# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'Pedro Valerga' _publ_contact_author_email PEDRO.VALERGA@UCA.ES _publ_section_title ; Oligomerization of Styrenes Mediated by Cationic Allyl Nickel Complexes Containing Triphenylstibine or Triphenylarsine ; loop_ _publ_author_name 'Pedro Valerga' I.d.l.Rios M.Jimenez-Tenorio 'Kurt Mereiter' 'M. Puerta' ; I.Salcedo ; # Attachment 'global_Ni2008.txt' #=== Data for 777m (compound 1b in the text) data_777m _database_code_depnum_ccdc_archive 'CCDC 703649' _audit_creation_method SHELXL-97 _chemical_name_systematic ; (\h^3^-allyl)-tris-(triphenyl-stibine)-nickel(II) tetrakis-(3,5-bis-trifluoromethyl-phenyl)-borate dichloromethane solvate ; _chemical_name_common ; (eta$3!-allyl)-tris-(triphenyl-stibine)-nickel(ii) tetrakis- (3,5-bis-trifluoromethyl-phenyl)-borate dichloromethane solvate ; _chemical_melting_point ? _chemical_formula_moiety 'C57 H50 Ni Sb3 1+,C32 H12 F24 B 1-,0.857(C H2 Cl2)' _chemical_formula_sum 'C89.86 H63.71 B Cl1.71 F24 Ni Sb3' _chemical_formula_weight 2094.95 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' Cl Cl 0.1484 0.1585 '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' Sb Sb -0.5866 1.5461 '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' _symmetry_space_group_name_Hall '-P 1' _symmetry_int_tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 13.2682(6) _cell_length_b 17.6246(7) _cell_length_c 19.2441(8) _cell_angle_alpha 68.634(1) _cell_angle_beta 84.927(1) _cell_angle_gamma 87.387(1) _cell_volume 4174.0(3) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9156 _cell_measurement_theta_min 2.3 _cell_measurement_theta_max 30.0 _exptl_crystal_description block _exptl_crystal_colour red-purple _exptl_crystal_size_max 0.65 _exptl_crystal_size_mid 0.55 _exptl_crystal_size_min 0.45 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.677 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2068.0 _exptl_absorpt_coefficient_mu 1.337 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.845 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details '(SADABS; Sheldrick, 2004)' _exptl_special_details ; Bruker Smart APEX CCD platform 3-circle diffractometer, sealed X-ray tube, Mo-Kalfa radiation, graphite monochromator, Bruker Kryoflex cooling unit. A complete sphere of the reciprocal space was recorded by omega-scan frames (4x600 frames, per frame 0.3deg and 5sec). Frame data evaluation (data integration) with program SAINT (Bruker); Lattice parameters by least-squares refinement of the geometric parameters of the strongest reflections with program SAINT (Bruker). Correction for absorption, crystal decay (insignificant) and effects of the CCD detector by semi-empirical method from equivalents using program SADABS V2.05 (G.M. Sheldrick, Univ. of Goettingen, Germany). Data reduction with program XPREP (BRUKER). ; _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 'BRUKER SMART APEX CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_standards_decay_% 0 _diffrn_reflns_number 62783 _diffrn_reflns_av_R_equivalents 0.0191 _diffrn_reflns_av_sigmaI/netI 0.0237 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 2.13 _diffrn_reflns_theta_max 30.00 _reflns_number_total 24062 _reflns_number_gt 21741 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT, SADABS, XPREP' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; 1) 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. 2) Four of the eight CF~3~ groups showed orientation disorder and were refined with 3 anisotropic major and 3 isotropic minor sites (no geometric restraints) with complementary site occupation factors. (values 0.812(3), 0.790(4), 0.769(4), and 0.896(4) for major sites). 3) Dichloromethane solvent molecule refined in population parameter ; _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^)+(0.0370P)^2^+4.4723P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 24062 _refine_ls_number_parameters 1132 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0347 _refine_ls_R_factor_gt 0.0304 _refine_ls_wR_factor_ref 0.0759 _refine_ls_wR_factor_gt 0.0737 _refine_ls_goodness_of_fit_ref 1.029 _refine_ls_restrained_S_all 1.029 _refine_ls_shift/su_max 0.013 _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 Ni Ni 0.575804(18) 0.280485(14) 0.206253(13) 0.01575(5) Uani 1 1 d . . . Sb1 Sb 0.659158(9) 0.170396(7) 0.304533(7) 0.01617(3) Uani 1 1 d . . . Sb2 Sb 0.392074(9) 0.235131(7) 0.216647(7) 0.01535(3) Uani 1 1 d . . . Sb3 Sb 0.570923(9) 0.394911(7) 0.254565(7) 0.01692(3) Uani 1 1 d . . . C1 C 0.58312(17) 0.37294(13) 0.10062(11) 0.0255(4) Uani 1 1 d . . . H1A H 0.5181 0.3973 0.0807 0.031 Uiso 1 1 calc R . . H1B H 0.6383 0.4127 0.0890 0.031 Uiso 1 1 calc R . . C2 C 0.60941(16) 0.29554(13) 0.09832(11) 0.0227(4) Uani 1 1 d . . . H2 H 0.5683 0.2694 0.0723 0.027 Uiso 1 1 calc R . . C3 C 0.69364(16) 0.25538(14) 0.13584(11) 0.0243(4) Uani 1 1 d . . . H3A H 0.7564 0.2871 0.1263 0.029 Uiso 1 1 calc R . . H3B H 0.7051 0.1977 0.1412 0.029 Uiso 1 1 calc R . . C5 C 0.59922(15) 0.12657(11) 0.41815(11) 0.0185(3) Uani 1 1 d . . . C6 C 0.49475(16) 0.12224(13) 0.43295(12) 0.0228(4) Uani 1 1 d . . . H6 H 0.4523 0.1361 0.3927 0.027 Uiso 1 1 calc R . . C7 C 0.45185(16) 0.09776(13) 0.50609(12) 0.0255(4) Uani 1 1 d . . . H7 H 0.3804 0.0948 0.5157 0.031 Uiso 1 1 calc R . . C8 C 0.51314(17) 0.07764(14) 0.56494(12) 0.0264(4) Uani 1 1 d . . . H8 H 0.4838 0.0624 0.6149 0.032 Uiso 1 1 calc R . . C9 C 0.61781(17) 0.07974(15) 0.55086(12) 0.0285(4) Uani 1 1 d . . . H9 H 0.6600 0.0644 0.5913 0.034 Uiso 1 1 calc R . . C10 C 0.66102(16) 0.10424(13) 0.47754(12) 0.0242(4) Uani 1 1 d . . . H10 H 0.7325 0.1057 0.4681 0.029 Uiso 1 1 calc R . . C11 C 0.80602(15) 0.20800(12) 0.31298(11) 0.0193(3) Uani 1 1 d . . . C12 C 0.82171(17) 0.24879(14) 0.36121(12) 0.0257(4) Uani 1 1 d . . . H12 H 0.7675 0.2560 0.3941 0.031 Uiso 1 1 calc R . . C13 C 0.91701(18) 0.27882(15) 0.36078(13) 0.0293(5) Uani 1 1 d . . . H13 H 0.9281 0.3058 0.3940 0.035 Uiso 1 1 calc R . . C14 C 0.99581(17) 0.26952(14) 0.31215(13) 0.0272(4) Uani 1 1 d . . . H14 H 1.0607 0.2903 0.3120 0.033 Uiso 1 1 calc R . . C15 C 0.98020(16) 0.23003(14) 0.26376(13) 0.0262(4) Uani 1 1 d . . . H15 H 1.0342 0.2241 0.2302 0.031 Uiso 1 1 calc R . . C16 C 0.88539(15) 0.19905(13) 0.26419(12) 0.0225(4) Uani 1 1 d . . . H16 H 0.8749 0.1717 0.2311 0.027 Uiso 1 1 calc R . . C17 C 0.69321(15) 0.05815(12) 0.28868(11) 0.0206(4) Uani 1 1 d . . . C18 C 0.75174(16) -0.00146(13) 0.33880(12) 0.0250(4) Uani 1 1 d . . . H18 H 0.7794 0.0094 0.3781 0.030 Uiso 1 1 calc R . . C19 C 0.76955(19) -0.07647(14) 0.33131(14) 0.0309(5) Uani 1 1 d . . . H19 H 0.8094 -0.1168 0.3654 0.037 Uiso 1 1 calc R . . C20 C 0.7293(2) -0.09270(15) 0.27418(15) 0.0353(5) Uani 1 1 d . . . H20 H 0.7412 -0.1442 0.2695 0.042 Uiso 1 1 calc R . . C21 C 0.6718(2) -0.03421(15) 0.22419(14) 0.0360(5) Uani 1 1 d . . . H21 H 0.6448 -0.0452 0.1848 0.043 Uiso 1 1 calc R . . C22 C 0.65350(18) 0.04108(14) 0.23162(13) 0.0279(4) Uani 1 1 d . . . H22 H 0.6135 0.0811 0.1974 0.033 Uiso 1 1 calc R . . C23 C 0.29596(14) 0.21801(11) 0.31587(11) 0.0175(3) Uani 1 1 d . . . C24 C 0.23226(16) 0.15110(13) 0.34745(12) 0.0228(4) Uani 1 1 d . . . H24 H 0.2270 0.1138 0.3227 0.027 Uiso 1 1 calc R . . C25 C 0.17667(17) 0.13932(14) 0.41507(12) 0.0274(4) Uani 1 1 d . . . H25 H 0.1332 0.0939 0.4364 0.033 Uiso 1 1 calc R . . C26 C 0.18404(17) 0.19326(14) 0.45169(12) 0.0251(4) Uani 1 1 d . . . H26 H 0.1457 0.1847 0.4979 0.030 Uiso 1 1 calc R . . C27 C 0.24739(16) 0.25975(13) 0.42097(11) 0.0227(4) Uani 1 1 d . . . H27 H 0.2525 0.2967 0.4461 0.027 Uiso 1 1 calc R . . C28 C 0.30316(15) 0.27193(12) 0.35351(11) 0.0200(4) Uani 1 1 d . . . H28 H 0.3467 0.3173 0.3326 0.024 Uiso 1 1 calc R . . C29 C 0.35572(15) 0.12692(12) 0.20014(11) 0.0200(4) Uani 1 1 d . . . C30 C 0.29154(18) 0.12724(14) 0.14682(14) 0.0291(5) Uani 1 1 d . . . H30 H 0.2641 0.1773 0.1149 0.035 Uiso 1 1 calc R . . C31 C 0.2673(2) 0.05402(16) 0.14004(15) 0.0356(5) Uani 1 1 d . . . H31 H 0.2236 0.0543 0.1034 0.043 Uiso 1 1 calc R . . C32 C 0.30697(19) -0.01872(15) 0.18657(14) 0.0324(5) Uani 1 1 d . . . H32 H 0.2902 -0.0684 0.1819 0.039 Uiso 1 1 calc R . . C33 C 0.3708(2) -0.01977(14) 0.23981(14) 0.0337(5) Uani 1 1 d . . . H33 H 0.3976 -0.0700 0.2718 0.040 Uiso 1 1 calc R . . C34 C 0.39563(18) 0.05320(13) 0.24633(13) 0.0269(4) Uani 1 1 d . . . H34 H 0.4401 0.0526 0.2826 0.032 Uiso 1 1 calc R . . C35 C 0.30343(14) 0.32065(12) 0.13499(11) 0.0182(3) Uani 1 1 d . . . C36 C 0.33715(17) 0.34611(14) 0.05959(12) 0.0256(4) Uani 1 1 d . . . H36 H 0.3968 0.3223 0.0446 0.031 Uiso 1 1 calc R . . C37 C 0.28467(17) 0.40590(14) 0.00593(12) 0.0276(4) Uani 1 1 d . . . H37 H 0.3086 0.4229 -0.0454 0.033 Uiso 1 1 calc R . . C38 C 0.19747(16) 0.44081(13) 0.02722(12) 0.0243(4) Uani 1 1 d . . . H38 H 0.1617 0.4821 -0.0093 0.029 Uiso 1 1 calc R . . C39 C 0.16277(16) 0.41511(14) 0.10212(13) 0.0269(4) Uani 1 1 d . . . H39 H 0.1028 0.4387 0.1168 0.032 Uiso 1 1 calc R . . C40 C 0.21508(15) 0.35509(13) 0.15595(12) 0.0227(4) Uani 1 1 d . . . H40 H 0.1904 0.3376 0.2071 0.027 Uiso 1 1 calc R . . C41 C 0.51730(15) 0.39123(12) 0.36350(11) 0.0202(4) Uani 1 1 d . . . C42 C 0.53649(18) 0.32316(13) 0.42619(13) 0.0272(4) Uani 1 1 d . . . H42 H 0.5732 0.2781 0.4202 0.033 Uiso 1 1 calc R . . C43 C 0.5026(2) 0.32025(15) 0.49745(13) 0.0325(5) Uani 1 1 d . . . H43 H 0.5158 0.2733 0.5399 0.039 Uiso 1 1 calc R . . C44 C 0.44950(19) 0.38592(17) 0.50644(14) 0.0348(5) Uani 1 1 d . . . H44 H 0.4264 0.3843 0.5551 0.042 Uiso 1 1 calc R . . C45 C 0.4302(2) 0.45393(19) 0.44443(15) 0.0406(6) Uani 1 1 d . . . H45 H 0.3939 0.4990 0.4508 0.049 Uiso 1 1 calc R . . C46 C 0.46341(19) 0.45714(15) 0.37284(14) 0.0317(5) Uani 1 1 d . . . H46 H 0.4495 0.5040 0.3305 0.038 Uiso 1 1 calc R . . C47 C 0.48452(15) 0.49770(12) 0.18922(11) 0.0201(4) Uani 1 1 d . . . C48 C 0.38204(16) 0.48874(13) 0.18323(13) 0.0259(4) Uani 1 1 d . . . H48 H 0.3507 0.4379 0.2102 0.031 Uiso 1 1 calc R . . C49 C 0.32538(17) 0.55330(14) 0.13831(13) 0.0275(4) Uani 1 1 d . . . H49 H 0.2557 0.5465 0.1345 0.033 Uiso 1 1 calc R . . C50 C 0.37076(17) 0.62816(13) 0.09880(12) 0.0260(4) Uani 1 1 d . . . H50 H 0.3323 0.6723 0.0677 0.031 Uiso 1 1 calc R . . C51 C 0.47176(17) 0.63791(13) 0.10506(12) 0.0257(4) Uani 1 1 d . . . H51 H 0.5026 0.6890 0.0785 0.031 Uiso 1 1 calc R . . C52 C 0.52884(16) 0.57303(12) 0.15027(12) 0.0224(4) Uani 1 1 d . . . H52 H 0.5982 0.5803 0.1545 0.027 Uiso 1 1 calc R . . C53 C 0.71182(16) 0.45412(13) 0.23983(12) 0.0242(4) Uani 1 1 d . . . C54 C 0.7203(2) 0.51928(15) 0.26379(14) 0.0346(5) Uani 1 1 d . . . H54 H 0.6648 0.5348 0.2907 0.041 Uiso 1 1 calc R . . C55 C 0.8113(2) 0.56147(18) 0.24773(16) 0.0461(7) Uani 1 1 d . . . H55 H 0.8173 0.6059 0.2639 0.055 Uiso 1 1 calc R . . C56 C 0.8914(2) 0.53973(19) 0.20930(16) 0.0499(8) Uani 1 1 d . . . H56 H 0.9524 0.5694 0.1983 0.060 Uiso 1 1 calc R . . C57 C 0.8841(2) 0.4747(2) 0.18626(18) 0.0482(8) Uani 1 1 d . . . H57 H 0.9403 0.4593 0.1599 0.058 Uiso 1 1 calc R . . C58 C 0.79392(17) 0.43150(16) 0.20185(15) 0.0337(5) Uani 1 1 d . . . H58 H 0.7890 0.3865 0.1863 0.040 Uiso 1 1 calc R . . B B 0.09646(17) 0.77828(13) 0.19497(12) 0.0174(4) Uani 1 1 d . . . C59 C 0.03113(15) 0.76335(11) 0.13251(11) 0.0181(3) Uani 1 1 d . . . C60 C 0.07142(15) 0.72236(11) 0.08596(11) 0.0183(3) Uani 1 1 d . . . H60 H 0.1417 0.7092 0.0852 0.022 Uiso 1 1 calc R . . C61 C 0.01162(15) 0.70035(12) 0.04085(11) 0.0190(3) Uani 1 1 d . A . C62 C -0.09140(16) 0.71831(13) 0.03978(11) 0.0224(4) Uani 1 1 d . . . H62 H -0.1321 0.7036 0.0086 0.027 Uiso 1 1 calc R . . C63 C -0.13277(15) 0.75865(13) 0.08593(12) 0.0219(4) Uani 1 1 d . B . C64 C -0.07281(15) 0.78010(12) 0.13130(11) 0.0207(4) Uani 1 1 d . . . H64 H -0.1035 0.8071 0.1626 0.025 Uiso 1 1 calc R . . C65 C 0.05628(16) 0.65350(13) -0.00562(11) 0.0221(4) Uani 1 1 d . . . C66 C -0.24342(17) 0.77949(16) 0.08717(14) 0.0309(5) Uani 1 1 d . . . C67 C 0.06780(15) 0.69726(12) 0.26873(11) 0.0179(3) Uani 1 1 d . . . C68 C -0.01368(16) 0.69624(12) 0.32009(11) 0.0211(4) Uani 1 1 d . . . H68 H -0.0472 0.7462 0.3166 0.025 Uiso 1 1 calc R . . C69 C -0.04751(16) 0.62471(13) 0.37626(11) 0.0234(4) Uani 1 1 d . C . C70 C -0.00256(16) 0.54988(12) 0.38318(11) 0.0224(4) Uani 1 1 d . . . H70 H -0.0263 0.5009 0.4212 0.027 Uiso 1 1 calc R . . C71 C 0.07849(15) 0.54946(12) 0.33236(11) 0.0189(3) Uani 1 1 d . D . C72 C 0.11337(15) 0.62137(11) 0.27717(11) 0.0184(3) Uani 1 1 d . . . H72 H 0.1700 0.6190 0.2441 0.022 Uiso 1 1 calc R . . C73 C -0.1381(2) 0.62981(16) 0.42653(14) 0.0388(6) Uani 1 1 d . . . C74 C 0.12832(16) 0.47051(12) 0.33454(12) 0.0227(4) Uani 1 1 d . . . C75 C 0.06158(15) 0.86263(12) 0.20818(11) 0.0194(4) Uani 1 1 d . . . C76 C 0.02322(16) 0.93031(12) 0.15159(12) 0.0236(4) Uani 1 1 d . . . H76 H 0.0158 0.9268 0.1042 0.028 Uiso 1 1 calc R . . C77 C -0.00428(19) 1.00231(13) 0.16262(13) 0.0292(5) Uani 1 1 d . E . C78 C 0.00629(18) 1.01029(13) 0.23065(14) 0.0299(5) Uani 1 1 d . . . H78 H -0.0129 1.0594 0.2383 0.036 Uiso 1 1 calc R . . C79 C 0.04560(16) 0.94472(13) 0.28710(13) 0.0251(4) Uani 1 1 d . F . C80 C 0.07338(15) 0.87259(12) 0.27583(12) 0.0220(4) Uani 1 1 d . . . H80 H 0.1012 0.8289 0.3153 0.026 Uiso 1 1 calc R . . C81 C -0.0463(3) 1.07104(16) 0.09972(16) 0.0465(7) Uani 1 1 d . . . C82 C 0.05798(18) 0.94995(15) 0.36172(14) 0.0305(5) Uani 1 1 d . . . C83 C 0.21801(15) 0.78632(11) 0.17184(11) 0.0175(3) Uani 1 1 d . . . C84 C 0.28903(15) 0.75665(12) 0.22590(11) 0.0207(4) Uani 1 1 d . . . H84 H 0.2659 0.7257 0.2760 0.025 Uiso 1 1 calc R . . C85 C 0.39189(16) 0.77104(13) 0.20847(12) 0.0233(4) Uani 1 1 d . G . C86 C 0.42940(16) 0.81579(13) 0.13618(12) 0.0236(4) Uani 1 1 d . . . H86 H 0.4997 0.8259 0.1244 0.028 Uiso 1 1 calc R . . C87 C 0.36110(16) 0.84542(12) 0.08163(11) 0.0213(4) Uani 1 1 d . H . C88 C 0.25772(15) 0.83119(12) 0.09913(11) 0.0201(4) Uani 1 1 d . . . H88 H 0.2128 0.8526 0.0605 0.024 Uiso 1 1 calc R . . C89 C 0.46354(18) 0.73764(17) 0.26922(14) 0.0329(5) Uani 1 1 d . . . C90 C 0.39814(18) 0.89336(15) 0.00247(13) 0.0290(4) Uani 1 1 d . . . F65A F 0.15724(10) 0.64425(10) -0.00408(8) 0.0333(3) Uani 1 1 d . A 1 F65B F 0.01986(10) 0.57737(8) 0.01813(8) 0.0297(3) Uani 1 1 d . A 1 F65C F 0.03754(13) 0.68746(9) -0.07777(8) 0.0390(4) Uani 1 1 d . A 1 F66A F -0.29683(16) 0.7447(2) 0.0549(2) 0.0938(15) Uani 0.812(3) 1 d P B 1 F66B F -0.28470(19) 0.7661(4) 0.15418(16) 0.125(2) Uani 0.812(3) 1 d P B 1 F66C F -0.26079(19) 0.85774(18) 0.0526(3) 0.1026(16) Uani 0.812(3) 1 d P B 1 F73A F -0.15150(13) 0.56352(10) 0.48779(8) 0.0408(4) Uani 1 1 d . C 1 F73B F -0.22407(14) 0.64117(16) 0.39141(11) 0.0749(7) Uani 1 1 d . C 1 F73C F -0.1324(2) 0.69187(12) 0.44941(13) 0.0834(9) Uani 1 1 d . C 1 F74A F 0.08091(11) 0.40541(8) 0.38394(8) 0.0311(3) Uani 1 1 d . D 1 F74B F 0.13142(12) 0.46198(8) 0.26765(8) 0.0339(3) Uani 1 1 d . D 1 F74C F 0.22477(10) 0.46517(8) 0.35230(9) 0.0316(3) Uani 1 1 d . D 1 F81A F 0.0151(2) 1.09147(16) 0.03728(14) 0.0501(7) Uani 0.790(4) 1 d P E 1 F81B F -0.0769(3) 1.13466(16) 0.11286(13) 0.0844(16) Uani 0.790(4) 1 d P E 1 F81C F -0.1334(2) 1.04784(18) 0.07541(19) 0.0879(13) Uani 0.790(4) 1 d P E 1 F82A F 0.01740(17) 1.01800(13) 0.36811(12) 0.0660(6) Uani 1 1 d . F 1 F82B F 0.01506(16) 0.88831(13) 0.41764(10) 0.0598(6) Uani 1 1 d . F 1 F82C F 0.15420(12) 0.94888(13) 0.37619(10) 0.0500(4) Uani 1 1 d . F 1 F89A F 0.5508(2) 0.7135(4) 0.24673(16) 0.129(2) Uani 0.769(4) 1 d P G 1 F89B F 0.4767(5) 0.78375(19) 0.3045(3) 0.136(3) Uani 0.769(4) 1 d P G 1 F89C F 0.4331(2) 0.66699(17) 0.32200(17) 0.0752(11) Uani 0.769(4) 1 d P G 1 F90A F 0.49696(15) 0.9015(2) -0.00749(12) 0.0756(10) Uani 0.896(4) 1 d P H 1 F90B F 0.3594(2) 0.96840(12) -0.02214(11) 0.0578(7) Uani 0.896(4) 1 d P H 1 F90C F 0.3708(2) 0.85978(16) -0.04443(11) 0.0623(8) Uani 0.896(4) 1 d P H 1 F66D F -0.2728(7) 0.8278(6) 0.1187(7) 0.0426(10) Uiso 0.188(3) 1 d P B 2 F66E F -0.2722(7) 0.8175(6) 0.0198(5) 0.0426(10) Uiso 0.188(3) 1 d P B 2 F66F F -0.2980(7) 0.7141(6) 0.1194(6) 0.0426(10) Uiso 0.188(3) 1 d P B 2 F81D F -0.1284(6) 1.0877(6) 0.1182(5) 0.0426(10) Uiso 0.210(4) 1 d P E 2 F81E F -0.0209(8) 1.0762(7) 0.0400(7) 0.0426(10) Uiso 0.210(4) 1 d P E 2 F81F F 0.0106(7) 1.1447(5) 0.1119(5) 0.0426(10) Uiso 0.210(4) 1 d P E 2 F89D F 0.4270(6) 0.7487(5) 0.3286(4) 0.0426(10) Uiso 0.231(4) 1 d P G 2 F89E F 0.4954(7) 0.6709(5) 0.2779(5) 0.0426(10) Uiso 0.231(4) 1 d P G 2 F89F F 0.5464(6) 0.7853(5) 0.2508(5) 0.0426(10) Uiso 0.231(4) 1 d P G 2 F90D F 0.3370(14) 0.8975(12) -0.0478(11) 0.0426(10) Uiso 0.104(4) 1 d P H 2 F90E F 0.4786(14) 0.8523(11) -0.0204(10) 0.0426(10) Uiso 0.104(4) 1 d P H 2 F90F F 0.4269(15) 0.9611(11) -0.0114(10) 0.0426(10) Uiso 0.104(4) 1 d P H 2 C4 C 0.2398(3) 0.6396(2) 0.45985(19) 0.0479(8) Uani 0.857(2) 1 d P . . H4A H 0.3067 0.6304 0.4368 0.057 Uiso 0.857(2) 1 calc PR . . H4B H 0.1875 0.6200 0.4370 0.057 Uiso 0.857(2) 1 calc PR . . Cl1 Cl 0.23410(7) 0.58275(5) 0.55609(5) 0.0453(2) Uani 0.857(2) 1 d P . . Cl2 Cl 0.22124(10) 0.74404(6) 0.43998(5) 0.0618(3) Uani 0.857(2) 1 d P . . 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 Ni 0.01642(11) 0.01547(11) 0.01426(11) -0.00449(8) 0.00083(8) -0.00058(8) Sb1 0.01613(6) 0.01597(6) 0.01571(6) -0.00504(4) -0.00036(4) -0.00058(4) Sb2 0.01541(6) 0.01559(6) 0.01573(6) -0.00661(4) -0.00026(4) -0.00094(4) Sb3 0.01614(6) 0.01559(6) 0.01928(6) -0.00665(4) -0.00009(4) -0.00255(4) C1 0.0306(11) 0.0223(9) 0.0179(9) -0.0015(7) 0.0019(8) 0.0007(8) C2 0.0249(10) 0.0258(10) 0.0152(8) -0.0062(7) 0.0034(7) -0.0004(8) C3 0.0234(10) 0.0281(10) 0.0183(9) -0.0062(8) 0.0054(7) -0.0001(8) C5 0.0214(9) 0.0160(8) 0.0164(8) -0.0039(7) 0.0000(7) -0.0012(7) C6 0.0211(9) 0.0236(9) 0.0208(9) -0.0047(7) -0.0025(7) 0.0017(7) C7 0.0209(9) 0.0253(10) 0.0253(10) -0.0044(8) 0.0019(8) 0.0008(8) C8 0.0290(11) 0.0271(10) 0.0195(9) -0.0047(8) 0.0027(8) -0.0028(8) C9 0.0270(11) 0.0354(12) 0.0190(9) -0.0042(8) -0.0042(8) -0.0040(9) C10 0.0202(9) 0.0285(10) 0.0208(9) -0.0050(8) -0.0014(7) -0.0024(8) C11 0.0186(8) 0.0181(8) 0.0202(9) -0.0056(7) -0.0018(7) -0.0006(7) C12 0.0241(10) 0.0306(11) 0.0254(10) -0.0142(9) 0.0044(8) -0.0075(8) C13 0.0291(11) 0.0336(12) 0.0301(11) -0.0171(9) 0.0017(9) -0.0102(9) C14 0.0221(10) 0.0298(11) 0.0300(11) -0.0108(9) -0.0018(8) -0.0058(8) C15 0.0190(9) 0.0308(11) 0.0294(11) -0.0126(9) 0.0013(8) 0.0006(8) C16 0.0202(9) 0.0234(9) 0.0257(10) -0.0116(8) -0.0008(7) 0.0013(7) C17 0.0197(9) 0.0185(9) 0.0229(9) -0.0076(7) 0.0028(7) -0.0022(7) C18 0.0257(10) 0.0233(10) 0.0262(10) -0.0088(8) -0.0035(8) 0.0007(8) C19 0.0326(12) 0.0225(10) 0.0346(12) -0.0072(9) -0.0027(9) 0.0037(8) C20 0.0454(14) 0.0237(11) 0.0392(13) -0.0159(10) 0.0034(11) 0.0000(10) C21 0.0530(16) 0.0305(12) 0.0313(12) -0.0184(10) -0.0079(11) -0.0004(11) C22 0.0363(12) 0.0228(10) 0.0248(10) -0.0085(8) -0.0048(9) 0.0004(8) C23 0.0166(8) 0.0178(8) 0.0175(8) -0.0058(7) -0.0010(6) -0.0001(6) C24 0.0242(9) 0.0224(9) 0.0230(9) -0.0100(8) 0.0027(8) -0.0064(7) C25 0.0277(10) 0.0276(10) 0.0252(10) -0.0085(8) 0.0068(8) -0.0086(8) C26 0.0257(10) 0.0285(10) 0.0190(9) -0.0073(8) 0.0037(8) -0.0005(8) C27 0.0251(10) 0.0232(9) 0.0212(9) -0.0103(8) -0.0011(7) 0.0029(7) C28 0.0208(9) 0.0188(9) 0.0213(9) -0.0085(7) -0.0003(7) -0.0014(7) C29 0.0205(9) 0.0202(9) 0.0211(9) -0.0101(7) 0.0010(7) -0.0023(7) C30 0.0319(11) 0.0264(11) 0.0334(12) -0.0147(9) -0.0086(9) -0.0008(8) C31 0.0381(13) 0.0371(13) 0.0422(14) -0.0249(11) -0.0089(11) -0.0058(10) C32 0.0387(13) 0.0270(11) 0.0382(13) -0.0214(10) 0.0094(10) -0.0105(9) C33 0.0482(14) 0.0188(10) 0.0341(12) -0.0101(9) -0.0009(10) -0.0015(9) C34 0.0364(12) 0.0199(9) 0.0257(10) -0.0094(8) -0.0047(9) -0.0003(8) C35 0.0175(8) 0.0190(8) 0.0203(9) -0.0093(7) -0.0020(7) -0.0011(6) C36 0.0244(10) 0.0314(11) 0.0206(9) -0.0101(8) -0.0008(8) 0.0079(8) C37 0.0293(11) 0.0316(11) 0.0195(9) -0.0067(8) -0.0015(8) 0.0028(9) C38 0.0242(10) 0.0220(9) 0.0259(10) -0.0071(8) -0.0063(8) 0.0020(7) C39 0.0194(9) 0.0325(11) 0.0292(11) -0.0125(9) -0.0023(8) 0.0067(8) C40 0.0193(9) 0.0264(10) 0.0219(9) -0.0085(8) 0.0011(7) -0.0007(7) C41 0.0190(9) 0.0211(9) 0.0230(9) -0.0109(7) -0.0009(7) -0.0028(7) C42 0.0345(11) 0.0219(10) 0.0263(10) -0.0104(8) 0.0011(9) -0.0026(8) C43 0.0406(13) 0.0322(12) 0.0233(10) -0.0085(9) 0.0013(9) -0.0061(10) C44 0.0313(12) 0.0516(15) 0.0272(11) -0.0217(11) 0.0010(9) -0.0011(10) C45 