Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2002 data_global #======================================================================= _journal_coden_Cambridge 186 _publ_requested_journal 'Dalton Transactions' # 1. SUBMISSION DETAILS _publ_contact_author 'Dr Thomas Braun' _publ_contact_author_address ; Dr Thomas Braun Fakultät für Chemie, ACIII Universität Bielefeld Postfach 100131 33501 Bielefeld D-33501 GERMANY ; _publ_contact_author_email 'THOMAS.BRAUN@UNI-BIELEFELD.DE' _publ_requested_coeditor_name ? _publ_contact_letter ; Please consider this CIF submission for deposition To: DALTON@RSC.ORG Subject: Depositing Crystal Structure Data Dear Madam or Sir, please find enclosed the crystallographic data of complex2 'C16 H30 Cl F3 N2 Ni P2' complex7 'C40 H66 Cl F3 N2 Ni P2' for deposition in your data file. With kind regards Beate Neumann ; #=========================================================================== # 2. PROCESSING SUMMARY _journal_coden_Cambridge 186 _journal_name_full ? _journal_year ? _journal_volume ? _journal_issue ? _journal_page_first ? _journal_page_last ? #=========================================================================== # 3. TITLE AND AUTHOR LIST _publ_section_title ; Synthesis, Structure and Reactivity of Fluorovinyl Nickel Complexes: Formation of a Phosphonioethenyl Complex ; # The loop structure below should contain the names and addresses of all # authors, in the required order of publication. Repeat as necessary. loop_ _publ_author_name _publ_author_address 'Braun, Thomas' ; Fakult\"at f. Chemie Universit\"at Bielefeld 33615 Bielefeld Germany ; 'Bl\"ocker, Berit' ; Fakult\"at f. Chemie Universit\"at Bielefeld 33615 Bielefeld Germany ; 'Schorlemer, Verena' ; Fakult\"at f. Chemie Universit\"at Bielefeld 33615 Bielefeld Germany ; 'Neumann, Beate' ; Fakult\"at f. Chemie Universit\"at Bielefeld 33615 Bielefeld Germany ; 'Stammler, Anja' ; Fakult\"at f. Chemie Universit\"at Bielefeld 33615 Bielefeld Germany ; 'Stammler, Hans-Georg' ; Fakult\"at f. Chemie Universit\"at Bielefeld 33615 Bielefeld Germany ; #======================================================================= data_complex2 _database_code_CSD 178083 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C14 H30 Br2 F2 Ni P2' _chemical_formula_weight 516.85 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' 'Br' 'Br' -0.2901 2.4595 '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' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ni' 'Ni' 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 21/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 11.9720(2) _cell_length_b 10.9550(2) _cell_length_c 16.3510(3) _cell_angle_alpha 90.00 _cell_angle_beta 99.1400(7) _cell_angle_gamma 90.00 _cell_volume 2117.26(7) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 6370 _cell_measurement_theta_min 2.910 _cell_measurement_theta_max 30.034 _exptl_crystal_description Irregular _exptl_crystal_colour Yellow _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.621 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1040 _exptl_absorpt_coefficient_mu 4.850 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.3059 _exptl_absorpt_correction_T_max 0.4756 _exptl_absorpt_process_details ? _exptl_special_details ; ; _diffrn_ambient_temperature 100(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 'Kappa CCD' _diffrn_measurement_method 'CCD; rotation images; thick slices' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 41632 _diffrn_reflns_av_R_equivalents 0.036 _diffrn_reflns_av_sigmaI/netI 0.0287 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.95 _diffrn_reflns_theta_max 29.97 _reflns_number_total 6140 _reflns_number_gt 5117 _reflns_threshold_expression >2sigma(I) _computing_data_collection KappaCCD _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'Denzo and Scalepak (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL-PLUS(1990)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0286P)^2^+0.7069P] 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 refall _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6140 _refine_ls_number_parameters 347 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0383 _refine_ls_R_factor_gt 0.0272 _refine_ls_wR_factor_ref 0.0632 _refine_ls_wR_factor_gt 0.0589 _refine_ls_goodness_of_fit_ref 1.062 _refine_ls_restrained_S_all 1.062 _refine_ls_shift/su_max 0.002 _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_symetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Br1 Br 0.525894(13) 0.420232(16) 0.134471(12) 0.02959(6) Uani 1 1 d . . . Ni1 Ni 0.720245(16) 0.454559(18) 0.167519(12) 0.01842(6) Uani 1 1 d . A . P1 P 0.75110(3) 0.29199(4) 0.09281(2) 0.01976(9) Uani 1 1 d . . . P2 P 0.68520(3) 0.62106(4) 0.23671(3) 0.01997(9) Uani 1 1 d . . . C1 C 0.68187(16) 0.15234(17) 0.11991(13) 0.0307(4) Uani 1 1 d . . . H1A H 0.6007(18) 0.1667(19) 0.1040(13) 0.029(5) Uiso 1 1 d . . . H1B H 0.705(2) 0.089(2) 0.0867(16) 0.050(7) Uiso 1 1 d . . . C2 C 0.7106(2) 0.1220(3) 0.21195(17) 0.0534(7) Uani 1 1 d . . . H2A H 0.673(2) 0.047(3) 0.2235(17) 0.058(8) Uiso 1 1 d . . . H2B H 0.678(3) 0.184(3) 0.246(2) 0.081(10) Uiso 1 1 d . . . H2C H 0.786(3) 0.113(3) 0.2285(19) 0.073(9) Uiso 1 1 d . . . C3 C 0.89817(15) 0.24568(18) 0.09238(12) 0.0284(4) Uani 1 1 d . . . H3A H 0.938(2) 0.315(2) 0.0822(14) 0.042(6) Uiso 1 1 d . . . H3B H 0.9264(19) 0.225(2) 0.1477(15) 0.036(6) Uiso 1 1 d . . . C4 C 0.91812(19) 0.1414(2) 0.03433(14) 0.0370(4) Uani 1 1 d . . . H4A H 0.998(2) 0.126(2) 0.0371(17) 0.060(8) Uiso 1 1 d . . . H4B H 0.888(2) 0.162(2) -0.0236(16) 0.049(7) Uiso 1 1 d . . . H4C H 0.881(2) 0.068(2) 0.0457(16) 0.044(7) Uiso 1 1 d . . . C5 C 0.69215(16) 0.31564(17) -0.01610(11) 0.0274(3) Uani 1 1 d . . . H5A H 0.701(2) 0.241(2) -0.0452(16) 0.055(7) Uiso 1 1 d . . . H5B H 0.612(2) 0.333(2) -0.0166(14) 0.044(6) Uiso 1 1 d . . . C6 C 0.74684(19) 0.4225(2) -0.05387(13) 0.0359(4) Uani 1 1 d . . . H6A H 0.714(2) 0.438(2) -0.1103(18) 0.052(7) Uiso 1 1 d . . . H6B H 0.822(2) 0.406(2) -0.0524(15) 0.046(7) Uiso 1 1 d . . . H6C H 0.736(2) 0.500(3) -0.0246(16) 0.054(7) Uiso 1 1 d . . . C7 C 0.59978(17) 0.59092(17) 0.31747(12) 0.0290(4) Uani 1 1 d . . . H7A H 0.5841(17) 0.670(2) 0.3403(13) 0.030(5) Uiso 1 1 d . . . H7B H 0.531(2) 0.560(2) 0.2886(14) 0.035(6) Uiso 1 1 d . . . C8 C 0.6554(3) 0.5022(3) 0.38271(16) 0.0541(7) Uani 1 1 d . . . H8A H 0.609(2) 0.488(3) 0.4234(18) 0.058(8) Uiso 1 1 d . . . H8B H 0.728(3) 0.533(3) 0.4103(19) 0.068(10) Uiso 1 1 d . . . H8C H 0.673(3) 0.425(3) 0.358(2) 0.077(10) Uiso 1 1 d . . . C9 