Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2004 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Prof Bun Yeoul Lee' _publ_contact_author_address ; Department of Molecular Science and Technology Ajou University Suwon 442-749 KOREA ; _publ_contact_author_email BUNYEOUL@AJOU.AC.KR _publ_section_title ; Synthesis, characterization, and ethylene reactivity of 2-diphenylphosphanylbenzamido nickel complexes ; loop_ _publ_author_name 'Bun Yeoul Lee' 'Young Keun Chung' 'Heon Yong Kwon' 'Su Yeon Lee' 'Dong Mok Shin' data_7 _database_code_depnum_ccdc_archive 'CCDC 228028' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C41 H41 N Ni O P2' _chemical_formula_weight 684.40 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' N N 0.0061 0.0033 '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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclnic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.0570(10) _cell_length_b 12.1230(10) _cell_length_c 13.9160(10) _cell_angle_alpha 102.270(5) _cell_angle_beta 109.119(5) _cell_angle_gamma 95.366(4) _cell_volume 1848.4(3) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 4240 _cell_measurement_theta_min 0.998 _cell_measurement_theta_max 25.028 _exptl_crystal_description block _exptl_crystal_colour brown _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.230 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 720 _exptl_absorpt_coefficient_mu 0.643 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _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 KappaCCD _diffrn_measurement_method CCD _diffrn_detector_area_resol_mean 9 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8431 _diffrn_reflns_av_R_equivalents 0.1013 _diffrn_reflns_av_sigmaI/netI 0.2650 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 3.73 _diffrn_reflns_theta_max 25.25 _reflns_number_total 5613 _reflns_number_gt 2099 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP 32' _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^)+(0.0719P)^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 mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0040(18) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 5613 _refine_ls_number_parameters 406 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.2605 _refine_ls_R_factor_gt 0.0914 _refine_ls_wR_factor_ref 0.2142 _refine_ls_wR_factor_gt 0.1593 _refine_ls_goodness_of_fit_ref 1.006 _refine_ls_restrained_S_all 1.006 _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 0.68948(11) 0.80144(9) 0.39334(10) 0.0645(5) Uani 1 1 d . . . P1 P 0.5255(2) 0.82244(19) 0.2768(2) 0.0614(8) Uani 1 1 d . . . P2 P 0.8073(3) 0.7890(2) 0.5459(2) 0.0755(9) Uani 1 1 d . . . O1 O 0.4786(6) 0.4766(5) 0.3065(6) 0.105(3) Uani 1 1 d . . . N1 N 0.6189(7) 0.6362(6) 0.3440(5) 0.059(2) Uani 1 1 d . . . C1 C 0.5105(9) 0.5807(8) 0.3324(7) 0.066(3) Uani 1 1 d . . . C2 C 0.4191(8) 0.6540(8) 0.3469(7) 0.061(3) Uani 1 1 d . . . C3 C 0.4134(8) 0.7586(7) 0.3193(7) 0.059(3) Uani 1 1 d . . . C4 C 0.3187(10) 0.8108(8) 0.3267(7) 0.075(3) Uani 1 1 d . . . H4 H 0.3114 0.8794 0.3074 0.090 Uiso 1 1 calc R . . C5 C 0.2332(9) 0.7650(10) 0.3621(8) 0.085(3) Uani 1 1 d . . . H5 H 0.1705 0.8025 0.3665 0.103 Uiso 1 1 calc R . . C6 C 0.2438(11) 0.6651(10) 0.3896(9) 0.091(4) Uani 1 1 d . . . H6 H 0.1892 0.6342 0.4152 0.109 Uiso 1 1 calc R . . C7 C 0.3345(11) 0.6093(8) 0.3799(8) 0.087(3) Uani 1 1 d . . . H7 H 0.3385 0.5389 0.3962 0.105 Uiso 1 1 calc R . . C8 C 0.4880(8) 0.9626(7) 0.2653(8) 0.060(3) Uani 1 1 d . . . C9 C 0.5101(8) 1.0465(8) 0.3563(8) 0.074(3) Uani 1 1 d . . . H9 H 0.5331 1.0272 0.4204 0.089 Uiso 1 1 calc R . . C10 C 0.4992(10) 1.1572(10) 0.3554(11) 0.093(4) Uani 1 1 d . . . H10 H 0.5163 1.2123 0.4185 0.111 Uiso 1 1 calc R . . C11 C 0.4622(11) 1.1886(10) 0.2595(13) 0.107(4) Uani 1 1 d . . . H11 H 0.4562 1.2643 0.2587 0.128 Uiso 1 1 calc R . . C12 C 0.4353(10) 1.1060(10) 0.1676(11) 0.102(4) Uani 1 1 d . . . H12 H 0.4080 1.1239 0.1031 0.122 Uiso 1 1 calc R . . C13 C 0.4495(9) 0.9945(9) 0.1728(9) 0.088(3) Uani 1 1 d . . . H13 H 0.4319 0.9387 0.1101 0.106 Uiso 1 1 calc R . . C14 C 0.4898(9) 0.7393(7) 0.1416(7) 0.059(2) Uani 1 1 d . . . C15 C 0.5750(10) 0.7454(8) 0.0974(9) 0.081(3) Uani 1 1 d . . . H15 H 0.6492 0.7910 0.1368 0.097 Uiso 1 1 calc R . . C16 C 0.5529(14) 0.6845(11) -0.0058(11) 0.097(4) Uani 1 1 d . . . H16 H 0.6109 0.6898 -0.0360 0.117 Uiso 1 1 calc R . . C17 C 0.4438(18) 0.6168(12) -0.0615(10) 0.124(5) Uani 1 1 d . . . H17 H 0.4278 0.5756 -0.1304 0.149 Uiso 1 1 calc R . . C18 C 0.3587(14) 0.6080(12) -0.0191(12) 0.139(6) Uani 1 1 d . . . H18 H 0.2853 0.5609 -0.0585 0.167 Uiso 1 1 calc R . . C19 C 0.3806(10) 0.6688(10) 0.0824(9) 0.093(4) Uani 1 1 d . . . H19 H 0.3218 0.6626 0.1116 0.112 Uiso 1 1 calc R . . C20 C 0.7077(9) 0.5696(9) 0.3298(7) 0.065(3) Uani 1 1 d . . . C21 C 0.7211(10) 0.4675(9) 0.3576(8) 0.085(3) Uani 1 1 d . . . H21 H 0.6680 0.4343 0.3834 0.101 Uiso 1 1 calc R . . C22 C 0.8158(14) 0.4153(10) 0.3464(11) 0.121(5) Uani 1 1 d . . . H22 H 0.8270 0.3473 0.3660 0.145 Uiso 1 1 calc R . . C23 C 0.8924(12) 0.4635(14) 0.3065(11) 0.119(5) Uani 1 1 d . . . H23 H 0.9553 0.4278 0.2994 0.142 Uiso 1 1 calc R . . C24 C 0.8780(12) 0.5626(12) 0.2773(9) 0.101(4) Uani 1 1 d . . . H24 H 0.9310 0.5949 0.2509 0.121 Uiso 1 1 calc R . . C25 C 0.7857(10) 0.6141(9) 0.2868(8) 0.082(3) Uani 1 1 d . . . H25 H 0.7742 0.6805 0.2643 0.098 Uiso 1 1 calc R . . C26 C 0.7831(8) 0.9555(7) 0.4213(8) 0.072(3) Uani 1 1 d . . . H26A H 0.7399 1.0141 0.4421 0.108 Uiso 1 1 calc R . . H26B H 0.8588 0.9652 0.4782 0.108 Uiso 1 1 calc R . . C27 C 0.8038(11) 0.9670(11) 0.3247(10) 0.086(3) Uani 1 1 d . . . C28 C 0.7546(10) 1.0396(11) 0.2669(11) 0.099(4) Uani 1 1 d . . . H28 H 0.7079 1.0866 0.2918 0.119 Uiso 1 1 calc R . . C29 C 0.7688(15) 1.0488(15) 0.1736(14) 0.140(6) Uani 1 1 d . . . H29 H 0.7325 1.0987 0.1362 0.168 Uiso 1 1 calc R . . C30 C 0.8426(19) 0.977(2) 0.1388(17) 0.160(8) Uani 1 1 d . . . H30 H 0.8552 0.9803 0.0769 0.192 Uiso 1 1 calc R . . C31 C 0.8936(16) 0.9051(16) 0.1918(17) 0.146(7) Uani 1 1 d . . . H31 H 0.9401 0.8580 0.1668 0.176 Uiso 1 1 calc R . . C32 C 0.8774(11) 0.9012(11) 0.2836(13) 0.109(4) Uani 1 1 d . . . H32 H 0.9166 0.8528 0.3214 0.131 Uiso 1 1 calc R . . C33 C 0.8226(10) 0.9112(8) 0.6547(7) 0.094(3) Uani 1 1 d . . . H33A H 0.7467 0.9146 0.6625 0.141 Uiso 1 1 calc R . . H33B H 0.8499 0.9806 0.6402 0.141 Uiso 1 1 calc R . . H33C H 0.8792 0.9025 0.7185 0.141 Uiso 1 1 calc R . . C34 C 0.9605(8) 0.7741(9) 0.5606(8) 0.098(4) Uani 1 1 d . . . H34A H 1.0032 0.7714 0.6314 0.148 Uiso 1 1 calc R . . H34B H 0.9982 0.8384 0.5458 0.148 Uiso 1 1 calc R . . H34C H 0.9608 0.7046 0.5124 0.148 Uiso 1 1 calc R . . C35 C 0.7586(9) 0.6717(7) 0.5892(7) 0.104(4) Uani 1 1 d . . . H35A H 0.7491 0.6012 0.5380 0.157 Uiso 1 1 calc R . . H35B H 0.6838 0.6800 0.5978 0.157 Uiso 1 1 calc R . . H35C H 0.8168 0.6708 0.6553 0.157 Uiso 1 1 calc R . . C01 C 0.1753(9) 0.3693(8) 0.1131(6) 0.212(9) Uani 1 1 d R . . H01 H 0.2526 0.4104 0.1466 0.255 Uiso 1 1 calc R . . C02 C 0.1505(9) 0.2565(7) 0.1158(6) 0.221(10) Uani 1 1 d R . . H02 H 0.2112 0.2218 0.1512 0.265 Uiso 1 1 calc R . . C03 C 0.0356(9) 0.1954(8) 0.0660(6) 0.237(11) Uani 1 1 d R . . H03 H 0.0190 0.1195 0.0678 0.284 Uiso 1 1 calc R . . C04 C -0.0546(8) 0.2469(8) 0.0134(6) 0.261(13) Uani 1 1 d R . . H04 H -0.1319 0.2058 -0.0202 0.313 Uiso 1 1 calc R . . C05 C -0.0298(8) 0.3597(8) 0.0106(6) 0.53(4) Uani 1 1 d R . . H05 H -0.0905 0.3944 -0.0248 0.636 Uiso 1 1 calc R . . C06 C 0.0851(8) 0.4209(8) 0.0605(6) 0.49(4) Uani 1 1 d R . . H06 H 0.1018 0.4967 0.0586 0.583 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 0.0632(9) 0.0412(7) 0.0760(10) 0.0160(6) 0.0093(7) 0.0016(6) P1 0.0638(19) 0.0414(14) 0.0727(18) 0.0170(13) 0.0165(16) 0.0039(13) P2 0.082(2) 0.0468(16) 0.083(2) 0.0170(15) 0.0109(18) 0.0045(15) O1 0.098(6) 0.035(4) 0.172(7) 0.017(4) 0.045(5) 0.003(4) N1 0.064(6) 0.040(4) 0.065(5) 0.013(4) 0.012(5) 0.003(5) C1 0.070(8) 0.040(6) 0.083(7) 0.009(5) 0.026(6) -0.001(6) C2 0.060(7) 0.040(6) 0.071(7) 0.004(5) 0.016(6) 0.004(6) C3 0.057(7) 0.042(6) 0.078(7) 0.006(5) 0.027(6) 0.011(5) C4 0.071(8) 0.054(6) 0.084(8) 0.015(6) 0.012(7) -0.003(6) C5 0.055(7) 0.080(8) 0.123(9) 0.021(7) 0.035(7) 0.016(6) C6 0.099(10) 0.070(8) 0.131(10) 0.042(7) 0.063(8) 0.022(7) C7 0.101(9) 0.057(7) 0.116(9) 0.035(6) 0.049(8) 0.004(7) C8 0.059(7) 0.041(5) 0.067(7) 0.016(6) 0.004(6) 0.003(5) C9 0.082(8) 0.040(6) 0.087(8) 0.013(6) 0.015(7) 0.006(6) C10 0.087(9) 0.062(8) 0.114(11) 0.006(8) 0.031(8) -0.005(7) C11 0.112(11) 0.047(7) 0.151(13) 0.025(9) 0.034(10) 0.018(7) C12 0.118(11) 0.063(8) 0.116(10) 0.052(8) 0.011(9) 0.019(8) C13 0.101(9) 0.072(8) 0.085(8) 0.035(7) 0.018(7) 0.012(7) C14 0.063(7) 0.045(5) 0.057(6) 0.013(5) 0.010(7) -0.001(5) C15 0.105(10) 0.067(7) 0.074(9) 0.020(7) 0.035(8) 0.009(6) C16 0.138(13) 0.088(9) 0.089(11) 0.038(8) 0.057(10) 0.039(9) C17 0.164(16) 0.112(11) 0.067(9) 0.004(8) 0.017(12) 0.012(12) C18 0.124(13) 0.156(14) 0.101(13) -0.012(10) 0.035(11) -0.030(10) C19 0.074(9) 0.111(9) 0.063(8) -0.002(7) 0.007(7) -0.013(8) C20 0.058(7) 0.056(7) 0.074(7) 0.017(6) 0.011(6) 0.021(6) C21 0.089(9) 0.066(7) 0.103(9) 0.029(6) 0.030(7) 0.031(7) C22 0.126(12) 0.079(9) 0.171(14) 0.051(9) 0.049(11) 0.053(10) C23 0.083(11) 0.113(13) 0.135(12) 0.001(10) 0.019(9) 0.039(10) C24 0.101(11) 0.084(9) 0.121(10) 0.024(8) 0.042(9) 0.029(8) C25 0.071(8) 0.062(7) 0.103(9) 0.016(6) 0.023(7) 0.005(7) C26 0.075(8) 0.041(6) 0.083(8) 0.026(5) 0.003(7) -0.001(5) C27 0.062(8) 0.073(8) 0.100(10) 0.023(8) 0.008(8) -0.021(6) C28 0.084(9) 0.102(9) 0.103(10) 0.044(8) 0.023(8) -0.030(8) C29 0.106(13) 0.159(16) 0.127(14) 0.059(12) 0.010(11) -0.044(11) C30 0.146(19) 0.17(2) 0.154(18) 0.054(15) 0.053(15) -0.043(15) C31 0.145(16) 0.141(16) 0.156(17) -0.007(12) 0.102(15) -0.036(13) C32 0.085(10) 0.095(10) 0.150(14) 0.046(9) 0.042(10) -0.003(8) C33 0.111(9) 0.065(7) 0.084(8) 0.016(6) 0.009(7) 0.011(7) C34 0.073(8) 0.087(8) 0.122(9) 0.025(7) 0.012(7) 0.034(7) C35 0.142(11) 0.056(7) 0.103(9) 0.033(6) 0.025(8) 0.001(7) C01 0.153(18) 0.19(2) 0.27(2) 0.055(18) 0.051(17) 0.004(16) C02 0.22(3) 0.29(3) 0.175(18) 0.07(2) 0.096(19) 0.05(2) C03 0.20(2) 0.29(3) 0.28(3) 0.16(2) 0.10(2) 0.04(2) C04 0.17(2) 0.32(3) 0.38(3) 0.21(3) 0.10(2) 0.12(2) C05 0.30(5) 0.39(5) 0.92(11) 0.41(7) 0.11(6) 0.05(4) C06 0.22(3) 0.34(5) 0.94(11) 0.36(6) 0.13(5) 0.09(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 C26 1.981(8) . ? Ni1 N1 1.981(7) . ? Ni1 P2 2.179(3) . ? Ni1 P1 2.185(3) . ? P1 C3 1.816(9) . ? P1 C14 1.823(9) . ? P1 C8 1.825(9) . ? P2 C35 1.780(8) . ? P2 C34 1.820(9) . ? P2 C33 1.826(9) . ? O1 C1 1.224(9) . ? N1 C1 1.355(10) . ? N1 C20 1.439(10) . ? C1 C2 1.515(12) . ? C2 C7 1.362(11) . ? C2 C3 1.403(11) . ? C3 C4 1.378(11) . ? C4 C5 1.398(12) . ? C5 C6 1.351(12) . ? C6 C7 1.367(12) . ? C8 C13 1.369(11) . ? C8 C9 1.375(11) . ? C9 C10 1.362(13) . ? C10 C11 1.409(14) . ? C11 C12 1.365(14) . ? C12 C13 1.393(13) . ? C14 C15 1.363(12) . ? C14 C19 1.387(12) . ? C15 C16 1.393(13) . ? C16 C17 1.366(16) . ? C17 C18 1.346(16) . ? C18 C19 1.372(14) . ? C20 C21 1.381(12) . ? C20 C25 1.394(12) . ? C21 C22 1.391(14) . ? C22 C23 1.370(15) . ? C23 C24 1.356(15) . ? C24 C25 1.355(13) . ? C26 C27 1.477(14) . ? C27 C28 1.364(14) . ? C27 C32 1.422(15) . ? C28 C29 1.389(16) . ? C29 C30 1.43(2) . ? C30 C31 1.32(2) . ? C31 C32 1.364(17) . ? C01 C06 1.3815 . ? C01 C02 1.3831 . ? C02 C03 1.3822 . ? C03 C04 1.3817 . ? C04 C05 1.3830 . ? C05 C06 1.3825 . ? 