0.0437(15) 0.0518(16) 0.0357(13) -0.0280(12) -0.0085(11) 0.0182(12) C46 0.0385(13) 0.0330(12) 0.0281(11) -0.0166(9) -0.0076(9) 0.0115(10) C47 0.0217(9) 0.0184(9) 0.0214(9) -0.0087(7) -0.0009(7) -0.0011(7) C48 0.0241(10) 0.0208(9) 0.0331(11) -0.0088(8) -0.0058(8) -0.0028(7) C49 0.0235(10) 0.0276(10) 0.0319(11) -0.0107(9) -0.0064(8) 0.0012(8) C50 0.0304(11) 0.0247(10) 0.0213(9) -0.0075(8) -0.0016(8) 0.0064(8) C51 0.0285(10) 0.0206(9) 0.0238(10) -0.0048(8) 0.0054(8) 0.0006(8) C52 0.0225(9) 0.0198(9) 0.0239(9) -0.0079(7) 0.0033(7) -0.0021(7) C53 0.0222(9) 0.0233(9) 0.0225(9) -0.0017(8) -0.0042(7) -0.0070(7) C54 0.0392(13) 0.0326(12) 0.0320(12) -0.0093(10) -0.0069(10) -0.0151(10) C55 0.0524(17) 0.0443(15) 0.0376(14) -0.0036(12) -0.0162(12) -0.0290(13) C56 0.0354(14) 0.0541(17) 0.0401(15) 0.0130(13) -0.0154(12) -0.0286(13) C57 0.0200(11) 0.0550(17) 0.0500(17) 0.0043(13) 0.0014(11) -0.0104(11) C58 0.0198(10) 0.0334(12) 0.0395(13) -0.0036(10) 0.0003(9) -0.0036(9) B 0.0207(10) 0.0151(9) 0.0173(9) -0.0069(7) -0.0028(7) 0.0010(7) C59 0.0205(9) 0.0151(8) 0.0173(8) -0.0041(7) -0.0013(7) -0.0016(6) C60 0.0194(8) 0.0171(8) 0.0177(8) -0.0054(7) -0.0011(7) -0.0012(6) C61 0.0222(9) 0.0178(8) 0.0162(8) -0.0052(7) 0.0008(7) -0.0043(7) C62 0.0215(9) 0.0254(10) 0.0198(9) -0.0071(8) -0.0021(7) -0.0047(7) C63 0.0172(9) 0.0250(9) 0.0224(9) -0.0073(8) -0.0011(7) -0.0011(7) C64 0.0208(9) 0.0210(9) 0.0199(9) -0.0070(7) -0.0007(7) -0.0010(7) C65 0.0237(9) 0.0237(9) 0.0206(9) -0.0097(8) -0.0018(7) -0.0035(7) C66 0.0211(10) 0.0421(13) 0.0331(12) -0.0176(10) -0.0045(9) 0.0012(9) C67 0.0201(9) 0.0184(8) 0.0172(8) -0.0083(7) -0.0040(7) 0.0006(7) C68 0.0252(9) 0.0199(9) 0.0191(9) -0.0086(7) -0.0011(7) 0.0030(7) C69 0.0270(10) 0.0231(9) 0.0194(9) -0.0082(7) 0.0029(7) 0.0007(8) C70 0.0262(10) 0.0206(9) 0.0183(9) -0.0052(7) 0.0002(7) -0.0006(7) C71 0.0218(9) 0.0170(8) 0.0191(8) -0.0077(7) -0.0026(7) 0.0000(7) C72 0.0191(8) 0.0177(8) 0.0198(9) -0.0086(7) -0.0014(7) 0.0006(7) C73 0.0459(15) 0.0335(12) 0.0287(12) -0.0064(10) 0.0159(11) 0.0053(11) C74 0.0243(10) 0.0177(9) 0.0255(10) -0.0072(7) -0.0019(8) 0.0003(7) C75 0.0189(9) 0.0172(8) 0.0226(9) -0.0085(7) 0.0007(7) -0.0009(7) C76 0.0276(10) 0.0175(9) 0.0236(10) -0.0062(7) 0.0032(8) 0.0016(7) C77 0.0362(12) 0.0173(9) 0.0284(11) -0.0041(8) 0.0067(9) 0.0040(8) C78 0.0322(11) 0.0180(9) 0.0401(13) -0.0144(9) 0.0121(9) -0.0016(8) C79 0.0215(9) 0.0245(10) 0.0348(11) -0.0180(9) 0.0031(8) -0.0035(7) C80 0.0209(9) 0.0203(9) 0.0280(10) -0.0124(8) -0.0031(7) 0.0003(7) C81 0.0630(19) 0.0247(12) 0.0372(14) 0.0006(10) 0.0107(13) 0.0165(12) C82 0.0275(11) 0.0332(12) 0.0400(13) -0.0246(10) 0.0001(9) -0.0023(9) C83 0.0206(9) 0.0145(8) 0.0198(8) -0.0090(7) -0.0026(7) -0.0002(6) C84 0.0223(9) 0.0210(9) 0.0200(9) -0.0085(7) -0.0037(7) 0.0005(7) C85 0.0217(9) 0.0282(10) 0.0231(10) -0.0121(8) -0.0061(7) 0.0013(8) C86 0.0204(9) 0.0279(10) 0.0253(10) -0.0132(8) -0.0005(8) -0.0020(7) C87 0.0251(10) 0.0210(9) 0.0200(9) -0.0101(7) 0.0009(7) -0.0034(7) C88 0.0229(9) 0.0180(8) 0.0209(9) -0.0087(7) -0.0030(7) -0.0003(7) C89 0.0255(11) 0.0435(14) 0.0282(11) -0.0102(10) -0.0076(9) 0.0024(9) C90 0.0296(11) 0.0318(11) 0.0258(10) -0.0109(9) 0.0019(8) -0.0074(9) F65A 0.0206(6) 0.0503(9) 0.0405(8) -0.0313(7) 0.0069(5) -0.0076(6) F65B 0.0271(6) 0.0199(6) 0.0441(8) -0.0145(6) 0.0018(6) -0.0028(5) F65C 0.0658(10) 0.0344(8) 0.0200(6) -0.0134(6) -0.0088(6) 0.0075(7) F66A 0.0200(10) 0.149(3) 0.183(4) -0.141(3) -0.0261(15) 0.0135(14) F66B 0.0249(12) 0.298(6) 0.0381(14) -0.048(3) 0.0004(10) 0.039(2) F66C 0.0318(13) 0.0507(16) 0.199(5) -0.015(2) -0.0175(19) 0.0159(11) F73A 0.0489(9) 0.0395(8) 0.0262(7) -0.0065(6) 0.0156(6) -0.0037(7) F73B 0.0345(9) 0.1140(19) 0.0465(11) -0.0009(11) 0.0131(8) 0.0275(11) F73C 0.131(2) 0.0413(10) 0.0754(14) -0.0335(10) 0.0710(14) -0.0173(12) F74A 0.0329(7) 0.0156(6) 0.0407(8) -0.0063(5) 0.0030(6) -0.0035(5) F74B 0.0478(8) 0.0269(7) 0.0323(7) -0.0179(6) -0.0030(6) 0.0067(6) F74C 0.0231(6) 0.0235(6) 0.0461(8) -0.0099(6) -0.0058(6) 0.0031(5) F81A 0.0607(18) 0.0418(14) 0.0312(10) 0.0029(9) 0.0078(12) 0.0086(12) F81B 0.174(4) 0.0419(15) 0.0356(12) -0.0170(11) -0.0221(17) 0.064(2) F81C 0.076(2) 0.0570(17) 0.098(2) 0.0210(16) -0.0564(18) -0.0003(14) F82A 0.0884(15) 0.0657(12) 0.0738(13) -0.0587(11) -0.0355(12) 0.0375(11) F82B 0.0791(13) 0.0765(13) 0.0336(9) -0.0317(9) 0.0175(9) -0.0435(11) F82C 0.0312(8) 0.0768(13) 0.0513(10) -0.0328(9) -0.0088(7) -0.0029(8) F89A 0.0346(15) 0.282(7) 0.0369(15) -0.025(2) -0.0100(12) 0.065(3) F89B 0.253(6) 0.0420(16) 0.148(4) -0.045(2) -0.178(5) 0.042(3) F89C 0.0595(17) 0.0608(17) 0.0711(19) 0.0268(14) -0.0436(16) -0.0138(13) F90A 0.0288(10) 0.132(3) 0.0367(11) 0.0041(13) 0.0084(8) -0.0176(12) F90B 0.089(2) 0.0298(9) 0.0368(10) 0.0033(8) 0.0165(11) 0.0059(10) F90C 0.114(2) 0.0564(14) 0.0235(9) -0.0228(9) 0.0148(11) -0.0388(15) C4 0.072(2) 0.0411(18) 0.0354(16) -0.0206(14) 0.0031(16) -0.0046(16) Cl1 0.0563(5) 0.0371(4) 0.0401(4) -0.0103(3) 0.0005(3) -0.0169(3) Cl2 0.1025(9) 0.0478(5) 0.0372(4) -0.0169(4) -0.0262(5) 0.0305(5) _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 Ni C2 2.007(2) . ? Ni C1 2.089(2) . ? Ni C3 2.115(2) . ? Ni Sb1 2.4628(3) . ? Ni Sb3 2.5059(3) . ? Ni Sb2 2.5684(3) . ? Sb1 C11 2.1248(19) . ? Sb1 C5 2.1278(19) . ? Sb1 C17 2.132(2) . ? Sb2 C29 2.1269(19) . ? Sb2 C23 2.1326(19) . ? Sb2 C35 2.1363(19) . ? Sb3 C53 2.129(2) . ? Sb3 C41 2.132(2) . ? Sb3 C47 2.141(2) . ? C1 C2 1.408(3) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 C3 1.403(3) . ? C2 H2 1.0000 . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C5 C6 1.390(3) . ? C5 C10 1.394(3) . ? C6 C7 1.389(3) . ? C6 H6 0.9500 . ? C7 C8 1.383(3) . ? C7 H7 0.9500 . ? C8 C9 1.391(3) . ? C8 H8 0.9500 . ? C9 C10 1.393(3) . ? C9 H9 0.9500 . ? C10 H10 0.9500 . ? C11 C16 1.390(3) . ? C11 C12 1.398(3) . ? C12 C13 1.391(3) . ? C12 H12 0.9500 . ? C13 C14 1.385(3) . ? C13 H13 0.9500 . ? C14 C15 1.383(3) . ? C14 H14 0.9500 . ? C15 C16 1.392(3) . ? C15 H15 0.9500 . ? C16 H16 0.9500 . ? C17 C22 1.390(3) . ? C17 C18 1.399(3) . ? C18 C19 1.389(3) . ? C18 H18 0.9500 . ? C19 C20 1.387(4) . ? C19 H19 0.9500 . ? C20 C21 1.380(4) . ? C20 H20 0.9500 . ? C21 C22 1.394(3) . ? C21 H21 0.9500 . ? C22 H22 0.9500 . ? C23 C24 1.397(3) . ? C23 C28 1.400(3) . ? C24 C25 1.388(3) . ? C24 H24 0.9500 . ? C25 C26 1.385(3) . ? C25 H25 0.9500 . ? C26 C27 1.388(3) . ? C26 H26 0.9500 . ? C27 C28 1.386(3) . ? C27 H27 0.9500 . ? C28 H28 0.9500 . ? C29 C30 1.388(3) . ? C29 C34 1.392(3) . ? C30 C31 1.398(3) . ? C30 H30 0.9500 . ? C31 C32 1.381(4) . ? C31 H31 0.9500 . ? C32 C33 1.380(4) . ? C32 H32 0.9500 . ? C33 C34 1.394(3) . ? C33 H33 0.9500 . ? C34 H34 0.9500 . ? C35 C40 1.391(3) . ? C35 C36 1.392(3) . ? C36 C37 1.389(3) . ? C36 H36 0.9500 . ? C37 C38 1.386(3) . ? C37 H37 0.9500 . ? C38 C39 1.386(3) . ? C38 H38 0.9500 . ? C39 C40 1.391(3) . ? C39 H39 0.9500 . ? C40 H40 0.9500 . ? C41 C42 1.390(3) . ? C41 C46 1.395(3) . ? C42 C43 1.388(3) . ? C42 H42 0.9500 . ? C43 C44 1.384(4) . ? C43 H43 0.9500 . ? C44 C45 1.382(4) . ? C44 H44 0.9500 . ? C45 C46 1.390(3) . ? C45 H45 0.9500 . ? C46 H46 0.9500 . ? C47 C52 1.392(3) . ? C47 C48 1.396(3) . ? C48 C49 1.388(3) . ? C48 H48 0.9500 . ? C49 C50 1.394(3) . ? C49 H49 0.9500 . ? C50 C51 1.380(3) . ? C50 H50 0.9500 . ? C51 C52 1.397(3) . ? C51 H51 0.9500 . ? C52 H52 0.9500 . ? C53 C58 1.383(3) . ? C53 C54 1.397(3) . ? C54 C55 1.398(3) . ? C54 H54 0.9500 . ? C55 C56 1.361(5) . ? C55 H55 0.9500 . ? C56 C57 1.382(5) . ? C56 H56 0.9500 . ? C57 C58 1.398(3) . ? C57 H57 0.9500 . ? C58 H58 0.9500 . ? B C83 1.633(3) . ? B C67 1.636(3) . ? B C75 1.637(3) . ? B C59 1.643(3) . ? C59 C64 1.398(3) . ? C59 C60 1.401(3) . ? C60 C61 1.389(3) . ? C60 H60 0.9500 . ? C61 C62 1.389(3) . ? C61 C65 1.494(3) . ? C62 C63 1.390(3) . ? C62 H62 0.9500 . ? C63 C64 1.389(3) . ? C63 C66 1.497(3) . ? C64 H64 0.9500 . ? C65 F65C 1.338(2) . ? C65 F65A 1.344(2) . ? C65 F65B 1.348(2) . ? C66 F66D 1.244(10) . ? C66 F66A 1.288(3) . ? C66 F66B 1.298(3) . ? C66 F66E 1.307(9) . ? C66 F66F 1.308(9) . ? C66 F66C 1.314(4) . ? C67 C68 1.395(3) . ? C67 C72 1.402(3) . ? C68 C69 1.390(3) . ? C68 H68 0.9500 . ? C69 C70 1.388(3) . ? C69 C73 1.495(3) . ? C70 C71 1.390(3) . ? C70 H70 0.9500 . ? C71 C72 1.391(3) . ? C71 C74 1.501(3) . ? C72 H72 0.9500 . ? C73 F73C 1.327(3) . ? C73 F73A 1.328(3) . ? C73 F73B 1.347(4) . ? C74 F74A 1.335(2) . ? C74 F74C 1.344(2) . ? C74 F74B 1.346(2) . ? C75 C80 1.398(3) . ? C75 C76 1.401(3) . ? C76 C77 1.389(3) . ? C76 H76 0.9500 . ? C77 C78 1.386(3) . ? C77 C81 1.494(3) . ? C78 C79 1.385(3) . ? C78 H78 0.9500 . ? C79 C80 1.394(3) . ? C79 C82 1.496(3) . ? C80 H80 0.9500 . ? C81 F81E 1.141(13) . ? C81 F81D 1.174(9) . ? C81 F81B 1.278(3) . ? C81 F81A 1.333(4) . ? C81 F81C 1.413(5) . ? C81 F81F 1.630(9) . ? C82 F82B 1.326(3) . ? C82 F82C 1.328(3) . ? C82 F82A 1.334(3) . ? C83 C88 1.401(3) . ? C83 C84 1.406(3) . ? C84 C85 1.389(3) . ? C84 H84 0.9500 . ? C85 C86 1.385(3) . ? C85 C89 1.504(3) . ? C86 C87 1.386(3) . ? C86 H86 0.9500 . ? C87 C88 1.395(3) . ? C87 C90 1.498(3) . ? C88 H88 0.9500 . ? C89 F89E 1.189(8) . ? C89 F89B 1.260(4) . ? C89 F89D 1.279(8) . ? C89 F89A 1.307(4) . ? C89 F89C 1.341(4) . ? C89 F89F 1.356(8) . ? C90 F90F 1.198(17) . ? C90 F90D 1.296(19) . ? C90 F90A 1.315(3) . ? C90 F90B 1.327(3) . ? C90 F90C 1.328(3) . ? C90 F90E 1.392(17) . ? C4 Cl2 1.749(4) . ? C4 Cl1 1.752(4) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? 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 C2 Ni C1 40.15(8) . . ? C2 Ni C3 39.69(8) . . ? C1 Ni C3 69.74(8) . . ? C2 Ni Sb1 119.76(6) . . ? C1 Ni Sb1 149.85(6) . . ? C3 Ni Sb1 82.87(6) . . ? C2 Ni Sb3 123.45(6) . . ? C1 Ni Sb3 84.82(6) . . ? C3 Ni Sb3 126.02(6) . . ? Sb1 Ni Sb3 102.220(10) . . ? C2 Ni Sb2 97.59(6) . . ? C1 Ni Sb2 100.52(7) . . ? C3 Ni Sb2 124.20(6) . . ? Sb1 Ni Sb2 105.326(10) . . ? Sb3 Ni Sb2 106.383(9) . . ? C11 Sb1 C5 102.15(8) . . ? C11 Sb1 C17 101.19(8) . . ? C5 Sb1 C17 100.46(7) . . ? C11 Sb1 Ni 109.20(5) . . ? C5 Sb1 Ni 122.15(5) . . ? C17 Sb1 Ni 118.68(6) . . ? C29 Sb2 C23 98.06(7) . . ? C29 Sb2 C35 99.14(7) . . ? C23 Sb2 C35 100.46(7) . . ? C29 Sb2 Ni 121.82(5) . . ? C23 Sb2 Ni 120.74(5) . . ? C35 Sb2 Ni 112.60(5) . . ? C53 Sb3 C41 100.97(8) . . ? C53 Sb3 C47 98.08(8) . . ? C41 Sb3 C47 98.99(8) . . ? C53 Sb3 Ni 114.22(6) . . ? C41 Sb3 Ni 127.42(5) . . ? C47 Sb3 Ni 112.47(5) . . ? C2 C1 Ni 66.81(11) . . ? C2 C1 H1A 117.0 . . ? Ni C1 H1A 117.0 . . ? C2 C1 H1B 117.0 . . ? Ni C1 H1B 117.0 . . ? H1A C1 H1B 114.1 . . ? C3 C2 C1 117.5(2) . . ? C3 C2 Ni 74.31(12) . . ? C1 C2 Ni 73.04(12) . . ? C3 C2 H2 121.2 . . ? C1 C2 H2 121.2 . . ? Ni C2 H2 121.2 . . ? C2 C3 Ni 65.99(11) . . ? C2 C3 H3A 117.1 . . ? Ni C3 H3A 117.1 . . ? C2 C3 H3B 117.1 . . ? Ni C3 H3B 117.1 . . ? H3A C3 H3B 114.2 . . ? C6 C5 C10 119.40(18) . . ? C6 C5 Sb1 118.40(14) . . ? C10 C5 Sb1 122.18(15) . . ? C7 C6 C5 120.55(19) . . ? C7 C6 H6 119.7 . . ? C5 C6 H6 119.7 . . ? C8 C7 C6 120.0(2) . . ? C8 C7 H7 120.0 . . ? C6 C7 H7 120.0 . . ? C7 C8 C9 119.9(2) . . ? C7 C8 H8 120.1 . . ? C9 C8 H8 120.1 . . ? C8 C9 C10 120.2(2) . . ? C8 C9 H9 119.9 . . ? C10 C9 H9 119.9 . . ? C9 C10 C5 119.94(19) . . ? C9 C10 H10 120.0 . . ? C5 C10 H10 120.0 . . ? C16 C11 C12 119.67(19) . . ? C16 C11 Sb1 118.95(15) . . ? C12 C11 Sb1 121.05(15) . . ? C13 C12 C11 119.7(2) . . ? C13 C12 H12 120.2 . . ? C11 C12 H12 120.2 . . ? C14 C13 C12 120.3(2) . . ? C14 C13 H13 119.8 . . ? C12 C13 H13 119.8 . . ? C15 C14 C13 120.1(2) . . ? C15 C14 H14 119.9 . . ? C13 C14 H14 119.9 . . ? C14 C15 C16 120.1(2) . . ? C14 C15 H15 120.0 . . ? C16 C15 H15 120.0 . . ? C11 C16 C15 120.14(19) . . ? C11 C16 H16 119.9 . . ? C15 C16 H16 119.9 . . ? C22 C17 C18 119.04(19) . . ? C22 C17 Sb1 121.06(15) . . ? C18 C17 Sb1 119.80(15) . . ? C19 C18 C17 120.2(2) . . ? C19 C18 H18 119.9 . . ? C17 C18 H18 119.9 . . ? C20 C19 C18 120.2(2) . . ? C20 C19 H19 119.9 . . ? C18 C19 H19 119.9 . . ? C21 C20 C19 120.2(2) . . ? C21 C20 H20 119.9 . . ? C19 C20 H20 119.9 . . ? C20 C21 C22 119.9(2) . . ? C20 C21 H21 120.1 . . ? C22 C21 H21 120.1 . . ? C17 C22 C21 120.6(2) . . ? C17 C22 H22 119.7 . . ? C21 C22 H22 119.7 . . ? C24 C23 C28 119.16(18) . . ? C24 C23 Sb2 121.93(14) . . ? C28 C23 Sb2 118.71(14) . . ? C25 C24 C23 119.83(19) . . ? C25 C24 H24 120.1 . . ? C23 C24 H24 120.1 . . ? C26 C25 C24 120.5(2) . . ? C26 C25 H25 119.7 . . ? C24 C25 H25 119.7 . . ? C25 C26 C27 120.12(19) . . ? C25 C26 H26 119.9 . . ? C27 C26 H26 119.9 . . ? C28 C27 C26 119.69(19) . . ? C28 C27 H27 120.2 . . ? C26 C27 H27 120.2 . . ? C27 C28 C23 120.66(18) . . ? C27 C28 H28 119.7 . . ? C23 C28 H28 119.7 . . ? C30 C29 C34 119.35(19) . . ? C30 C29 Sb2 122.34(16) . . ? C34 C29 Sb2 118.28(15) . . ? C29 C30 C31 120.0(2) . . ? C29 C30 H30 120.0 . . ? C31 C30 H30 120.0 . . ? C32 C31 C30 120.0(2) . . ? C32 C31 H31 120.0 . . ? C30 C31 H31 120.0 . . ? C33 C32 C31 120.5(2) . . ? C33 C32 H32 119.8 . . ? C31 C32 H32 119.8 . . ? C32 C33 C34 119.7(2) . . ? C32 C33 H33 120.2 . . ? C34 C33 H33 120.2 . . ? C29 C34 C33 120.5(2) . . ? C29 C34 H34 119.8 . . ? C33 C34 H34 119.8 . . ? C40 C35 C36 118.97(19) . . ? C40 C35 Sb2 121.25(15) . . ? C36 C35 Sb2 119.68(14) . . ? C37 C36 C35 120.79(19) . . ? C37 C36 H36 119.6 . . ? C35 C36 H36 119.6 . . ? C38 C37 C36 120.0(2) . . ? C38 C37 H37 120.0 . . ? C36 C37 H37 120.0 . . ? C37 C38 C39 119.5(2) . . ? C37 C38 H38 120.2 . . ? C39 C38 H38 120.2 . . ? C38 C39 C40 120.57(19) . . ? C38 C39 H39 119.7 . . ? C40 C39 H39 119.7 . . ? C35 C40 C39 120.12(19) . . ? C35 C40 H40 119.9 . . ? C39 C40 H40 119.9 . . ? C42 C41 C46 119.2(2) . . ? C42 C41 Sb3 120.19(15) . . ? C46 C41 Sb3 120.58(16) . . ? C43 C42 C41 120.8(2) . . ? C43 C42 H42 119.6 . . ? C41 C42 H42 119.6 . . ? C44 C43 C42 119.8(2) . . ? C44 C43 H43 120.1 . . ? C42 C43 H43 120.1 . . ? C45 C44 C43 119.8(2) . . ? C45 C44 H44 120.1 . . ? C43 C44 H44 120.1 . . ? C44 C45 C46 120.7(2) . . ? C44 C45 H45 119.6 . . ? C46 C45 H45 119.6 . . ? C45 C46 C41 119.7(2) . . ? C45 C46 H46 120.2 . . ? C41 C46 H46 120.2 . . ? C52 C47 C48 118.86(19) . . ? C52 C47 Sb3 121.57(15) . . ? C48 C47 Sb3 119.53(15) . . ? C49 C48 C47 120.7(2) . . ? C49 C48 H48 119.6 . . ? C47 C48 H48 119.6 . . ? C48 C49 C50 119.9(2) . . ? C48 C49 H49 120.0 . . ? C50 C49 H49 120.0 . . ? C51 C50 C49 119.7(2) . . ? C51 C50 H50 120.1 . . ? C49 C50 H50 120.1 . . ? C50 C51 C52 120.4(2) . . ? C50 C51 H51 119.8 . . ? C52 C51 H51 119.8 . . ? C47 C52 C51 120.3(2) . . ? C47 C52 H52 119.8 . . ? C51 C52 H52 119.8 . . ? C58 C53 C54 119.6(2) . . ? C58 C53 Sb3 119.75(17) . . ? C54 C53 Sb3 120.54(18) . . ? C53 C54 C55 119.3(3) . . ? C53 C54 H54 120.3 . . ? C55 C54 H54 120.3 . . ? C56 C55 C54 120.9(3) . . ? C56 C55 H55 119.6 . . ? C54 C55 H55 119.6 . . ? C55 C56 C57 120.2(2) . . ? C55 C56 H56 119.9 . . ? C57 C56 H56 119.9 . . ? C56 C57 C58 119.9(3) . . ? C56 C57 H57 120.1 . . ? C58 C57 H57 120.1 . . ? C53 C58 C57 120.1(3) . . ? C53 C58 H58 119.9 . . ? C57 C58 H58 119.9 . . ? C83 B C67 112.74(16) . . ? C83 B C75 105.53(15) . . ? C67 B C75 112.20(16) . . ? C83 B C59 113.77(16) . . ? C67 B C59 101.13(15) . . ? C75 B C59 111.69(16) . . ? C64 C59 C60 116.03(18) . . ? C64 C59 B 120.68(17) . . ? C60 C59 B 122.59(17) . . ? C61 C60 C59 121.88(18) . . ? C61 C60 H60 119.1 . . ? C59 C60 H60 119.1 . . ? C60 C61 C62 121.27(18) . . ? C60 C61 C65 120.41(18) . . ? C62 C61 C65 118.27(18) . . ? C61 C62 C63 117.63(18) . . ? C61 C62 H62 121.2 . . ? C63 C62 H62 121.2 . . ? C64 C63 C62 120.92(19) . . ? C64 C63 C66 119.12(19) . . ? C62 C63 C66 119.97(19) . . ? C63 C64 C59 122.27(19) . . ? C63 C64 H64 118.9 . . ? C59 C64 H64 118.9 . . ? F65C C65 F65A 106.46(17) . . ? F65C C65 F65B 105.69(16) . . ? F65A C65 F65B 105.44(17) . . ? F65C C65 C61 113.45(18) . . ? F65A C65 C61 113.08(16) . . ? F65B C65 C61 112.07(17) . . ? F66D C66 F66A 127.9(5) . . ? F66D C66 F66B 49.4(5) . . ? F66A C66 F66B 108.5(3) . . ? F66D C66 F66E 101.5(7) . . ? F66A C66 F66E 57.9(5) . . ? F66B C66 F66E 134.5(5) . . ? F66D C66 F66F 106.2(7) . . ? F66A C66 F66F 53.0(5) . . ? F66B C66 F66F 62.0(5) . . ? F66E C66 F66F 108.6(6) . . ? F66D C66 F66C 55.1(5) . . ? F66A C66 F66C 104.3(3) . . ? F66B C66 F66C 102.8(3) . . ? F66E C66 F66C 51.1(5) . . ? F66F C66 F66C 136.5(5) . . ? F66D C66 C63 117.0(5) . . ? F66A C66 C63 115.2(2) . . ? F66B C66 C63 112.9(2) . . ? F66E C66 C63 111.7(4) . . ? F66F C66 C63 111.3(5) . . ? F66C C66 C63 112.1(2) . . ? C68 C67 C72 115.73(18) . . ? C68 C67 B 122.26(17) . . ? C72 C67 B 121.22(17) . . ? C69 C68 C67 122.27(18) . . ? C69 C68 H68 118.9 . . ? C67 C68 H68 118.9 . . ? C70 C69 C68 121.31(19) . . ? C70 C69 C73 120.6(2) . . ? C68 C69 C73 118.04(19) . . ? C69 C70 C71 117.36(19) . . ? C69 C70 H70 121.3 . . ? C71 C70 H70 121.3 . . ? C70 C71 C72 121.13(18) . . ? C70 C71 C74 120.35(18) . . ? C72 C71 C74 118.49(18) . . ? C71 C72 C67 122.18(18) . . ? C71 C72 H72 118.9 . . ? C67 C72 H72 118.9 . . ? F73C C73 F73A 106.5(2) . . ? F73C C73 F73B 106.5(3) . . ? F73A C73 F73B 106.3(2) . . ? F73C C73 C69 111.7(2) . . ? F73A C73 C69 113.7(2) . . ? F73B C73 C69 111.6(2) . . ? F74A C74 F74C 106.96(17) . . ? F74A C74 F74B 106.62(17) . . ? F74C C74 F74B 106.08(17) . . ? F74A C74 C71 112.90(17) . . ? F74C C74 C71 112.05(17) . . ? F74B C74 C71 111.80(17) . . ? C80 C75 C76 116.07(18) . . ? C80 C75 B 121.55(17) . . ? C76 C75 B 122.30(18) . . ? C77 C76 C75 122.1(2) . . ? C77 C76 H76 119.0 . . ? C75 C76 H76 119.0 . . ? C78 C77 C76 120.9(2) . . ? C78 C77 C81 120.5(2) . . ? C76 C77 C81 118.6(2) . . ? C79 C78 C77 118.19(19) . . ? C79 C78 H78 120.9 . . ? C77 C78 H78 120.9 . . ? C78 C79 C80 120.8(2) . . ? C78 C79 C82 120.3(2) . . ? C80 C79 C82 118.8(2) . . ? C79 C80 C75 121.9(2) . . ? C79 C80 H80 119.0 . . ? C75 C80 H80 119.0 . . ? F81E C81 F81D 123.5(8) . . ? F81E C81 F81B 119.7(7) . . ? F81D C81 F81B 51.4(5) . . ? F81E C81 F81A 24.1(5) . . ? F81D C81 F81A 137.7(5) . . ? F81B C81 F81A 110.3(3) . . ? F81E C81 F81C 77.1(6) . . ? F81D C81 F81C 57.9(5) . . ? F81B C81 F81C 102.7(3) . . ? F81A C81 F81C 100.8(3) . . ? F81E C81 C77 118.1(7) . . ? F81D C81 C77 109.7(5) . . ? F81B C81 C77 117.3(3) . . ? F81A C81 C77 112.2(2) . . ? F81C C81 C77 111.8(2) . . ? F81E C81 F81F 104.9(6) . . ? F81D C81 F81F 96.5(6) . . ? F81B C81 F81F 46.0(3) . . ? F81A C81 F81F 83.1(4) . . ? F81C C81 F81F 145.9(4) . . ? C77 C81 F81F 97.4(4) . . ? F82B C82 F82C 105.8(2) . . ? F82B C82 F82A 106.6(2) . . ? F82C C82 F82A 105.9(2) . . ? F82B C82 C79 112.29(19) . . ? F82C C82 C79 113.1(2) . . ? F82A C82 C79 112.7(2) . . ? C88 C83 C84 115.68(18) . . ? C88 C83 B 122.39(17) . . ? C84 C83 B 121.52(17) . . ? C85 C84 C83 122.21(19) . . ? C85 C84 H84 118.9 . . ? C83 C84 H84 118.9 . . ? C86 C85 C84 121.09(19) . . ? C86 C85 C89 119.6(2) . . ? C84 C85 C89 119.3(2) . . ? C85 C86 C87 117.93(19) . . ? C85 C86 H86 121.0 . . ? C87 C86 H86 121.0 . . ? C86 C87 C88 121.02(19) . . ? C86 C87 C90 119.91(19) . . ? C88 C87 C90 119.07(19) . . ? C87 C88 C83 122.07(19) . . ? C87 C88 H88 119.0 . . ? C83 C88 H88 119.0 . . ? F89E C89 F89B 130.7(4) . . ? F89E C89 F89D 115.6(6) . . ? F89B C89 F89D 41.4(4) . . ? F89E C89 F89A 49.6(5) . . ? F89B C89 F89A 110.2(4) . . ? F89D C89 F89A 135.4(4) . . ? F89E C89 F89C 52.0(4) . . ? F89B C89 F89C 104.9(3) . . ? F89D C89 F89C 69.3(4) . . ? F89A C89 F89C 99.1(3) . . ? F89E C89 F89F 105.1(6) . . ? F89B C89 F89F 60.4(4) . . ? F89D C89 F89F 101.0(5) . . ? F89A C89 F89F 58.1(4) . . ? F89C C89 F89F 137.8(4) . . ? F89E C89 C85 114.7(4) . . ? F89B C89 C85 114.5(2) . . ? F89D C89 C85 110.3(4) . . ? F89A C89 C85 113.7(2) . . ? F89C C89 C85 113.0(2) . . ? F89F C89 C85 108.9(4) . . ? F90F C90 F90D 106.8(12) . . ? F90F C90 F90A 65.1(10) . . ? F90D C90 F90A 126.8(9) . . ? F90F C90 F90B 42.8(9) . . ? F90D C90 F90B 72.4(9) . . ? F90A C90 F90B 106.0(2) . . ? F90F C90 F90C 128.6(9) . . ? F90D C90 F90C 34.1(8) . . ? F90A C90 F90C 107.7(3) . . ? F90B C90 F90C 104.9(2) . . ? F90F C90 F90E 105.9(12) . . ? F90D C90 F90E 98.9(11) . . ? F90A C90 F90E 44.7(8) . . ? F90B C90 F90E 136.0(8) . . ? F90C C90 F90E 68.3(8) . . ? F90F C90 C87 117.8(8) . . ? F90D C90 C87 115.5(9) . . ? F90A C90 C87 113.6(2) . . ? F90B C90 C87 112.6(2) . . ? F90C C90 C87 111.52(19) . . ? F90E C90 C87 110.0(7) . . ? Cl2 C4 Cl1 112.76(18) . . ? Cl2 C4 H4A 109.0 . . ? Cl1 C4 H4A 109.0 . . ? Cl2 C4 H4B 109.0 . . ? Cl1 C4 H4B 109.0 . . ? H4A C4 H4B 107.8 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C2 