C 0.60017(17) 0.73442(17) 0.17212(12) 0.0298(4) Uani 1 1 d . . . H9A H 0.5288(19) 0.697(2) 0.1547(14) 0.036(6) Uiso 1 1 d . . . H9B H 0.5882(18) 0.801(2) 0.2046(14) 0.037(6) Uiso 1 1 d . . . C10 C 0.6502(3) 0.7737(2) 0.09659(17) 0.0545(7) Uani 1 1 d . . . H10A H 0.603(2) 0.837(3) 0.0651(17) 0.057(7) Uiso 1 1 d . . . H10B H 0.660(3) 0.706(3) 0.060(2) 0.081(10) Uiso 1 1 d . . . H10C H 0.721(2) 0.803(2) 0.1118(16) 0.045(7) Uiso 1 1 d . . . C11 C 0.80661(15) 0.70652(19) 0.29014(14) 0.0327(4) Uani 1 1 d . . . H11A H 0.857(2) 0.647(2) 0.3239(15) 0.042(6) Uiso 1 1 d . . . H11B H 0.847(2) 0.735(2) 0.2523(17) 0.056(8) Uiso 1 1 d . . . C12 C 0.78116(17) 0.80991(19) 0.34698(14) 0.0361(4) Uani 1 1 d . . . H12A H 0.848(2) 0.855(2) 0.3677(16) 0.053(7) Uiso 1 1 d . . . H12B H 0.750(2) 0.779(2) 0.3945(17) 0.053(7) Uiso 1 1 d . . . H12C H 0.725(2) 0.865(2) 0.3188(16) 0.050(7) Uiso 1 1 d . . . C13 C 0.87570(14) 0.48164(17) 0.19549(12) 0.0282(4) Uani 1 1 d . . . Br2 Br 0.94965(11) 0.40604(11) 0.28937(6) 0.0371(3) Uani 0.5260(12) 1 d P A 1 C14 C 0.9431(7) 0.5514(6) 0.1567(4) 0.0324(13) Uani 0.5260(12) 1 d P A 1 F1 F 0.9015(2) 0.6198(2) 0.08515(17) 0.0412(6) Uani 0.5260(12) 1 d P A 1 F2 F 1.05002(17) 0.5762(2) 0.17416(17) 0.0485(7) Uani 0.5260(12) 1 d P A 1 Br2A Br 0.95420(7) 0.57979(7) 0.13215(6) 0.0400(2) Uani 0.4740(12) 1 d P A 2 C14A C 0.9452(10) 0.4313(11) 0.2668(7) 0.038(3) Uani 0.4740(12) 1 d P A 2 F1A F 0.9044(3) 0.3579(3) 0.32006(18) 0.0409(6) Uani 0.4740(12) 1 d P A 2 F2A F 1.0547(2) 0.4491(3) 0.29081(19) 0.0540(8) Uani 0.4740(12) 1 d P A 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 Br1 0.01644(8) 0.02609(9) 0.04519(11) -0.00498(7) 0.00171(7) -0.00160(6) Ni1 0.01515(9) 0.01928(10) 0.02094(10) -0.00028(8) 0.00323(7) -0.00042(7) P1 0.01949(18) 0.01912(19) 0.02062(19) 0.00002(15) 0.00300(15) -0.00033(15) P2 0.01688(18) 0.01914(19) 0.0241(2) -0.00015(15) 0.00389(15) 0.00082(14) C1 0.0310(9) 0.0225(9) 0.0396(10) 0.0037(7) 0.0092(8) -0.0004(7) C2 0.0392(12) 0.0607(16) 0.0580(15) 0.0381(14) 0.0008(11) -0.0049(12) C3 0.0230(8) 0.0298(9) 0.0325(9) -0.0077(8) 0.0044(7) 0.0028(7) C4 0.0337(10) 0.0396(12) 0.0377(11) -0.0113(9) 0.0061(8) 0.0094(9) C5 0.0324(9) 0.0274(9) 0.0216(8) -0.0023(7) 0.0017(7) 0.0004(7) C6 0.0379(11) 0.0426(12) 0.0286(10) 0.0099(9) 0.0093(8) 0.0020(9) C7 0.0330(9) 0.0240(8) 0.0330(9) 0.0015(7) 0.0149(8) 0.0046(7) C8 0.084(2) 0.0455(14) 0.0389(12) 0.0177(11) 0.0293(13) 0.0242(14) C9 0.0354(10) 0.0216(8) 0.0309(9) 0.0020(7) 0.0009(7) 0.0051(7) C10 0.080(2) 0.0411(13) 0.0457(13) 0.0217(11) 0.0204(13) 0.0131(13) C11 0.0210(8) 0.0329(10) 0.0444(11) -0.0164(9) 0.0057(8) -0.0020(7) C12 0.0269(9) 0.0305(10) 0.0491(12) -0.0160(9) 0.0003(9) 0.0018(8) C13 0.0204(8) 0.0300(9) 0.0346(9) -0.0126(7) 0.0058(7) -0.0016(7) Br2 0.0313(3) 0.0457(6) 0.0305(4) -0.0105(3) -0.0070(3) 0.0163(3) C14 0.037(3) 0.033(3) 0.029(3) -0.004(2) 0.008(2) -0.008(2) F1 0.0386(13) 0.0473(14) 0.0405(14) 0.0003(12) 0.0146(12) -0.0152(11) F2 0.0180(10) 0.0635(16) 0.0666(16) -0.0243(13) 0.0146(10) -0.0141(10) Br2A 0.0300(3) 0.0371(4) 0.0572(6) -0.0108(4) 0.0207(4) -0.0118(3) C14A 0.021(4) 0.035(5) 0.061(7) -0.025(4) 0.012(4) -0.008(3) F1A 0.0391(15) 0.0491(17) 0.0317(14) 0.0048(13) -0.0032(12) 0.0147(13) F2A 0.0211(12) 0.0679(19) 0.0655(19) -0.0322(15) -0.0162(12) 0.0139(12) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Br1 Ni1 2.3341(2) . ? Ni1 C13 1.8683(17) . ? Ni1 P2 2.2212(5) . ? Ni1 P1 2.2235(4) . ? P1 C5 1.8268(18) . ? P1 C1 1.8277(18) . ? P1 C3 1.8335(18) . ? P2 C7 1.8242(18) . ? P2 C11 1.8301(18) . ? P2 C9 1.8308(18) . ? C1 C2 1.526(3) . ? C1 H1A 0.98(2) . ? C1 H1B 0.95(3) . ? C2 H2A 0.97(3) . ? C2 H2B 1.00(4) . ? C2 H2C 0.91(3) . ? C3 C4 1.528(3) . ? C3 H3A 0.93(2) . ? C3 H3B 0.94(2) . ? C4 H4A 0.97(3) . ? C4 H4B 0.98(3) . ? C4 H4C 0.95(2) . ? C5 C6 1.519(3) . ? C5 H5A 0.96(3) . ? C5 H5B 0.97(2) . ? C6 H6A 0.96(3) . ? C6 H6B 0.92(3) . ? C6 H6C 1.00(3) . ? C7 C8 1.516(3) . ? C7 H7A 0.97(2) . ? C7 H7B 0.94(2) . ? C8 H8A 0.95(3) . ? C8 H8B 0.97(3) . ? C8 H8C 0.98(3) . ? C9 C10 1.518(3) . ? C9 H9A 0.95(2) . ? C9 H9B 0.92(2) . ? C10 H10A 0.99(3) . ? C10 H10B 0.97(3) . ? C10 H10C 0.90(3) . ? C11 C12 1.526(3) . ? C11 H11A 0.99(2) . ? C11 H11B 0.90(3) . ? C12 H12A 0.95(3) . ? C12 H12B 0.97(3) . ? C12 H12C 0.96(3) . ? C13 C14 1.341(6) . ? C13 C14A 1.431(10) . ? C13 Br2 1.842(2) . ? C13 Br2A 1.850(2) . ? C14 F2 1.296(8) . ? C14 F1 1.412(7) . ? C14A F2A 1.321(12) . ? C14A F1A 1.334(11) . ? 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 C13 Ni1 P2 90.36(5) . . ? C13 Ni1 P1 90.90(5) . . ? P2 Ni1 P1 177.285(18) . . ? C13 Ni1 Br1 179.22(6) . . ? P2 Ni1 Br1 89.324(13) . . ? P1 Ni1 Br1 89.441(13) . . ? C5 P1 C1 103.61(9) . . ? C5 P1 C3 104.95(9) . . ? C1 P1 C3 104.01(9) . . ? C5 P1 Ni1 110.47(6) . . ? C1 P1 Ni1 114.58(7) . . ? C3 P1 Ni1 117.85(6) . . ? C7 P2 C11 103.94(10) . . ? C7 P2 C9 102.48(9) . . ? C11 P2 C9 104.77(10) . . ? C7 P2 Ni1 113.15(6) . . ? C11 P2 Ni1 117.60(6) . . ? C9 P2 Ni1 113.33(6) . . ? C2 C1 P1 112.41(16) . . ? C2 C1 H1A 110.9(12) . . ? P1 C1 H1A 105.7(12) . . ? C2 C1 H1B 111.3(15) . . ? P1 C1 H1B 106.7(15) . . ? H1A C1 H1B 109.6(19) . . ? C1 C2 H2A 109.7(17) . . ? C1 C2 H2B 110.9(19) . . ? H2A C2 H2B 103(2) . . ? C1 C2 H2C 112(2) . . ? H2A C2 H2C 108(2) . . ? H2B C2 H2C 112(3) . . ? C4 C3 P1 117.01(14) . . ? C4 C3 H3A 111.2(15) . . ? P1 C3 H3A 107.5(14) . . ? C4 C3 H3B 110.5(13) . . ? P1 C3 H3B 105.2(13) . . ? H3A C3 H3B 104(2) . . ? C3 C4 H4A 110.8(16) . . ? C3 C4 H4B 111.0(15) . . ? H4A C4 H4B 107(2) . . ? C3 C4 H4C 112.5(15) . . ? H4A C4 H4C 110(2) . . ? H4B C4 H4C 106(2) . . ? C6 C5 P1 112.39(13) . . ? C6 C5 H5A 111.7(16) . . ? P1 C5 H5A 107.9(16) . . ? C6 C5 H5B 109.7(14) . . ? P1 C5 H5B 105.2(14) . . ? H5A C5 H5B 110(2) . . ? C5 C6 H6A 112.6(15) . . ? C5 C6 H6B 108.7(15) . . ? H6A C6 H6B 108(2) . . ? C5 C6 H6C 111.7(16) . . ? H6A C6 H6C 105(2) . . ? H6B C6 H6C 111(2) . . ? C8 C7 P2 113.03(15) . . ? C8 C7 H7A 112.9(12) . . ? P2 C7 H7A 106.4(12) . . ? C8 C7 H7B 111.6(13) . . ? P2 C7 H7B 104.2(14) . . ? H7A C7 H7B 108.1(18) . . ? C7 C8 H8A 110.7(17) . . ? C7 C8 H8B 111.2(18) . . ? H8A C8 H8B 108(2) . . ? C7 C8 H8C 111.1(19) . . ? H8A C8 H8C 110(2) . . ? H8B C8 H8C 105(3) . . ? C10 C9 P2 113.96(16) . . ? C10 C9 H9A 109.3(14) . . ? P2 C9 H9A 105.8(14) . . ? C10 C9 H9B 111.3(14) . . ? P2 C9 H9B 108.9(14) . . ? H9A C9 H9B 107.3(19) . . ? C9 C10 H10A 111.1(16) . . ? C9 C10 H10B 112.5(19) . . ? H10A C10 H10B 110(2) . . ? C9 C10 H10C 110.5(16) . . ? H10A C10 H10C 109(2) . . ? H10B C10 H10C 104(2) . . ? C12 C11 P2 116.75(13) . . ? C12 C11 H11A 