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 C26 Ni1 N1 166.1(4) . . ? C26 Ni1 P2 88.4(3) . . ? N1 Ni1 P2 94.2(2) . . ? C26 Ni1 P1 97.9(3) . . ? N1 Ni1 P1 84.9(2) . . ? P2 Ni1 P1 157.23(11) . . ? C3 P1 C14 104.7(4) . . ? C3 P1 C8 104.7(4) . . ? C14 P1 C8 104.8(4) . . ? C3 P1 Ni1 101.2(3) . . ? C14 P1 Ni1 116.5(3) . . ? C8 P1 Ni1 122.8(3) . . ? C35 P2 C34 102.6(5) . . ? C35 P2 C33 101.9(4) . . ? C34 P2 C33 104.0(5) . . ? C35 P2 Ni1 114.8(3) . . ? C34 P2 Ni1 117.7(4) . . ? C33 P2 Ni1 113.8(3) . . ? C1 N1 C20 118.8(7) . . ? C1 N1 Ni1 131.1(6) . . ? C20 N1 Ni1 109.7(6) . . ? O1 C1 N1 125.5(9) . . ? O1 C1 C2 117.3(9) . . ? N1 C1 C2 117.1(8) . . ? C7 C2 C3 120.2(9) . . ? C7 C2 C1 117.0(9) . . ? C3 C2 C1 122.6(8) . . ? C4 C3 C2 116.6(8) . . ? C4 C3 P1 121.7(7) . . ? C2 C3 P1 121.7(7) . . ? C3 C4 C5 122.8(9) . . ? C6 C5 C4 118.5(10) . . ? C5 C6 C7 120.1(10) . . ? C2 C7 C6 121.8(10) . . ? C13 C8 C9 116.8(9) . . ? C13 C8 P1 124.8(8) . . ? C9 C8 P1 118.2(8) . . ? C10 C9 C8 121.9(10) . . ? C9 C10 C11 120.3(11) . . ? C12 C11 C10 118.9(10) . . ? C11 C12 C13 118.5(11) . . ? C8 C13 C12 123.5(10) . . ? C15 C14 C19 118.6(9) . . ? C15 C14 P1 118.5(8) . . ? C19 C14 P1 122.9(8) . . ? C14 C15 C16 121.2(11) . . ? C17 C16 C15 118.2(12) . . ? C18 C17 C16 121.7(13) . . ? C17 C18 C19 119.9(13) . . ? C18 C19 C14 120.4(11) . . ? C21 C20 C25 119.1(10) . . ? C21 C20 N1 124.3(10) . . ? C25 C20 N1 116.6(10) . . ? C20 C21 C22 118.7(10) . . ? C23 C22 C21 120.4(12) . . ? C24 C23 C22 121.0(13) . . ? C25 C24 C23 119.5(12) . . ? C24 C25 C20 121.3(11) . . ? C27 C26 Ni1 108.9(6) . . ? C28 C27 C32 114.2(12) . . ? C28 C27 C26 123.9(13) . . ? C32 C27 C26 121.9(13) . . ? C27 C28 C29 125.0(15) . . ? C28 C29 C30 115.9(19) . . ? C31 C30 C29 122(2) . . ? C30 C31 C32 119(2) . . ? C31 C32 C27 123.6(15) . . ? C06 C01 C02 120.0 . . ? C03 C02 C01 120.1 . . ? C04 C03 C02 119.9 . . ? C03 C04 C05 120.0 . . ? C06 C05 C04 120.0 . . ? C01 C06 C05 119.9 . . ? _diffrn_measured_fraction_theta_max 0.837 _diffrn_reflns_theta_full 25.25 _diffrn_measured_fraction_theta_full 0.837 _refine_diff_density_max 0.317 _refine_diff_density_min -0.370 _refine_diff_density_rms 0.060 #===END data_8 _database_code_depnum_ccdc_archive 'CCDC 228029' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C39 H45 N Ni O P2' _chemical_formula_weight 664.41 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' N N 0.0061 0.0033 '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 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 24.6360(10) _cell_length_b 13.7920(10) _cell_length_c 21.9550(10) _cell_angle_alpha 90.00 _cell_angle_beta 108.448(2) _cell_angle_gamma 90.00 _cell_volume 7076.5(7) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour black _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.247 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2816 _exptl_absorpt_coefficient_mu 0.669 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _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 ? _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 13742 _diffrn_reflns_av_R_equivalents 0.0778 _diffrn_reflns_av_sigmaI/netI 0.1188 _diffrn_reflns_limit_h_min -31 _diffrn_reflns_limit_h_max 31 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 1.71 _diffrn_reflns_theta_max 27.50 _reflns_number_total 8101 _reflns_number_gt 4134 _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^)+(0.0899P)^2^+1.6690P] 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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8101 _refine_ls_number_parameters 401 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1625 _refine_ls_R_factor_gt 0.0715 _refine_ls_wR_factor_ref 0.1969 _refine_ls_wR_factor_gt 0.1598 _refine_ls_goodness_of_fit_ref 1.025 _refine_ls_restrained_S_all 1.025 _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 0.12573(3) 0.29313(4) 0.60774(2) 0.0452(2) Uani 1 1 d . . . P1 P 0.14146(5) 0.14657(8) 0.57997(5) 0.0447(3) Uani 1 1 d . . . P2 P 0.16906(6) 0.43393(9) 0.62653(6) 0.0525(3) Uani 1 1 d . . . O1 O 0.23240(16) 0.1995(3) 0.78332(14) 0.0715(10) Uani 1 1 d . . . N1 N 0.15519(18) 0.2409(3) 0.69571(15) 0.0515(10) Uani 1 1 d . . . C7 C 0.1218(2) 0.0358(3) 0.6140(2) 0.0484(11) Uani 1 1 d . . . C1 C 0.21934(19) 0.1459(3) 0.61749(19) 0.0453(10) Uani 1 1 d . . . C2 C 0.2430(2) 0.1776(3) 0.6819(2) 0.0477(11) Uani 1 1 d . . . C3 C 0.3019(2) 0.1682(4) 0.7111(2) 0.0567(13) Uani 1 1 d . . . H3 H 0.3178 0.1885 0.7535 0.068 Uiso 1 1 calc R . . C4 C 0.3373(2) 0.1302(4) 0.6802(3) 0.0679(15) Uani 1 1 d . . . H4 H 0.3764 0.1252 0.7010 0.082 Uiso 1 1 calc R . . C5 C 0.3139(2) 0.0995(4) 0.6179(3) 0.0705(15) Uani 1 1 d . . . H5 H 0.3374 0.0735 0.5963 0.085 Uiso 1 1 calc R . . C6 C 0.2560(2) 0.1069(4) 0.5871(2) 0.0578(13) Uani 1 1 d . . . H6 H 0.2411 0.0853 0.5450 0.069 Uiso 1 1 calc R . . C8 C 0.1620(2) -0.0353(4) 0.6405(2) 0.0596(13) Uani 1 1 d . . . H8 H 0.1998 -0.0260 0.6424 0.072 Uiso 1 1 calc R . . C9 C 0.1465(3) -0.1195(4) 0.6642(3) 0.0804(18) Uani 1 1 d . . . H9 H 0.1736 -0.1675 0.6808 0.096 Uiso 1 1 calc R . . C10 C 0.0924(3) -0.1325(5) 0.6634(3) 0.099(2) Uani 1 1 d . . . H10 H 0.0828 -0.1891 0.6806 0.118 Uiso 1 1 calc R . . C11 C 0.0511(3) -0.0646(5) 0.6379(3) 0.094(2) Uani 1 1 d . . . H11 H 0.0138 -0.0746 0.6379 0.113 Uiso 1 1 calc R . . C12 C 0.0658(3) 0.0207(4) 0.6116(3) 0.0728(15) Uani 1 1 d . . . H12 H 0.0379 0.0666 0.5927 0.087 Uiso 1 1 calc R . . C13 C 0.1319(2) 0.1110(3) 0.49685(19) 0.0478(11) Uani 1 1 d . . . C14 C 0.1509(3) 0.1715(4) 0.4577(2) 0.0662(15) Uani 1 1 d . . . H14 H 0.1681 0.2301 0.4740 0.079 Uiso 1 1 calc R . . C15 C 0.1451(3) 0.1468(4) 0.3950(2) 0.0799(18) Uani 1 1 d . . . H15 H 0.1588 0.1881 0.3698 0.096 Uiso 1 1 calc R . . C16 C 0.1191(3) 0.0612(5) 0.3700(3) 0.0805(18) Uani 1 1 d . . . H16 H 0.1151 0.0446 0.3278 0.097 Uiso 1 1 calc R . . C17 C 0.0992(3) 0.0006(4) 0.4069(2) 0.0765(17) Uani 1 1 d . . . H17 H 0.0812 -0.0571 0.3898 0.092 Uiso 1 1 calc R . . C18 C 0.1059(2) 0.0255(4) 0.4712(2) 0.0600(13) Uani 1 1 d . . . H18 H 0.0927 -0.0164 0.4966 0.072 Uiso 1 1 calc R . . C19 C 0.0780(2) 0.3420(4) 0.5224(2) 0.0574(13) Uani 1 1 d . . . H19A H 0.0865 0.4093 0.5163 0.086 Uiso 1 1 calc R . . H19B H 0.0834 0.3034 0.4878 0.086 Uiso 1 1 calc R . . C20 C 0.0194(2) 0.3310(4) 0.5261(2) 0.0576(13) Uani 1 1 d . . . C21 C -0.0057(2) 0.4037(4) 0.5522(2) 0.0609(13) Uani 1 1 d . . . H21 H 0.0145 0.4607 0.5664 0.073 Uiso 1 1 calc R . . C22 C -0.0601(3) 0.3936(5) 0.5577(3) 0.0796(17) Uani 1 1 d . . . H22 H -0.0753 0.4428 0.5764 0.096 Uiso 1 1 calc R . . C23 C -0.0913(3) 0.3121(6) 0.5359(4) 0.100(2) Uani 1 1 d . . . H23 H -0.1276 0.3048 0.5397 0.120 Uiso 1 1 calc R . . C24 C -0.0681(4) 0.2409(6) 0.5080(4) 0.112(3) Uani 1 1 d . . . H24 H -0.0897 0.1860 0.4915 0.134 Uiso 1 1 calc R . . C25 C -0.0135(3) 0.2489(4) 0.5039(3) 0.0870(19) Uani 1 1 d . . . H25 H 0.0014 0.1985 0.4859 0.104 Uiso 1 1 calc R . . C26 C 0.1319(2) 0.5471(4) 0.6277(3) 0.0734(16) Uani 1 1 d . . . H26A H 0.1146 0.5449 0.6613 0.110 Uiso 1 1 calc R . . H26B H 0.1027 0.5563 0.5871 0.110 Uiso 1 1 calc R . . H26C H 0.1586 0.5998 0.6355 0.110 Uiso 1 1 calc R . . C27 C 0.2304(3) 0.4436(4) 0.6988(3) 0.0833(18) Uani 1 1 d . . . H27A H 0.2454 0.5083 0.7024 0.125 Uiso 1 1 calc R . . H27B H 0.2593 0.3984 0.6965 0.125 Uiso 1 1 calc R . . H27C H 0.2188 0.4292 0.7356 0.125 Uiso 1 1 calc R . . C28 C 0.2030(3) 0.4576(5) 0.5651(3) 0.095(2) Uani 1 1 d . . . H28A H 0.1740 0.4667 0.5244 0.142 Uiso 1 1 calc R . . H28B H 0.2267 0.4035 0.5626 0.142 Uiso 1 1 calc R . . H28C H 0.2260 0.5150 0.5762 0.142 Uiso 1 1 calc R . . C29 C 0.2082(2) 0.2090(3) 0.72455(19) 0.0512(12) Uani 1 1 d . . . C30 C 0.1173(2) 0.2545(4) 0.7368(2) 0.0660(15) Uani 1 1 d . . . C31 C 0.1368(3) 0.3394(5) 0.7831(3) 0.094(2) Uani 1 1 d . . . H31A H 0.1757 0.3292 0.8095 0.141 Uiso 1 1 calc R . . H31B H 0.1127 0.3439 0.8099 0.141 Uiso 1 1 calc R . . H31C H 0.1342 0.3984 0.7592 0.141 Uiso 1 1 calc R . . C32 C 0.1135(3) 0.1608(5) 0.7725(3) 0.0857(19) Uani 1 1 d . . . H32A H 0.1007 0.1090 0.7421 0.129 Uiso 1 1 calc R . . H32B H 0.0869 0.1694 0.7959 0.129 Uiso 1 1 calc R . . H32C H 0.1506 0.1453 0.8018 0.129 Uiso 1 1 calc R . . C33 C 0.0568(3) 0.2754(5) 0.6899(3) 0.089(2) Uani 1 1 d . . . H33A H 0.0581 0.3312 0.6643 0.134 Uiso 1 1 calc R . . H33B H 0.0310 0.2875 0.7139 0.134 Uiso 1 1 calc R . . H33C H 0.0436 0.2204 0.6624 0.134 Uiso 1 1 calc R . . C01 C 0.0040(3) 0.4523(7) 0.2814(4) 0.112(3) Uani 1 1 d . . . H01 H 0.0065 0.5103 0.3038 0.134 Uiso 1 1 calc R . . C02 C 0.0041(10) 0.2838(7) 0.2810(12) 0.250(19) Uani 1 1 d . . . H02 H 0.0070 0.2256 0.3033 0.300 Uiso 1 1 calc R . . C03 C 0.0082(4) 0.3674(11) 0.3116(6) 0.170(6) Uani 1 1 d . . . H03 H 0.0142 0.3669 0.3556 0.203 Uiso 1 1 calc R . . C04 C 0.2231(7) 0.8231(15) 0.4587(12) 0.070(5) Uiso 0.46(2) 1 d P . 1 H04 H 0.2053 0.8717 0.4301 0.083 Uiso 0.46(2) 1 calc PR . 1 C05 C 0.2506(6) 0.745(2) 0.4362(8) 0.060(5) Uiso 0.46(2) 1 d P . 1 H05 H 0.2506 0.7425 0.3938 0.072 Uiso 0.46(2) 1 calc PR . 1 C06 C 0.2778(7) 0.6715(13) 0.4812(11) 0.065(5) Uiso 0.46(2) 1 d P . 1 H06 H 0.2961 0.6200 0.4685 0.078 Uiso 0.46(2) 1 calc PR . 1 C04' C 0.2272(6) 0.8404(13) 0.4910(12) 0.084(5) Uiso 0.54(2) 1 d P . 2 H04' H 0.2124 0.9030 0.4851 0.101 Uiso 0.54(2) 1 calc PR . 2 C05' C 0.2367(7) 0.7927(14) 0.4420(7) 0.062(4) Uiso 0.54(2) 1 d P . 2 H05' H 0.2269 0.8210 0.4015 0.075 Uiso 0.54(2) 1 calc PR . 2 C06' C 0.2606(8) 0.7028(16) 0.4518(11) 0.081(5) Uiso 0.54(2) 1 d P . 2 H06' H 0.2686 0.6710 0.4183 0.097 Uiso 0.54(2) 1 calc PR . 2 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 0.0571(4) 0.0392(3) 0.0385(3) 0.0034(2) 0.0142(2) 0.0037(3) P1 0.0534(7) 0.0389(6) 0.0415(6) 0.0018(5) 0.0148(5) 0.0000(6) P2 0.0594(9) 0.0454(7) 0.0505(7) -0.0002(5) 0.0142(6) -0.0020(6) O1 0.081(3) 0.086(3) 0.0393(17) 0.0025(17) 0.0077(16) 0.026(2) N1 0.068(3) 0.051(2) 0.0359(18) 0.0061(17) 0.0164(18) 0.014(2) C7 0.051(3) 0.046(3) 0.047(2) 0.000(2) 0.015(2) -0.010(2) C1 0.049(3) 0.039(2) 0.048(2) 0.002(2) 0.017(2) -0.002(2) C2 0.049(3) 0.039(3) 0.051(2) 0.002(2) 0.010(2) -0.001(2) C3 0.064(4) 0.048(3) 0.051(3) 0.005(2) 0.008(2) -0.004(3) C4 0.048(3) 0.078(4) 0.076(4) 0.015(3) 0.018(3) 0.000(3) C5 0.064(4) 0.079(4) 0.077(4) 0.001(3) 0.035(3) 0.010(3) C6 0.054(3) 0.060(3) 0.059(3) -0.005(2) 0.018(2) 0.000(3) C8 0.056(3) 0.051(3) 0.065(3) 0.011(2) 0.009(2) -0.004(3) C9 0.065(4) 0.068(4) 0.092(4) 0.032(3) 0.003(3) -0.009(3) C10 0.085(5) 0.085(5) 0.121(5) 0.046(4) 0.026(4) -0.014(4) C11 0.073(4) 0.076(4) 0.140(6) 0.032(4) 0.043(4) -0.014(4) C12 0.066(4) 0.055(3) 0.094(4) 0.014(3) 0.021(3) -0.001(3) C13 0.055(3) 0.045(3) 0.041(2) -0.001(2) 0.011(2) 0.007(2) C14 0.104(4) 0.049(3) 0.053(3) -0.003(2) 0.035(3) -0.004(3) C15 0.126(5) 0.067(4) 0.055(3) 0.007(3) 0.040(3) 0.015(4) C16 0.109(5) 0.079(4) 0.049(3) -0.004(3) 0.020(3) 0.027(4) C17 0.091(5) 0.065(4) 0.061(3) -0.016(3) 0.007(3) 0.003(3) C18 0.067(3) 0.054(3) 0.050(3) -0.003(2) 0.006(2) 0.002(3) C19 0.075(4) 0.051(3) 0.040(2) 0.009(2) 0.009(2) 0.010(3) C20 0.059(3) 0.050(3) 0.052(3) 0.011(2) 0.000(2) 0.000(3) C21 0.055(3) 0.056(3) 0.063(3) 0.007(3) 0.007(2) -0.004(3) C22 0.071(4) 0.089(5) 0.074(4) 0.017(3) 0.015(3) 0.008(4) C23 0.071(5) 0.095(6) 0.125(6) 0.031(5) 0.018(4) -0.015(4) C24 0.081(6) 0.072(5) 0.147(7) 0.017(5) -0.013(5) -0.030(4) C25 0.084(5) 0.053(3) 0.100(4) 0.005(3) -0.004(4) -0.006(3) C26 0.077(4) 0.047(3) 0.084(4) -0.009(3) 0.008(3) 0.000(3) C27 0.080(4) 0.072(4) 0.075(4) -0.003(3) -0.009(3) -0.004(3) C28 0.093(5) 0.108(5) 0.096(4) -0.010(4) 0.049(4) -0.034(4) C29 0.065(3) 0.044(3) 0.041(2) 0.006(2) 0.011(2) 0.008(3) C30 0.079(4) 0.080(4) 0.046(3) 0.014(3) 0.030(3) 0.024(3) C31 0.135(6) 0.094(5) 0.064(3) 0.007(3) 0.049(4) 0.047(5) C32 0.101(5) 0.102(5) 0.064(3) 0.035(3) 0.041(3) 0.013(4) C33 0.077(4) 0.133(6) 0.071(3) 0.032(4) 0.041(3) 0.034(4) C01 0.086(5) 0.112(6) 0.129(6) -0.016(4) 0.022(6) 0.012(5) C02 0.134(11) 0.110(8) 0.57(6) 0.130(18) 0.20(3) 0.047(13) C03 0.090(6) 0.254(16) 0.179(10) 0.109(12) 0.063(7) 0.045(10) _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 N1 1.972(3) . ? Ni1 C19 1.989(4) . ? Ni1 P1 2.1812(13) . ? Ni1 P2 2.1913(14) . ? P1 C7 1.831(4) . ? P1 C13 1.831(4) . ? P1 C1 1.833(5) . ? P2 C26 1.814(5) . ? P2 C27 1.816(5) . ? P2 C28 1.825(6) . ? O1 C29 1.245(5) . ? N1 C29 1.334(6) . ? N1 C30 1.501(6) . ? C7 C12 1.381(7) . ? C7 C8 1.383(7) . ? C1 C6 1.390(6) . ? C1 C2 1.417(6) . ? C2 C3 1.394(7) . ? C2 C29 1.520(7) . ? C3 C4 1.368(7) . ? C4 C5 1.372(7) . ? C5 C6 1.375(7) . ? C8 C9 1.375(7) . ? C9 C10 1.338(8) . ? C10 C11 1.367(9) . ? C11 C12 1.408(8) . ? C13 C18 1.375(7) . ? C13 C14 1.381(7) . ? C14 C15 1.382(7) . ? C15 C16 1.373(8) . ? C16 C17 1.358(8) . ? C17 C18 1.411(7) . ? C19 C20 1.480(7) . ? C20 C25 1.388(8) . ? C20 C21 1.394(7) . ? C21 C22 1.390(8) . ? C22 C23 1.359(9) . ? C23 C24 1.374(11) . ? C24 C25 1.381(10) . ? C30 C31 1.525(9) . ? C30 C32 1.530(8) . ? C30 C33 1.547(8) . ? C01 C01 1.332(15) 2 ? C01 C03 1.334(12) . ? C02 C02 1.31(5) 2 ? C02 C03 1.32(2) . ? C04 C06 1.33(2) 7_566 ? C04 C05 1.44(2) . ? C05 C06 1.43(2) . ? C06 C04 1.33(2) 7_566 ? C04' C06' 1.34(2) 7_566 ? C04' C05' 1.34(2) . ? C05' C06' 1.36(2) . ? C06' C04' 1.34(2) 7_566 ? 