Ni Sb1 C11 80.06(9) . . . . ? C1 Ni Sb1 C11 40.30(14) . . . . ? C3 Ni Sb1 C11 64.80(9) . . . . ? Sb3 Ni Sb1 C11 -60.60(6) . . . . ? Sb2 Ni Sb1 C11 -171.61(6) . . . . ? C2 Ni Sb1 C5 -161.11(10) . . . . ? C1 Ni Sb1 C5 159.13(14) . . . . ? C3 Ni Sb1 C5 -176.37(9) . . . . ? Sb3 Ni Sb1 C5 58.23(6) . . . . ? Sb2 Ni Sb1 C5 -52.79(6) . . . . ? C2 Ni Sb1 C17 -35.07(9) . . . . ? C1 Ni Sb1 C17 -74.84(14) . . . . ? C3 Ni Sb1 C17 -50.34(9) . . . . ? Sb3 Ni Sb1 C17 -175.74(6) . . . . ? Sb2 Ni Sb1 C17 73.25(6) . . . . ? C2 Ni Sb2 C29 62.15(9) . . . . ? C1 Ni Sb2 C29 102.73(9) . . . . ? C3 Ni Sb2 C29 30.16(10) . . . . ? Sb1 Ni Sb2 C29 -61.61(6) . . . . ? Sb3 Ni Sb2 C29 -169.63(6) . . . . ? C2 Ni Sb2 C23 -173.73(8) . . . . ? C1 Ni Sb2 C23 -133.15(9) . . . . ? C3 Ni Sb2 C23 154.28(9) . . . . ? Sb1 Ni Sb2 C23 62.51(6) . . . . ? Sb3 Ni Sb2 C23 -45.50(6) . . . . ? C2 Ni Sb2 C35 -55.28(8) . . . . ? C1 Ni Sb2 C35 -14.71(8) . . . . ? C3 Ni Sb2 C35 -87.28(9) . . . . ? Sb1 Ni Sb2 C35 -179.04(6) . . . . ? Sb3 Ni Sb2 C35 72.94(6) . . . . ? C2 Ni Sb3 C53 -61.77(10) . . . . ? C1 Ni Sb3 C53 -73.34(9) . . . . ? C3 Ni Sb3 C53 -13.06(10) . . . . ? Sb1 Ni Sb3 C53 76.97(6) . . . . ? Sb2 Ni Sb3 C53 -172.81(6) . . . . ? C2 Ni Sb3 C41 170.87(10) . . . . ? C1 Ni Sb3 C41 159.29(9) . . . . ? C3 Ni Sb3 C41 -140.42(10) . . . . ? Sb1 Ni Sb3 C41 -50.39(7) . . . . ? Sb2 Ni Sb3 C41 59.82(7) . . . . ? C2 Ni Sb3 C47 48.89(9) . . . . ? C1 Ni Sb3 C47 37.32(9) . . . . ? C3 Ni Sb3 C47 97.60(9) . . . . ? Sb1 Ni Sb3 C47 -172.37(6) . . . . ? Sb2 Ni Sb3 C47 -62.15(6) . . . . ? C3 Ni C1 C2 33.43(13) . . . . ? Sb1 Ni C1 C2 59.45(19) . . . . ? Sb3 Ni C1 C2 164.95(13) . . . . ? Sb2 Ni C1 C2 -89.31(12) . . . . ? Ni C1 C2 C3 -61.47(16) . . . . ? C1 Ni C2 C3 125.98(19) . . . . ? Sb1 Ni C2 C3 -24.14(15) . . . . ? Sb3 Ni C2 C3 107.92(12) . . . . ? Sb2 Ni C2 C3 -136.68(12) . . . . ? C3 Ni C2 C1 -125.98(19) . . . . ? Sb1 Ni C2 C1 -150.12(11) . . . . ? Sb3 Ni C2 C1 -18.06(15) . . . . ? Sb2 Ni C2 C1 97.35(12) . . . . ? C1 C2 C3 Ni 60.79(16) . . . . ? C1 Ni C3 C2 -33.79(13) . . . . ? Sb1 Ni C3 C2 159.04(13) . . . . ? Sb3 Ni C3 C2 -101.01(13) . . . . ? Sb2 Ni C3 C2 55.32(14) . . . . ? C11 Sb1 C5 C6 158.60(16) . . . . ? C17 Sb1 C5 C6 -97.42(16) . . . . ? Ni Sb1 C5 C6 36.41(18) . . . . ? C11 Sb1 C5 C10 -19.76(18) . . . . ? C17 Sb1 C5 C10 84.23(18) . . . . ? Ni Sb1 C5 C10 -141.95(15) . . . . ? C10 C5 C6 C7 1.5(3) . . . . ? Sb1 C5 C6 C7 -176.90(16) . . . . ? C5 C6 C7 C8 0.2(3) . . . . ? C6 C7 C8 C9 -1.8(3) . . . . ? C7 C8 C9 C10 1.8(4) . . . . ? C8 C9 C10 C5 -0.1(4) . . . . ? C6 C5 C10 C9 -1.5(3) . . . . ? Sb1 C5 C10 C9 176.82(17) . . . . ? C5 Sb1 C11 C16 145.68(16) . . . . ? C17 Sb1 C11 C16 42.27(17) . . . . ? Ni Sb1 C11 C16 -83.67(16) . . . . ? C5 Sb1 C11 C12 -40.88(18) . . . . ? C17 Sb1 C11 C12 -144.29(17) . . . . ? Ni Sb1 C11 C12 89.77(17) . . . . ? C16 C11 C12 C13 -1.1(3) . . . . ? Sb1 C11 C12 C13 -174.47(17) . . . . ? C11 C12 C13 C14 0.9(4) . . . . ? C12 C13 C14 C15 -0.2(4) . . . . ? C13 C14 C15 C16 -0.4(4) . . . . ? C12 C11 C16 C15 0.5(3) . . . . ? Sb1 C11 C16 C15 174.01(16) . . . . ? C14 C15 C16 C11 0.3(3) . . . . ? C11 Sb1 C17 C22 -131.10(17) . . . . ? C5 Sb1 C17 C22 124.15(18) . . . . ? Ni Sb1 C17 C22 -11.73(19) . . . . ? C11 Sb1 C17 C18 52.54(17) . . . . ? C5 Sb1 C17 C18 -52.21(17) . . . . ? Ni Sb1 C17 C18 171.91(14) . . . . ? C22 C17 C18 C19 0.0(3) . . . . ? Sb1 C17 C18 C19 176.41(17) . . . . ? C17 C18 C19 C20 -0.1(4) . . . . ? C18 C19 C20 C21 0.4(4) . . . . ? C19 C20 C21 C22 -0.6(4) . . . . ? C18 C17 C22 C21 -0.2(3) . . . . ? Sb1 C17 C22 C21 -176.55(19) . . . . ? C20 C21 C22 C17 0.5(4) . . . . ? C29 Sb2 C23 C24 -2.05(18) . . . . ? C35 Sb2 C23 C24 98.85(17) . . . . ? Ni Sb2 C23 C24 -136.78(15) . . . . ? C29 Sb2 C23 C28 172.73(15) . . . . ? C35 Sb2 C23 C28 -86.36(16) . . . . ? Ni Sb2 C23 C28 38.00(17) . . . . ? C28 C23 C24 C25 0.5(3) . . . . ? Sb2 C23 C24 C25 175.22(17) . . . . ? C23 C24 C25 C26 -0.2(3) . . . . ? C24 C25 C26 C27 -0.1(3) . . . . ? C25 C26 C27 C28 0.0(3) . . . . ? C26 C27 C28 C23 0.2(3) . . . . ? C24 C23 C28 C27 -0.5(3) . . . . ? Sb2 C23 C28 C27 -175.41(15) . . . . ? C23 Sb2 C29 C30 102.90(18) . . . . ? C35 Sb2 C29 C30 0.87(19) . . . . ? Ni Sb2 C29 C30 -123.04(17) . . . . ? C23 Sb2 C29 C34 -75.07(17) . . . . ? C35 Sb2 C29 C34 -177.10(17) . . . . ? Ni Sb2 C29 C34 58.99(18) . . . . ? C34 C29 C30 C31 0.2(3) . . . . ? Sb2 C29 C30 C31 -177.76(18) . . . . ? C29 C30 C31 C32 0.2(4) . . . . ? C30 C31 C32 C33 -0.2(4) . . . . ? C31 C32 C33 C34 -0.3(4) . . . . ? C30 C29 C34 C33 -0.7(3) . . . . ? Sb2 C29 C34 C33 177.37(18) . . . . ? C32 C33 C34 C29 0.7(4) . . . . ? C29 Sb2 C35 C40 106.82(16) . . . . ? C23 Sb2 C35 C40 6.79(17) . . . . ? Ni Sb2 C35 C40 -122.98(15) . . . . ? C29 Sb2 C35 C36 -76.81(17) . . . . ? C23 Sb2 C35 C36 -176.84(16) . . . . ? Ni Sb2 C35 C36 53.38(17) . . . . ? C40 C35 C36 C37 1.0(3) . . . . ? Sb2 C35 C36 C37 -175.40(17) . . . . ? C35 C36 C37 C38 -0.2(4) . . . . ? C36 C37 C38 C39 -0.6(3) . . . . ? C37 C38 C39 C40 0.4(3) . . . . ? C36 C35 C40 C39 -1.2(3) . . . . ? Sb2 C35 C40 C39 175.20(16) . . . . ? C38 C39 C40 C35 0.5(3) . . . . ? C53 Sb3 C41 C42 -93.41(18) . . . . ? C47 Sb3 C41 C42 166.47(17) . . . . ? Ni Sb3 C41 C42 39.00(19) . . . . ? C53 Sb3 C41 C46 86.05(19) . . . . ? C47 Sb3 C41 C46 -14.06(19) . . . . ? Ni Sb3 C41 C46 -141.53(16) . . . . ? C46 C41 C42 C43 0.1(3) . . . . ? Sb3 C41 C42 C43 179.55(18) . . . . ? C41 C42 C43 C44 -0.3(4) . . . . ? C42 C43 C44 C45 0.2(4) . . . . ? C43 C44 C45 C46 0.1(4) . . . . ? C44 C45 C46 C41 -0.4(4) . . . . ? C42 C41 C46 C45 0.3(4) . . . . ? Sb3 C41 C46 C45 -179.2(2) . . . . ? C53 Sb3 C47 C52 3.50(18) . . . . ? C41 Sb3 C47 C52 106.03(17) . . . . ? Ni Sb3 C47 C52 -116.98(16) . . . . ? C53 Sb3 C47 C48 -178.70(17) . . . . ? C41 Sb3 C47 C48 -76.17(17) . . . . ? Ni Sb3 C47 C48 60.82(17) . . . . ? C52 C47 C48 C49 1.0(3) . . . . ? Sb3 C47 C48 C49 -176.84(17) . . . . ? C47 C48 C49 C50 -0.2(3) . . . . ? C48 C49 C50 C51 -0.6(3) . . . . ? C49 C50 C51 C52 0.5(3) . . . . ? C48 C47 C52 C51 -1.1(3) . . . . ? Sb3 C47 C52 C51 176.76(16) . . . . ? C50 C51 C52 C47 0.3(3) . . . . ? C41 Sb3 C53 C58 143.99(18) . . . . ? C47 Sb3 C53 C58 -115.16(18) . . . . ? Ni Sb3 C53 C58 4.0(2) . . . . ? C41 Sb3 C53 C54 -40.30(19) . . . . ? C47 Sb3 C53 C54 60.55(19) . . . . ? Ni Sb3 C53 C54 179.71(16) . . . . ? C58 C53 C54 C55 1.1(4) . . . . ? Sb3 C53 C54 C55 -174.59(19) . . . . ? C53 C54 C55 C56 -0.1(4) . . . . ? C54 C55 C56 C57 -0.8(4) . . . . ? C55 C56 C57 C58 0.6(4) . . . . ? C54 C53 C58 C57 -1.3(4) . . . . ? Sb3 C53 C58 C57 174.47(19) . . . . ? C56 C57 C58 C53 0.4(4) . . . . ? C83 B C59 C64 -159.98(17) . . . . ? C67 B C59 C64 78.9(2) . . . . ? C75 B C59 C64 -40.6(2) . . . . ? C83 B C59 C60 30.0(2) . . . . ? C67 B C59 C60 -91.1(2) . . . . ? C75 B C59 C60 149.35(18) . . . . ? C64 C59 C60 C61 0.5(3) . . . . ? B C59 C60 C61 170.98(17) . . . . ? C59 C60 C61 C62 0.2(3) . . . . ? C59 C60 C61 C65 -177.35(18) . . . . ? C60 C61 C62 C63 -0.5(3) . . . . ? C65 C61 C62 C63 177.10(18) . . . . ? C61 C62 C63 C64 0.1(3) . . . . ? C61 C62 C63 C66 -179.9(2) . . . . ? C62 C63 C64 C59 0.7(3) . . . . ? C66 C63 C64 C59 -179.4(2) . . . . ? C60 C59 C64 C63 -0.9(3) . . . . ? B C59 C64 C63 -171.58(18) . . . . ? C60 C61 C65 F65C -127.9(2) . . . . ? C62 C61 C65 F65C 54.6(2) . . . . ? C60 C61 C65 F65A -6.5(3) . . . . ? C62 C61 C65 F65A 175.93(18) . . . . ? C60 C61 C65 F65B 112.5(2) . . . . ? C62 C61 C65 F65B -65.0(2) . . . . ? C64 C63 C66 F66D 12.6(7) . . . . ? C62 C63 C66 F66D -167.5(7) . . . . ? C64 C63 C66 F66A -167.6(3) . . . . ? C62 C63 C66 F66A 12.4(4) . . . . ? C64 C63 C66 F66B -42.1(4) . . . . ? C62 C63 C66 F66B 137.9(4) . . . . ? C64 C63 C66 F66E 128.8(6) . . . . ? C62 C63 C66 F66E -51.2(6) . . . . ? C64 C63 C66 F66F -109.7(6) . . . . ? C62 C63 C66 F66F 70.3(6) . . . . ? C64 C63 C66 F66C 73.5(4) . . . . ? C62 C63 C66 F66C -106.6(3) . . . . ? C83 B C67 C68 146.81(18) . . . . ? C75 B C67 C68 27.8(3) . . . . ? C59 B C67 C68 -91.3(2) . . . . ? C83 B C67 C72 -43.9(2) . . . . ? C75 B C67 C72 -162.85(17) . . . . ? C59 B C67 C72 78.0(2) . . . . ? C72 C67 C68 C69 0.2(3) . . . . ? B C67 C68 C69 170.08(19) . . . . ? C67 C68 C69 C70 -1.2(3) . . . . ? C67 C68 C69 C73 -177.6(2) . . . . ? C68 C69 C70 C71 0.9(3) . . . . ? C73 C69 C70 C71 177.2(2) . . . . ? C69 C70 C71 C72 0.4(3) . . . . ? C69 C70 C71 C74 -177.65(19) . . . . ? C70 C71 C72 C67 -1.5(3) . . . . ? C74 C71 C72 C67 176.65(18) . . . . ? C68 C67 C72 C71 1.1(3) . . . . ? B C67 C72 C71 -168.88(18) . . . . ? C70 C69 C73 F73C 138.4(3) . . . . ? C68 C69 C73 F73C -45.2(3) . . . . ? C70 C69 C73 F73A 17.8(4) . . . . ? C68 C69 C73 F73A -165.8(2) . . . . ? C70 C69 C73 F73B -102.5(3) . . . . ? C68 C69 C73 F73B 73.9(3) . . . . ? C70 C71 C74 F74A 5.6(3) . . . . ? C72 C71 C74 F74A -172.55(18) . . . . ? C70 C71 C74 F74C -115.3(2) . . . . ? C72 C71 C74 F74C 66.6(2) . . . . ? C70 C71 C74 F74B 125.8(2) . . . . ? C72 C71 C74 F74B -52.3(2) . . . . ? C83 B C75 C80 -82.3(2) . . . . ? C67 B C75 C80 40.8(2) . . . . ? C59 B C75 C80 153.56(18) . . . . ? C83 B C75 C76 94.3(2) . . . . ? C67 B C75 C76 -142.55(19) . . . . ? C59 B C75 C76 -29.8(3) . . . . ? C80 C75 C76 C77 -1.8(3) . . . . ? B C75 C76 C77 -178.6(2) . . . . ? C75 C76 C77 C78 0.7(4) . . . . ? C75 C76 C77 C81 -178.9(2) . . . . ? C76 C77 C78 C79 0.4(3) . . . . ? C81 C77 C78 C79 180.0(2) . . . . ? C77 C78 C79 C80 -0.3(3) . . . . ? C77 C78 C79 C82 -179.6(2) . . . . ? C78 C79 C80 C75 -1.0(3) . . . . ? C82 C79 C80 C75 178.38(19) . . . . ? C76 C75 C80 C79 2.0(3) . . . . ? B C75 C80 C79 178.81(19) . . . . ? C78 C77 C81 F81E 151.3(7) . . . . ? C76 C77 C81 F81E -29.1(7) . . . . ? C78 C77 C81 F81D -59.7(6) . . . . ? C76 C77 C81 F81D 119.8(6) . . . . ? C78 C77 C81 F81B -3.8(5) . . . . ? C76 C77 C81 F81B 175.7(3) . . . . ? C78 C77 C81 F81A 125.5(3) . . . . ? C76 C77 C81 F81A -55.0(4) . . . . ? C78 C77 C81 F81C -122.0(3) . . . . ? C76 C77 C81 F81C 57.5(4) . . . . ? C78 C77 C81 F81F 40.0(4) . . . . ? C76 C77 C81 F81F -140.5(4) . . . . ? C78 C79 C82 F82B 127.4(2) . . . . ? C80 C79 C82 F82B -51.9(3) . . . . ? C78 C79 C82 F82C -112.9(2) . . . . ? C80 C79 C82 F82C 67.7(3) . . . . ? C78 C79 C82 F82A 7.1(3) . . . . ? C80 C79 C82 F82A -172.3(2) . . . . ? C67 B C83 C88 156.72(17) . . . . ? C75 B C83 C88 -80.5(2) . . . . ? C59 B C83 C88 42.3(2) . . . . ? C67 B C83 C84 -31.0(2) . . . . ? C75 B C83 C84 91.8(2) . . . . ? C59 B C83 C84 -145.43(17) . . . . ? C88 C83 C84 C85 0.2(3) . . . . ? B C83 C84 C85 -172.56(18) . . . . ? C83 C84 C85 C86 0.0(3) . . . . ? C83 C84 C85 C89 179.8(2) . . . . ? C84 C85 C86 C87 -0.3(3) . . . . ? C89 C85 C86 C87 179.8(2) . . . . ? C85 C86 C87 C88 0.5(3) . . . . ? C85 C86 C87 C90 -179.3(2) . . . . ? C86 C87 C88 C83 -0.4(3) . . . . ? C90 C87 C88 C83 179.48(19) . . . . ? C84 C83 C88 C87 0.0(3) . . . . ? B C83 C88 C87 172.68(18) . . . . ? C86 C85 C89 F89E -91.0(6) . . . . ? C84 C85 C89 F89E 89.2(6) . . . . ? C86 C85 C89 F89B 91.8(4) . . . . ? C84 C85 C89 F89B -88.1(5) . . . . ? C86 C85 C89 F89D 136.5(5) . . . . ? C84 C85 C89 F89D -43.4(5) . . . . ? C86 C85 C89 F89A -36.2(4) . . . . ? C84 C85 C89 F89A 144.0(4) . . . . ? C86 C85 C89 F89C -148.2(3) . . . . ? C84 C85 C89 F89C 32.0(4) . . . . ? C86 C85 C89 F89F 26.5(5) . . . . ? C84 C85 C89 F89F -153.4(5) . . . . ? C86 C87 C90 F90F -72.2(11) . . . . ? C88 C87 C90 F90F 108.0(11) . . . . ? C86 C87 C90 F90D 160.0(10) . . . . ? C88 C87 C90 F90D -19.8(11) . . . . ? C86 C87 C90 F90A 1.0(3) . . . . ? C88 C87 C90 F90A -178.8(3) . . . . ? C86 C87 C90 F90B -119.4(3) . . . . ? C88 C87 C90 F90B 60.7(3) . . . . ? C86 C87 C90 F90C 123.0(3) . . . . ? C88 C87 C90 F90C -56.9(3) . . . . ? C86 C87 C90 F90E 49.2(9) . . . . ? C88 C87 C90 F90E -130.7(9) . . . . ? _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 30.00 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 1.490 _refine_diff_density_min -0.913 _refine_diff_density_rms 0.093 #===END #=== Data for pv0626 (compound 2b in the text) data_pv0626 _database_code_depnum_ccdc_archive 'CCDC 703650' _audit_creation_method SHELXL-97 _chemical_name_systematic ; trihapto-allyl-bis(triphenylarsine)-nickel (II) tetrakis{3,5-bis(trifluoromethyl)phenyl}borate ; _chemical_name_common ; trihapto-allyl-bis(triphenylarsine)-nickel (ii) tetrakis(3,5- bis(trifluoromethyl)phenyl)borate ; _chemical_melting_point ? _chemical_formula_moiety 'C39 H35 As2 Ni, C32 H12 B F24' _chemical_formula_sum 'C71 H47 As2 B F24 Ni' _chemical_formula_weight 1575.45 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' As As 0.0499 2.0058 '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 triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' _symmetry_int_tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 13.038(3) _cell_length_b 14.663(3) _cell_length_c 17.637(4) _cell_angle_alpha 74.84(3) _cell_angle_beta 81.73(3) _cell_angle_gamma 88.15(3) _cell_volume 3220.4(11) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 6392 _cell_measurement_theta_min 2.373 _cell_measurement_theta_max 24.925 _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.55 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.625 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1576 _exptl_absorpt_coefficient_mu 1.434 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.736 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details 'semi-empirical from equiv.(prg.SADABS)' _exptl_special_details ; Bruker SMART APEX 3-circle diffractometer with CCD area detector, sealed X-ray tube, graphite monochromator. A hemisphere of the reciprocal space up to theta(max) = 25.03 deg was measured by omega scan frames with delta(omega) = 0.30 deg and 10 sec per frame, 1700 frames were recorded using program SMART (Bruker). Frame data evaluation and integration were done with program SAINT+(Bruker); Lattice parameters by least-squares refinement of the geometric parameters of the strongest reflections with program SAINT + (Bruker). Correction for absorption and crystal decay (insignificant) were applied by semi-empirical method from equivalents using program SADABS (G.M. Sheldrick, version of 2001, Univ. of Goettingen, Germany). Data reduction was done with program XPREP (BRUKER). ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'fine-focus sealed tube' _diffrn_source_type 'Bruker SMART APEX' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART APEX CCD area detector' _diffrn_measurement_method '1700 omega scan frames, 0.3 deg, 10 sec' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0.0002 _diffrn_reflns_number 22658 _diffrn_reflns_av_R_equivalents 0.0339 _diffrn_reflns_av_sigmaI/netI 0.0534 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.21 _diffrn_reflns_theta_max 25.03 _reflns_number_total 11163 _reflns_number_gt 10142 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT +' _computing_data_reduction 'Bruker SAINT +, SADABS, XPREP' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP-3 vers. 1.08 (L.J. Faruggia, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; 1) 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. 2) The allyl ligand was found disordered. To model it the central carbon atom in the allyl ligand was splitted in two positions being only refined anisotropically the part with s.o.f. > 0.5. 3) Two of the CF~3~ groups in the anion were totally splitted in two positions being only refined anisotropically the part with s.o.f. > 0.5. ; _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^)+(0.0341P)^2^+8.0251P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 11163 _refine_ls_number_parameters 923 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0591 _refine_ls_R_factor_gt 0.0527 _refine_ls_wR_factor_ref 0.1135 _refine_ls_wR_factor_gt 0.1072 _refine_ls_goodness_of_fit_ref 1.065 _refine_ls_restrained_S_all 1.065 _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 0.76009(4) 0.17281(4) 0.22097(3) 0.01849(13) Uani 1 1 d . . . As1 As 0.85967(3) 0.12749(3) 0.11884(2) 0.01765(11) Uani 1 1 d . B . As2 As 0.85127(3) 0.11312(3) 0.32648(2) 0.02042(11) Uani 1 1 d . B . C1 C 0.6465(3) 0.2259(3) 0.1553(3) 0.0280(10) Uani 1 1 d . B . H1A H 0.6681 0.2688 0.1022 0.034 Uiso 1 1 calc R A 1 H1B H 0.5890 0.1826 0.1571 0.034 Uiso 1 1 calc R A 1 C2A C 0.6454(5) 0.2633(6) 0.2200(4) 0.032(2) Uani 0.663(14) 1 d P B 1 H2A H 0.6654 0.3314 0.2078 0.039 Uiso 0.663(14) 1 calc PR B 1 C2B C 0.6050(9) 0.2013(10) 0.2325(7) 0.017(4) Uiso 0.337(14) 1 d P B 2 H2B H 0.5614 0.1427 0.2465 0.021 Uiso 0.337(14) 1 calc PR B 2 C3 C 0.6435(4) 0.2144(4) 0.2937(3) 0.0447(14) Uani 1 1 d . B . H3A H 0.5849 0.1697 0.3163 0.054 Uiso 1 1 calc R C 1 H3B H 0.6636 0.2481 0.3312 0.054 Uiso 1 1 calc R C 1 C4 C 0.8125(3) 0.1493(3) 0.0155(2) 0.0183(8) Uani 1 1 d . . . C5 C 0.7885(3) 0.0758(3) -0.0150(2) 0.0196(9) Uani 1 1 d . B . H5 H 0.7945 0.0121 0.0145 0.024 Uiso 1 1 calc R . . C6 C 0.7554(3) 0.0959(3) -0.0896(2) 0.0246(9) Uani 1 1 d . . . H6 H 0.7394 0.0459 -0.1111 0.030 Uiso 1 1 calc R B . C7 C 0.7459(3) 0.1887(3) -0.1319(2) 0.0273(10) Uani 1 1 d . B . H7 H 0.7225 0.2023 -0.1823 0.033 Uiso 1 1 calc R . . C8 C 0.7702(3) 0.2617(3) -0.1016(2) 0.0274(10) Uani 1 1 d . . . H8 H 0.7643 0.3253 -0.1313 0.033 Uiso 1 1 calc R B . C9 C 0.8033(3) 0.2422(3) -0.0278(2) 0.0246(9) Uani 1 1 d . B . H9 H 0.8196 0.2925 -0.0068 0.030 Uiso 1 1 calc R . . C10 C 0.9954(3) 0.1847(3) 0.0872(2) 0.0210(9) Uani 1 1 d . . . C11 C 1.0645(3) 0.1618(3) 0.0267(2) 0.0253(9) Uani 1 1 d . B . H11 H 1.0453 0.1165 0.0013 0.030 Uiso 1 1 calc R . . C12 C 1.1609(3) 0.2052(3) 0.0036(3) 0.0317(11) Uani 1 1 d . . . H12 H 1.2082 0.1894 -0.0372 0.038 Uiso 1 1 calc R B . C13 C 1.1879(3) 0.2719(3) 0.0403(3) 0.0346(11) Uani 1 1 d . B . H13 H 1.2545 0.3008 0.0253 0.042 Uiso 1 1 calc R . . C14 C 1.1191(4) 0.2965(3) 0.0984(3) 0.0346(11) Uani 1 1 d . . . H14 H 1.1372 0.3440 0.1219 0.042 Uiso 1 1 calc R B . C15 C 1.0228(3) 0.2518(3) 0.1226(2) 0.0252(9) Uani 1 1 d . B . H15 H 0.9760 0.2677 0.1636 0.030 Uiso 1 1 calc R . . C16 C 0.8758(3) -0.0085(3) 0.1496(2) 0.0198(9) Uani 1 1 d . . . C17 C 0.9701(3) -0.0538(3) 0.1484(2) 0.0222(9) Uani 1 1 d . B . H17 H 1.0327 -0.0185 0.1300 0.027 Uiso 1 1 calc R . . C18 C 0.9724(3) -0.1520(3) 0.1746(2) 0.0269(10) Uani 1 1 d . . . H18 H 1.0372 -0.1836 0.1743 0.032 Uiso 1 1 calc R B . C19 C 0.8820(4) -0.2042(3) 0.2010(3) 0.0313(10) Uani 1 1 d . B . H19 H 0.8844 -0.2712 0.2185 0.038 Uiso 1 1 calc R . . C20 C 0.7881(4) -0.1578(3) 0.2016(3) 0.0368(12) Uani 1 1 d . . . H20 H 0.7254 -0.1930 0.2195 0.044 Uiso 1 1 calc R B . C21 C 0.7849(3) -0.0611(3) 0.1765(3) 0.0312(10) Uani 1 1 d . B . H21 H 0.7200 -0.0298 0.1776 0.037 Uiso 1 1 calc R . . C22 C 0.9680(3) 0.0277(3) 0.3196(2) 0.0238(9) Uani 1 1 d . . . C23 C 0.9558(4) -0.0697(3) 0.3519(3) 0.0304(10) Uani 1 1 d . B . H23 H 0.8898 -0.0953 0.3773 0.036 Uiso 1 1 calc R . . C24 C 1.0397(4) -0.1283(3) 0.3469(3) 0.0357(11) Uani 1 1 d . . . H24 H 1.0315 -0.1946 0.3689 0.043 Uiso 1 1 calc R B . C25 C 1.1355(4) -0.0916(4) 0.3102(3) 0.0360(12) Uani 1 1 d . B . H25 H 1.1930 -0.1325 0.3070 0.043 Uiso 1 1 calc R . . C26 C 1.1481(4) 0.0048(4) 0.2779(3) 0.0345(11) Uani 1 1 d . . . H26 H 1.2142 0.0299 0.2527 0.041 Uiso 1 1 calc R B . C27 C 1.0648(3) 0.0644(3) 0.2822(2) 0.0274(10) Uani 1 1 d . B . H27 H 1.0734 0.1305 0.2596 0.033 Uiso 1 1 calc R . . C28 C 0.7587(3) 0.0381(3) 0.4155(2) 0.0255(9) Uani 1 1 d . . . C29 C 0.7616(4) 0.0410(4) 0.4932(3) 0.0353(11) Uani 1 1 d . B . H29 H 0.8102 0.0805 0.5048 0.042 Uiso 1 1 calc R . . C30 C 0.6930(4) -0.0145(4) 0.5537(3) 0.0446(13) Uani 1 1 d . . . H30 H 0.6940 -0.0123 0.6069 0.054 Uiso 1 1 calc R B . C31 C 0.6231(4) -0.0728(4) 0.5371(3) 0.0430(13) Uani 1 1 d . B . H31 H 0.5766 -0.1109 0.5790 0.052 Uiso 1 1 calc R . . C32 C 0.6207(4) -0.0759(4) 0.4607(3) 0.0451(13) Uani 1 1 d . . . H32 H 0.5726 -0.1163 0.4496 0.054 Uiso 1 1 calc R B . C33 C 0.6880(4) -0.0206(4) 0.3996(3) 0.0368(12) Uani 1 1 d . B . H33 H 0.6859 -0.0227 0.3465 0.044 Uiso 1 1 calc R . . C34 C 0.9094(3) 0.2076(3) 0.3685(2) 0.0244(9) Uani 1 1 d . . . C35 C 0.9867(4) 0.1833(3) 0.4167(2) 0.0305(10) Uani 1 1 d . B . H35 H 1.0136 0.1210 0.4281 0.037 Uiso 1 1 calc R . . C36 C 1.0240(4) 0.2508(4) 0.4480(3) 0.0396(12) Uani 1 1 d . . . H36 H 1.0779 0.2350 0.4801 0.048 Uiso 1 1 calc R B . C37 C 0.9835(4) 0.3412(4) 0.4330(3) 0.0417(13) Uani 1 1 d . B . H37 H 1.0082 0.3866 0.4560 0.050 Uiso 1 1 calc R . . C38 C 