108.0(14) . . ? P2 C11 H11A 107.3(14) . . ? C12 C11 H11B 110.1(17) . . ? P2 C11 H11B 108.9(17) . . ? H11A C11 H11B 105(2) . . ? C11 C12 H12A 111.3(16) . . ? C11 C12 H12B 111.6(15) . . ? H12A C12 H12B 107(2) . . ? C11 C12 H12C 111.4(15) . . ? H12A C12 H12C 109(2) . . ? H12B C12 H12C 106(2) . . ? C14 C13 C14A 106.8(6) . . ? C14 C13 Br2 113.9(4) . . ? C14A C13 Br2 7.1(5) . . ? C14 C13 Br2A 6.7(4) . . ? C14A C13 Br2A 113.5(5) . . ? Br2 C13 Br2A 120.55(10) . . ? C14 C13 Ni1 128.7(4) . . ? C14A C13 Ni1 124.5(5) . . ? Br2 C13 Ni1 117.43(11) . . ? Br2A C13 Ni1 122.02(11) . . ? F2 C14 C13 131.5(6) . . ? F2 C14 F1 106.1(4) . . ? C13 C14 F1 122.3(6) . . ? F2A C14A F1A 110.1(8) . . ? F2A C14A C13 127.4(9) . . ? F1A C14A C13 122.5(9) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 29.97 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.383 _refine_diff_density_min -0.804 _refine_diff_density_rms 0.074 #======================================================================== data_complex7 _database_code_CSD 178084 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C91 H83 B2 F50 N Ni O0.50 P3' _chemical_formula_weight 2321.82 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 13.40000(10) _cell_length_b 16.90400(10) _cell_length_c 24.1850(2) _cell_angle_alpha 75.4550(3) _cell_angle_beta 78.5900(4) _cell_angle_gamma 74.6890(5) _cell_volume 5063.45(6) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 16559 _cell_measurement_theta_min 2.910 _cell_measurement_theta_max 25.028 _exptl_crystal_description needle _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.523 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2346 _exptl_absorpt_coefficient_mu 0.376 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9020 _exptl_absorpt_correction_T_max 0.9634 _exptl_absorpt_process_details ? _exptl_special_details ; ; _diffrn_ambient_temperature 100(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; rotation images' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 69322 _diffrn_reflns_av_R_equivalents 0.091 _diffrn_reflns_av_sigmaI/netI 0.0843 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 3.06 _diffrn_reflns_theta_max 25.00 _reflns_number_total 17524 _reflns_number_gt 10945 _reflns_threshold_expression >2sigma(I) _computing_data_collection KappaCCD _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'Denzo and Scalepak (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL-PLUS (1990)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0250P)^2^+13.2801P] 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 17524 _refine_ls_number_parameters 1386 _refine_ls_number_restraints 9 _refine_ls_R_factor_all 0.1273 _refine_ls_R_factor_gt 0.0678 _refine_ls_wR_factor_ref 0.1409 _refine_ls_wR_factor_gt 0.1188 _refine_ls_goodness_of_fit_ref 1.071 _refine_ls_restrained_S_all 1.075 _refine_ls_shift/su_max 0.147 _refine_ls_shift/su_mean 0.003 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_symetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ni1 Ni 0.33615(4) 0.51615(3) 0.75605(3) 0.02736(15) Uani 1 1 d . . . P1 P 0.18315(9) 0.60485(8) 0.77323(6) 0.0336(3) Uani 1 1 d . . . P2 P 0.48431(8) 0.42278(7) 0.73726(5) 0.0249(3) Uani 1 1 d . . . P3 P 0.17894(9) 0.29019(7) 0.79167(5) 0.0277(3) Uani 1 1 d . . . F1 F 0.26857(19) 0.39425(16) 0.84726(11) 0.0352(6) Uani 1 1 d . . . F2 F 0.2274(2) 0.41062(16) 0.70491(11) 0.0394(7) Uani 1 1 d . . . N1 N 0.4411(3) 0.6574(2) 0.69774(17) 0.0344(9) Uani 1 1 d . . . C1 C 0.1033(3) 0.5709(3) 0.8406(2) 0.0411(13) Uani 1 1 d . . . H1A H 0.0830 0.5196 0.8386 0.049 Uiso 1 1 calc R . . H1B H 0.1462 0.5558 0.8723 0.049 Uiso 1 1 calc R . . C2 C 0.0035(4) 0.6363(3) 0.8557(2) 0.0478(14) Uani 1 1 d . . . H2A H 0.0226 0.6831 0.8649 0.072 Uiso 1 1 calc R . . H2B H -0.0401 0.6102 0.8892 0.072 Uiso 1 1 calc R . . H2C H -0.0354 0.6571 0.8227 0.072 Uiso 1 1 calc R . . C3 C 0.1003(4) 0.6156(4) 0.7192(2) 0.0588(17) Uani 1 1 d . . . H3A H 0.0854 0.5604 0.7216 0.071 Uiso 1 1 calc R . . H3B H 0.0329 0.6549 0.7280 0.071 Uiso 1 1 calc R . . C4 C 0.1467(5) 0.6459(5) 0.6610(3) 0.094(3) Uani 1 1 d . . . H4A H 0.1574 0.7021 0.6576 0.141 Uiso 1 1 calc R . . H4B H 0.1000 0.6481 0.6339 0.141 Uiso 1 1 calc R . . H4C H 0.2140 0.6078 0.6522 0.141 Uiso 1 1 calc R . . C5 C 0.1907(4) 0.7109(3) 0.7733(2) 0.0383(12) Uani 1 1 d . . . H5A H 0.2274 0.7347 0.7356 0.046 Uiso 1 1 calc R . . H5B H 0.1189 0.7462 0.7778 0.046 Uiso 1 1 calc R . . C6 C 0.2473(4) 0.7152(3) 0.8212(2) 0.0480(14) Uani 1 1 d . . . H6A H 0.2099 0.6940 0.8588 0.072 Uiso 1 1 calc R . . H6B H 0.2498 0.7735 0.8184 0.072 Uiso 1 1 calc R . . H6C H 0.3187 0.6808 0.8169 0.072 Uiso 1 1 calc R . . C7 C 0.6023(3) 0.4625(3) 0.7256(2) 0.0321(11) Uani 1 1 d . . . H7A H 0.5971 0.5118 0.6930 0.038 Uiso 1 1 calc R . . H7B H 0.6053 0.4821 0.7604 0.038 Uiso 1 1 calc R . . C8 C 0.7044(4) 0.3993(3) 0.7126(2) 0.0450(13) Uani 1 1 d . . . H8A H 0.7133 0.3522 0.7458 0.067 Uiso 1 1 calc R . . H8B H 0.7632 0.4267 0.7052 0.067 Uiso 1 1 calc R . . H8C H 0.7021 0.3787 0.6786 0.067 Uiso 1 1 calc R . . C9 C 0.5094(3) 0.3251(3) 0.79109(19) 0.0308(11) Uani 1 1 d . . . H9A H 0.4498 0.2981 0.7975 0.037 Uiso 1 1 calc R . . H9B H 0.5724 0.2866 0.7758 0.037 Uiso 1 1 calc R . . C10 C 0.5257(4) 0.3376(3) 0.8487(2) 0.0414(13) Uani 1 1 d . . . H10A H 0.5899 0.3575 0.8437 0.062 Uiso 1 1 calc R . . H10B H 0.5315 0.2841 0.8769 0.062 Uiso 1 1 calc R . . H10C H 0.4661 0.3791 0.8627 0.062 Uiso 1 1 calc R . . C11 C 0.4844(4) 0.3912(3) 0.67072(19) 0.0339(11) Uani 1 1 d . . . H11A H 0.5505 0.3501 0.6626 0.041 Uiso 1 1 calc R . . H11B H 0.4261 0.3631 0.6758 0.041 Uiso 1 1 calc R . . C12 C 0.4732(5) 0.4651(4) 0.6195(2) 0.0626(17) Uani 1 1 d . . . H12A H 0.4074 0.5056 0.6271 0.094 Uiso 1 1 calc R . . H12B H 0.4732 0.4451 0.5848 0.094 Uiso 1 1 calc R . . H12C H 0.5318 0.4922 0.6136 0.094 Uiso 1 1 calc R . . C13 C 0.2708(3) 0.4250(3) 0.7880(2) 0.0312(11) Uani 1 1 d . . . C14 C 0.2301(3) 0.3826(3) 0.7634(2) 0.0301(11) Uani 1 1 d . . . C15 C 0.2119(4) 0.2320(3) 0.7356(2) 0.0376(12) Uani 1 1 d . . . H15A H 0.1746 0.1857 0.7470 0.045 Uiso 1 1 calc R . . H15B H 0.1869 0.2693 0.7001 0.045 Uiso 1 1 calc R . . C16 C 0.3291(4) 0.1950(3) 0.7223(2) 0.0527(15) Uani 1 1 d . . . H16A H 0.3661 0.2406 0.7079 0.079 Uiso 1 1 calc R . . H16B H 0.3411 0.1615 0.6929 0.079 Uiso 1 1 calc R . . H16C H 0.3551 0.1592 0.7575 0.079 Uiso 1 1 calc R . . C17 C 0.2329(4) 0.2274(3) 0.85547(19) 0.0320(11) Uani 1 1 d . . . H17A H 0.3094 0.2228 0.8491 0.038 Uiso 1 1 calc R . . H17B H 0.2024 0.2557 0.8882 0.038 Uiso 1 1 calc R . . C18 C 0.2112(4) 0.1392(3) 0.8710(2) 