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 N1 Ni1 C19 166.3(2) . . ? N1 Ni1 P1 83.82(12) . . ? C19 Ni1 P1 98.93(15) . . ? N1 Ni1 P2 97.64(13) . . ? C19 Ni1 P2 89.11(16) . . ? P1 Ni1 P2 139.01(5) . . ? C7 P1 C13 102.5(2) . . ? C7 P1 C1 100.7(2) . . ? C13 P1 C1 103.5(2) . . ? C7 P1 Ni1 124.48(15) . . ? C13 P1 Ni1 123.24(15) . . ? C1 P1 Ni1 97.61(15) . . ? C26 P2 C27 102.0(3) . . ? C26 P2 C28 102.0(3) . . ? C27 P2 C28 100.5(3) . . ? C26 P2 Ni1 123.2(2) . . ? C27 P2 Ni1 116.8(2) . . ? C28 P2 Ni1 109.2(2) . . ? C29 N1 C30 117.3(3) . . ? C29 N1 Ni1 126.0(3) . . ? C30 N1 Ni1 115.9(3) . . ? C12 C7 C8 118.8(4) . . ? C12 C7 P1 120.0(4) . . ? C8 C7 P1 121.2(4) . . ? C6 C1 C2 118.2(4) . . ? C6 C1 P1 122.2(3) . . ? C2 C1 P1 119.3(3) . . ? C3 C2 C1 118.1(4) . . ? C3 C2 C29 116.7(4) . . ? C1 C2 C29 124.6(4) . . ? C4 C3 C2 122.7(5) . . ? C3 C4 C5 118.7(5) . . ? C4 C5 C6 120.7(5) . . ? C5 C6 C1 121.5(5) . . ? C9 C8 C7 120.8(5) . . ? C10 C9 C8 120.2(6) . . ? C9 C10 C11 121.5(6) . . ? C10 C11 C12 119.1(6) . . ? C7 C12 C11 119.6(5) . . ? C18 C13 C14 118.0(4) . . ? C18 C13 P1 122.3(4) . . ? C14 C13 P1 119.8(4) . . ? C13 C14 C15 121.6(5) . . ? C16 C15 C14 119.8(5) . . ? C17 C16 C15 120.2(5) . . ? C16 C17 C18 119.8(5) . . ? C13 C18 C17 120.7(5) . . ? C20 C19 Ni1 102.1(3) . . ? C25 C20 C21 116.5(6) . . ? C25 C20 C19 122.4(5) . . ? C21 C20 C19 121.1(5) . . ? C22 C21 C20 121.9(5) . . ? C23 C22 C21 120.3(7) . . ? C22 C23 C24 118.7(7) . . ? C23 C24 C25 121.5(7) . . ? C24 C25 C20 121.0(7) . . ? O1 C29 N1 127.0(4) . . ? O1 C29 C2 115.5(4) . . ? N1 C29 C2 117.4(4) . . ? N1 C30 C31 111.9(5) . . ? N1 C30 C32 110.7(4) . . ? C31 C30 C32 111.3(4) . . ? N1 C30 C33 106.0(4) . . ? C31 C30 C33 109.6(5) . . ? C32 C30 C33 107.2(5) . . ? C01 C01 C03 118.5(8) 2 . ? C02 C02 C03 119.3(10) 2 . ? C02 C03 C01 122.2(14) . . ? C06 C04 C05 122.8(12) 7_566 . ? C06 C05 C04 117.5(11) . . ? C04 C06 C05 119.8(12) 7_566 . ? C06' C04' C05' 119.4(13) 7_566 . ? C04' C05' C06' 119.8(12) . . ? C04' C06' C05' 120.8(13) 7_566 . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.439 _refine_diff_density_min -0.346 _refine_diff_density_rms 0.070 #===END data_9 _database_code_depnum_ccdc_archive 'CCDC 228030' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C50 H26 B F15 N Ni O P' _chemical_formula_weight 1042.21 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' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 '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' O O 0.0106 0.0060 '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 37.7580(10) _cell_length_b 12.0400(10) _cell_length_c 20.9810(10) _cell_angle_alpha 90.00 _cell_angle_beta 109.45(6) _cell_angle_gamma 90.00 _cell_volume 8993.8(9) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.539 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4192 _exptl_absorpt_coefficient_mu 0.569 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _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 ? _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 18092 _diffrn_reflns_av_R_equivalents 0.0273 _diffrn_reflns_av_sigmaI/netI 0.0393 _diffrn_reflns_limit_h_min -48 _diffrn_reflns_limit_h_max 48 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 3.37 _diffrn_reflns_theta_max 27.51 _reflns_number_total 10292 _reflns_number_gt 7109 _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^)+(0.0415P)^2^+8.7466P] 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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10292 _refine_ls_number_parameters 631 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0767 _refine_ls_R_factor_gt 0.0456 _refine_ls_wR_factor_ref 0.1135 _refine_ls_wR_factor_gt 0.0996 _refine_ls_goodness_of_fit_ref 1.023 _refine_ls_restrained_S_all 1.023 _refine_ls_shift/su_max 0.000 _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 0.129365(9) 0.00621(2) 0.112162(16) 0.04947(10) Uani 1 1 d . . . P1 P 0.105894(17) 0.10131(5) 0.02400(3) 0.04479(15) Uani 1 1 d . . . O1 O 0.11710(4) 0.28203(12) 0.22021(7) 0.0401(3) Uani 1 1 d . . . N1 N 0.13087(5) 0.12572(15) 0.17440(9) 0.0413(4) Uani 1 1 d . . . B1 B 0.12210(7) 0.4067(2) 0.23170(13) 0.0387(5) Uani 1 1 d . . . F1 F 0.13671(4) 0.29170(12) 0.35893(7) 0.0557(4) Uani 1 1 d . . . F2 F 0.19860(5) 0.29575(16) 0.46683(8) 0.0776(5) Uani 1 1 d . . . F3 F 0.25629(4) 0.43408(19) 0.47097(8) 0.0915(6) Uani 1 1 d . . . F4 F 0.25007(4) 0.56937(16) 0.36430(8) 0.0788(5) Uani 1 1 d . . . F5 F 0.19014(4) 0.56235(12) 0.25452(7) 0.0584(4) Uani 1 1 d . . . F6 F 0.06159(4) 0.28456(14) 0.27333(8) 0.0654(4) Uani 1 1 d . . . F7 F 0.01666(5) 0.3774(2) 0.33017(9) 0.1036(7) Uani 1 1 d . . . F8 F 0.01544(5) 0.6009(2) 0.34588(11) 0.1306(10) Uani 1 1 d . . . F9 F 0.06368(6) 0.73041(18) 0.30665(12) 0.1170(8) Uani 1 1 d . . . F10 F 0.11241(4) 0.63751(13) 0.25534(9) 0.0732(4) Uani 1 1 d . . . F11 F 0.06649(4) 0.56291(13) 0.13087(8) 0.0620(4) Uani 1 1 d . . . F12 F 0.07290(5) 0.63499(17) 0.01697(9) 0.0931(6) Uani 1 1 d . . . F13 F 0.13370(6) 0.5815(2) -0.01861(10) 0.1131(8) Uani 1 1 d . . . F14 F 0.18907(5) 0.45146(18) 0.06551(9) 0.0868(6) Uani 1 1 d . . . F15 F 0.18153(4) 0.36816(13) 0.17731(7) 0.0581(4) Uani 1 1 d . . . C1 C 0.11077(5) 0.21558(18) 0.16837(11) 0.0367(5) Uani 1 1 d . . . C2 C 0.07866(6) 0.24340(18) 0.10518(11) 0.0382(5) Uani 1 1 d . . . C3 C 0.07502(6) 0.20627(19) 0.03942(11) 0.0425(5) Uani 1 1 d . . . C4 C 0.04539(7) 0.2461(2) -0.01487(12) 0.0544(6) Uani 1 1 d . . . H4 H 0.0434 0.2233 -0.0583 0.065 Uiso 1 1 calc R . . C5 C 0.01888(7) 0.3182(2) -0.00649(12) 0.0568(7) Uani 1 1 d . . . H5 H -0.0003 0.3449 -0.0438 0.068 Uiso 1 1 calc R . . C6 C 0.02126(6) 0.3499(2) 0.05749(12) 0.0518(6) Uani 1 1 d . . . H6 H 0.0030 0.3958 0.0640 0.062 Uiso 1 1 calc R . . C7 C 0.05080(6) 0.3137(2) 0.11237(12) 0.0447(5) Uani 1 1 d . . . H7 H 0.0522 0.3368 0.1554 0.054 Uiso 1 1 calc R . . C8 C 0.16176(6) 0.11340(19) 0.23773(12) 0.0452(5) Uani 1 1 d . . . C9 C 0.19807(7) 0.1199(2) 0.23673(14) 0.0552(6) Uani 1 1 d . . . H9 H 0.2025 0.1342 0.1965 0.066 Uiso 1 1 calc R . . C10 C 0.22794(8) 0.1047(3) 0.29638(17) 0.0729(8) Uani 1 1 d . . . H10 H 0.2524 0.1083 0.2958 0.087 Uiso 1 1 calc R . . C11 C 0.22168(9) 0.0847(3) 0.35595(16) 0.0804(9) Uani 1 1 d . . . H11 H 0.2418 0.0761 0.3958 0.097 Uiso 1 1 calc R . . C12 C 0.18547(10) 0.0776(3) 0.35642(15) 0.0773(9) Uani 1 1 d . . . H12 H 0.1811 0.0635 0.3968 0.093 Uiso 1 1 calc R . . C13 C 0.15535(8) 0.0910(2) 0.29734(13) 0.0589(7) Uani 1 1 d . . . H13 H 0.1309 0.0850 0.2979 0.071 Uiso 1 1 calc R . . C14 C 0.15467(9) -0.1521(2) 0.12829(17) 0.0699(8) Uani 1 1 d . . . C15 C 0.13915(10) -0.1510(2) 0.18063(19) 0.0800(9) Uani 1 1 d . . . H15 H 0.1133 -0.1449 0.1703 0.096 Uiso 1 1 calc R . . C16 C 0.16270(14) -0.1590(3) 0.2490(2) 0.0943(11) Uani 1 1 d . . . H16 H 0.1524 -0.1600 0.2836 0.113 Uiso 1 1 calc R . . C17 C 0.20014(16) -0.1652(3) 0.2633(3) 0.1104(14) Uani 1 1 d . . . H17 H 0.2157 -0.1709 0.3081 0.132 Uiso 1 1 calc R . . C18 C 0.21577(13) -0.1632(3) 0.2132(3) 0.1141(15) Uani 1 1 d . . . H18 H 0.2417 -0.1665 0.2245 0.137 Uiso 1 1 calc R . . C19 C 0.19428(11) -0.1566(3) 0.1480(2) 0.0934(11) Uani 1 1 d . . . H19 H 0.2057 -0.1548 0.1149 0.112 Uiso 1 1 calc R . . C20 C 0.13060(10) -0.1282(2) 0.06081(17) 0.0800(9) Uani 1 1 d . . . H20A H 0.1074 -0.1702 0.0449 0.096 Uiso 1 1 calc R . . H20B H 0.1429 -0.1214 0.0271 0.096 Uiso 1 1 calc R . . C21 C 0.13903(6) 0.1735(2) -0.00768(11) 0.0451(5) Uani 1 1 d . . . C22 C 0.13040(8) 0.2712(2) -0.04448(15) 0.0648(7) Uani 1 1 d . . . H22 H 0.1073 0.3054 -0.0514 0.078 Uiso 1 1 calc R . . C23 C 0.15588(8) 0.3183(3) -0.07097(15) 0.0734(8) Uani 1 1 d . . . H23 H 0.1499 0.3842 -0.0954 0.088 Uiso 1 1 calc R . . C24 C 0.18985(8) 0.2682(3) -0.06136(15) 0.0723(8) Uani 1 1 d . . . H24 H 0.2067 0.2992 -0.0801 0.087 Uiso 1 1 calc R . . C25 C 0.19896(8) 0.1732(3) -0.02448(18) 0.0787(9) Uani 1 1 d . . . H25 H 0.2222 0.1400 -0.0176 0.094 Uiso 1 1 calc R . . C26 C 0.17381(7) 0.1256(2) 0.00299(15) 0.0631(7) Uani 1 1 d . . . H26 H 0.1804 0.0611 0.0287 0.076 Uiso 1 1 calc R . . C27 C 0.07388(7) 0.0282(2) -0.04841(13) 0.0543(6) Uani 1 1 d . . . C28 C 0.04346(9) -0.0253(3) -0.03901(16) 0.0780(9) Uani 1 1 d . . . H28 H 0.0401 -0.0213 0.0029 0.094 Uiso 1 1 calc R . . C29 C 0.01824(10) -0.0840(3) -0.0903(2) 0.0945(11) Uani 1 1 d . . . H29 H -0.0022 -0.1185 -0.0835 0.113 Uiso 1 1 calc R . . C30 C 0.02353(11) -0.0911(3) -0.1518(2) 0.1006(12) Uani 1 1 d . . . H30 H 0.0068 -0.1317 -0.1866 0.121 Uiso 1 1 calc R . . C31 C 0.05332(12) -0.0388(4) -0.16204(19) 0.1051(13) Uani 1 1 d . . . H31 H 0.0565 -0.0431 -0.2041 0.126 Uiso 1 1 calc R . . C32 C 0.07885(9) 0.0206(3) -0.11022(15) 0.0743(9) Uani 1 1 d . . . H32 H 0.0993 0.0551 -0.1173 0.089 Uiso 1 1 calc R . . C33 C 0.16091(6) 0.41965(19) 0.29816(11) 0.0412(5) Uani 1 1 d . . . C34 C 0.16507(6) 0.3578(2) 0.35590(12) 0.0473(5) Uani 1 1 d . . . C35 C 0.19641(7) 0.3604(2) 0.41348(13) 0.0570(6) Uani 1 1 d . . . C36 C 0.22518(7) 0.4300(3) 0.41534(13) 0.0606(7) Uani 1 1 d . . . C37 C 0.22237(6) 0.4967(2) 0.36160(14) 0.0567(7) Uani 1 1 d . . . C38 C 0.19064(6) 0.4916(2) 0.30446(12) 0.0477(5) Uani 1 1 d . . . C39 C 0.08934(6) 0.4570(2) 0.25990(11) 0.0432(5) Uani 1 1 d . . . C40 C 0.06432(6) 0.3953(2) 0.28123(12) 0.0521(6) Uani 1 1 d . . . C41 C 0.04026(7) 0.4434(3) 0.31095(14) 0.0706(9) Uani 1 1 d . . . C42 C 0.03983(8) 0.5546(4) 0.31919(16) 0.0820(11) Uani 1 1 d . . . C43 C 0.06379(9) 0.6195(3) 0.29945(16) 0.0763(9) Uani 1 1 d . . . C44 C 0.08822(7) 0.5695(2) 0.27180(13) 0.0553(6) Uani 1 1 d . . . C45 C 0.12429(6) 0.46391(19) 0.16207(11) 0.0418(5) Uani 1 1 d . . . C46 C 0.09803(6) 0.5318(2) 0.11799(12) 0.0485(6) Uani 1 1 d . . . C47 C 0.10045(8) 0.5709(2) 0.05806(14) 0.0637(7) Uani 1 1 d . . . C48 C 0.13101(9) 0.5445(3) 0.04003(14) 0.0705(8) Uani 1 1 d . . . C49 C 0.15830(7) 0.4775(3) 0.08151(14) 0.0609(7) Uani 1 1 d . . . C50 C 0.15424(6) 0.4375(2) 0.13988(12) 0.0477(5) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ni1 0.0622(2) 0.03504(16) 0.05395(19) -0.00166(14) 0.02310(15) 0.00131(14) P1 0.0499(3) 0.0422(3) 0.0445(3) -0.0064(3) 0.0187(3) -0.0018(3) O1 0.0453(8) 0.0387(8) 0.0360(8) -0.0019(7) 0.0130(6) 0.0004(6) N1 0.0452(10) 0.0376(10) 0.0428(10) 0.0021(8) 0.0171(8) 0.0010(8) B1 0.0375(12) 0.0369(13) 0.0441(14) -0.0009(11) 0.0169(10) -0.0011(10) F1 0.0570(8) 0.0637(9) 0.0479(8) 0.0047(7) 0.0194(6) -0.0060(7) F2 0.0807(11) 0.0970(13) 0.0473(9) 0.0144(9) 