0.9078(4) 0.3652(4) 0.3851(3) 0.0431(13) Uani 1 1 d . . . H38 H 0.8809 0.4275 0.3739 0.052 Uiso 1 1 calc R B . C39 C 0.8702(4) 0.2979(3) 0.3526(3) 0.0346(11) Uani 1 1 d . B . H39 H 0.8176 0.3145 0.3194 0.042 Uiso 1 1 calc R . . F1 F 0.3597(3) 0.73564(19) 0.52728(16) 0.0483(8) Uani 1 1 d . . . F2 F 0.3654(3) 0.6826(2) 0.42542(15) 0.0530(9) Uani 1 1 d . . . F3 F 0.5026(2) 0.6914(2) 0.4746(2) 0.0544(9) Uani 1 1 d . . . F4 F 0.2441(3) 0.3574(2) 0.48265(16) 0.0538(9) Uani 1 1 d . . . F5 F 0.2442(3) 0.2644(2) 0.59783(18) 0.0564(9) Uani 1 1 d . . . F6 F 0.1307(2) 0.3721(3) 0.5784(2) 0.0657(10) Uani 1 1 d . . . F7 F 0.54691(19) 0.11091(18) 1.02948(14) 0.0315(6) Uani 1 1 d . . . F8 F 0.4465(2) 0.22660(18) 1.04299(14) 0.0345(6) Uani 1 1 d . . . F9 F 0.38253(19) 0.09463(19) 1.03934(15) 0.0365(6) Uani 1 1 d . . . F10A F 0.6024(5) 0.0305(5) 0.7673(4) 0.097(3) Uani 0.738(8) 1 d P D 1 F11A F 0.5654(9) 0.1274(3) 0.6689(3) 0.139(5) Uani 0.738(8) 1 d P D 1 F12A F 0.4549(4) 0.0331(6) 0.7419(5) 0.112(4) Uani 0.738(8) 1 d P D 1 F10B F 0.5055(11) 0.0033(8) 0.7828(6) 0.037(4) Uiso 0.262(8) 1 d P D 2 F11B F 0.6179(8) 0.0955(8) 0.7134(7) 0.027(3) Uiso 0.262(8) 1 d P D 2 F12B F 0.4728(8) 0.1048(8) 0.6865(7) 0.025(3) Uiso 0.262(8) 1 d P D 2 F13 F 0.8684(2) 0.4526(2) 0.59737(15) 0.0453(7) Uani 1 1 d . . . F14 F 0.8242(2) 0.3314(2) 0.6907(2) 0.0620(10) Uani 1 1 d . . . F15 F 0.9246(2) 0.4349(3) 0.7065(2) 0.0626(10) Uani 1 1 d . . . F16 F 0.6640(3) 0.7211(2) 0.81616(17) 0.0571(9) Uani 1 1 d . . . F17 F 0.6231(3) 0.7740(2) 0.7020(2) 0.0667(11) Uani 1 1 d . . . F18 F 0.7817(2) 0.7503(2) 0.7172(2) 0.0642(10) Uani 1 1 d . . . F19 F 0.39310(19) 0.44873(17) 1.05559(14) 0.0280(6) Uani 1 1 d . . . F20 F 0.25269(18) 0.52537(18) 1.07704(13) 0.0288(6) Uani 1 1 d . . . F21 F 0.39143(18) 0.60010(17) 1.01231(13) 0.0267(5) Uani 1 1 d . . . F22A F 0.0330(3) 0.5570(3) 0.8064(3) 0.0597(14) Uani 0.922(7) 1 d P E 1 F23A F 0.0461(2) 0.4102(3) 0.8323(3) 0.0678(16) Uani 0.922(7) 1 d P E 1 F24A F 0.0000(2) 0.4778(4) 0.9244(2) 0.079(2) Uani 0.922(7) 1 d P E 1 F22B F 0.017(2) 0.548(2) 0.867(2) 0.017(9) Uiso 0.078(7) 1 d P E 2 F23B F 0.051(2) 0.474(3) 0.7953(19) 0.026(9) Uiso 0.078(7) 1 d P E 2 F24B F 0.020(2) 0.409(2) 0.914(2) 0.024(9) Uiso 0.078(7) 1 d P E 2 C40 C 0.4056(3) 0.4575(3) 0.6718(2) 0.0171(8) Uani 1 1 d . . . C41 C 0.4254(3) 0.5456(3) 0.6174(2) 0.0200(9) Uani 1 1 d . . . H41 H 0.4693 0.5891 0.6290 0.024 Uiso 1 1 calc R . . C42 C 0.3829(3) 0.5717(3) 0.5469(2) 0.0197(9) Uani 1 1 d . . . C43 C 0.3209(3) 0.5094(3) 0.5267(2) 0.0233(9) Uani 1 1 d . . . H43 H 0.2933 0.5266 0.4780 0.028 Uiso 1 1 calc R . . C44 C 0.3001(3) 0.4216(3) 0.5791(2) 0.0239(9) Uani 1 1 d . . . C45 C 0.3412(3) 0.3974(3) 0.6502(2) 0.0197(9) Uani 1 1 d . . . H45 H 0.3245 0.3372 0.6857 0.024 Uiso 1 1 calc R . . C46 C 0.4021(3) 0.6695(3) 0.4940(2) 0.0256(10) Uani 1 1 d . . . C47 C 0.2316(4) 0.3539(3) 0.5592(3) 0.0336(11) Uani 1 1 d . . . C48 C 0.4585(3) 0.3193(3) 0.7994(2) 0.0174(8) Uani 1 1 d . . . C49 C 0.4517(3) 0.2843(3) 0.8824(2) 0.0173(8) Uani 1 1 d . . . H49 H 0.4356 0.3269 0.9148 0.021 Uiso 1 1 calc R . . C50 C 0.4676(3) 0.1902(3) 0.9183(2) 0.0190(8) Uani 1 1 d . . . C51 C 0.4906(3) 0.1250(3) 0.8743(2) 0.0225(9) Uani 1 1 d . . . H51 H 0.4997 0.0602 0.8994 0.027 Uiso 1 1 calc R . . C52 C 0.4999(3) 0.1575(3) 0.7923(2) 0.0215(9) Uani 1 1 d . D . C53 C 0.4846(3) 0.2524(3) 0.7561(2) 0.0191(8) Uani 1 1 d . . . H53 H 0.4922 0.2725 0.6999 0.023 Uiso 1 1 calc R . . C54 C 0.4606(3) 0.1572(3) 1.0070(2) 0.0227(9) Uani 1 1 d . . . C55 C 0.5281(3) 0.0891(3) 0.7431(3) 0.0272(10) Uani 1 1 d . . . C56 C 0.5621(3) 0.4826(3) 0.7462(2) 0.0173(8) Uani 1 1 d . . . C57 C 0.6512(3) 0.4352(3) 0.7217(2) 0.0192(9) Uani 1 1 d . . . H57 H 0.6439 0.3727 0.7171 0.023 Uiso 1 1 calc R . . C58 C 0.7490(3) 0.4757(3) 0.7042(2) 0.0204(9) Uani 1 1 d . . . C59 C 0.7637(3) 0.5670(3) 0.7107(2) 0.0222(9) Uani 1 1 d . . . H59 H 0.8308 0.5949 0.6992 0.027 Uiso 1 1 calc R . . C60 C 0.6773(3) 0.6159(3) 0.7345(2) 0.0206(9) Uani 1 1 d . . . C61 C 0.5793(3) 0.5734(3) 0.7524(2) 0.0191(8) Uani 1 1 d . . . H61 H 0.5218 0.6081 0.7695 0.023 Uiso 1 1 calc R . . C62 C 0.8405(3) 0.4231(3) 0.6761(2) 0.0246(9) Uani 1 1 d . . . C63 C 0.6880(3) 0.7140(3) 0.7419(3) 0.0276(10) Uani 1 1 d . . . C64 C 0.3591(3) 0.4731(3) 0.8193(2) 0.0168(8) Uani 1 1 d . . . C65 C 0.3818(3) 0.4941(3) 0.8884(2) 0.0175(8) Uani 1 1 d . . . H65 H 0.4522 0.4971 0.8958 0.021 Uiso 1 1 calc R . . C66 C 0.3046(3) 0.5104(3) 0.9464(2) 0.0180(8) Uani 1 1 d . . . C67 C 0.2005(3) 0.5088(3) 0.9381(2) 0.0202(9) Uani 1 1 d . . . H67 H 0.1479 0.5204 0.9776 0.024 Uiso 1 1 calc R . . C68 C 0.1761(3) 0.4895(3) 0.8694(2) 0.0190(8) Uani 1 1 d . E . C69 C 0.2540(3) 0.4723(3) 0.8119(2) 0.0184(8) Uani 1 1 d . . . H69 H 0.2347 0.4596 0.7657 0.022 Uiso 1 1 calc R . . C70 C 0.3346(3) 0.5216(3) 1.0224(2) 0.0216(9) Uani 1 1 d . . . C71 C 0.0655(3) 0.4818(3) 0.8595(2) 0.0250(10) Uani 1 1 d . . . B1 B 0.4474(3) 0.4341(3) 0.7585(3) 0.0175(9) 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 0.0190(3) 0.0202(3) 0.0162(3) -0.0046(2) -0.0029(2) 0.0013(2) As1 0.0175(2) 0.0190(2) 0.0160(2) -0.00371(17) -0.00249(16) 0.00084(16) As2 0.0191(2) 0.0267(2) 0.0157(2) -0.00511(18) -0.00385(16) -0.00012(17) C1 0.016(2) 0.040(3) 0.027(2) -0.008(2) -0.0030(18) 0.0093(19) C2A 0.025(4) 0.031(5) 0.039(4) -0.008(3) -0.002(3) 0.018(3) C3 0.019(2) 0.086(4) 0.033(3) -0.024(3) -0.004(2) 0.017(3) C4 0.0136(19) 0.026(2) 0.0143(19) -0.0059(17) 0.0001(15) 0.0068(16) C5 0.016(2) 0.024(2) 0.018(2) -0.0038(17) -0.0001(16) 0.0000(16) C6 0.018(2) 0.033(3) 0.025(2) -0.015(2) 0.0038(17) -0.0053(18) C7 0.023(2) 0.042(3) 0.015(2) -0.005(2) -0.0009(17) 0.002(2) C8 0.030(2) 0.030(3) 0.020(2) -0.0046(19) -0.0014(18) 0.0066(19) C9 0.029(2) 0.023(2) 0.023(2) -0.0080(19) -0.0070(18) 0.0068(18) C10 0.017(2) 0.022(2) 0.019(2) 0.0034(17) -0.0032(16) -0.0021(17) C11 0.025(2) 0.025(2) 0.025(2) -0.0024(19) -0.0051(18) -0.0008(18) C12 0.024(2) 0.036(3) 0.027(2) -0.001(2) 0.0073(19) 0.001(2) C13 0.023(2) 0.026(3) 0.049(3) 0.000(2) -0.002(2) -0.0030(19) C14 0.031(3) 0.025(3) 0.048(3) -0.007(2) -0.010(2) -0.002(2) C15 0.024(2) 0.024(2) 0.025(2) -0.0051(19) -0.0003(18) -0.0018(18) C16 0.026(2) 0.016(2) 0.017(2) -0.0038(17) -0.0016(17) 0.0003(17) C17 0.022(2) 0.023(2) 0.022(2) -0.0078(18) -0.0012(17) 0.0002(17) C18 0.026(2) 0.031(3) 0.023(2) -0.0072(19) -0.0054(18) 0.0087(19) C19 0.037(3) 0.017(2) 0.037(3) -0.002(2) -0.006(2) -0.0006(19) C20 0.027(3) 0.030(3) 0.046(3) 0.001(2) 0.003(2) -0.008(2) C21 0.023(2) 0.028(3) 0.038(3) -0.001(2) -0.002(2) -0.0006(19) C22 0.024(2) 0.032(3) 0.018(2) -0.0096(19) -0.0065(17) 0.0064(18) C23 0.035(3) 0.031(3) 0.025(2) -0.007(2) -0.0038(19) 0.004(2) C24 0.051(3) 0.027(3) 0.024(2) -0.002(2) -0.001(2) 0.009(2) C25 0.039(3) 0.046(3) 0.030(3) -0.018(2) -0.014(2) 0.021(2) C26 0.024(2) 0.050(3) 0.030(3) -0.013(2) -0.004(2) 0.004(2) C27 0.027(2) 0.031(3) 0.025(2) -0.007(2) -0.0064(19) -0.0013(19) C28 0.021(2) 0.032(3) 0.021(2) -0.0037(19) -0.0015(17) 0.0024(18) C29 0.037(3) 0.044(3) 0.026(2) -0.011(2) -0.003(2) -0.006(2) C30 0.047(3) 0.059(4) 0.025(3) -0.012(3) 0.003(2) -0.007(3) C31 0.033(3) 0.054(3) 0.032(3) 0.002(2) 0.006(2) -0.005(2) C32 0.037(3) 0.053(4) 0.039(3) 0.000(3) -0.005(2) -0.017(3) C33 0.037(3) 0.050(3) 0.023(2) -0.007(2) -0.008(2) -0.015(2) C34 0.028(2) 0.028(2) 0.018(2) -0.0067(18) 0.0016(17) -0.0060(19) C35 0.037(3) 0.033(3) 0.022(2) -0.006(2) -0.009(2) -0.004(2) C36 0.049(3) 0.049(3) 0.023(2) -0.009(2) -0.007(2) -0.010(3) C37 0.048(3) 0.049(3) 0.032(3) -0.019(2) 0.006(2) -0.020(3) C38 0.045(3) 0.032(3) 0.049(3) -0.013(2) 0.006(3) -0.001(2) C39 0.031(3) 0.037(3) 0.035(3) -0.008(2) -0.004(2) -0.003(2) F1 0.082(2) 0.0229(15) 0.0294(15) -0.0011(12) 0.0128(15) 0.0120(14) F2 0.094(3) 0.0408(18) 0.0214(14) 0.0077(13) -0.0249(15) -0.0146(16) F3 0.0360(17) 0.0364(17) 0.071(2) 0.0172(16) 0.0021(15) -0.0054(13) F4 0.084(2) 0.056(2) 0.0293(15) -0.0142(14) -0.0206(15) -0.0255(17) F5 0.091(3) 0.0282(16) 0.056(2) -0.0021(14) -0.0425(18) -0.0190(16) F6 0.0354(18) 0.081(3) 0.095(3) -0.043(2) -0.0157(18) -0.0145(17) F7 0.0287(14) 0.0376(15) 0.0226(13) 0.0026(11) -0.0066(11) 0.0085(11) F8 0.0537(17) 0.0293(15) 0.0201(13) -0.0065(11) -0.0062(12) 0.0105(12) F9 0.0308(15) 0.0419(16) 0.0268(14) 0.0066(12) 0.0022(11) -0.0096(12) F10A 0.106(5) 0.130(6) 0.110(5) -0.102(5) -0.082(4) 0.100(5) F11A 0.329(13) 0.025(3) 0.033(3) -0.006(2) 0.074(5) 0.009(5) F12A 0.029(3) 0.157(7) 0.208(9) -0.168(7) 0.021(4) -0.026(3) F13 0.0477(18) 0.0547(19) 0.0275(15) -0.0081(14) 0.0061(13) 0.0165(14) F14 0.0426(18) 0.0303(17) 0.094(3) -0.0054(17) 0.0327(17) 0.0050(14) F15 0.0297(16) 0.107(3) 0.072(2) -0.054(2) -0.0242(15) 0.0278(17) F16 0.095(3) 0.0405(18) 0.0384(17) -0.0214(15) 0.0067(17) -0.0173(17) F17 0.080(2) 0.0263(17) 0.102(3) -0.0091(18) -0.056(2) 0.0038(16) F18 0.0412(18) 0.047(2) 0.107(3) -0.039(2) 0.0243(18) -0.0249(15) F19 0.0363(14) 0.0263(14) 0.0237(13) -0.0066(11) -0.0130(11) 0.0076(11) F20 0.0270(13) 0.0419(16) 0.0191(12) -0.0132(11) 0.0013(10) -0.0017(11) F21 0.0318(14) 0.0276(14) 0.0244(13) -0.0116(11) -0.0055(10) -0.0053(11) F22A 0.036(2) 0.054(2) 0.081(3) 0.010(2) -0.033(2) 0.0011(16) F23A 0.0253(18) 0.055(3) 0.152(4) -0.071(3) -0.027(2) 0.0083(16) F24A 0.0171(17) 0.189(6) 0.037(2) -0.045(3) 0.0044(14) -0.011(2) C40 0.0160(19) 0.020(2) 0.0150(19) -0.0063(17) 0.0019(15) -0.0002(16) C41 0.018(2) 0.023(2) 0.019(2) -0.0078(18) -0.0005(16) 0.0001(17) C42 0.023(2) 0.021(2) 0.0150(19) -0.0054(17) -0.0003(16) 0.0040(17) C43 0.027(2) 0.028(2) 0.016(2) -0.0052(18) -0.0060(17) 0.0043(18) C44 0.022(2) 0.028(2) 0.023(2) -0.0092(19) -0.0055(18) -0.0010(18) C45 0.020(2) 0.021(2) 0.016(2) -0.0019(17) -0.0007(16) 0.0016(17) C46 0.032(2) 0.026(2) 0.017(2) -0.0038(18) -0.0029(18) 0.0015(19) C47 0.043(3) 0.033(3) 0.028(2) -0.006(2) -0.017(2) -0.005(2) C48 0.0113(19) 0.022(2) 0.018(2) -0.0044(17) -0.0025(15) -0.0007(16) C49 0.0130(19) 0.020(2) 0.019(2) -0.0067(17) -0.0022(16) -0.0001(16) C50 0.0140(19) 0.021(2) 0.020(2) -0.0022(17) -0.0019(16) -0.0026(16) C51 0.023(2) 0.016(2) 0.027(2) -0.0020(18) -0.0049(18) 0.0014(17) C52 0.015(2) 0.025(2) 0.026(2) -0.0096(19) -0.0031(17) 0.0000(17) C53 0.015(2) 0.024(2) 0.017(2) -0.0047(17) -0.0021(16) 0.0010(16) C54 0.023(2) 0.020(2) 0.022(2) -0.0012(18) -0.0012(17) 0.0036(17) C55 0.027(2) 0.025(2) 0.030(2) -0.006(2) -0.0052(19) -0.0043(19) C56 0.021(2) 0.019(2) 0.0101(18) -0.0001(16) -0.0026(15) -0.0011(16) C57 0.022(2) 0.021(2) 0.0130(19) -0.0015(17) -0.0043(16) -0.0012(17) C58 0.021(2) 0.027(2) 0.0123(19) -0.0020(17) -0.0034(16) 0.0031(17) C59 0.018(2) 0.030(2) 0.017(2) -0.0030(18) -0.0016(16) -0.0055(17) C60 0.021(2) 0.023(2) 0.016(2) -0.0009(17) -0.0046(16) -0.0012(17) C61 0.017(2) 0.024(2) 0.0148(19) -0.0024(17) -0.0026(16) 0.0031(17) C62 0.022(2) 0.029(3) 0.021(2) -0.0030(19) -0.0020(17) -0.0024(18) C63 0.028(2) 0.026(2) 0.028(2) -0.006(2) -0.0022(19) -0.0071(19) C64 0.021(2) 0.012(2) 0.0154(19) 0.0004(16) -0.0023(16) 0.0005(16) C65 0.016(2) 0.015(2) 0.021(2) -0.0022(16) -0.0051(16) 0.0011(15) C66 0.021(2) 0.014(2) 0.018(2) -0.0027(16) -0.0028(16) 0.0001(16) C67 0.022(2) 0.017(2) 0.020(2) -0.0043(17) 0.0009(17) 0.0035(16) C68 0.021(2) 0.014(2) 0.022(2) -0.0037(17) -0.0050(17) 0.0036(16) C69 0.022(2) 0.020(2) 0.0139(19) -0.0043(17) -0.0072(16) 0.0005(17) C70 0.019(2) 0.025(2) 0.023(2) -0.0098(18) -0.0004(17) 0.0002(17) C71 0.020(2) 0.033(3) 0.025(2) -0.013(2) -0.0012(18) 0.0029(19) B1 0.019(2) 0.019(2) 0.014(2) -0.0045(19) -0.0030(18) -0.0012(18) _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 C2A 1.965(6) . ? Ni1 C1 2.022(4) . ? Ni1 C3 2.029(5) . ? Ni1 C2B 2.044(11) . ? Ni1 As1 2.2955(9) . ? Ni1 As2 2.3150(10) . ? As1 C10 1.927(4) . ? As1 C16 1.938(4) . ? As1 C4 1.951(4) . ? As2 C28 1.941(4) . ? As2 C22 1.950(4) . ? As2 C34 1.952(4) . ? C1 C2B 1.350(12) . ? C1 C2A 1.386(8) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2A C3 1.307(8) . ? C2A H2A 1.0000 . ? C2B C3 1.313(12) . ? C2B H2B 1.0000 . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 C9 1.387(6) . ? C4 C5 1.388(6) . ? C5 C6 1.397(6) . ? C5 H5 0.9500 . ? C6 C7 1.381(6) . ? C6 H6 0.9500 . ? C7 C8 1.379(6) . ? C7 H7 0.9500 . ? C8 C9 1.385(6) . ? C8 H8 0.9500 . ? C9 H9 0.9500 . ? C10 C15 1.375(6) . ? C10 C11 1.399(6) . ? C11 C12 1.385(6) . ? C11 H11 0.9500 . ? C12 C13 1.385(7) . ? C12 H12 0.9500 . ? C13 C14 1.376(7) . ? C13 H13 0.9500 . ? C14 C15 1.393(6) . ? C14 H14 0.9500 . ? C15 H15 0.9500 . ? C16 C17 1.379(6) . ? C16 C21 1.389(6) . ? C17 C18 1.393(6) . ? C17 H17 0.9500 . ? C18 C19 1.380(6) . ? C18 H18 0.9500 . ? C19 C20 1.382(6) . ? C19 H19 0.9500 . ? C20 C21 1.371(6) . ? C20 H20 0.9500 . ? C21 H21 0.9500 . ? C22 C27 1.391(6) . ? C22 C23 1.397(6) . ? C23 C24 1.378(6) . ? C23 H23 0.9500 . ? C24 C25 1.377(7) . ? C24 H24 0.9500 . ? C25 C26 1.384(7) . ? C25 H25 0.9500 . ? C26 C27 1.378(6) . ? C26 H26 0.9500 . ? C27 H27 0.9500 . ? C28 C33 1.386(6) . ? C28 C29 1.389(6) . ? C29 C30 1.385(7) . ? C29 H29 0.9500 . ? C30 C31 1.380(7) . ? C30 H30 0.9500 . ? C31 C32 1.365(7) . ? C31 H31 0.9500 . ? C32 C33 1.381(7) . ? C32 H32 0.9500 . ? C33 H33 0.9500 . ? C34 C39 1.376(6) . ? C34 C35 1.390(6) . ? C35 C36 1.384(6) . ? C35 H35 0.9500 . ? C36 C37 1.385(7) . ? C36 H36 0.9500 . ? C37 C38 1.369(7) . ? C37 H37 0.9500 . ? C38 C39 1.396(7) . ? C38 H38 0.9500 . ? C39 H39 0.9500 . ? F1 C46 1.327(5) . ? F2 C46 1.329(5) . ? F3 C46 1.334(5) . ? F4 C47 1.324(5) . ? F5 C47 1.329(5) . ? F6 C47 1.346(6) . ? F7 C54 1.350(5) . ? F8 C54 1.329(5) . ? F9 C54 1.349(5) . ? F10A C55 1.317(6) . ? F11A C55 1.310(6) . ? F12A C55 1.286(6) . ? F10B C55 1.291(12) . ? F11B C55 1.208(11) . ? F12B C55 1.283(10) . ? F13 C62 1.341(5) . ? F14 C62 1.320(5) . ? F15 C62 1.322(5) . ? F16 C63 1.332(5) . ? F17 C63 1.336(5) . ? F18 C63 1.316(5) . ? F19 C70 1.346(5) . ? F20 C70 1.342(5) . ? F21 C70 1.348(5) . ? F22A C71 1.348(6) . ? F23A C71 1.308(5) . ? F24A C71 1.315(5) . ? F22B C71 1.16(3) . ? F23B C71 1.21(3) . ? F24B C71 1.33(3) . ? C40 C45 1.394(5) . ? C40 C41 1.399(5) . ? C40 B1 1.646(5) . ? C41 C42 1.391(5) . ? C41 H41 0.9500 . ? C42 C43 1.383(6) . ? C42 C46 1.499(6) . ? C43 C44 1.384(6) . ? C43 H43 0.9500 . ? C44 C45 1.391(5) . ? C44 C47 1.494(6) . ? C45 H45 0.9500 . ? C48 C53 1.399(5) . ? C48 C49 1.410(5) . ? C48 B1 1.659(6) . ? C49 C50 1.383(5) . ? C49 H49 0.9500 . ? C50 C51 1.380(6) . ? C50 C54 1.502(5) . ? C51 C52 1.388(6) . ? C51 H51 0.9500 . ? C52 C53 1.392(6) . ? C52 C55 1.494(6) . ? C53 H53 0.9500 . ? C56 C61 1.392(6) . ? C56 C57 1.406(6) . ? C56 B1 1.638(6) . ? C57 C58 1.383(6) . ? C57 H57 0.9500 . ? C58 C59 1.395(6) . ? C58 C62 1.495(6) . ? C59 C60 1.389(6) . ? C59 H59 0.9500 . ? C60 C61 1.397(5) . ? C60 C63 1.491(6) . ? C61 H61 0.9500 . ? C64 C69 1.396(5) . ? C64 C65 1.405(5) . ? C64 B1 1.651(6) . ? C65 C66 1.390(6) . ? C65 H65 0.9500 . ? C66 C67 1.388(5) . ? C66 C70 1.498(5) . ? C67 C68 1.395(5) . ? C67 H67 0.9500 . ? C68 C69 1.394(6) . ? C68 C71 1.488(5) . ? C69 H69 0.9500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2A Ni1 C1 40.7(2) . . ? C2A Ni1 C3 38.2(2) . . ? C1 Ni1 C3 72.54(18) . . ? C2A Ni1 C2B 29.5(4) . . ? C1 Ni1 C2B 38.8(3) . . ? C3 Ni1 C2B 37.6(3) . . ? C2A Ni1 As1 130.7(2) . . ? C1 Ni1 As1 93.55(12) . . ? C3 Ni1 As1 165.43(14) . . ? C2B Ni1 As1 127.8(3) . . ? C2A Ni1 As2 125.4(2) . . ? C1 Ni1 As2 162.99(12) . . ? C3 Ni1 As2 90.89(13) . . ? C2B Ni1 As2 124.3(3) . . ? As1 Ni1 As2 102.62(3) . . ? C10 As1 C16 108.43(17) . . ? C10 As1 C4 100.17(16) . . ? C16 As1 C4 102.56(17) . . ? C10 As1 Ni1 115.16(13) . . ? C16 As1 Ni1 108.67(12) . . ? C4 As1 Ni1 120.65(11) . . ? C28 As2 C22 101.73(18) . . ? C28 As2 C34 104.64(18) . . ? C22 As2 C34 101.68(18) . . ? C28 As2 Ni1 109.39(12) . . ? C22 As2 Ni1 122.05(12) . . ? C34 As2 Ni1 115.32(13) . . ? C2B C1 C2A 43.9(6) . . ? C2B C1 Ni1 71.5(5) . . ? C2A C1 Ni1 67.5(3) . . ? C2B C1 H1A 157.0 . . ? C2A C1 H1A 116.9 . . ? Ni1 C1 H1A 116.9 . . ? C2B C1 H1B 76.1 . . ? C2A C1 H1B 116.9 . . ? Ni1 C1 H1B 116.9 . . ? H1A C1 H1B 114.0 . . ? C3 C2A C1 125.6(7) . . ? C3 C2A Ni1 73.5(4) . . ? C1 C2A Ni1 71.9(3) . . ? C3 C2A H2A 116.3 . . ? C1 C2A H2A 116.3 . . ? Ni1 C2A H2A 116.3 . . ? C3 C2B C1 128.3(11) . . ? C3 C2B Ni1 70.6(5) . . ? C1 C2B Ni1 69.7(5) . . ? C3 C2B H2B 112.5 . . ? C1 C2B H2B 112.5 . . ? Ni1 C2B H2B 112.5 . . ? C2A C3 C2B 46.0(6) . . ? C2A C3 Ni1 68.3(3) . . ? C2B C3 Ni1 71.8(5) . . ? C2A C3 H3A 116.8 . . ? C2B C3 H3A 74.4 . . ? Ni1 C3 H3A 116.8 . . ? C2A C3 H3B 116.8 . . ? C2B C3 H3B 158.8 . . ? Ni1 C3 H3B 116.8 . . ? H3A C3 H3B 113.9 . . ? C9 C4 C5 119.9(4) . . ? C9 C4 As1 117.8(3) . . ? C5 C4 As1 122.3(3) . . ? C4 C5 C6 119.6(4) . . ? C4 C5 H5 120.2 . . ? C6 C5 H5 120.2 . . ? C7 C6 C5 119.9(4) . . ? C7 C6 H6 120.1 . . ? C5 C6 H6 120.1 . . ? C8 C7 C6 120.4(4) . . ? C8 C7 H7 119.8 . . ? C6 C7 H7 119.8 . . ? C7 C8 C9 120.0(4) . . ? C7 C8 H8 120.0 . . ? C9 C8 H8 120.0 . . ? C8 C9 C4 120.1(4) . . ? C8 C9 H9 119.9 . . ? C4 C9 H9 119.9 . . ? C15 C10 C11 119.7(4) . . ? C15 C10 As1 119.4(3) . . ? C11 C10 As1 120.9(3) . . ? C12 C11 C10 120.0(4) . . ? C12 C11 H11 120.0 . . ? C10 C11 H11 120.0 . . ? C13 C12 C11 119.7(4) . . ? C13 C12 H12 120.2 . . ? C11 C12 H12 120.2 . . ? C14 C13 C12 120.5(4) . . ? C14 C13 H13 119.8 . . ? C12 C13 H13 119.8 . . ? C13 C14 C15 119.9(4) . . ? C13 C14 H14 120.1 . . ? C15 C14 H14 120.1 . . ? C10 C15 C14 120.2(4) . . ? C10 C15 H15 119.9 . . ? C14 C15 H15 119.9 . . ? C17 C16 C21 119.8(4) . . ? C17 C16 As1 124.1(3) . . ? C21 C16 As1 116.0(3) . . ? C16 C17 C18 119.1(4) . . ? C16 C17 H17 120.4 . . ? C18 C17 H17 120.4 . . ? C19 C18 C17 121.0(4) . . ? C19 C18 H18 119.5 . . ? C17 C18 H18 119.5 . . ? C18 C19 C20 119.2(4) . . ? C18 C19 H19 120.4 . . ? C20 C19 H19 120.4 . . ? C21 C20 C19 120.3(4) . . ? C21 C20 H20 119.8 . . ? C19 C20 H20 119.8 . . ? C20 C21 C16 120.6(4) . . ? C20 C21 H21 119.7 . . ? C16 C21 H21 119.7 . . ? C27 C22 C23 119.7(4) . . ? C27 C22 As2 119.5(3) . . ? C23 C22 As2 120.9(3) . . ? C24 C23 C22 119.7(4) . . ? C24 C23 H23 120.1 . . ? C22 C23 H23 120.1 . . ? C25 C24 C23 120.4(5) . . ? C25 C24 H24 119.8 . . ? C23 C24 H24 119.8 . . ? C24 C25 C26 120.2(4) . . ? C24 C25 H25 119.9 . . ? C26 C25 H25 119.9 . . ? C27 C26 C25 120.2(4) . . ? C27 C26 H26 119.9 . . ? C25 C26 H26 119.9 . . ? C26 C27 C22 119.9(4) . . ? C26 C27 H27 120.0 . . ? C22 C27 H27 120.0 . . ? C33 C28 C29 119.7(4) . . ? C33 C28 As2 117.7(3) . . ? C29 C28 As2 122.6(3) . . ? C30 C29 C28 119.3(4) . . ? C30 C29 H29 120.4 . . ? C28 C29 H29 120.4 . . ? C31 C30 C29 120.5(5) . . ? C31 C30 H30 119.7 . . ? C29 C30 H30 119.7 . . ? C32 C31 C30 120.1(5) . . ? C32 C31 H31 119.9 . . ? C30 C31 H31 119.9 . . ? C31 C32 C33 120.2(5) . . ? C31 C32 H32 119.9 . . ? C33 C32 H32 119.9 . . ? C32 C33 C28 120.2(4) . . ? C32 C33 H33 119.9 . . ? C28 C33 H33 119.9 . . ? C39 C34 C35 120.1(4) . . ? C39 C34 As2 119.4(3) . . ? C35 C34 As2 120.5(3) . . ? C36 C35 C34 119.3(5) . . ? C36 C35 H35 120.3 . . ? C34 C35 H35 120.3 . . ? C35 C36 C37 120.6(5) . . ? C35 C36 H36 119.7 . . ? C37 C36 H36 119.7 . . ? C38 C37 C36 120.0(5) . . ? C38 C37 H37 120.0 . . ? C36 C37 H37 120.0 . . ? C37 C38 C39 120.0(5) . . ? C37 C38 H38 120.0 . . ? C39 C38 H38 120.0 . . ? C34 C39 C38 120.1(5) . . ? C34 C39 H39 120.0 . . ? C38 C39 H39 120.0 . . ? C45 C40 C41 115.4(3) . . ? C45 C40 B1 123.8(3) . . ? C41 C40 B1 120.4(3) . . ? C42 C41 C40 122.3(4) . . ? C42 C41 H41 118.9 . . ? C40 C41 H41 118.9 . . ? C43 C42 C41 120.6(4) . . ? C43 C42 C46 120.1(4) . . ? C41 C42 C46 119.2(4) . . ? C42 C43 C44 118.6(4) . . ? C42 C43 H43 120.7 . . ? C44 C43 H43 120.7 . . ? C43 C44 C45 120.1(4) . . ? C43 C44 C47 119.4(4) . . ? C45 C44 C47 120.5(4) . . ? C44 C45 C40 123.0(4) . . ? C44 C45 H45 118.5 . . ? C40 C45 H45 118.5 . . ? F1 C46 F2 106.5(4) . . ? F1 C46 F3 105.7(4) . . ? F2 C46 F3 105.4(4) . . ? F1 C46 C42 112.7(3) . . ? F2 C46 C42 113.1(4) . . ? F3 C46 C42 112.9(4) . . ? F4 C47 F5 106.8(4) . . ? F4 C47 F6 105.8(4) . . ? F5 C47 F6 105.1(4) . . ? F4 C47 C44 113.3(4) . . ? F5 C47 C44 113.7(4) . . ? F6 C47 C44 111.5(4) . . ? C53 C48 C49 115.2(4) . . ? C53 C48 B1 124.0(3) . . ? C49 C48 B1 120.5(3) . . ? C50 C49 C48 122.2(4) . . ? C50 C49 H49 118.9 . . ? C48 C49 H49 118.9 . . ? C51 C50 C49 121.5(4) . . ? C51 C50 C54 118.7(4) . . ? C49 C50 C54 119.8(4) . . ? C50 C51 C52 117.8(4) . . ? C50 C51 H51 121.1 . . ? C52 C51 H51 121.1 . . ? C51 C52 C53 120.7(4) . . ? C51 