# Electronic Supplementary Material (ESI) for Chemical Science # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full 'Chemical Science' _journal_coden_cambridge 1475 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_name 'Charlene Tsay' _publ_contact_author_email ctsay@caltech.edu loop_ _publ_author_name 'Charlene Tsay' 'Jonas C. Peters' data_09401 _database_code_depnum_ccdc_archive 'CCDC 844852' #TrackingRef 'Ni combined cif.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common '[SiP(iPr)3]Ni-CH3' _chemical_melting_point 'not measured' _chemical_formula_moiety 'C37 H57 Ni P3 Si' _chemical_formula_sum 'C37 H57 Ni P3 Si' _chemical_formula_weight 681.54 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' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pbca loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 16.1008(13) _cell_length_b 16.9634(13) _cell_length_c 25.931(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 7082.4(10) _cell_formula_units_Z 8 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9997 _cell_measurement_theta_min 2.35 _cell_measurement_theta_max 30.73 _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.278 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2928 _exptl_absorpt_coefficient_mu 0.742 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7079 _exptl_absorpt_correction_T_max 0.8362 _exptl_absorpt_process_details 'SADABS (Sheldrick, 2008)' _exptl_special_details ; 'Siemens three-circle diffractometer, Bruker APEX CCD' ; _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 APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean 8.3 _diffrn_reflns_number 152436 _diffrn_reflns_av_R_equivalents 0.0595 _diffrn_reflns_av_sigmaI/netI 0.0264 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -37 _diffrn_reflns_limit_l_max 37 _diffrn_reflns_theta_min 1.57 _diffrn_reflns_theta_max 30.51 _reflns_number_total 10796 _reflns_number_gt 8926 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. Rigid bond restraints ('DELU') and similarity restraints on displacement amplitudes (SIMU) were applied globally using the default standard uncertainty values (0.01 square Angstroms and 0.08 square Angstroms, respectively). ; _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^)+(0.0395P)^2^+6.0909P] 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 10796 _refine_ls_number_parameters 392 _refine_ls_number_restraints 309 _refine_ls_R_factor_all 0.0482 _refine_ls_R_factor_gt 0.0356 _refine_ls_wR_factor_ref 0.0939 _refine_ls_wR_factor_gt 0.0848 _refine_ls_goodness_of_fit_ref 1.078 _refine_ls_restrained_S_all 1.062 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ni1 Ni 0.514415(12) 0.180815(10) 0.357191(7) 0.01142(5) Uani 1 1 d U . . C100 C 0.41753(9) 0.10138(8) 0.35299(6) 0.0143(3) Uani 1 1 d U . . H10A H 0.4339 0.0566 0.3314 0.021 Uiso 1 1 calc R . . H10B H 0.3688 0.1272 0.3379 0.021 Uiso 1 1 calc R . . H10C H 0.4039 0.0826 0.3877 0.021 Uiso 1 1 calc R . . Si1 Si 0.62072(3) 0.26372(2) 0.365105(16) 0.01264(8) Uani 1 1 d U . . P1 P 0.53401(2) 0.19872(2) 0.271352(15) 0.01275(8) Uani 1 1 d U . . C11 C 0.59004(9) 0.29199(8) 0.26015(6) 0.0141(3) Uani 1 1 d U . . C12 C 0.59232(10) 0.33296(9) 0.21313(6) 0.0181(3) Uani 1 1 d U . . H12 H 0.5592 0.3156 0.1850 0.022 Uiso 1 1 calc R . . C13 C 0.64303(11) 0.39904(10) 0.20759(7) 0.0219(3) Uani 1 1 d U . . H13 H 0.6449 0.4264 0.1756 0.026 Uiso 1 1 calc R . . C14 C 0.69096(11) 0.42496(9) 0.24897(7) 0.0227(3) Uani 1 1 d U . . H14 H 0.7263 0.4694 0.2450 0.027 Uiso 1 1 calc R . . C15 C 0.68718(10) 0.38593(9) 0.29608(7) 0.0193(3) Uani 1 1 d U . . H15 H 0.7191 0.4048 0.3243 0.023 Uiso 1 1 calc R . . C16 C 0.63693(9) 0.31917(8) 0.30256(6) 0.0141(3) Uani 1 1 d U . . C111 C 0.60176(10) 0.13078(9) 0.23211(6) 0.0158(3) Uani 1 1 d U . . H111 H 0.5829 0.0757 0.2393 0.019 Uiso 1 1 calc R . . C112 C 0.60018(11) 0.14176(10) 0.17328(6) 0.0211(3) Uani 1 1 d U . . H11A H 0.6192 0.1950 0.1646 0.032 Uiso 1 1 calc R . . H11B H 0.5434 0.1343 0.1606 0.032 Uiso 1 1 calc R . . H11C H 0.6370 0.1029 0.1571 0.032 Uiso 1 1 calc R . . C113 C 0.69208(10) 0.13682(9) 0.25019(7) 0.0198(3) Uani 1 1 d U . . H11D H 0.7251 0.0955 0.2335 0.030 Uiso 1 1 calc R . . H11E H 0.6945 0.1302 0.2877 0.030 Uiso 1 1 calc R . . H11F H 0.7144 0.1886 0.2409 0.030 Uiso 1 1 calc R . . C121 C 0.44198(10) 0.20294(9) 0.22819(6) 0.0157(3) Uani 1 1 d U . . H121 H 0.4611 0.2212 0.1935 0.019 Uiso 1 1 calc R . . C122 C 0.37708(10) 0.26151(9) 0.24768(7) 0.0197(3) Uani 1 1 d U . . H12A H 0.3311 0.2644 0.2230 0.030 Uiso 1 1 calc R . . H12B H 0.4025 0.3137 0.2513 0.030 Uiso 1 1 calc R . . H12C H 0.3561 0.2440 0.2813 0.030 Uiso 1 1 calc R . . C123 C 0.40399(10) 0.12031(10) 0.22178(6) 0.0190(3) Uani 1 1 d U . . H12D H 0.3867 0.1002 0.2555 0.028 Uiso 1 1 calc R . . H12E H 0.4454 0.0847 0.2068 0.028 Uiso 1 1 calc R . . H12F H 0.3556 0.1234 0.1989 0.028 Uiso 1 1 calc R . . P2 P 0.44340(2) 0.27759(2) 0.399069(15) 0.01376(8) Uani 1 1 d U . . C21 C 0.51691(10) 