0.0106(8) 0.0063(9) F3 0.0616(10) 0.1294(17) 0.0620(10) -0.0073(11) -0.0083(8) -0.0093(10) F4 0.0518(8) 0.0989(14) 0.0802(11) -0.0170(10) 0.0146(8) -0.0297(9) F5 0.0567(8) 0.0565(9) 0.0622(9) 0.0002(7) 0.0202(7) -0.0149(7) F6 0.0632(9) 0.0701(11) 0.0708(10) 0.0071(8) 0.0328(8) -0.0140(8) F7 0.0678(11) 0.182(2) 0.0796(12) 0.0016(13) 0.0495(9) -0.0138(12) F8 0.0839(13) 0.210(3) 0.1082(16) -0.0692(17) 0.0454(12) 0.0308(15) F9 0.1070(15) 0.0894(15) 0.1403(19) -0.0585(14) 0.0223(13) 0.0295(12) F10 0.0759(10) 0.0455(9) 0.0966(12) -0.0132(8) 0.0265(9) -0.0080(8) F11 0.0506(8) 0.0655(10) 0.0692(10) 0.0138(8) 0.0188(7) 0.0113(7) F12 0.0823(11) 0.1037(15) 0.0818(12) 0.0486(11) 0.0118(9) 0.0070(10) F13 0.1144(15) 0.162(2) 0.0741(12) 0.0478(13) 0.0469(11) -0.0129(14) F14 0.0707(10) 0.1323(17) 0.0753(11) -0.0055(11) 0.0479(9) -0.0138(11) F15 0.0506(8) 0.0674(10) 0.0613(9) -0.0001(7) 0.0253(7) 0.0088(7) C1 0.0366(11) 0.0367(11) 0.0404(11) 0.0002(9) 0.0178(9) -0.0055(9) C2 0.0371(11) 0.0376(12) 0.0408(12) -0.0003(9) 0.0140(9) -0.0044(9) C3 0.0417(12) 0.0453(13) 0.0426(12) -0.0033(10) 0.0169(10) -0.0014(10) C4 0.0536(14) 0.0714(18) 0.0384(13) -0.0016(12) 0.0156(11) 0.0055(13) C5 0.0469(13) 0.0752(19) 0.0452(14) 0.0053(13) 0.0111(11) 0.0096(13) C6 0.0415(12) 0.0625(16) 0.0528(14) 0.0010(12) 0.0175(11) 0.0080(11) C7 0.0405(12) 0.0518(14) 0.0426(12) -0.0047(10) 0.0151(10) -0.0009(10) C8 0.0503(13) 0.0364(12) 0.0488(13) 0.0034(10) 0.0165(10) 0.0060(10) C9 0.0551(14) 0.0515(15) 0.0611(16) 0.0058(12) 0.0221(12) 0.0048(12) C10 0.0516(15) 0.069(2) 0.088(2) 0.0031(17) 0.0092(15) 0.0096(14) C11 0.080(2) 0.081(2) 0.0626(19) 0.0054(17) 0.0000(16) 0.0272(17) C12 0.097(2) 0.081(2) 0.0512(16) 0.0189(15) 0.0207(16) 0.0330(18) C13 0.0660(16) 0.0609(17) 0.0553(15) 0.0135(13) 0.0274(13) 0.0159(13) C14 0.090(2) 0.0332(14) 0.090(2) -0.0010(14) 0.0352(18) 0.0039(13) C15 0.098(2) 0.0432(16) 0.105(3) 0.0100(17) 0.043(2) -0.0011(15) C16 0.147(4) 0.0479(19) 0.089(3) 0.0188(18) 0.041(3) -0.001(2) C17 0.132(4) 0.057(2) 0.117(4) 0.024(2) 0.007(3) 0.010(2) C18 0.094(3) 0.062(2) 0.169(5) 0.014(3) 0.019(3) 0.019(2) C19 0.095(3) 0.057(2) 0.133(4) 0.005(2) 0.044(3) 0.0175(18) C20 0.113(3) 0.0442(16) 0.084(2) -0.0115(16) 0.034(2) 0.0031(16) C21 0.0469(12) 0.0452(13) 0.0440(12) -0.0062(10) 0.0162(10) -0.0043(10) C22 0.0552(15) 0.0643(18) 0.0740(19) 0.0152(15) 0.0203(14) 0.0044(13) C23 0.0730(19) 0.074(2) 0.0718(19) 0.0214(16) 0.0215(15) -0.0073(16) C24 0.0654(18) 0.084(2) 0.074(2) 0.0021(17) 0.0321(15) -0.0161(16) C25 0.0547(16) 0.076(2) 0.114(3) 0.006(2) 0.0397(17) 0.0015(15) C26 0.0526(15) 0.0592(17) 0.0796(19) 0.0075(14) 0.0249(13) 0.0037(13) C27 0.0561(14) 0.0540(15) 0.0521(14) -0.0128(12) 0.0169(12) -0.0076(12) C28 0.077(2) 0.092(2) 0.071(2) -0.0189(17) 0.0318(16) -0.0305(17) C29 0.091(2) 0.095(3) 0.097(3) -0.024(2) 0.030(2) -0.044(2) C30 0.099(3) 0.102(3) 0.089(3) -0.040(2) 0.016(2) -0.039(2) C31 0.118(3) 0.130(3) 0.071(2) -0.048(2) 0.036(2) -0.035(3) C32 0.0749(18) 0.089(2) 0.0638(18) -0.0292(16) 0.0294(15) -0.0222(16) C33 0.0394(11) 0.0439(13) 0.0418(12) -0.0060(10) 0.0155(9) 0.0016(9) C34 0.0445(12) 0.0537(14) 0.0458(13) -0.0048(11) 0.0178(10) -0.0006(11) C35 0.0577(15) 0.0672(18) 0.0439(14) 0.0000(13) 0.0141(11) 0.0074(13) C36 0.0447(14) 0.079(2) 0.0484(15) -0.0116(14) 0.0029(11) 0.0001(13) C37 0.0396(12) 0.0676(17) 0.0607(16) -0.0169(14) 0.0137(11) -0.0080(12) C38 0.0453(12) 0.0498(14) 0.0498(13) -0.0078(11) 0.0184(10) -0.0016(10) C39 0.0389(11) 0.0501(13) 0.0402(12) -0.0058(10) 0.0128(9) 0.0008(10) C40 0.0424(12) 0.0713(18) 0.0444(13) -0.0029(12) 0.0167(10) -0.0014(12) C41 0.0473(15) 0.121(3) 0.0486(15) -0.0097(17) 0.0230(12) -0.0039(16) C42 0.0534(17) 0.129(3) 0.0665(19) -0.037(2) 0.0240(14) 0.0162(19) C43 0.0649(18) 0.075(2) 0.079(2) -0.0364(17) 0.0100(15) 0.0165(16) C44 0.0492(13) 0.0551(16) 0.0590(15) -0.0131(13) 0.0145(12) 0.0010(12) C45 0.0408(11) 0.0433(12) 0.0414(12) -0.0006(10) 0.0138(9) -0.0062(9) C46 0.0439(13) 0.0464(14) 0.0539(14) 0.0054(11) 0.0146(11) -0.0049(10) C47 0.0582(16) 0.0658(18) 0.0609(17) 0.0192(14) 0.0117(13) -0.0068(13) C48 0.0728(19) 0.088(2) 0.0525(16) 0.0181(15) 0.0231(14) -0.0189(16) C49 0.0526(15) 0.081(2) 0.0564(16) -0.0049(14) 0.0282(13) -0.0154(14) C50 0.0442(12) 0.0546(15) 0.0443(13) -0.0023(11) 0.0146(10) -0.0056(11) _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 N1 1.9311(18) . ? Ni1 C20 1.953(3) . ? Ni1 P1 2.1039(11) . ? Ni1 C14 2.109(3) . ? Ni1 C15 2.330(3) . ? P1 C3 1.820(2) . ? P1 C21 1.821(2) . ? P1 C27 1.822(3) . ? O1 C1 1.307(2) . ? O1 B1 1.522(3) . ? N1 C1 1.303(3) . ? N1 C8 1.455(3) . ? B1 C45 1.642(3) . ? B1 C39 1.653(3) . ? B1 C33 1.660(3) . ? F1 C34 1.352(3) . ? F2 C35 1.343(3) . ? F3 C36 1.353(3) . ? F4 C37 1.350(3) . ? F5 C38 1.346(3) . ? F6 C40 1.343(3) . ? F7 C41 1.351(4) . ? F8 C42 1.348(3) . ? F9 C43 1.344(4) . ? F10 C44 1.354(3) . ? F11 C46 1.359(3) . ? F12 C47 1.350(3) . ? F13 C48 1.344(3) . ? F14 C49 1.349(3) . ? F15 C50 1.355(3) . ? C1 C2 1.506(3) . ? C2 C7 1.397(3) . ? C2 C3 1.413(3) . ? C3 C4 1.389(3) . ? C4 C5 1.380(3) . ? C5 C6 1.369(3) . ? C6 C7 1.380(3) . ? C8 C13 1.377(3) . ? C8 C9 1.380(3) . ? C9 C10 1.390(4) . ? C10 C11 1.368(4) . ? C11 C12 1.373(4) . ? C12 C13 1.385(4) . ? C14 C15 1.407(4) . ? C14 C19 1.414(5) . ? C14 C20 1.434(4) . ? C15 C16 1.417(5) . ? C16 C17 1.346(6) . ? C17 C18 1.367(6) . ? C18 C19 1.340(6) . ? C21 C26 1.383(3) . ? C21 C22 1.385(4) . ? C22 C23 1.383(4) . ? C23 C24 1.370(4) . ? C24 C25 1.359(4) . ? C25 C26 1.388(4) . ? C27 C32 1.374(4) . ? C27 C28 1.387(4) . ? C28 C29 1.372(4) . ? C29 C30 1.372(5) . ? C30 C31 1.367(5) . ? C31 C32 1.387(4) . ? C33 C34 1.386(3) . ? C33 C38 1.389(3) . ? C34 C35 1.382(3) . ? C35 C36 1.362(4) . ? C36 C37 1.359(4) . ? C37 C38 1.386(4) . ? C39 C44 1.380(4) . ? C39 C40 1.388(3) . ? C40 C41 1.388(4) . ? C41 C42 1.351(5) . ? C42 C43 1.360(5) . ? C43 C44 1.381(4) . ? C45 C46 1.377(3) . ? C45 C50 1.396(3) . ? C46 C47 1.374(3) . ? C47 C48 1.366(4) . ? C48 C49 1.368(4) . ? C49 C50 1.372(3) . ? 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 N1 Ni1 C20 171.72(11) . . ? N1 Ni1 P1 95.62(6) . . ? C20 Ni1 P1 92.65(10) . . ? N1 Ni1 C14 130.95(11) . . ? C20 Ni1 C14 41.13(13) . . ? P1 Ni1 C14 131.98(10) . . ? N1 Ni1 C15 103.02(10) . . ? C20 Ni1 C15 68.85(13) . . ? P1 Ni1 C15 156.64(9) . . ? C14 Ni1 C15 36.52(11) . . ? C3 P1 C21 106.99(11) . . ? C3 P1 C27 101.37(11) . . ? C21 P1 C27 105.77(11) . . ? C3 P1 Ni1 109.19(8) . . ? C21 P1 Ni1 116.18(9) . . ? C27 P1 Ni1 116.01(10) . . ? C1 O1 B1 135.59(17) . . ? C1 N1 C8 115.93(18) . . ? C1 N1 Ni1 131.90(16) . . ? C8 N1 Ni1 112.07(14) . . ? O1 B1 C45 108.24(18) . . ? O1 B1 C39 110.47(17) . . ? C45 B1 C39 115.48(19) . . ? O1 B1 C33 104.70(17) . . ? C45 B1 C33 114.59(18) . . ? C39 B1 C33 102.80(17) . . ? N1 C1 O1 119.24(19) . . ? N1 C1 C2 122.82(19) . . ? O1 C1 C2 117.83(18) . . ? C7 C2 C3 117.7(2) . . ? C7 C2 C1 117.01(19) . . ? C3 C2 C1 125.25(19) . . ? C4 C3 C2 118.8(2) . . ? C4 C3 P1 118.84(17) . . ? C2 C3 P1 122.24(17) . . ? C5 C4 C3 122.2(2) . . ? C6 C5 C4 119.1(2) . . ? C5 C6 C7 120.0(2) . . ? C6 C7 C2 122.0(2) . . ? C13 C8 C9 120.0(2) . . ? C13 C8 N1 121.3(2) . . ? C9 C8 N1 118.6(2) . . ? C8 C9 C10 119.4(3) . . ? C11 C10 C9 120.7(3) . . ? C10 C11 C12 119.5(3) . . ? C11 C12 C13 120.6(3) . . ? C8 C13 C12 119.7(3) . . ? C15 C14 C19 116.6(3) . . ? C15 C14 C20 118.5(3) . . ? C19 C14 C20 123.9(3) . . ? C15 C14 Ni1 80.31(18) . . ? C19 C14 Ni1 117.4(2) . . ? C20 C14 Ni1 63.60(16) . . ? C14 C15 C16 120.3(3) . . ? C14 C15 Ni1 63.16(16) . . ? C16 C15 Ni1 126.6(2) . . ? C17 C16 C15 119.2(4) . . ? C16 C17 C18 121.2(4) . . ? C19 C18 C17 121.1(4) . . ? C18 C19 C14 121.5(4) . . ? C14 C20 Ni1 75.27(17) . . ? C26 C21 C22 118.6(2) . . ? C26 C21 P1 118.2(2) . . ? C22 C21 P1 123.09(19) . . ? C23 C22 C21 120.4(3) . . ? C24 C23 C22 120.2(3) . . ? C25 C24 C23 120.1(3) . . ? C24 C25 C26 120.4(3) . . ? C21 C26 C25 120.3(3) . . ? C32 C27 C28 118.9(3) . . ? C32 C27 P1 123.9(2) . . ? C28 C27 P1 117.2(2) . . ? C29 C28 C27 121.3(3) . . ? C28 C29 C30 119.3(3) . . ? C31 C30 C29 120.2(3) . . ? C30 C31 C32 120.5(3) . . ? C27 C32 C31 119.8(3) . . ? C34 C33 C38 113.5(2) . . ? C34 C33 B1 119.68(19) . . ? C38 C33 B1 126.7(2) . . ? F1 C34 C35 115.7(2) . . ? F1 C34 C33 119.8(2) . . ? C35 C34 C33 124.5(2) . . ? F2 C35 C36 120.4(2) . . ? F2 C35 C34 120.8(2) . . ? C36 C35 C34 118.8(2) . . ? F3 C36 C37 120.0(3) . . ? F3 C36 C35 120.1(3) . . ? C37 C36 C35 119.9(2) . . ? F4 C37 C36 120.2(2) . . ? F4 C37 C38 120.0(3) . . ? C36 C37 C38 119.8(2) . . ? F5 C38 C37 115.4(2) . . ? F5 C38 C33 121.3(2) . . ? C37 C38 C33 123.3(2) . . ? C44 C39 C40 113.7(2) . . ? C44 C39 B1 119.7(2) . . ? C40 C39 B1 126.2(2) . . ? F6 C40 C41 115.8(3) . . ? F6 C40 C39 121.6(2) . . ? C41 C40 C39 122.6(3) . . ? C42 C41 F7 120.4(3) . . ? C42 C41 C40 120.6(3) . . ? F7 C41 C40 119.0(3) . . ? F8 C42 C41 120.1(4) . . ? F8 C42 C43 120.3(4) . . ? C41 C42 C43 119.5(3) . . ? F9 C43 C42 120.6(3) . . ? F9 C43 C44 120.5(3) . . ? C42 C43 C44 118.8(3) . . ? F10 C44 C39 118.9(2) . . ? F10 C44 C43 116.4(3) . . ? C39 C44 C43 124.7(3) . . ? C46 C45 C50 113.2(2) . . ? C46 C45 B1 127.5(2) . . ? C50 C45 B1 119.2(2) . . ? F11 C46 C47 114.7(2) . . ? F11 C46 C45 120.9(2) . . ? C47 C46 C45 124.5(2) . . ? F12 C47 C48 119.9(3) . . ? F12 C47 C46 120.6(3) . . ? C48 C47 C46 119.6(3) . . ? F13 C48 C47 120.3(3) . . ? F13 C48 C49 120.5(3) . . ? C47 C48 C49 119.2(2) . . ? F14 C49 C48 120.5(2) . . ? F14 C49 C50 120.1(3) . . ? C48 C49 C50 119.4(2) . . ? F15 C50 C49 116.4(2) . . ? F15 C50 C45 119.4(2) . . ? C49 C50 C45 124.2(2) . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 27.51 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.252 _refine_diff_density_min -0.348 _refine_diff_density_rms 0.047 #===END data_11 _database_code_depnum_ccdc_archive 'CCDC 228031' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C97 H53 B2 F30 N2 Ni2 O2 P2' _chemical_formula_weight 2049.39 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' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 '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 TRICLINIC _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 14.9305(4) _cell_length_b 17.2883(6) _cell_length_c 20.1574(6) _cell_angle_alpha 92.828(2) _cell_angle_beta 105.688(2) _cell_angle_gamma 106.531(2) _cell_volume 4757.0(3) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.431 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2062 _exptl_absorpt_coefficient_mu 0.537 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _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 ? _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 32685 _diffrn_reflns_av_R_equivalents 0.0412 _diffrn_reflns_av_sigmaI/netI 0.0801 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 1.49 _diffrn_reflns_theta_max 27.53 _reflns_number_total 21169 _reflns_number_gt 11813 _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^)+(0.2000P)^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 mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0002(8) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 21169 _refine_ls_number_parameters 1235 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.1576 _refine_ls_R_factor_gt 0.1042 _refine_ls_wR_factor_ref 0.3398 _refine_ls_wR_factor_gt 0.3106 _refine_ls_goodness_of_fit_ref 1.125 _refine_ls_restrained_S_all 1.126 _refine_ls_shift/su_max 0.010 _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 0.69580(5) 0.16267(4) 0.48810(4) 0.0433(2) Uani 1 1 d . . . P1 P 0.72874(10) 0.07082(9) 0.54703(7) 0.0418(4) Uani 1 1 d . . . O1 O 0.8246(3) 0.0717(2) 0.35692(19) 0.0438(9) Uani 1 1 d . . . N1 N 0.7637(3) 0.1410(3) 0.4258(2) 0.0396(10) Uani 1 1 d . . . H1 H 0.7913 0.1837 0.4100 0.048 Uiso 1 1 calc R . . B1 B 0.8773(4) 0.1399(4) 0.3233(3) 0.0377(13) Uani 1 1 d . . . F1 F 1.0922(2) 0.1994(2) 0.32582(19) 0.0627(10) Uani 1 1 d . . . F2 F 1.1776(3) 0.1205(3) 0.2629(2) 0.0787(12) Uani 1 1 d . . . F3 F 1.0779(4) -0.0267(3) 0.1839(2) 0.0881(14) Uani 1 1 d . . . F4 F 0.8847(4) -0.0907(3) 0.1692(3) 0.1008(16) Uani 1 1 d . . . F5 F 0.7931(3) -0.0135(3) 0.2317(2) 0.0737(11) Uani 1 1 d . . . F6 F 1.0221(3) 0.1248(3) 0.4439(2) 0.0752(11) Uani 1 1 d . . . F7 F 1.1548(3) 0.2422(4) 0.5414(2) 0.1012(16) Uani 1 1 d . . . F8 F 1.1578(4) 0.3994(4) 0.5372(3) 0.125(2) Uani 1 1 d . . . F9 F 1.0238(5) 0.4369(3) 0.4344(3) 0.123(2) Uani 1 1 d . . . F10 F 0.8940(3) 0.3225(2) 0.3371(2) 0.0771(12) Uani 1 1 d . . . F11 F 0.9375(3) 0.2474(2) 0.2287(2) 0.0674(11) Uani 1 1 d . . . F12 F 0.8275(3) 0.2923(3) 0.1205(2) 0.0893(15) Uani 1 1 d . . . F13 F 0.6295(3) 0.2403(3) 0.0905(2) 0.0915(15) Uani 1 1 d . . . F14 F 0.5458(3) 0.1400(3) 0.1718(2) 0.0867(14) Uani 1 1 d . . . F15 F 0.6529(2) 0.0910(3) 0.27757(19) 0.0706(12) Uani 1 1 d . . . C1 C 0.6660(6) 0.2682(4) 0.5055(4) 0.0658(18) Uani 1 1 d . . . C2 C 0.7494(8) 0.3340(5) 0.5392(5) 0.093(3) Uani 1 1 d . . . H2 H 0.7704 0.3445 0.5875 0.112 Uiso 1 1 calc R . . C3 C 0.8005(8) 0.3835(5) 0.5013(7) 0.109(3) Uani 1 1 d . . . H3 H 0.8562 0.4266 0.5243 0.131 Uiso 1 1 calc R . . C4 C 0.7694(7) 0.3694(6) 0.4291(6) 0.092(3) Uani 1 1 d . . . H4 H 0.8026 0.4046 0.4040 0.110 Uiso 1 1 calc R . . C5 C 0.6926(7) 0.3061(5) 0.3954(5) 0.081(2) Uani 1 1 d . . . H5 H 0.6737 0.2959 0.3471 0.097 Uiso 1 1 calc R . . C6 C 0.6405(5) 0.2549(5) 0.4330(4) 0.0625(17) Uani 1 1 d . . . H6 H 0.5872 0.2105 0.4089 0.075 Uiso 1 1 calc R . . C7 C 0.6244(7) 0.2055(5) 0.5421(4) 0.080(2) Uani 1 1 d . . . H7A H 0.5537 0.1826 0.5267 0.120 Uiso 1 1 calc R . . H7B H 0.6522 0.2141 0.5923 0.120 Uiso 1 1 calc R . . C8 C 0.7118(4) -0.0166(3) 0.4854(3) 0.0390(11) Uani 1 1 d . . . C9 C 0.7350(4) -0.0058(3) 0.4220(3) 0.0399(12) Uani 1 1 d . . . C10 C 0.7220(4) -0.0738(4) 0.3777(3) 0.0512(14) Uani 1 1 d . . . H10 H 0.7393 -0.0671 0.3369 0.061 Uiso 1 1 calc R . . C11 C 0.6839(5) -0.1525(4) 0.3917(4) 0.0645(17) Uani 1 1 d . . . H11 H 0.6746 -0.1974 0.3604 0.077 Uiso 1 1 calc R . . C12 C 0.6602(5) -0.1625(4) 0.4526(4) 0.0658(18) Uani 1 1 d . . . H12 H 0.6352 -0.2147 0.4629 0.079 Uiso 1 1 calc R . . C13 C 0.6731(5) -0.0964(4) 0.4980(3) 0.0554(16) Uani 1 1 d . . . H13 H 0.6556 -0.1045 0.5387 0.067 Uiso 1 1 calc R . . C14 C 0.7772(3) 0.0761(3) 0.4022(3) 0.0379(11) Uani 1 1 d . . . C15 C 0.6675(4) 0.0289(4) 0.6095(3) 0.0442(13) Uani 1 1 d . . . C16 C 0.5681(4) 0.0186(4) 0.5960(3) 0.0529(15) Uani 1 1 d . . . H16 H 0.5346 0.0354 0.5563 0.063 Uiso 1 1 calc R . . C17 C 0.5187(5) -0.0167(4) 0.6414(4) 0.0634(18) Uani 1 1 d . . . H17 H 0.4524 -0.0227 0.6320 0.076 Uiso 1 1 calc R . . C18 C 0.5661(5) -0.0432(5) 0.7002(4) 0.068(2) Uani 1 1 d . . . H18 H 0.5320 -0.0677 0.7299 0.081 Uiso 1 1 calc R . . C19 C 0.6639(5) -0.0328(6) 0.7142(4) 0.078(2) Uani 1 1 d . . . H19 H 0.6969 -0.0490 0.7545 0.094 Uiso 1 1 calc R . . C20 C 0.7147(5) 0.0020(5) 0.6689(4) 0.071(2) Uani 1 1 d . . . H20 H 0.7808 0.0072 0.6785 0.085 Uiso 1 1 calc R . . C21 C 0.8585(4) 0.1031(4) 0.5925(3) 0.0507(15) Uani 1 1 d . . . C22 C 0.9186(5) 0.0572(5) 0.5874(4) 0.069(2) Uani 1 1 d . . . H22 H 0.8915 0.0060 0.5610 0.083 Uiso 1 1 calc R . . C23 C 1.0174(6) 0.0848(7) 0.6201(4) 0.088(3) Uani 1 1 d . . . H23 H 1.0573 0.0537 0.6151 0.105 Uiso 1 1 calc R . . C25 C 0.9999(8) 0.2059(7) 0.6682(6) 0.119(4) Uani 1 1 d . . . H25 H 1.0276 0.2555 0.6972 0.143 Uiso 1 1 calc R . . C24 C 1.0559(7) 0.1592(9) 0.6603(5) 0.106(4) Uani 1 1 d . . . H24 H 1.1228 0.1782 0.6829 0.128 Uiso 1 1 calc R . . C26 C 0.8983(6) 0.1786(6) 0.6321(5) 0.093(3) Uani 1 1 d . . . H26 H 0.8593 0.2113 0.6351 0.112 Uiso 1 1 calc R . . C27 C 0.9381(4) 0.0956(3) 0.2847(3) 0.0409(12) Uani 1 1 d . . . C28 C 1.0355(4) 0.1262(4) 0.2889(3) 0.0449(13) Uani 1 1 d . . . C29 C 1.0838(4) 0.0872(4) 0.2576(3) 0.0537(15) Uani 1 1 d . . . C30 C 1.0330(5) 0.0128(5) 0.2168(3) 0.0618(18) Uani 1 1 d . . . C31 C 0.9360(5) -0.0192(4) 0.2088(3) 0.0619(17) Uani 1 1 d . . . C32 C 0.8912(4) 0.0220(4) 0.2430(3) 0.0488(14) Uani 1 1 d . . . C33 C 0.9504(4) 0.2151(4) 0.3841(3) 0.0459(13) Uani 1 1 d . . . C34 C 1.0194(4) 0.2016(4) 0.4408(3) 0.0522(15) Uani 1 1 d . . . C35 C 1.0891(5) 0.2612(6) 0.4919(3) 0.068(2) Uani 1 1 d . . . C36 C 1.0893(6) 0.3405(6) 0.4887(4) 0.080(2) Uani 1 1 d . . . C37 C 1.0234(6) 0.3587(5) 0.4369(4) 0.073(2) Uani 1 1 d . . . C38 C 0.9567(4) 0.2971(4) 0.3867(3) 0.0556(15) Uani 1 1 d . . . C39 C 0.8014(4) 0.1670(4) 0.2592(3) 0.0433(12) Uani 1 1 d . . . C40 C 0.8407(4) 0.2183(4) 0.2168(3) 0.0493(14) Uani 1 1 d . . . C41 C 0.7843(5) 0.2433(4) 0.1610(3) 0.0585(17) Uani 1 1 d . . . C42 C 0.6848(5) 0.2174(5) 0.1452(3) 0.0599(17) Uani 1 1 d . . . C43 C 0.6425(5) 0.1663(5) 0.1864(3) 0.0616(17) Uani 1 1 d . . . C44 C 0.7013(4) 0.1432(4) 0.2419(3) 0.0496(14) Uani 1 1 d . . . Ni2 Ni 0.09724(5) 0.33881(5) 0.01440(4) 0.0508(3) Uani 1 1 d . . . P2 P 0.15328(11) 0.42605(10) -0.04658(7) 0.0466(4) Uani 1 1 d . . . O2 O 0.3722(3) 0.4456(2) 0.15699(19) 0.0449(9) Uani 1 1 d . . . N2 N 0.2191(3) 0.3696(3) 0.0864(2) 0.0478(12) Uani 1 1 d . . . H2A H 0.2276 0.3306 0.1096 0.057 Uiso 1 1 calc R . . B2 B 0.4096(5) 0.3827(5) 0.1964(4) 0.0488(16) Uani 1 1 d . . . F16 F 0.2559(3) 0.4403(3) 0.2401(2) 0.0757(12) Uani 1 1 d . . . F17 F 0.1998(3) 0.4058(4) 0.3515(2) 0.0985(17) Uani 1 1 d . . . F18 F 0.2722(3) 0.3068(3) 0.4364(2) 0.0900(15) Uani 1 1 d . . . F19 F 0.4044(3) 0.2431(3) 0.4061(2) 0.0956(16) Uani 1 1 d . . . F20 F 0.4646(3) 0.2782(3) 0.2950(2) 0.0798(13) Uani 1 1 d . . . F21 F 0.4860(3) 0.5463(3) 0.27260(19) 0.0729(11) Uani 1 1 d . . . F22 F 0.6720(4) 0.6381(3) 0.3239(2) 0.0996(16) Uani 1 1 d . . . F23 F 0.8179(3) 0.5765(4) 0.3167(2) 0.112(2) Uani 1 1 d . . . F24 F 0.7721(3) 0.4195(4) 0.2613(2) 0.0940(16) Uani 1 1 d . . . F25 F 0.5895(3) 0.3288(3) 0.2075(2) 0.0698(11) Uani 1 1 d . . . F26 F 0.2966(3) 0.2015(3) 0.1856(3) 0.0861(14) Uani 1 1 d . . . F27 F 0.2771(5) 0.0865(3) 0.0873(4) 0.133(2) Uani 1 1 d . . . F28 F 0.3597(5) 0.1236(4) -0.0170(3) 0.132(2) Uani 1 1 d . . . F29 F 0.4693(4) 0.2784(3) -0.0171(2) 0.0953(15) Uani 1 1 d . . . F30 F 0.4869(3) 0.3952(3) 0.08016(19) 0.0722(11) Uani 1 1 d . . . C45 C -0.0123(5) 0.2318(5) -0.0074(4) 0.075(2) Uani 1 1 d . . . C46 C 0.0117(5) 0.2490(5) 0.0662(4) 0.075(2) Uani 1 1 d . . . H46 H -0.0019 0.2926 0.0859 0.089 Uiso 1 1 calc R . . C47 C 0.0558(7) 0.2001(6) 0.1093(5) 0.087(3) Uani 1 1 d . . . H47 H 0.0716 0.2116 0.1574 0.104 Uiso 1 1 calc R . . C48 C 0.0748(8) 0.1377(6) 0.0813(6) 0.101(3) Uani 1 1 d . . . H48 H 0.1034 0.1056 0.1104 0.121 Uiso 1 1 calc R . . C49 C 0.0527(9) 0.1187(5) 0.0089(6) 0.110(4) Uani 1 1 d . . . H49 H 0.0671 0.0747 -0.0091 0.132 Uiso 1 1 calc R . . C50 C 0.0109(7) 0.1635(6) -0.0346(5) 0.095(3) Uani 1 1 d . . . H50 H -0.0031 0.1505 -0.0823 0.114 Uiso 1 1 calc R . . C51 C -0.0358(5) 0.2933(6) -0.0483(5) 0.091(3) Uani 1 1 d . . . H51A H -0.0846 0.3153 -0.0388 0.136 Uiso 1 1 calc R . . H51B H -0.0422 0.2840 -0.0974 0.136 Uiso 1 1 calc R . . C52 C 0.2304(4) 0.5175(3) 0.0124(3) 0.0439(13) Uani 1 1 d . . . C53 C 0.2879(4) 0.5143(3) 0.0805(3) 0.0409(12) Uani 1 1 d . . . C54 C 0.3440(5) 0.5856(4) 0.1235(3) 0.0559(15) Uani 1 1 d . . . H54 H 0.3812 0.5829 0.1680 0.067 Uiso 1 1 calc R . . C55 C 0.3471(6) 0.6609(4) 0.1030(3) 0.0653(18) Uani 1 1 d . . . H55 H 0.3860 0.7083 0.1330 0.078 Uiso 1 1 calc R . . C56 C 0.2915(6) 0.6648(4) 0.0370(4) 0.070(2) Uani 1 1 d . . . H56 H 0.2927 0.7152 0.0225 0.085 Uiso 1 1 calc R . . C57 C 0.2348(5) 0.5950(4) -0.0071(3) 0.0584(16) Uani 1 1 d . . . H57 H 0.1980 0.5990 -0.0513 0.070 Uiso 1 1 calc R . . C58 C 0.2910(4) 0.4357(3) 0.1078(2) 0.0386(12) Uani 1 1 d . . . C59 C 0.2329(4) 0.3930(4) -0.0868(3) 0.0506(14) Uani 1 1 d . . . C60 C 0.3262(5) 0.4430(4) -0.0829(3) 0.0593(16) Uani 1 1 d . . . H60 H 0.3490 0.4959 -0.0596 0.071 Uiso 1 1 calc R . . C61 C 0.3856(6) 0.4138(5) -0.1140(4) 0.075(2) Uani 1 1 d . . . H61 H 0.4477 0.4475 -0.1115 0.090 Uiso 1 1 calc R . . C62 C 0.3538(6) 0.3376(5) -0.1476(4) 0.0703(19) Uani 1 1 d . . . H62 H 0.3939 0.3191 -0.1682 0.084 Uiso 1 1 calc R . . C63 C 0.2646(7) 0.2877(6) -0.1516(5) 0.092(3) Uani 1 1 d . . . H63 H 0.2430 0.2353 -0.1757 0.110 Uiso 1 1 calc R . . C64 C 0.2041(6) 0.3139(5) -0.1200(4) 0.077(2) Uani 1 1 d . . . H64 H 0.1439 0.2780 -0.1211 0.092 Uiso 1 1 calc R . . C65 C 0.0738(4) 0.4615(4) -0.1147(3) 0.0497(14) Uani 1 1 d . . . C66 C 0.0900(5) 0.4723(5) -0.1791(3) 0.073(2) Uani 1 1 d . . . H66 H 0.1395 0.4565 -0.1900 0.087 Uiso 1 1 calc R . . C67 C 0.0326(5) 0.5063(6) -0.2265(4) 0.092(3) Uani 1 1 d . . . H67 H 0.0450 0.5147 -0.2688 0.111 Uiso 1 1 calc R . . C68 C -0.0424(5) 0.5280(6) -0.2125(4) 0.083(3) Uani 1 1 d . . . H68 H -0.0810 0.5507 -0.2451 0.099 Uiso 1 1 calc R . . C69 C -0.0599(6) 0.5158(5) -0.1497(4) 0.076(2) Uani 1 1 d . . . H69 H -0.1101 0.5310 -0.1394 0.092 Uiso 1 1 calc R . . C70 C -0.0036(5) 0.4811(5) -0.1019(3) 0.0642(18) Uani 1 1 d . . . H70 H -0.0182 0.4708 -0.0605 0.077 Uiso 1 1 calc R . . C71 C 0.3619(4) 0.3605(4) 0.2607(3) 0.0474(13) Uani 1 1 d . . . C72 C 0.2961(4) 0.3896(4) 0.2787(3) 0.0541(15) Uani 1 1 d . . . C73 C 0.2651(5) 0.3738(5) 0.3383(3) 0.0637(19) Uani 1 1 d . . . C74 C 0.3010(4) 0.3234(5) 0.3794(3) 0.0621(18) Uani 1 1 d . . . C75 C 0.3672(5) 0.2934(5) 0.3643(3) 0.0605(17) Uani 1 1 d . . . C76 C 0.3976(4) 0.3103(4) 0.3072(4) 0.0568(16) Uani 1 1 d . . . C77 C 0.5267(4) 0.4345(4) 0.2337(3) 0.0432(13) Uani 1 1 d . . . C78 C 0.5545(4) 0.5128(4) 0.2661(3) 0.0549(15) Uani 1 1 d . . . C79 C 0.6518(5) 0.5617(5) 0.2952(3) 0.069(2) Uani 1 1 d . . . C80 C 0.7242(5) 0.5308(6) 0.2916(4) 0.078(3) Uani 1 1 d . . . C81 C 0.7000(5) 0.4519(6) 0.2624(4) 0.066(2) Uani 1 1 d . . . C82 C 0.6039(4) 0.4062(4) 0.2342(3) 0.0514(15) Uani 1 1 d . . . C83 C 0.3938(4) 0.3066(4) 0.1392(3) 0.0501(14) Uani 1 1 d . . . C84 C 0.3425(5) 0.2260(4) 0.1378(4) 0.0605(17) Uani 1 1 d . . . C85 C 0.3290(7) 0.1628(5) 0.0854(5) 0.085(2) Uani 1 1 d . . . C86 C 0.3700(7) 0.1828(6) 0.0330(5) 0.089(3) Uani 1 1 d . . . C87 C 0.4249(6) 0.2615(5) 0.0329(4) 0.0692(19) Uani 1 1 d . . . C88 C 0.4334(5) 0.3201(4) 0.0845(3) 0.0553(15) Uani 1 1 d . . . C100 C 0.4086(11) 0.7780(12) 0.2852(6) 0.130(5) Uani 1 1 d . . . H100 H 0.4741 0.8095 0.2976 0.156 Uiso 1 1 calc R . . C101 C 0.3379(15) 0.8082(9) 0.2584(7) 0.134(5) Uani 1 1 d . . . H101 H 0.3531 0.8624 0.2507 0.161 Uiso 1 1 calc R . . C102 C 0.2445(14) 0.7625(14) 0.2418(6) 0.150(6) Uani 1 1 d . . . H102 H 0.1979 0.7873 0.2219 0.180 Uiso 1 1 calc R . . C103 C 0.213(2) 0.6890(14) 0.2504(12) 0.189(10) Uani 1 1 d . . . H103 H 0.1462 0.6625 0.2393 0.227 Uiso 1 1 calc R . . C104 C 0.272(3) 0.6531(13) 0.2737(12) 0.204(15) Uani 1 1 d . . . H104 H 0.2480 0.5984 0.2783 0.245 Uiso 1 1 calc R . . C105 C 0.379(2) 0.692(2) 0.2948(7) 0.199(11) Uani 1 1 d . . . H105 H 0.4236 0.6642 0.3125 0.238 Uiso 1 1 calc R . . C106 C 0.543(3) 0.4399(17) 0.5124(19) 0.30(3) Uani 1 1 d D . . H106 H 0.5671 0.3957 0.5164 0.357 Uiso 1 1 calc R . . C107 C 0.5626(16) 0.496(2) 0.4673(13) 0.200(12) Uani 1 1 d D . . H107 H 0.6111 0.4986 0.4458 0.240 Uiso 1 1 calc R . . C108 C 0.504(4) 0.5473(12) 0.4562(12) 0.27(2) Uani 1 1 d D . . H108 H 0.5047 0.5747 0.4176 0.326 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 0.0512(4) 0.0429(4) 0.0492(4) 0.0170(3) 0.0254(3) 0.0234(3) P1 0.0446(7) 0.0475(9) 0.0420(7) 0.0175(6) 0.0207(6) 0.0182(6) O1 0.050(2) 0.041(2) 0.052(2) 0.0195(17) 0.0290(18) 0.0174(17) N1 0.047(2) 0.039(3) 0.044(2) 0.021(2) 0.023(2) 0.019(2) B1 0.037(3) 0.038(3) 0.045(3) 0.016(3) 0.019(2) 0.014(2) F1 0.0489(19) 