C52 C55 119.0(4) . . ? C53 C52 C55 120.3(4) . . ? C52 C53 C48 122.6(4) . . ? C52 C53 H53 118.7 . . ? C48 C53 H53 118.7 . . ? F8 C54 F9 106.9(3) . . ? F8 C54 F7 106.9(3) . . ? F9 C54 F7 105.0(3) . . ? F8 C54 C50 113.7(3) . . ? F9 C54 C50 112.1(3) . . ? F7 C54 C50 111.7(3) . . ? F11B C55 F12B 107.4(8) . . ? F11B C55 F12A 131.9(6) . . ? F12B C55 F12A 57.6(6) . . ? F11B C55 F10B 110.6(8) . . ? F12B C55 F10B 104.3(8) . . ? F12A C55 F10B 48.0(6) . . ? F11B C55 F11A 52.4(6) . . ? F12B C55 F11A 56.9(6) . . ? F12A C55 F11A 106.2(6) . . ? F10B C55 F11A 133.0(6) . . ? F11B C55 F10A 54.3(6) . . ? F12B C55 F10A 136.7(6) . . ? F12A C55 F10A 102.8(6) . . ? F10B C55 F10A 60.2(6) . . ? F11A C55 F10A 102.1(6) . . ? F11B C55 C52 112.7(6) . . ? F12B C55 C52 109.6(6) . . ? F12A C55 C52 115.3(4) . . ? F10B C55 C52 111.8(6) . . ? F11A C55 C52 115.1(4) . . ? F10A C55 C52 113.7(4) . . ? C61 C56 C57 115.2(4) . . ? C61 C56 B1 124.4(4) . . ? C57 C56 B1 120.2(3) . . ? C58 C57 C56 122.8(4) . . ? C58 C57 H57 118.6 . . ? C56 C57 H57 118.6 . . ? C57 C58 C59 120.7(4) . . ? C57 C58 C62 120.5(4) . . ? C59 C58 C62 118.7(4) . . ? C60 C59 C58 118.0(4) . . ? C60 C59 H59 121.0 . . ? C58 C59 H59 121.0 . . ? C59 C60 C61 120.3(4) . . ? C59 C60 C63 120.5(4) . . ? C61 C60 C63 119.2(4) . . ? C56 C61 C60 123.0(4) . . ? C56 C61 H61 118.5 . . ? C60 C61 H61 118.5 . . ? F14 C62 F15 107.7(4) . . ? F14 C62 F13 105.1(4) . . ? F15 C62 F13 104.6(3) . . ? F14 C62 C58 113.6(3) . . ? F15 C62 C58 113.0(4) . . ? F13 C62 C58 112.1(3) . . ? F18 C63 F16 105.9(4) . . ? F18 C63 F17 106.8(4) . . ? F16 C63 F17 103.7(4) . . ? F18 C63 C60 114.3(4) . . ? F16 C63 C60 113.1(4) . . ? F17 C63 C60 112.3(3) . . ? C69 C64 C65 115.5(3) . . ? C69 C64 B1 121.2(3) . . ? C65 C64 B1 122.5(3) . . ? C66 C65 C64 122.2(4) . . ? C66 C65 H65 118.9 . . ? C64 C65 H65 118.9 . . ? C67 C66 C65 121.5(4) . . ? C67 C66 C70 119.5(4) . . ? C65 C66 C70 118.8(3) . . ? C66 C67 C68 117.4(4) . . ? C66 C67 H67 121.3 . . ? C68 C67 H67 121.3 . . ? C69 C68 C67 120.7(4) . . ? C69 C68 C71 119.6(3) . . ? C67 C68 C71 119.6(4) . . ? C68 C69 C64 122.7(3) . . ? C68 C69 H69 118.6 . . ? C64 C69 H69 118.6 . . ? F20 C70 F19 106.6(3) . . ? F20 C70 F21 106.7(3) . . ? F19 C70 F21 105.9(3) . . ? F20 C70 C66 113.0(3) . . ? F19 C70 C66 111.2(3) . . ? F21 C70 C66 112.9(3) . . ? F22B C71 F23B 104(2) . . ? F22B C71 F23A 132.1(14) . . ? F23B C71 F23A 45.9(18) . . ? F22B C71 F24A 59.5(17) . . ? F23B C71 F24A 130.5(16) . . ? F23A C71 F24A 108.1(4) . . ? F22B C71 F24B 106(2) . . ? F23B C71 F24B 108(2) . . ? F23A C71 F24B 65.6(15) . . ? F24A C71 F24B 48.9(15) . . ? F22B C71 F22A 47.8(17) . . ? F23B C71 F22A 60.6(19) . . ? F23A C71 F22A 103.6(4) . . ? F24A C71 F22A 103.5(4) . . ? F24B C71 F22A 135.5(14) . . ? F22B C71 C68 113.1(14) . . ? F23B C71 C68 115.2(15) . . ? F23A C71 C68 113.8(4) . . ? F24A C71 C68 114.0(3) . . ? F24B C71 C68 110.6(13) . . ? F22A C71 C68 112.9(4) . . ? C56 B1 C40 108.4(3) . . ? C56 B1 C64 114.3(3) . . ? C40 B1 C64 107.1(3) . . ? C56 B1 C48 107.9(3) . . ? C40 B1 C48 113.2(3) . . ? C64 B1 C48 106.0(3) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C2A Ni1 As1 C10 101.6(4) . . . . ? C1 Ni1 As1 C10 119.97(19) . . . . ? C3 Ni1 As1 C10 137.0(7) . . . . ? C2B Ni1 As1 C10 139.8(5) . . . . ? As2 Ni1 As1 C10 -65.35(13) . . . . ? C2A Ni1 As1 C16 -136.6(3) . . . . ? C1 Ni1 As1 C16 -118.21(19) . . . . ? C3 Ni1 As1 C16 -101.2(7) . . . . ? C2B Ni1 As1 C16 -98.4(5) . . . . ? As2 Ni1 As1 C16 56.47(13) . . . . ? C2A Ni1 As1 C4 -18.8(4) . . . . ? C1 Ni1 As1 C4 -0.4(2) . . . . ? C3 Ni1 As1 C4 16.7(7) . . . . ? C2B Ni1 As1 C4 19.4(5) . . . . ? As2 Ni1 As1 C4 174.31(14) . . . . ? C2A Ni1 As2 C28 64.4(3) . . . . ? C1 Ni1 As2 C28 33.8(5) . . . . ? C3 Ni1 As2 C28 46.8(2) . . . . ? C2B Ni1 As2 C28 28.3(5) . . . . ? As1 Ni1 As2 C28 -127.74(14) . . . . ? C2A Ni1 As2 C22 -177.2(3) . . . . ? C1 Ni1 As2 C22 152.2(5) . . . . ? C3 Ni1 As2 C22 165.1(2) . . . . ? C2B Ni1 As2 C22 146.7(5) . . . . ? As1 Ni1 As2 C22 -9.40(16) . . . . ? C2A Ni1 As2 C34 -53.1(3) . . . . ? C1 Ni1 As2 C34 -83.7(5) . . . . ? C3 Ni1 As2 C34 -70.8(2) . . . . ? C2B Ni1 As2 C34 -89.2(5) . . . . ? As1 Ni1 As2 C34 114.69(14) . . . . ? C2A Ni1 C1 C2B -46.8(6) . . . . ? C3 Ni1 C1 C2B -20.8(7) . . . . ? As1 Ni1 C1 C2B 154.7(6) . . . . ? As2 Ni1 C1 C2B -7.3(9) . . . . ? C3 Ni1 C1 C2A 26.0(4) . . . . ? C2B Ni1 C1 C2A 46.8(6) . . . . ? As1 Ni1 C1 C2A -158.4(4) . . . . ? As2 Ni1 C1 C2A 39.6(7) . . . . ? C2B C1 C2A C3 33.3(8) . . . . ? Ni1 C1 C2A C3 -53.0(6) . . . . ? C2B C1 C2A Ni1 86.3(8) . . . . ? C1 Ni1 C2A C3 137.4(7) . . . . ? C2B Ni1 C2A C3 69.2(8) . . . . ? As1 Ni1 C2A C3 166.3(3) . . . . ? As2 Ni1 C2A C3 -29.4(5) . . . . ? C3 Ni1 C2A C1 -137.4(7) . . . . ? C2B Ni1 C2A C1 -68.2(8) . . . . ? As1 Ni1 C2A C1 28.9(5) . . . . ? As2 Ni1 C2A C1 -166.8(2) . . . . ? C2A C1 C2B C3 -34.5(9) . . . . ? Ni1 C1 C2B C3 42.0(10) . . . . ? C2A C1 C2B Ni1 -76.4(6) . . . . ? C2A Ni1 C2B C3 -71.3(8) . . . . ? C1 Ni1 C2B C3 -146.2(10) . . . . ? As1 Ni1 C2B C3 -178.9(4) . . . . ? As2 Ni1 C2B C3 31.2(8) . . . . ? C2A Ni1 C2B C1 75.0(8) . . . . ? C3 Ni1 C2B C1 146.2(10) . . . . ? As1 Ni1 C2B C1 -32.7(8) . . . . ? As2 Ni1 C2B C1 177.4(3) . . . . ? C1 C2A C3 C2B -33.0(8) . . . . ? Ni1 C2A C3 C2B -85.3(8) . . . . ? C1 C2A C3 Ni1 52.3(6) . . . . ? C1 C2B C3 C2A 35.4(9) . . . . ? Ni1 C2B C3 C2A 77.0(6) . . . . ? C1 C2B C3 Ni1 -41.7(10) . . . . ? C1 Ni1 C3 C2A -27.5(5) . . . . ? C2B Ni1 C3 C2A -48.9(6) . . . . ? As1 Ni1 C3 C2A -45.4(10) . . . . ? As2 Ni1 C3 C2A 156.4(5) . . . . ? C2A Ni1 C3 C2B 48.9(6) . . . . ? C1 Ni1 C3 C2B 21.4(7) . . . . ? As1 Ni1 C3 C2B 3.6(11) . . . . ? As2 Ni1 C3 C2B -154.6(7) . . . . ? C10 As1 C4 C9 -61.9(3) . . . . ? C16 As1 C4 C9 -173.5(3) . . . . ? Ni1 As1 C4 C9 65.6(3) . . . . ? C10 As1 C4 C5 118.1(3) . . . . ? C16 As1 C4 C5 6.5(4) . . . . ? Ni1 As1 C4 C5 -114.4(3) . . . . ? C9 C4 C5 C6 0.2(6) . . . . ? As1 C4 C5 C6 -179.8(3) . . . . ? C4 C5 C6 C7 -0.6(6) . . . . ? C5 C6 C7 C8 0.9(6) . . . . ? C6 C7 C8 C9 -0.7(6) . . . . ? C7 C8 C9 C4 0.4(6) . . . . ? C5 C4 C9 C8 -0.1(6) . . . . ? As1 C4 C9 C8 179.9(3) . . . . ? C16 As1 C10 C15 -125.9(3) . . . . ? C4 As1 C10 C15 127.1(3) . . . . ? Ni1 As1 C10 C15 -3.9(4) . . . . ? C16 As1 C10 C11 56.9(4) . . . . ? C4 As1 C10 C11 -50.1(4) . . . . ? Ni1 As1 C10 C11 178.9(3) . . . . ? C15 C10 C11 C12 1.4(6) . . . . ? As1 C10 C11 C12 178.6(3) . . . . ? C10 C11 C12 C13 -0.6(7) . . . . ? C11 C12 C13 C14 -1.2(7) . . . . ? C12 C13 C14 C15 2.3(7) . . . . ? C11 C10 C15 C14 -0.3(6) . . . . ? As1 C10 C15 C14 -177.5(3) . . . . ? C13 C14 C15 C10 -1.6(7) . . . . ? C10 As1 C16 C17 0.2(4) . . . . ? C4 As1 C16 C17 105.5(3) . . . . ? Ni1 As1 C16 C17 -125.7(3) . . . . ? C10 As1 C16 C21 178.1(3) . . . . ? C4 As1 C16 C21 -76.5(3) . . . . ? Ni1 As1 C16 C21 52.3(3) . . . . ? C21 C16 C17 C18 -0.2(6) . . . . ? As1 C16 C17 C18 177.7(3) . . . . ? C16 C17 C18 C19 0.5(6) . . . . ? C17 C18 C19 C20 -0.3(7) . . . . ? C18 C19 C20 C21 -0.2(7) . . . . ? C19 C20 C21 C16 0.5(7) . . . . ? C17 C16 C21 C20 -0.3(7) . . . . ? As1 C16 C21 C20 -178.4(4) . . . . ? C28 As2 C22 C27 -158.1(3) . . . . ? C34 As2 C22 C27 -50.3(4) . . . . ? Ni1 As2 C22 C27 79.9(3) . . . . ? C28 As2 C22 C23 21.8(4) . . . . ? C34 As2 C22 C23 129.6(3) . . . . ? Ni1 As2 C22 C23 -100.2(3) . . . . ? C27 C22 C23 C24 0.5(6) . . . . ? As2 C22 C23 C24 -179.5(3) . . . . ? C22 C23 C24 C25 -0.1(7) . . . . ? C23 C24 C25 C26 -0.1(7) . . . . ? C24 C25 C26 C27 -0.1(7) . . . . ? C25 C26 C27 C22 0.5(6) . . . . ? C23 C22 C27 C26 -0.7(6) . . . . ? As2 C22 C27 C26 179.2(3) . . . . ? C22 As2 C28 C33 -89.2(4) . . . . ? C34 As2 C28 C33 165.3(4) . . . . ? Ni1 As2 C28 C33 41.2(4) . . . . ? C22 As2 C28 C29 90.3(4) . . . . ? C34 As2 C28 C29 -15.2(4) . . . . ? Ni1 As2 C28 C29 -139.3(4) . . . . ? C33 C28 C29 C30 -0.6(7) . . . . ? As2 C28 C29 C30 179.9(4) . . . . ? C28 C29 C30 C31 0.8(8) . . . . ? C29 C30 C31 C32 -0.4(9) . . . . ? C30 C31 C32 C33 -0.1(9) . . . . ? C31 C32 C33 C28 0.3(8) . . . . ? C29 C28 C33 C32 0.1(8) . . . . ? As2 C28 C33 C32 179.6(4) . . . . ? C28 As2 C34 C39 -100.9(4) . . . . ? C22 As2 C34 C39 153.5(4) . . . . ? Ni1 As2 C34 C39 19.3(4) . . . . ? C28 As2 C34 C35 76.5(4) . . . . ? C22 As2 C34 C35 -29.0(4) . . . . ? Ni1 As2 C34 C35 -163.3(3) . . . . ? C39 C34 C35 C36 -0.4(7) . . . . ? As2 C34 C35 C36 -177.7(3) . . . . ? C34 C35 C36 C37 1.4(7) . . . . ? C35 C36 C37 C38 -1.8(7) . . . . ? C36 C37 C38 C39 1.2(8) . . . . ? C35 C34 C39 C38 -0.2(7) . . . . ? As2 C34 C39 C38 177.2(4) . . . . ? C37 C38 C39 C34 -0.2(7) . . . . ? C45 C40 C41 C42 0.5(6) . . . . ? B1 C40 C41 C42 -173.5(4) . . . . ? C40 C41 C42 C43 -1.8(6) . . . . ? C40 C41 C42 C46 176.1(4) . . . . ? C41 C42 C43 C44 1.5(6) . . . . ? C46 C42 C43 C44 -176.4(4) . . . . ? C42 C43 C44 C45 0.0(6) . . . . ? C42 C43 C44 C47 178.8(4) . . . . ? C43 C44 C45 C40 -1.3(6) . . . . ? C47 C44 C45 C40 179.9(4) . . . . ? C41 C40 C45 C44 1.0(6) . . . . ? B1 C40 C45 C44 174.9(4) . . . . ? C43 C42 C46 F1 112.9(4) . . . . ? C41 C42 C46 F1 -65.0(5) . . . . ? C43 C42 C46 F2 -7.9(6) . . . . ? C41 C42 C46 F2 174.2(4) . . . . ? C43 C42 C46 F3 -127.5(4) . . . . ? C41 C42 C46 F3 54.6(5) . . . . ? C43 C44 C47 F4 36.6(6) . . . . ? C45 C44 C47 F4 -144.6(4) . . . . ? C43 C44 C47 F5 158.7(4) . . . . ? C45 C44 C47 F5 -22.5(6) . . . . ? C43 C44 C47 F6 -82.6(5) . . . . ? C45 C44 C47 F6 96.2(5) . . . . ? C53 C48 C49 C50 -1.3(5) . . . . ? B1 C48 C49 C50 -175.4(3) . . . . ? C48 C49 C50 C51 -0.4(6) . . . . ? C48 C49 C50 C54 179.3(3) . . . . ? C49 C50 C51 C52 1.7(6) . . . . ? C54 C50 C51 C52 -178.0(4) . . . . ? C50 C51 C52 C53 -1.2(6) . . . . ? C50 C51 C52 C55 178.0(4) . . . . ? C51 C52 C53 C48 -0.6(6) . . . . ? C55 C52 C53 C48 -179.8(4) . . . . ? C49 C48 C53 C52 1.8(5) . . . . ? B1 C48 C53 C52 175.7(4) . . . . ? C51 C50 C54 F8 174.9(3) . . . . ? C49 C50 C54 F8 -4.8(5) . . . . ? C51 C50 C54 F9 -63.7(5) . . . . ? C49 C50 C54 F9 116.6(4) . . . . ? C51 C50 C54 F7 53.8(5) . . . . ? C49 C50 C54 F7 -125.9(4) . . . . ? C51 C52 C55 F11B -102.6(8) . . . . ? C53 C52 C55 F11B 76.5(9) . . . . ? C51 C52 C55 F12B 137.8(7) . . . . ? C53 C52 C55 F12B -43.0(8) . . . . ? C51 C52 C55 F12A 75.3(7) . . . . ? C53 C52 C55 F12A -105.5(7) . . . . ? C51 C52 C55 F10B 22.7(8) . . . . ? C53 C52 C55 F10B -158.1(7) . . . . ? C51 C52 C55 F11A -160.4(7) . . . . ? C53 C52 C55 F11A 18.8(8) . . . . ? C51 C52 C55 F10A -43.1(7) . . . . ? C53 C52 C55 F10A 136.1(6) . . . . ? C61 C56 C57 C58 -0.6(5) . . . . ? B1 C56 C57 C58 174.6(3) . . . . ? C56 C57 C58 C59 0.4(6) . . . . ? C56 C57 C58 C62 -178.2(3) . . . . ? C57 C58 C59 C60 -0.6(6) . . . . ? C62 C58 C59 C60 178.0(3) . . . . ? C58 C59 C60 C61 0.9(6) . . . . ? C58 C59 C60 C63 -179.5(4) . . . . ? C57 C56 C61 C60 1.0(5) . . . . ? B1 C56 C61 C60 -174.0(3) . . . . ? C59 C60 C61 C56 -1.2(6) . . . . ? C63 C60 C61 C56 179.3(4) . . . . ? C57 C58 C62 F14 -17.4(5) . . . . ? C59 C58 C62 F14 164.0(4) . . . . ? C57 C58 C62 F15 -140.4(4) . . . . ? C59 C58 C62 F15 40.9(5) . . . . ? C57 C58 C62 F13 101.6(4) . . . . ? C59 C58 C62 F13 -77.1(5) . . . . ? C59 C60 C63 F18 6.1(6) . . . . ? C61 C60 C63 F18 -174.4(4) . . . . ? C59 C60 C63 F16 -115.2(4) . . . . ? C61 C60 C63 F16 64.3(5) . . . . ? C59 C60 C63 F17 127.8(4) . . . . ? C61 C60 C63 F17 -52.6(5) . . . . ? C69 C64 C65 C66 1.6(6) . . . . ? B1 C64 C65 C66 -168.2(4) . . . . ? C64 C65 C66 C67 -1.3(6) . . . . ? C64 C65 C66 C70 173.2(4) . . . . ? C65 C66 C67 C68 0.4(6) . . . . ? C70 C66 C67 C68 -174.1(4) . . . . ? C66 C67 C68 C69 0.2(6) . . . . ? C66 C67 C68 C71 176.7(4) . . . . ? C67 C68 C69 C64 0.2(6) . . . . ? C71 C68 C69 C64 -176.4(4) . . . . ? C65 C64 C69 C68 -1.0(6) . . . . ? B1 C64 C69 C68 168.9(4) . . . . ? C67 C66 C70 F20 2.4(5) . . . . ? C65 C66 C70 F20 -172.3(3) . . . . ? C67 C66 C70 F19 122.2(4) . . . . ? C65 C66 C70 F19 -52.4(5) . . . . ? C67 C66 C70 F21 -118.8(4) . . . . ? C65 C66 C70 F21 66.5(5) . . . . ? C69 C68 C71 F22B -129.2(19) . . . . ? C67 C68 C71 F22B 54(2) . . . . ? C69 C68 C71 F23B -10(2) . . . . ? C67 C68 C71 F23B 173(2) . . . . ? C69 C68 C71 F23A 40.7(6) . . . . ? C67 C68 C71 F23A -135.9(5) . . . . ? C69 C68 C71 F24A 165.2(5) . . . . ? C67 C68 C71 F24A -11.4(6) . . . . ? C69 C68 C71 F24B 112.2(18) . . . . ? C67 C68 C71 F24B -64.4(18) . . . . ? C69 C68 C71 F22A -77.0(5) . . . . ? C67 C68 C71 F22A 106.4(5) . . . . ? C61 C56 B1 C40 90.8(4) . . . . ? C57 C56 B1 C40 -84.0(4) . . . . ? C61 C56 B1 C64 -28.6(5) . . . . ? C57 C56 B1 C64 156.6(3) . . . . ? C61 C56 B1 C48 -146.2(4) . . . . ? C57 C56 B1 C48 39.0(4) . . . . ? C45 C40 B1 C56 148.7(4) . . . . ? C41 C40 B1 C56 -37.8(5) . . . . ? C45 C40 B1 C64 -87.5(4) . . . . ? C41 C40 B1 C64 86.0(4) . . . . ? C45 C40 B1 C48 28.9(5) . . . . ? C41 C40 B1 C48 -157.5(3) . . . . ? C69 C64 B1 C56 152.6(3) . . . . ? C65 C64 B1 C56 -38.2(5) . . . . ? C69 C64 B1 C40 32.5(5) . . . . ? C65 C64 B1 C40 -158.3(3) . . . . ? C69 C64 B1 C48 -88.7(4) . . . . ? C65 C64 B1 C48 80.5(4) . . . . ? C53 C48 B1 C56 -87.7(4) . . . . ? C49 C48 B1 C56 85.8(4) . . . . ? C53 C48 B1 C40 32.3(5) . . . . ? C49 C48 B1 C40 -154.2(3) . . . . ? C53 C48 B1 C64 149.4(3) . . . . ? C49 C48 B1 C64 -37.0(4) . . . . ? _diffrn_measured_fraction_theta_max 0.981 _diffrn_reflns_theta_full 25.03 _diffrn_measured_fraction_theta_full 0.981 _refine_diff_density_max 0.675 _refine_diff_density_min -0.442 _refine_diff_density_rms 0.083 #===END #=== Data for pv0618 (compound 3 in the text) data_pv0618 _database_code_depnum_ccdc_archive 'CCDC 703651' _audit_creation_method SHELXL-97 _chemical_name_systematic ; (\h^3^-allyl)-bis(triphenylphosphine)-nickel (II) tetrakis(3,5-bis(trifluoromethyl)phenyl)borate and (\h^3^-allyl)-(triphenylstibine)-(triphenylphosphine)-nickel (II) tetrakis(3,5-bis(trifluoromethyl)phenyl)borate ; _chemical_name_common ; (eta$3!-allyl)-bis(triphenylphosphine)-nickel (ii) tetrakis(3,5-bis(trifluoromethyl)phenyl)borate and (eta$3!-allyl)- (triphenylstibine)-(triphenylphosphine)-nickel (ii) tetrakis(3,5- bis(trifluoromethyl)phenyl)borate ; _chemical_melting_point ? _chemical_formula_moiety 'C39 H35 Ni P1.54 Sb0.46, C32 H12 B F24' _chemical_formula_sum 'C71 H47 B F24 Ni P1.54 Sb0.46' _chemical_formula_weight 1529.56 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' 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' Sb Sb -0.5866 1.5461 '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' _symmetry_int_tables_number 2 _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 13.093(3) _cell_length_b 14.560(3) _cell_length_c 17.565(4) _cell_angle_alpha 75.09(3) _cell_angle_beta 81.42(3) _cell_angle_gamma 88.28(3) _cell_volume 3199.4(13) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 2983 _cell_measurement_theta_min 2.379 _cell_measurement_theta_max 20.968 _exptl_crystal_description needle _exptl_crystal_colour yellow _exptl_crystal_size_max 0.47 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.588 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1537.3 _exptl_absorpt_coefficient_mu 0.647 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.908 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details '(SADABS; Sheldrick, 2004)' _exptl_special_details ; Bruker SMART APEX 3-circle diffractometer with CCD area detector, sealed X-ray tube, graphite monochromator. A hemisphere of the reciprocal space up to theta(max) = 23.26 deg was measured by omega scan frames with delta(omega) = 0.30 deg and 10 sec per frame, 1700 frames were recorded using program SMART (Bruker). Frame data evaluation and integration were done with program SAINT+(Bruker); Lattice parameters by least-squares refinement of the geometric parameters of the strongest reflections with program SAINT + (Bruker). Correction for absorption and crystal decay (insignificant) were applied by semi-empirical method from equivalents using program SADABS (G.M. Sheldrick, version of 2001, Univ. of Goettingen, Germany). Data reduction was done with program XPREP (BRUKER). ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'sealed X-ray tube' _diffrn_source_type 'Bruker SMART APEX' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART APEX CCD area detector' _diffrn_measurement_method '1700 omega scan frames, 0.3 deg, 10 sec' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0.0032 _diffrn_reflns_number 19259 _diffrn_reflns_av_R_equivalents 0.0483 _diffrn_reflns_av_sigmaI/netI 0.0756 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.45 _diffrn_reflns_theta_max 23.26 _reflns_number_total 9068 _reflns_number_gt 7736 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2001)' _computing_cell_refinement 'SAINT (Bruker, 2001)' _computing_data_reduction 'SAINT (Bruker, 2001)' _computing_structure_solution 'SHELXTL (Sheldrick, 2001)' _computing_structure_refinement 'SHELXTL (Sheldrick, 2001)' _computing_molecular_graphics 'ORTEP-3 vers. 1.08 (Faruggia, 2005)' _computing_publication_material 'SHELXTL (Sheldrick, 2001)' _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^)+(0.0295P)^2^+18.7721P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9068 _refine_ls_number_parameters 904 _refine_ls_number_restraints 8 _refine_ls_R_factor_all 0.0937 _refine_ls_R_factor_gt 0.0772 _refine_ls_wR_factor_ref 0.1535 _refine_ls_wR_factor_gt 0.1448 _refine_ls_goodness_of_fit_ref 1.076 _refine_ls_restrained_S_all 1.077 _refine_ls_shift/su_max 0.073 _refine_ls_shift/su_mean 0.002 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ni1 Ni 0.26541(7) 0.17143(6) 0.21487(5) 0.0259(3) Uani 1 1 d D . . Sb1 Sb 0.3557(8) 0.1112(8) 0.3244(5) 0.0161(7) Uani 0.463(3) 1 d PD A 1 P2 P 0.348(3) 0.113(3) 0.3163(19) 0.0161(7) Uani 0.537(3) 1 d PD A 2 P1 P 0.36181(12) 0.12700(11) 0.11768(9) 0.0141(4) Uani 1 1 d . A . C1 C 0.1520(5) 0.2245(5) 0.1511(4) 0.0359(18) Uani 1 1 d . A . H1A H 0.1730 0.2668 0.0974 0.043 Uiso 1 1 calc R B 1 H1B H 0.0937 0.1813 0.1543 0.043 Uiso 1 1 calc R B 1 C2A C 0.1532(12) 0.2638(12) 0.2158(7) 0.029(5) Uani 0.60(3) 1 d P A 1 H2A H 0.1734 0.3323 0.2035 0.035 Uiso 0.60(3) 1 calc PR A 1 C2B C 0.1116(16) 0.204(2) 0.2253(12) 0.033(8) Uani 0.40(3) 1 d P A 2 H2B H 0.0684 0.1453 0.2392 0.040 Uiso 0.40(3) 1 calc PR A 2 C3 C 0.1493(6) 0.2147(7) 0.2891(5) 0.049(2) Uani 1 1 d . A . H3A H 0.0897 0.1709 0.3113 0.059 Uiso 1 1 calc R C 1 H3B H 0.1700 0.2477 0.3272 0.059 Uiso 1 1 calc R C 1 C4 C 0.4718(6) 0.0244(5) 0.3182(4) 0.0326(18) Uani 1 1 d . . . C5 C 0.4604(6) -0.0733(5) 0.3513(4) 0.0365(19) Uani 1 1 d . A . H5 H 0.3944 -0.0987 0.3768 0.044 Uiso 1 1 calc R . . C6 C 0.5422(6) -0.1330(6) 0.3478(4) 0.043(2) Uani 1 1 d . . . H6 H 0.5328 -0.1994 0.3707 0.051 Uiso 1 1 calc R A . C7 C 0.6389(7) -0.0974(6) 0.3112(4) 0.047(2) Uani 1 1 d . A . H7 H 0.6959 -0.1390 0.3091 0.057 Uiso 1 1 calc R . . C8 C 0.6522(7) -0.0010(7) 0.2776(5) 0.050(2) Uani 1 1 d . . . H8 H 0.7186 0.0235 0.2521 0.060 Uiso 1 1 calc R A . C9 C 0.5707(6) 0.0594(6) 0.2806(4) 0.0388(19) Uani 1 1 d . A . H9 H 0.5808 0.1256 0.2572 0.047 Uiso 1 1 calc R . . C10 C 0.2598(6) 0.0370(5) 0.4141(4) 0.0347(18) Uani 1 1 d . . . C11 C 0.2624(6) 0.0373(6) 0.4915(4) 0.041(2) Uani 1 1 d . A . H11 H 0.3120 0.0761 0.5032 0.049 Uiso 1 1 calc R . . C12 C 0.1949(7) -0.0172(7) 0.5528(5) 0.057(3) Uani 1 1 d . . . H12 H 0.1976 -0.0160 0.6063 0.069 Uiso 1 1 calc R A . C13 C 0.1232(6) -0.0736(6) 0.5359(5) 0.052(2) Uani 1 1 d . A . H13 H 0.0752 -0.1104 0.5778 0.063 Uiso 1 1 calc R . . C14 C 0.1210(7) -0.0768(6) 0.4596(5) 0.058(2) Uani 1 1 d . . . H14 H 0.0728 -0.1172 0.4482 0.069 Uiso 1 1 calc R A . C15 C 0.1888(6) -0.0213(6) 0.3986(5) 0.045(2) Uani 1 1 d . A . H15 H 0.1865 -0.0233 0.3453 0.054 Uiso 1 1 calc R . . C16 C 0.4110(5) 0.2081(5) 0.3663(4) 0.0310(17) Uani 1 1 d . . . C17 C 0.4886(6) 0.1849(5) 0.4139(4) 0.0357(18) Uani 1 1 d . A . H17 H 0.5163 0.1226 0.4242 0.043 Uiso 1 1 calc R . . C18 C 0.5259(7) 0.2520(6) 0.4463(4) 0.045(2) Uani 1 1 d . . . H18 H 0.5800 0.2359 0.4778 0.054 Uiso 1 1 calc R A . C19 C 0.4854(7) 0.3415(6) 0.4332(5) 0.049(2) Uani 1 1 d . A . H19 H 0.5094 0.3865 0.4572 0.058 Uiso 1 1 calc R . . C20 C 0.4096(7) 0.3663(6) 0.3849(6) 0.061(3) Uani 1 1 d . . . H20 H 0.3828 0.4290 0.3743 0.074 Uiso 1 1 calc R A . C21 C 0.3727(6) 0.2992(6) 0.3522(5) 0.051(2) Uani 1 1 d . A . H21 H 0.3201 0.3163 0.3194 0.061 Uiso 1 1 calc R . . C22 C 0.4897(5) 0.1812(4) 0.0888(4) 0.0219(15) Uani 1 1 d . . . C23 C 0.5171(5) 0.2496(5) 0.1251(4) 0.0272(16) Uani 1 1 d . A . H23 H 0.4694 0.2663 0.1655 0.033 