5) . . ? C10 C9 Ni1 125.2(4) . . ? C14 C9 Ni1 117.8(4) . . ? C9 C10 C11 122.6(6) . . ? C9 C10 H10 118.7 . . ? C11 C10 H10 118.7 . . ? C12 C11 C10 119.0(7) . . ? C12 C11 H11 120.5 . . ? C10 C11 H11 120.5 . . ? C11 C12 C13 120.6(7) . . ? C11 C12 H12 119.7 . . ? C13 C12 H12 119.7 . . ? C14 C13 C12 119.0(6) . . ? C14 C13 H13 120.5 . . ? C12 C13 H13 120.5 . . ? O2 C14 C13 123.7(5) . . ? O2 C14 C9 114.4(4) . . ? C13 C14 C9 121.8(5) . . ? O2 C15 C16 107.1(5) . . ? O2 C15 C17 110.2(4) . . ? C16 C15 C17 110.1(6) . . ? O2 C15 H15 109.8 . . ? C16 C15 H15 109.8 . . ? C17 C15 H15 109.8 . . ? C15 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C15 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C15 C17 H17A 109.5 . . ? C15 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C15 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C19 C18 C23 117.7(5) . . ? C19 C18 P1 117.3(4) . . ? C23 C18 P1 125.0(4) . . ? C20 C19 C18 121.4(5) . . ? C20 C19 H19 119.3 . . ? C18 C19 H19 119.3 . . ? C21 C20 C19 119.0(5) . . ? C21 C20 H20 120.5 . . ? C19 C20 H20 120.5 . . ? C22 C21 C20 121.9(6) . . ? C22 C21 H21 119.0 . . ? C20 C21 H21 119.0 . . ? C21 C22 C23 119.8(6) . . ? C21 C22 H22 120.1 . . ? C23 C22 H22 120.1 . . ? O3 C23 C22 125.5(5) . . ? O3 C23 C18 114.4(4) . . ? C22 C23 C18 120.1(5) . . ? O3 C24 C26 109.0(6) . . ? O3 C24 C25 103.3(5) . . ? C26 C24 C25 108.8(6) . . ? O3 C24 H24 111.8 . . ? C26 C24 H24 111.8 . . ? C25 C24 H24 111.8 . . ? C24 C25 H25A 109.5 . . ? C24 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C24 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C24 C26 H26A 109.5 . . ? C24 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C24 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C32 C27 C28 118.2(4) . . ? C32 C27 P1 119.7(3) . . ? C28 C27 P1 121.9(3) . . ? O4 C28 C29 124.9(4) . . ? O4 C28 C27 114.5(4) . . ? C29 C28 C27 120.5(4) . . ? C30 C29 C28 120.2(5) . . ? C30 C29 H29 119.9 . . ? C28 C29 H29 119.9 . . ? C29 C30 C31 120.4(5) . . ? C29 C30 H30 119.8 . . ? C31 C30 H30 119.8 . . ? C30 C31 C32 119.6(5) . . ? C30 C31 H31 120.2 . . ? C32 C31 H31 120.2 . . ? C27 C32 C31 121.1(4) . . ? C27 C32 H32 119.5 . . ? C31 C32 H32 119.5 . . ? O4 C33 C35 107.9(4) . . ? O4 C33 C34 106.9(4) . . ? C35 C33 C34 112.4(5) . . ? O4 C33 H33 109.8 . . ? C35 C33 H33 109.8 . . ? C34 C33 H33 109.8 . . ? C33 C34 H34A 109.5 . . ? C33 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C33 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C33 C35 H35A 109.5 . . ? C33 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C33 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? C37 C36 C41 118.1(5) . . ? C37 C36 P2 120.6(4) . . ? C41 C36 P2 121.0(4) . . ? C36 C37 C38 121.0(6) . . ? C36 C37 H37 119.5 . . ? C38 C37 H37 119.5 . . ? C39 C38 C37 119.8(7) . . ? C39 C38 H38 120.1 . . ? C37 C38 H38 120.1 . . ? C40 C39 C38 119.7(7) . . ? C40 C39 H39 120.1 . . ? C38 C39 H39 120.1 . . ? C39 C40 C41 121.2(7) . . ? C39 C40 H40 119.4 . . ? C41 C40 H40 119.4 . . ? C40 C41 C36 120.2(6) . . ? C40 C41 H41 119.9 . . ? C36 C41 H41 119.9 . . ? C43 C42 C47 118.8(5) . . ? C43 C42 P2 118.9(4) . . ? C47 C42 P2 122.3(4) . . ? C42 C43 C44 121.9(6) . . ? C42 C43 H43 119.1 . . ? C44 C43 H43 119.1 . . ? C45 C44 C43 119.1(7) . . ? C45 C44 H44 120.4 . . ? C43 C44 H44 120.4 . . ? C46 C45 C44 119.8(8) . . ? C46 C45 H45 120.1 . . ? C44 C45 H45 120.1 . . ? C45 C46 C47 121.4(8) . . ? C45 C46 H46 119.3 . . ? C47 C46 H46 119.3 . . ? C46 C47 C42 118.9(6) . . ? C46 C47 H47 120.5 . . ? C42 C47 H47 120.5 . . ? C53 C48 C49 117.9(5) . . ? C53 C48 P2 117.6(4) . . ? C49 C48 P2 124.3(5) . . ? C48 C49 C50 120.2(7) . . ? C48 C49 H49 119.9 . . ? C50 C49 H49 119.9 . . ? C51 C50 C49 121.2(8) . . ? C51 C50 H50 119.4 . . ? C49 C50 H50 119.4 . . ? C52 C51 C50 118.1(8) . . ? C52 C51 H51 120.9 . . ? C50 C51 H51 120.9 . . ? C51 C52 C53 121.7(8) . . ? C51 C52 H52 119.1 . . ? C53 C52 H52 119.1 . . ? C52 C53 C48 120.8(6) . . ? C52 C53 H53 119.6 . . ? C48 C53 H53 119.6 . . ? 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_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C9 Ni1 P1 C2 -177.3(2) . . . . ? O1 Ni1 P1 C2 0.91(17) . . . . ? P2 Ni1 P1 C2 69.9(3) . . . . ? C9 Ni1 P1 C27 -61.5(2) . . . . ? O1 Ni1 P1 C27 116.61(19) . . . . ? P2 Ni1 P1 C27 -174.4(2) . . . . ? C9 Ni1 P1 C18 70.2(2) . . . . ? O1 Ni1 P1 C18 -111.65(19) . . . . ? P2 Ni1 P1 C18 -42.7(3) . . . . ? C9 Ni1 P2 C42 147.5(2) . . . . ? O1 Ni1 P2 C42 -30.45(19) . . . . ? P1 Ni1 P2 C42 -99.1(3) . . . . ? C9 Ni1 P2 C36 23.3(3) . . . . ? O1 Ni1 P2 C36 -154.7(2) . . . . ? P1 Ni1 P2 C36 136.7(3) . . . . ? C9 Ni1 P2 C48 -98.0(2) . . . . ? O1 Ni1 P2 C48 84.09(18) . . . . ? P1 Ni1 P2 C48 15.5(3) . . . . ? C9 Ni1 O1 C1 122(4) . . . . ? P1 Ni1 O1 C1 -2.5(3) . . . . ? P2 Ni1 O1 C1 -169.8(3) . . . . ? Ni1 O1 C1 C2 3.7(5) . . . . ? Ni1 O1 C1 C3 -175.6(3) . . . . ? O1 C1 C2 P1 -2.6(6) . . . . ? C3 C1 C2 P1 176.7(3) . . . . ? C27 P1 C2 C1 -126.8(3) . . . . ? C18 P1 C2 C1 118.2(3) . . . . ? Ni1 P1 C2 C1 0.5(3) . . . . ? O1 C1 C3 C8 167.9(4) . . . . ? C2 C1 C3 C8 -11.4(7) . . . . ? O1 C1 C3 C4 -12.6(6) . . . . ? C2 C1 C3 C4 168.1(4) . . . . ? C8 C3 C4 C5 0.8(7) . . . . ? C1 C3 C4 C5 -178.7(4) . . . . ? C3 C4 C5 C6 -0.5(7) . . . . ? C4 C5 C6 C7 0.1(8) . . . . ? C5 C6 C7 C8 -0.1(8) . . . . ? C6 C7 C8 C3 0.5(8) . . . . ? C4 C3 C8 C7 -0.8(7) . . . . ? C1 C3 C8 C7 178.7(4) . . . . ? O1 Ni1 C9 C10 164(4) . . . . ? P1 Ni1 C9 C10 -71.6(4) . . . . ? P2 Ni1 C9 C10 95.9(4) . . . . ? O1 Ni1 C9 C14 -13(4) . . . . ? P1 Ni1 C9 C14 111.2(3) . . . . ? P2 Ni1 C9 C14 -81.3(3) . . . . ? C14 C9 C10 C11 2.9(8) . . . . ? Ni1 C9 C10 C11 -174.3(5) . . . . ? C9 C10 C11 C12 -2.8(10) . . . . ? C10 C11 C12 C13 0.1(12) . . . . ? C11 C12 C13 C14 2.2(11) . . . . ? C15 O2 C14 C13 -0.5(7) . . . . ? C15 O2 C14 C9 177.1(4) . . . . ? C12 C13 C14 O2 175.4(5) . . . . ? C12 C13 C14 C9 -2.0(8) . . . . ? C10 C9 C14 O2 -178.1(4) . . . . ? Ni1 C9 C14 O2 -0.7(5) . . . . ? C10 C9 C14 C13 -0.4(7) . . . . ? Ni1 C9 C14 C13 176.9(4) . . . . ? C14 O2 C15 C16 -158.7(5) . . . . ? C14 O2 C15 C17 81.5(6) . . . . ? C2 P1 C18 C19 -31.7(4) . . . . ? C27 P1 C18 C19 -145.6(3) . . . . ? Ni1 P1 C18 C19 76.0(3) . . . . ? C2 P1 C18 C23 150.3(4) . . . . ? C27 P1 C18 C23 36.4(4) . . . . ? Ni1 P1 C18 C23 -102.0(4) . . . . ? C23 C18 C19 C20 -2.0(7) . . . . ? P1 C18 C19 C20 179.9(4) . . . . ? C18 C19 C20 C21 -0.6(8) . . . . ? C19 C20 C21 C22 1.9(9) . . . . ? C20 C21 C22 C23 -0.5(9) . . . . ? C24 O3 C23 C22 -2.8(8) . . . . ? C24 O3 C23 C18 179.9(5) . . . . ? C21 C22 C23 O3 -179.3(5) . . . . ? C21 C22 C23 C18 -2.2(8) . . . . ? C19 C18 C23 O3 -179.2(4) . . . . ? P1 C18 C23 O3 -1.2(6) . . . . ? C19 C18 C23 C22 3.3(7) . . . . ? P1 C18 C23 C22 -178.7(4) . . . . ? C23 O3 C24 C26 82.0(7) . . . . ? C23 O3 C24 C25 -162.5(5) . . . . ? C2 P1 C27 C32 113.4(4) . . . . ? C18 P1 C27 C32 -132.5(4) . . . . ? Ni1 P1 C27 C32 1.5(4) . . . . ? C2 P1 C27 C28 -60.8(4) . . . . ? C18 P1 C27 C28 53.4(4) . . . . ? Ni1 P1 C27 C28 -172.7(3) . . . . ? C33 O4 C28 C29 -6.1(7) . . . . ? C33 O4 C28 C27 176.5(4) . . . . ? C32 C27 C28 O4 178.6(4) . . . . ? P1 C27 C28 O4 -7.1(5) . . . . ? C32 C27 C28 C29 1.1(6) . . . . ? P1 C27 C28 C29 175.3(4) . . . . ? O4 C28 C29 C30 -178.2(5) . . . . ? C27 C28 C29 C30 -0.9(7) . . . . ? C28 C29 C30 C31 0.0(8) . . . . ? C29 C30 C31 C32 0.7(7) . . . . ? C28 C27 C32 C31 -0.3(6) . . . . ? P1 C27 C32 C31 -174.7(3) . . . . ? C30 C31 C32 C27 -0.6(7) . . . . ? C28 O4 C33 C35 157.5(5) . . . . ? C28 O4 C33 C34 -81.4(5) . . . . ? C42 P2 C36 C37 165.2(4) . . . . ? C48 P2 C36 C37 57.3(4) . . . . ? Ni1 P2 C36 C37 -65.7(4) . . . . ? C42 P2 C36 C41 -20.1(5) . . . . ? C48 P2 C36 C41 -128.1(4) . . . . ? Ni1 P2 C36 C41 108.9(4) . . . . ? C41 C36 C37 C38 0.6(8) . . . . ? P2 C36 C37 C38 175.4(4) . . . . ? C36 C37 C38 C39 -0.6(9) . . . . ? C37 C38 C39 C40 0.4(11) . . . . ? C38 C39 C40 C41 -0.3(11) . . . . ? C39 C40 C41 C36 0.4(10) . . . . ? C37 C36 C41 C40 -0.5(8) . . . . ? P2 C36 C41 C40 -175.3(4) . . . . ? C36 P2 C42 C43 100.0(4) . . . . ? C48 P2 C42 C43 -151.7(4) . . . . ? Ni1 P2 C42 C43 -34.7(4) . . . . ? C36 P2 C42 C47 -79.3(4) . . . . ? C48 P2 C42 C47 29.0(5) . . . . ? Ni1 P2 C42 C47 146.0(4) . . . . ? C47 C42 C43 C44 1.5(8) . . . . ? P2 C42 C43 C44 -177.8(4) . . . . ? C42 C43 C44 C45 -1.5(9) . . . . ? C43 C44 C45 C46 0.8(11) . . . . ? C44 C45 C46 C47 -0.2(12) . . . . ? C45 C46 C47 C42 0.2(10) . . . . ? C43 C42 C47 C46 -0.8(8) . . . . ? P2 C42 C47 C46 178.4(4) . . . . ? C42 P2 C48 C53 93.9(4) . . . . ? C36 P2 C48 C53 -159.2(4) . . . . ? Ni1 P2 C48 C53 -26.9(4) . . . . ? C42 P2 C48 C49 -81.3(5) . . . . ? C36 P2 C48 C49 25.7(5) . . . . ? Ni1 P2 C48 C49 157.9(4) . . . . ? C53 C48 C49 C50 -1.4(8) . . . . ? P2 C48 C49 C50 173.8(5) . . . . ? C48 C49 C50 C51 0.1(11) . . . . ? C49 C50 C51 C52 2.2(12) . . . . ? C50 C51 C52 C53 -3.3(11) . . . . ? C51 C52 C53 C48 2.1(9) . . . . ? C49 C48 C53 C52 0.3(8) . . . . ? P2 C48 C53 C52 -175.2(4) . . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.50 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.687 _refine_diff_density_min -0.213 _refine_diff_density_rms 0.059 # Attachment 'cu_dm11125_0m.cif' data_cu_dm11125_0m _database_code_depnum_ccdc_archive 'CCDC 847792' #TrackingRef 'cu_dm11125_0m.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C65 H80 Ni O4 P2' _chemical_formula_weight 1045.94 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni -3.0029 0.5091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_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' _cell_length_a 14.5218(3) _cell_length_b 23.7365(5) _cell_length_c 18.5141(4) _cell_angle_alpha 90.00 _cell_angle_beta 112.5510(10) _cell_angle_gamma 90.00 _cell_volume 5893.8(2) _cell_formula_units_Z 4 _cell_measurement_temperature 133(2) _cell_measurement_reflns_used 9891 _cell_measurement_theta_min 6.365 _cell_measurement_theta_max 135.174 _exptl_crystal_description prismatic _exptl_crystal_colour colorless _exptl_crystal_size_max 0.203 _exptl_crystal_size_mid 0.126 _exptl_crystal_size_min 0.095 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.179 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2240 _exptl_absorpt_coefficient_mu 1.332 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6454 _exptl_absorpt_correction_T_max 0.7456 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 133(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 39123 _diffrn_reflns_av_R_equivalents 0.0240 _diffrn_reflns_av_sigmaI/netI 0.0198 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -27 _diffrn_reflns_limit_k_max 28 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 3.19 _diffrn_reflns_theta_max 67.48 _reflns_number_total 10463 _reflns_number_gt 9376 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0930P)^2^+6.3348P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10463 _refine_ls_number_parameters 624 _refine_ls_number_restraints 7 _refine_ls_R_factor_all 0.0569 _refine_ls_R_factor_gt 0.0521 _refine_ls_wR_factor_ref 0.1592 _refine_ls_wR_factor_gt 0.1524 _refine_ls_goodness_of_fit_ref 1.026 _refine_ls_restrained_S_all 1.040 _refine_ls_shift/su_max 0.034 _refine_ls_shift/su_mean 0.002 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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ni1 Ni 0.18485(3) 0.178938(16) 0.13534(2) 0.02491(13) Uani 1 1 d . . . O1 O 0.11836(13) 0.21544(7) 0.19265(10) 0.0330(4) Uani 1 1 d . . . O2 O 0.37218(12) 0.21727(7) 0.13029(10) 0.0328(4) Uani 1 1 d . . . O3 O 0.30240(13) 0.01209(7) 0.16577(10) 0.0351(4) Uani 1 1 d . . . O4 O 0.27337(13) 0.03483(7) 0.35772(9) 0.0322(4) Uani 1 1 d . . . P1 P 0.21107(4) 0.11022(2) 0.21888(3) 0.02483(15) Uani 1 1 d . . . P2 P 0.12421(4) 0.24732(2) 0.04924(3) 0.02466(15) Uani 1 1 d . . . C1 C 0.11152(17) 0.19065(10) 0.25379(13) 0.0280(5) Uani 1 1 d . . . C2 C 0.14613(18) 0.13744(11) 0.27504(14) 0.0305(5) Uani 1 1 d . . . H2 H 0.1365 0.1170 0.3157 0.037 Uiso 1 1 calc R . . C3 C 0.06581(18) 0.22634(11) 0.29698(15) 0.0315(5) Uani 1 1 d . . . C4 C 0.0610(2) 0.20984(13) 0.36756(18) 0.0472(7) Uani 1 1 d . . . H4 H 0.0860 0.1740 0.3889 0.057 Uiso 1 1 calc R . . C5 C 0.0202(3) 0.24492(16) 0.4069(2) 0.0644(10) Uani 1 1 d . . . H5 H 0.0175 0.2330 0.4551 0.077 Uiso 1 1 calc R . . C6 C -0.0165(3) 0.29665(15) 0.3774(2) 0.0608(9) Uani 1 1 d . . . H6 H -0.0457 0.3203 0.4042 0.073 Uiso 1 1 calc R . . C7 C -0.0107(3) 0.31428(14) 0.3082(2) 0.0522(8) Uani 1 1 d . . . H7 H -0.0343 0.3506 0.2881 0.063 Uiso 1 1 calc R . . C8 C 0.0293(2) 0.27936(12) 0.26815(17) 0.0400(6) Uani 1 1 d . . . H8 H 0.0320 0.2917 0.2202 0.048 Uiso 1 1 calc R . . C9 C 0.25281(17) 0.14659(10) 0.07652(13) 0.0266(5) Uani 1 1 d . . . C10 C 0.21782(19) 0.10116(11) 0.02516(14) 0.0322(5) Uani 1 1 d . . . H10 H 0.1580 0.0829 0.0215 0.039 Uiso 1 1 calc R . . C11 C 0.2680(2) 0.08189(12) -0.02072(15) 0.0396(6) Uani 1 1 d . . . H11 H 0.2416 0.0515 -0.0560 0.047 Uiso 1 1 calc R . . C12 C 0.3564(2) 0.10711(13) -0.01478(16) 0.0416(6) Uani 1 1 d . . . H12 H 0.3913 0.0937 -0.0455 0.050 Uiso 1 1 calc R . . C13 C 0.3941(2) 0.15200(12) 0.03595(15) 0.0376(6) Uani 1 1 d . . . H13 H 0.4552 0.1692 0.0405 0.045 Uiso 1 1 calc R . . C14 C 0.34206(18) 0.17167(10) 0.07995(14) 0.0298(5) Uani 1 1 d . . . C15 C 0.4562(2) 0.24897(12) 0.13147(17) 0.0394(6) Uani 1 1 d . . . H15A H 0.4451 0.2628 0.0783 0.047 Uiso 1 1 calc R . . H15B H 0.5168 0.2252 0.1499 0.047 Uiso 1 1 calc R . . C16 C 0.4689(2) 0.29837(13) 0.18675(18) 0.0426(6) Uani 1 1 d . . . H16A H 0.4827 0.2839 0.2400 0.051 Uiso 1 1 calc R . . H16B H 0.4059 0.3201 0.1697 0.051 Uiso 1 1 calc R . . C17 C 0.5535(2) 0.33742(14) 0.18925(18) 0.0465(7) Uani 1 1 d . . . H17A H 0.5381 0.3532 0.1364 0.056 Uiso 1 1 calc R . . H17B H 0.6157 0.3152 0.2036 0.056 Uiso 1 1 calc R . . C18 C 0.5710(3) 0.38590(14) 0.24727(19) 0.0510(8) Uani 1 1 d . . . H18A H 0.5089 0.4082 0.2329 0.061 Uiso 1 1 calc R . . H18B H 0.5866 0.3702 0.3002 0.061 Uiso 1 1 calc R . . C19 C 0.6548(3) 0.42436(18) 0.2493(2) 0.0731(11) Uani 1 1 d . . . H19A H 0.7175 0.4032 0.2674 0.110 Uiso 1 1 calc R . . H19B H 0.6605 0.4557 0.2851 0.110 Uiso 1 1 calc R . . H19C H 0.6409 0.4391 0.1967 0.110 Uiso 1 1 calc R . . C20 C 0.15455(18) 0.04327(11) 0.17698(13) 0.0307(5) Uani 1 1 d . . . C21 C 0.0543(2) 0.03476(13) 0.16304(16) 0.0415(6) Uani 1 1 d . . . H21 H 0.0191 0.0622 0.1798 0.050 Uiso 1 1 calc R . . C22 C 0.0048(2) -0.01360(15) 0.1247(2) 0.0543(8) Uani 1 1 d . . . H22 H -0.0635 -0.0191 0.1157 0.065 Uiso 1 1 calc R . . C23 C 0.0548(2) -0.05313(14) 0.09996(19) 0.0529(8) Uani 1 1 d . . . H23 H 0.0209 -0.0860 0.0738 0.064 Uiso 1 1 calc R . . C24 C 0.1542(2) -0.04570(12) 0.11261(17) 0.0435(7) Uani 1 1 d . . . H24 H 0.1884 -0.0733 0.0952 0.052 Uiso 1 1 calc R . . C25 C 0.20405(19) 0.00234(11) 0.15086(14) 0.0331(5) Uani 1 1 d . . . C26 C 0.3506(2) -0.02268(12) 0.12662(16) 0.0426(6) Uani 1 1 d . . . H26A H 0.3121 -0.0221 0.0694 0.051 Uiso 1 1 calc R . . H26B H 0.3549 -0.0621 0.1451 0.051 Uiso 1 1 calc R . . C27 C 0.4536(2) 0.00087(14) 0.14537(18) 0.0469(7) Uani 1 1 d . . . H27A H 0.4479 0.0416 0.1328 0.056 Uiso 1 1 calc R . . H27B H 0.4830 -0.0177 0.1113 0.056 Uiso 1 1 calc R . . C28 C 0.5241(2) -0.00676(13) 0.23026(17) 0.0430(6) Uani 1 1 d . . . H28A H 0.4946 0.0115 0.2645 0.052 Uiso 1 1 calc R . . H28B H 0.5308 -0.0475 0.2427 0.052 Uiso 1 1 calc R . . C29 C 0.6269(2) 0.01769(16) 0.2482(2) 0.0591(9) Uani 1 1 d . . . H29A H 0.6205 0.0587 0.2379 0.071 Uiso 1 1 calc R . . H29B H 0.6551 0.0007 0.2124 0.071 Uiso 1 1 calc R . . C30 C 0.6989(3) 0.0079(2) 0.3322(2) 0.0730(11) Uani 1 1 d . . . H30A H 0.6725 0.0256 0.3681 0.110 Uiso 1 1 calc R . . H30B H 0.7638 0.0246 0.3399 0.110 Uiso 1 1 calc R . . H30C H 0.7069 -0.0326 0.3426 0.110 Uiso 1 1 calc R . . C31 C 0.33685(17) 0.09660(10) 0.28865(13) 0.0257(5) Uani 1 1 d . . . C32 C 0.41614(18) 0.12500(10) 0.28106(14) 0.0293(5) Uani 1 1 d . . . H32 H 0.4047 0.1480 0.2364 0.035 Uiso 1 1 calc R . . C33 C 0.51219(19) 0.12038(11) 0.33769(15) 