0.062(2) 0.077(2) 0.0069(19) 0.0294(17) 0.0069(17) F2 0.055(2) 0.101(3) 0.100(3) 0.026(3) 0.042(2) 0.036(2) F3 0.109(3) 0.090(3) 0.101(3) 0.014(3) 0.063(3) 0.055(3) F4 0.115(4) 0.072(3) 0.102(3) -0.030(3) 0.047(3) 0.003(3) F5 0.058(2) 0.078(3) 0.073(2) -0.009(2) 0.0260(19) 0.000(2) F6 0.077(3) 0.079(3) 0.071(2) 0.029(2) 0.008(2) 0.037(2) F7 0.086(3) 0.138(5) 0.062(3) 0.014(3) -0.003(2) 0.032(3) F8 0.108(4) 0.116(5) 0.098(4) -0.036(3) 0.001(3) -0.010(3) F9 0.147(5) 0.048(3) 0.148(5) -0.012(3) 0.023(4) 0.012(3) F10 0.084(3) 0.050(2) 0.098(3) 0.014(2) 0.012(2) 0.036(2) F11 0.053(2) 0.075(3) 0.088(3) 0.050(2) 0.0312(18) 0.0237(18) F12 0.092(3) 0.112(4) 0.094(3) 0.073(3) 0.047(3) 0.050(3) F13 0.089(3) 0.138(5) 0.072(3) 0.053(3) 0.020(2) 0.071(3) F14 0.046(2) 0.130(4) 0.086(3) 0.036(3) 0.0133(19) 0.032(2) F15 0.0410(18) 0.107(3) 0.066(2) 0.040(2) 0.0220(16) 0.0152(19) C1 0.090(5) 0.052(4) 0.084(5) 0.021(4) 0.046(4) 0.045(4) C2 0.130(8) 0.064(6) 0.090(6) 0.009(5) 0.032(6) 0.038(6) C3 0.119(8) 0.045(5) 0.150(10) 0.009(6) 0.041(7) 0.006(5) C4 0.108(7) 0.073(6) 0.115(7) 0.046(6) 0.055(6) 0.031(5) C5 0.097(6) 0.068(5) 0.100(6) 0.040(5) 0.041(5) 0.043(5) C6 0.058(4) 0.064(4) 0.076(4) 0.024(4) 0.021(3) 0.032(3) C7 0.118(6) 0.069(5) 0.098(6) 0.030(4) 0.077(5) 0.053(5) C8 0.044(3) 0.037(3) 0.042(3) 0.012(2) 0.018(2) 0.017(2) C9 0.038(3) 0.041(3) 0.048(3) 0.021(2) 0.019(2) 0.014(2) C10 0.060(3) 0.045(3) 0.055(3) 0.011(3) 0.024(3) 0.019(3) C11 0.069(4) 0.047(4) 0.077(4) 0.011(3) 0.027(3) 0.012(3) C12 0.084(5) 0.043(4) 0.076(4) 0.023(3) 0.040(4) 0.012(3) C13 0.065(4) 0.049(4) 0.069(4) 0.034(3) 0.036(3) 0.023(3) C14 0.033(2) 0.045(3) 0.043(3) 0.019(2) 0.016(2) 0.017(2) C15 0.048(3) 0.048(3) 0.047(3) 0.012(2) 0.024(2) 0.019(3) C16 0.045(3) 0.065(4) 0.049(3) 0.015(3) 0.016(3) 0.014(3) C17 0.049(3) 0.072(5) 0.069(4) 0.020(4) 0.025(3) 0.009(3) C18 0.066(4) 0.095(6) 0.065(4) 0.036(4) 0.044(3) 0.033(4) C19 0.076(5) 0.123(7) 0.071(4) 0.057(5) 0.045(4) 0.058(5) C20 0.055(4) 0.116(6) 0.069(4) 0.058(4) 0.033(3) 0.046(4) C21 0.043(3) 0.060(4) 0.052(3) 0.021(3) 0.019(3) 0.014(3) C22 0.048(4) 0.095(6) 0.071(4) 0.029(4) 0.020(3) 0.028(4) C23 0.056(4) 0.133(9) 0.076(5) 0.026(6) 0.012(4) 0.037(5) C25 0.100(8) 0.092(8) 0.119(8) -0.018(6) -0.004(6) 0.000(6) C24 0.062(5) 0.148(11) 0.095(7) 0.033(7) 0.012(5) 0.018(6) C26 0.070(5) 0.102(7) 0.092(6) -0.006(5) 0.015(4) 0.016(5) C27 0.049(3) 0.043(3) 0.036(3) 0.013(2) 0.019(2) 0.015(2) C28 0.043(3) 0.048(3) 0.058(3) 0.022(3) 0.027(3) 0.021(3) C29 0.052(3) 0.067(4) 0.063(4) 0.030(3) 0.034(3) 0.031(3) C30 0.076(4) 0.075(5) 0.062(4) 0.023(4) 0.040(3) 0.046(4) C31 0.082(5) 0.047(4) 0.059(4) 0.003(3) 0.029(3) 0.017(3) C32 0.049(3) 0.056(4) 0.046(3) 0.015(3) 0.024(3) 0.015(3) C33 0.041(3) 0.052(4) 0.052(3) 0.014(3) 0.022(2) 0.015(2) C34 0.053(3) 0.063(4) 0.049(3) 0.025(3) 0.018(3) 0.026(3) C35 0.055(4) 0.101(6) 0.045(3) 0.018(4) 0.015(3) 0.021(4) C36 0.070(5) 0.082(6) 0.068(5) -0.012(4) 0.015(4) 0.001(4) C37 0.083(5) 0.059(5) 0.074(5) -0.003(4) 0.027(4) 0.015(4) C38 0.050(3) 0.048(4) 0.071(4) 0.012(3) 0.021(3) 0.015(3) C39 0.045(3) 0.049(3) 0.045(3) 0.014(2) 0.019(2) 0.022(3) C40 0.046(3) 0.054(4) 0.061(3) 0.023(3) 0.025(3) 0.024(3) C41 0.073(4) 0.068(4) 0.058(4) 0.039(3) 0.033(3) 0.039(3) C42 0.061(4) 0.079(5) 0.057(4) 0.025(3) 0.019(3) 0.044(4) C43 0.050(3) 0.087(5) 0.056(4) 0.016(3) 0.018(3) 0.030(3) C44 0.047(3) 0.060(4) 0.047(3) 0.014(3) 0.021(3) 0.018(3) Ni2 0.0462(4) 0.0505(5) 0.0498(4) 0.0174(3) 0.0109(3) 0.0071(3) P2 0.0491(8) 0.0479(9) 0.0396(7) 0.0156(6) 0.0079(6) 0.0137(7) O2 0.043(2) 0.046(2) 0.045(2) 0.0163(17) 0.0073(16) 0.0177(17) N2 0.048(3) 0.048(3) 0.049(3) 0.023(2) 0.015(2) 0.014(2) B2 0.043(3) 0.054(4) 0.062(4) 0.026(3) 0.021(3) 0.027(3) F16 0.084(3) 0.111(4) 0.069(2) 0.044(2) 0.034(2) 0.070(3) F17 0.091(3) 0.170(5) 0.081(3) 0.043(3) 0.051(3) 0.083(3) F18 0.080(3) 0.143(5) 0.065(2) 0.046(3) 0.041(2) 0.039(3) F19 0.093(3) 0.129(4) 0.096(3) 0.082(3) 0.045(3) 0.054(3) F20 0.078(3) 0.103(3) 0.103(3) 0.072(3) 0.052(2) 0.063(2) F21 0.078(3) 0.084(3) 0.060(2) -0.004(2) 0.0083(19) 0.043(2) F22 0.102(3) 0.074(3) 0.087(3) -0.021(3) 0.001(3) 0.004(3) F23 0.056(2) 0.159(5) 0.083(3) 0.004(3) 0.009(2) -0.014(3) F24 0.049(2) 0.151(5) 0.101(3) 0.041(3) 0.031(2) 0.047(3) F25 0.062(2) 0.072(3) 0.096(3) 0.026(2) 0.030(2) 0.042(2) F26 0.105(3) 0.054(3) 0.117(4) 0.026(2) 0.068(3) 0.015(2) F27 0.179(6) 0.044(3) 0.187(6) -0.004(3) 0.098(5) 0.013(3) F28 0.179(6) 0.086(4) 0.144(5) -0.032(4) 0.075(4) 0.044(4) F29 0.119(4) 0.119(4) 0.072(3) 0.021(3) 0.047(3) 0.055(3) F30 0.091(3) 0.068(3) 0.060(2) 0.0227(19) 0.035(2) 0.016(2) C45 0.064(4) 0.065(5) 0.073(5) 0.017(4) 0.011(4) -0.009(4) C46 0.067(4) 0.061(5) 0.093(5) 0.021(4) 0.039(4) -0.001(4) C47 0.108(6) 0.071(6) 0.094(6) 0.042(5) 0.056(5) 0.017(5) C48 0.129(8) 0.067(6) 0.114(8) 0.037(5) 0.051(6) 0.023(6) C49 0.178(11) 0.048(5) 0.114(8) 0.003(5) 0.071(8) 0.024(6) C50 0.117(7) 0.062(6) 0.084(6) 0.004(5) 0.031(5) -0.006(5) C51 0.052(4) 0.090(6) 0.101(6) 0.029(5) -0.005(4) 0.000(4) C52 0.054(3) 0.041(3) 0.039(3) 0.016(2) 0.015(2) 0.016(3) C53 0.048(3) 0.040(3) 0.041(3) 0.013(2) 0.016(2) 0.020(2) C54 0.077(4) 0.052(4) 0.040(3) 0.014(3) 0.015(3) 0.023(3) C55 0.096(5) 0.042(4) 0.051(4) 0.004(3) 0.011(3) 0.022(3) C56 0.110(6) 0.034(3) 0.064(4) 0.018(3) 0.021(4) 0.022(4) C57 0.076(4) 0.048(4) 0.051(3) 0.024(3) 0.007(3) 0.025(3) C58 0.044(3) 0.046(3) 0.033(2) 0.017(2) 0.015(2) 0.020(2) C59 0.053(3) 0.053(4) 0.042(3) 0.014(3) 0.008(2) 0.015(3) C60 0.064(4) 0.051(4) 0.066(4) 0.015(3) 0.024(3) 0.018(3) C61 0.069(4) 0.082(6) 0.087(5) 0.024(4) 0.033(4) 0.031(4) C62 0.081(5) 0.070(5) 0.078(5) 0.014(4) 0.036(4) 0.037(4) C63 0.108(7) 0.062(5) 0.107(7) -0.010(5) 0.040(5) 0.024(5) C64 0.073(5) 0.060(5) 0.094(5) 0.001(4) 0.034(4) 0.009(4) C65 0.042(3) 0.058(4) 0.046(3) 0.015(3) 0.007(2) 0.015(3) C66 0.048(3) 0.122(7) 0.055(4) 0.039(4) 0.015(3) 0.032(4) C67 0.052(4) 0.156(9) 0.077(5) 0.068(6) 0.017(4) 0.039(5) C68 0.054(4) 0.112(7) 0.084(5) 0.048(5) 0.010(4) 0.034(4) C69 0.073(5) 0.100(6) 0.066(4) 0.013(4) 0.008(4) 0.053(4) C70 0.060(4) 0.085(5) 0.049(3) 0.007(3) 0.010(3) 0.031(4) C71 0.043(3) 0.053(4) 0.054(3) 0.021(3) 0.017(3) 0.022(3) C72 0.046(3) 0.072(4) 0.048(3) 0.017(3) 0.014(3) 0.022(3) C73 0.049(3) 0.099(6) 0.055(4) 0.020(4) 0.023(3) 0.033(4) C74 0.047(3) 0.091(5) 0.052(3) 0.028(4) 0.018(3) 0.022(3) C75 0.052(3) 0.074(5) 0.060(4) 0.030(3) 0.016(3) 0.023(3) C76 0.045(3) 0.065(4) 0.076(4) 0.035(3) 0.029(3) 0.027(3) C77 0.043(3) 0.050(3) 0.041(3) 0.023(3) 0.012(2) 0.019(2) C78 0.049(3) 0.069(4) 0.048(3) 0.017(3) 0.011(3) 0.023(3) C79 0.072(5) 0.076(5) 0.044(3) 0.011(3) 0.005(3) 0.011(4) C80 0.041(4) 0.128(8) 0.051(4) 0.028(4) 0.006(3) 0.006(4) C81 0.045(4) 0.103(6) 0.055(4) 0.034(4) 0.015(3) 0.025(4) C82 0.049(3) 0.067(4) 0.050(3) 0.028(3) 0.023(3) 0.025(3) C83 0.055(3) 0.048(4) 0.057(3) 0.021(3) 0.019(3) 0.026(3) C84 0.064(4) 0.051(4) 0.081(4) 0.020(3) 0.036(3) 0.026(3) C85 0.103(6) 0.055(5) 0.110(6) 0.005(4) 0.053(5) 0.025(4) C86 0.105(6) 0.089(7) 0.089(6) 0.000(5) 0.028(5) 0.058(6) C87 0.076(5) 0.079(6) 0.066(4) 0.015(4) 0.027(4) 0.038(4) C88 0.061(4) 0.051(4) 0.061(4) 0.016(3) 0.023(3) 0.024(3) C100 0.128(10) 0.190(17) 0.077(7) -0.021(8) 0.027(7) 0.063(11) C101 0.171(13) 0.115(10) 0.096(8) -0.009(7) 0.034(9) 0.021(11) C102 0.175(16) 0.172(16) 0.088(8) -0.029(10) 0.004(9) 0.071(13) C103 0.24(3) 0.108(16) 0.185(18) -0.029(14) 0.047(17) 0.032(16) C104 0.36(4) 0.101(13) 0.16(2) -0.022(12) 0.17(3) 0.016(19) C105 0.34(3) 0.29(3) 0.080(8) 0.020(14) 0.080(14) 0.25(3) C106 0.36(4) 0.40(5) 0.17(3) -0.08(3) -0.04(3) 0.30(4) C107 0.139(13) 0.31(4) 0.128(14) -0.016(16) 0.062(12) 0.027(17) C108 0.48(5) 0.110(13) 0.117(15) 0.003(10) -0.08(2) 0.09(2) _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 N1 1.897(4) . ? Ni1 C7 1.967(6) . ? Ni1 C1 2.032(7) . ? Ni1 P1 2.1187(16) . ? Ni1 C6 2.210(7) . ? P1 C21 1.811(6) . ? P1 C15 1.812(5) . ? P1 C8 1.821(6) . ? O1 C14 1.309(6) . ? O1 B1 1.519(6) . ? N1 C14 1.286(7) . ? B1 C33 1.641(9) . ? B1 C27 1.655(8) . ? B1 C39 1.656(8) . ? F1 C28 1.352(7) . ? F2 C29 1.326(7) . ? F3 C30 1.345(7) . ? F4 C31 1.337(8) . ? F5 C32 1.367(6) . ? F6 C34 1.343(8) . ? F7 C35 1.323(8) . ? F8 C36 1.345(9) . ? F9 C37 1.353(9) . ? F10 C38 1.356(8) . ? F11 C40 1.335(6) . ? F12 C41 1.356(7) . ? F13 C42 1.338(7) . ? F14 C43 1.327(7) . ? F15 C44 1.352(6) . ? C1 C6 1.397(10) . ? C1 C2 1.403(12) . ? C1 C7 1.431(10) . ? C2 C3 1.381(13) . ? C3 C4 1.390(14) . ? C4 C5 1.328(13) . ? C5 C6 1.398(10) . ? C8 C13 1.401(8) . ? C8 C9 1.420(7) . ? C9 C10 1.375(8) . ? C9 C14 1.498(7) . ? C10 C11 1.392(9) . ? C11 C12 1.371(9) . ? C12 C13 1.364(10) . ? C15 C20 1.390(8) . ? C15 C16 1.391(8) . ? C16 C17 1.384(8) . ? C17 C18 1.378(9) . ? C18 C19 1.366(9) . ? C19 C20 1.393(8) . ? C21 C22 1.375(10) . ? C21 C26 1.377(11) . ? C22 C23 1.371(10) . ? C23 C24 1.365(15) . ? C25 C24 1.349(16) . ? C25 C26 1.419(13) . ? C27 C32 1.373(8) . ? C27 C28 1.375(7) . ? C28 C29 1.363(8) . ? C29 C30 1.382(10) . ? C30 C31 1.355(10) . ? C31 C32 1.379(9) . ? C33 C38 1.391(9) . ? C33 C34 1.397(8) . ? C34 C35 1.383(10) . ? C35 C36 1.375(12) . ? C36 C37 1.345(12) . ? C37 C38 1.378(10) . ? C39 C44 1.371(8) . ? C39 C40 1.383(7) . ? C40 C41 1.381(8) . ? C41 C42 1.364(9) . ? C42 C43 1.382(9) . ? C43 C44 1.376(9) . ? Ni2 N2 1.908(5) . ? Ni2 C51 1.953(7) . ? Ni2 C45 2.025(7) . ? Ni2 P2 2.1230(16) . ? Ni2 C46 2.211(6) . ? P2 C59 1.805(7) . ? P2 C52 1.810(6) . ? P2 C65 1.812(6) . ? O2 C58 1.303(6) . ? O2 B2 1.522(7) . ? N2 C58 1.283(7) . ? B2 C83 1.627(10) . ? B2 C71 1.650(8) . ? B2 C77 1.661(9) . ? F16 C72 1.359(7) . ? F17 C73 1.328(8) . ? F18 C74 1.348(7) . ? F19 C75 1.367(7) . ? F20 C76 1.342(7) . ? F21 C78 1.341(7) . ? F22 C79 1.331(9) . ? F23 C80 1.336(8) . ? F24 C81 1.352(9) . ? F25 C82 1.353(8) . ? F26 C84 1.344(7) . ? F27 C85 1.335(9) . ? F28 C86 1.345(10) . ? F29 C87 1.350(8) . ? F30 C88 1.337(7) . ? C45 C46 1.424(11) . ? C45 C51 1.441(11) . ? C45 C50 1.444(13) . ? C46 C47 1.408(12) . ? C47 C48 1.329(13) . ? C48 C49 1.406(14) . ? C49 C50 1.342(14) . ? C52 C57 1.403(8) . ? C52 C53 1.423(7) . ? C53 C54 1.373(8) . ? C53 C58 1.499(7) . ? C54 C55 1.378(9) . ? C55 C56 1.380(9) . ? C56 C57 1.367(9) . ? C59 C64 1.386(10) . ? C59 C60 1.395(8) . ? C60 C61 1.400(10) . ? C61 C62 1.342(11) . ? C62 C63 1.343(11) . ? C63 C64 1.394(11) . ? C65 C70 1.376(9) . ? C65 C66 1.396(8) . ? C66 C67 1.376(10) . ? C67 C68 1.368(12) . ? C68 C69 1.375(10) . ? C69 C70 1.379(10) . ? C71 C72 1.345(9) . ? C71 C76 1.411(8) . ? C72 C73 1.411(8) . ? C73 C74 1.352(10) . ? C74 C75 1.333(10) . ? C75 C76 1.364(9) . ? C77 C82 1.371(8) . ? C77 C78 1.372(9) . ? C78 C79 1.400(9) . ? C79 C80 1.352(12) . ? C80 C81 1.365(12) . ? C81 C82 1.370(9) . ? C83 C84 1.380(9) . ? C83 C88 1.386(8) . ? C84 C85 1.413(11) . ? C85 C86 1.369(12) . ? C86 C87 1.375(12) . ? C87 C88 1.370(10) . ? C100 C101 1.309(19) . ? C100 C105 1.47(3) . ? C101 C102 1.333(19) . ? C102 C103 1.26(2) . ? C103 C104 1.22(3) . ? C104 C105 1.48(3) . ? C106 C108 1.13(4) 2_666 ? C106 C107 1.381(18) . ? C107 C108 1.402(18) . ? C108 C106 1.13(4) 2_666 ? 