Uiso 1 1 calc R . . C24 C 0.6132(5) 0.2933(5) 0.1027(5) 0.0366(19) Uani 1 1 d . . . H24 H 0.6312 0.3404 0.1272 0.044 Uiso 1 1 calc R A . C25 C 0.6827(5) 0.2682(5) 0.0447(5) 0.0359(19) Uani 1 1 d . A . H25 H 0.7494 0.2969 0.0303 0.043 Uiso 1 1 calc R . . C26 C 0.6566(5) 0.2023(5) 0.0076(4) 0.0315(17) Uani 1 1 d . . . H26 H 0.7046 0.1857 -0.0328 0.038 Uiso 1 1 calc R A . C27 C 0.5608(5) 0.1602(5) 0.0290(4) 0.0250(16) Uani 1 1 d . A . H27 H 0.5426 0.1155 0.0022 0.030 Uiso 1 1 calc R . . C28 C 0.3747(5) -0.0019(5) 0.1477(4) 0.0219(15) Uani 1 1 d . . . C29 C 0.4676(5) -0.0503(5) 0.1475(4) 0.0239(16) Uani 1 1 d . A . H29 H 0.5310 -0.0162 0.1290 0.029 Uiso 1 1 calc R . . C30 C 0.4676(5) -0.1486(5) 0.1745(4) 0.0295(17) Uani 1 1 d . . . H30 H 0.5310 -0.1820 0.1749 0.035 Uiso 1 1 calc R A . C31 C 0.3761(5) -0.1974(5) 0.2007(4) 0.0331(18) Uani 1 1 d . A . H31 H 0.3762 -0.2648 0.2182 0.040 Uiso 1 1 calc R . . C32 C 0.2840(6) -0.1498(5) 0.2019(4) 0.0381(19) Uani 1 1 d . . . H32 H 0.2209 -0.1844 0.2204 0.046 Uiso 1 1 calc R A . C33 C 0.2827(5) -0.0532(5) 0.1769(4) 0.0296(17) Uani 1 1 d . A . H33 H 0.2188 -0.0207 0.1793 0.036 Uiso 1 1 calc R . . C34 C 0.3176(5) 0.1478(5) 0.0193(4) 0.0211(15) Uani 1 1 d . . . C35 C 0.2905(5) 0.0763(5) -0.0119(4) 0.0236(15) Uani 1 1 d . A . H35 H 0.2940 0.0120 0.0177 0.028 Uiso 1 1 calc R . . C36 C 0.2580(5) 0.0965(5) -0.0860(4) 0.0264(16) Uani 1 1 d . . . H36 H 0.2401 0.0464 -0.1073 0.032 Uiso 1 1 calc R A . C37 C 0.2517(5) 0.1897(5) -0.1286(4) 0.0287(17) Uani 1 1 d . A . H37 H 0.2282 0.2040 -0.1789 0.034 Uiso 1 1 calc R . . C38 C 0.2792(6) 0.2621(5) -0.0984(4) 0.0318(17) Uani 1 1 d . . . H38 H 0.2759 0.3262 -0.1283 0.038 Uiso 1 1 calc R A . C39 C 0.3115(5) 0.2415(5) -0.0251(4) 0.0271(16) Uani 1 1 d . A . H39 H 0.3300 0.2918 -0.0044 0.033 Uiso 1 1 calc R . . F1A F -0.1089(8) 0.8784(7) 0.3170(6) 0.0569(12) Uani 0.548(7) 1 d PD D 1 F2A F -0.0693(8) 0.9931(7) 0.2184(6) 0.0569(12) Uani 0.548(7) 1 d PD D 1 F3A F 0.0463(7) 0.9310(7) 0.2885(6) 0.0569(12) Uani 0.548(7) 1 d PD D 1 F1B F -0.1166(10) 0.9609(9) 0.2392(7) 0.0569(12) Uani 0.452(7) 1 d PD D 2 F2B F 0.0402(9) 0.9802(9) 0.2473(8) 0.0569(12) Uani 0.452(7) 1 d PD D 2 F3B F -0.0541(10) 0.8732(8) 0.3368(7) 0.0569(12) Uani 0.452(7) 1 d PD D 2 F4 F -0.0454(3) 0.8899(3) -0.0297(2) 0.0325(10) Uani 1 1 d . . . F5 F 0.0534(3) 0.7733(3) -0.0431(2) 0.0369(10) Uani 1 1 d . . . F6 F 0.1187(3) 0.9044(3) -0.0381(2) 0.0391(11) Uani 1 1 d . . . F7 F -0.1686(5) 0.2760(3) 0.1834(3) 0.0717(17) Uani 1 1 d . . . F8 F -0.1139(4) 0.2235(3) 0.2913(4) 0.0728(17) Uani 1 1 d . . . F9 F -0.2743(4) 0.2411(3) 0.2892(3) 0.0698(17) Uani 1 1 d . . . F10 F -0.3655(3) 0.5471(3) 0.4025(2) 0.0427(11) Uani 1 1 d . . . F11 F -0.3260(3) 0.6659(3) 0.3053(3) 0.0559(14) Uani 1 1 d . . . F12 F -0.4240(3) 0.5573(4) 0.2950(3) 0.0560(14) Uani 1 1 d . . . F13 F 0.2480(3) 0.4785(3) -0.0797(2) 0.0300(9) Uani 1 1 d . . . F14 F 0.1066(3) 0.5524(3) -0.0563(2) 0.0304(9) Uani 1 1 d . . . F15 F 0.1118(3) 0.4006(2) -0.0146(2) 0.0277(9) Uani 1 1 d . . . F16 F 0.4517(3) 0.5913(4) 0.1695(3) 0.0669(16) Uani 1 1 d . . . F17 F 0.4980(3) 0.5328(6) 0.0731(3) 0.104(3) Uani 1 1 d . . . F18 F 0.4663(4) 0.4456(4) 0.1887(4) 0.0774(18) Uani 1 1 d . . . F19 F 0.2543(4) 0.6454(3) 0.5163(2) 0.0577(14) Uani 1 1 d . . . F20 F 0.3678(4) 0.6300(4) 0.4209(3) 0.0721(16) Uani 1 1 d . . . F21 F 0.2542(4) 0.7380(3) 0.4010(3) 0.0604(15) Uani 1 1 d . . . F22 F 0.1400(4) 0.2638(3) 0.4701(2) 0.0541(13) Uani 1 1 d . . . F23 F 0.0005(3) 0.3083(3) 0.5279(3) 0.0525(13) Uani 1 1 d . . . F24 F 0.1411(4) 0.3163(3) 0.5724(2) 0.0552(14) Uani 1 1 d . . . C40 C 0.0396(4) 0.6804(4) 0.2010(3) 0.0165(14) Uani 1 1 d . . . C41 C 0.0128(4) 0.7474(4) 0.2448(4) 0.0199(15) Uani 1 1 d . . . H41 H 0.0058 0.7273 0.3012 0.024 Uiso 1 1 calc R . . C42 C -0.0041(5) 0.8433(4) 0.2086(4) 0.0199(14) Uani 1 1 d . D . C43 C 0.0064(5) 0.8752(4) 0.1276(4) 0.0205(15) Uani 1 1 d . . . H43 H -0.0033 0.9404 0.1029 0.025 Uiso 1 1 calc R . . C44 C 0.0315(5) 0.8099(4) 0.0816(4) 0.0197(14) Uani 1 1 d . . . C45 C 0.0483(4) 0.7161(4) 0.1184(3) 0.0193(14) Uani 1 1 d . . . H45 H 0.0668 0.6735 0.0859 0.023 Uiso 1 1 calc R . . C46 C -0.0311(5) 0.9094(5) 0.2578(4) 0.0244(15) Uani 1 1 d D . . C47 C 0.0398(5) 0.8432(4) -0.0065(4) 0.0234(15) Uani 1 1 d . . . C48 C -0.0615(4) 0.5159(4) 0.2540(3) 0.0149(13) Uani 1 1 d . . . C49 C -0.0773(5) 0.4242(4) 0.2481(3) 0.0189(14) Uani 1 1 d . . . H49 H -0.0192 0.3896 0.2315 0.023 Uiso 1 1 calc R . . C50 C -0.1742(5) 0.3805(4) 0.2653(3) 0.0194(15) Uani 1 1 d . . . C51 C -0.2602(5) 0.4281(5) 0.2887(3) 0.0237(16) Uani 1 1 d . . . H51 H -0.3265 0.3989 0.2998 0.028 Uiso 1 1 calc R . . C52 C -0.2483(5) 0.5208(5) 0.2959(3) 0.0212(15) Uani 1 1 d . . . C53 C -0.1513(5) 0.5618(4) 0.2780(3) 0.0174(14) Uani 1 1 d . . . H53 H -0.1450 0.6250 0.2823 0.021 Uiso 1 1 calc R . . C54 C -0.1834(5) 0.2820(5) 0.2582(4) 0.0290(17) Uani 1 1 d . . . C55 C -0.3397(5) 0.5727(5) 0.3231(4) 0.0239(16) Uani 1 1 d . . . C56 C 0.1404(5) 0.5275(4) 0.1803(3) 0.0142(13) Uani 1 1 d . . . C57 C 0.1191(5) 0.5061(4) 0.1110(3) 0.0171(14) Uani 1 1 d . . . H57 H 0.0490 0.5016 0.1041 0.020 Uiso 1 1 calc R . . C58 C 0.1965(5) 0.4912(4) 0.0517(3) 0.0175(14) Uani 1 1 d . . . C59 C 0.2989(5) 0.4944(4) 0.0603(4) 0.0189(14) Uani 1 1 d . . . H59 H 0.3517 0.4843 0.0200 0.023 Uiso 1 1 calc R . . C60 C 0.3232(5) 0.5129(4) 0.1291(4) 0.0202(15) Uani 1 1 d . . . C61 C 0.2458(5) 0.5293(4) 0.1870(3) 0.0180(14) Uani 1 1 d . . . H61 H 0.2649 0.5423 0.2333 0.022 Uiso 1 1 calc R . . C62 C 0.1663(5) 0.4800(5) -0.0237(4) 0.0233(15) Uani 1 1 d . . . C63 C 0.4342(5) 0.5216(5) 0.1388(4) 0.0262(16) Uani 1 1 d . . . C64 C 0.0936(5) 0.5425(4) 0.3279(3) 0.0169(14) Uani 1 1 d . . . C65 C 0.0756(5) 0.4537(4) 0.3828(3) 0.0194(14) Uani 1 1 d . . . H65 H 0.0323 0.4092 0.3713 0.023 Uiso 1 1 calc R . . C66 C 0.1180(5) 0.4278(5) 0.4527(3) 0.0218(15) Uani 1 1 d . . . C67 C 0.1797(5) 0.4909(5) 0.4728(4) 0.0230(15) Uani 1 1 d . . . H67 H 0.2082 0.4735 0.5211 0.028 Uiso 1 1 calc R . . C68 C 0.1993(5) 0.5809(4) 0.4200(4) 0.0220(15) Uani 1 1 d . . . C69 C 0.1576(5) 0.6038(4) 0.3500(4) 0.0213(15) Uani 1 1 d . . . H69 H 0.1731 0.6647 0.3146 0.026 Uiso 1 1 calc R . . C70 C 0.2678(6) 0.6479(5) 0.4397(4) 0.0353(19) Uani 1 1 d . . . C71 C 0.1007(5) 0.3297(5) 0.5053(4) 0.0256(16) Uani 1 1 d . . . B1 B 0.0525(5) 0.5652(5) 0.2413(4) 0.0176(16) 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 0.0237(5) 0.0214(5) 0.0314(5) -0.0084(4) 0.0039(4) -0.0034(4) Sb1 0.0151(17) 0.0221(6) 0.013(2) -0.0043(14) -0.0073(10) -0.0009(10) P2 0.0151(17) 0.0221(6) 0.013(2) -0.0043(14) -0.0073(10) -0.0009(10) P1 0.0129(8) 0.0124(9) 0.0166(8) -0.0043(6) 0.0007(6) -0.0018(7) C1 0.024(4) 0.041(5) 0.042(5) -0.015(4) 0.006(3) 0.000(3) C2A 0.035(9) 0.019(9) 0.032(8) -0.008(6) 0.000(6) 0.005(7) C2B 0.012(11) 0.045(19) 0.047(14) -0.021(11) -0.005(9) 0.009(11) C3 0.022(4) 0.080(7) 0.055(6) -0.035(5) -0.003(4) 0.012(4) C4 0.041(5) 0.041(5) 0.018(4) -0.008(3) -0.009(3) -0.009(4) C5 0.043(5) 0.035(5) 0.033(4) -0.013(4) 0.002(4) -0.008(4) C6 0.055(6) 0.034(5) 0.037(5) -0.010(4) 0.001(4) 0.001(4) C7 0.050(6) 0.063(6) 0.035(5) -0.022(4) -0.008(4) 0.007(5) C8 0.042(5) 0.073(7) 0.040(5) -0.022(5) -0.006(4) -0.011(5) C9 0.042(5) 0.043(5) 0.033(4) -0.010(4) -0.007(4) -0.014(4) C10 0.041(5) 0.030(4) 0.041(5) -0.016(3) -0.017(4) 0.011(4) C11 0.037(5) 0.055(5) 0.035(5) -0.022(4) -0.002(4) -0.004(4) C12 0.052(6) 0.086(7) 0.038(5) -0.025(5) 0.003(4) -0.012(5) C13 0.043(5) 0.062(6) 0.045(5) -0.006(4) 0.006(4) -0.008(5) C14 0.057(6) 0.052(6) 0.066(6) -0.008(5) -0.025(5) -0.014(5) C15 0.054(5) 0.046(5) 0.040(5) -0.005(4) -0.026(4) -0.011(4) C16 0.034(4) 0.033(5) 0.020(4) 0.000(3) 0.002(3) -0.007(4) C17 0.053(5) 0.026(4) 0.029(4) -0.005(3) -0.011(4) -0.001(4) C18 0.062(6) 0.042(5) 0.034(5) -0.010(4) -0.009(4) -0.008(4) C19 0.045(5) 0.047(6) 0.054(5) -0.023(4) 0.014(4) -0.018(4) C20 0.038(5) 0.026(5) 0.111(8) -0.012(5) 0.009(5) -0.005(4) C21 0.028(5) 0.034(5) 0.082(7) 0.005(4) -0.009(4) -0.006(4) C22 0.020(4) 0.019(4) 0.025(4) -0.002(3) -0.004(3) -0.002(3) C23 0.027(4) 0.027(4) 0.025(4) -0.007(3) 0.002(3) 0.000(3) C24 0.029(4) 0.024(4) 0.056(5) -0.008(4) -0.008(4) -0.005(3) C25 0.021(4) 0.026(4) 0.056(5) 0.000(4) -0.005(4) -0.007(3) C26 0.026(4) 0.028(4) 0.034(4) -0.002(3) 0.005(3) -0.003(3) C27 0.027(4) 0.023(4) 0.028(4) -0.008(3) -0.012(3) 0.002(3) C28 0.025(4) 0.024(4) 0.017(3) -0.005(3) -0.003(3) -0.006(3) C29 0.021(4) 0.029(4) 0.024(4) -0.011(3) -0.002(3) -0.008(3) C30 0.028(4) 0.034(5) 0.029(4) -0.014(3) -0.002(3) 0.008(3) C31 0.034(5) 0.027(4) 0.032(4) 0.000(3) 0.001(3) -0.007(4) C32 0.025(4) 0.037(5) 0.043(5) 0.002(4) 0.000(3) -0.005(4) C33 0.019(4) 0.024(4) 0.039(4) 0.000(3) 0.001(3) 0.000(3) C34 0.012(3) 0.030(4) 0.023(4) -0.012(3) 0.000(3) 0.005(3) C35 0.020(4) 0.020(4) 0.029(4) -0.004(3) -0.003(3) 0.000(3) C36 0.025(4) 0.030(4) 0.026(4) -0.009(3) -0.002(3) -0.005(3) C37 0.020(4) 0.044(5) 0.019(4) -0.007(3) 0.002(3) 0.004(3) C38 0.043(5) 0.023(4) 0.029(4) -0.006(3) -0.006(3) 0.007(3) C39 0.040(4) 0.020(4) 0.022(4) -0.008(3) -0.002(3) 0.003(3) F1A 0.062(3) 0.051(3) 0.069(3) -0.043(2) -0.001(3) 0.002(3) F2A 0.062(3) 0.051(3) 0.069(3) -0.043(2) -0.001(3) 0.002(3) F3A 0.062(3) 0.051(3) 0.069(3) -0.043(2) -0.001(3) 0.002(3) F1B 0.062(3) 0.051(3) 0.069(3) -0.043(2) -0.001(3) 0.002(3) F2B 0.062(3) 0.051(3) 0.069(3) -0.043(2) -0.001(3) 0.002(3) F3B 0.062(3) 0.051(3) 0.069(3) -0.043(2) -0.001(3) 0.002(3) F4 0.031(2) 0.035(2) 0.029(2) 0.0006(18) -0.0128(18) 0.0092(19) F5 0.060(3) 0.028(2) 0.022(2) -0.0043(17) -0.0077(19) 0.008(2) F6 0.031(2) 0.043(3) 0.031(2) 0.0110(19) 0.0016(18) -0.011(2) F7 0.127(5) 0.050(3) 0.040(3) -0.023(2) 0.007(3) -0.028(3) F8 0.070(4) 0.025(3) 0.133(5) -0.014(3) -0.055(4) 0.004(3) F9 0.044(3) 0.043(3) 0.119(5) -0.036(3) 0.031(3) -0.027(2) F10 0.039(3) 0.057(3) 0.027(2) -0.010(2) 0.0047(19) 0.014(2) F11 0.040(3) 0.027(3) 0.083(4) 0.000(2) 0.023(2) 0.005(2) F12 0.026(2) 0.092(4) 0.067(3) -0.045(3) -0.022(2) 0.021(2) F13 0.024(2) 0.045(3) 0.022(2) -0.0145(18) 0.0019(16) -0.0035(18) F14 0.038(2) 0.031(2) 0.024(2) -0.0060(17) -0.0169(18) 0.0075(19) F15 0.033(2) 0.024(2) 0.030(2) -0.0110(17) -0.0087(17) -0.0073(18) F16 0.031(3) 0.068(4) 0.130(5) -0.067(3) -0.029(3) 0.006(2) F17 0.018(3) 0.259(9) 0.046(3) -0.061(4) 0.002(2) -0.022(4) F18 0.046(3) 0.050(3) 0.135(5) 0.000(3) -0.050(3) 0.005(3) F19 0.094(4) 0.054(3) 0.033(3) -0.011(2) -0.025(2) -0.028(3) F20 0.038(3) 0.078(4) 0.115(5) -0.043(3) -0.021(3) -0.015(3) F21 0.101(4) 0.024(3) 0.063(3) -0.002(2) -0.047(3) -0.020(3) F22 0.092(4) 0.026(3) 0.033(2) -0.0010(19) 0.012(2) 0.014(2) F23 0.039(3) 0.033(3) 0.066(3) 0.017(2) 0.002(2) -0.008(2) F24 0.095(4) 0.034(3) 0.033(3) 0.015(2) -0.035(3) -0.012(3) C40 0.011(3) 0.022(4) 0.014(3) -0.001(3) -0.002(2) -0.002(3) C41 0.012(3) 0.023(4) 0.024(3) -0.003(3) -0.003(3) -0.002(3) C42 0.018(3) 0.020(4) 0.021(4) -0.005(3) 0.001(3) -0.002(3) C43 0.020(4) 0.013(3) 0.028(4) -0.004(3) -0.007(3) 0.002(3) C44 0.013(3) 0.019(4) 0.024(4) 0.000(3) -0.002(3) 0.002(3) C45 0.013(3) 0.026(4) 0.021(3) -0.010(3) -0.003(3) 0.002(3) C46 0.020(4) 0.021(4) 0.029(4) -0.004(3) 0.000(3) -0.001(3) C47 0.024(4) 0.016(4) 0.029(4) -0.005(3) -0.004(3) 0.002(3) C48 0.015(3) 0.019(4) 0.010(3) -0.002(3) -0.002(2) 0.000(3) C49 0.013(3) 0.028(4) 0.014(3) -0.003(3) -0.002(3) 0.003(3) C50 0.026(4) 0.017(4) 0.014(3) 0.000(3) -0.004(3) -0.007(3) C51 0.025(4) 0.029(4) 0.013(3) 0.002(3) 0.000(3) -0.008(3) C52 0.017(4) 0.028(4) 0.017(3) -0.003(3) -0.005(3) 0.001(3) C53 0.022(4) 0.013(3) 0.016(3) 0.000(3) -0.003(3) -0.004(3) C54 0.024(4) 0.030(4) 0.034(4) -0.009(3) -0.003(3) -0.007(3) C55 0.018(4) 0.027(4) 0.023(4) -0.002(3) 0.002(3) -0.004(3) C56 0.019(3) 0.007(3) 0.017(3) -0.001(2) -0.005(3) -0.005(3) C57 0.021(4) 0.009(3) 0.021(3) -0.001(3) -0.006(3) -0.003(3) C58 0.021(4) 0.015(3) 0.015(3) -0.001(3) -0.002(3) -0.002(3) C59 0.018(4) 0.016(4) 0.024(4) -0.009(3) 0.001(3) 0.001(3) C60 0.016(3) 0.020(4) 0.023(4) -0.003(3) -0.004(3) 0.002(3) C61 0.031(4) 0.013(3) 0.009(3) 0.000(2) -0.003(3) -0.003(3) C62 0.029(4) 0.020(4) 0.023(4) -0.010(3) -0.004(3) 0.002(3) C63 0.017(4) 0.042(5) 0.021(4) -0.011(3) -0.002(3) 0.000(3) C64 0.016(3) 0.015(4) 0.019(3) -0.006(3) 0.000(3) -0.001(3) C65 0.020(4) 0.023(4) 0.018(3) -0.010(3) -0.002(3) -0.001(3) C66 0.029(4) 0.025(4) 0.010(3) -0.003(3) -0.002(3) 0.006(3) C67 0.028(4) 0.026(4) 0.015(3) -0.002(3) -0.008(3) 0.004(3) C68 0.025(4) 0.017(4) 0.027(4) -0.009(3) -0.007(3) 0.003(3) C69 0.025(4) 0.019(4) 0.019(3) -0.005(3) 0.000(3) 0.000(3) C70 0.053(5) 0.031(5) 0.023(4) -0.002(3) -0.019(4) -0.003(4) C71 0.026(4) 0.031(4) 0.018(4) -0.002(3) -0.005(3) 0.006(3) B1 0.017(4) 0.016(4) 0.020(4) -0.006(3) -0.004(3) 0.005(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 C2A 1.962(12) . ? Ni1 C1 2.010(8) . ? Ni1 C3 2.045(7) . ? Ni1 C2B 2.048(18) . ? Ni1 P1 2.1915(19) . ? Ni1 P2 2.19(2) . ? Ni1 Sb1 2.370(6) . ? Sb1 C16 1.953(13) . ? Sb1 C4 1.957(14) . ? Sb1 C10 1.960(14) . ? P2 C10 2.00(4) . ? P2 C4 2.03(4) . ? P2 C16 2.07(4) . ? P1 C22 1.818(6) . ? P1 C28 1.825(7) . ? P1 C34 1.852(6) . ? C1 C2B 1.29(2) . ? C1 C2A 1.400(16) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2A C3 1.295(14) . ? C2A H2A 1.0000 . ? C2B C3 1.33(2) . ? C2B H2B 1.0000 . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 C5 1.395(10) . ? C4 C9 1.408(10) . ? C5 C6 1.364(11) . ? C5 H5 0.9500 . ? C6 C7 1.382(11) . ? C6 H6 0.9500 . ? C7 C8 1.381(12) . ? C7 H7 0.9500 . ? C8 C9 1.366(11) . ? C8 H8 0.9500 . ? C9 H9 0.9500 . ? C10 C11 1.367(10) . ? C10 C15 1.379(10) . ? C11 C12 1.375(11) . ? C11 H11 0.9500 . ? C12 C13 1.378(11) . ? C12 H12 0.9500 . ? C13 C14 1.358(11) . ? C13 H13 0.9500 . ? C14 C15 1.379(11) . ? C14 H14 0.9500 . ? C15 H15 0.9500 . ? C16 C21 1.379(10) . ? C16 C17 1.390(10) . ? C17 C18 1.385(10) . ? C17 H17 0.9500 . ? C18 C19 1.368(11) . ? C18 H18 0.9500 . ? C19 C20 1.380(12) . ? C19 H19 0.9500 . ? C20 C21 1.385(12) . ? C20 H20 0.9500 . ? C21 H21 0.9500 . ? C22 C27 1.385(9) . ? C22 C23 1.393(9) . ? C23 C24 1.384(9) . ? C23 H23 0.9500 . ? C24 C25 1.375(10) . ? C24 H24 0.9500 . ? C25 C26 1.369(10) . ? C25 H25 0.9500 . ? C26 C27 1.370(9) . ? C26 H26 0.9500 . ? C27 H27 0.9500 . ? C28 C29 1.388(9) . ? C28 C33 1.394(9) . ? C29 C30 1.387(9) . ? C29 H29 0.9500 . ? C30 C31 1.368(9) . ? C30 H30 0.9500 . ? C31 C32 1.372(10) . ? C31 H31 0.9500 . ? C32 C33 1.361(10) . ? C32 H32 0.9500 . ? C33 H33 0.9500 . ? C34 C35 1.373(9) . ? C34 C39 1.393(9) . ? C35 C36 1.386(9) . ? C35 H35 0.9500 . ? C36 C37 1.378(9) . ? C36 H36 0.9500 . ? C37 C38 1.373(10) . ? C37 H37 0.9500 . ? C38 C39 1.373(9) . ? C38 H38 0.9500 . ? C39 H39 0.9500 . ? F1A C46 1.340(11) . ? F2A C46 1.359(11) . ? F3A C46 1.299(11) . ? F1B C46 1.362(13) . ? F2B C46 1.370(13) . ? F3B C46 1.344(13) . ? F4 C47 1.350(7) . ? F5 C47 1.331(7) . ? F6 C47 1.342(7) . ? F7 C54 1.325(8) . ? F8 C54 1.323(8) . ? F9 C54 1.323(8) . ? F10 C55 1.342(7) . ? F11 C55 1.323(7) . ? F12 C55 1.320(7) . ? F13 C62 1.345(7) . ? F14 C62 1.350(7) . ? F15 C62 1.339(7) . ? F16 C63 1.307(8) . ? F17 C63 1.297(8) . ? F18 C63 1.323(8) . ? F19 C70 1.321(8) . ? F20 C70 1.337(9) . ? F21 C70 1.333(8) . ? F22 C71 1.323(8) . ? F23 C71 1.334(8) . ? F24 C71 1.329(7) . ? C40 C41 1.396(8) . ? C40 C45 1.399(8) . ? C40 B1 1.658(9) . ? C41 C42 1.403(9) . ? C41 H41 0.9500 . ? C42 C43 1.366(8) . ? C42 C46 1.454(9) . ? C43 C44 1.401(9) . ? C43 H43 0.9500 . ? C44 C45 1.379(8) . ? C44 C47 1.485(9) . ? C45 H45 0.9500 . ? C48 C49 1.389(8) . ? C48 C53 1.400(8) . ? C48 B1 1.636(9) . ? C49 C50 1.393(8) . ? C49 H49 0.9500 . ? C50 C51 1.370(9) . ? C50 C54 1.480(9) . ? C51 C52 1.403(9) . ? C51 H51 0.9500 . ? C52 C53 1.378(8) . ? C52 C55 1.481(9) . ? C53 H53 0.9500 . ? C56 C57 1.399(8) . ? C56 C61 1.404(8) . ? C56 B1 1.633(9) . ? C57 C58 1.397(8) . ? C57 H57 0.9500 . ? C58 C59 1.374(8) . ? C58 C62 1.486(8) . ? C59 C60 1.386(8) . ? C59 H59 0.9500 . ? C60 C61 1.387(8) . ? C60 C63 1.501(9) . ? C61 H61 0.9500 . ? C64 C65 1.401(8) . ? C64 C69 1.403(8) . ? C64 B1 1.640(9) . ? C65 C66 1.383(8) . ? C65 H65 0.9500 . ? C66 C67 1.384(9) . ? C66 C71 1.491(9) . ? C67 C68 1.403(9) . ? C67 H67 0.9500 . ? C68 C69 1.379(9) . ? C68 C70 1.482(9) . ? C69 H69 0.9500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2A Ni1 C1 41.2(5) . . ? C2A Ni1 C3 37.6(4) . . ? C1 Ni1 C3 72.1(3) . . ? C2A Ni1 C2B 28.8(6) . . ? C1 Ni1 C2B 37.1(6) . . ? C3 Ni1 C2B 38.0(6) . . ? C2A Ni1 P1 132.2(4) . . ? C1 Ni1 P1 95.1(2) . . ? C3 Ni1 P1 166.6(2) . . ? C2B Ni1 P1 128.6(6) . . ? C2A Ni1 P2 124.0(12) . . ? C1 Ni1 P2 161.3(11) . . ? C3 Ni1 P2 90.0(11) . . ? C2B Ni1 P2 124.2(12) . . ? P1 Ni1 P2 102.4(11) . . ? C2A Ni1 Sb1 123.3(5) . . ? C1 Ni1 Sb1 161.2(4) . . ? C3 Ni1 Sb1 89.6(4) . . ? C2B Ni1 Sb1 124.2(6) . . ? P1 Ni1 Sb1 102.9(3) . . ? P2 Ni1 Sb1 1.2(14) . . ? C16 Sb1 C4 102.8(5) . . ? C16 Sb1 C10 104.4(5) . . ? C4 Sb1 C10 102.4(6) . . ? C16 Sb1 Ni1 114.7(5) . . ? C4 Sb1 Ni1 121.6(5) . . ? C10 Sb1 Ni1 109.1(5) . . ? C10 P2 C4 98.2(16) . . ? C10 P2 C16 98.6(15) . . ? C4 P2 C16 96.1(13) . . ? C10 P2 Ni1 114.6(17) . . ? C4 P2 Ni1 126.7(19) . . ? C16 P2 Ni1 117.4(19) . . ? C22 P1 C28 109.1(3) . . ? C22 P1 C34 100.8(3) . . ? C28 P1 C34 103.0(3) . . ? C22 P1 Ni1 115.0(2) . . ? C28 P1 Ni1 108.1(2) . . ? C34 P1 Ni1 119.9(2) . . ? C2B C1 C2A 43.3(11) . . ? C2B C1 Ni1 73.0(8) . . ? C2A C1 Ni1 67.6(6) . . ? C2B C1 H1A 155.4 . . ? C2A C1 H1A 116.9 . . ? Ni1 C1 H1A 116.9 . . ? C2B C1 H1B 76.0 . . ? C2A C1 H1B 116.9 . . ? Ni1 C1 H1B 116.9 . . ? H1A C1 H1B 114.0 . . ? C3 C2A C1 124.5(14) . . ? C3 C2A Ni1 74.7(7) . . ? C1 C2A Ni1 71.2(6) . . ? C3 C2A H2A 117.1 . . ? C1 C2A H2A 117.1 . . ? Ni1 C2A H2A 117.1 . . ? C1 C2B C3 131(2) . . ? C1 C2B Ni1 69.8(9) . . ? C3 C2B Ni1 70.9(9) . . ? C1 C2B H2B 110.4 . . ? C3 C2B H2B 110.4 . . ? Ni1 C2B H2B 110.4 . . ? C2A C3 C2B 44.7(11) . . ? C2A C3 Ni1 67.7(6) . . ? C2B C3 Ni1 71.1(8) . . ? C2A C3 H3A 116.9 . . ? C2B C3 H3A 75.7 . . ? Ni1 C3 H3A 116.9 . . ? C2A C3 H3B 116.9 . . ? C2B C3 H3B 158.0 . . ? Ni1 C3 H3B 116.9 . . ? H3A C3 H3B 113.9 . . ? C5 C4 C9 117.8(7) . . ? C5 C4 Sb1 121.7(6) . . ? C9 C4 Sb1 120.5(7) . . ? C5 C4 P2 121.3(13) . . ? C9 C4 P2 120.7(13) . . ? Sb1 C4 P2 4.7(11) . . ? C6 C5 C4 121.2(7) . . ? C6 C5 H5 119.4 . . ? C4 C5 H5 119.4 . . ? C5 C6 C7 120.2(8) . . ? C5 C6 H6 119.9 . . ? C7 C6 H6 119.9 . . ? C6 C7 C8 119.7(8) . . ? C6 C7 H7 120.1 . . ? C8 C7 H7 120.1 . . ? C9 C8 C7 120.5(8) . . ? C9 C8 H8 119.8 . . ? C7 C8 H8 119.8 . . ? C8 C9 C4 120.6(8) . . ? C8 C9 H9 119.7 . . ? C4 C9 H9 119.7 . . ? C11 C10 C15 118.3(7) . . ? C11 C10 Sb1 123.3(6) . . ? C15 C10 Sb1 118.3(6) . . ? C11 C10 P2 127.9(11) . . ? C15 C10 P2 113.8(11) . . ? Sb1 C10 P2 5.1(10) . . ? C10 C11 C12 121.4(7) . . ? C10 C11 H11 119.3 . . ? C12 C11 H11 119.3 . . ? C11 C12 C13 119.3(8) . . ? C11 C12 H12 120.3 . . ? C13 C12 H12 120.3 . . ? C14 C13 C12 120.2(8) . . ? C14 C13 H13 119.9 . . ? C12 C13 H13 119.9 . . ? C13 C14 C15 119.8(8) . . ? C13 C14 H14 120.1 . . ? C15 C14 H14 120.1 . . ? C14 C15 C10 120.9(8) . . ? C14 C15 H15 119.6 . . ? C10 C15 H15 119.6 . . ? C21 C16 C17 118.5(7) . . ? C21 C16 Sb1 121.6(6) . . ? C17 C16 Sb1 119.9(6) . . ? C21 C16 P2 118.0(11) . . ? C17 C16 P2 123.6(11) . . ? Sb1 C16 P2 3.9(11) . . ? C18 C17 C16 120.4(7) . . ? C18 C17 H17 119.8 . . ? C16 C17 H17 119.8 . . ? C19 C18 C17 120.3(8) . . ? C19 C18 H18 119.8 . . ? C17 C18 H18 119.8 . . ? C18 C19 C20 120.0(8) . . ? C18 C19 H19 120.0 . . ? C20 C19 H19 120.0 . . ? C19 C20 C21 119.6(8) . . ? C19 C20 H20 120.2 . . ? C21 C20 H20 120.2 . . ? C16 C21 C20 121.1(8) . . ? C16 C21 H21 119.4 . . ? C20 C21 H21 119.4 . . ? C27 C22 C23 117.9(6) . . ? C27 C22 P1 122.4(5) . . ? C23 C22 P1 119.6(5) . . ? C24 C23 C22 120.6(6) . . ? C24 C23 H23 119.7 . . ? C22 C23 H23 119.7 . . ? C25 C24 C23 119.6(7) . . ? C25 C24 H24 120.2 . . ? C23 C24 H24 120.2 . . ? C26 C25 C24 120.6(7) . . ? C26 C25 H25 119.7 . . ? C24 C25 H25 119.7 . . ? C25 C26 C27 119.6(7) . . ? C25 C26 H26 120.2 . . ? C27 C26 H26 120.2 . . ? C26 C27 C22 121.7(6) . . ? C26 C27 H27 119.2 . . ? C22 C27 H27 119.2 . . ? C29 C28 C33 119.1(6) . . ? C29 C28 P1 125.1(5) . . ? C33 C28 P1 115.7(5) . . ? C28 C29 C30 119.7(6) . . ? C28 C29 H29 120.1 . . ? C30 C29 H29 120.1 . . ? C31 C30 C29 120.0(7) . . ? C31 C30 H30 120.0 . . ? C29 C30 H30 120.0 . . ? C30 C31 C32 120.5(7) . . ? C30 C31 H31 119.7 . . ? C32 