0.0441(13) Uani 1 1 d . . . H18A H 0.1357 0.1436 0.8765 0.066 Uiso 1 1 calc R . . H18B H 0.2392 0.1079 0.9067 0.066 Uiso 1 1 calc R . . H18C H 0.2449 0.1097 0.8396 0.066 Uiso 1 1 calc R . . C19 C 0.0390(3) 0.3197(3) 0.8079(2) 0.0366(12) Uani 1 1 d . . . H19A H 0.0119 0.2685 0.8254 0.044 Uiso 1 1 calc R . . H19B H 0.0204 0.3557 0.8366 0.044 Uiso 1 1 calc R . . C20 C -0.0140(4) 0.3667(3) 0.7547(2) 0.0472(14) Uani 1 1 d . . . H20A H 0.0126 0.4173 0.7370 0.071 Uiso 1 1 calc R . . H20B H -0.0897 0.3825 0.7662 0.071 Uiso 1 1 calc R . . H20C H 0.0011 0.3303 0.7269 0.071 Uiso 1 1 calc R . . C21 C 0.4000(3) 0.6035(3) 0.7210(2) 0.0325(11) Uani 1 1 d . . . C22 C 0.4962(4) 0.7253(3) 0.6684(2) 0.0377(12) Uani 1 1 d . . . C23 C 0.4134(4) 0.8073(3) 0.6636(3) 0.0663(19) Uani 1 1 d . . . H23A H 0.3772 0.8138 0.7021 0.099 Uiso 1 1 calc R . . H23B H 0.3628 0.8065 0.6396 0.099 Uiso 1 1 calc R . . H23C H 0.4468 0.8544 0.6459 0.099 Uiso 1 1 calc R . . C24 C 0.5744(4) 0.7229(3) 0.7066(2) 0.0428(13) Uani 1 1 d . . . H24A H 0.5379 0.7287 0.7452 0.064 Uiso 1 1 calc R . . H24B H 0.6099 0.7691 0.6900 0.064 Uiso 1 1 calc R . . H24C H 0.6261 0.6693 0.7094 0.064 Uiso 1 1 calc R . . C25 C 0.5482(5) 0.7067(4) 0.6100(2) 0.0637(18) Uani 1 1 d . . . H25A H 0.5845 0.7509 0.5888 0.096 Uiso 1 1 calc R . . H25B H 0.4951 0.7045 0.5882 0.096 Uiso 1 1 calc R . . H25C H 0.5987 0.6525 0.6154 0.096 Uiso 1 1 calc R . . B1 B -0.0200(4) 0.2039(3) 0.6056(2) 0.0250(11) Uani 1 1 d . . . F3 F 0.2737(2) 0.00944(19) 0.73121(16) 0.0667(10) Uani 1 1 d . . . F4 F 0.1946(3) -0.0417(2) 0.81264(13) 0.0717(11) Uani 1 1 d . . . F5 F 0.1877(2) -0.08088(17) 0.73725(14) 0.0544(8) Uani 1 1 d . . . F6 F -0.1446(4) 0.1201(5) 0.87395(18) 0.130(4) Uani 0.850(8) 1 d P A 1 F7 F -0.2520(3) 0.1618(3) 0.81350(17) 0.0649(17) Uani 0.850(8) 1 d P A 1 F8 F -0.1731(4) 0.2450(3) 0.8252(2) 0.0739(17) Uani 0.850(8) 1 d P A 1 F6# F -0.2000(16) 0.0966(10) 0.8441(9) 0.043(7) Uiso 0.150(8) 1 d PD A 2 F7# F -0.222(2) 0.2355(12) 0.8098(12) 0.074(10) Uiso 0.150(8) 1 d PD A 2 F8# F -0.1128(17) 0.1627(14) 0.8667(8) 0.039(7) Uiso 0.150(8) 1 d PD A 2 F9 F -0.3364(2) 0.04730(18) 0.63588(13) 0.0510(8) Uani 1 1 d . . . F10 F -0.3873(2) 0.1199(2) 0.70083(13) 0.0594(9) Uani 1 1 d . . . F11 F -0.4728(2) 0.1470(2) 0.62963(14) 0.0623(9) Uani 1 1 d . . . F12 F -0.4080(4) 0.4119(3) 0.49734(18) 0.149(3) Uani 1 1 d . . . F13 F -0.3328(3) 0.3292(2) 0.44228(15) 0.0822(12) Uani 1 1 d . . . F14 F -0.2519(3) 0.4114(2) 0.45727(15) 0.0764(11) Uani 1 1 d . . . F15 F -0.0829(4) 0.5347(2) 0.64877(14) 0.0964(15) Uani 1 1 d . . . F16 F -0.1626(3) 0.53071(19) 0.58311(18) 0.0827(12) Uani 1 1 d . . . F17 F -0.0332(3) 0.58711(18) 0.56071(15) 0.0735(11) Uani 1 1 d . . . F18 F 0.3186(4) 0.4135(4) 0.5190(3) 0.098(3) Uani 0.798(9) 1 d P B 1 F19 F 0.3430(3) 0.3217(5) 0.59704(19) 0.096(3) Uani 0.798(9) 1 d P B 1 F20 F 0.3356(4) 0.2877(4) 0.5222(3) 0.099(3) Uani 0.798(9) 1 d P B 1 F18# F 0.3112(11) 0.4030(8) 0.5792(6) 0.039(5) Uiso 0.202(9) 1 d PD B 2 F19# F 0.3418(14) 0.2723(9) 0.5756(11) 0.075(7) Uiso 0.202(9) 1 d PD B 2 F20# F 0.3145(13) 0.3677(14) 0.5001(5) 0.055(6) Uiso 0.202(9) 1 d PD B 2 F21 F 0.0977(4) 0.2303(3) 0.37802(18) 0.0719(19) Uani 0.778(9) 1 d P C 1 F22 F 0.2338(6) 0.2258(5) 0.4049(2) 0.107(3) Uani 0.778(9) 1 d P C 1 F23 F 0.2175(8) 0.1279(5) 0.3680(3) 0.124(4) Uani 0.778(9) 1 d P C 1 F21# F 0.166(2) 0.2496(8) 0.3903(10) 0.089(7) Uiso 0.222(9) 1 d PD C 2 F22# F 0.2869(7) 0.1428(9) 0.4024(6) 0.045(5) Uiso 0.222(9) 1 d PD C 2 F23# F 0.1779(18) 0.1160(14) 0.3726(10) 0.058(7) Uiso 0.222(9) 1 d PD C 2 F24 F 0.1341(3) -0.12462(19) 0.51171(15) 0.0685(10) Uani 1 1 d . . . F25 F 0.2230(3) -0.1180(2) 0.5734(2) 0.1011(16) Uani 1 1 d . . . F26 F 0.0605(3) -0.11286(19) 0.59578(16) 0.0731(10) Uani 1 1 d . . . C26 C -0.0066(3) 0.1575(2) 0.67268(18) 0.0224(10) Uani 1 1 d . . . C27 C 0.0813(3) 0.0951(2) 0.68866(19) 0.0235(10) Uani 1 1 d . . . H27 H 0.1365 0.0801 0.6592 0.028 Uiso 1 1 calc R . . C28 C 0.0914(3) 0.0543(3) 0.74539(19) 0.0258(10) Uani 1 1 d . . . C29 C 0.0142(3) 0.0755(3) 0.78996(19) 0.0302(11) Uani 1 1 d . . . H29 H 0.0201 0.0476 0.8289 0.036 Uiso 1 1 calc R . . C30 C -0.0722(3) 0.1392(3) 0.77561(18) 0.0279(10) Uani 1 1 d . A . C31 C -0.0820(3) 0.1789(3) 0.71901(18) 0.0262(10) Uani 1 1 d . . . H31 H -0.1420 0.2224 0.7111 0.031 Uiso 1 1 calc R . . C32 C 0.1859(4) -0.0141(3) 0.7573(2) 0.0327(11) Uani 1 1 d . . . C33 C -0.1581(4) 0.1630(3) 0.8228(2) 0.0439(14) Uani 1 1 d D . . C34 C -0.1413(3) 0.2238(3) 0.59396(18) 0.0263(10) Uani 1 1 d . . . C35 C -0.2100(3) 0.1729(3) 0.62446(19) 0.0268(10) Uani 1 1 d . . . H35 H -0.1878 0.1288 0.6557 0.032 Uiso 1 1 calc R . . C36 C -0.3099(3) 0.1846(3) 0.61051(19) 0.0295(11) Uani 1 1 d . . . C37 C -0.3453(4) 0.2472(3) 0.5655(2) 0.0375(12) Uani 1 1 d . . . H37 H -0.4133 0.2551 0.5561 0.045 Uiso 1 1 calc R . . C38 C -0.2794(4) 0.2983(3) 0.5343(2) 0.0381(12) Uani 1 1 d . . . C39 C -0.1798(4) 0.2865(3) 0.54811(19) 0.0319(11) Uani 1 1 d . . . H39 H -0.1361 0.3223 0.5256 0.038 Uiso 1 1 calc R . . C40 C -0.3761(4) 0.1251(3) 0.6443(2) 0.0387(12) Uani 1 1 d . . . C41 C -0.3175(5) 0.3639(4) 0.4841(2) 0.0559(16) Uani 1 1 d . . . C42 C 0.0246(3) 0.2892(3) 0.59392(17) 0.0255(10) Uani 1 1 d . . . C43 C -0.0375(4) 0.3685(3) 0.59876(18) 0.0320(11) Uani 1 1 d . . . H43 H -0.1108 0.3746 0.6091 0.038 Uiso 1 1 calc R . . C44 C 0.0040(4) 0.4395(3) 0.5890(2) 0.0379(12) Uani 1 1 d . . . C45 C 0.1103(4) 0.4334(3) 0.5745(2) 0.0414(13) Uani 1 1 d . . . H45 H 0.1389 0.4814 0.5677 0.050 Uiso 1 1 calc R . . C46 C 0.1743(4) 0.3552(3) 0.57010(19) 0.0338(11) Uani 1 1 d . B . C47 C 0.1320(4) 0.2858(3) 0.58004(18) 0.0299(11) Uani 1 1 d . . . H47 H 0.1782 0.2331 0.5773 0.036 Uiso 1 1 calc R . . C48 C -0.0662(5) 0.5220(3) 0.5953(2) 0.0511(15) Uani 1 1 d . . . C49 C 0.2898(5) 0.3468(3) 0.5544(3) 0.0495(15) Uani 1 1 d D . . C50 C 0.0458(3) 0.1443(3) 0.56042(18) 0.0261(10) Uani 1 1 d . . . C51 C 0.0845(3) 0.1789(3) 0.50381(19) 0.0301(11) Uani 1 1 d . . . H51 H 0.0752 0.2381 0.4922 0.036 Uiso 1 1 calc R . . C52 C 0.1363(4) 0.1296(3) 0.4640(2) 0.0384(12) Uani 1 1 d . C . C53 C 0.1523(4) 0.0431(3) 0.4795(2) 0.0394(13) Uani 1 1 d . . . H53 H 0.1900 0.0091 0.4530 0.047 Uiso 1 1 calc R . . C54 C 0.1120(3) 0.0071(3) 0.5347(2) 0.0325(11) Uani 1 1 d . . . C55 C 0.0591(3) 0.0570(3) 0.57361(19) 0.0279(10) Uani 1 1 d . . . H55 H 0.0306 0.0309 0.6108 0.033 Uiso 1 1 calc R . . C56 C 0.1785(5) 0.1702(5) 0.4049(2) 0.0619(18) Uani 1 1 d D . . C57 C 0.1334(4) -0.0863(3) 0.5538(3) 0.0469(14) Uani 1 1 d . . . B2 B 0.3135(4) 0.2432(3) 1.0531(2) 0.0216(11) Uani 1 1 d . . . F27 F 