0.33458(9) 0.43857(6) 0.0151(3) Uani 1 1 d U . . C22 C 0.49709(10) 0.37497(9) 0.48404(6) 0.0183(3) Uani 1 1 d U . . H22 H 0.4414 0.3753 0.4961 0.022 Uiso 1 1 calc R . . C23 C 0.55856(11) 0.41469(9) 0.51171(6) 0.0206(3) Uani 1 1 d U . . H23 H 0.5448 0.4408 0.5430 0.025 Uiso 1 1 calc R . . C24 C 0.63979(11) 0.41618(9) 0.49359(6) 0.0200(3) Uani 1 1 d U . . H24 H 0.6815 0.4439 0.5121 0.024 Uiso 1 1 calc R . . C25 C 0.65983(10) 0.37676(9) 0.44808(6) 0.0171(3) Uani 1 1 d U . . H25 H 0.7153 0.3783 0.4357 0.020 Uiso 1 1 calc R . . C26 C 0.59966(10) 0.33494(8) 0.42026(6) 0.0146(3) Uani 1 1 d U . . C211 C 0.38881(10) 0.36172(9) 0.36486(6) 0.0178(3) Uani 1 1 d U . . H211 H 0.3506 0.3375 0.3389 0.021 Uiso 1 1 calc R . . C212 C 0.33553(11) 0.41529(10) 0.39931(7) 0.0242(3) Uani 1 1 d U . . H21A H 0.3706 0.4394 0.4259 0.036 Uiso 1 1 calc R . . H21B H 0.2919 0.3839 0.4158 0.036 Uiso 1 1 calc R . . H21C H 0.3101 0.4567 0.3782 0.036 Uiso 1 1 calc R . . C213 C 0.45050(11) 0.41297(10) 0.33479(7) 0.0222(3) Uani 1 1 d U . . H21D H 0.4199 0.4501 0.3129 0.033 Uiso 1 1 calc R . . H21E H 0.4855 0.3792 0.3131 0.033 Uiso 1 1 calc R . . H21F H 0.4855 0.4423 0.3591 0.033 Uiso 1 1 calc R . . C221 C 0.35968(10) 0.24961(9) 0.44561(6) 0.0180(3) Uani 1 1 d U . . H221 H 0.3448 0.2980 0.4656 0.022 Uiso 1 1 calc R . . C222 C 0.38953(11) 0.18777(9) 0.48431(7) 0.0222(3) Uani 1 1 d U . . H22A H 0.3438 0.1737 0.5075 0.033 Uiso 1 1 calc R . . H22B H 0.4357 0.2093 0.5045 0.033 Uiso 1 1 calc R . . H22C H 0.4082 0.1407 0.4657 0.033 Uiso 1 1 calc R . . C223 C 0.28055(11) 0.22128(10) 0.41792(7) 0.0241(3) Uani 1 1 d U . . H22D H 0.2916 0.1708 0.4009 0.036 Uiso 1 1 calc R . . H22E H 0.2639 0.2604 0.3921 0.036 Uiso 1 1 calc R . . H22F H 0.2358 0.2146 0.4432 0.036 Uiso 1 1 calc R . . P3 P 0.59870(2) 0.09814(2) 0.399178(15) 0.01299(8) Uani 1 1 d U . . C31 C 0.70844(9) 0.12838(9) 0.39369(6) 0.0146(3) Uani 1 1 d U . . C32 C 0.77725(10) 0.08047(9) 0.40463(6) 0.0174(3) Uani 1 1 d U . . H32 H 0.7698 0.0255 0.4100 0.021 Uiso 1 1 calc R . . C33 C 0.85652(10) 0.11308(10) 0.40765(6) 0.0191(3) Uani 1 1 d U . . H33 H 0.9028 0.0803 0.4152 0.023 Uiso 1 1 calc R . . C34 C 0.86800(10) 0.19342(10) 0.39973(6) 0.0191(3) Uani 1 1 d U . . H34 H 0.9217 0.2161 0.4033 0.023 Uiso 1 1 calc R . . C35 C 0.80033(10) 0.24052(9) 0.38653(6) 0.0171(3) Uani 1 1 d U . . H35 H 0.8089 0.2950 0.3798 0.021 Uiso 1 1 calc R . . C36 C 0.71987(9) 0.20921(9) 0.38301(6) 0.0143(3) Uani 1 1 d U . . C311 C 0.59265(10) 0.09043(9) 0.47167(6) 0.0168(3) Uani 1 1 d U . . H311 H 0.5340 0.0763 0.4804 0.020 Uiso 1 1 calc R . . C312 C 0.64861(11) 0.02803(10) 0.49699(6) 0.0208(3) Uani 1 1 d U . . H31A H 0.7070 0.0429 0.4924 0.031 Uiso 1 1 calc R . . H31B H 0.6387 -0.0233 0.4808 0.031 Uiso 1 1 calc R . . H31C H 0.6358 0.0247 0.5339 0.031 Uiso 1 1 calc R . . C313 C 0.61090(11) 0.16978(9) 0.49774(6) 0.0212(3) Uani 1 1 d U . . H31D H 0.5980 0.1661 0.5346 0.032 Uiso 1 1 calc R . . H31E H 0.5766 0.2110 0.4820 0.032 Uiso 1 1 calc R . . H31F H 0.6697 0.1829 0.4933 0.032 Uiso 1 1 calc R . . C321 C 0.60115(10) -0.00940(8) 0.38202(6) 0.0162(3) Uani 1 1 d U . . H321 H 0.6524 -0.0321 0.3979 0.019 Uiso 1 1 calc R . . C322 C 0.60783(11) -0.02235(9) 0.32396(6) 0.0200(3) Uani 1 1 d U . . H32A H 0.6128 -0.0789 0.3168 0.030 Uiso 1 1 calc R . . H32B H 0.6570 0.0051 0.3108 0.030 Uiso 1 1 calc R . . H32C H 0.5580 -0.0016 0.3070 0.030 Uiso 1 1 calc R . . C323 C 0.52714(11) -0.05600(9) 0.40352(7) 0.0204(3) Uani 1 1 d U . . H32D H 0.4758 -0.0372 0.3874 0.031 Uiso 1 1 calc R . . H32E H 0.5239 -0.0484 0.4409 0.031 Uiso 1 1 calc R . . H32F H 0.5345 -0.1122 0.3959 0.031 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ni1 0.01189(9) 0.01011(9) 0.01225(9) 0.00004(6) 0.00026(6) -0.00083(6) C100 0.0151(7) 0.0144(6) 0.0133(7) -0.0016(5) -0.0008(5) 0.0012(5) Si1 0.01342(19) 0.01102(17) 0.01347(19) -0.00023(13) 0.00030(14) -0.00099(14) P1 0.01295(17) 0.01263(16) 0.01268(17) 0.00087(12) -0.00044(13) -0.00089(13) C11 0.0129(7) 0.0123(6) 0.0169(7) 0.0011(5) 0.0016(5) 0.0001(5) C12 0.0194(7) 0.0180(7) 0.0169(7) 0.0033(5) -0.0011(6) 0.0002(6) C13 0.0247(8) 0.0189(7) 0.0221(8) 0.0090(6) -0.0004(6) -0.0023(6) C14 0.0246(8) 0.0162(7) 0.0275(9) 0.0061(6) -0.0008(7) -0.0061(6) C15 0.0195(8) 0.0153(7) 0.0233(8) 0.0020(6) -0.0014(6) -0.0032(5) C16 0.0141(7) 0.0122(6) 0.0160(7) 0.0011(5) 0.0012(5) 0.0007(5) C111 0.0164(7) 0.0143(6) 0.0167(7) -0.0006(5) 0.0002(5) 0.0005(5) C112 0.0254(8) 0.0223(8) 0.0155(7) -0.0005(6) 0.0033(6) 0.0013(6) C113 0.0169(7) 0.0193(7) 0.0231(8) -0.0017(6) 0.0013(6) 0.0011(6) C121 0.0145(7) 0.0180(7) 0.0147(7) 0.0017(5) -0.0017(5) -0.0011(5) C122 0.0175(7) 0.0206(7) 0.0209(8) 0.0008(6) -0.0032(6) 0.0009(6) C123 0.0179(7) 0.0219(7) 0.0172(7) -0.0009(6) -0.0021(6) -0.0036(6) P2 0.01387(18) 0.01174(16) 0.01568(18) -0.00160(12) 0.00158(13) -0.00074(13) C21 0.0167(7) 0.0117(6) 0.0168(7) 0.0009(5) 0.0013(5) -0.0012(5) C22 0.0189(7) 0.0165(7) 0.0195(8) -0.0030(5) 0.0037(6) -0.0020(5) C23 0.0256(8) 