0.0334(5) Uani 1 1 d . . . H33 H 0.5662 0.1394 0.3314 0.040 Uiso 1 1 calc R . . C34 C 0.52798(19) 0.08787(11) 0.40313(15) 0.0361(6) Uani 1 1 d . . . H34 H 0.5931 0.0854 0.4427 0.043 Uiso 1 1 calc R . . C35 C 0.45022(19) 0.05869(11) 0.41192(14) 0.0334(5) Uani 1 1 d . . . H35 H 0.4623 0.0362 0.4571 0.040 Uiso 1 1 calc R . . C36 C 0.35459(18) 0.06236(10) 0.35463(13) 0.0284(5) Uani 1 1 d . . . C37 C 0.2866(2) 0.00238(11) 0.42631(15) 0.0362(6) Uani 1 1 d . . . H37A H 0.3027 0.0276 0.4722 0.043 Uiso 1 1 calc R . . H37B H 0.3423 -0.0245 0.4368 0.043 Uiso 1 1 calc R . . C38 C 0.1909(2) -0.02918(12) 0.41259(17) 0.0425(6) Uani 1 1 d . . . H38A H 0.2009 -0.0524 0.4594 0.051 Uiso 1 1 calc R . . H38B H 0.1786 -0.0553 0.3682 0.051 Uiso 1 1 calc R . . C39 C 0.0976(2) 0.00661(12) 0.39544(17) 0.0431(6) Uani 1 1 d . . . H39A H 0.0825 0.0266 0.3452 0.052 Uiso 1 1 calc R . . H39B H 0.0408 -0.0187 0.3890 0.052 Uiso 1 1 calc R . . C40 C 0.1060(2) 0.04947(13) 0.45783(19) 0.0471(7) Uani 1 1 d . . . H40A H 0.1531 0.0794 0.4570 0.057 Uiso 1 1 calc R . . H40B H 0.1339 0.0309 0.5097 0.057 Uiso 1 1 calc R . . C41 C 0.0059(3) 0.07648(16) 0.4472(3) 0.0669(10) Uani 1 1 d . . . H41A H -0.0241 0.0930 0.3948 0.100 Uiso 1 1 calc R . . H41B H 0.0165 0.1060 0.4866 0.100 Uiso 1 1 calc R . . H41C H -0.0389 0.0477 0.4535 0.100 Uiso 1 1 calc R . . C42 C -0.00417(18) 0.23013(10) -0.01376(14) 0.0299(5) Uani 1 1 d . . . C43 C -0.0557(2) 0.19254(11) 0.01456(16) 0.0360(6) Uani 1 1 d . . . H43 H -0.0233 0.1757 0.0645 0.043 Uiso 1 1 calc R . . C44 C -0.1547(2) 0.17962(13) -0.03013(19) 0.0469(7) Uani 1 1 d . . . H44 H -0.1897 0.1540 -0.0105 0.056 Uiso 1 1 calc R . . C45 C -0.2022(2) 0.20367(13) -0.1025(2) 0.0529(8) Uani 1 1 d . . . H45 H -0.2699 0.1947 -0.1329 0.063 Uiso 1 1 calc R . . C46 C -0.1514(2) 0.24101(13) -0.13096(19) 0.0550(9) Uani 1 1 d . . . H46 H -0.1842 0.2577 -0.1810 0.066 Uiso 1 1 calc R . . C47 C -0.0528(2) 0.25435(12) -0.08710(17) 0.0443(7) Uani 1 1 d . . . H47 H -0.0183 0.2801 -0.1071 0.053 Uiso 1 1 calc R . . C48 C 0.11755(18) 0.31279(10) 0.09898(13) 0.0272(5) Uani 1 1 d . . . C49 C 0.0346(2) 0.34792(10) 0.07554(15) 0.0328(5) Uani 1 1 d . . . H49 H -0.0233 0.3385 0.0312 0.039 Uiso 1 1 calc R . . C50 C 0.0370(2) 0.39688(12) 0.11737(16) 0.0402(6) Uani 1 1 d . . . H50 H -0.0201 0.4206 0.1021 0.048 Uiso 1 1 calc R . . C51 C 0.1220(2) 0.41141(12) 0.18137(16) 0.0416(6) Uani 1 1 d . . . H51 H 0.1239 0.4455 0.2088 0.050 Uiso 1 1 calc R . . C52 C 0.2037(2) 0.37634(12) 0.20501(15) 0.0391(6) Uani 1 1 d . . . H52 H 0.2620 0.3862 0.2489 0.047 Uiso 1 1 calc R . . C53 C 0.2012(2) 0.32654(11) 0.16484(15) 0.0331(5) Uani 1 1 d . . . H53 H 0.2569 0.3018 0.1825 0.040 Uiso 1 1 calc R . . C54 C 0.18243(18) 0.26861(10) -0.01821(13) 0.0286(5) Uani 1 1 d . . . C55 C 0.23399(19) 0.31894(11) -0.00925(15) 0.0323(5) Uani 1 1 d . . . H55 H 0.2375 0.3440 0.0318 0.039 Uiso 1 1 calc R . . C56 C 0.2806(2) 0.33306(13) -0.05975(18) 0.0425(6) Uani 1 1 d . . . H56 H 0.3156 0.3677 -0.0532 0.051 Uiso 1 1 calc R . . C57 C 0.2760(2) 0.29693(15) -0.11931(18) 0.0508(8) Uani 1 1 d . . . H57 H 0.3072 0.3069 -0.1542 0.061 Uiso 1 1 calc R . . C58 C 0.2262(3) 0.24644(14) -0.12818(18) 0.0537(8) Uani 1 1 d . . . H58 H 0.2240 0.2213 -0.1687 0.064 Uiso 1 1 calc R . . C59 C 0.1792(2) 0.23211(12) -0.07820(15) 0.0424(6) Uani 1 1 d . . . H59 H 0.1446 0.1973 -0.0848 0.051 Uiso 1 1 calc R . . C60 C 0.7747(12) 0.0841(5) 0.1372(10) 0.315(8) Uiso 1 1 d D . . H60A H 0.7297 0.0533 0.1374 0.472 Uiso 1 1 calc R . . H60B H 0.8279 0.0875 0.1892 0.472 Uiso 1 1 calc R . . H60C H 0.8040 0.0761 0.0986 0.472 Uiso 1 1 calc R . . C61 C 0.7158(9) 0.1395(5) 0.1159(7) 0.221(5) Uiso 1 1 d D . . H61A H 0.6953 0.1495 0.0600 0.266 Uiso 1 1 calc RD . . H61B H 0.6574 0.1399 0.1311 0.266 Uiso 1 1 calc R . . C62 C 0.8007(8) 0.1745(4) 0.1686(6) 0.180(4) Uiso 1 1 d D . . H62A H 0.8630 0.1686 0.1597 0.216 Uiso 1 1 calc R . . H62B H 0.8131 0.1693 0.2247 0.216 Uiso 1 1 calc R . . C63 C 0.7503(9) 0.2308(4) 0.1361(7) 0.204(4) Uiso 1 1 d D . . H63A H 0.6839 0.2207 0.0967 0.245 Uiso 1 1 calc RD . . H63B H 0.7379 0.2487 0.1799 0.245 Uiso 1 1 calc R . . C64 C 0.7842(8) 0.2735(5) 0.1027(6) 0.186(4) Uiso 1 1 d D . . H64A H 0.8574 0.2726 0.1318 0.224 Uiso 1 1 calc R . . H64B H 0.7732 0.2588 0.0500 0.224 Uiso 1 1 calc R . . C65 C 0.7632(7) 0.3301(4) 0.0901(6) 0.174(4) Uiso 1 1 d D . . H65A H 0.6914 0.3360 0.0744 0.261 Uiso 1 1 calc R . . H65B H 0.7840 0.3434 0.0486 0.261 Uiso 1 1 calc R . . H65C H 0.7993 0.3510 0.1384 0.261 Uiso 1 1 calc R . . 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 0.0283(2) 0.0245(2) 0.0224(2) 0.00506(15) 0.01019(17) 0.00260(15) O1 0.0436(10) 0.0306(9) 0.0311(9) 0.0096(7) 0.0214(8) 0.0092(7) O2 0.0320(9) 0.0341(9) 0.0327(9) -0.0009(7) 0.0126(7) -0.0077(7) O3 0.0372(9) 0.0310(9) 0.0352(9) -0.0048(7) 0.0117(8) 0.0021(7) O4 0.0371(9) 0.0300(9) 0.0268(8) 0.0089(7) 0.0094(7) 0.0025(7) P1 0.0274(3) 0.0239(3) 0.0224(3) 0.0046(2) 0.0087(2) 0.0021(2) P2 0.0296(3) 0.0216(3) 0.0214(3) 0.0028(2) 0.0083(2) 0.0002(2) C1 0.0271(11) 0.0310(12) 0.0265(11) 0.0047(9) 0.0112(9) 0.0010(9) C2 0.0346(12) 0.0327(13) 0.0285(12) 0.0081(10) 0.0169(10) 0.0042(10) C3 0.0302(12) 0.0322(13) 0.0357(13) 0.0028(10) 0.0168(10) -0.0004(10) C4 0.0668(19) 0.0413(16) 0.0488(16) 0.0112(13) 0.0390(15) 0.0110(14) C5 0.098(3) 0.062(2) 0.061(2) 0.0140(17) 0.061(2) 0.019(2) C6 0.083(2) 0.054(2) 0.068(2) 0.0006(17) 0.055(2) 0.0168(18) C7 0.066(2) 0.0400(16) 0.063(2) 0.0081(14) 0.0392(17) 0.0175(14) C8 0.0456(15) 0.0384(15) 0.0430(15) 0.0083(12) 0.0248(12) 0.0094(12) C9 0.0302(11) 0.0260(11) 0.0220(10) 0.0050(9) 0.0083(9) 0.0018(9) C10 0.0356(13) 0.0324(13) 0.0270(12) 0.0019(10) 0.0103(10) -0.0017(10) C11 0.0531(16) 0.0368(14) 0.0301(13) -0.0035(11) 0.0174(12) -0.0007(12) C12 0.0505(16) 0.0459(16) 0.0366(14) 0.0002(12) 0.0258(12) 0.0046(13) C13 0.0364(13) 0.0439(15) 0.0362(13) 0.0048(12) 0.0182(11) -0.0004(11) C14 0.0319(12) 0.0317(13) 0.0254(11) 0.0050(10) 0.0106(10) 0.0012(10) C15 0.0330(13) 0.0408(15) 0.0451(15) 0.0032(12) 0.0159(12) -0.0072(11) C16 0.0407(15) 0.0410(15) 0.0485(16) -0.0021(13) 0.0195(13) -0.0094(12) C17 0.0457(16) 0.0487(17) 0.0446(16) 0.0030(13) 0.0168(13) -0.0124(13) C18 0.0605(19) 0.0436(17) 0.0463(16) 0.0002(13) 0.0178(15) -0.0132(14) C19 0.080(3) 0.067(2) 0.069(2) -0.0048(19) 0.024(2) -0.033(2) C20 0.0334(12) 0.0294(12) 0.0250(11) 0.0057(9) 0.0064(10) -0.0017(10) C21 0.0355(14) 0.0441(16) 0.0412(15) 0.0011(12) 0.0104(12) -0.0055(12) C22 0.0388(15) 0.0558(19) 0.0591(19) -0.0026(16) 0.0085(14) -0.0157(14) C23 0.0526(18) 0.0399(16) 0.0525(18) -0.0060(14) 0.0050(14) -0.0145(14) C24 0.0507(16) 0.0321(14) 0.0388(14) -0.0013(12) 0.0072(12) -0.0019(12) C25 0.0378(13) 0.0286(12) 0.0270(11) 0.0041(10) 0.0058(10) -0.0010(10) C26 0.0535(17) 0.0385(15) 0.0357(14) -0.0052(12) 0.0169(12) 0.0084(12) C27 0.0544(17) 0.0486(17) 0.0448(16) 0.0000(13) 0.0270(14) 0.0090(14) C28 0.0467(16) 0.0388(15) 0.0466(16) -0.0017(12) 0.0214(13) 0.0060(12) C29 0.0463(17) 0.064(2) 0.073(2) -0.0019(18) 0.0294(16) 0.0071(16) C30 0.0456(19) 0.092(3) 0.075(2) -0.017(2) 0.0167(18) 0.0127(19) C31 0.0300(11) 0.0222(11) 0.0225(10) -0.0019(9) 0.0073(9) 0.0035(9) C32 0.0348(12) 0.0255(12) 0.0265(11) -0.0013(9) 0.0107(10) 0.0023(10) C33 0.0332(13) 0.0309(13) 0.0338(13) -0.0043(10) 0.0102(10) -0.0007(10) C34 0.0342(13) 0.0353(14) 0.0293(12) -0.0031(10) 0.0016(10) 0.0048(11) C35 0.0404(14) 0.0289(12) 0.0248(11) 0.0023(10) 0.0057(10) 0.0057(10) C36 0.0356(12) 0.0228(11) 0.0253(11) 0.0003(9) 0.0100(10) 0.0044(9) C37 0.0474(15) 0.0321(13) 0.0306(12) 0.0117(10) 0.0167(11) 0.0098(11) C38 0.0581(17) 0.0320(14) 0.0445(15) 0.0078(12) 0.0277(14) 0.0040(12) C39 0.0446(15) 0.0406(15) 0.0458(15) 0.0085(12) 0.0191(13) -0.0029(12) C40 0.0486(16) 0.0428(16) 0.0551(17) 0.0070(14) 0.0255(14) 0.0036(13) C41 0.060(2) 0.056(2) 0.097(3) 0.006(2) 0.044(2) 0.0089(17) C42 0.0337(12) 0.0217(11) 0.0295(12) -0.0027(9) 0.0067(10) 0.0025(9) C43 0.0372(13) 0.0344(13) 