0.7306(3) 0.2711(2) 0.96620(16) 0.0706(10) Uani 1 1 d . . . F28 F 0.7051(2) 0.2161(2) 1.05453(14) 0.0601(9) Uani 1 1 d . . . F29 F 0.7948(2) 0.1424(2) 0.99453(17) 0.0684(11) Uani 1 1 d . . . F30 F 0.6203(2) 0.01610(17) 0.89190(12) 0.0438(7) Uani 1 1 d . . . F31 F 0.4573(2) 0.01848(16) 0.92019(11) 0.0388(7) Uani 1 1 d . . . F32 F 0.5034(2) 0.11718(17) 0.85302(11) 0.0459(7) Uani 1 1 d . . . F33 F 0.56151(19) 0.12284(16) 1.21199(11) 0.0388(7) Uani 1 1 d . . . F34 F 0.5486(2) 0.00005(18) 1.21044(14) 0.0551(9) Uani 1 1 d . . . F35 F 0.4833(2) 0.05201(19) 1.28545(12) 0.0503(8) Uani 1 1 d . . . F36 F 0.1174(2) 0.04353(19) 1.28542(14) 0.0611(9) Uani 1 1 d . . . F37 F 0.0439(2) 0.1072(2) 1.20999(13) 0.0552(8) Uani 1 1 d . . . F38 F 0.0573(2) 0.17674(19) 1.26925(12) 0.0499(8) Uani 1 1 d . . . F39 F 0.1456(2) 0.01689(17) 1.02289(17) 0.0681(11) Uani 1 1 d . . . F40 F -0.0060(3) 0.06377(18) 1.06749(12) 0.0553(8) Uani 1 1 d . . . F41 F 0.0189(2) 0.07942(17) 0.97579(12) 0.0435(7) Uani 1 1 d . . . F42 F -0.0879(2) 0.38342(19) 0.93264(13) 0.0552(9) Uani 1 1 d . . . F43 F -0.1034(2) 0.4135(2) 1.01439(14) 0.0664(10) Uani 1 1 d . . . F44 F 0.0093(3) 0.4548(2) 0.9461(2) 0.0982(16) Uani 1 1 d . . . F45 F 0.1426(3) 0.48605(19) 1.17532(13) 0.0555(8) Uani 1 1 d . . . F46 F 0.2492(2) 0.56885(17) 1.14938(13) 0.0511(8) Uani 1 1 d . . . F47 F 0.2975(3) 0.4436(2) 1.19792(14) 0.0765(12) Uani 1 1 d . . . F48 F 0.3244(2) 0.5299(2) 0.90168(13) 0.0592(9) Uani 1 1 d . . . F49 F 0.3766(4) 0.6055(2) 0.94478(15) 0.0924(14) Uani 1 1 d . . . F50 F 0.4776(2) 0.4961(2) 0.92089(14) 0.0596(9) Uani 1 1 d . . . C58 C 0.4227(3) 0.2036(2) 1.01435(17) 0.0205(9) Uani 1 1 d . . . C59 C 0.5172(3) 0.2190(2) 1.02082(17) 0.0209(9) Uani 1 1 d . . . H59 H 0.5155 0.2562 1.0448 0.025 Uiso 1 1 calc R . . C60 C 0.6130(3) 0.1819(3) 0.99357(18) 0.0239(10) Uani 1 1 d . . . C61 C 0.6184(3) 0.1294(3) 0.95654(18) 0.0241(10) Uani 1 1 d . . . H61 H 0.6839 0.1032 0.9382 0.029 Uiso 1 1 calc R . . C62 C 0.5259(3) 0.1162(2) 0.94706(17) 0.0224(10) Uani 1 1 d . . . C63 C 0.4299(3) 0.1523(2) 0.97597(17) 0.0223(10) Uani 1 1 d . . . H63 H 0.3677 0.1415 0.9693 0.027 Uiso 1 1 calc R . . C64 C 0.7103(3) 0.2001(3) 1.0030(2) 0.0344(12) Uani 1 1 d . . . C65 C 0.5274(3) 0.0670(3) 0.90376(19) 0.0296(11) Uani 1 1 d . . . C66 C 0.3093(3) 0.1868(2) 1.11959(18) 0.0201(9) Uani 1 1 d . . . C67 C 0.3990(3) 0.1523(2) 1.14693(18) 0.0238(10) Uani 1 1 d . . . H67 H 0.4646 0.1602 1.1258 0.029 Uiso 1 1 calc R . . C68 C 0.3959(3) 0.1073(3) 1.20344(18) 0.0243(10) Uani 1 1 d . . . C69 C 0.3023(3) 0.0930(3) 1.23600(19) 0.0268(10) Uani 1 1 d . . . H69 H 0.2999 0.0618 1.2747 0.032 Uiso 1 1 calc R . . C70 C 0.2124(3) 0.1257(3) 1.21011(19) 0.0260(10) Uani 1 1 d . . . C71 C 0.2157(3) 0.1720(3) 1.15395(18) 0.0240(10) Uani 1 1 d . . . H71 H 0.1521 0.1947 1.1380 0.029 Uiso 1 1 calc R . . C72 C 0.4962(3) 0.0705(3) 1.22788(19) 0.0305(11) Uani 1 1 d . . . C73 C 0.1088(4) 0.1124(3) 1.2438(2) 0.0361(12) Uani 1 1 d . . . C74 C 0.2091(3) 0.2425(2) 1.02770(17) 0.0199(9) Uani 1 1 d . . . C75 C 0.1820(3) 0.1663(3) 1.03142(18) 0.0254(10) Uani 1 1 d . . . H75 H 0.2282 0.1153 1.0460 0.030 Uiso 1 1 calc R . . C76 C 0.0903(3) 0.1627(3) 1.01465(19) 0.0274(10) Uani 1 1 d . . . C77 C 0.0200(3) 0.2356(3) 0.99410(19) 0.0290(11) Uani 1 1 d . . . H77 H -0.0435 0.2334 0.9832 0.035 Uiso 1 1 calc R . . C78 C 0.0445(3) 0.3115(3) 0.98980(18) 0.0227(10) Uani 1 1 d . . . C79 C 0.1378(3) 0.3147(3) 1.00568(18) 0.0225(10) Uani 1 1 d . . . H79 H 0.1532 0.3678 1.0013 0.027 Uiso 1 1 calc R . . C80 C 0.0629(4) 0.0809(3) 1.0206(2) 0.0370(12) Uani 1 1 d . . . C81 C -0.0329(4) 0.3910(3) 0.9709(2) 0.0358(12) Uani 1 1 d . . . C82 C 0.3149(3) 0.3393(3) 1.05328(19) 0.0227(10) Uani 1 1 d . . . C83 C 0.2832(3) 0.3740(3) 1.1022(2) 0.0264(10) Uani 1 1 d . . . H83 H 0.2620 0.3397 1.1380 0.032 Uiso 1 1 calc R . . C84 C 0.2814(3) 0.4577(3) 1.1006(2) 0.0290(11) Uani 1 1 d . . . C85 C 0.3127(3) 0.5091(3) 1.0493(2) 0.0321(11) Uani 1 1 d . . . H85 H 0.3120 0.5659 1.0480 0.039 Uiso 1 1 calc R . . C86 C 0.3449(3) 0.4765(3) 1.0002(2) 0.0273(10) Uani 1 1 d . . . C87 C 0.3451(3) 0.3937(3) 1.00231(19) 0.0259(10) Uani 1 1 d . . . H87 H 0.3666 0.3730 0.9677 0.031 Uiso 1 1 calc R . . C88 C 0.2438(5) 0.4887(3) 1.1551(2) 0.0443(14) Uani 1 1 d . . . C89 C 0.3796(4) 0.5290(3) 0.9430(2) 0.0423(13) Uani 1 1 d . . . O1 O 0.5063(8) 0.0161(6) 0.4834(4) 0.064(3) Uiso 0.50 1 d P D -1 C90 C 0.5662(17) -0.0585(15) 0.4691(9) 0.106(6) Uiso 0.50 1 d P D -1 H90A H 0.5191 -0.0938 0.4672 0.127 Uiso 0.50 1 calc PR D -1 H90B H 0.6095 -0.0892 0.4999 0.127 Uiso 0.50 1 calc PR D -1 C91 C 0.6331(10) -0.0458(8) 0.4151(6) 0.062(3) Uiso 0.50 1 d P D -1 H91A H 0.6733 -0.1002 0.4071 0.093 Uiso 0.50 1 calc PR D -1 H91B H 0.6811 -0.0120 0.4170 0.093 Uiso 0.50 1 calc PR D -1 H91C H 0.5906 -0.0164 0.3842 0.093 Uiso 0.50 1 calc PR D -1 C92 C 0.4466(17) 0.0053(15) 0.5390(9) 0.119(8) Uiso 0.50 1 d P D -1 H92A H 0.4939 -0.0171 0.5687 0.143 Uiso 0.50 1 calc PR D -1 H92B H 0.4035 -0.0356 0.5425 0.143 Uiso 0.50 1 calc PR D -1 C93 C 0.3786(16) 0.0860(11) 0.5481(9) 0.106(6) Uiso 0.50 1 d P D -1 H93A H 0.3384 0.0784 0.5868 0.159 Uiso 0.50 1 calc PR D -1 H93B H 0.3305 0.1071 0.5192 0.159 Uiso 0.50 1 calc PR D -1 H93C H 0.4215 0.1264 0.5443 0.159 Uiso 0.50 1 calc PR D -1 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ni1 0.0205(3) 0.0211(3) 0.0399(4) -0.0078(3) -0.0061(3) -0.0012(2) P1 0.0253(7) 0.0300(7) 0.0456(8) -0.0150(6) -0.0112(6) 0.0049(5) P2 0.0206(6) 0.0213(6) 0.0308(7) -0.0046(5) -0.0055(5) -0.0009(5) P3 0.0258(6) 0.0278(7) 0.0317(7) -0.0097(5) -0.0044(5) -0.0065(5) F1 0.0341(15) 0.0404(16) 0.0326(16) -0.0127(13) -0.0022(12) -0.0081(12) F2 0.0452(17) 0.0387(16) 0.0358(16) -0.0001(13) -0.0126(13) -0.0143(13) N1 0.033(2) 0.022(2) 0.048(3) -0.0048(19) -0.0112(19) -0.0033(18) C1 0.024(3) 0.037(3) 0.060(4) -0.017(3) -0.003(2) 0.001(2) C2 0.029(3) 0.044(3) 0.069(4) -0.023(3) -0.003(3) 0.001(2) C3 0.040(3) 0.073(4) 0.057(4) -0.030(3) -0.015(3) 0.020(3) C4 0.065(5) 0.142(8) 0.064(5) -0.015(5) -0.021(4) -0.001(5) C5 0.042(3) 0.024(3) 0.043(3) -0.007(2) -0.013(2) 0.008(2) C6 0.064(4) 0.024(3) 0.059(4) -0.010(3) -0.019(3) -0.006(2) C7 0.024(2) 0.032(3) 0.041(3) -0.007(2) -0.006(2) -0.007(2) C8 0.021(3) 0.046(3) 0.060(4) -0.008(3) -0.003(2) -0.001(2) C9 0.026(2) 0.023(2) 0.039(3) -0.004(2) -0.005(2) 0.0003(19) C10 0.041(3) 0.046(3) 0.034(3) 0.002(2) -0.010(2) -0.010(2) C11 0.032(3) 0.033(3) 0.035(3) -0.007(2) -0.007(2) -0.003(2) C12 0.101(5) 0.051(4) 0.035(3) -0.004(3) -0.020(3) -0.012(3) C13 0.024(2) 0.030(3) 0.037(3) -0.012(2) -0.003(2) 0.002(2) C14 