0.0177(7) 0.0186(8) -0.0051(5) 0.0014(6) -0.0022(6) C24 0.0227(8) 0.0174(7) 0.0198(8) -0.0045(5) -0.0020(6) -0.0039(6) C25 0.0172(7) 0.0149(6) 0.0191(7) -0.0013(5) 0.0001(6) -0.0024(5) C26 0.0177(7) 0.0114(6) 0.0147(7) 0.0002(5) -0.0004(5) -0.0001(5) C211 0.0180(7) 0.0144(7) 0.0211(8) -0.0009(5) 0.0001(6) 0.0030(5) C212 0.0246(8) 0.0188(7) 0.0292(9) -0.0029(6) 0.0026(7) 0.0066(6) C213 0.0228(8) 0.0179(7) 0.0259(8) 0.0032(6) 0.0027(7) 0.0031(6) C221 0.0172(7) 0.0159(7) 0.0210(7) -0.0023(5) 0.0054(6) -0.0012(5) C222 0.0254(8) 0.0181(7) 0.0231(8) 0.0014(6) 0.0073(7) -0.0022(6) C223 0.0180(8) 0.0237(8) 0.0305(9) -0.0065(6) 0.0056(7) -0.0040(6) P3 0.01446(17) 0.01131(16) 0.01319(17) 0.00116(12) -0.00021(13) -0.00006(13) C31 0.0148(7) 0.0164(6) 0.0125(6) -0.0005(5) 0.0001(5) 0.0007(5) C32 0.0192(7) 0.0175(7) 0.0154(7) 0.0009(5) -0.0011(6) 0.0025(5) C33 0.0154(7) 0.0257(8) 0.0164(7) -0.0006(6) -0.0012(6) 0.0046(6) C34 0.0142(7) 0.0271(8) 0.0160(7) -0.0037(6) 0.0001(6) -0.0013(6) C35 0.0172(7) 0.0186(7) 0.0157(7) -0.0022(5) 0.0012(5) -0.0018(5) C36 0.0154(7) 0.0163(7) 0.0111(6) -0.0010(5) -0.0001(5) -0.0003(5) C311 0.0193(7) 0.0162(7) 0.0149(7) 0.0018(5) 0.0002(6) -0.0005(5) C312 0.0250(8) 0.0206(7) 0.0170(7) 0.0052(6) -0.0019(6) 0.0018(6) C313 0.0287(9) 0.0190(7) 0.0158(7) -0.0005(6) 0.0002(6) -0.0011(6) C321 0.0184(7) 0.0122(6) 0.0180(7) 0.0013(5) -0.0010(6) 0.0007(5) C322 0.0244(8) 0.0160(7) 0.0196(8) -0.0010(5) 0.0019(6) 0.0012(6) C323 0.0257(8) 0.0152(7) 0.0204(8) 0.0021(5) -0.0006(6) -0.0037(6) _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 C100 2.0643(15) . ? Ni1 Si1 2.2247(5) . ? Ni1 P3 2.2346(4) . ? Ni1 P1 2.2686(5) . ? Ni1 P2 2.2764(4) . ? Si1 C16 1.8929(15) . ? Si1 C36 1.9024(16) . ? Si1 C26 1.9026(15) . ? P1 C11 1.8443(15) . ? P1 C121 1.8584(16) . ? P1 C111 1.8850(16) . ? C11 C12 1.404(2) . ? C11 C16 1.412(2) . ? C12 C13 1.394(2) . ? C13 C14 1.393(2) . ? C14 C15 1.391(2) . ? C15 C16 1.402(2) . ? C111 C113 1.531(2) . ? C111 C112 1.537(2) . ? C121 C122 1.528(2) . ? C121 C123 1.538(2) . ? P2 C21 1.8398(16) . ? P2 C221 1.8704(16) . ? P2 C211 1.8962(16) . ? C21 C22 1.400(2) . ? C21 C26 1.414(2) . ? C22 C23 1.396(2) . ? C23 C24 1.390(2) . ? C24 C25 1.394(2) . ? C25 C26 1.401(2) . ? C211 C213 1.533(2) . ? C211 C212 1.536(2) . ? C221 C222 1.529(2) . ? C221 C223 1.539(2) . ? P3 C31 1.8454(16) . ? P3 C321 1.8782(15) . ? P3 C311 1.8867(16) . ? C31 C32 1.403(2) . ? C31 C36 1.411(2) . ? C32 C33 1.393(2) . ? C33 C34 1.391(2) . ? C34 C35 1.394(2) . ? C35 C36 1.403(2) . ? C311 C313 1.535(2) . ? C311 C312 1.537(2) . ? C321 C322 1.525(2) . ? C321 C323 1.535(2) . ? 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 C100 Ni1 Si1 177.33(4) . . ? C100 Ni1 P3 94.29(4) . . ? Si1 Ni1 P3 83.376(17) . . ? C100 Ni1 P1 98.09(4) . . ? Si1 Ni1 P1 84.196(16) . . ? P3 Ni1 P1 118.530(16) . . ? C100 Ni1 P2 96.68(4) . . ? Si1 Ni1 P2 83.484(16) . . ? P3 Ni1 P2 121.683(17) . . ? P1 Ni1 P2 116.192(16) . . ? C16 Si1 C36 109.56(7) . . ? C16 Si1 C26 110.68(7) . . ? C36 Si1 C26 105.94(7) . . ? C16 Si1 Ni1 109.95(5) . . ? C36 Si1 Ni1 111.15(5) . . ? C26 Si1 Ni1 109.49(5) . . ? C11 P1 C121 105.19(7) . . ? C11 P1 C111 99.00(7) . . ? C121 P1 C111 99.20(7) . . ? C11 P1 Ni1 109.72(5) . . ? C121 P1 Ni1 119.03(5) . . ? C111 P1 Ni1 121.89(5) . . ? C12 C11 C16 120.06(14) . . ? C12 C11 P1 125.06(12) . . ? C16 C11 P1 114.77(11) . . ? C13 C12 C11 120.19(15) . . ? C14 C13 C12 119.93(15) . . ? C15 C14 C13 120.14(15) . . ? C14 C15 C16 121.00(15) . . ? C15 C16 C11 118.63(14) . . ? C15 C16 Si1 125.71(12) . . ? C11 C16 Si1 115.57(11) . . ? C113 C111 C112 108.14(13) . . ? C113 C111 P1 110.09(11) . . ? C112 C111 P1 116.88(11) . . ? C122 C121 C123 110.88(13) . . ? C122 C121 P1 111.78(11) . . ? C123 C121 P1 110.30(10) . . ? C21 P2 C221 103.75(7) . . ? C21 P2 C211 99.39(7) . . ? C221 P2 C211 99.14(7) . . ? C21 P2 Ni1 108.75(5) . . ? C221 P2 Ni1 119.13(5) . . ? C211 P2 Ni1 123.54(5) . . ? C22 C21 C26 119.68(14) . . ? C22 C21 P2 125.40(12) . . ? C26 C21 P2 114.92(11) . . ? C23 C22 C21 120.48(15) . . ? C24 C23 C22 120.16(15) . . ? C23 C24 C25 119.67(15) . . ? C24 C25 C26 121.25(15) . . ? C25 C26 C21 118.73(14) . . ? C25 C26 Si1 125.83(12) . . ? C21 C26 Si1 114.68(11) . . ? C213 C211 C212 108.79(13) . . ? C213 C211 P2 111.37(11) . . ? C212 C211 P2 115.60(12) . . ? C222 C221 C223 110.61(14) . . ? C222 C221 P2 111.78(11) . . ? C223 C221 P2 112.01(12) . . ? C31 P3 C321 103.39(7) . . ? C31 P3 C311 98.36(7) . . ? C321 P3 C311 99.77(7) . . ? C31 P3 Ni1 111.68(5) . . ? C321 P3 Ni1 120.46(5) . . ? C311 P3 Ni1 119.84(5) . . ? C32 C31 C36 119.98(14) . . ? C32 C31 P3 125.42(12) . . ? C36 C31 P3 114.21(11) . . ? C33 C32 C31 120.32(14) . . ? C34 C33 C32 120.17(15) . . ? C33 C34 C35 119.61(15) . . ? C34 C35 C36 121.39(15) . . ? C35 C36 C31 118.39(14) . . ? C35 C36 Si1 127.35(12) . . ? C31 C36 Si1 114.26(11) . . ? C313 C311 C312 107.67(13) . . ? C313 C311 P3 111.61(10) . . ? C312 C311 P3 116.29(11) . . ? C322 C321 C323 109.82(13) . . ? C322 C321 P3 112.03(10) . . ? C323 C321 P3 113.45(11) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 30.51 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.697 _refine_diff_density_min -0.360 _refine_diff_density_rms 0.079 ####################################################### # Compound 2a: {[SiP(iPr)3]Ni-N2}{BArF} # ####################################################### data_09450 _database_code_depnum_ccdc_archive 'CCDC 844853' #TrackingRef 'Ni combined cif.