0.0359(13) -0.0047(11) 0.0135(11) -0.0037(11) C44 0.0401(15) 0.0456(17) 0.0559(18) -0.0146(14) 0.0195(14) -0.0104(12) C45 0.0348(14) 0.0437(17) 0.063(2) -0.0182(15) -0.0001(14) 0.0008(13) C46 0.0504(18) 0.0404(16) 0.0477(17) 0.0006(14) -0.0107(14) 0.0028(14) C47 0.0466(16) 0.0327(14) 0.0386(15) 0.0065(11) -0.0003(12) -0.0025(12) C48 0.0357(12) 0.0240(11) 0.0239(11) 0.0020(9) 0.0138(10) -0.0024(9) C49 0.0417(14) 0.0268(12) 0.0290(12) 0.0038(10) 0.0125(10) 0.0021(10) C50 0.0553(17) 0.0303(13) 0.0383(14) 0.0064(11) 0.0216(13) 0.0098(12) C51 0.0679(19) 0.0288(13) 0.0344(13) -0.0039(11) 0.0267(13) -0.0047(13) C52 0.0483(15) 0.0393(15) 0.0302(13) -0.0080(11) 0.0155(12) -0.0124(12) C53 0.0369(13) 0.0337(13) 0.0293(12) -0.0005(10) 0.0134(10) -0.0037(10) C54 0.0332(12) 0.0276(12) 0.0242(11) 0.0068(9) 0.0100(9) 0.0046(10) C55 0.0328(12) 0.0327(13) 0.0330(13) 0.0037(10) 0.0143(10) 0.0006(10) C56 0.0413(15) 0.0433(16) 0.0477(16) 0.0077(13) 0.0223(13) -0.0019(12) C57 0.0605(19) 0.0582(19) 0.0469(17) 0.0114(15) 0.0354(15) 0.0049(15) C58 0.086(2) 0.0481(18) 0.0386(15) 0.0017(13) 0.0362(16) 0.0048(16) C59 0.0661(19) 0.0343(14) 0.0306(13) 0.0012(11) 0.0229(13) -0.0029(13) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ni1 C9 1.890(2) . ? Ni1 O1 1.8959(17) . ? Ni1 P1 2.1785(7) . ? Ni1 P2 2.2078(7) . ? O1 C1 1.313(3) . ? O2 C14 1.385(3) . ? O2 C15 1.427(3) . ? O3 C25 1.366(3) . ? O3 C26 1.444(3) . ? O4 C36 1.369(3) . ? O4 C37 1.434(3) . ? P1 C2 1.772(2) . ? P1 C31 1.817(2) . ? P1 C20 1.820(3) . ? P2 C42 1.826(2) . ? P2 C48 1.828(2) . ? P2 C54 1.828(2) . ? C1 C2 1.360(3) . ? C1 C3 1.485(3) . ? C2 H2 0.9500 . ? C3 C8 1.390(4) . ? C3 C4 1.392(4) . ? C4 C5 1.381(4) . ? C4 H4 0.9500 . ? C5 C6 1.366(5) . ? C5 H5 0.9500 . ? C6 C7 1.380(5) . ? C6 H6 0.9500 . ? C7 C8 1.381(4) . ? C7 H7 0.9500 . ? C8 H8 0.9500 . ? C9 C10 1.398(4) . ? C9 C14 1.405(3) . ? C10 C11 1.392(4) . ? C10 H10 0.9500 . ? C11 C12 1.382(4) . ? C11 H11 0.9500 . ? C12 C13 1.387(4) . ? C12 H12 0.9500 . ? C13 C14 1.388(4) . ? C13 H13 0.9500 . ? C15 C16 1.520(4) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 C17 1.526(4) . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C17 C18 1.528(4) . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C18 C19 1.510(5) . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 C21 1.393(4) . ? C20 C25 1.400(4) . ? C21 C22 1.395(4) . ? C21 H21 0.9500 . ? C22 C23 1.369(5) . ? C22 H22 0.9500 . ? C23 C24 1.381(5) . ? C23 H23 0.9500 . ? C24 C25 1.390(4) . ? C24 H24 0.9500 . ? C26 C27 1.507(4) . ? C26 H26A 0.9900 . ? C26 H26B 0.9900 . ? C27 C28 1.522(4) . ? C27 H27A 0.9900 . ? C27 H27B 0.9900 . ? C28 C29 1.514(4) . ? C28 H28A 0.9900 . ? C28 H28B 0.9900 . ? C29 C30 1.523(5) . ? C29 H29A 0.9900 . ? C29 H29B 0.9900 . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C31 C32 1.387(3) . ? C31 C36 1.406(3) . ? C32 C33 1.391(3) . ? C32 H32 0.9500 . ? C33 C34 1.379(4) . ? C33 H33 0.9500 . ? C34 C35 1.386(4) . ? C34 H34 0.9500 . ? C35 C36 1.390(3) . ? C35 H35 0.9500 . ? C37 C38 1.512(4) . ? C37 H37A 0.9900 . ? C37 H37B 0.9900 . ? C38 C39 1.526(4) . ? C38 H38A 0.9900 . ? C38 H38B 0.9900 . ? C39 C40 1.509(4) . ? C39 H39A 0.9900 . ? C39 H39B 0.9900 . ? C40 C41 1.532(4) . ? C40 H40A 0.9900 . ? C40 H40B 0.9900 . ? C41 H41A 0.9800 . ? C41 H41B 0.9800 . ? C41 H41C 0.9800 . ? C42 C43 1.390(4) . ? C42 C47 1.392(4) . ? C43 C44 1.390(4) . ? C43 H43 0.9500 . ? C44 C45 1.374(5) . ? C44 H44 0.9500 . ? C45 C46 1.381(5) . ? C45 H45 0.9500 . ? C46 C47 1.384(4) . ? C46 H46 0.9500 . ? C47 H47 0.9500 . ? C48 C49 1.391(4) . ? C48 C53 1.390(4) . ? C49 C50 1.390(4) . ? C49 H49 0.9500 . ? C50 C51 1.388(4) . ? C50 H50 0.9500 . ? C51 C52 1.376(4) . ? C51 H51 0.9500 . ? C52 C53 1.389(4) . ? C52 H52 0.9500 . ? C53 H53 0.9500 . ? C54 C55 1.386(4) . ? C54 C59 1.395(4) . ? C55 C56 1.389(4) . ? C55 H55 0.9500 . ? C56 C57 1.378(5) . ? C56 H56 0.9500 . ? C57 C58 1.377(5) . ? C57 H57 0.9500 . ? C58 C59 1.387(4) . ? C58 H58 0.9500 . ? C59 H59 0.9500 . ? C60 C61 1.535(13) . ? C60 H60A 0.9827 . ? C60 H60B 0.9827 . ? C60 H60C 0.9828 . ? C61 C62 1.498(11) . ? C61 H61A 0.9900 . ? C61 H61B 0.9900 . ? C62 C63 1.531(11) . ? C62 H62A 0.9900 . ? C62 H62B 0.9900 . ? C63 C64 1.373(11) . ? C63 H63A 0.9900 . ? C63 H63B 0.9900 . ? C64 C65 1.377(10) . ? C64 H64A 0.9900 . ? C64 H64B 0.9900 . ? C65 H65A 0.9800 . ? C65 H65B 0.9800 . ? C65 H65C 0.9800 . ? 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 _geom_angle_publ_flag C9 Ni1 O1 176.77(9) . . ? C9 Ni1 P1 96.72(7) . . ? O1 Ni1 P1 86.15(5) . . ? C9 Ni1 P2 91.97(7) . . ? O1 Ni1 P2 85.43(5) . . ? P1 Ni1 P2 167.36(3) . . ? C1 O1 Ni1 120.05(15) . . ? C14 O2 C15 118.0(2) . . ? C25 O3 C26 118.2(2) . . ? C36 O4 C37 117.93(19) . . ? C2 P1 C31 105.30(11) . . ? C2 P1 C20 108.30(12) . . ? C31 P1 C20 108.29(11) . . ? C2 P1 Ni1 98.98(8) . . ? C31 P1 Ni1 119.50(8) . . ? C20 P1 Ni1 115.07(8) . . ? C42 P2 C48 105.88(11) . . ? C42 P2 C54 104.58(11) . . ? C48 P2 C54 103.70(11) . . ? C42 P2 Ni1 108.89(8) . . ? C48 P2 Ni1 110.17(8) . . ? C54 P2 Ni1 122.39(8) . . ? O1 C1 C2 121.6(2) . . ? O1 C1 C3 113.9(2) . . ? C2 C1 C3 124.5(2) . . ? C1 C2 P1 112.93(18) . . ? C1 C2 H2 123.5 . . ? P1 C2 H2 123.5 . . ? C8 C3 C4 117.8(2) . . ? C8 C3 C1 119.5(2) . . ? C4 C3 C1 122.6(2) . . ? C5 C4 C3 120.8(3) . . ? C5 C4 H4 119.6 . . ? C3 C4 H4 119.6 . . ? C6 C5 C4 120.7(3) . . ? C6 C5 H5 119.6 . . ? C4 C5 H5 119.6 . . ? C5 C6 C7 119.4(3) . . ? C5 C6 H6 120.3 . . ? C7 C6 H6 120.3 . . ? C6 C7 C8 120.3(3) . . ? C6 C7 H7 119.8 . . ? C8 C7 H7 119.8 . . ? C7 C8 C3 120.9(3) . . ? C7 C8 H8 119.5 . . ? C3 C8 H8 119.5 . . ? C10 C9 C14 116.5(2) . . ? C10 C9 Ni1 124.83(18) . . ? C14 C9 Ni1 118.56(18) . . ? C11 C10 C9 122.0(2) . . ? C11 C10 H10 119.0 . . ? C9 C10 H10 119.0 . . ? C12 C11 C10 119.8(3) . . ? C12 C11 H11 120.1 . . ? C10 C11 H11 120.1 . . ? C11 C12 C13 120.0(2) . . ? C11 C12 H12 120.0 . . ? C13 C12 H12 120.0 . . ? C12 C13 C14 119.6(2) . . ? C12 C13 H13 120.2 . . ? C14 C13 H13 120.2 . . ? O2 C14 C13 123.7(2) . . ? O2 C14 C9 114.1(2) . . ? C13 C14 C9 122.1(2) . . ? O2 C15 C16 107.4(2) . . ? O2 C15 H15A 110.2 . . ? C16 C15 H15A 110.2 . . ? O2 C15 H15B 110.2 . . ? C16 C15 H15B 110.2 . . ? H15A C15 H15B 108.5 . . ? C15 C16 C17 112.1(2) . . ? C15 C16 H16A 109.2 . . ? C17 C16 H16A 109.2 . . ? C15 C16 H16B 109.2 . . ? C17 C16 H16B 109.2 . . ? H16A C16 H16B 107.9 . . ? C16 C17 C18 113.2(3) . . ? C16 C17 H17A 108.9 . . ? C18 C17 H17A 108.9 . . ? C16 C17 H17B 108.9 . . ? C18 C17 H17B 108.9 . . ? H17A C17 H17B 107.8 . . ? C19 C18 C17 112.8(3) . . ? C19 C18 H18A 109.0 . . ? C17 C18 H18A 109.0 . . ? C19 C18 H18B 109.0 . . ? C17 C18 H18B 109.0 . . ? H18A C18 H18B 107.8 . . ? C18 C19 H19A 109.5 . . ? C18 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C18 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C21 C20 C25 118.3(2) . . ? C21 C20 P1 118.3(2) . . ? C25 C20 P1 123.07(19) . . ? C20 C21 C22 120.7(3) . . ? C20 C21 H21 119.6 . . ? C22 C21 H21 119.6 . . ? C23 C22 C21 119.9(3) . . ? C23 C22 H22 120.0 . . ? C21 C22 H22 120.0 . . ? C22 C23 C24 120.6(3) . . ? C22 C23 H23 119.7 . . ? C24 C23 H23 119.7 . . ? C23 C24 C25 119.8(3) . . ? C23 C24 H24 120.1 . . ? C25 C24 H24 120.1 . . ? O3 C25 C24 122.8(2) . . ? O3 C25 C20 116.6(2) . . ? C24 C25 C20 120.6(3) . . ? O3 C26 C27 107.6(2) . . ? O3 C26 H26A 110.2 . . ? C27 C26 H26A 110.2 . . ? O3 C26 H26B 110.2 . . ? C27 C26 H26B 110.2 . . ? H26A C26 H26B 108.5 . . ? C26 C27 C28 114.1(3) . . ? C26 C27 H27A 108.7 . . ? C28 C27 H27A 108.7 . . ? C26 C27 H27B 108.7 . . ? C28 C27 H27B 108.7 . . ? H27A C27 H27B 107.6 . . ? C29 C28 C27 113.4(3) . . ? C29 C28 H28A 108.9 . . ? C27 C28 H28A 108.9 . . ? C29 C28 H28B 108.9 . . ? C27 C28 H28B 108.9 . . ? H28A C28 H28B 107.7 . . ? C28 C29 C30 113.5(3) . . ? C28 C29 H29A 108.8 . . ? C30 C29 H29A 108.8 . . ? C28 C29 H29B 108.9 . . ? C30 C29 H29B 108.9 . . ? H29A C29 H29B 107.7 . . ? C29 C30 H30A 109.5 . . ? C29 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C29 C30 H30C 109.4 