0.026(3) 0.030(3) 0.032(3) -0.007(2) -0.008(2) 0.000(2) C15 0.057(3) 0.031(3) 0.028(3) -0.011(2) -0.001(2) -0.015(2) C16 0.054(4) 0.036(3) 0.059(4) -0.018(3) 0.020(3) -0.008(3) C17 0.031(3) 0.033(3) 0.032(3) -0.005(2) -0.009(2) -0.007(2) C18 0.046(3) 0.043(3) 0.041(3) -0.001(3) -0.009(3) -0.012(3) C19 0.024(3) 0.043(3) 0.045(3) -0.014(2) -0.004(2) -0.008(2) C20 0.039(3) 0.047(3) 0.056(4) -0.010(3) -0.019(3) -0.002(2) C21 0.026(3) 0.023(3) 0.048(3) -0.009(2) -0.016(2) 0.004(2) C22 0.038(3) 0.030(3) 0.047(3) -0.001(2) -0.009(2) -0.014(2) C23 0.056(4) 0.036(3) 0.107(5) 0.013(3) -0.039(4) -0.017(3) C24 0.041(3) 0.038(3) 0.052(3) -0.006(3) -0.007(3) -0.017(2) C25 0.080(5) 0.076(4) 0.047(4) -0.005(3) -0.002(3) -0.051(4) B1 0.034(3) 0.019(3) 0.023(3) -0.005(2) -0.004(2) -0.007(2) F3 0.0253(16) 0.050(2) 0.109(3) 0.0179(19) -0.0221(17) -0.0066(14) F4 0.072(2) 0.076(2) 0.041(2) -0.0019(17) -0.0257(17) 0.0325(18) F5 0.0432(18) 0.0336(17) 0.085(2) -0.0195(16) -0.0203(16) 0.0082(13) F6 0.073(4) 0.194(7) 0.027(3) 0.032(3) 0.018(2) 0.066(4) F7 0.028(2) 0.106(4) 0.067(3) -0.038(3) 0.0148(19) -0.022(2) F8 0.052(3) 0.090(4) 0.088(3) -0.058(3) 0.034(2) -0.025(2) F9 0.0476(18) 0.0377(18) 0.063(2) -0.0042(15) 0.0018(15) -0.0145(14) F10 0.060(2) 0.085(2) 0.0380(19) -0.0099(17) 0.0065(15) -0.0360(18) F11 0.0259(16) 0.074(2) 0.078(2) 0.0049(18) -0.0149(16) -0.0113(15) F12 0.119(4) 0.138(4) 0.079(3) 0.042(3) 0.002(3) 0.086(3) F13 0.113(3) 0.089(3) 0.062(2) 0.022(2) -0.052(2) -0.058(2) F14 0.114(3) 0.053(2) 0.072(2) 0.0308(18) -0.060(2) -0.044(2) F15 0.185(4) 0.041(2) 0.044(2) -0.0181(17) -0.014(2) 0.016(2) F16 0.084(3) 0.0306(19) 0.126(3) -0.021(2) -0.012(2) 0.0028(18) F17 0.112(3) 0.0243(17) 0.072(2) 0.0020(16) 0.002(2) -0.0163(18) F18 0.059(3) 0.063(4) 0.146(6) 0.033(4) 0.000(3) -0.031(3) F19 0.042(3) 0.195(8) 0.045(3) -0.027(4) -0.016(2) -0.006(3) F20 0.060(3) 0.145(6) 0.129(5) -0.092(5) 0.038(3) -0.061(3) F21 0.093(4) 0.069(3) 0.040(3) 0.008(2) 0.010(2) -0.028(3) F22 0.117(5) 0.202(8) 0.036(3) -0.012(3) 0.013(3) -0.123(6) F23 0.206(11) 0.092(5) 0.030(3) -0.022(3) 0.055(5) -0.004(5) F24 0.091(3) 0.046(2) 0.082(2) -0.0384(19) -0.026(2) -0.0042(18) F25 0.086(3) 0.044(2) 0.193(5) -0.023(2) -0.101(3) 0.0102(19) F26 0.099(3) 0.0305(18) 0.083(3) -0.0128(17) -0.001(2) -0.0107(18) C26 0.027(2) 0.017(2) 0.025(2) -0.0042(18) -0.006(2) -0.0063(18) C27 0.022(2) 0.019(2) 0.030(3) -0.008(2) -0.0016(19) -0.0049(18) C28 0.026(2) 0.023(2) 0.030(3) -0.001(2) -0.011(2) -0.0097(19) C29 0.030(3) 0.034(3) 0.025(3) 0.001(2) -0.005(2) -0.012(2) C30 0.024(2) 0.031(3) 0.025(3) -0.004(2) 0.000(2) -0.003(2) C31 0.024(2) 0.026(2) 0.026(3) -0.004(2) -0.006(2) -0.0011(19) C32 0.030(3) 0.029(3) 0.036(3) -0.003(2) -0.007(2) -0.004(2) C33 0.038(3) 0.051(4) 0.031(3) 0.002(3) -0.002(2) -0.001(3) C34 0.032(3) 0.022(2) 0.022(2) -0.006(2) -0.004(2) -0.0003(19) C35 0.029(3) 0.020(2) 0.026(3) -0.0004(19) -0.008(2) 0.0015(19) C36 0.025(2) 0.030(3) 0.030(3) -0.006(2) -0.006(2) 0.002(2) C37 0.031(3) 0.039(3) 0.041(3) -0.011(2) -0.013(2) 0.002(2) C38 0.043(3) 0.033(3) 0.033(3) -0.004(2) -0.014(2) 0.002(2) C39 0.039(3) 0.022(2) 0.031(3) -0.002(2) -0.005(2) -0.004(2) C40 0.022(3) 0.044(3) 0.044(3) -0.003(3) -0.005(2) -0.003(2) C41 0.059(4) 0.058(4) 0.044(4) 0.004(3) -0.019(3) -0.006(3) C42 0.034(3) 0.028(3) 0.014(2) -0.0014(19) -0.0034(19) -0.008(2) C43 0.048(3) 0.028(3) 0.020(2) -0.003(2) -0.005(2) -0.010(2) C44 0.067(4) 0.022(3) 0.025(3) -0.003(2) -0.005(2) -0.011(2) C45 0.065(4) 0.037(3) 0.031(3) -0.001(2) -0.010(3) -0.029(3) C46 0.048(3) 0.034(3) 0.026(3) -0.002(2) -0.012(2) -0.020(2) C47 0.039(3) 0.027(3) 0.027(3) -0.004(2) -0.009(2) -0.011(2) C48 0.077(5) 0.033(3) 0.042(3) -0.006(3) -0.007(3) -0.014(3) C49 0.061(4) 0.043(3) 0.056(4) -0.005(3) -0.014(3) -0.031(3) C50 0.025(2) 0.033(3) 0.025(3) -0.008(2) -0.005(2) -0.012(2) C51 0.033(3) 0.035(3) 0.026(3) -0.007(2) -0.006(2) -0.012(2) C52 0.038(3) 0.056(4) 0.027(3) -0.018(3) 0.003(2) -0.018(3) C53 0.033(3) 0.052(4) 0.040(3) -0.028(3) -0.003(2) -0.006(2) C54 0.026(3) 0.035(3) 0.042(3) -0.019(2) -0.012(2) -0.001(2) C55 0.026(2) 0.030(3) 0.031(3) -0.010(2) -0.007(2) -0.006(2) C56 0.064(4) 0.101(6) 0.034(3) -0.023(4) 0.010(3) -0.043(4) C57 0.046(3) 0.039(3) 0.063(4) -0.027(3) -0.019(3) 0.001(3) B2 0.019(3) 0.020(3) 0.025(3) -0.005(2) -0.004(2) -0.002(2) F27 0.058(2) 0.061(2) 0.100(3) 0.000(2) -0.0136(19) -0.0398(18) F28 0.0295(16) 0.102(3) 0.066(2) -0.047(2) -0.0047(15) -0.0185(16) F29 0.0200(15) 0.070(2) 0.134(3) -0.067(2) -0.0134(17) 0.0028(15) F30 0.0338(16) 0.0425(17) 0.0597(19) -0.0328(15) -0.0007(14) 0.0002(13) F31 0.0424(16) 0.0398(16) 0.0435(17) -0.0192(13) 0.0005(13) -0.0201(13) F32 0.076(2) 0.0389(17) 0.0251(15) -0.0068(13) -0.0138(14) -0.0120(15) F33 0.0255(14) 0.0440(17) 0.0476(17) 0.0010(13) -0.0146(13) -0.0120(12) F34 0.0466(18) 0.0402(18) 0.085(2) -0.0302(17) -0.0397(17) 0.0183(14) F35 0.0404(17) 0.076(2) 0.0321(17) 0.0099(15) -0.0158(13) -0.0211(15) F36 0.0328(17) 0.058(2) 0.065(2) 0.0249(17) 0.0059(15) -0.0083(14) F37 0.0378(17) 0.087(2) 0.0489(19) -0.0129(17) 0.0016(15) -0.0345(16) F38 0.0319(16) 0.060(2) 0.0478(18) -0.0164(15) 0.0085(14) 0.0016(14) F39 0.0437(18) 0.0262(16) 0.145(3) -0.0185(19) -0.043(2) -0.0026(14) F40 0.082(2) 0.0495(19) 0.0429(18) -0.0024(15) 0.0009(17) -0.0432(17) F41 0.0499(18) 0.0442(17) 0.0473(18) -0.0095(14) -0.0119(14) -0.0257(14) F42 0.0504(19) 0.059(2) 0.0534(19) -0.0199(16) -0.0354(16) 0.0215(15) F43 0.057(2) 0.071(2) 0.059(2) -0.0317(18) -0.0230(17) 0.0354(17) F44 0.051(2) 0.041(2) 0.184(4) 0.044(2) -0.056(2) -0.0140(17) F45 0.068(2) 0.054(2) 0.0509(19) -0.0268(16) 0.0043(17) -0.0190(16) F46 0.069(2) 0.0293(16) 0.066(2) -0.0242(15) -0.0193(17) -0.0098(14) F47 0.125(3) 0.049(2) 0.065(2) -0.0282(18) -0.065(2) 0.018(2) F48 0.052(2) 0.067(2) 0.052(2) 0.0175(16) -0.0197(16) -0.0225(16) F49 0.169(4) 0.0313(19) 0.072(3) -0.0073(17) 0.022(3) -0.046(2) F50 0.0382(18) 0.063(2) 0.065(2) 0.0067(17) -0.0016(16) -0.0131(15) C58 0.022(2) 0.013(2) 0.024(2) 0.0034(18) -0.0081(18) -0.0024(17) C59 0.020(2) 0.018(2) 0.024(2) -0.0043(18) -0.0048(18) -0.0002(17) C60 0.018(2) 0.025(2) 0.026(2) -0.003(2) -0.0022(19) -0.0053(18) C61 0.019(2) 0.025(2) 0.024(2) -0.003(2) 0.0010(19) -0.0029(18) C62 0.025(2) 0.019(2) 0.022(2) -0.0018(18) -0.0037(19) -0.0047(18) C63 0.019(2) 0.021(2) 0.027(2) -0.0017(19) -0.0075(19) -0.0044(18) C64 0.020(3) 0.041(3) 0.045(3) -0.023(3) 0.004(2) -0.005(2) C65 0.032(3) 0.028(3) 0.029(3) -0.008(2) 0.001(2) -0.008(2) C66 0.018(2) 0.014(2) 0.029(2) -0.0091(18) -0.0048(19) -0.0009(17) C67 0.021(2) 0.022(2) 