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 N1 Ni1 C7 167.7(3) . . ? N1 Ni1 C1 126.1(2) . . ? C7 Ni1 C1 41.9(3) . . ? N1 Ni1 P1 91.75(13) . . ? C7 Ni1 P1 100.4(2) . . ? C1 Ni1 P1 136.8(2) . . ? N1 Ni1 C6 96.6(2) . . ? C7 Ni1 C6 71.4(3) . . ? C1 Ni1 C6 38.1(3) . . ? P1 Ni1 C6 170.69(17) . . ? C21 P1 C15 106.1(3) . . ? C21 P1 C8 103.7(3) . . ? C15 P1 C8 105.0(3) . . ? C21 P1 Ni1 109.0(2) . . ? C15 P1 Ni1 124.1(2) . . ? C8 P1 Ni1 107.10(17) . . ? C14 O1 B1 128.6(4) . . ? C14 N1 Ni1 133.7(3) . . ? O1 B1 C33 109.1(4) . . ? O1 B1 C27 102.8(4) . . ? C33 B1 C27 112.3(4) . . ? O1 B1 C39 112.7(4) . . ? C33 B1 C39 114.5(5) . . ? C27 B1 C39 104.8(4) . . ? C6 C1 C2 116.4(7) . . ? C6 C1 C7 119.7(8) . . ? C2 C1 C7 121.9(8) . . ? C6 C1 Ni1 77.8(4) . . ? C2 C1 Ni1 113.6(6) . . ? C7 C1 Ni1 66.6(4) . . ? C3 C2 C1 120.6(9) . . ? C2 C3 C4 120.4(9) . . ? C5 C4 C3 120.7(8) . . ? C4 C5 C6 119.6(9) . . ? C1 C6 C5 122.2(8) . . ? C1 C6 Ni1 64.0(4) . . ? C5 C6 Ni1 122.0(5) . . ? C1 C7 Ni1 71.5(4) . . ? C13 C8 C9 117.8(5) . . ? C13 C8 P1 121.3(4) . . ? C9 C8 P1 120.9(4) . . ? C10 C9 C8 118.5(5) . . ? C10 C9 C14 118.2(5) . . ? C8 C9 C14 123.2(5) . . ? C9 C10 C11 122.4(6) . . ? C12 C11 C10 118.9(7) . . ? C13 C12 C11 120.3(6) . . ? C12 C13 C8 122.1(5) . . ? N1 C14 O1 125.6(4) . . ? N1 C14 C9 122.6(4) . . ? O1 C14 C9 111.7(5) . . ? C20 C15 C16 118.2(5) . . ? C20 C15 P1 122.5(4) . . ? C16 C15 P1 119.3(4) . . ? C17 C16 C15 120.4(6) . . ? C18 C17 C16 121.1(6) . . ? C19 C18 C17 119.1(6) . . ? C18 C19 C20 120.7(6) . . ? C15 C20 C19 120.6(6) . . ? C22 C21 C26 119.2(7) . . ? C22 C21 P1 123.3(6) . . ? C26 C21 P1 117.5(6) . . ? C23 C22 C21 121.9(9) . . ? C24 C23 C22 118.4(10) . . ? C24 C25 C26 119.4(10) . . ? C25 C24 C23 122.0(9) . . ? C21 C26 C25 118.9(10) . . ? C32 C27 C28 113.7(5) . . ? C32 C27 B1 120.3(5) . . ? C28 C27 B1 126.0(5) . . ? F1 C28 C29 113.8(5) . . ? F1 C28 C27 121.7(5) . . ? C29 C28 C27 124.5(6) . . ? F2 C29 C28 121.6(6) . . ? F2 C29 C30 119.1(6) . . ? C28 C29 C30 119.2(6) . . ? F3 C30 C31 120.2(7) . . ? F3 C30 C29 120.9(6) . . ? C31 C30 C29 118.9(6) . . ? F4 C31 C30 120.3(6) . . ? F4 C31 C32 120.3(6) . . ? C30 C31 C32 119.4(6) . . ? F5 C32 C27 119.7(5) . . ? F5 C32 C31 116.0(6) . . ? C27 C32 C31 124.2(6) . . ? C38 C33 C34 111.4(6) . . ? C38 C33 B1 127.7(5) . . ? C34 C33 B1 120.8(5) . . ? F6 C34 C35 117.1(6) . . ? F6 C34 C33 117.3(6) . . ? C35 C34 C33 125.5(7) . . ? F7 C35 C36 121.4(7) . . ? F7 C35 C34 120.6(8) . . ? C36 C35 C34 118.0(7) . . ? C37 C36 F8 120.8(9) . . ? C37 C36 C35 120.4(7) . . ? F8 C36 C35 118.8(8) . . ? C36 C37 F9 120.0(8) . . ? C36 C37 C38 119.2(8) . . ? F9 C37 C38 120.8(8) . . ? F10 C38 C37 114.1(6) . . ? F10 C38 C33 120.5(6) . . ? C37 C38 C33 125.5(7) . . ? C44 C39 C40 114.7(5) . . ? C44 C39 B1 127.2(5) . . ? C40 C39 B1 118.2(5) . . ? F11 C40 C41 116.0(5) . . ? F11 C40 C39 120.9(5) . . ? C41 C40 C39 123.1(5) . . ? F12 C41 C42 119.6(5) . . ? F12 C41 C40 120.1(6) . . ? C42 C41 C40 120.3(5) . . ? F13 C42 C41 120.7(6) . . ? F13 C42 C43 120.8(6) . . ? C41 C42 C43 118.5(6) . . ? F14 C43 C44 121.0(6) . . ? F14 C43 C42 119.5(6) . . ? C44 C43 C42 119.5(6) . . ? F15 C44 C39 120.9(5) . . ? F15 C44 C43 115.0(5) . . ? C39 C44 C43 124.0(5) . . ? N2 Ni2 C51 169.6(3) . . ? N2 Ni2 C45 128.2(3) . . ? C51 Ni2 C45 42.4(3) . . ? N2 Ni2 P2 92.33(14) . . ? C51 Ni2 P2 98.1(2) . . ? C45 Ni2 P2 134.3(2) . . ? N2 Ni2 C46 97.7(2) . . ? C51 Ni2 C46 71.9(3) . . ? C45 Ni2 C46 39.0(3) . . ? P2 Ni2 C46 169.2(2) . . ? C59 P2 C52 105.6(3) . . ? C59 P2 C65 105.7(3) . . ? C52 P2 C65 104.4(3) . . ? C59 P2 Ni2 110.7(2) . . ? C52 P2 Ni2 107.24(17) . . ? C65 P2 Ni2 121.99(19) . . ? C58 O2 B2 129.5(5) . . ? C58 N2 Ni2 134.2(4) . . ? O2 B2 C83 107.2(5) . . ? O2 B2 C71 111.8(5) . . ? C83 B2 C71 116.3(5) . . ? O2 B2 C77 101.8(5) . . ? C83 B2 C77 112.8(5) . . ? C71 B2 C77 106.0(5) . . ? C46 C45 C51 117.8(9) . . ? C46 C45 C50 117.2(8) . . ? C51 C45 C50 123.3(8) . . ? C46 C45 Ni2 77.6(4) . . ? C51 C45 Ni2 66.1(4) . . ? C50 C45 Ni2 114.5(6) . . ? C47 C46 C45 120.1(9) . . ? C47 C46 Ni2 120.6(5) . . ? C45 C46 Ni2 63.5(4) . . ? C48 C47 C46 120.0(9) . . ? C47 C48 C49 121.8(10) . . ? C50 C49 C48 120.7(10) . . ? C49 C50 C45 120.2(9) . . ? C45 C51 Ni2 71.5(4) . . ? C57 C52 C53 117.0(5) . . ? C57 C52 P2 121.1(4) . . ? C53 C52 P2 121.8(4) . . ? C54 C53 C52 119.4(5) . . ? C54 C53 C58 117.9(5) . . ? C52 C53 C58 122.7(5) . . ? C53 C54 C55 122.3(6) . . ? C54 C55 C56 118.8(6) . . ? C57 C56 C55 120.5(6) . . ? C56 C57 C52 122.0(6) . . ? N2 C58 O2 126.3(5) . . ? N2 C58 C53 122.4(5) . . ? O2 C58 C53 111.1(5) . . ? C64 C59 C60 117.5(6) . . ? C64 C59 P2 120.1(5) . . ? C60 C59 P2 122.4(5) . . ? C59 C60 C61 120.0(7) . . ? C62 C61 C60 120.6(7) . . ? C61 C62 C63 120.8(7) . . ? C62 C63 C64 120.4(8) . . ? C59 C64 C63 120.7(7) . . ? C70 C65 C66 118.5(6) . . ? C70 C65 P2 119.0(5) . . ? C66 C65 P2 122.4(5) . . ? C67 C66 C65 119.8(7) . . ? C68 C67 C66 121.3(7) . . ? C67 C68 C69 119.0(7) . . ? C68 C69 C70 120.5(7) . . ? C65 C70 C69 120.8(6) . . ? C72 C71 C76 113.3(5) . . ? C72 C71 B2 127.8(5) . . ? C76 C71 B2 118.7(5) . . ? C71 C72 F16 120.7(5) . . ? C71 C72 C73 124.8(6) . . ? F16 C72 C73 114.5(6) . . ? F17 C73 C74 121.6(6) . . ? F17 C73 C72 120.0(6) . . ? C74 C73 C72 118.3(6) . . ? C75 C74 F18 121.0(6) . . ? C75 C74 C73 119.4(6) . . ? F18 C74 C73 119.6(6) . . ? C74 C75 C76 121.6(6) . . ? C74 C75 F19 119.6(6) . . ? C76 C75 F19 118.8(6) . . ? F20 C76 C75 118.6(6) . . ? F20 C76 C71 118.8(5) . . ? C75 C76 C71 122.6(6) . . ? C82 C77 C78 113.6(5) . . ? C82 C77 B2 125.3(6) . . ? C78 C77 B2 121.1(5) . . ? F21 C78 C77 119.7(5) . . ? F21 C78 C79 116.1(7) . . ? C77 C78 C79 124.2(7) . . ? F22 C79 C80 120.9(7) . . ? F22 C79 C78 120.2(7) . . ? C80 C79 C78 118.9(8) . . ? F23 C80 C79 120.6(9) . . ? F23 C80 C81 120.6(8) . . ? C79 C80 C81 118.8(7) . . ? F24 C81 C80 119.2(7) . . ? F24 C81 C82 120.3(8) . . ? C80 C81 C82 120.5(7) . . ? F25 C82 C81 114.8(6) . . ? F25 C82 C77 121.4(5) . . ? C81 C82 C77 123.8(7) . . ? C84 C83 C88 113.5(6) . . ? C84 C83 B2 126.8(5) . . ? C88 C83 B2 119.7(5) . . ? F26 C84 C83 122.0(6) . . ? F26 C84 C85 113.9(6) . . ? C83 C84 C85 124.1(6) . . ? F27 C85 C86 121.8(8) . . ? F27 C85 C84 120.3(7) . . ? C86 C85 C84 117.9(7) . . ? F28 C86 C85 119.1(9) . . ? F28 C86 C87 120.1(8) . . ? C85 C86 C87 120.7(8) . . ? F29 C87 C88 122.2(7) . . ? F29 C87 C86 119.3(7) . . ? C88 C87 C86 118.4(7) . . ? F30 C88 C87 114.7(6) . . ? F30 C88 C83 119.9(6) . . ? C87 C88 C83 125.4(6) . . ? C101 C100 C105 116.4(16) . . ? C100 C101 C102 121.0(17) . . ? C103 C102 C101 127(2) . . ? C104 C103 C102 119(3) . . ? C103 C104 C105 124(3) . . ? C100 C105 C104 113.6(17) . . ? C108 C106 C107 114(2) 2_666 . ? C106 C107 C108 115.4(18) . . ? C106 C108 C107 129(2) 2_666 . ? _diffrn_measured_fraction_theta_max 0.965 _diffrn_reflns_theta_full 27.53 _diffrn_measured_fraction_theta_full 0.965 _refine_diff_density_max 1.969 _refine_diff_density_min -0.531 _refine_diff_density_rms 0.133 #===END data_13 _database_code_depnum_ccdc_archive 'CCDC 228032' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C47 H28 B F15 N Ni O P' _chemical_formula_weight 1008.19 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' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 '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 P21/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 12.5838(4) _cell_length_b 15.4674(5) _cell_length_c 22.3179(8) _cell_angle_alpha 90.00 _cell_angle_beta 89.4179(16) _cell_angle_gamma 90.00 _cell_volume 4343.7(3) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 11706 _cell_measurement_theta_min 0.998 _cell_measurement_theta_max 26.373 _exptl_crystal_description block _exptl_crystal_colour black _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.542 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2032 _exptl_absorpt_coefficient_mu 0.587 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _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 KappaCCD _diffrn_measurement_method CCD _diffrn_detector_area_resol_mean 9 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 22317 _diffrn_reflns_av_R_equivalents 0.1684 _diffrn_reflns_av_sigmaI/netI 0.1231 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.83 _diffrn_reflns_theta_max 26.12 _reflns_number_total 8540 _reflns_number_gt 5404 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _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^)+(0.0904P)^2^+10.6411P] 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 mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0033(9) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 8540 _refine_ls_number_parameters 607 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1426 _refine_ls_R_factor_gt 0.0957 _refine_ls_wR_factor_ref 0.2672 _refine_ls_wR_factor_gt 0.2362 _refine_ls_goodness_of_fit_ref 1.047 _refine_ls_restrained_S_all 1.047 _refine_ls_shift/su_max 0.000 _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 0.80778(6) 0.65343(7) 0.11804(4) 0.0635(3) Uani 1 1 d . . . P1 P 0.94678(12) 0.70864(10) 0.08222(7) 0.0489(4) Uani 1 1 d . . . N1 N 0.8545(4) 0.6727(4) 0.1999(2) 0.0593(14) Uani 1 1 d . . . O1 O 0.9607(3) 0.6582(3) 0.27826(16) 0.0538(10) Uani 1 1 d . . . B1 B 1.0493(5) 0.6699(4) 0.3233(3) 0.0423(13) Uani 1 1 d . . . F1 F 1.0657(4) 0.8263(3) 0.25497(17) 0.0753(11) Uani 1 1 d . . . F2 F 1.2434(5) 0.8986(3) 0.2094(2) 0.1146(19) Uani 1 1 d . . . F3 F 1.4326(5) 0.8189(5) 0.2202(3) 0.133(2) Uani 1 1 d . . . F4 F 1.4433(3) 0.6629(4) 0.2757(2) 0.1081(18) Uani 1 1 d . . . F5 F 1.2706(3) 0.5889(3) 0.31860(19) 0.0767(11) Uani 1 1 d . . . F6 F 0.8466(3) 0.6535(3) 0.38484(17) 0.0736(11) Uani 1 1 d . . . F7 F 0.7591(4) 0.7589(4) 0.4652(2) 0.1018(17) Uani 1 1 d . . . F8 F 0.8602(4) 0.9033(3) 0.50112(19) 0.0975(16) Uani 1 1 d . . . F9 F 1.0565(4) 0.9399(3) 0.45565(18) 0.0810(12) Uani 1 1 d . . . F10 F 1.1469(3) 0.8381(3) 0.37690(17) 0.0701(10) Uani 1 1 d . . . F11 F 0.9355(4) 0.4948(3) 0.31045(19) 0.0829(13) Uani 1 1 d . . . F12 F 0.9472(7) 0.3667(3) 0.3885(3) 0.134(3) Uani 1 1 d . . . F13 F 1.0762(8) 0.3745(4) 0.4829(3) 0.168(3) Uani 1 1 d . . . F14 F 1.1944(7) 0.5206(5) 0.5021(2) 0.147(3) Uani 1 1 d . . . F15 F 1.1835(4) 0.6520(3) 0.42582(18) 0.0827(13) Uani 1 1 d . . . C1 C 1.0502(4) 0.6479(4) 0.1218(2) 0.0452(12) Uani 1 1 d . . . C2 C 1.0338(4) 0.6194(4) 0.1809(2) 0.0420(12) Uani 1 1 d . . . C3 C 1.1064(5) 0.5592(4) 0.2043(2) 0.0482(13) Uani 1 1 d . . . H3 H 1.0958 0.5383 0.2429 0.058 Uiso 1 1 calc R . . C4 C 1.1923(5) 0.5306(4) 0.1715(3) 0.0578(15) Uani 1 1 d . . . H4 H 1.2379 0.4898 0.1878 0.069 Uiso 1 1 calc R . . C5 C 1.2110(5) 0.5617(5) 0.1153(3) 0.0682(18) Uani 1 1 d . . . H5 H 1.2703 0.5433 0.0935 0.082 Uiso 1 1 calc R . . C6 C 1.1407(5) 0.6213(5) 0.0905(3) 0.0582(16) Uani 1 1 d . . . H6 H 1.1545 0.6435 0.0525 0.070 Uiso 1 1 calc R . . C7 C 0.9782(5) 0.6957(4) 0.0025(3) 0.0559(15) Uani 1 1 d . . . C8 C 0.9785(7) 0.6135(5) -0.0221(3) 0.0690(19) Uani 1 1 d . . . H8 H 0.9647 0.5661 0.0024 0.083 Uiso 1 1 calc R . . C9 C 0.9988(7) 0.6008(6) -0.0823(3) 0.083(2) Uani 1 1 d . . . H9 H 0.9996 0.5450 -0.0979 0.100 Uiso 1 1 calc R . . C10 C 1.0174(9) 0.6682(7) -0.1187(3) 0.100(3) Uani 1 1 d . . . H10 H 1.0299 0.6595 -0.1594 0.121 Uiso 1 1 calc R . . C11 C 1.0177(11) 0.7504(7) -0.0951(4) 0.124(4) Uani 1 1 d . . . H11 H 1.0302 0.7975 -0.1201 0.149 Uiso 1 1 calc R . . C12 C 0.9997(8) 0.7636(5) -0.0348(3) 0.089(3) Uani 1 1 d . . . H12 H 1.0023 0.8194 -0.0193 0.107 Uiso 1 1 calc R . . C13 C 0.9675(7) 0.8229(5) 0.0952(3) 0.076(2) Uani 1 1 d . . . C14 C 1.0656(10) 0.8582(6) 0.1054(5) 0.117(4) Uani 1 1 d . . . H14 H 1.1252 0.8229 0.1080 0.140 Uiso 1 1 calc R . . C15 C 1.0750(15) 0.9455(8) 0.1118(7) 0.173(7) Uani 1 1 d . . . H15 H 1.1421 0.9679 0.1194 0.208 Uiso 1 1 calc R . . C16 C 0.9967(19) 0.9990(8) 0.1079(8) 0.212(11) Uani 1 1 d . . . H16 H 1.0076 1.0582 0.1117 0.255 Uiso 1 1 calc R . . C17 C 0.8973(19) 0.9666(8) 0.0979(8) 0.210(10) Uani 1 1 d . . . H17 H 0.8393 1.0037 0.0957 0.252 Uiso 1 1 calc R . . C18 C 0.8834(13) 0.8783(7) 0.0912(6) 0.147(6) Uani 1 1 d . . . H18 H 0.8159 0.8564 0.0838 0.176 Uiso 1 1 calc R . . C19 C 0.9468(4) 0.6519(4) 0.2208(2) 0.0445(12) Uani 1 1 d . . . C20 C 0.6970(9) 0.5258(9) 0.1160(5) 0.118(4) Uani 1 1 d . . . H20 H 0.7621 0.4996 0.1081 0.141 Uiso 1 1 calc R . . C21 C 