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C32 C31 C36 119.1(2) . . ? C32 C31 P1 119.26(18) . . ? C36 C31 P1 121.32(18) . . ? C31 C32 C33 121.1(2) . . ? C31 C32 H32 119.4 . . ? C33 C32 H32 119.4 . . ? C34 C33 C32 119.1(2) . . ? C34 C33 H33 120.4 . . ? C32 C33 H33 120.4 . . ? C33 C34 C35 120.9(2) . . ? C33 C34 H34 119.5 . . ? C35 C34 H34 119.5 . . ? C34 C35 C36 120.0(2) . . ? C34 C35 H35 120.0 . . ? C36 C35 H35 120.0 . . ? O4 C36 C35 124.3(2) . . ? O4 C36 C31 116.0(2) . . ? C35 C36 C31 119.7(2) . . ? O4 C37 C38 108.3(2) . . ? O4 C37 H37A 110.0 . . ? C38 C37 H37A 110.0 . . ? O4 C37 H37B 110.0 . . ? C38 C37 H37B 110.0 . . ? H37A C37 H37B 108.4 . . ? C37 C38 C39 116.4(2) . . ? C37 C38 H38A 108.2 . . ? C39 C38 H38A 108.2 . . ? C37 C38 H38B 108.2 . . ? C39 C38 H38B 108.2 . . ? H38A C38 H38B 107.3 . . ? C40 C39 C38 114.3(3) . . ? C40 C39 H39A 108.7 . . ? C38 C39 H39A 108.7 . . ? C40 C39 H39B 108.7 . . ? C38 C39 H39B 108.7 . . ? H39A C39 H39B 107.6 . . ? C39 C40 C41 112.9(3) . . ? C39 C40 H40A 109.0 . . ? C41 C40 H40A 109.0 . . ? C39 C40 H40B 109.0 . . ? C41 C40 H40B 109.0 . . ? H40A C40 H40B 107.8 . . ? C40 C41 H41A 109.5 . . ? C40 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? C40 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? C43 C42 C47 119.2(2) . . ? C43 C42 P2 117.90(19) . . ? C47 C42 P2 122.9(2) . . ? C42 C43 C44 120.0(3) . . ? C42 C43 H43 120.0 . . ? C44 C43 H43 120.0 . . ? C45 C44 C43 120.4(3) . . ? C45 C44 H44 119.8 . . ? C43 C44 H44 119.8 . . ? C44 C45 C46 119.8(3) . . ? C44 C45 H45 120.1 . . ? C46 C45 H45 120.1 . . ? C45 C46 C47 120.5(3) . . ? C45 C46 H46 119.8 . . ? C47 C46 H46 119.8 . . ? C46 C47 C42 120.1(3) . . ? C46 C47 H47 120.0 . . ? C42 C47 H47 120.0 . . ? C49 C48 C53 119.6(2) . . ? C49 C48 P2 124.02(19) . . ? C53 C48 P2 116.38(19) . . ? C50 C49 C48 119.6(2) . . ? C50 C49 H49 120.2 . . ? C48 C49 H49 120.2 . . ? C51 C50 C49 120.5(3) . . ? C51 C50 H50 119.8 . . ? C49 C50 H50 119.8 . . ? C52 C51 C50 119.9(3) . . ? C52 C51 H51 120.1 . . ? C50 C51 H51 120.1 . . ? C51 C52 C53 120.1(3) . . ? C51 C52 H52 119.9 . . ? C53 C52 H52 119.9 . . ? C52 C53 C48 120.3(3) . . ? C52 C53 H53 119.9 . . ? C48 C53 H53 119.9 . . ? C55 C54 C59 118.8(2) . . ? C55 C54 P2 121.80(19) . . ? C59 C54 P2 119.3(2) . . ? C54 C55 C56 120.5(3) . . ? C54 C55 H55 119.7 . . ? C56 C55 H55 119.7 . . ? C57 C56 C55 120.1(3) . . ? C57 C56 H56 119.9 . . ? C55 C56 H56 119.9 . . ? C58 C57 C56 119.9(3) . . ? C58 C57 H57 120.0 . . ? C56 C57 H57 120.0 . . ? C57 C58 C59 120.3(3) . . ? C57 C58 H58 119.9 . . ? C59 C58 H58 119.9 . . ? C58 C59 C54 120.3(3) . . ? C58 C59 H59 119.9 . . ? C54 C59 H59 119.9 . . ? C61 C60 H60A 109.4 . . ? C61 C60 H60B 109.6 . . ? H60A C60 H60B 109.2 . . ? C61 C60 H60C 110.2 . . ? H60A C60 H60C 109.2 . . ? H60B C60 H60C 109.2 . . ? C62 C61 C60 94.0(9) . . ? C62 C61 H61A 112.9 . . ? C60 C61 H61A 112.6 . . ? C62 C61 H61B 112.9 . . ? C60 C61 H61B 113.3 . . ? H61A C61 H61B 110.3 . . ? C61 C62 C63 94.5(8) . . ? C61 C62 H62A 112.8 . . ? C63 C62 H62A 112.7 . . ? C61 C62 H62B 112.8 . . ? C63 C62 H62B 113.0 . . ? H62A C62 H62B 110.2 . . ? C64 C63 C62 128.4(11) . . ? C64 C63 H63A 105.3 . . ? C62 C63 H63A 105.3 . . ? C64 C63 H63B 105.2 . . ? C62 C63 H63B 105.0 . . ? H63A C63 H63B 105.9 . . ? C65 C64 C63 134.5(11) . . ? C65 C64 H64A 103.6 . . ? C63 C64 H64A 103.7 . . ? C65 C64 H64B 103.6 . . ? C63 C64 H64B 103.5 . . ? H64A C64 H64B 105.3 . . ? C64 C65 H65A 109.5 . . ? C64 C65 H65B 109.4 . . ? H65A C65 H65B 109.5 . . ? C64 C65 H65C 109.5 . . ? H65A C65 H65C 109.5 . . ? H65B C65 H65C 109.5 . . ? 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_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C9 Ni1 O1 C1 -152.8(15) . . . . ? P1 Ni1 O1 C1 -0.14(17) . . . . ? P2 Ni1 O1 C1 170.43(18) . . . . ? C9 Ni1 P1 C2 -178.74(11) . . . . ? O1 Ni1 P1 C2 2.76(10) . . . . ? P2 Ni1 P1 C2 -45.55(16) . . . . ? C9 Ni1 P1 C31 67.91(11) . . . . ? O1 Ni1 P1 C31 -110.60(10) . . . . ? P2 Ni1 P1 C31 -158.90(14) . . . . ? C9 Ni1 P1 C20 -63.60(12) . . . . ? O1 Ni1 P1 C20 117.89(11) . . . . ? P2 Ni1 P1 C20 69.59(17) . . . . ? C9 Ni1 P2 C42 99.79(11) . . . . ? O1 Ni1 P2 C42 -82.15(10) . . . . ? P1 Ni1 P2 C42 -33.78(16) . . . . ? C9 Ni1 P2 C48 -144.51(11) . . . . ? O1 Ni1 P2 C48 33.56(10) . . . . ? P1 Ni1 P2 C48 81.92(16) . . . . ? C9 Ni1 P2 C54 -22.37(12) . . . . ? O1 Ni1 P2 C54 155.69(11) . . . . ? P1 Ni1 P2 C54 -155.94(15) . . . . ? Ni1 O1 C1 C2 -3.9(3) . . . . ? Ni1 O1 C1 C3 174.67(15) . . . . ? O1 C1 C2 P1 6.4(3) . . . . ? C3 C1 C2 P1 -172.00(19) . . . . ? C31 P1 C2 C1 118.75(19) . . . . ? C20 P1 C2 C1 -125.58(19) . . . . ? Ni1 P1 C2 C1 -5.3(2) . . . . ? O1 C1 C3 C8 4.1(3) . . . . ? C2 C1 C3 C8 -177.4(3) . . . . ? O1 C1 C3 C4 -173.5(3) . . . . ? C2 C1 C3 C4 5.0(4) . . . . ? C8 C3 C4 C5 0.7(5) . . . . ? C1 C3 C4 C5 178.3(3) . . . . ? C3 C4 C5 C6 0.1(6) . . . . ? C4 C5 C6 C7 -1.3(7) . . . . ? C5 C6 C7 C8 1.8(6) . . . . ? C6 C7 C8 C3 -1.0(5) . . . . ? C4 C3 C8 C7 -0.2(4) . . . . ? C1 C3 C8 C7 -177.9(3) . . . . ? O1 Ni1 C9 C10 -134.8(15) . . . . ? P1 Ni1 C9 C10 72.7(2) . . . . ? P2 Ni1 C9 C10 -98.1(2) . . . . ? O1 Ni1 C9 C14 40.9(17) . . . . ? P1 Ni1 C9 C14 -111.66(17) . . . . ? P2 Ni1 C9 C14 77.53(18) . . . . ? C14 C9 C10 C11 -0.5(4) . . . . ? Ni1 C9 C10 C11 175.26(19) . . . . ? C9 C10 C11 C12 1.5(4) . . . . ? C10 C11 C12 C13 -0.9(4) . . . . ? C11 C12 C13 C14 -0.6(4) . . . . ? C15 O2 C14 C13 6.1(3) . . . . ? C15 O2 C14 C9 -173.6(2) . . . . ? C12 C13 C14 O2 -177.9(2) . . . . ? C12 C13 C14 C9 1.7(4) . . . . ? C10 C9 C14 O2 178.6(2) . . . . ? Ni1 C9 C14 O2 2.5(3) . . . . ? C10 C9 C14 C13 -1.1(3) . . . . ? Ni1 C9 C14 C13 -177.14(19) . . . . ? C14 O2 C15 C16 176.2(2) . . . . ? O2 C15 C16 C17 -176.8(2) . . . . ? C15 C16 C17 C18 -177.3(3) . . . . ? C16 C17 C18 C19 -180.0(3) . . . . ? C2 P1 C20 C21 27.5(2) . . . . ? C31 P1 C20 C21 141.2(2) . . . . ? Ni1 P1 C20 C21 -82.1(2) . . . . ? C2 P1 C20 C25 -159.1(2) . . . . ? C31 P1 C20 C25 -45.4(2) . . . . ? Ni1 P1 C20 C25 91.2(2) . . . . ? C25 C20 C21 C22 0.6(4) . . . . ? P1 C20 C21 C22 174.2(2) . . . . ? C20 C21 C22 C23 -0.3(5) . . . . ? C21 C22 C23 C24 0.0(5) . . . . ? C22 C23 C24 C25 0.1(5) . . . . ? C26 O3 C25 C24 13.0(4) . . . . ? C26 O3 C25 C20 -167.7(2) . . . . ? C23 C24 C25 O3 179.5(3) . . . . ? C23 C24 C25 C20 0.2(4) . . . . ? C21 C20 C25 O3 -179.8(2) . . . . ? P1 C20 C25 O3 6.8(3) . . . . ? C21 C20 C25 C24 -0.5(4) . . . . ? P1 C20 C25 C24 -173.9(2) . . . . ? C25 O3 C26 C27 173.4(2) . . . . ? O3 C26 C27 C28 69.1(3) . . . . ? C26 C27 C28 C29 -179.4(3) . . . . ? C27 C28 C29 C30 -177.5(3) . . . . ? C2 P1 C31 C32 -118.6(2) . . . . ? C20 P1 C31 C32 125.76(19) . . . . ? Ni1 P1 C31 C32 -8.7(2) . . . . ? C2 P1 C31 C36 54.8(2) . . . . ? C20 P1 C31 C36 -60.9(2) . . . . ? Ni1 P1 C31 C36 164.74(16) . . . . ? C36 C31 C32 C33 -0.4(3) . . . . ? P1 C31 C32 C33 173.14(18) . . . . ? C31 C32 C33 C34 -1.4(4) . . . . ? C32 C33 C34 C35 1.8(4) . . . . ? C33 C34 C35 C36 -0.6(4) . . . . ? C37 O4 C36 C35 3.3(3) . . . . ? C37 O4 C36 C31 -176.0(2) . . . . ? C34 C35 C36 O4 179.4(2) . . . . ? C34 C35 C36 C31 -1.2(4) . . . . ? C32 C31 C36 O4 -178.9(2) . . . . ? P1 C31 C36 O4 7.7(3) . . . . ? C32 C31 C36 C35 1.7(3) . . . . ? P1 C31 C36 C35 -171.70(18) . . . . ? C36 O4 C37 C38 -173.6(2) . . . . ? O4 C37 C38 C39 -59.6(3) . . . . ? C37 C38 C39 C40 -57.0(3) . . . . ? C38 C39 C40 C41 -168.7(3) . . . . ? C48 P2 C42 C43 -95.9(2) . . . . ? C54 P2 C42 C43 154.9(2) . . . . ? Ni1 P2 C42 C43 22.5(2) . . . . ? C48 P2 C42 C47 81.9(2) . . . . ? C54 P2 C42 C47 -27.2(3) . . . . ? Ni1 P2 C42 C47 -159.6(2) . . . . ? C47 C42 C43 C44 -0.1(4) . . . . ? P2 C42 C43 C44 177.8(2) . . . . ? C42 C43 C44 C45 0.2(4) . . . . ? C43 C44 C45 C46 -0.1(5) . . . . ? C44 C45 C46 C47 0.0(5) . . . . ? C45 C46 C47 C42 0.0(5) . . . . ? C43 C42 C47 C46 0.1(4) . . . . ? P2 C42 C47 C46 -177.8(2) . . . . ? C42 P2 C48 C49 -15.5(2) . . . . ? C54 P2 C48 C49 94.3(2) . . . . ? Ni1 P2 C48 C49 -133.06(19) . . . . ? C42 P2 C48 C53 163.38(19) . . . . ? C54 