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common {[SiP(iPr)3]Ni-N2}{BArF} _chemical_melting_point 'not measured' _chemical_formula_moiety 'C36 H54 N2 Ni P3 Si, C32 H12 B F24' _chemical_formula_sum 'C77.75 H75.75 B F24 N2 Ni P3 Si' _chemical_formula_weight 1684.67 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' N N 0.0061 0.0033 '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' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 47.534(4) _cell_length_b 13.9003(11) _cell_length_c 30.423(2) _cell_angle_alpha 90.00 _cell_angle_beta 128.6300(10) _cell_angle_gamma 90.00 _cell_volume 15703(2) _cell_formula_units_Z 8 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9748 _cell_measurement_theta_min 2.49 _cell_measurement_theta_max 30.72 _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.425 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 6914 _exptl_absorpt_coefficient_mu 0.425 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8158 _exptl_absorpt_correction_T_max 0.9199 _exptl_absorpt_process_details 'SADABS (Sheldrick, 2008)' _exptl_special_details ; 'Siemens three-circle diffractometer, Bruker APEX CCD' ; _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' _diffrn_measurement_method 'omega and phi scans' _diffrn_detector_area_resol_mean 8.3 _diffrn_reflns_number 211753 _diffrn_reflns_av_R_equivalents 0.0677 _diffrn_reflns_av_sigmaI/netI 0.0377 _diffrn_reflns_limit_h_min -66 _diffrn_reflns_limit_h_max 66 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -42 _diffrn_reflns_limit_l_max 42 _diffrn_reflns_theta_min 1.10 _diffrn_reflns_theta_max 30.03 _reflns_number_total 22976 _reflns_number_gt 17358 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 3.0 (Bruker-AXS, 2008)' _computing_cell_refinement 'SAINT 7.46A (Bruker-AXS, 2008)' _computing_data_reduction 'SAINT 7.46A (Bruker-AXS, 2008)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. One solvent benzene molecule was disorded around a mirror plane and required the use of more stringent constraints and restraints. A rigid group constraint (AFIX 66) was used to refine its parameter. Rigid bond restraints (DELU) were applied with half the default standard uncertainty (0.005 square Angstroms instead of the 0.01 default). The anisotropic displacement parameters were also restrained to be approximately isotropic (ISOR) with a standard uncertainty of 0.03 square Angstroms. checkCIF reports one level A alert (PLAT213_ALERT_2_A) due to a high ratio of maximum to minimum anisotropic displacement parameters (ADP) for atom C34B. As this atom is part of the benzene molecule that is highly disordered around a mirror plane (see above) and required the use of a rigid group constraint (AFIX 66), we did not deem it appropriate to model any further disorder. ; _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^)+(0.0558P)^2^+32.5934P] 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 22976 _refine_ls_number_parameters 1037 _refine_ls_number_restraints 48 _refine_ls_R_factor_all 0.0680 _refine_ls_R_factor_gt 0.0464 _refine_ls_wR_factor_ref 0.1291 _refine_ls_wR_factor_gt 0.1140 _refine_ls_goodness_of_fit_ref 1.021 _refine_ls_restrained_S_all 1.024 _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 0.136576(6) 0.132119(17) 0.198400(10) 0.01432(6) Uani 1 1 d . . . N1 N 0.17091(4) 0.13417(12) 0.18538(7) 0.0186(3) Uani 1 1 d . . . N2 N 0.19054(5) 0.13504(14) 0.17803(8) 0.0284(4) Uani 1 1 d . . . Si1 Si 0.095113(13) 0.12838(4) 0.21164(2) 0.01534(10) Uani 1 1 d . . . P1 P 0.089009(12) 0.18843(3) 0.11060(2) 0.01495(9) Uani 1 1 d . . . C11 C 0.05621(5) 0.24532(14) 0.11529(8) 0.0181(3) Uani 1 1 d . . . C12 C 0.03073(5) 0.31474(15) 0.07778(9) 0.0220(4) Uani 1 1 d . . . H12 H 0.0299 0.3366 0.0474 0.026 Uiso 1 1 calc R . . C13 C 0.00680(6) 0.35122(16) 0.08538(10) 0.0270(4) Uani 1 1 d . . . H13 H -0.0100 0.3993 0.0606 0.032 Uiso 1 1 calc R . . C14 C 0.00730(6) 0.31813(16) 0.12886(10) 0.0275(4) Uani 1 1 d . . . H14 H -0.0096 0.3422 0.1330 0.033 Uiso 1 1 calc R . . C15 C 0.03252(5) 0.24989(15) 0.16641(9) 0.0220(4) Uani 1 1 d . . . H15 H 0.0329 0.2280 0.1963 0.026 Uiso 1 1 calc R . . C16 C 0.05751(5) 0.21307(14) 0.16051(8) 0.0172(3) Uani 1 1 d . . . C111 C 0.06048(5) 0.10396(14) 0.05015(8) 0.0173(3) Uani 1 1 d . . . H111 H 0.0767 0.0702 0.0448 0.021 Uiso 1 1 calc R . . C112 C 0.04376(5) 0.02710(15) 0.06333(8) 0.0214(4) Uani 1 1 d . . . H11A H 0.0258 0.0568 0.0651 0.032 Uiso 1 1 calc R . . H11B H 0.0626 -0.0029 0.0996 0.032 Uiso 1 1 calc R . . H11C H 0.0321 -0.0220 0.0337 0.032 Uiso 1 1 calc R . . C113 C 0.03069(5) 0.15275(15) -0.00605(8) 0.0225(4) Uani 1 1 d . . . H11D H 0.0182 0.1043 -0.0360 0.034 Uiso 1 1 calc R . . H11E H 0.0414 0.2012 -0.0150 0.034 Uiso 1 1 calc R . . H11F H 0.0135 0.1839 -0.0030 0.034 Uiso 1 1 calc R . . C121 C 0.09993(5) 0.28168(14) 0.07917(8) 0.0182(3) Uani 1 1 d . . . H121 H 0.0767 0.3135 0.0483 0.022 Uiso 1 1 calc R . . C122 C 0.12463(6) 0.36021(14) 0.12151(9) 0.0225(4) Uani 1 1 d . . . H12A H 0.1479 0.3320 0.1521 0.034 Uiso 1 1 calc R . . H12B H 0.1136 0.3888 0.1369 0.034 Uiso 1 1 calc R . . H12C H 0.1282 0.4100 0.1026 0.034 Uiso 1 1 calc R . . C123 C 0.11585(5) 0.23874(15) 0.05231(9) 0.0226(4) Uani 1 1 d . . . H12D H 0.1201 0.2903 0.0352 0.034 Uiso 1 1 calc R . . H12E H 0.0989 0.1920 0.0233 0.034 Uiso 1 1 calc R . . H12F H 0.1387 0.2065 0.0813 0.034 Uiso 1 1 calc R . . P2 P 0.141007(12) -0.03154(3) 0.21900(2) 0.01615(9) Uani 1 1 d . . . C21 C 0.09717(5) -0.07043(14) 0.19721(8) 0.0174(3) Uani 1 1 d . . . C22 C 0.08329(5) -0.16368(15) 0.18051(9) 0.0220(4) Uani 1 1 d . . . H22 H 0.0969 -0.2127 0.1798 0.026 Uiso 1 1 calc R . . C23 C 0.04952(6) -0.18465(16) 0.16491(9) 0.0258(4) Uani 1 1 d . . . H23 H 0.0400 -0.2479 0.1532 0.031 Uiso 1 1 calc R . . C24 C 0.02955(6) -0.11343(16) 0.16643(9) 0.0261(4) Uani 1 1 d . . . H24 H 0.0067 -0.1284 0.1564 0.031 Uiso 1 1 calc R . . C25 C 0.04311(5) -0.02043(15) 0.18269(9) 0.0227(4) Uani 1 1 d . . . H25 H 0.0294 0.0281 0.1836 0.027 Uiso 1 1 calc R . . C26 C 0.07694(5) 0.00242(14) 0.19785(8) 0.0180(3) Uani 1 1 d . . . C211 C 0.17214(5) -0.08430(14) 0.29185(8) 0.0194(4) Uani 1 1 d . . . H211 H 0.1972 -0.0656 0.3081 0.023 Uiso 1 1 calc R . . C212 C 0.16502(6) -0.04479(15) 0.33123(9) 0.0237(4) Uani 1 1 d . . . H21A H 0.1403 -0.0604 0.3159 0.036 Uiso 1 1 calc R . . H21B H 0.1682 0.0252 0.3343 0.036 Uiso 1 1 calc R . . H21C H 0.1820 -0.0740 0.3685 0.036 Uiso 1 1 calc R . . C213 C 0.17087(6) -0.19502(15) 0.29254(9) 0.0250(4) Uani 1 1 d . . . H21D H 0.1878 -0.2181 0.3314 0.038 Uiso 1 1 calc R . . H21E H 0.1775 -0.2215 0.2703 0.038 Uiso 1 1 calc R . . H21F H 0.1465 -0.2159 0.2764 0.038 Uiso 1 1 calc R . . C221 C 0.15105(5) -0.11120(15) 0.18076(9) 0.0216(4) Uani 1 1 d . . . H221 H 0.1455 -0.1785 0.1848 0.026 Uiso 1 1 calc R . . C222 C 0.12738(6) -0.09010(17) 0.11765(9) 0.0279(4) Uani 1 1 d . . . H22A H 0.1320 -0.0244 0.1118 0.042 Uiso 1 1 calc R . . H22B H 0.1020 -0.0965 0.1011 0.042 Uiso 1 1 calc R . . H22C H 0.1330 -0.1359 0.0997 0.042 Uiso 1 1 calc R . . C223 C 0.19121(6) -0.10873(16) 0.20771(10) 0.0280(4) Uani 1 1 d . . . H22D H 0.1957 -0.1530 0.1876 0.042 Uiso 1 1 calc R . . H22E H 0.2056 -0.1284 0.2472 0.042 Uiso 1 1 calc R . . H22F H 0.1979 -0.0433 0.2055 0.042 Uiso 1 1 calc R . . P3 P 0.164799(12) 0.23828(3) 0.27310(2) 0.01608(9) Uani 1 1 d . . . C31 C 0.15202(5) 0.20552(13) 0.31678(8) 0.0177(3) Uani 1 1 d . . . C32 C 0.17321(6) 0.21959(15) 0.37496(8) 0.0222(4) Uani 1 1 d . . . H32 H 0.1962 0.2493 0.3949 0.027 Uiso 1 1 calc R . . C33 C 0.16065(6) 0.19007(16) 0.40355(9) 0.0253(4) Uani 1 1 d . . . H33 H 0.1754 0.1978 0.4432 0.030 Uiso 1 1 calc R . . C34 C 0.12654(6) 0.14905(16) 0.37424(9) 0.0263(4) Uani 1 1 d . . . H34 H 0.1178 0.1306 0.3938 0.032 Uiso 1 1 calc R . . C35 C 0.10527(6) 0.13507(15) 0.31627(9) 0.0229(4) Uani 1 1 d . . . H35 H 0.0820 0.1071 0.2965 0.027 Uiso 1 1 calc R . . C36 C 0.11791(5) 0.16205(13) 0.28700(8) 0.0177(3) Uani 1 1 d . . . C311 C 0.15631(5) 0.37134(14) 0.26472(8) 0.0190(4) Uani 1 1 d . . . H311 H 0.1631 0.3965 0.2417 0.023 Uiso 1 1 calc R . . C312 C 0.11645(5) 0.39487(15) 0.23332(9) 0.0221(4) Uani 1 1 d . . . H31A H 0.1088 0.3692 0.2544 0.033 Uiso 1 1 calc R . . H31B H 0.1020 0.3657 0.1958 0.033 Uiso 1 1 calc R . . H31C H 0.1131 0.4648 0.2297 0.033 Uiso 1 1 calc R . . C313 C 0.17881(6) 0.42565(15) 0.32098(9) 0.0265(4) Uani 1 1 d . . . H31D H 0.1737 0.4947 0.3140 0.040 Uiso 1 1 calc R . . H31E H 0.2045 0.4145 0.3404 0.040 Uiso 1 1 calc R . . H31F H 0.1726 0.4025 0.3444 0.040 Uiso 1 1 calc R . . C321 C 0.21491(5) 0.23278(14) 0.32079(8) 0.0203(4) Uani 1 1 d . . . H321 H 0.2239 0.2646 0.3569 0.024 Uiso 1 1 calc R . . C322 C 0.22844(5) 0.12850(15) 0.33469(9) 0.0242(4) Uani 1 1 d . . . H32A H 0.2211 0.0959 0.3004 0.036 Uiso 1 1 calc R . . H32B H 0.2181 0.0949 0.3500 0.036 Uiso 1 1 calc R . . H32C H 0.2548 0.1281 0.3626 0.036 Uiso 1 1 calc R . . C323 C 0.23065(6) 0.28853(16) 0.29682(10) 0.0267(4) Uani 1 1 d . . . H32D H 0.2569 0.2812 0.3221 0.040 Uiso 1 1 calc R . . H32E H 0.2245 0.3568 0.2935 0.040 Uiso 1 1 calc R . . H32F H 0.2206 0.2630 0.2596 0.040 Uiso 1 1 calc R . . B1 B 0.13411(6) 0.62902(16) 0.01737(9) 0.0182(4) Uani 1 1 d . . . C411 C 0.16849(5) 0.56817(14) 0.03187(8) 0.0181(3) Uani 1 1 d . . . C412 C 0.18800(5) 0.59217(14) 0.01306(8) 0.0179(3) Uani 1 1 d . . . H412 H 0.1824 0.6504 -0.0073 0.021 Uiso 1 1 calc R . . C413 C 0.21536(5) 0.53363(14) 0.02313(8) 0.0178(3) Uani 1 1 d . . . C414 C 0.23489(5) 0.56482(15) 0.00142(9) 