C31 H31 119.7 . . ? C33 C32 C31 120.3(7) . . ? C33 C32 H32 119.8 . . ? C31 C32 H32 119.8 . . ? C32 C33 C28 120.3(7) . . ? C32 C33 H33 119.8 . . ? C28 C33 H33 119.8 . . ? C35 C34 C39 118.5(6) . . ? C35 C34 P1 123.7(5) . . ? C39 C34 P1 117.8(5) . . ? C34 C35 C36 120.9(6) . . ? C34 C35 H35 119.5 . . ? C36 C35 H35 119.5 . . ? C37 C36 C35 119.6(6) . . ? C37 C36 H36 120.2 . . ? C35 C36 H36 120.2 . . ? C38 C37 C36 120.2(6) . . ? C38 C37 H37 119.9 . . ? C36 C37 H37 119.9 . . ? C37 C38 C39 119.9(7) . . ? C37 C38 H38 120.0 . . ? C39 C38 H38 120.0 . . ? C38 C39 C34 120.9(6) . . ? C38 C39 H39 119.6 . . ? C34 C39 H39 119.6 . . ? C41 C40 C45 114.9(6) . . ? C41 C40 B1 124.2(5) . . ? C45 C40 B1 120.8(5) . . ? C40 C41 C42 122.6(6) . . ? C40 C41 H41 118.7 . . ? C42 C41 H41 118.7 . . ? C43 C42 C41 120.5(6) . . ? C43 C42 C46 119.8(6) . . ? C41 C42 C46 119.7(6) . . ? C42 C43 C44 118.7(6) . . ? C42 C43 H43 120.7 . . ? C44 C43 H43 120.7 . . ? C45 C44 C43 119.8(6) . . ? C45 C44 C47 121.0(6) . . ? C43 C44 C47 119.2(6) . . ? C44 C45 C40 123.6(6) . . ? C44 C45 H45 118.2 . . ? C40 C45 H45 118.2 . . ? F3A C46 F1A 108.0(7) . . ? F3A C46 F3B 73.8(7) . . ? F1A C46 F3B 36.3(6) . . ? F3A C46 F1B 129.5(8) . . ? F1A C46 F1B 71.9(7) . . ? F3B C46 F1B 102.8(8) . . ? F3A C46 F2A 106.3(7) . . ? F1A C46 F2A 101.3(7) . . ? F3B C46 F2A 123.1(8) . . ? F1B C46 F2A 33.0(5) . . ? F3A C46 F2B 38.8(6) . . ? F1A C46 F2B 130.1(8) . . ? F3B C46 F2B 106.1(8) . . ? F1B C46 F2B 101.2(8) . . ? F2A C46 F2B 70.8(7) . . ? F3A C46 C42 113.1(7) . . ? F1A C46 C42 113.4(6) . . ? F3B C46 C42 117.8(7) . . ? F1B C46 C42 112.4(7) . . ? F2A C46 C42 113.8(6) . . ? F2B C46 C42 114.7(7) . . ? F5 C47 F6 106.5(5) . . ? F5 C47 F4 106.2(5) . . ? F6 C47 F4 105.7(5) . . ? F5 C47 C44 113.7(5) . . ? F6 C47 C44 112.1(5) . . ? F4 C47 C44 112.2(5) . . ? C49 C48 C53 114.6(5) . . ? C49 C48 B1 123.9(5) . . ? C53 C48 B1 121.3(5) . . ? C48 C49 C50 123.2(6) . . ? C48 C49 H49 118.4 . . ? C50 C49 H49 118.4 . . ? C51 C50 C49 120.3(6) . . ? C51 C50 C54 120.3(6) . . ? C49 C50 C54 119.4(6) . . ? C50 C51 C52 118.7(6) . . ? C50 C51 H51 120.7 . . ? C52 C51 H51 120.7 . . ? C53 C52 C51 119.3(6) . . ? C53 C52 C55 121.0(6) . . ? C51 C52 C55 119.6(6) . . ? C52 C53 C48 123.9(6) . . ? C52 C53 H53 118.1 . . ? C48 C53 H53 118.1 . . ? F8 C54 F9 106.0(6) . . ? F8 C54 F7 103.5(6) . . ? F9 C54 F7 105.1(6) . . ? F8 C54 C50 113.8(6) . . ? F9 C54 C50 114.5(6) . . ? F7 C54 C50 113.0(6) . . ? F12 C55 F11 106.9(6) . . ? F12 C55 F10 104.9(5) . . ? F11 C55 F10 104.6(5) . . ? F12 C55 C52 113.7(5) . . ? F11 C55 C52 113.8(5) . . ? F10 C55 C52 112.1(5) . . ? C57 C56 C61 114.8(5) . . ? C57 C56 B1 122.8(5) . . ? C61 C56 B1 121.6(5) . . ? C58 C57 C56 122.7(6) . . ? C58 C57 H57 118.6 . . ? C56 C57 H57 118.6 . . ? C59 C58 C57 120.6(6) . . ? C59 C58 C62 120.7(5) . . ? C57 C58 C62 118.5(6) . . ? C58 C59 C60 118.4(6) . . ? C58 C59 H59 120.8 . . ? C60 C59 H59 120.8 . . ? C59 C60 C61 120.5(6) . . ? C59 C60 C63 119.9(5) . . ? C61 C60 C63 119.4(6) . . ? C60 C61 C56 122.9(6) . . ? C60 C61 H61 118.5 . . ? C56 C61 H61 118.5 . . ? F15 C62 F13 106.5(5) . . ? F15 C62 F14 105.8(5) . . ? F13 C62 F14 106.0(5) . . ? F15 C62 C58 113.6(5) . . ? F13 C62 C58 112.7(5) . . ? F14 C62 C58 111.6(5) . . ? F17 C63 F16 106.8(6) . . ? F17 C63 F18 105.7(6) . . ? F16 C63 F18 103.7(6) . . ? F17 C63 C60 113.9(5) . . ? F16 C63 C60 113.6(6) . . ? F18 C63 C60 112.4(6) . . ? C65 C64 C69 114.6(6) . . ? C65 C64 B1 121.0(5) . . ? C69 C64 B1 124.0(5) . . ? C66 C65 C64 123.0(6) . . ? C66 C65 H65 118.5 . . ? C64 C65 H65 118.5 . . ? C65 C66 C67 120.6(6) . . ? C65 C66 C71 119.6(6) . . ? C67 C66 C71 119.7(6) . . ? C66 C67 C68 118.5(6) . . ? C66 C67 H67 120.8 . . ? C68 C67 H67 120.8 . . ? C69 C68 C67 119.5(6) . . ? C69 C68 C70 121.5(6) . . ? C67 C68 C70 118.9(6) . . ? C68 C69 C64 123.8(6) . . ? C68 C69 H69 118.1 . . ? C64 C69 H69 118.1 . . ? F19 C70 F21 106.4(6) . . ? F19 C70 F20 105.9(6) . . ? F21 C70 F20 105.9(6) . . ? F19 C70 C68 113.2(6) . . ? F21 C70 C68 112.6(6) . . ? F20 C70 C68 112.3(6) . . ? F22 C71 F24 106.7(6) . . ? F22 C71 F23 106.0(6) . . ? F24 C71 F23 105.6(5) . . ? F22 C71 C66 112.6(5) . . ? F24 C71 C66 113.2(6) . . ? F23 C71 C66 112.3(6) . . ? C56 B1 C48 114.8(5) . . ? C56 B1 C64 107.3(5) . . ? C48 B1 C64 108.3(5) . . ? C56 B1 C40 106.1(5) . . ? C48 B1 C40 107.2(5) . . ? C64 B1 C40 113.2(5) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C2A Ni1 Sb1 C16 -51.9(10) . . . . ? C1 Ni1 Sb1 C16 -82.2(12) . . . . ? C3 Ni1 Sb1 C16 -69.8(6) . . . . ? C2B Ni1 Sb1 C16 -86.6(13) . . . . ? P1 Ni1 Sb1 C16 115.1(5) . . . . ? P2 Ni1 Sb1 C16 -176(66) . . . . ? C2A Ni1 Sb1 C4 -176.7(8) . . . . ? C1 Ni1 Sb1 C4 153.0(8) . . . . ? C3 Ni1 Sb1 C4 165.4(7) . . . . ? C2B Ni1 Sb1 C4 148.6(12) . . . . ? P1 Ni1 Sb1 C4 -9.7(7) . . . . ? P2 Ni1 Sb1 C4 59(65) . . . . ? C2A Ni1 Sb1 C10 64.7(9) . . . . ? C1 Ni1 Sb1 C10 34.4(15) . . . . ? C3 Ni1 Sb1 C10 46.9(6) . . . . ? C2B Ni1 Sb1 C10 30.0(13) . . . . ? P1 Ni1 Sb1 C10 -128.3(5) . . . . ? P2 Ni1 Sb1 C10 -60(65) . . . . ? C2A Ni1 P2 C10 62(2) . . . . ? C1 Ni1 P2 C10 29(5) . . . . ? C3 Ni1 P2 C10 45.1(19) . . . . ? C2B Ni1 P2 C10 27(3) . . . . ? P1 Ni1 P2 C10 -129.8(17) . . . . ? Sb1 Ni1 P2 C10 118(66) . . . . ? C2A Ni1 P2 C4 -175.2(17) . . . . ? C1 Ni1 P2 C4 151.6(18) . . . . ? C3 Ni1 P2 C4 168(2) . . . . ? C2B Ni1 P2 C4 150(2) . . . . ? P1 Ni1 P2 C4 -7(3) . . . . ? Sb1 Ni1 P2 C4 -119(66) . . . . ? C2A Ni1 P2 C16 -53(2) . . . . ? C1 Ni1 P2 C16 -86(4) . . . . ? C3 Ni1 P2 C16 -69.9(19) . . . . ? C2B Ni1 P2 C16 -88(2) . . . . ? P1 Ni1 P2 C16 115.2(18) . . . . ? Sb1 Ni1 P2 C16 3(63) . . . . ? C2A Ni1 P1 C22 100.1(8) . . . . ? C1 Ni1 P1 C22 120.3(3) . . . . ? C3 Ni1 P1 C22 136.3(12) . . . . ? C2B Ni1 P1 C22 137.9(12) . . . . ? P2 Ni1 P1 C22 -66.4(11) . . . . ? Sb1 Ni1 P1 C22 -65.2(4) . . . . ? C2A Ni1 P1 C28 -137.7(8) . . . . ? C1 Ni1 P1 C28 -117.5(3) . . . . ? C3 Ni1 P1 C28 -101.5(12) . . . . ? C2B Ni1 P1 C28 -99.9(12) . . . . ? P2 Ni1 P1 C28 55.8(11) . . . . ? Sb1 Ni1 P1 C28 57.0(4) . . . . ? C2A Ni1 P1 C34 -20.3(8) . . . . ? C1 Ni1 P1 C34 -0.1(3) . . . . ? C3 Ni1 P1 C34 15.9(12) . . . . ? C2B Ni1 P1 C34 17.5(12) . . . . ? P2 Ni1 P1 C34 173.2(11) . . . . ? Sb1 Ni1 P1 C34 174.4(4) . . . . ? C2A Ni1 C1 C2B -45.8(11) . . . . ? C3 Ni1 C1 C2B -19.1(15) . . . . ? P1 Ni1 C1 C2B 157.0(15) . . . . ? P2 Ni1 C1 C2B -2(4) . . . . ? Sb1 Ni1 C1 C2B -6(2) . . . . ? C3 Ni1 C1 C2A 26.7(9) . . . . ? C2B Ni1 C1 C2A 45.8(11) . . . . ? P1 Ni1 C1 C2A -157.2(8) . . . . ? P2 Ni1 C1 C2A 44(4) . . . . ? Sb1 Ni1 C1 C2A 39.8(15) . . . . ? C2B C1 C2A C3 33.7(14) . . . . ? Ni1 C1 C2A C3 -55.0(11) . . . . ? C2B C1 C2A Ni1 88.7(13) . . . . ? C1 Ni1 C2A C3 135.6(14) . . . . ? C2B Ni1 C2A C3 71.4(14) . . . . ? P1 Ni1 C2A C3 167.1(5) . . . . ? P2 Ni1 C2A C3 -28.9(18) . . . . ? Sb1 Ni1 C2A C3 -30.2(12) . . . . ? C3 Ni1 C2A C1 -135.6(14) . . . . ? C2B Ni1 C2A C1 -64.2(15) . . . . ? P1 Ni1 C2A C1 31.5(12) . . . . ? P2 Ni1 C2A C1 -164.5(14) . . . . ? Sb1 Ni1 C2A C1 -165.8(5) . . . . ? C2A C1 C2B C3 -36(2) . . . . ? Ni1 C1 C2B C3 39(2) . . . . ? C2A C1 C2B Ni1 -75.0(11) . . . . ? C2A Ni1 C2B C1 79.5(19) . . . . ? C3 Ni1 C2B C1 150(2) . . . . ? P1 Ni1 C2B C1 -30(2) . . . . ? P2 Ni1 C2B C1 179.1(15) . . . . ? Sb1 Ni1 C2B C1 177.6(8) . . . . ? C2A Ni1 C2B C3 -70.1(15) . . . . ? C1 Ni1 C2B C3 -150(2) . . . . ? P1 Ni1 C2B C3 -179.4(6) . . . . ? P2 Ni1 C2B C3 30(2) . . . . ? Sb1 Ni1 C2B C3 28.1(19) . . . . ? C1 C2A C3 C2B -31.7(13) . . . . ? Ni1 C2A C3 C2B -85.3(12) . . . . ? C1 C2A C3 Ni1 53.5(11) . . . . ? C1 C2B C3 C2A 38(2) . . . . ? Ni1 C2B C3 C2A 77.0(11) . . . . ? C1 C2B C3 Ni1 -39(2) . . . . ? C1 Ni1 C3 C2A -29.0(10) . . . . ? C2B Ni1 C3 C2A -47.8(11) . . . . ? P1 Ni1 C3 C2A -45.8(17) . . . . ? P2 Ni1 C3 C2A 156.3(15) . . . . ? Sb1 Ni1 C3 C2A 155.2(10) . . . . ? C2A Ni1 C3 C2B 47.8(11) . . . . ? C1 Ni1 C3 C2B 18.8(15) . . . . ? P1 Ni1 C3 C2B 2(2) . . . . ? P2 Ni1 C3 C2B -155.9(19) . . . . ? Sb1 Ni1 C3 C2B -157.1(16) . . . . ? C16 Sb1 C4 C5 128.8(6) . . . . ? C10 Sb1 C4 C5 20.7(7) . . . . ? Ni1 Sb1 C4 C5 -101.1(8) . . . . ? C16 Sb1 C4 C9 -50.3(7) . . . . ? C10 Sb1 C4 C9 -158.4(6) . . . . ? Ni1 Sb1 C4 C9 79.8(8) . . . . ? C16 Sb1 C4 P2 -144(19) . . . . ? C10 Sb1 C4 P2 108(19) . . . . ? Ni1 Sb1 C4 P2 -14(18) . . . . ? C10 P2 C4 C5 29.0(17) . . . . ? C16 P2 C4 C5 128.6(11) . . . . ? Ni1 P2 C4 C5 -100(2) . . . . ? C10 P2 C4 C9 -155.8(9) . . . . ? C16 P2 C4 C9 -56.2(15) . . . . ? Ni1 P2 C4 C9 75(2) . . . . ? C10 P2 C4 Sb1 -67(18) . . . . ? C16 P2 C4 Sb1 33(17) . . . . ? Ni1 P2 C4 Sb1 164(21) . . . . ? C9 C4 C5 C6 0.2(10) . . . . ? Sb1 C4 C5 C6 -178.9(6) . . . . ? P2 C4 C5 C6 175.6(11) . . . . ? C4 C5 C6 C7 0.2(11) . . . . ? C5 C6 C7 C8 -0.4(11) . . . . ? C6 C7 C8 C9 0.3(11) . . . . ? C7 C8 C9 C4 0.1(11) . . . . ? C5 C4 C9 C8 -0.4(10) . . . . ? Sb1 C4 C9 C8 178.8(6) . . . . ? P2 C4 C9 C8 -175.7(11) . . . . ? C16 Sb1 C10 C11 -18.9(9) . . . . ? C4 Sb1 C10 C11 88.0(8) . . . . ? Ni1 Sb1 C10 C11 -142.0(6) . . . . ? C16 Sb1 C10 C15 163.7(6) . . . . ? C4 Sb1 C10 C15 -89.3(7) . . . . ? Ni1 Sb1 C10 C15 40.6(9) . . . . ? C16 Sb1 C10 P2 136(18) . . . . ? C4 Sb1 C10 P2 -117(18) . . . . ? Ni1 Sb1 C10 P2 13(18) . . . . ? C4 P2 C10 C11 84.3(19) . . . . ? C16 P2 C10 C11 -13(2) . . . . ? Ni1 P2 C10 C11 -138.8(13) . . . . ? C4 P2 C10 C15 -95.8(11) . . . . ? C16 P2 C10 C15 166.7(9) . . . . ? Ni1 P2 C10 C15 41(2) . . . . ? C4 P2 C10 Sb1 58(17) . . . . ? C16 P2 C10 Sb1 -40(17) . . . . ? Ni1 P2 C10 Sb1 -165(20) . . . . ? C15 C10 C11 C12 -1.4(12) . . . . ? Sb1 C10 C11 C12 -178.8(8) . . . . ? P2 C10 C11 C12 178.5(16) . . . . ? C10 C11 C12 C13 0.2(14) . . . . ? C11 C12 C13 C14 1.5(14) . . . . ? C12 C13 C14 C15 -1.9(14) . . . . ? C13 C14 C15 C10 0.6(14) . . . . ? C11 C10 C15 C14 1.0(12) . . . . ? Sb1 C10 C15 C14 178.5(8) . . . . ? P2 C10 C15 C14 -178.9(14) . . . . ? C4 Sb1 C16 C21 154.6(6) . . . . ? C10 Sb1 C16 C21 -98.8(7) . . . . ? Ni1 Sb1 C16 C21 20.5(9) . . . . ? C4 Sb1 C16 C17 -27.5(8) . . . . ? C10 Sb1 C16 C17 79.1(8) . . . . ? Ni1 Sb1 C16 C17 -161.6(6) . . . . ? C4 Sb1 C16 P2 135(23) . . . . ? C10 Sb1 C16 P2 -118(23) . . . . ? Ni1 Sb1 C16 P2 1(22) . . . . ? C10 P2 C16 C21 -103.7(12) . . . . ? C4 P2 C16 C21 157.0(9) . . . . ? Ni1 P2 C16 C21 20(2) . . . . ? C10 P2 C16 C17 75.6(18) . . . . ? C4 P2 C16 C17 -24(2) . . . . ? Ni1 P2 C16 C17 -160.8(12) . . . . ? C10 P2 C16 Sb1 58(22) . . . . ? C4 P2 C16 Sb1 -42(21) . . . . ? Ni1 P2 C16 Sb1 -179(24) . . . . ? C21 C16 C17 C18 0.3(11) . . . . ? Sb1 C16 C17 C18 -177.7(7) . . . . ? P2 C16 C17 C18 -179.1(15) . . . . ? C16 C17 C18 C19 1.3(11) . . . . ? C17 C18 C19 C20 -2.4(12) . . . . ? C18 C19 C20 C21 2.0(13) . . . . ? C17 C16 C21 C20 -0.6(11) . . . . ? Sb1 C16 C21 C20 177.3(7) . . . . ? P2 C16 C21 C20 178.7(14) . . . . ? C19 C20 C21 C16 -0.5(13) . . . . ? C28 P1 C22 C27 57.6(6) . . . . ? C34 P1 C22 C27 -50.3(6) . . . . ? Ni1 P1 C22 C27 179.3(5) . . . . ? C28 P1 C22 C23 -125.2(5) . . . . ? C34 P1 C22 C23 126.9(5) . . . . ? Ni1 P1 C22 C23 -3.6(6) . . . . ? C27 C22 C23 C24 -1.3(10) . . . . ? P1 C22 C23 C24 -178.5(5) . . . . ? C22 C23 C24 C25 -0.7(11) . . . . ? C23 C24 C25 C26 1.7(11) . . . . ? C24 C25 C26 C27 -0.7(11) . . . . ? C25 C26 C27 C22 -1.4(11) . . . . ? C23 C22 C27 C26 2.3(10) . . . . ? P1 C22 C27 C26 179.5(5) . . . . ? C22 P1 C28 C29 -0.6(6) . . . . ? C34 P1 C28 C29 105.8(6) . . . . ? Ni1 P1 C28 C29 -126.4(5) . . . . ? C22 P1 C28 C33 175.7(5) . . . . ? C34 P1 C28 C33 -77.9(5) . . . . ? Ni1 P1 C28 C33 50.0(5) . . . . ? C33 C28 C29 C30 1.4(9) . . . . ? P1 C28 C29 C30 177.6(5) . . . . ? C28 C29 C30 C31 0.4(10) . . . . ? C29 C30 C31 C32 -1.3(10) . . . . ? C30 C31 C32 C33 0.2(11) . . . . ? C31 C32 C33 C28 1.7(11) . . . . ? C29 C28 C33 C32 -2.5(10) . . . . ? P1 C28 C33 C32 -179.1(6) . . . . ? C22 P1 C34 C35 120.2(6) . . . . ? C28 P1 C34 C35 7.4(6) . . . . ? Ni1 P1 C34 C35 -112.6(5) . . . . ? C22 P1 C34 C39 -59.9(5) . . . . ? C28 P1 C34 C39 -172.6(5) . . . . ? Ni1 P1 C34 C39 67.3(5) . . . . ? C39 C34 C35 C36 0.1(9) . . . . ? P1 C34 C35 C36 -180.0(5) . . . . ? C34 C35 C36 C37 -0.7(10) . . . . ? C35 C36 C37 C38 1.2(10) . . . . ? C36 C37 C38 C39 -1.0(10) . . . . ? C37 C38 C39 C34 0.4(10) . . . . ? C35 C34 C39 C38 0.0(10) . . . . ? P1 C34 C39 C38 -179.9(5) . . . . ? C45 C40 C41 C42 0.0(8) . . . . ? B1 C40 C41 C42 -175.6(5) . . . . ? C40 C41 C42 C43 -0.7(9) . . . . ? C40 C41 C42 C46 -179.6(6) . . . . ? C41 C42 C43 C44 1.7(9) . . . . ? C46 C42 C43 C44 -179.4(6) . . . . ? C42 C43 C44 C45 -2.0(9) . . . . ? C42 C43 C44 C47 178.1(6) . . . . ? C43 C44 C45 C40 1.4(9) . . . . ? C47 C44 C45 C40 -178.7(6) . . . . ? C41 C40 C45 C44 -0.4(9) . . . . ? B1 C40 C45 C44 175.4(5) . . . . ? C43 C42 C46 F3A -105.5(9) . . . . ? C41 C42 C46 F3A 73.5(9) . . . . ? C43 C42 C46 F1A 131.2(8) . . . . ? C41 C42 C46 F1A -49.9(10) . . . . ? C43 C42 C46 F3B 171.3(9) . . . . ? C41 C42 C46 F3B -9.8(11) . . . . ? C43 C42 C46 F1B 52.0(10) . . . . ? C41 C42 C46 F1B -129.0(8) . . . . ? C43 C42 C46 F2A 16.0(10) . . . . ? C41 C42 C46 F2A -165.0(7) . . . . ? C43 C42 C46 F2B -62.8(10) . . . . ? C41 C42 C46 F2B 116.1(9) . . . . ? C45 C44 C47 F5 6.6(9) . . . . ? C43 C44 C47 F5 -173.4(5) . . . . ? C45 C44 C47 F6 -114.2(6) . . . . ? C43 C44 C47 F6 65.8(8) . . . . ? C45 C44 C47 F4 127.1(6) . . . . ? C43 C44 C47 F4 -53.0(8) . . . . ? C53 C48 C49 C50 -0.6(8) . . . . ? B1 C48 C49 C50 174.7(5) . . . . ? C48 C49 C50 C51 0.6(9) . . . . ? C48 C49 C50 C54 -179.3(6) . . . . ? C49 C50 C51 C52 -0.9(9) . . . . ? C54 C50 C51 C52 179.0(6) . . . . ? C50 C51 C52 C53 1.1(9) . . . . ? C50 C51 C52 C55 -178.4(6) . . . . ? C51 C52 C53 C48 -1.2(9) . . . . ? C55 C52 C53 C48 178.4(6) . . . . ? C49 C48 C53 C52 0.8(8) . . . . ? B1 C48 C53 C52 -174.5(6) . . . . ? C51 C50 C54 F8 -133.6(6) . . . . ? C49 C50 C54 F8 46.3(8) . . . . ? C51 C50 C54 F9 -11.5(9) . . . . ? C49 C50 C54 F9 168.4(6) . . . . ? C51 C50 C54 F7 108.8(7) . . . . ? C49 C50 C54 F7 -71.3(8) . . . . ? C53 C52 C55 F12 142.4(6) . . . . ? C51 C52 C55 F12 -38.1(8) . . . . ? C53 C52 C55 F11 19.6(9) . . . . ? C51 C52 C55 F11 -160.9(6) . . . . ? C53 C52 C55 F10 -98.9(7) . . . . ? C51 C52 C55 F10 80.7(7) . . . . ? C61 C56 C57 C58 -2.3(8) . . . . ? B1 C56 C57 C58 167.7(6) . . . . ? C56 C57 C58 C59 1.8(9) . . . . ? C56 C57 C58 C62 -173.1(5) . . . . ? C57 C58 C59 C60 -0.1(9) . . . . ? C62 C58 C59 C60 174.7(6) . . . . ? C58 C59 C60 C61 -1.1(9) . . . . ? C58 C59 C60 C63 -177.1(6) . . . . ? C59 C60 C61 C56 0.5(9) . . . . ? C63 C60 C61 C56 176.5(6) . . . . ? C57 C56 C61 C60 1.1(8) . . . . ? B1 C56 C61 C60 -169.0(6) . . . . ? C59 C58 C62 F15 118.2(6) . . . . ? C57 C58 C62 F15 -66.9(7) . . . . ? C59 C58 C62 F13 -3.1(8) . . . . ? C57 C58 C62 F13 171.8(5) . . . . ? C59 C58 C62 F14 -122.3(6) . . . . ? C57 C58 C62 F14 52.6(7) . . . . ? C59 C60 C63 F17 15.4(10) . . . . ? C61 C60 C63 F17 -160.7(7) . . . . ? C59 C60 C63 F16 137.9(6) . . . . ? C61 C60 C63 F16 -38.1(9) . . . . ? C59 C60 C63 F18 -104.7(7) . . . . ? C61 C60 C63 F18 79.2(8) . . . . ? C69 C64 C65 C66 -0.5(9) . . . . ? B1 C64 C65 C66 172.9(6) . . . . ? C64 C65 C66 C67 1.4(10) . . . . ? C64 C65 C66 C71 -176.0(6) . . . . ? C65 C66 C67 C68 -0.8(9) . . . . ? C71 C66 C67 C68 176.6(6) . . . . ? C66 C67 C68 C69 -0.5(9) . . . . ? C66 C67 C68 C70 -178.2(6) . . . . ? C67 C68 C69 C64 1.4(10) . . . . ? C70 C68 C69 C64 179.0(6) . . . . ? C65 C64 C69 C68 -0.8(9) . . . . ? B1 C64 C69 C68 -174.1(6) . . . . ? C69 C68 C70 F19 143.4(6) . . . . ? C67 C68 C70 F19 -38.9(9) . . . . ? C69 C68 C70 F21 22.8(10) . . . . ? C67 C68 C70 F21 -159.6(6) . . . . ? C69 C68 C70 F20 -96.7(8) . . . . ? C67 C68 C70 F20 80.9(8) . . . . ? C65 C66 C71 F22 62.3(8) . . . . ? C67 C66 C71 F22 -115.1(7) . . . . ? C65 C66 C71 F24 -176.6(6) . . . . ? C67 C66 C71 F24 6.0(9) . . . . ? C65 C66 C71 F23 -57.2(8) . . . . ? C67 C66 C71 F23 125.4(6) . . . . ? C57 C56 B1 C48 37.9(8) . . . . ? C61 C56 B1 C48 -152.8(5) . . . . ? C57 C56 B1 C64 158.4(5) . . . . ? C61 C56 B1 C64 -32.3(7) . . . . ? C57 C56 B1 C40 -80.3(7) . . . . ? C61 C56 B1 C40 89.0(6) . . . . ? C49 C48 B1 C56 29.4(8) . . . . ? C53 C48 B1 C56 -155.7(5) . . . . ? C49 C48 B1 C64 -90.5(7) . . . . ? C53 C48 B1 C64 84.4(7) . . . . ? C49 C48 B1 C40 147.0(5) . . . . ? C53 C48 B1 C40 -38.1(7) . . . . ? C65 C64 B1 C56 -85.7(7) . . . . ? C69 C64 B1 C56 87.1(7) . . . . ? C65 C64 B1 C48 38.7(8) . . . . ? C69 C64 B1 C48 -148.4(6) . . . . ? C65 C64 B1 C40 157.5(5) . . . . ? C69 C64 B1 C40 -29.7(8) . . . . ? C41 C40 B1 C56 -149.1(6) . . . . ? C45 C40 B1 C56 35.5(7) . . . . ? C41 C40 B1 C48 87.8(7) . . . . ? C45 C40 B1 C48 -87.6(6) . . . . ? C41 C40 B1 C64 -31.6(8) . . . . ? C45 C40 B1 C64 153.0(5) . . . . ? _diffrn_measured_fraction_theta_max 0.987 _diffrn_reflns_theta_full 23.26 _diffrn_measured_fraction_theta_full 0.987 _refine_diff_density_max 1.421 _refine_diff_density_min -0.817 _refine_diff_density_rms 0.088 #===END #=== Data for pv0203 (compound 5a in the text) data_pva0203 _database_code_depnum_ccdc_archive 'CCDC 703652' _audit_creation_method SHELXL-97 _chemical_name_systematic ; Bromo-(tri-hapto-2-methyl-allyl)-(triphenylestibine) nickel (II) ; _chemical_name_common ;Bromo-(tri-hapto-2-methyl-allyl)-(triphenylestibine) nickel (ii) ; _chemical_melting_point ? _chemical_formula_moiety 'C22 H22 Br Ni Sb' _chemical_formula_sum 'C22 H22 Br Ni Sb' _chemical_formula_weight 546.77 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Sb Sb -0.5866 1.5461 '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' _symmetry_int_tables_number 14 _symmetry_space_group_name_Hall '-P 2ybc' 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 12.160(2) _cell_length_b 10.1466(17) _cell_length_c 17.556(4) _cell_angle_alpha 90.00 _cell_angle_beta 97.557(8) _cell_angle_gamma 90.00 _cell_volume 2147.3(7) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 7364 _cell_measurement_theta_min 2.325 _cell_measurement_theta_max 25.484 _exptl_crystal_description plate _exptl_crystal_colour red _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.17 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.691 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1072 _exptl_absorpt_coefficient_mu 3.997 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.649 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details 'semi-empirical from equiv.