P2 C48 C53 -86.8(2) . . . . ? Ni1 P2 C48 C53 45.8(2) . . . . ? C53 C48 C49 C50 1.2(4) . . . . ? P2 C48 C49 C50 179.98(19) . . . . ? C48 C49 C50 C51 1.2(4) . . . . ? C49 C50 C51 C52 -1.9(4) . . . . ? C50 C51 C52 C53 0.1(4) . . . . ? C51 C52 C53 C48 2.2(4) . . . . ? C49 C48 C53 C52 -2.9(4) . . . . ? P2 C48 C53 C52 178.2(2) . . . . ? C42 P2 C54 C55 128.2(2) . . . . ? C48 P2 C54 C55 17.5(2) . . . . ? Ni1 P2 C54 C55 -107.6(2) . . . . ? C42 P2 C54 C59 -54.9(2) . . . . ? C48 P2 C54 C59 -165.7(2) . . . . ? Ni1 P2 C54 C59 69.2(2) . . . . ? C59 C54 C55 C56 0.8(4) . . . . ? P2 C54 C55 C56 177.6(2) . . . . ? C54 C55 C56 C57 -0.1(4) . . . . ? C55 C56 C57 C58 -0.8(5) . . . . ? C56 C57 C58 C59 1.0(5) . . . . ? C57 C58 C59 C54 -0.4(5) . . . . ? C55 C54 C59 C58 -0.5(4) . . . . ? P2 C54 C59 C58 -177.5(2) . . . . ? C60 C61 C62 C63 169.5(10) . . . . ? C61 C62 C63 C64 -122.0(13) . . . . ? C62 C63 C64 C65 -159.5(12) . . . . ? _diffrn_measured_fraction_theta_max 0.985 _diffrn_reflns_theta_full 67.48 _diffrn_measured_fraction_theta_full 0.985 _refine_diff_density_max 1.227 _refine_diff_density_min -0.644 _refine_diff_density_rms 0.065 # Attachment 'z.cif' data_z _database_code_depnum_ccdc_archive 'CCDC 847793' #TrackingRef 'z.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C47 H42 Ni O4 P2' _chemical_formula_weight 791.46 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' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 18.1954(9) _cell_length_b 10.2494(5) _cell_length_c 21.1754(10) _cell_angle_alpha 90.00 _cell_angle_beta 94.797(2) _cell_angle_gamma 90.00 _cell_volume 3935.2(3) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 9990 _cell_measurement_theta_min 4.301 _cell_measurement_theta_max 53.020 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.362 _exptl_crystal_size_mid 0.255 _exptl_crystal_size_min 0.214 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.336 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1656 _exptl_absorpt_coefficient_mu 0.619 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.77273 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 48002 _diffrn_reflns_av_R_equivalents 0.0507 _diffrn_reflns_av_sigmaI/netI 0.0347 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 1.93 _diffrn_reflns_theta_max 26.00 _reflns_number_total 7714 _reflns_number_gt 5954 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0520P)^2^+2.3553P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7714 _refine_ls_number_parameters 490 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0592 _refine_ls_R_factor_gt 0.0387 _refine_ls_wR_factor_ref 0.1067 _refine_ls_wR_factor_gt 0.0949 _refine_ls_goodness_of_fit_ref 1.063 _refine_ls_restrained_S_all 1.063 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ni1 Ni 0.260355(16) 0.52045(3) 0.018209(14) 0.02270(10) Uani 1 1 d . . . P1 P 0.24950(3) 0.38315(6) 0.09571(3) 0.02261(15) Uani 1 1 d . . . P2 P 0.25287(3) 0.64790(6) -0.06676(3) 0.02049(14) Uani 1 1 d . . . O1 O 0.19266(9) 0.41116(17) -0.03062(8) 0.0296(4) Uani 1 1 d . . . O2 O 0.25158(11) 0.78511(18) 0.07603(10) 0.0407(5) Uani 1 1 d . . . O3 O 0.35610(11) 0.4565(2) 0.20579(10) 0.0457(5) Uani 1 1 d . . . O4 O 0.19556(10) 0.21941(19) 0.19920(9) 0.0379(5) Uani 1 1 d . . . C1 C 0.16768(12) 0.3055(2) -0.00471(12) 0.0237(5) Uani 1 1 d . . . C2 C 0.19065(13) 0.2672(2) 0.05497(12) 0.0260(5) Uani 1 1 d . . . H2 H 0.1767 0.1870 0.0730 0.031 Uiso 1 1 calc R . . C3 C 0.10926(13) 0.2368(2) -0.04622(11) 0.0239(5) Uani 1 1 d . . . C4 C 0.07045(14) 0.3073(3) -0.09360(12) 0.0317(6) Uani 1 1 d . . . H4 H 0.0835 0.3955 -0.1007 0.038 Uiso 1 1 calc R . . C5 C 0.01278(16) 0.2509(3) -0.13084(14) 0.0423(7) Uani 1 1 d . . . H5 H -0.0142 0.3009 -0.1627 0.051 Uiso 1 1 calc R . . C6 C -0.00537(16) 0.1221(3) -0.12154(14) 0.0436(7) Uani 1 1 d . . . H6 H -0.0448 0.0830 -0.1471 0.052 Uiso 1 1 calc R . . C7 C 0.03355(16) 0.0507(3) -0.07544(14) 0.0406(7) Uani 1 1 d . . . H7 H 0.0214 -0.0383 -0.0694 0.049 Uiso 1 1 calc R . . C8 C 0.09030(14) 0.1075(3) -0.03764(13) 0.0326(6) Uani 1 1 d . . . H8 H 0.1166 0.0574 -0.0054 0.039 Uiso 1 1 calc R . . C9 C 0.33602(14) 0.6219(3) 0.06033(12) 0.0291(6) Uani 1 1 d . . . C10 C 0.40934(15) 0.5769(3) 0.06351(14) 0.0419(7) Uani 1 1 d . . . H10 H 0.4195 0.4916 0.0490 0.050 Uiso 1 1 calc R . . C11 C 0.46746(17) 0.6568(4) 0.08794(16) 0.0535(9) Uani 1 1 d . . . H11 H 0.5168 0.6259 0.0900 0.064 Uiso 1 1 calc R . . C12 C 0.45259(18) 0.7801(4) 0.10883(15) 0.0544(9) Uani 1 1 d . . . H12 H 0.4921 0.8339 0.1254 0.065 Uiso 1 1 calc R . . C13 C 0.38115(19) 0.8275(3) 0.10615(13) 0.0463(8) Uani 1 1 d . . . H13 H 0.3715 0.9132 0.1203 0.056 Uiso 1 1 calc R . . C14 C 0.32367(15) 0.7470(3) 0.08226(12) 0.0333(6) Uani 1 1 d . . . C15 C 0.2351(2) 0.9175(3) 0.08861(17) 0.0596(10) Uani 1 1 d . . . H15A H 0.2513 0.9382 0.1328 0.089 Uiso 1 1 calc R . . H15B H 0.1818 0.9316 0.0814 0.089 Uiso 1 1 calc R . . H15C H 0.2607 0.9742 0.0604 0.089 Uiso 1 1 calc R . . C16 C 0.20381(12) 0.4357(3) 0.16445(11) 0.0248(5) Uani 1 1 d . . . C17 C 0.18003(14) 0.3473(3) 0.20929(12) 0.0297(6) Uani 1 1 d . . . C18 C 0.14204(15) 0.3926(3) 0.25928(13) 0.0361(7) Uani 1 1 d . . . H18 H 0.1256 0.3330 0.2894 0.043 Uiso 1 1 calc R . . C19 C 0.12832(15) 0.5242(3) 0.26498(14) 0.0406(7) Uani 1 1 d . . . H19 H 0.1023 0.5546 0.2992 0.049 Uiso 1 1 calc R . . C20 C 0.15184(15) 0.6124(3) 0.22171(13) 0.0369(7) Uani 1 1 d . . . H20 H 0.1425 0.7030 0.2262 0.044 Uiso 1 1 calc R . . C21 C 0.18917(14) 0.5674(3) 0.17170(12) 0.0312(6) Uani 1 1 d . . . H21 H 0.2051 0.6279 0.1417 0.037 Uiso 1 1 calc R . . C22 C 0.16308(18) 0.1252(3) 0.23806(16) 0.0492(8) Uani 1 1 d . . . H22A H 0.1805 0.1399 0.2825 0.074 Uiso 1 1 calc R . . H22B H 0.1772 0.0373 0.2254 0.074 Uiso 1 1 calc R . . H22C H 0.1093 0.1337 0.2329 0.074 Uiso 1 1 calc R . . C23 C 0.33655(13) 0.3069(2) 0.12291(11) 0.0232(5) Uani 1 1 d . . . C24 C 0.36237(14) 0.2086(3) 0.08598(13) 0.0312(6) Uani 1 1 d . . . H24 H 0.3304 0.1717 0.0530 0.037 Uiso 1 1 calc R . . C25 C 0.43389(15) 0.1631(3) 0.09621(14) 0.0395(7) Uani 1 1 d . . . H25 H 0.4508 0.0956 0.0704 0.047 Uiso 1 1 calc R . . C26 C 0.48033(15) 0.2161(3) 0.14393(14) 0.0358(6) Uani 1 1 d . . . H26 H 0.5297 0.1855 0.1506 0.043 Uiso 1 1 calc R . . C27 C 0.45619(14) 0.3129(3) 0.18216(13) 0.0336(6) Uani 1 1 d . . . H27 H 0.4884 0.3480 0.2155 0.040 Uiso 1 1 calc R . . C28 C 0.38441(14) 0.3590(2) 0.17163(12) 0.0288(6) Uani 1 1 d . . . C29 C 0.40453(19) 0.5259(3) 0.24986(17) 0.0585(10) Uani 1 1 d . . . H29A H 0.4236 0.4668 0.2837 0.088 Uiso 1 1 calc R . . H29B H 0.3777 0.5976 0.2681 0.088 Uiso 1 1 calc R . . H29C H 0.4457 0.5613 0.2281 0.088 Uiso 1 1 calc R . . C30 C 0.29482(12) 0.5758(3) -0.13399(11) 0.0251(5) Uani 1 1 d . . . C31 C 0.31182(15) 0.4438(3) -0.13402(13) 0.0355(6) Uani 1 1 d . . . H31 H 0.3020 0.3909 -0.0989 0.043 Uiso 1 1 calc R . . C32 C 0.34305(18) 0.3893(3) -0.18515(15) 0.0480(8) Uani 1 1 d . . . H32 H 0.3546 0.2989 -0.1848 0.058 Uiso 1 1 calc R . . C33 C 0.35768(16) 0.4643(3) -0.23654(15) 0.0457(8) Uani 1 1 d . . . H33 H 0.3786 0.4258 -0.2717 0.055 Uiso 1 1 calc R . . C34 C 0.34178(17) 0.5951(3) -0.23664(14) 0.0447(8) Uani 1 1 d . . . H34 H 0.3525 0.6474 -0.2717 0.054 Uiso 1 1 calc R . . C35 C 0.31014(15) 0.6515(3) -0.18596(13) 0.0355(6) Uani 1 1 d . . . H35 H 0.2989 0.7420 -0.1867 0.043 Uiso 1 1 calc R . . C36 C 0.28669(13) 0.8155(2) -0.06835(11) 0.0218(5) Uani 1 1 d . . . C37 C 0.36126(13) 0.8401(2) -0.05221(11) 0.0260(5) Uani 1 1 d . . . H37 H 0.3935 0.7702 -0.0396 0.031 Uiso 1 1 calc R . . C38 C 0.38853(14) 0.9654(3) -0.05451(12) 0.0305(6) Uani 1 1 d . . . H38 H 0.4394 0.9811 -0.0432 0.037 Uiso 1 1 calc R . . C39 C 0.34287(15) 1.0680(3) -0.07307(13) 0.0328(6) Uani 1 1 d . . . H39 H 0.3624 1.1537 -0.0749 0.039 Uiso 1 1 calc R . . C40 C 0.26915(15) 1.0463(3) -0.08899(13) 0.0352(6) Uani 1 1 d . . . H40 H 0.2375 1.1169 -0.1016 0.042 Uiso 1 1 calc R . . C41 C 0.24106(14) 0.9198(3) -0.08654(12) 0.0301(6) Uani 1 1 d . . . H41 H 0.1900 0.9049 -0.0974 0.036 Uiso 1 1 calc R . . C42 C 0.15461(13) 0.6607(2) -0.09195(12) 0.0239(5) Uani 1 1 d . . . C43 C 0.12565(14) 0.6471(3) -0.15407(13) 0.0299(6) Uani 1 1 d . . . H43 H 0.1577 0.6365 -0.1869 0.036 Uiso 1 1 calc R . . C44 C 0.04953(15) 0.6491(3) -0.16867(14) 0.0399(7) Uani 1 1 d . . . H44 H 0.0299 0.6405 -0.2115 0.048 Uiso 1 1 calc R . . C45 C 0.00294(15) 0.6633(3) -0.12169(16) 0.0441(8) Uani 1 1 d . . . H45 H -0.0489 0.6635 -0.1318 0.053 Uiso 1 1 calc R . . C46 C 0.03137(15) 0.6773(3) -0.05960(16) 0.0432(7) Uani 1 1 d . . . H46 H -0.0010 0.6878 -0.0270 0.052 Uiso 1 1 calc R . . C47 C 0.10668(14) 0.6763(3) -0.04456(14) 0.0339(6) Uani 1 1 d . . . H47 H 0.1259 0.6862 -0.0017 0.041 Uiso 1 1 calc R . . 