0.0224(4) Uani 1 1 d . . . F11 F 0.23915(4) 0.66089(10) 0.00403(7) 0.0386(3) Uani 1 1 d . . . F12 F 0.21713(4) 0.54057(12) -0.05255(6) 0.0381(3) Uani 1 1 d . . . F13 F 0.26784(3) 0.52660(10) 0.03025(6) 0.0287(3) Uani 1 1 d . . . C415 C 0.22422(5) 0.44690(14) 0.05182(8) 0.0190(4) Uani 1 1 d . . . H415 H 0.2427 0.4068 0.0583 0.023 Uiso 1 1 calc R . . C416 C 0.20515(5) 0.42078(14) 0.07072(8) 0.0189(4) Uani 1 1 d . . . C417 C 0.21297(5) 0.32740(15) 0.10139(9) 0.0232(4) Uani 1 1 d . . . F14 F 0.19161(4) 0.25541(9) 0.06675(6) 0.0352(3) Uani 1 1 d . . . F15 F 0.24688(3) 0.29738(10) 0.12834(6) 0.0348(3) Uani 1 1 d . . . F16 F 0.20772(4) 0.33341(10) 0.13990(6) 0.0382(3) Uani 1 1 d . . . C418 C 0.17797(5) 0.47938(14) 0.06068(8) 0.0188(4) Uani 1 1 d . . . H418 H 0.1652 0.4590 0.0737 0.023 Uiso 1 1 calc R . . C421 C 0.09954(5) 0.58209(14) -0.04226(8) 0.0180(3) Uani 1 1 d . . . C422 C 0.09110(5) 0.61425(14) -0.09311(8) 0.0198(4) Uani 1 1 d . . . H422 H 0.1041 0.6671 -0.0922 0.024 Uiso 1 1 calc R . . C423 C 0.06447(5) 0.57153(15) -0.14455(8) 0.0213(4) Uani 1 1 d . . . C424 C 0.05713(6) 0.61218(18) -0.19633(9) 0.0305(5) Uani 1 1 d . . . F21 F 0.08751(4) 0.62937(11) -0.18921(6) 0.0378(3) Uani 1 1 d . . . F22 F 0.03993(4) 0.69736(13) -0.21110(7) 0.0482(4) Uani 1 1 d . . . F23 F 0.03682(5) 0.55448(14) -0.24121(6) 0.0552(5) Uani 1 1 d . . . C425 C 0.04445(5) 0.49464(15) -0.14796(9) 0.0236(4) Uani 1 1 d . . . H425 H 0.0261 0.4657 -0.1831 0.028 Uiso 1 1 calc R . . C426 C 0.05220(5) 0.46158(15) -0.09839(9) 0.0232(4) Uani 1 1 d . . . C427 C 0.03125(6) 0.37890(18) -0.10051(10) 0.0361(6) Uani 1 1 d . . . F24 F -0.00030(5) 0.36726(18) -0.15094(8) 0.0949(10) Uani 1 1 d . . . F25 F 0.04892(5) 0.29564(11) -0.08595(9) 0.0560(5) Uani 1 1 d . . . F26 F 0.02400(5) 0.38903(12) -0.06449(8) 0.0520(4) Uani 1 1 d . . . C428 C 0.07929(5) 0.50392(14) -0.04667(9) 0.0209(4) Uani 1 1 d . . . H428 H 0.0841 0.4790 -0.0135 0.025 Uiso 1 1 calc R . . C431 C 0.13229(5) 0.61952(14) 0.06929(8) 0.0193(4) Uani 1 1 d . . . C432 C 0.10010(5) 0.62062(14) 0.06197(9) 0.0212(4) Uani 1 1 d . . . H432 H 0.0779 0.6265 0.0250 0.025 Uiso 1 1 calc R . . C433 C 0.09955(5) 0.61339(14) 0.10709(9) 0.0215(4) Uani 1 1 d . . . C434 C 0.06335(6) 0.60920(16) 0.09391(10) 0.0263(4) Uani 1 1 d . . . F31 F 0.04287(4) 0.53709(11) 0.05798(8) 0.0449(4) Uani 1 1 d . . . F32 F 0.04400(3) 0.68965(10) 0.06855(6) 0.0320(3) Uani 1 1 d . . . F33 F 0.06567(4) 0.59677(11) 0.13974(6) 0.0370(3) Uani 1 1 d . . . C435 C 0.13120(6) 0.60650(14) 0.16210(9) 0.0219(4) Uani 1 1 d . . . H435 H 0.1307 0.6009 0.1928 0.026 Uiso 1 1 calc R . . C436 C 0.16361(5) 0.60810(14) 0.17073(8) 0.0197(4) Uani 1 1 d . . . C437 C 0.19903(6) 0.59623(15) 0.22837(9) 0.0250(4) Uani 1 1 d . . . F34 F 0.19600(4) 0.59356(13) 0.26914(6) 0.0422(4) Uani 1 1 d . . . F35 F 0.22199(4) 0.66745(12) 0.24166(6) 0.0446(4) Uani 1 1 d . . . F36 F 0.21543(4) 0.51441(12) 0.23296(6) 0.0486(4) Uani 1 1 d . . . C438 C 0.16405(5) 0.61504(14) 0.12549(8) 0.0195(4) Uani 1 1 d . . . H438 H 0.1866 0.6168 0.1328 0.023 Uiso 1 1 calc R . . C441 C 0.13527(5) 0.74585(14) 0.01028(8) 0.0183(3) Uani 1 1 d . . . C442 C 0.10284(5) 0.79834(15) -0.02104(8) 0.0207(4) Uani 1 1 d . . . H442 H 0.0807 0.7643 -0.0404 0.025 Uiso 1 1 calc R . . C443 C 0.10201(5) 0.89819(15) -0.02469(8) 0.0214(4) Uani 1 1 d . . . C444 C 0.06603(6) 0.94756(18) -0.05911(11) 0.0355(5) Uani 1 1 d . . . F41 F 0.04487(5) 0.91807(16) -0.11214(8) 0.0810(8) Uani 1 1 d . . . F42 F 0.04797(5) 0.92887(13) -0.03945(10) 0.0643(6) Uani 1 1 d . . . F43 F 0.06825(4) 1.04324(10) -0.05943(7) 0.0431(4) Uani 1 1 d . . . C445 C 0.13369(5) 0.95124(15) 0.00246(9) 0.0223(4) Uani 1 1 d . . . H445 H 0.1332 1.0194 -0.0005 0.027 Uiso 1 1 calc R . . C446 C 0.16608(5) 0.90127(15) 0.03396(8) 0.0207(4) Uani 1 1 d . . . C447 C 0.20070(6) 0.95618(17) 0.06554(10) 0.0296(5) Uani 1 1 d . . . F44 F 0.19716(4) 1.04080(12) 0.04190(8) 0.0567(5) Uani 1 1 d . . . F45 F 0.21436(5) 0.97477(14) 0.11876(7) 0.0556(5) Uani 1 1 d . . . F46 F 0.22646(4) 0.90834(12) 0.06944(8) 0.0478(4) Uani 1 1 d . . . C448 C 0.16683(5) 0.80107(14) 0.03805(8) 0.0197(4) Uani 1 1 d . . . H448 H 0.1895 0.7692 0.0604 0.024 Uiso 1 1 calc R . . C11B C 0.09944(14) 0.2396(4) -0.17713(19) 0.0912(15) Uani 1 1 d . A 3 H11G H 0.0888 0.1929 -0.2062 0.109 Uiso 1 1 calc R A 3 C12B C 0.10906(14) 0.2156(4) -0.1265(2) 0.0932(15) Uani 1 1 d . A 3 H12G H 0.1055 0.1514 -0.1202 0.112 Uiso 1 1 calc R A 3 C13B C 0.12370(11) 0.2810(5) -0.08437(17) 0.0890(16) Uani 1 1 d . A 3 H13B H 0.1291 0.2637 -0.0496 0.107 Uiso 1 1 calc R A 3 C14B C 0.13053(10) 0.3715(4) -0.0923(2) 0.0878(17) Uani 1 1 d . A 3 H14B H 0.1418 0.4170 -0.0625 0.105 Uiso 1 1 calc R A 3 C15B C 0.12102(12) 0.3973(3) -0.1442(3) 0.0872(15) Uani 1 1 d . A 3 H15B H 0.1256 0.4605 -0.1502 0.105 Uiso 1 1 calc R A 3 C16B C 0.10490(14) 0.3303(4) -0.1866(2) 0.0899(15) Uani 1 1 d . A 3 H16B H 0.0976 0.3476 -0.2226 0.108 Uiso 1 1 calc R A 3 C21B C 0.21592(7) -0.26969(19) 0.45065(11) 0.0355(5) Uani 1 1 