0.029(3) -0.009(2) -0.0007(19) -0.0041(18) C68 0.026(2) 0.021(2) 0.027(3) -0.008(2) -0.008(2) -0.0009(18) C69 0.029(3) 0.024(2) 0.025(2) -0.002(2) -0.004(2) -0.0052(19) C70 0.020(2) 0.023(2) 0.034(3) -0.009(2) 0.002(2) -0.0043(18) C71 0.015(2) 0.023(2) 0.031(3) -0.006(2) -0.0039(19) 0.0010(18) C72 0.029(3) 0.037(3) 0.028(3) -0.004(2) -0.008(2) -0.012(2) C73 0.029(3) 0.039(3) 0.033(3) 0.001(2) -0.005(2) -0.005(2) C74 0.014(2) 0.022(2) 0.023(2) -0.0073(18) 0.0022(18) -0.0047(17) C75 0.018(2) 0.025(2) 0.033(3) -0.008(2) -0.0041(19) -0.0021(18) C76 0.024(2) 0.026(3) 0.035(3) -0.006(2) -0.006(2) -0.0074(19) C77 0.018(2) 0.034(3) 0.036(3) -0.008(2) -0.005(2) -0.006(2) C78 0.017(2) 0.023(2) 0.026(2) -0.0029(19) -0.0070(19) -0.0003(18) C79 0.019(2) 0.019(2) 0.029(2) -0.0056(19) -0.0032(19) -0.0039(18) C80 0.030(3) 0.034(3) 0.050(3) -0.004(2) -0.013(3) -0.011(2) C81 0.030(3) 0.034(3) 0.044(3) -0.001(2) -0.017(2) -0.007(2) C82 0.011(2) 0.025(2) 0.032(3) -0.008(2) -0.0089(18) 0.0023(17) C83 0.019(2) 0.024(2) 0.038(3) -0.004(2) -0.012(2) -0.0032(18) C84 0.026(2) 0.026(3) 0.040(3) -0.009(2) -0.018(2) -0.0012(19) C85 0.029(3) 0.019(2) 0.053(3) -0.007(2) -0.022(2) -0.0009(19) C86 0.016(2) 0.021(2) 0.044(3) 0.000(2) -0.012(2) -0.0035(18) C87 0.018(2) 0.024(2) 0.035(3) -0.005(2) -0.006(2) -0.0020(18) C88 0.066(4) 0.028(3) 0.047(3) -0.012(2) -0.030(3) -0.004(3) C89 0.037(3) 0.032(3) 0.059(4) 0.003(3) -0.015(3) -0.015(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 C21 1.839(5) . ? Ni1 C13 1.893(5) . ? Ni1 P1 2.2307(13) . ? Ni1 P2 2.2333(12) . ? P1 C1 1.815(5) . ? P1 C5 1.823(5) . ? P1 C3 1.824(6) . ? P2 C11 1.818(5) . ? P2 C7 1.822(4) . ? P2 C9 1.826(4) . ? P3 C15 1.790(4) . ? P3 C14 1.794(5) . ? P3 C19 1.798(4) . ? P3 C17 1.801(5) . ? F1 C13 1.394(5) . ? F2 C14 1.380(5) . ? N1 C21 1.156(6) . ? N1 C22 1.482(6) . ? C1 C2 1.540(6) . ? C3 C4 1.444(8) . ? C5 C6 1.529(7) . ? C7 C8 1.529(6) . ? C9 C10 1.525(6) . ? C11 C12 1.522(7) . ? C13 C14 1.309(6) . ? C15 C16 1.531(7) . ? C17 C18 1.535(6) . ? C19 C20 1.529(7) . ? C22 C24 1.515(7) . ? C22 C25 1.516(7) . ? C22 C23 1.525(7) . ? B1 C26 1.637(6) . ? B1 C34 1.638(7) . ? B1 C50 1.640(6) . ? B1 C42 1.642(6) . ? F3 C32 1.330(5) . ? F4 C32 1.320(5) . ? F5 C32 1.329(5) . ? F6 C33 1.288(6) . ? F7 C33 1.327(6) . ? F8 C33 1.361(7) . ? F6# C33 1.330(9) . ? F7# C33 1.301(10) . ? F8# C33 1.322(10) . ? F9 C40 1.333(5) . ? F10 C40 1.328(6) . ? F11 C40 1.343(5) . ? F12 C41 1.299(7) . ? F13 C41 1.362(7) . ? F14 C41 1.314(7) . ? F15 C48 1.329(6) . ? F16 C48 1.344(7) . ? F17 C48 1.325(6) . ? F18 C49 1.328(7) . ? F19 C49 1.289(7) . ? F20 C49 1.363(7) . ? F18# C49 1.357(8) . ? F19# C49 1.299(9) . ? F20# C49 1.271(9) . ? F21 C56 1.412(8) . ? F22 C56 1.342(8) . ? F23 C56 1.233(8) . ? F21# C56 1.273(10) . ? F22# C56 1.397(8) . ? F23# C56 1.348(10) . ? F24 C57 1.335(6) . ? F25 C57 1.309(6) . ? F26 C57 1.340(6) . ? C26 C27 1.402(6) . ? C26 C31 1.404(6) . ? C27 C28 1.388(6) . ? C28 C29 1.385(6) . ? C28 C32 1.492(6) . ? C29 C30 1.390(6) . ? C30 C31 1.380(6) . ? C30 C33 1.501(6) . ? C34 C35 1.401(6) . ? C34 C39 1.402(6) . ? C35 C36 1.397(6) . ? C36 C37 1.375(6) . ? C36 C40 1.496(7) . ? C37 C38 1.381(7) . ? C38 C39 1.391(7) . ? C38 C41 1.494(7) . ? C42 C43 1.399(6) . ? C42 C47 1.401(6) . ? C43 C44 1.400(6) . ? C44 C45 1.380(7) . ? C44 C48 1.487(7) . ? C45 C46 1.389(7) . ? C46 C47 1.383(6) . ? C46 C49 1.496(7) . ? C50 C55 1.401(6) . ? C50 C51 1.401(6) . ? C51 C52 1.392(6) . ? C52 C53 1.384(7) . ? C52 C56 1.493(7) . ? C53 C54 1.387(7) . ? C54 C55 1.385(6) . ? C54 C57 1.494(7) . ? B2 C82 1.631(6) . ? B2 C74 1.640(6) . ? B2 C66 1.649(6) . ? B2 C58 1.649(6) . ? F27 C64 1.359(6) . ? F28 C64 1.324(5) . ? F29 C64 1.305(5) . ? F30 C65 1.338(5) . ? F31 C65 1.345(5) . ? F32 C65 1.349(5) . ? F33 C72 1.342(5) . ? F34 C72 1.335(5) . ? F35 C72 1.335(5) . ? F36 C73 1.330(5) . ? F37 C73 1.339(5) . ? F38 C73 1.345(5) . ? F39 C80 1.328(5) . ? F40 C80 1.336(6) . ? F41 C80 1.341(5) . ? F42 C81 1.340(5) . ? F43 C81 1.327(6) . ? F44 C81 1.307(5) . ? F45 C88 1.356(6) . ? F46 C88 1.347(5) . ? F47 C88 1.334(6) . ? F48 C89 1.351(6) . ? F49 C89 1.295(6) . ? F50 C89 1.344(6) . ? C58 C63 1.396(6) . ? C58 C59 1.404(6) . ? C59 C60 1.387(6) . ? C60 C61 1.391(6) . ? C60 C64 1.488(6) . ? C61 C62 1.387(6) . ? C62 C63 1.400(6) . ? C62 C65 1.487(6) . ? C66 C67 1.404(6) . ? C66 C71 1.406(6) . ? C67 C68 1.386(6) . ? C68 C69 1.388(6) . ? C68 C72 1.493(6) . ? C69 C70 1.386(6) . ? C70 C71 1.386(6) . ? C70 C73 1.506(6) . ? C74 C79 1.395(6) . ? C74 C75 1.405(6) . ? C75 C76 1.389(6) . ? C76 C77 1.385(6) . ? C76 C80 1.488(6) . ? C77 C78 1.382(6) . ? C78 C79 1.396(6) . ? C78 C81 1.494(6) . ? C82 C83 1.395(6) . ? C82 C87 1.399(6) . ? C83 C84 1.398(6) . ? C84 C85 1.383(6) . ? C84 C88 1.488(7) . ? C85 C86 1.380(6) . ? C86 C87 1.386(6) . ? C86 C89 1.504(7) . ? O1 C90 1.39(3) . ? O1 C92 1.42(2) . ? C90 C91 1.43(2) . ? C92 C93 1.47(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 C21 Ni1 C13 176.8(2) . . ? C21 Ni1 P1 91.47(14) . . ? C13 Ni1 P1 89.48(13) . . ? C21 Ni1 P2 90.98(14) . . ? C13 Ni1 P2 87.95(13) . . ? P1 Ni1 P2 176.64(5) . . ? C1 P1 C5 105.6(2) . . ? C1 P1 C3 103.1(3) . . ? C5 P1 C3 106.2(3) . . ? C1 P1 Ni1 114.87(16) . . ? C5 P1 Ni1 115.44(17) . . ? C3 P1 Ni1 110.64(17) . . ? C11 P2 C7 105.1(2) . . ? C11 P2 C9 105.3(2) . . ? C7 P2 C9 104.8(2) . . ? C11 P2 Ni1 109.62(15) . . ? C7 P2 Ni1 114.43(15) . . ? C9 P2 Ni1 116.67(15) . . ? C15 P3 C14 106.5(2) . . ? C15 P3 C19 108.7(2) . . ? C14 P3 C19 109.6(2) . . ? C15 P3 C17 110.3(2) . . ? C14 P3 C17 112.0(2) . . ? C19 P3 C17 109.6(2) . . ? C21 N1 C22 178.5(5) . . ? C2 C1 P1 114.8(4) . . ? C4 C3 P1 113.2(5) . . ? C6 C5 P1 113.6(3) . . ? C8 C7 P2 115.0(3) . . ? C10 C9 P2 113.4(3) . . ? C12 C11 P2 112.4(3) . . ? C14 C13 F1 113.0(4) . . ? C14 C13 Ni1 130.9(4) . . ? F1 C13 Ni1 116.0(3) . . ? C13 C14 F2 116.3(4) . . ? C13 C14 P3 131.6(4) . . ? F2 C14 P3 112.1(3) . . ? C16 C15 P3 113.8(4) . . ? C18 C17 P3 112.0(3) . . ? C20 C19 P3 113.0(3) . . ? N1 C21 Ni1 178.2(5) . . ? N1 C22 C24 106.7(4) . . ? N1 C22 C25 106.8(4) . . ? C24 C22 C25 112.5(4) . . ? N1 C22 C23 106.6(4) . . ? C24 C22 C23 111.3(4) . . ? C25 C22 C23 112.5(5) . . ? C26 B1 C34 111.9(4) . . ? C26 B1 C50 112.0(4) . . ? C34 B1 C50 104.5(3) . . ? C26 B1 C42 105.4(3) . . ? C34 B1 C42 112.8(4) . . ? C50 B1 C42 110.4(4) . . ? C27 C26 C31 114.7(4) . . ? C27 C26 B1 123.2(4) . . ? C31 C26 B1 122.1(4) . . ? C28 C27 C26 123.2(4) . . ? C29 C28 C27 120.6(4) . . ? C29 C28 C32 120.7(4) . . ? C27 C28 C32 118.8(4) . . ? C28 C29 C30 117.5(4) . . ? C31 C30 C29 121.4(4) . . ? C31 C30 C33 119.6(4) . . ? C29 