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 0.02307(16) 0.02385(17) 0.02068(17) 0.00046(13) -0.00110(12) -0.00184(12) P1 0.0232(3) 0.0233(3) 0.0208(3) 0.0011(2) -0.0011(2) 0.0005(2) P2 0.0199(3) 0.0233(3) 0.0182(3) -0.0002(2) 0.0015(2) -0.0002(2) O1 0.0347(10) 0.0290(10) 0.0238(9) 0.0025(8) -0.0046(8) -0.0080(8) O2 0.0512(12) 0.0293(10) 0.0428(12) -0.0016(9) 0.0116(10) 0.0023(9) O3 0.0365(11) 0.0539(13) 0.0439(12) -0.0246(10) -0.0131(9) 0.0115(9) O4 0.0447(11) 0.0333(11) 0.0370(11) 0.0118(9) 0.0102(9) 0.0002(9) C1 0.0212(12) 0.0240(13) 0.0258(13) -0.0037(10) 0.0014(10) 0.0012(10) C2 0.0281(12) 0.0219(12) 0.0272(13) 0.0013(10) -0.0022(10) -0.0017(10) C3 0.0217(11) 0.0277(13) 0.0229(13) -0.0036(10) 0.0052(10) -0.0001(10) C4 0.0315(14) 0.0357(15) 0.0274(14) -0.0008(11) -0.0007(11) -0.0019(11) C5 0.0368(15) 0.0529(19) 0.0353(16) 0.0007(14) -0.0092(13) -0.0033(14) C6 0.0320(15) 0.061(2) 0.0372(17) -0.0111(15) -0.0032(13) -0.0145(14) C7 0.0411(16) 0.0379(17) 0.0432(17) -0.0074(13) 0.0059(13) -0.0124(13) C8 0.0316(14) 0.0323(15) 0.0340(15) -0.0010(12) 0.0041(11) -0.0017(11) C9 0.0316(13) 0.0322(14) 0.0229(13) 0.0036(11) -0.0015(11) -0.0076(11) C10 0.0297(14) 0.0517(18) 0.0427(17) 0.0150(14) -0.0062(12) -0.0095(13) C11 0.0377(17) 0.061(2) 0.059(2) 0.0160(18) -0.0139(15) -0.0135(15) C12 0.0508(19) 0.065(2) 0.0435(19) 0.0102(17) -0.0165(15) -0.0292(17) C13 0.075(2) 0.0381(17) 0.0249(15) -0.0021(13) -0.0010(15) -0.0195(16) C14 0.0428(16) 0.0353(15) 0.0215(14) 0.0034(11) 0.0013(11) -0.0085(12) C15 0.085(3) 0.0377(18) 0.056(2) -0.0083(16) 0.0015(19) 0.0141(18) C16 0.0199(11) 0.0338(14) 0.0202(12) 0.0006(10) -0.0015(9) 0.0006(10) C17 0.0255(12) 0.0353(15) 0.0275(14) 0.0030(11) -0.0027(11) -0.0006(11) C18 0.0325(14) 0.0500(18) 0.0259(14) 0.0041(13) 0.0038(11) -0.0039(13) C19 0.0336(15) 0.059(2) 0.0293(15) -0.0102(14) 0.0057(12) 0.0033(14) C20 0.0385(15) 0.0396(16) 0.0328(16) -0.0078(13) 0.0040(12) 0.0049(12) C21 0.0302(13) 0.0334(14) 0.0296(14) -0.0016(12) 0.0006(11) 0.0005(11) C22 0.0557(19) 0.0422(18) 0.051(2) 0.0172(15) 0.0133(16) -0.0048(15) C23 0.0231(12) 0.0235(12) 0.0228(13) 0.0041(10) 0.0005(10) -0.0004(9) C24 0.0304(13) 0.0302(14) 0.0323(15) -0.0037(11) -0.0013(11) 0.0007(11) C25 0.0355(15) 0.0381(16) 0.0451(18) -0.0079(14) 0.0048(13) 0.0089(12) C26 0.0273(13) 0.0401(16) 0.0397(16) 0.0050(13) 0.0016(12) 0.0086(12) C27 0.0286(13) 0.0388(16) 0.0319(15) 0.0061(12) -0.0061(11) 0.0003(11) C28 0.0310(13) 0.0290(14) 0.0258(14) -0.0005(11) -0.0013(11) 0.0030(11) C29 0.055(2) 0.058(2) 0.058(2) -0.0308(18) -0.0215(17) 0.0109(17) C30 0.0192(11) 0.0327(14) 0.0236(13) -0.0049(11) 0.0020(10) -0.0002(10) C31 0.0405(15) 0.0359(15) 0.0302(15) -0.0006(12) 0.0035(12) 0.0108(12) C32 0.0535(19) 0.0457(18) 0.0451(19) -0.0134(15) 0.0062(15) 0.0170(15) C33 0.0392(16) 0.066(2) 0.0338(17) -0.0195(16) 0.0137(13) 0.0022(15) C34 0.0507(18) 0.056(2) 0.0297(16) -0.0134(14) 0.0176(14) -0.0162(15) C35 0.0409(15) 0.0365(16) 0.0300(15) -0.0056(12) 0.0091(12) -0.0091(12) C36 0.0242(12) 0.0266(13) 0.0152(12) -0.0013(10) 0.0054(9) -0.0002(10) C37 0.0265(12) 0.0292(13) 0.0226(13) -0.0009(10) 0.0044(10) 0.0017(10) C38 0.0256(12) 0.0378(15) 0.0288(14) -0.0040(12) 0.0065(11) -0.0066(11) C39 0.0411(15) 0.0251(13) 0.0334(15) -0.0031(11) 0.0099(12) -0.0052(12) C40 0.0373(15) 0.0260(14) 0.0425(17) 0.0022(12) 0.0049(13) 0.0028(11) C41 0.0253(13) 0.0327(14) 0.0320(14) 0.0008(11) 0.0005(11) 0.0006(11) C42 0.0222(12) 0.0218(12) 0.0275(13) 0.0019(10) 0.0016(10) -0.0007(9) C43 0.0277(13) 0.0334(14) 0.0281(14) 0.0063(11) -0.0007(11) -0.0026(11) C44 0.0334(15) 0.0427(17) 0.0412(17) 0.0074(13) -0.0121(13) -0.0028(13) C45 0.0217(13) 0.0474(18) 0.062(2) 0.0067(16) -0.0043(14) 0.0004(12) C46 0.0280(14) 0.0499(18) 0.054(2) -0.0021(15) 0.0142(14) 0.0028(13) C47 0.0282(13) 0.0394(16) 0.0345(15) -0.0033(12) 0.0053(12) 0.0018(12) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ni1 C9 1.889(2) . ? Ni1 O1 1.9048(16) . ? Ni1 P1 2.1833(7) . ? Ni1 P2 2.2184(7) . ? P1 C2 1.774(2) . ? P1 C23 1.816(2) . ? P1 C16 1.817(3) . ? P2 C36 1.826(2) . ? P2 C30 1.827(2) . ? P2 C42 1.827(2) . ? O1 C1 1.313(3) . ? O2 C14 1.365(3) . ? O2 C15 1.420(4) . ? O3 C28 1.360(3) . ? O3 C29 1.420(3) . ? O4 C17 1.362(3) . ? O4 C22 1.428(3) . ? C1 C2 1.356(3) . ? C1 C3 1.497(3) . ? C2 H2 0.9500 . ? C3 C4 1.382(3) . ? C3 C8 1.385(4) . ? C4 C5 1.385(4) . ? C4 H4 0.9500 . ? C5 C6 1.379(4) . ? C5 H5 0.9500 . ? C6 C7 1.369(4) . ? C6 H6 0.9500 . ? C7 C8 1.381(4) . ? C7 H7 0.9500 . ? C8 H8 0.9500 . ? C9 C14 1.388(4) . ? C9 C10 1.408(4) . ? C10 C11 1.402(4) . ? C10 H10 0.9500 . ? C11 C12 1.373(5) . ? C11 H11 0.9500 . ? C12 C13 1.385(5) . ? C12 H12 0.9500 . ? C13 C14 1.393(4) . ? C13 H13 0.9500 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 C21 1.387(4) . ? C16 C17 1.406(4) . ? C17 C18 1.391(4) . ? C18 C19 1.379(4) . ? C18 H18 0.9500 . ? C19 C20 1.380(4) . ? C19 H19 0.9500 . ? C20 C21 1.384(4) . ? C20 H20 0.9500 . ? C21 H21 0.9500 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 C24 1.381(4) . ? C23 C28 1.399(3) . ? C24 C25 1.382(4) . ? C24 H24 0.9500 . ? C25 C26 1.374(4) . ? C25 H25 0.9500 . ? C26 C27 1.376(4) . ? C26 H26 0.9500 . ? C27 C28 1.389(3) . ? C27 H27 0.9500 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C30 C31 1.388(4) . ? C30 C35 1.394(4) . ? C31 C32 1.382(4) . ? C31 H31 0.9500 . ? C32 C33 1.376(5) . ? C32 H32 0.9500 . ? C33 C34 1.371(5) . ? C33 H33 0.9500 . ? C34 C35 1.386(4) . ? C34 H34 0.9500 . ? C35 H35 0.9500 . ? C36 C41 1.388(3) . ? C36 C37 1.394(3) . ? C37 C38 1.379(4) . ? C37 H37 0.9500 . ? C38 C39 1.377(4) . ? C38 H38 0.9500 . ? C39 C40 1.374(4) . ? C39 H39 0.9500 . ? C40 C41 1.396(4) . ? C40 H40 0.9500 . ? C41 H41 0.9500 . ? C42 C43 1.382(3) . ? C42 C47 1.393(4) . ? C43 C44 1.394(4) . ? C43 H43 0.9500 . ? C44 C45 1.368(4) . ? C44 H44 0.9500 . ? C45 C46 1.380(4) . ? C45 H45 0.9500 . ? C46 C47 1.381(4) . ? C46 H46 0.9500 . ? C47 H47 0.9500 . ? 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 _geom_angle_publ_flag C9 Ni1 O1 173.18(10) . . ? C9 Ni1 P1 96.21(8) . . ? O1 Ni1 P1 86.21(5) . . ? C9 Ni1 P2 92.96(8) . . ? O1 Ni1 P2 85.00(5) . . ? P1 Ni1 P2 170.37(3) . . ? C2 P1 C23 109.93(11) . . ? C2 P1 C16 106.86(12) . . ? C23 P1 C16 108.58(11) . . ? C2 P1 Ni1 98.93(8) . . ? C23 P1 Ni1 112.61(8) . . ? C16 P1 Ni1 119.16(9) . . ? C36 P2 C30 101.70(11) . . ? C36 P2 C42 104.46(11) . . ? C30 P2 C42 105.32(11) . . ? C36 P2 Ni1 124.82(8) . . ? C30 P2 Ni1 113.12(9) . . ? C42 P2 Ni1 105.75(8) . . ? C1 O1 Ni1 119.29(15) . . ? C14 O2 C15 118.2(2) . . ? C28 O3 C29 118.4(2) . . ? C17 O4 C22 117.3(2) . . ? O1 C1 C2 122.5(2) . . ? O1 C1 C3 113.3(2) . . ? C2 C1 C3 124.0(2) . . ? C1 C2 P1 112.70(19) . . ? C1 C2 H2 123.7 . . ? P1 C2 H2 123.7 . . ? C4 C3 C8 118.6(2) . . ? C4 C3 C1 118.4(2) . . ? C8 C3 C1 123.0(2) . . ? C3 C4 C5 120.8(3) . . ? C3 C4 H4 119.6 . . ? C5 C4 H4 119.6 . . ? C6 C5 C4 119.8(3) . . ? C6 C5 H5 120.1 . . ? C4 C5 H5 120.1 . . ? C7 C6 C5 119.9(3) . . ? C7 C6 H6 120.1 . . ? C5 C6 H6 120.1 . . ? C6 C7 C8 120.3(3) . . ? C6 C7 H7 119.8 . . ? C8 C7 H7 119.8 . . ? C7 C8 C3 120.6(3) . . ? C7 C8 H8 119.7 . . ? C3 C8 H8 119.7 . . ? C14 C9 C10 117.8(2) . . ? C14 C9 Ni1 122.3(2) . . ? C10 C9 Ni1 119.5(2) . . ? C11 C10 C9 120.6(3) . . ? C11 