d . . . H21G H 0.1925 -0.2833 0.4169 0.043 Uiso 1 1 calc R . . C22B C 0.24572(7) -0.31381(18) 0.46108(11) 0.0356(5) Uani 1 1 d . . . H22G H 0.2428 -0.3573 0.4344 0.043 Uiso 1 1 calc R . . C23B C 0.27986(7) -0.29422(19) 0.51067(12) 0.0369(5) Uani 1 1 d . . . H23B H 0.3003 -0.3246 0.5181 0.044 Uiso 1 1 calc R . . C31B C -0.0222(4) -0.1157(6) 0.2174(6) 0.089(5) Uani 0.344(3) 1 d PGU B -1 H31G H -0.0326 -0.1772 0.2022 0.107 Uiso 0.344(3) 1 calc PR B -1 C32B C -0.0416(3) -0.0328(9) 0.1888(5) 0.217(13) Uani 0.344(3) 1 d PGU B -1 H32G H -0.0653 -0.0376 0.1541 0.260 Uiso 0.344(3) 1 calc PR B -1 C33B C -0.0263(2) 0.0570(7) 0.2111(5) 0.218(13) Uani 0.344(3) 1 d PGU B -1 H33B H -0.0396 0.1137 0.1916 0.261 Uiso 0.344(3) 1 calc PR B -1 C34B C 0.0083(2) 0.0641(5) 0.2619(4) 0.075(4) Uani 0.344(3) 1 d PGU B -1 H34B H 0.0187 0.1255 0.2771 0.090 Uiso 0.344(3) 1 calc PR B -1 C35B C 0.0277(2) -0.0188(6) 0.2904(4) 0.100(4) Uani 0.344(3) 1 d PGU B -1 H35B H 0.0514 -0.0140 0.3251 0.120 Uiso 0.344(3) 1 calc PR B -1 C36B C 0.0125(3) -0.1087(5) 0.2681(6) 0.079(4) Uani 0.344(3) 1 d PGU B -1 H36B H 0.0258 -0.1654 0.2876 0.095 Uiso 0.344(3) 1 calc PR B -1 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ni1 0.01321(10) 0.01526(11) 0.01441(11) 0.00015(8) 0.00858(9) -0.00018(8) N1 0.0156(7) 0.0172(8) 0.0175(8) 0.0026(6) 0.0077(6) 0.0004(6) N2 0.0260(9) 0.0315(10) 0.0307(10) 0.0031(8) 0.0192(8) 0.0024(7) Si1 0.0149(2) 0.0160(2) 0.0159(2) 0.00021(18) 0.01002(19) -0.00048(17) P1 0.01349(19) 0.0158(2) 0.0145(2) 0.00046(17) 0.00820(17) -0.00044(16) C11 0.0152(8) 0.0180(9) 0.0201(9) -0.0012(7) 0.0105(7) -0.0007(6) C12 0.0209(9) 0.0214(10) 0.0215(10) 0.0038(8) 0.0122(8) 0.0027(7) C13 0.0213(9) 0.0252(11) 0.0289(11) 0.0046(8) 0.0130(9) 0.0072(8) C14 0.0231(9) 0.0298(11) 0.0325(12) 0.0019(9) 0.0187(9) 0.0066(8) C15 0.0206(9) 0.0249(10) 0.0245(10) 0.0006(8) 0.0161(8) 0.0017(7) C16 0.0151(7) 0.0173(9) 0.0178(9) -0.0015(7) 0.0096(7) -0.0007(6) C111 0.0151(8) 0.0180(9) 0.0153(8) -0.0001(7) 0.0078(7) -0.0017(6) C112 0.0186(8) 0.0222(10) 0.0171(9) 0.0006(7) 0.0082(7) -0.0041(7) C113 0.0195(8) 0.0243(10) 0.0171(9) 0.0005(7) 0.0082(7) -0.0022(7) C121 0.0185(8) 0.0186(9) 0.0173(9) 0.0019(7) 0.0110(7) -0.0013(7) C122 0.0271(9) 0.0186(9) 0.0231(10) -0.0007(7) 0.0163(8) -0.0045(7) C123 0.0236(9) 0.0260(10) 0.0216(10) -0.0006(8) 0.0158(8) -0.0031(8) P2 0.0154(2) 0.0151(2) 0.0166(2) 0.00076(17) 0.00937(18) 0.00040(16) C21 0.0165(8) 0.0188(9) 0.0143(8) 0.0003(7) 0.0083(7) -0.0021(6) C22 0.0216(9) 0.0189(9) 0.0221(10) -0.0001(7) 0.0120(8) -0.0033(7) C23 0.0255(10) 0.0211(10) 0.0273(11) -0.0033(8) 0.0147(9) -0.0072(8) C24 0.0205(9) 0.0285(11) 0.0274(11) -0.0021(9) 0.0141(8) -0.0063(8) C25 0.0203(9) 0.0249(10) 0.0244(10) 0.0005(8) 0.0147(8) -0.0014(7) C26 0.0182(8) 0.0185(9) 0.0164(9) 0.0005(7) 0.0104(7) -0.0010(7) C211 0.0185(8) 0.0166(9) 0.0194(9) 0.0025(7) 0.0100(7) 0.0013(7) C212 0.0268(9) 0.0219(10) 0.0201(10) 0.0031(8) 0.0135(8) 0.0023(8) C213 0.0263(10) 0.0176(9) 0.0261(10) 0.0045(8) 0.0139(9) 0.0022(7) C221 0.0234(9) 0.0195(9) 0.0243(10) 0.0005(8) 0.0161(8) 0.0033(7) C222 0.0335(11) 0.0269(11) 0.0245(11) -0.0001(8) 0.0186(9) 0.0063(9) C223 0.0268(10) 0.0260(11) 0.0358(12) 0.0039(9) 0.0217(10) 0.0070(8) P3 0.0160(2) 0.0163(2) 0.0149(2) -0.00074(17) 0.00917(18) -0.00154(16) C31 0.0221(8) 0.0158(9) 0.0172(9) 0.0008(7) 0.0132(7) 0.0014(7) C32 0.0252(9) 0.0212(10) 0.0185(9) -0.0001(7) 0.0128(8) -0.0004(7) C33 0.0340(11) 0.0244(10) 0.0195(10) -0.0008(8) 0.0176(9) 0.0004(8) C34 0.0355(11) 0.0276(11) 0.0270(11) 0.0012(8) 0.0250(10) 0.0006(9) C35 0.0260(9) 0.0228(10) 0.0255(10) -0.0001(8) 0.0189(9) -0.0006(8) C36 0.0204(8) 0.0150(8) 0.0191(9) 0.0009(7) 0.0130(7) 0.0016(7) C311 0.0225(8) 0.0170(9) 0.0174(9) -0.0007(7) 0.0124(7) -0.0015(7) C312 0.0258(9) 0.0191(9) 0.0239(10) 0.0005(8) 0.0168(8) 0.0010(7) C313 0.0322(10) 0.0190(10) 0.0216(10) -0.0039(8) 0.0135(9) -0.0035(8) C321 0.0169(8) 0.0220(9) 0.0174(9) -0.0003(7) 0.0086(7) -0.0028(7) C322 0.0182(8) 0.0261(10) 0.0216(10) 0.0030(8) 0.0091(8) -0.0003(7) C323 0.0221(9) 0.0279(11) 0.0296(11) -0.0003(9) 0.0159(9) -0.0050(8) B1 0.0161(9) 0.0203(10) 0.0195(10) 0.0001(8) 0.0118(8) 0.0003(7) C411 0.0170(8) 0.0189(9) 0.0179(9) -0.0025(7) 0.0106(7) -0.0016(7) C412 0.0178(8) 0.0173(9) 0.0174(9) 0.0005(7) 0.0104(7) -0.0003(7) C413 0.0161(8) 0.0197(9) 0.0175(9) -0.0018(7) 0.0105(7) -0.0014(7) C414 0.0215(9) 0.0235(10) 0.0259(10) 0.0051(8) 0.0166(8) 0.0030(7) F11 0.0452(8) 0.0241(7) 0.0677(10) 0.0081(7) 0.0456(8) 0.0012(6) F12 0.0317(7) 0.0652(10) 0.0208(7) 0.0038(6) 0.0180(6) 0.0008(7) F13 0.0211(6) 0.0368(7) 0.0327(7) 0.0103(6) 0.0190(6) 0.0067(5) C415 0.0169(8) 0.0204(9) 0.0191(9) -0.0014(7) 0.0110(7) 0.0000(7) C416 0.0188(8) 0.0160(9) 0.0212(9) 0.0001(7) 0.0122(7) -0.0006(7) C417 0.0235(9) 0.0201(10) 0.0300(11) 0.0011(8) 0.0188(9) 0.0005(7) F14 0.0363(7) 0.0187(6) 0.0465(9) -0.0001(6) 0.0239(7) -0.0062(5) F15 0.0242(6) 0.0307(7) 0.0475(8) 0.0173(6) 0.0215(6) 0.0092(5) F16 0.0579(9) 