C30 C33 119.0(4) . . ? C30 C31 C26 122.5(4) . . ? F4 C32 F5 106.1(4) . . ? F4 C32 F3 107.2(4) . . ? F5 C32 F3 104.7(4) . . ? F4 C32 C28 114.0(4) . . ? F5 C32 C28 112.2(4) . . ? F3 C32 C28 112.0(4) . . ? F6 C33 F7# 126.3(14) . . ? F6 C33 F8# 40.1(8) . . ? F7# C33 F8# 108.9(18) . . ? F6 C33 F7 108.1(5) . . ? F7# C33 F7 63.4(15) . . ? F8# C33 F7 137.8(11) . . ? F6 C33 F6# 60.4(10) . . ? F7# C33 F6# 117.0(18) . . ? F8# C33 F6# 100.5(13) . . ? F7 C33 F6# 57.6(10) . . ? F6 C33 F8 106.3(6) . . ? F7# C33 F8 38.7(14) . . ? F8# C33 F8 74.3(10) . . ? F7 C33 F8 100.6(4) . . ? F6# C33 F8 141.8(9) . . ? F6 C33 C30 115.3(4) . . ? F7# C33 C30 116.0(13) . . ? F8# C33 C30 106.9(11) . . ? F7 C33 C30 113.5(4) . . ? F6# C33 C30 106.0(9) . . ? F8 C33 C30 111.8(4) . . ? C35 C34 C39 115.1(4) . . ? C35 C34 B1 122.2(4) . . ? C39 C34 B1 122.2(4) . . ? C36 C35 C34 122.2(4) . . ? C37 C36 C35 121.0(4) . . ? C37 C36 C40 120.7(4) . . ? C35 C36 C40 118.3(4) . . ? C36 C37 C38 118.3(4) . . ? C37 C38 C39 120.7(4) . . ? C37 C38 C41 117.6(5) . . ? C39 C38 C41 121.7(5) . . ? C38 C39 C34 122.7(4) . . ? F10 C40 F9 106.4(4) . . ? F10 C40 F11 106.7(4) . . ? F9 C40 F11 105.9(4) . . ? F10 C40 C36 112.9(4) . . ? F9 C40 C36 112.2(4) . . ? F11 C40 C36 112.3(4) . . ? F12 C41 F14 108.7(6) . . ? F12 C41 F13 104.1(5) . . ? F14 C41 F13 104.0(5) . . ? F12 C41 C38 113.3(5) . . ? F14 C41 C38 114.3(5) . . ? F13 C41 C38 111.7(5) . . ? C43 C42 C47 114.6(4) . . ? C43 C42 B1 124.6(4) . . ? C47 C42 B1 120.7(4) . . ? C42 C43 C44 122.8(5) . . ? C45 C44 C43 120.5(5) . . ? C45 C44 C48 119.3(5) . . ? C43 C44 C48 120.1(5) . . ? C44 C45 C46 118.2(4) . . ? C47 C46 C45 120.5(5) . . ? C47 C46 C49 120.2(4) . . ? C45 C46 C49 119.3(4) . . ? C46 C47 C42 123.4(4) . . ? F17 C48 F15 107.2(5) . . ? F17 C48 F16 104.5(5) . . ? F15 C48 F16 103.9(5) . . ? F17 C48 C44 113.9(5) . . ? F15 C48 C44 113.4(5) . . ? F16 C48 C44 113.0(5) . . ? F20# C49 F19 133.4(10) . . ? F20# C49 F19# 112.0(15) . . ? F19 C49 F19# 50.0(11) . . ? F20# C49 F18 45.7(9) . . ? F19 C49 F18 109.6(6) . . ? F19# C49 F18 132.8(10) . . ? F20# C49 F18# 108.4(12) . . ? F19 C49 F18# 59.4(7) . . ? F19# C49 F18# 108.7(14) . . ? F18 C49 F18# 63.2(7) . . ? F20# C49 F20 59.0(10) . . ? F19 C49 F20 101.8(6) . . ? F19# C49 F20 56.7(11) . . ? F18 C49 F20 99.9(6) . . ? F18# C49 F20 142.6(8) . . ? F20# C49 C46 110.9(9) . . ? F19 C49 C46 115.7(5) . . ? F19# C49 C46 112.0(10) . . ? F18 C49 C46 115.0(5) . . ? F18# C49 C46 104.5(7) . . ? F20 C49 C46 112.9(4) . . ? C55 C50 C51 115.5(4) . . ? C55 C50 B1 122.8(4) . . ? C51 C50 B1 121.4(4) . . ? C52 C51 C50 122.3(4) . . ? C53 C52 C51 120.5(4) . . ? C53 C52 C56 119.8(5) . . ? C51 C52 C56 119.6(5) . . ? C52 C53 C54 118.6(4) . . ? C55 C54 C53 120.4(4) . . ? C55 C54 C57 119.7(5) . . ? C53 C54 C57 119.7(4) . . ? C54 C55 C50 122.7(4) . . ? F23 C56 F21# 119.1(12) . . ? F23 C56 F22 112.6(7) . . ? F21# C56 F22 44.5(11) . . ? F23 C56 F23# 26.3(11) . . ? F21# C56 F23# 128.5(17) . . ? F22 C56 F23# 138.2(11) . . ? F23 C56 F22# 67.6(8) . . ? F21# C56 F22# 102.9(14) . . ? F22 C56 F22# 61.8(7) . . ? F23# C56 F22# 90.4(12) . . ? F23 C56 F21 101.8(7) . . ? F21# C56 F21 50.6(13) . . ? F22 C56 F21 95.0(6) . . ? F23# C56 F21 91.0(12) . . ? F22# C56 F21 144.1(8) . . ? F23 C56 C52 120.1(7) . . ? F21# C56 C52 120.5(11) . . ? F22 C56 C52 113.3(5) . . ? F23# C56 C52 103.0(12) . . ? F22# C56 C52 104.5(8) . . ? F21 C56 C52 110.2(5) . . ? F25 C57 F24 107.0(4) . . ? F25 C57 F26 106.4(5) . . ? F24 C57 F26 104.1(4) . . ? F25 C57 C54 112.7(4) . . ? F24 C57 C54 112.8(5) . . ? F26 C57 C54 113.1(4) . . ? C82 B2 C74 109.7(3) . . ? C82 B2 C66 109.8(3) . . ? C74 B2 C66 108.1(3) . . ? C82 B2 C58 107.9(3) . . ? C74 B2 C58 112.4(3) . . ? C66 B2 C58 108.9(3) . . ? C63 C58 C59 115.9(4) . . ? C63 C58 B2 124.8(4) . . ? C59 C58 B2 119.3(4) . . ? C60 C59 C58 122.5(4) . . ? C59 C60 C61 120.5(4) . . ? C59 C60 C64 119.6(4) . . ? C61 C60 C64 119.9(4) . . ? C62 C61 C60 118.4(4) . . ? C61 C62 C63 120.6(4) . . ? C61 C62 C65 120.1(4) . . ? C63 C62 C65 119.3(4) . . ? C58 C63 C62 122.1(4) . . ? F29 C64 F28 108.1(4) . . ? F29 C64 F27 104.6(4) . . ? F28 C64 F27 103.3(4) . . ? F29 C64 C60 114.7(4) . . ? F28 C64 C60 113.7(4) . . ? F27 C64 C60 111.4(4) . . ? F30 C65 F31 106.5(3) . . ? F30 C65 F32 106.3(3) . . ? F31 C65 F32 105.4(4) . . ? F30 C65 C62 113.4(4) . . ? F31 C65 C62 112.9(3) . . ? F32 C65 C62 111.8(4) . . ? C67 C66 C71 114.8(4) . . ? C67 C66 B2 122.3(4) . . ? C71 C66 B2 122.8(4) . . ? C68 C67 C66 122.9(4) . . ? C67 C68 C69 120.9(4) . . ? C67 C68 C72 118.8(4) . . ? C69 C68 C72 120.3(4) . . ? C70 C69 C68 117.7(4) . . ? C71 C70 C69 121.2(4) . . ? C71 C70 C73 119.1(4) . . ? C69 C70 C73 119.7(4) . . ? C70 C71 C66 122.5(4) . . ? F35 C72 F34 106.8(4) . . ? F35 C72 F33 105.6(3) . . ? F34 C72 F33 106.0(4) . . ? F35 C72 C68 113.3(4) . . ? F34 C72 C68 112.3(4) . . ? F33 C72 C68 112.3(4) . . ? F36 C73 F37 107.3(4) . . ? F36 C73 F38 106.5(4) . . ? F37 C73 F38 104.9(4) . . ? F36 C73 C70 113.2(4) . . ? F37 C73 C70 112.1(4) . . ? F38 C73 C70 112.2(4) . . ? C79 C74 C75 115.5(4) . . ? C79 C74 B2 124.0(4) . . ? C75 C74 B2 120.3(4) . . ? C76 C75 C74 122.5(4) . . ? C77 C76 C75 120.6(4) . . ? C77 C76 C80 118.4(4) . . ? C75 C76 C80 121.0(4) . . ? C78 C77 C76 118.3(4) . . ? C77 C78 C79 120.9(4) . . ? C77 C78 C81 119.1(4) . . ? C79 C78 C81 119.9(4) . . ? C74 C79 C78 122.2(4) . . ? F39 C80 F40 107.8(4) . . ? F39 C80 F41 105.5(4) . . ? F40 C80 F41 105.8(4) . . ? F39 C80 C76 112.9(4) . . ? F40 C80 C76 112.3(4) . . ? F41 C80 C76 112.1(4) . . ? F44 C81 F43 107.1(4) . . ? F44 C81 F42 105.8(4) . . ? F43 C81 F42 105.3(4) . . ? F44 C81 C78 113.8(4) . . ? F43 C81 C78 112.3(4) . . ? F42 C81 C78 112.0(4) . . ? C83 C82 C87 115.6(4) . . ? C83 C82 B2 123.6(4) . . ? C87 C82 B2 120.8(4) . . ? C82 C83 C84 122.3(4) . . ? C85 C84 C83 120.2(4) . . ? C85 C84 C88 122.0(4) . . ? C83 C84 C88 117.8(4) . . ? C86 C85 C84 118.9(4) . . ? C85 C86 C87 120.3(4) . . ? C85 C86 C89 121.6(4) . . ? C87 C86 C89 118.1(4) . . ? C86 C87 C82 122.8(4) . . ? F47 C88 F46 106.4(4) . . ? F47 C88 F45 105.5(5) . . ? F46 C88 F45 105.9(4) . . ? F47 C88 C84 112.9(4) . . ? F46 C88 C84 113.1(4) . . ? F45 C88 C84 112.5(4) . . ? F49 C89 F50 106.9(4) . . ? F49 C89 F48 109.0(4) . . ? F50 C89 F48 101.9(4) . . ? F49 C89 C86 114.1(5) . . ? F50 C89 C86 112.1(4) . . ? F48 C89 C86 112.0(4) . . ? C90 O1 C92 113.6(11) . . ? O1 C90 C91 112.9(17) . . ? O1 C92 C93 109.7(19) . . ? _diffrn_measured_fraction_theta_max 0.984 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.984 _refine_diff_density_max 0.750 _refine_diff_density_min -0.460 _refine_diff_density_rms 0.073