C10 H10 119.7 . . ? C9 C10 H10 119.7 . . ? C12 C11 C10 119.6(3) . . ? C12 C11 H11 120.2 . . ? C10 C11 H11 120.2 . . ? C11 C12 C13 121.3(3) . . ? C11 C12 H12 119.4 . . ? C13 C12 H12 119.4 . . ? C12 C13 C14 118.7(3) . . ? C12 C13 H13 120.6 . . ? C14 C13 H13 120.6 . . ? O2 C14 C9 114.4(2) . . ? O2 C14 C13 123.5(3) . . ? C9 C14 C13 122.0(3) . . ? O2 C15 H15A 109.5 . . ? O2 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? O2 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C21 C16 C17 118.6(2) . . ? C21 C16 P1 118.83(19) . . ? C17 C16 P1 122.5(2) . . ? O4 C17 C18 124.3(2) . . ? O4 C17 C16 115.8(2) . . ? C18 C17 C16 119.9(3) . . ? C19 C18 C17 119.9(3) . . ? C19 C18 H18 120.1 . . ? C17 C18 H18 120.1 . . ? C18 C19 C20 120.9(3) . . ? C18 C19 H19 119.5 . . ? C20 C19 H19 119.5 . . ? C19 C20 C21 119.3(3) . . ? C19 C20 H20 120.4 . . ? C21 C20 H20 120.4 . . ? C20 C21 C16 121.4(3) . . ? C20 C21 H21 119.3 . . ? C16 C21 H21 119.3 . . ? O4 C22 H22A 109.5 . . ? O4 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? O4 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C24 C23 C28 118.4(2) . . ? C24 C23 P1 117.58(18) . . ? C28 C23 P1 122.85(19) . . ? C23 C24 C25 121.2(2) . . ? C23 C24 H24 119.4 . . ? C25 C24 H24 119.4 . . ? C26 C25 C24 119.7(3) . . ? C26 C25 H25 120.2 . . ? C24 C25 H25 120.2 . . ? C25 C26 C27 120.7(2) . . ? C25 C26 H26 119.6 . . ? C27 C26 H26 119.6 . . ? C26 C27 C28 119.5(2) . . ? C26 C27 H27 120.2 . . ? C28 C27 H27 120.2 . . ? O3 C28 C27 123.9(2) . . ? O3 C28 C23 115.6(2) . . ? C27 C28 C23 120.5(2) . . ? O3 C29 H29A 109.5 . . ? O3 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? O3 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C31 C30 C35 118.9(2) . . ? C31 C30 P2 120.2(2) . . ? C35 C30 P2 121.0(2) . . ? C32 C31 C30 120.0(3) . . ? C32 C31 H31 120.0 . . ? C30 C31 H31 120.0 . . ? C33 C32 C31 120.9(3) . . ? C33 C32 H32 119.6 . . ? C31 C32 H32 119.6 . . ? C34 C33 C32 119.5(3) . . ? C34 C33 H33 120.3 . . ? C32 C33 H33 120.3 . . ? C33 C34 C35 120.5(3) . . ? C33 C34 H34 119.7 . . ? C35 C34 H34 119.7 . . ? C34 C35 C30 120.2(3) . . ? C34 C35 H35 119.9 . . ? C30 C35 H35 119.9 . . ? C41 C36 C37 118.4(2) . . ? C41 C36 P2 122.33(18) . . ? C37 C36 P2 119.21(18) . . ? C38 C37 C36 120.4(2) . . ? C38 C37 H37 119.8 . . ? C36 C37 H37 119.8 . . ? C39 C38 C37 120.7(2) . . ? C39 C38 H38 119.6 . . ? C37 C38 H38 119.6 . . ? C40 C39 C38 120.0(2) . . ? C40 C39 H39 120.0 . . ? C38 C39 H39 120.0 . . ? C39 C40 C41 119.6(2) . . ? C39 C40 H40 120.2 . . ? C41 C40 H40 120.2 . . ? C36 C41 C40 120.9(2) . . ? C36 C41 H41 119.6 . . ? C40 C41 H41 119.6 . . ? C43 C42 C47 119.0(2) . . ? C43 C42 P2 123.8(2) . . ? C47 C42 P2 117.02(19) . . ? C42 C43 C44 120.1(3) . . ? C42 C43 H43 119.9 . . ? C44 C43 H43 119.9 . . ? C45 C44 C43 120.3(3) . . ? C45 C44 H44 119.8 . . ? C43 C44 H44 119.8 . . ? C44 C45 C46 119.9(3) . . ? C44 C45 H45 120.1 . . ? C46 C45 H45 120.1 . . ? C45 C46 C47 120.3(3) . . ? C45 C46 H46 119.8 . . ? C47 C46 H46 119.8 . . ? C46 C47 C42 120.3(3) . . ? C46 C47 H47 119.9 . . ? C42 C47 H47 119.9 . . ? 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_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C9 Ni1 P1 C2 -170.28(12) . . . . ? O1 Ni1 P1 C2 3.32(10) . . . . ? P2 Ni1 P1 C2 27.6(2) . . . . ? C9 Ni1 P1 C23 -54.23(12) . . . . ? O1 Ni1 P1 C23 119.37(10) . . . . ? P2 Ni1 P1 C23 143.61(18) . . . . ? C9 Ni1 P1 C16 74.65(12) . . . . ? O1 Ni1 P1 C16 -111.75(10) . . . . ? P2 Ni1 P1 C16 -87.52(19) . . . . ? C9 Ni1 P2 C36 -19.62(13) . . . . ? O1 Ni1 P2 C36 166.90(11) . . . . ? P1 Ni1 P2 C36 142.63(18) . . . . ? C9 Ni1 P2 C30 104.81(12) . . . . ? O1 Ni1 P2 C30 -68.66(10) . . . . ? P1 Ni1 P2 C30 -92.94(19) . . . . ? C9 Ni1 P2 C42 -140.43(12) . . . . ? O1 Ni1 P2 C42 46.09(10) . . . . ? P1 Ni1 P2 C42 21.8(2) . . . . ? C9 Ni1 O1 C1 110.0(8) . . . . ? P1 Ni1 O1 C1 -1.01(17) . . . . ? P2 Ni1 O1 C1 -177.06(17) . . . . ? Ni1 O1 C1 C2 -3.0(3) . . . . ? Ni1 O1 C1 C3 174.04(15) . . . . ? O1 C1 C2 P1 6.1(3) . . . . ? C3 C1 C2 P1 -170.59(18) . . . . ? C23 P1 C2 C1 -123.72(19) . . . . ? C16 P1 C2 C1 118.6(2) . . . . ? Ni1 P1 C2 C1 -5.6(2) . . . . ? O1 C1 C3 C4 -21.9(3) . . . . ? C2 C1 C3 C4 155.1(3) . . . . ? O1 C1 C3 C8 160.9(2) . . . . ? C2 C1 C3 C8 -22.1(4) . . . . ? C8 C3 C4 C5 1.4(4) . . . . ? C1 C3 C4 C5 -176.0(2) . . . . ? C3 C4 C5 C6 -1.3(4) . . . . ? C4 C5 C6 C7 0.2(5) . . . . ? C5 C6 C7 C8 0.8(5) . . . . ? C6 C7 C8 C3 -0.7(4) . . . . ? C4 C3 C8 C7 -0.4(4) . . . . ? C1 C3 C8 C7 176.9(2) . . . . ? O1 Ni1 C9 C14 141.6(7) . . . . ? P1 Ni1 C9 C14 -107.9(2) . . . . ? P2 Ni1 C9 C14 69.1(2) . . . . ? O1 Ni1 C9 C10 -30.9(9) . . . . ? P1 Ni1 C9 C10 79.6(2) . . . . ? P2 Ni1 C9 C10 -103.3(2) . . . . ? C14 C9 C10 C11 -0.2(4) . . . . ? Ni1 C9 C10 C11 172.6(2) . . . . ? C9 C10 C11 C12 -0.1(5) . . . . ? C10 C11 C12 C13 -0.1(5) . . . . ? C11 C12 C13 C14 0.6(5) . . . . ? C15 O2 C14 C9 -171.0(3) . . . . ? C15 O2 C14 C13 6.5(4) . . . . ? C10 C9 C14 O2 178.3(2) . . . . ? Ni1 C9 C14 O2 5.7(3) . . . . ? C10 C9 C14 C13 0.7(4) . . . . ? Ni1 C9 C14 C13 -171.9(2) . . . . ? C12 C13 C14 O2 -178.3(3) . . . . ? C12 C13 C14 C9 -0.9(4) . . . . ? C2 P1 C16 C21 -122.6(2) . . . . ? C23 P1 C16 C21 118.83(19) . . . . ? Ni1 P1 C16 C21 -11.9(2) . . . . ? C2 P1 C16 C17 54.7(2) . . . . ? C23 P1 C16 C17 -63.8(2) . . . . ? Ni1 P1 C16 C17 165.50(16) . . . . ? C22 O4 C17 C18 7.8(4) . . . . ? C22 O4 C17 C16 -171.0(2) . . . . ? C21 C16 C17 O4 179.5(2) . . . . ? P1 C16 C17 O4 2.1(3) . . . . ? C21 C16 C17 C18 0.6(4) . . . . ? P1 C16 C17 C18 -176.77(18) . . . . ? O4 C17 C18 C19 -179.3(2) . . . . ? C16 C17 C18 C19 -0.5(4) . . . . ? C17 C18 C19 C20 -0.1(4) . . . . ? C18 C19 C20 C21 0.5(4) . . . . ? C19 C20 C21 C16 -0.4(4) . . . . ? C17 C16 C21 C20 -0.1(4) . . . . ? P1 C16 C21 C20 177.3(2) . . . . ? C2 P1 C23 C24 32.7(2) . . . . ? C16 P1 C23 C24 149.3(2) . . . . ? Ni1 P1 C23 C24 -76.6(2) . . . . ? C2 P1 C23 C28 -160.0(2) . . . . ? C16 P1 C23 C28 -43.4(2) . . . . ? Ni1 P1 C23 C28 90.7(2) . . . . ? C28 C23 C24 C25 -0.6(4) . . . . ? P1 C23 C24 C25 167.3(2) . . . . ? C23 C24 C25 C26 0.1(4) . . . . ? C24 C25 C26 C27 0.8(5) . . . . ? C25 C26 C27 C28 -1.1(4) . . . . ? C29 O3 C28 C27 7.6(4) . . . . ? C29 O3 C28 C23 -171.3(3) . . . . ? C26 C27 C28 O3 -178.3(3) . . . . ? C26 C27 C28 C23 0.5(4) . . . . ? C24 C23 C28 O3 179.2(2) . . . . ? P1 C23 C28 O3 12.0(3) . . . . ? C24 C23 C28 C27 0.3(4) . . . . ? P1 C23 C28 C27 -166.9(2) . . . . ? C36 P2 C30 C31 150.9(2) . . . . ? C42 P2 C30 C31 -100.4(2) . . . . ? Ni1 P2 C30 C31 14.6(2) . . . . ? C36 P2 C30 C35 -29.3(2) . . . . ? C42 P2 C30 C35 79.5(2) . . . . ? Ni1 P2 C30 C35 -165.51(18) . . . . ? C35 C30 C31 C32 -0.3(4) . . . . ? P2 C30 C31 C32 179.5(2) . . . . ? C30 C31 C32 C33 0.0(5) . . . . ? C31 C32 C33 C34 0.7(5) . . . . ? C32 C33 C34 C35 -1.0(5) . . . . ? C33 C34 C35 C30 0.6(4) . . . . ? C31 C30 C35 C34 0.1(4) . . . . ? P2 C30 C35 C34 -179.8(2) . . . . ? C30 P2 C36 C41 108.8(2) . . . . ? C42 P2 C36 C41 -0.6(2) . . . . ? Ni1 P2 C36 C41 -122.01(19) . . . . ? C30 P2 C36 C37 -69.7(2) . . . . ? C42 P2 C36 C37 -179.10(19) . . . . ? Ni1 P2 C36 C37 59.5(2) . . . . ? C41 C36 C37 C38 -0.1(4) . . . . ? P2 C36 C37 C38 178.43(19) . . . . ? C36 C37 C38 C39 -0.4(4) . . . . ? C37 C38 C39 C40 0.6(4) . . . . ? C38 C39 C40 C41 -0.3(4) . . . . ? C37 C36 C41 C40 0.4(4) . . . . ? P2 C36 C41 C40 -178.1(2) . . . . ? C39 C40 C41 C36 -0.2(4) . . . . ? C36 P2 C42 C43 92.9(2) . . . . ? C30 P2 C42 C43 -13.8(2) . . . . ? Ni1 P2 C42 C43 -133.8(2) . . . . ? C36 P2 C42 C47 -91.6(2) . . . . ? C30 P2 C42 C47 161.6(2) . . . . ? Ni1 P2 C42 C47 41.6(2) . . . . ? C47 C42 C43 C44 0.0(4) . . . . ? P2 C42 C43 C44 175.4(2) . . . . ? C42 C43 C44 C45 -0.6(4) . . . . ? C43 C44 C45 C46 0.8(5) . . . . ? C44 C45 C46 C47 -0.4(5) . . . . ? C45 C46 C47 C42 -0.1(5) . . . . ? C43 C42 C47 C46 0.3(4) . . . . ? P2 C42 C47 C46 -175.4(2) . . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.508 _refine_diff_density_min -0.276 _refine_diff_density_rms 0.063