0.6673(7) 0.5981(7) 0.0845(4) 0.088(3) Uani 1 1 d . . . C22 C 0.5696(8) 0.6360(10) 0.1010(5) 0.124(4) Uani 1 1 d . . . H22 H 0.5486 0.6864 0.0817 0.149 Uiso 1 1 calc R . . C23 C 0.5044(12) 0.6016(15) 0.1443(9) 0.161(9) Uani 1 1 d . . . H23 H 0.4403 0.6283 0.1540 0.194 Uiso 1 1 calc R . . C24 C 0.5327(15) 0.5317(17) 0.1715(9) 0.170(10) Uani 1 1 d . . . H24 H 0.4848 0.5091 0.1994 0.204 Uiso 1 1 calc R . . C25 C 0.6232(17) 0.4891(10) 0.1638(6) 0.155(6) Uani 1 1 d . . . H25 H 0.6401 0.4402 0.1860 0.186 Uiso 1 1 calc R . . C26 C 0.7397(7) 0.6319(8) 0.0417(3) 0.101(3) Uani 1 1 d . . . H26A H 0.7160 0.6828 0.0202 0.151 Uiso 1 1 calc R . . H26B H 0.7743 0.5899 0.0159 0.151 Uiso 1 1 calc R . . C27 C 0.7776(6) 0.7169(7) 0.2424(3) 0.091(3) Uani 1 1 d . . . H27 H 0.8192 0.7441 0.2741 0.136 Uiso 1 1 calc R . . C28 C 0.7102(7) 0.6421(10) 0.2719(4) 0.135(5) Uani 1 1 d . . . H28A H 0.6648 0.6168 0.2423 0.203 Uiso 1 1 calc R . . H28B H 0.6675 0.6653 0.3040 0.203 Uiso 1 1 calc R . . H28C H 0.7570 0.5987 0.2873 0.203 Uiso 1 1 calc R . . C29 C 0.7184(10) 0.7868(11) 0.2105(6) 0.165(7) Uani 1 1 d . . . H29A H 0.7652 0.8348 0.2030 0.248 Uiso 1 1 calc R . . H29B H 0.6595 0.8056 0.2349 0.248 Uiso 1 1 calc R . . H29C H 0.6926 0.7650 0.1731 0.248 Uiso 1 1 calc R . . C30 C 1.1582(4) 0.7054(4) 0.2916(2) 0.0470(12) Uani 1 1 d . . . C31 C 1.1578(5) 0.7828(4) 0.2606(3) 0.0555(15) Uani 1 1 d . . . C32 C 1.2496(7) 0.8212(5) 0.2366(3) 0.074(2) Uani 1 1 d . . . C33 C 1.3440(6) 0.7797(7) 0.2428(3) 0.080(2) Uani 1 1 d . . . C34 C 1.3481(5) 0.7023(6) 0.2704(3) 0.0697(19) Uani 1 1 d . . . C35 C 1.2580(5) 0.6665(4) 0.2936(3) 0.0547(14) Uani 1 1 d . . . C36 C 1.0615(5) 0.5808(4) 0.3635(2) 0.0521(14) Uani 1 1 d . . . C37 C 1.0035(6) 0.5050(5) 0.3569(3) 0.0668(18) Uani 1 1 d . . . C38 C 1.0085(10) 0.4367(6) 0.3966(4) 0.100(3) Uani 1 1 d . . . C39 C 1.0728(10) 0.4400(6) 0.4443(4) 0.103(3) Uani 1 1 d . . . C40 C 1.1319(9) 0.5145(7) 0.4536(4) 0.093(3) Uani 1 1 d . . . C41 C 1.1248(7) 0.5815(5) 0.4139(3) 0.0692(19) Uani 1 1 d . . . C42 C 1.0004(4) 0.7413(4) 0.3730(2) 0.0464(13) Uani 1 1 d . . . C43 C 0.9008(5) 0.7247(4) 0.3990(2) 0.0538(15) Uani 1 1 d . . . C44 C 0.8555(5) 0.7784(6) 0.4415(3) 0.0669(19) Uani 1 1 d . . . C45 C 0.9068(6) 0.8503(5) 0.4606(3) 0.0675(19) Uani 1 1 d . . . C46 C 1.0053(6) 0.8689(5) 0.4376(3) 0.0622(17) Uani 1 1 d . . . C47 C 1.0494(5) 0.8143(4) 0.3958(3) 0.0554(15) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ni1 0.0407(4) 0.0932(7) 0.0569(5) -0.0105(4) -0.0086(3) -0.0068(4) P1 0.0458(8) 0.0467(8) 0.0545(8) -0.0010(6) -0.0113(6) -0.0012(7) N1 0.039(3) 0.089(4) 0.050(3) -0.012(2) -0.0056(19) 0.010(3) O1 0.0357(19) 0.080(3) 0.046(2) -0.0042(19) -0.0005(15) 0.003(2) B1 0.033(3) 0.048(3) 0.046(3) 0.000(3) -0.003(2) 0.001(3) F1 0.089(3) 0.059(2) 0.078(3) 0.0115(18) 0.000(2) 0.018(2) F2 0.156(5) 0.081(3) 0.106(4) 0.026(3) -0.006(3) -0.055(4) F3 0.090(4) 0.177(6) 0.133(4) 0.000(4) 0.026(3) -0.078(4) F4 0.041(2) 0.165(5) 0.118(4) -0.029(3) 0.005(2) 0.010(3) F5 0.055(2) 0.064(2) 0.111(3) 0.001(2) -0.006(2) 0.023(2) F6 0.054(2) 0.094(3) 0.073(2) -0.015(2) 0.0149(17) -0.017(2) F7 0.065(3) 0.145(5) 0.095(3) -0.024(3) 0.033(2) 0.003(3) F8 0.109(4) 0.108(4) 0.075(3) -0.032(2) 0.019(2) 0.032(3) F9 0.104(3) 0.064(2) 0.075(2) -0.020(2) -0.009(2) 0.005(2) F10 0.064(2) 0.069(2) 0.077(2) -0.0156(19) 0.0052(18) -0.009(2) F11 0.088(3) 0.072(3) 0.088(3) -0.015(2) 0.006(2) -0.031(2) F12 0.192(7) 0.069(3) 0.140(5) 0.002(3) 0.053(4) -0.051(4) F13 0.285(11) 0.101(4) 0.116(4) 0.061(4) 0.024(5) 0.024(6) F14 0.209(7) 0.143(5) 0.090(4) 0.028(3) -0.060(4) 0.034(5) F15 0.087(3) 0.084(3) 0.077(3) -0.001(2) -0.033(2) 0.002(3) C1 0.034(3) 0.047(3) 0.055(3) -0.001(2) 0.000(2) 0.003(2) C2 0.034(3) 0.042(3) 0.050(3) -0.006(2) -0.004(2) -0.002(2) C3 0.049(3) 0.048(3) 0.048(3) 0.001(2) 0.002(2) 0.001(3) C4 0.047(3) 0.068(4) 0.058(3) 0.004(3) 0.003(3) 0.019(3) C5 0.053(4) 0.084(5) 0.067(4) 0.004(3) 0.013(3) 0.015(4) C6 0.050(3) 0.073(4) 0.052(3) 0.015(3) 0.007(2) 0.002(3) C7 0.058(4) 0.059(4) 0.051(3) 0.003(3) -0.010(3) -0.005(3) C8 0.091(5) 0.052(4) 0.064(4) 0.006(3) 0.004(3) -0.002(4) C9 0.104(6) 0.083(5) 0.063(4) -0.004(4) -0.003(4) -0.011(5) C10 0.132(8) 0.123(8) 0.046(4) 0.010(5) -0.002(4) -0.008(7) C11 0.207(14) 0.089(7) 0.076(6) 0.028(5) -0.005(7) -0.001(8) C12 0.142(8) 0.063(5) 0.063(4) 0.019(4) -0.013(4) -0.003(5) C13 0.105(6) 0.051(4) 0.073(4) -0.003(3) -0.040(4) 0.007(4) C14 0.144(10) 0.073(6) 0.135(8) 0.018(5) -0.065(7) -0.047(6) C15 0.239(18) 0.065(7) 0.219(14) 0.023(8) -0.131(13) -0.063(10) C16 0.35(3) 0.051(6) 0.240(17) -0.006(8) -0.187(19) -0.012(12) C17 0.32(3) 0.058(7) 0.260(18) -0.039(9) -0.154(18) 0.056(11) C18 0.179(14) 0.085(7) 0.178(11) -0.031(7) -0.087(10) 0.049(8) C19 0.032(3) 0.051(3) 0.051(3) -0.005(2) -0.001(2) 0.000(2) C20 0.096(7) 0.135(10) 0.121(8) -0.062(8) 0.012(6) -0.048(8) C21 0.065(5) 0.107(7) 0.091(6) -0.033(5) -0.010(4) -0.023(5) C22 0.065(6) 0.193(13) 0.115(8) -0.062(8) -0.018(5) -0.018(7) C23 0.057(6) 0.23(2) 0.194(18) -0.121(16) 0.006(9) -0.018(11) C24 0.113(15) 0.24(3) 0.152(15) -0.112(17) 0.039(11) -0.083(16) C25 0.208(18) 0.121(11) 0.137(11) -0.029(8) -0.018(11) -0.083(12) C26 0.065(5) 0.166(10) 0.070(5) -0.019(5) -0.019(4) -0.031(6) C27 0.048(4) 0.153(9) 0.072(4) -0.026(5) -0.009(3) 0.030(5) C28 0.049(4) 0.251(15) 0.105(7) -0.073(8) 0.019(4) -0.050(7) C29 0.122(10) 0.227(16) 0.147(10) -0.062(10) -0.038(7) 0.113(11) C30 0.042(3) 0.046(3) 0.052(3) -0.003(2) 0.000(2) 0.003(3) C31 0.065(4) 0.043(3) 0.058(3) 0.001(3) 0.006(3) -0.001(3) C32 0.103(6) 0.061(4) 0.058(4) 0.000(3) 0.004(4) -0.022(4) C33 0.058(4) 0.110(7) 0.071(5) -0.014(4) 0.012(3) -0.030(5) C34 0.045(4) 0.090(6) 0.074(4) -0.019(4) 0.005(3) -0.003(4) C35 0.041(3) 0.059(4) 0.064(4) -0.010(3) -0.001(2) 0.000(3) C36 0.059(4) 0.047(3) 0.050(3) 0.002(2) 0.002(3) 0.003(3) C37 0.082(5) 0.057(4) 0.061(4) -0.002(3) 0.012(3) 0.001(4) C38 0.157(10) 0.065(5) 0.078(6) 0.008(4) 0.035(6) -0.018(6) C39 0.168(10) 0.075(6) 0.067(5) 0.028(4) 0.012(6) 0.022(7) C40 0.124(8) 0.091(6) 0.065(5) 0.016(4) -0.012(4) 0.024(6) C41 0.090(5) 0.064(4) 0.054(4) 0.006(3) -0.004(3) 0.011(4) C42 0.042(3) 0.054(3) 0.043(3) 0.002(2) -0.004(2) 0.005(3) C43 0.041(3) 0.070(4) 0.051(3) -0.006(3) 0.003(2) 0.002(3) C44 0.049(4) 0.098(6) 0.054(4) 0.004(4) 0.011(3) 0.020(4) C45 0.075(5) 0.079(5) 0.048(3) -0.015(3) 0.002(3) 0.029(4) C46 0.070(4) 0.067(4) 0.050(3) -0.009(3) -0.005(3) 0.013(4) C47 0.054(3) 0.063(4) 0.049(3) 0.001(3) -0.002(2) 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 C26 1.944(7) . ? Ni1 N1 1.948(5) . ? Ni1 P1 2.0975(18) . ? Ni1 C21 2.109(8) . ? Ni1 C20 2.417(11) . ? P1 C13 1.810(7) . ? P1 C7 1.829(6) . ? P1 C1 1.838(6) . ? N1 C19 1.297(7) . ? N1 C27 1.511(9) . ? O1 C19 1.299(6) . ? O1 B1 1.520(7) . ? B1 C30 1.631(8) . ? B1 C36 1.652(9) . ? B1 C42 1.678(8) . ? F1 C31 1.347(8) . ? F2 C32 1.345(9) . ? F3 C33 1.362(8) . ? F4 C34 1.350(9) . ? F5 C35 1.332(8) . ? F6 C43 1.335(7) . ? F7 C44 1.353(8) . ? F8 C45 1.349(7) . ? F9 C46 1.337(8) . ? F10 C47 1.344(7) . ? F11 C37 1.361(8) . ? F12 C38 1.342(11) . ? F13 C39 1.332(9) . ? F14 C40 1.348(10) . ? F15 C41 1.345(9) . ? C1 C6 1.392(8) . ? C1 C2 1.403(8) . ? C2 C3 1.408(8) . ? C2 C19 1.492(7) . ? C3 C4 1.372(8) . ? C4 C5 1.363(9) . ? C5 C6 1.395(9) . ? C7 C12 1.367(10) . ? C7 C8 1.385(10) . ? C8 C9 1.381(10) . ? C9 C10 1.340(12) . ? C10 C11 1.376(14) . ? C11 C12 1.378(12) . ? C13 C18 1.366(14) . ? C13 C14 1.371(13) . ? C14 C15 1.363(15) . ? C15 C16 1.29(2) . ? C16 C17 1.37(3) . ? C17 C18 1.386(17) . ? C20 C21 1.374(16) . ? C20 C25 1.517(19) . ? C21 C22 1.407(14) . ? C21 C26 1.414(13) . ? C22 C23 1.37(2) . ? C23 C24 1.29(3) . ? C24 C25 1.33(2) . ? C27 C29 1.498(15) . ? C27 C28 1.574(16) . ? C30 C31 1.382(8) . ? C30 C35 1.394(8) . ? C31 C32 1.401(10) . ? C32 C33 1.359(12) . ? C33 C34 1.347(12) . ? C34 C35 1.361(9) . ? C36 C41 1.385(9) . ? C36 C37 1.390(9) . ? C37 C38 1.379(11) . ? C38 C39 1.345(15) . ? C39 C40 1.388(14) . ? C40 C41 1.367(11) . ? C42 C47 1.384(9) . ? C42 C43 1.400(8) . ? C43 C44 1.379(9) . ? C44 C45 1.357(11) . ? C45 C46 1.367(11) . ? C46 C47 1.373(9) . ? 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 C26 Ni1 N1 171.3(3) . . ? C26 Ni1 P1 96.3(3) . . ? N1 Ni1 P1 92.10(17) . . ? C26 Ni1 C21 40.6(4) . . ? N1 Ni1 C21 131.1(3) . . ? P1 Ni1 C21 136.8(3) . . ? C26 Ni1 C20 65.4(4) . . ? N1 Ni1 C20 108.8(3) . . ? P1 Ni1 C20 143.5(3) . . ? C21 Ni1 C20 34.5(4) . . ? C13 P1 C7 103.5(3) . . ? C13 P1 C1 108.5(3) . . ? C7 P1 C1 105.3(3) . . ? C13 P1 Ni1 117.2(3) . . ? C7 P1 Ni1 119.8(2) . . ? C1 P1 Ni1 101.56(18) . . ? C19 N1 C27 117.2(5) . . ? C19 N1 Ni1 125.4(4) . . ? C27 N1 Ni1 117.4(4) . . ? C19 O1 B1 140.3(4) . . ? O1 B1 C30 111.8(4) . . ? O1 B1 C36 109.4(5) . . ? C30 B1 C36 115.8(5) . . ? O1 B1 C42 104.4(4) . . ? C30 B1 C42 111.5(5) . . ? C36 B1 C42 103.0(4) . . ? C6 C1 C2 119.3(5) . . ? C6 C1 P1 119.3(4) . . ? C2 C1 P1 120.9(4) . . ? C1 C2 C3 117.8(5) . . ? C1 C2 C19 123.7(5) . . ? C3 C2 C19 118.4(5) . . ? C4 C3 C2 121.7(5) . . ? C5 C4 C3 120.3(6) . . ? C4 C5 C6 119.5(6) . . ? C1 C6 C5 121.1(5) . . ? C12 C7 C8 117.7(6) . . ? C12 C7 P1 123.2(6) . . ? C8 C7 P1 119.1(5) . . ? C9 C8 C7 121.1(7) . . ? C10 C9 C8 120.5(8) . . ? C9 C10 C11 119.3(8) . . ? C10 C11 C12 120.6(8) . . ? C7 C12 C11 120.7(8) . . ? C18 C13 C14 117.4(9) . . ? C18 C13 P1 119.3(8) . . ? C14 C13 P1 123.2(7) . . ? C15 C14 C13 119.4(13) . . ? C16 C15 C14 124.2(15) . . ? C15 C16 C17 118.4(12) . . ? C16 C17 C18 119.8(16) . . ? C13 C18 C17 120.8(15) . . ? N1 C19 O1 117.8(5) . . ? N1 C19 C2 121.5(5) . . ? O1 C19 C2 120.6(4) . . ? C21 C20 C25 119.8(13) . . ? C21 C20 Ni1 60.4(5) . . ? C25 C20 Ni1 129.9(7) . . ? C20 C21 C22 116.5(11) . . ? C20 C21 C26 118.0(10) . . ? C22 C21 C26 125.3(12) . . ? C20 C21 Ni1 85.1(6) . . ? C22 C21 Ni1 118.1(7) . . ? C26 C21 Ni1 63.4(4) . . ? C23 C22 C21 122.6(15) . . ? C24 C23 C22 119.4(18) . . ? C23 C24 C25 127(2) . . ? C24 C25 C20 115.1(18) . . ? C21 C26 Ni1 76.0(5) . . ? C29 C27 N1 110.3(7) . . ? C29 C27 C28 117.5(9) . . ? N1 C27 C28 105.6(8) . . ? C31 C30 C35 113.5(6) . . ? C31 C30 B1 120.1(5) . . ? C35 C30 B1 126.4(5) . . ? F1 C31 C30 119.1(6) . . ? F1 C31 C32 117.4(6) . . ? C30 C31 C32 123.5(7) . . ? F2 C32 C33 121.4(8) . . ? F2 C32 C31 119.9(8) . . ? C33 C32 C31 118.6(7) . . ? C34 C33 C32 120.3(7) . . ? C34 C33 F3 122.0(9) . . ? C32 C33 F3 117.7(9) . . ? C33 C34 F4 118.6(7) . . ? C33 C34 C35 120.0(7) . . ? F4 C34 C35 121.3(8) . . ? F5 C35 C34 115.1(6) . . ? F5 C35 C30 120.9(6) . . ? C34 C35 C30 124.0(7) . . ? C41 C36 C37 113.6(6) . . ? C41 C36 B1 119.4(6) . . ? C37 C36 B1 126.5(5) . . ? F11 C37 C38 115.7(8) . . ? F11 C37 C36 120.8(6) . . ? C38 C37 C36 123.4(8) . . ? F12 C38 C39 119.2(8) . . ? F12 C38 C37 120.1(10) . . ? C39 C38 C37 120.7(9) . . ? F13 C39 C38 120.5(11) . . ? F13 C39 C40 120.9(10) . . ? C38 C39 C40 118.6(7) . . ? F14 C40 C41 120.7(10) . . ? F14 C40 C39 119.8(8) . . ? C41 C40 C39 119.6(8) . . ? F15 C41 C40 116.5(7) . . ? F15 C41 C36 119.3(6) . . ? C40 C41 C36 124.2(8) . . ? C47 C42 C43 113.4(5) . . ? C47 C42 B1 128.1(5) . . ? C43 C42 B1 118.3(5) . . ? F6 C43 C44 116.9(6) . . ? F6 C43 C42 120.7(5) . . ? C44 C43 C42 122.4(6) . . ? F7 C44 C45 119.2(6) . . ? F7 C44 C43 119.8(7) . . ? C45 C44 C43 121.0(6) . . ? F8 C45 C44 120.3(7) . . ? F8 C45 C46 120.6(7) . . ? C44 C45 C46 119.1(6) . . ? F9 C46 C45 119.8(6) . . ? F9 C46 C47 121.1(6) . . ? C45 C46 C47 119.1(7) . . ? F10 C47 C46 114.0(6) . . ? F10 C47 C42 121.1(5) . . ? C46 C47 C42 124.9(6) . . ? _diffrn_measured_fraction_theta_max 0.986 _diffrn_reflns_theta_full 26.12 _diffrn_measured_fraction_theta_full 0.986 _refine_diff_density_max 1.095 _refine_diff_density_min -0.551 _refine_diff_density_rms 0.087