(prg.SADABS)' _exptl_special_details ; Bruker SMART APEX 3-circle diffractometer with CCD area detector, sealed X-ray tube, graphite monochromator. A hemisphere of the reciprocal space up to theta(max) = 25.00 deg was measured by omega scan frames with delta(omega) = 0.30 deg and 20 sec per frame, 2400 frames were recorded using program SMART (Bruker). Frame data evaluation and integration were done with program SAINT + (Bruker) Lattice parameters by least-squares refinement of the geometric parameters of the strongest reflections with program SAINT + (Bruker). Correction for absorption and crystal decay (insignificant) were applied by semi-empirical method from equivalents using program SADABS (G.M. Sheldrick, version of 2001, Univ. of Goettingen, Germany). Data reduction was done with program XPREP (BRUKER). ; _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 'Bruker SMART APEX CCD area detector' _diffrn_measurement_method '2400 omega scan frames, 0.3 deg, 20 sec' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% -0.0026 _diffrn_reflns_number 19720 _diffrn_reflns_av_R_equivalents 0.0468 _diffrn_reflns_av_sigmaI/netI 0.0353 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.69 _diffrn_reflns_theta_max 25.00 _reflns_number_total 3771 _reflns_number_gt 3516 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT +' _computing_data_reduction 'Bruker SAINT +, SADABS, XPREP' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP-3 vers.1.076(L.J. Faruggia, 1997)' _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^)+(0.0346P)^2^+16.4300P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0035(3) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 3771 _refine_ls_number_parameters 230 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0550 _refine_ls_R_factor_gt 0.0503 _refine_ls_wR_factor_ref 0.1075 _refine_ls_wR_factor_gt 0.1051 _refine_ls_goodness_of_fit_ref 1.046 _refine_ls_restrained_S_all 1.046 _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 Ni Ni 0.66959(7) 1.05558(8) 0.02917(5) 0.0298(2) Uani 1 1 d . . . Br Br 0.66565(7) 1.11231(7) 0.15673(4) 0.0499(2) Uani 1 1 d . . . Sb Sb 0.77031(3) 0.84802(4) 0.05819(2) 0.02788(16) Uani 1 1 d . . . C1 C 0.6526(7) 1.0338(8) -0.0850(4) 0.050(2) Uani 1 1 d . . . H1A H 0.7171 1.0027 -0.1069 0.06(3) Uiso 1 1 calc R . . H1B H 0.5832 0.9967 -0.1092 0.11(4) Uiso 1 1 calc R . . C2 C 0.6516(7) 1.1675(8) -0.0647(4) 0.051(2) Uani 1 1 d . . . C3 C 0.5714(7) 1.2013(9) -0.0186(5) 0.059(2) Uani 1 1 d . . . H3A H 0.4954 1.1780 -0.0375 0.089 Uiso 1 1 calc R . . H3B H 0.5791 1.2866 0.0065 0.089 Uiso 1 1 calc R . . C4 C 0.7456(10) 1.2575(10) -0.0775(7) 0.092(4) Uani 1 1 d . . . H4A H 0.7315 1.2954 -0.1279 0.139 Uiso 1 1 calc R . . H4B H 0.8135 1.2082 -0.0729 0.139 Uiso 1 1 calc R . . H4C H 0.7519 1.3265 -0.0397 0.139 Uiso 1 1 calc R . . C5 C 0.9232(5) 0.8735(6) 0.1304(4) 0.0316(14) Uani 1 1 d . . . C6 C 0.9694(6) 0.7731(7) 0.1780(4) 0.0413(17) Uani 1 1 d . . . H6 H 0.9342 0.6917 0.1782 0.050 Uiso 1 1 calc R . . C7 C 1.0686(7) 0.7953(10) 0.2253(4) 0.060(2) Uani 1 1 d . . . H7 H 1.1005 0.7279 0.2567 0.072 Uiso 1 1 calc R . . C8 C 1.1201(7) 0.9166(11) 0.2260(5) 0.066(3) Uani 1 1 d . . . H8 H 1.1857 0.9318 0.2584 0.079 Uiso 1 1 calc R . . C9 C 1.0740(7) 1.0142(10) 0.1786(5) 0.063(2) Uani 1 1 d . . . H9 H 1.1093 1.0955 0.1781 0.075 Uiso 1 1 calc R . . C10 C 0.9754(6) 0.9934(7) 0.1314(4) 0.0441(17) Uani 1 1 d . . . H10 H 0.9441 1.0611 0.1000 0.053 Uiso 1 1 calc R . . C11 C 0.6870(5) 0.7049(6) 0.1192(4) 0.0319(14) Uani 1 1 d . . . C12 C 0.6835(8) 0.5740(8) 0.1005(5) 0.058(2) Uani 1 1 d . . . H12 H 0.7202 0.5438 0.0607 0.069 Uiso 1 1 calc R . . C13 C 0.6255(9) 0.4864(9) 0.1405(6) 0.075(3) Uani 1 1 d . . . H13 H 0.6250 0.3973 0.1282 0.089 Uiso 1 1 calc R . . C14 C 0.5696(8) 0.5293(10) 0.1976(5) 0.068(3) Uani 1 1 d . . . H14 H 0.5295 0.4699 0.2234 0.082 Uiso 1 1 calc R . . C15 C 0.5718(9) 0.6581(10) 0.2169(6) 0.073(3) Uani 1 1 d . . . H15 H 0.5343 0.6875 0.2566 0.087 Uiso 1 1 calc R . . C16 C 0.6302(8) 0.7464(8) 0.1771(5) 0.061(2) Uani 1 1 d . . . H16 H 0.6308 0.8353 0.1901 0.074 Uiso 1 1 calc R . . C17 C 0.8194(6) 0.7253(7) -0.0299(4) 0.0385(16) Uani 1 1 d . . . C18 C 0.9287(7) 0.6890(9) -0.0314(5) 0.055(2) Uani 1 1 d . . . H18 H 0.9830 0.7165 0.0077 0.066 Uiso 1 1 calc R . . C19 C 0.9574(9) 0.6124(11) -0.0903(6) 0.078(3) Uani 1 1 d . . . H19 H 1.0313 0.5890 -0.0909 0.093 Uiso 1 1 calc R . . C20 C 0.8792(11) 0.5706(9) -0.1477(5) 0.072(3) Uani 1 1 d . . . H20 H 0.8998 0.5197 -0.1876 0.087 Uiso 1 1 calc R . . C21 C 0.7708(10) 0.6034(9) -0.1469(5) 0.072(3) Uani 1 1 d . . . H21 H 0.7167 0.5732 -0.1853 0.086 Uiso 1 1 calc R . . C22 C 0.7422(8) 0.6819(9) -0.0882(5) 0.058(2) Uani 1 1 d . . . H22 H 0.6684 0.7059 -0.0884 0.070 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 Ni 0.0278(5) 0.0272(4) 0.0346(4) 0.0053(3) 0.0049(3) 0.0027(3) Br 0.0725(6) 0.0367(4) 0.0424(4) -0.0042(3) 0.0146(4) 0.0083(4) Sb 0.0307(3) 0.0242(2) 0.0285(2) 0.00146(16) 0.00276(16) 0.00317(17) C1 0.058(5) 0.053(5) 0.038(4) 0.008(4) 0.003(4) 0.002(4) C2 0.064(5) 0.044(5) 0.045(4) 0.023(4) 0.010(4) 0.008(4) C3 0.058(5) 0.057(5) 0.060(5) 0.017(4) -0.004(4) 0.025(4) C4 0.130(10) 0.057(6) 0.099(8) 0.015(6) 0.050(8) -0.030(6) C5 0.030(3) 0.035(4) 0.031(3) -0.004(3) 0.010(3) -0.005(3) C6 0.041(4) 0.039(4) 0.044(4) 0.007(3) 0.004(3) -0.001(3) C7 0.040(5) 0.092(7) 0.044(4) 0.002(4) -0.008(4) 0.013(5) C8 0.033(5) 0.111(8) 0.054(5) -0.030(5) 0.001(4) -0.009(5) C9 0.048(5) 0.063(6) 0.079(6) -0.027(5) 0.017(5) -0.025(4) C10 0.040(4) 0.041(4) 0.051(4) -0.008(3) 0.006(3) -0.005(3) C11 0.031(4) 0.028(3) 0.034(3) 0.010(3) -0.005(3) -0.002(3) C12 0.079(6) 0.034(4) 0.060(5) -0.004(4) 0.011(4) -0.003(4) C13 0.108(8) 0.037(5) 0.075(6) 0.012(4) 0.000(6) -0.018(5) C14 0.066(6) 0.079(7) 0.057(5) 0.027(5) -0.001(5) -0.031(5) C15 0.091(7) 0.067(6) 0.067(6) 0.009(5) 0.037(5) -0.014(6) C16 0.097(7) 0.040(4) 0.054(5) 0.005(4) 0.033(5) -0.013(5) C17 0.054(5) 0.035(4) 0.027(3) -0.001(3) 0.006(3) 0.006(3) C18 0.059(5) 0.063(5) 0.045(4) -0.008(4) 0.009(4) 0.015(4) C19 0.087(7) 0.087(7) 0.065(6) -0.009(5) 0.030(6) 0.028(6) C20 0.130(10) 0.045(5) 0.047(5) -0.002(4) 0.030(6) 0.014(6) C21 0.113(9) 0.055(5) 0.044(5) -0.014(4) -0.002(5) -0.003(6) C22 0.069(6) 0.057(5) 0.047(4) -0.011(4) 0.001(4) 0.009(4) _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 Ni C2 1.990(7) . ? Ni C1 2.000(7) . ? Ni C3 2.012(7) . ? Ni Br 2.3189(12) . ? Ni Sb 2.4558(9) . ? Sb C5 2.123(6) . ? Sb C17 2.132(7) . ? Sb C11 2.138(6) . ? C1 C2 1.404(11) . ? C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? C2 C3 1.390(11) . ? C2 C4 1.503(12) . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C4 H4A 0.9600 . ? C4 H4B 0.9600 . ? C4 H4C 0.9600 . ? C5 C10 1.371(10) . ? C5 C6 1.389(9) . ? C6 C7 1.390(10) . ? C6 H6 0.9300 . ? C7 C8 1.381(14) . ? C7 H7 0.9300 . ? C8 C9 1.366(13) . ? C8 H8 0.9300 . ? C9 C10 1.381(11) . ? C9 H9 0.9300 . ? C10 H10 0.9300 . ? C11 C12 1.368(10) . ? C11 C16 1.368(10) . ? C12 C13 1.381(12) . ? C12 H12 0.9300 . ? C13 C14 1.354(14) . ? C13 H13 0.9300 . ? C14 C15 1.350(14) . ? C14 H14 0.9300 . ? C15 C16 1.388(11) . ? C15 H15 0.9300 . ? C16 H16 0.9300 . ? C17 C22 1.367(10) . ? C17 C18 1.382(10) . ? C18 C19 1.375(12) . ? C18 H18 0.9300 . ? C19 C20 1.359(14) . ? C19 H19 0.9300 . ? C20 C21 1.361(14) . ? C20 H20 0.9300 . ? C21 C22 1.382(12) . ? C21 H21 0.9300 . ? C22 H22 0.9300 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 Ni C1 41.2(3) . . ? C2 Ni C3 40.6(3) . . ? C1 Ni C3 71.7(3) . . ? C2 Ni Br 130.1(2) . . ? C1 Ni Br 169.4(2) . . ? C3 Ni Br 97.7(3) . . ? C2 Ni Sb 131.2(2) . . ? C1 Ni Sb 95.5(2) . . ? C3 Ni Sb 165.6(3) . . ? Br Ni Sb 94.91(4) . . ? C5 Sb C17 101.4(3) . . ? C5 Sb C11 102.6(2) . . ? C17 Sb C11 99.4(3) . . ? C5 Sb Ni 113.14(18) . . ? C17 Sb Ni 122.02(18) . . ? C11 Sb Ni 115.48(18) . . ? C2 C1 Ni 69.0(4) . . ? C2 C1 H1A 116.8 . . ? Ni C1 H1A 116.8 . . ? C2 C1 H1B 116.8 . . ? Ni C1 H1B 116.8 . . ? H1A C1 H1B 113.8 . . ? C3 C2 C1 114.7(8) . . ? C3 C2 C4 122.9(9) . . ? C1 C2 C4 121.1(8) . . ? C3 C2 Ni 70.6(4) . . ? C1 C2 Ni 69.8(4) . . ? C4 C2 Ni 117.9(7) . . ? C2 C3 Ni 68.8(4) . . ? C2 C3 H3A 116.8 . . ? Ni C3 H3A 116.8 . . ? C2 C3 H3B 116.8 . . ? Ni C3 H3B 116.8 . . ? H3A C3 H3B 113.8 . . ? C2 C4 H4A 109.5 . . ? C2 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C2 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? C10 C5 C6 119.6(6) . . ? C10 C5 Sb 118.9(5) . . ? C6 C5 Sb 121.5(5) . . ? C5 C6 C7 119.4(7) . . ? C5 C6 H6 120.3 . . ? C7 C6 H6 120.3 . . ? C8 C7 C6 120.5(8) . . ? C8 C7 H7 119.8 . . ? C6 C7 H7 119.8 . . ? C9 C8 C7 119.5(7) . . ? C9 C8 H8 120.3 . . ? C7 C8 H8 120.3 . . ? C8 C9 C10 120.6(8) . . ? C8 C9 H9 119.7 . . ? C10 C9 H9 119.7 . . ? C5 C10 C9 120.5(8) . . ? C5 C10 H10 119.8 . . ? C9 C10 H10 119.8 . . ? C12 C11 C16 118.3(7) . . ? C12 C11 Sb 122.8(6) . . ? C16 C11 Sb 118.8(5) . . ? C11 C12 C13 120.3(8) . . ? C11 C12 H12 119.8 . . ? C13 C12 H12 119.8 . . ? C14 C13 C12 120.6(9) . . ? C14 C13 H13 119.7 . . ? C12 C13 H13 119.7 . . ? C15 C14 C13 120.1(8) . . ? C15 C14 H14 120.0 . . ? C13 C14 H14 120.0 . . ? C14 C15 C16 119.6(9) . . ? C14 C15 H15 120.2 . . ? C16 C15 H15 120.2 . . ? C11 C16 C15 121.1(8) . . ? C11 C16 H16 119.4 . . ? C15 C16 H16 119.4 . . ? C22 C17 C18 117.9(7) . . ? C22 C17 Sb 120.0(6) . . ? C18 C17 Sb 122.1(5) . . ? C19 C18 C17 120.3(8) . . ? C19 C18 H18 119.9 . . ? C17 C18 H18 119.9 . . ? C20 C19 C18 120.8(10) . . ? C20 C19 H19 119.6 . . ? C18 C19 H19 119.6 . . ? C19 C20 C21 120.0(9) . . ? C19 C20 H20 120.0 . . ? C21 C20 H20 120.0 . . ? C20 C21 C22 119.2(9) . . ? C20 C21 H21 120.4 . . ? C22 C21 H21 120.4 . . ? C17 C22 C21 121.8(9) . . ? C17 C22 H22 119.1 . . ? C21 C22 H22 119.1 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C2 Ni Sb C5 103.2(4) . . . . ? C1 Ni Sb C5 126.2(3) . . . . ? C3 Ni Sb C5 153.0(11) . . . . ? Br Ni Sb C5 -55.97(18) . . . . ? C2 Ni Sb C17 -18.1(4) . . . . ? C1 Ni Sb C17 4.8(3) . . . . ? C3 Ni Sb C17 31.6(11) . . . . ? Br Ni Sb C17 -177.3(2) . . . . ? C2 Ni Sb C11 -138.9(4) . . . . ? C1 Ni Sb C11 -115.9(3) . . . . ? C3 Ni Sb C11 -89.1(11) . . . . ? Br Ni Sb C11 61.89(19) . . . . ? C3 Ni C1 C2 33.2(5) . . . . ? Br Ni C1 C2 38.3(16) . . . . ? Sb Ni C1 C2 -153.5(5) . . . . ? Ni C1 C2 C3 -56.0(6) . . . . ? Ni C1 C2 C4 111.1(8) . . . . ? C1 Ni C2 C3 126.9(8) . . . . ? Br Ni C2 C3 -44.4(6) . . . . ? Sb Ni C2 C3 163.1(4) . . . . ? C3 Ni C2 C1 -126.9(8) . . . . ? Br Ni C2 C1 -171.4(4) . . . . ? Sb Ni C2 C1 36.2(6) . . . . ? C1 Ni C2 C4 -115.4(9) . . . . ? C3 Ni C2 C4 117.7(10) . . . . ? Br Ni C2 C4 73.2(8) . . . . ? Sb Ni C2 C4 -79.2(8) . . . . ? C1 C2 C3 Ni 55.6(6) . . . . ? C4 C2 C3 Ni -111.2(8) . . . . ? C1 Ni C3 C2 -33.7(5) . . . . ? Br Ni C3 C2 147.3(5) . . . . ? Sb Ni C3 C2 -61.9(13) . . . . ? C17 Sb C5 C10 107.5(6) . . . . ? C11 Sb C5 C10 -150.0(5) . . . . ? Ni Sb C5 C10 -24.9(6) . . . . ? C17 Sb C5 C6 -74.4(6) . . . . ? C11 Sb C5 C6 28.1(6) . . . . ? Ni Sb C5 C6 153.2(5) . . . . ? C10 C5 C6 C7 -0.7(11) . . . . ? Sb C5 C6 C7 -178.8(6) . . . . ? C5 C6 C7 C8 1.0(12) . . . . ? C6 C7 C8 C9 -1.3(13) . . . . ? C7 C8 C9 C10 1.4(13) . . . . ? C6 C5 C10 C9 0.8(11) . . . . ? Sb C5 C10 C9 178.9(6) . . . . ? C8 C9 C10 C5 -1.1(12) . . . . ? C5 Sb C11 C12 -99.8(6) . . . . ? C17 Sb C11 C12 4.2(6) . . . . ? Ni Sb C11 C12 136.6(6) . . . . ? C5 Sb C11 C16 83.3(6) . . . . ? C17 Sb C11 C16 -172.6(6) . . . . ? Ni Sb C11 C16 -40.2(6) . . . . ? C16 C11 C12 C13 -1.2(12) . . . . ? Sb C11 C12 C13 -178.1(7) . . . . ? C11 C12 C13 C14 1.4(14) . . . . ? C12 C13 C14 C15 -1.3(15) . . . . ? C13 C14 C15 C16 1.0(16) . . . . ? C12 C11 C16 C15 0.9(13) . . . . ? Sb C11 C16 C15 177.9(7) . . . . ? C14 C15 C16 C11 -0.8(15) . . . . ? C5 Sb C17 C22 178.1(6) . . . . ? C11 Sb C17 C22 73.0(7) . . . . ? Ni Sb C17 C22 -55.1(7) . . . . ? C5 Sb C17 C18 -3.2(7) . . . . ? C11 Sb C17 C18 -108.3(6) . . . . ? Ni Sb C17 C18 123.6(6) . . . . ? C22 C17 C18 C19 0.4(13) . . . . ? Sb C17 C18 C19 -178.3(7) . . . . ? C17 C18 C19 C20 -0.4(15) . . . . ? C18 C19 C20 C21 -0.7(16) . . . . ? C19 C20 C21 C22 1.6(15) . . . . ? C18 C17 C22 C21 0.5(13) . . . . ? Sb C17 C22 C21 179.3(7) . . . . ? C20 C21 C22 C17 -1.6(14) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.725 _refine_diff_density_min -1.053 _refine_diff_density_rms 0.118 #===END #=== Data for pv0205 (compound 6a in the text) data_pva0205 _database_code_depnum_ccdc_archive 'CCDC 703653' _audit_creation_method SHELXL-97 _chemical_name_systematic ; Bromo-(tri-hapto-2-methyl-allyl)-(triphenylarsine) nickel (II) ; _chemical_name_common 'Bromo-(tri-hapto-2-methyl-allyl)-(triphenylarsine) nickel (ii)' _chemical_melting_point ? _chemical_formula_moiety 'C22 H22 As Br Ni' _chemical_formula_sum 'C22 H22 As Br Ni' _chemical_formula_weight 499.94 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' As As 0.0499 2.0058 '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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_int_tables_number 14 _symmetry_space_group_name_Hall '-P 2ybc' 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 12.021(2) _cell_length_b 9.9974(18) _cell_length_c 17.404(3) _cell_angle_alpha 90.00 _cell_angle_beta 98.246(3) _cell_angle_gamma 90.00 _cell_volume 2070.0(6) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 9309 _cell_measurement_theta_min 2.215 _cell_measurement_theta_max 24.983 _exptl_crystal_description irregular _exptl_crystal_colour 'dark red' _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.27 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.604 _exptl_crystal_F_000 1000 _exptl_absorpt_coefficient_mu 4.455 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.762 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details 'semi-empirical from equiv.(prg.SADABS)' _exptl_special_details ; Bruker SMART APEX 3-circle diffractometer with CCD area detector, sealed X-ray tube, graphite monochromator. A hemisphere of the reciprocal space up to theta(max) = 24.98 deg was measured by omega scan frames with delta(omega) = 0.30 deg and 15 sec per frame, 1900 frames were recorded using program SMART (Bruker). Frame data evaluation and integration were done with program SAINT + (Bruker) Lattice parameters by least-squares refinement of the geometric parameters of the strongest reflections with program SAINT + (Bruker). Correction for absorption and crystal decay (insignificant) were applied by semi-empirical method from equivalents using program SADABS (G.M. Sheldrick, version of 2001, Univ. of Goettingen, Germany). Data reduction was done with program XPREP (BRUKER). ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'fine-focus sealed tube' _diffrn_source_type 'Bruker SMART APEX' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART APEX CCD area detector' _diffrn_measurement_method '1900 omega scan frames,0.3 deg,15 sec' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% -0.0013 _diffrn_reflns_number 15210 _diffrn_reflns_av_R_equivalents 0.0254 _diffrn_reflns_av_sigmaI/netI 0.0242 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.36 _diffrn_reflns_theta_max 24.98 _reflns_number_total 3645 _reflns_number_gt 3209 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT +' _computing_data_reduction 'Bruker SAINT +, SADABS, XPREP' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP-3 vers.1.076(L.J. Faruggia, 1997)' _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^)+(0.0559P)^2^+0.7343P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0071(5) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 3645 _refine_ls_number_parameters 228 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0368 _refine_ls_R_factor_gt 0.0315 _refine_ls_wR_factor_ref 0.0849 _refine_ls_wR_factor_gt 0.0821 _refine_ls_goodness_of_fit_ref 1.055 _refine_ls_restrained_S_all 1.055 _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 Ni Ni 0.17339(3) 1.03851(4) 0.03158(2) 0.02630(13) Uani 1 1 d . . . As As 0.26669(2) 0.83846(3) 0.060426(16) 0.02445(12) Uani 1 1 d . . . Br Br 0.16811(3) 1.10717(3) 0.158951(19) 0.04555(14) Uani 1 1 d . . . C1 C 0.1590(3) 1.0201(4) -0.08339(18) 0.0428(8) Uani 1 1 d . . . H1A H 0.2248 0.9885 -0.1043 0.051 Uiso 1 1 calc R . . H1B H 0.0889 0.9833 -0.1094 0.051 Uiso 1 1 calc R . . C2 C 0.1581(3) 1.1546(3) -0.0626(2) 0.0420(8) Uani 1 1 d . . . C3 C 0.0762(3) 1.1895(4) -0.0175(2) 0.0486(9) Uani 1 1 d . . . H3A H -0.0009 1.1675 -0.0381 0.058 Uiso 1 1 calc R . . H3B H 0.0845 1.2756 0.0085 0.058 Uiso 1 1 calc R . . C4 C 0.2545(4) 1.2485(5) -0.0717(3) 0.0756(14) Uani 1 1 d . . . H4A H 0.3225 1.1979 -0.0707 0.113 Uiso 1 1 calc R . . H4B H 0.2634 1.3119 -0.0299 0.113 Uiso 1 1 calc R . . H4C H 0.2386 1.2952 -0.1203 0.113 Uiso 1 1 calc R . . C5 C 0.4083(2) 0.8650(3) 0.12769(17) 0.0281(6) Uani 1 1 d . . . C6 C 0.4611(3) 0.9879(3) 0.1256(2) 0.0397(8) Uani 1 1 d . . . H6 H 0.4286 1.0547 0.0926 0.048 Uiso 1 1 calc R . . C7 C 0.5624(3) 1.0115(4) 0.1729(2) 0.0514(10) Uani 1 1 d . . . H7 H 0.5981 1.0937 0.1711 0.062 Uiso 1 1 calc R . . C8 C 0.6097(3) 0.9134(5) 0.2222(2) 0.0545(11) Uani 1 1 d . . . H8 H 0.6773 0.9295 0.2541 0.065 Uiso 1 1 calc R . . C9 C 0.5577(3) 0.7914(4) 0.2248(2) 0.0508(10) Uani 1 1 d . . . H9 H 0.5905 0.7253 0.2582 0.061 Uiso 1 1 calc R . . C10 C 0.4568(3) 0.7665(4) 0.17777(18) 0.0375(8) Uani 1 1 d . . . H10 H 0.4217 0.6839 0.1798 0.045 Uiso 1 1 calc R . . C11 C 0.3103(3) 0.7304(3) -0.02321(16) 0.0312(7) Uani 1 1 d . . . C12 C 0.4211(3) 0.6959(4) -0.0265(2) 0.0493(9) Uani 1 1 d . . . H12 H 0.4776 0.7231 0.0125 0.059 Uiso 1 1 calc R . . C13 C 0.4473(4) 0.6204(5) -0.0884(2) 0.0646(12) Uani 1 1 d . . . H13 H 0.5220 0.5992 -0.0911 0.078 Uiso 1 1 calc R . . C14 C 0.3662(4) 0.5772(4) -0.1447(2) 0.0609(12) Uani 1 1 d . . . H14 H 0.3851 0.5259 -0.1855 0.073 Uiso 1 1 calc R . . C15 C 0.2559(4) 0.6090(4) -0.1419(2) 0.0593(11) Uani 1 1 d . . . H15 H 0.1998 0.5789 -0.1804 0.071 Uiso 1 1 calc R . . C16 C 0.2288(3) 0.6863(4) -0.0812(2) 0.0500(9) Uani 1 1 d . . . H16 H 0.1541 0.7089 -0.0797 0.060 Uiso 1 1 calc R . . C17 C 0.1895(2) 0.7063(3) 0.11578(16) 0.0284(6) Uani 1 1 d . . . C18 C 0.1302(4) 0.7482(4) 0.1727(2) 0.0573(11) Uani 1 1 d . . . H18 H 0.1284 0.8389 0.1843 0.069 Uiso 1 1 calc R . . C19 C 0.0730(4) 0.6593(4) 0.2135(3) 0.0722(14) Uani 1 1 d . . . H19 H 0.0342 0.6900 0.2526 0.087 Uiso 1 1 calc R . . C20 C 0.0735(4) 0.5284(4) 0.1965(2) 0.0625(12) Uani 1 1 d . . . H20 H 0.0340 0.4687 0.2233 0.075 Uiso 1 1 calc R . . C21 C 0.1308(4) 0.4831(4) 0.1406(3) 0.0703(13) Uani 1 1 d . . . H21 H 0.1311 0.3922 0.1294 0.084 Uiso 1 1 calc R . . C22 C 0.1897(4) 0.5723(4) 0.0996(2) 0.0564(10) Uani 1 1 d . . . H22 H 0.2293 0.5406 0.0612 0.068 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 Ni 0.0258(2) 0.0225(2) 0.0311(2) 0.00367(15) 0.00573(16) 0.00258(15) As 0.02724(19) 0.02008(19) 0.02570(18) 0.00043(11) 0.00268(12) 0.00218(12) Br 0.0674(3) 0.0323(2) 0.0390(2) -0.00471(14) 0.01464(17) 0.00762(16) C1 0.053(2) 0.043(2) 0.0332(17) 0.0061(15) 0.0061(15) 0.0022(17) C2 0.051(2) 0.037(2) 0.0379(18) 0.0150(14) 0.0063(16) 0.0056(16) C3 0.049(2) 0.043(2) 0.053(2) 0.0128(17) 0.0028(18) 0.0199(18) C4 0.095(4) 0.050(3) 0.090(3) 0.014(2) 0.041(3) -0.018(3) C5 0.0263(15) 0.0299(16) 0.0287(15) -0.0048(12) 0.0059(12) 0.0011(13) C6 0.0376(18) 0.0314(18) 0.051(2) -0.0053(15) 0.0093(15) -0.0013(15) C7 0.038(2) 0.051(2) 0.067(2) -0.024(2) 0.0122(18) -0.0129(18) C8 0.0295(19) 0.085(3) 0.048(2) -0.020(2) 0.0015(16) -0.009(2) C9 0.037(2) 0.075(3) 0.0382(18) 0.0082(18) -0.0022(15) 0.010(2) C10 0.0357(18) 0.0397(19) 0.0366(16) 0.0035(14) 0.0035(14) 0.0025(15) C11 0.0403(18) 0.0248(16) 0.0284(15) 0.0009(12) 0.0051(13) 0.0045(14) C12 0.049(2) 0.058(2) 0.0420(19) -0.0078(17) 0.0095(16) 0.0121(19) C13 0.072(3) 0.070(3) 0.058(3) -0.011(2) 0.031(2) 0.020(2) C14 0.106(4) 0.044(2) 0.038(2) -0.0058(17) 0.026(2) 0.011(2) C15 0.091(3) 0.046(2) 0.039(2) -0.0134(17) 0.002(2) 0.000(2) C16 0.053(2) 0.049(2) 0.0441(19) -0.0116(17) -0.0031(17) 0.0074(18) C17 0.0296(16) 0.0236(15) 0.0297(14) 0.0034(12) -0.0030(12) -0.0018(13) C18 0.094(3) 0.033(2) 0.052(2) 0.0016(17) 0.035(2) -0.009(2) C19 0.101(4) 0.057(3) 0.069(3) 0.015(2) 0.046(3) -0.012(3) C20 0.063(3) 0.061(3) 0.061(3) 0.022(2) -0.001(2) -0.029(2) C21 0.104(4) 0.031(2) 0.072(3) 0.005(2) -0.001(3) -0.027(2) C22 0.085(3) 0.0296(19) 0.057(2) -0.0023(17) 0.018(2) -0.006(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 Ni C1 1.992(3) . ? Ni C2 1.996(3) . ? Ni C3 2.022(3) . ? Ni As 2.3128(6) . ? Ni Br 2.3302(6) . ? As C5 1.941(3) . ? As C11 1.944(3) . ? As C17 1.947(3) . ? C1 C2 1.393(5) . ? C2 C3 1.390(5) . ? C2 C4 1.516(6) . ? C5 C10 1.387(4) . ? C5 C6 1.386(4) . ? C6 C7 1.388(5) . ? C7 C8 1.372(6) . ? C8 C9 1.373(6) . ? C9 C10 1.385(5) . ? C11 C16 1.375(5) . ? C11 C12 1.385(5) . ? C12 C13 1.388(5) . ? C13 C14 1.351(6) . ? C14 C15 1.370(6) . ? C15 C16 1.385(5) . ? C17 C18 1.367(5) . ? C17 C22 1.368(5) . ? C18 C19 1.381(5) . ? C19 C20 1.342(6) . ? C20 C21 1.347(6) . ? C21 C22 1.397(6) . ? 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 C1 Ni C2 40.89(14) . . ? C1 Ni C3 71.54(15) . . ? C2 Ni C3 40.49(14) . . ? C1 Ni As 96.19(10) . . ? C2 Ni As 131.75(11) . . ? C3 Ni As 166.03(12) . . ? C1 Ni Br 166.54(11) . . ? C2 Ni Br 126.75(11) . . ? C3 Ni Br 95.09(11) . . ? As Ni Br 97.279(18) . . ? C5 As C11 102.73(13) . . ? C5 As C17 103.49(12) . . ? C11 As C17 101.07(13) . . ? C5 As Ni 111.64(9) . . ? C11 As Ni 119.50(9) . . ? C17 As Ni 116.34(9) . . ? C2 C1 Ni 69.71(19) . . ? C3 C2 C1 114.9(3) . . ? C3 C2 C4 121.2(4) . . ? C1 C2 C4 122.4(4) . . ? C3 C2 Ni 70.74(19) . . ? C1 C2 Ni 69.40(18) . . ? C4 C2 Ni 117.6(3) . . ? C2 C3 Ni 68.77(19) . . ? C10 C5 C6 119.5(3) . . ? C10 C5 As 122.4(2) . . ? C6 C5 As 118.1(2) . . ? C5 C6 C7 120.1(3) . . ? C8 C7 C6 119.9(4) . . ? C7 C8 C9 120.3(3) . . ? C8 C9 C10 120.3(4) . . ? C5 C10 C9 119.8(3) . . ? C16 C11 C12 118.5(3) . . ? C16 C11 As 119.2(3) . . ? C12 C11 As 122.3(2) . . ? C13 C12 C11 119.7(4) . . ? C14 C13 C12 121.0(4) . . ? C13 C14 C15 120.1(4) . . ? C14 C15 C16 119.4(4) . . ? C11 C16 C15 121.2(4) . . ? C18 C17 C22 117.8(3) . . ? C18 C17 As 119.0(2) . . ? C22 C17 As 123.2(3) . . ? C17 C18 C19 121.7(4) . . ? C20 C19 C18 119.7(4) . . ? C19 C20 C21 120.4(4) . . ? C20 C21 C22 120.2(4) . . ? C17 C22 C21 120.2(4) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 24.98 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.714 _refine_diff_density_min -0.744 _refine_diff_density_rms 0.097 #===END #===END OF GLOBAL CIF