0.0319(7) 0.0451(9) 0.0149(6) 0.0421(8) 0.0131(7) C418 0.0178(8) 0.0183(9) 0.0216(9) -0.0007(7) 0.0128(7) -0.0022(7) C421 0.0147(8) 0.0192(9) 0.0202(9) 0.0016(7) 0.0109(7) 0.0018(6) C422 0.0188(8) 0.0209(9) 0.0222(9) -0.0005(7) 0.0140(8) -0.0022(7) C423 0.0198(8) 0.0245(10) 0.0207(9) 0.0001(8) 0.0131(8) -0.0015(7) C424 0.0303(11) 0.0387(13) 0.0229(11) -0.0036(9) 0.0169(9) -0.0118(9) F21 0.0390(8) 0.0525(9) 0.0335(8) -0.0040(7) 0.0283(7) -0.0129(7) F22 0.0499(9) 0.0550(10) 0.0398(9) 0.0247(8) 0.0281(8) 0.0136(8) F23 0.0671(11) 0.0691(12) 0.0243(8) -0.0174(7) 0.0261(8) -0.0424(9) C425 0.0178(8) 0.0242(10) 0.0222(10) 0.0007(8) 0.0093(8) -0.0028(7) C426 0.0179(8) 0.0208(10) 0.0269(10) 0.0046(8) 0.0120(8) -0.0024(7) C427 0.0292(11) 0.0341(13) 0.0284(12) 0.0058(10) 0.0099(10) -0.0132(9) F24 0.0595(12) 0.1156(19) 0.0375(10) 0.0252(11) -0.0050(9) -0.0661(13) F25 0.0818(13) 0.0241(8) 0.0829(14) 0.0029(8) 0.0615(12) -0.0077(8) F26 0.0552(10) 0.0439(9) 0.0794(13) 0.0063(9) 0.0530(10) -0.0109(8) C428 0.0179(8) 0.0211(9) 0.0219(9) 0.0050(7) 0.0116(8) 0.0013(7) C431 0.0212(8) 0.0177(9) 0.0205(9) 0.0004(7) 0.0137(8) 0.0001(7) C432 0.0206(9) 0.0200(9) 0.0242(10) 0.0016(8) 0.0146(8) 0.0015(7) C433 0.0244(9) 0.0168(9) 0.0304(11) 0.0011(8) 0.0206(9) 0.0015(7) C434 0.0307(10) 0.0234(10) 0.0350(12) -0.0002(9) 0.0255(10) 0.0015(8) F31 0.0421(8) 0.0406(9) 0.0697(11) -0.0218(8) 0.0436(9) -0.0189(7) F32 0.0260(6) 0.0377(8) 0.0346(7) 0.0079(6) 0.0200(6) 0.0109(5) F33 0.0382(7) 0.0478(9) 0.0432(8) 0.0154(7) 0.0344(7) 0.0112(6) C435 0.0299(10) 0.0175(9) 0.0263(10) 0.0007(8) 0.0215(9) 0.0013(7) C436 0.0235(9) 0.0154(9) 0.0204(9) -0.0005(7) 0.0138(8) 0.0004(7) C437 0.0297(10) 0.0221(10) 0.0246(10) 0.0030(8) 0.0177(9) 0.0026(8) F34 0.0407(8) 0.0643(11) 0.0222(7) 0.0031(7) 0.0200(6) 0.0000(7) F35 0.0316(7) 0.0452(9) 0.0324(8) 0.0099(7) 0.0080(6) -0.0128(6) F36 0.0504(9) 0.0388(9) 0.0320(8) 0.0036(7) 0.0137(7) 0.0259(7) C438 0.0214(8) 0.0170(9) 0.0226(10) -0.0001(7) 0.0149(8) -0.0002(7) C441 0.0200(8) 0.0206(9) 0.0170(9) -0.0008(7) 0.0129(7) -0.0003(7) C442 0.0182(8) 0.0233(10) 0.0208(9) -0.0023(7) 0.0124(8) 0.0006(7) C443 0.0201(8) 0.0221(10) 0.0185(9) 0.0003(7) 0.0104(8) 0.0055(7) C444 0.0238(10) 0.0293(12) 0.0374(13) -0.0065(10) 0.0112(10) 0.0075(9) F41 0.0457(10) 0.0747(14) 0.0442(10) -0.0240(10) -0.0103(8) 0.0358(10) F42 0.0421(9) 0.0449(10) 0.1190(18) 0.0101(10) 0.0566(11) 0.0141(8) F43 0.0372(8) 0.0275(7) 0.0515(9) 0.0037(7) 0.0212(7) 0.0121(6) C445 0.0260(9) 0.0162(9) 0.0226(10) 0.0013(7) 0.0141(8) 0.0024(7) C446 0.0217(9) 0.0209(9) 0.0187(9) 0.0013(7) 0.0123(8) -0.0021(7) C447 0.0264(10) 0.0251(11) 0.0338(12) 0.0038(9) 0.0171(9) -0.0036(8) F44 0.0373(8) 0.0349(9) 0.0732(12) 0.0232(8) 0.0225(9) -0.0069(7) F45 0.0476(9) 0.0675(12) 0.0391(9) -0.0205(8) 0.0209(8) -0.0289(9) F46 0.0275(7) 0.0399(9) 0.0739(12) -0.0028(8) 0.0307(8) -0.0053(6) C448 0.0192(8) 0.0212(9) 0.0199(9) 0.0026(7) 0.0127(8) 0.0012(7) C11B 0.100(4) 0.105(4) 0.058(3) -0.027(3) 0.044(3) -0.004(3) C12B 0.101(4) 0.103(4) 0.077(3) -0.012(3) 0.055(3) -0.012(3) C13B 0.055(2) 0.158(5) 0.048(2) -0.016(3) 0.0296(19) 0.014(3) C14B 0.0384(18) 0.113(4) 0.088(3) -0.049(3) 0.028(2) 0.009(2) C15B 0.064(2) 0.070(3) 0.132(5) -0.003(3) 0.063(3) 0.019(2) C16B 0.098(3) 0.106(4) 0.081(3) 0.009(3) 0.064(3) 0.033(3) C21B 0.0360(12) 0.0377(13) 0.0342(13) 0.0060(10) 0.0225(11) -0.0023(10) C22B 0.0484(14) 0.0301(12) 0.0413(14) 0.0008(10) 0.0344(13) -0.0013(10) C23B 0.0408(13) 0.0353(13) 0.0459(15) 0.0086(11) 0.0325(12) 0.0073(10) C31B 0.081(8) 0.148(9) 0.089(11) -0.066(8) 0.078(8) -0.069(7) C32B 0.140(15) 0.156(12) 0.155(17) -0.077(12) -0.005(9) -0.051(10) C33B 0.175(17) 0.150(10) 0.19(2) -0.052(13) 0.050(10) -0.068(11) C34B 0.107(9) 0.093(5) 0.108(10) -0.090(6) 0.107(8) -0.090(6) C35B 0.109(8) 0.129(8) 0.132(10) -0.069(7) 0.110(7) -0.071(6) C36B 0.106(11) 0.113(6) 0.059(9) -0.037(6) 0.071(7) -0.046(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ni1 N1 1.9049(16) . ? Ni1 Si1 2.2452(5) . ? Ni1 P1 2.3064(5) . ? Ni1 P3 2.3099(5) . ? Ni1 P2 2.3340(6) . ? N1 N2 1.087(2) . ? Si1 C16 1.8786(19) . ? Si1 C26 1.880(2) . ? Si1 C36 1.883(2) . ? P1 C11 1.8314(19) . ? P1 C121 1.8665(19) . ? P1 C111 1.8671(19) . ? C11 C12 1.405(3) . ? C11 C16 1.411(3) . ? C12 C13 1.390(3) . ? C13 C14 1.387(3) . ? C14 C15 1.390(3) . ? C15 C16 1.404(2) . ? C111 C112 1.527(3) . ? C111 C113 1.538(3) . ? C121 C122 1.530(3) . ? C121 C123 1.539(3) . ? P2 C21 1.8301(18) . ? P2 C221 1.871(2) . ? P2 C211 1.883(2) . ? C21 C22 1.398(3) . ? C21 C26 1.405(3) . ? C22 C23 1.391(3) . ? C23 C24 1.392(3) . ? C24 C25 1.390(3) . ? C25 C26 1.405(3) . ? C211 C212 1.535(3) . ? C211 C213 1.541(3) . ? C221 C222 1.530(3) . ? C221 C223 1.537(3) . ? P3 C31 1.8304(19) . ? P3 C321 1.8627(19) . ? P3 C311 1.876(2) . ? C31 C32 1.400(3) . ? C31 C36 1.407(3) . ? C32 C33 1.389(3) . ? C33 C34 1.394(3) . ? C34 C35 1.394(3) . ? C35 C36 1.401(3) . ? C311 C312 1.533(3) . ? C311 C313 1.535(3) . ? C321 C322 1.534(3) . ? C321 C323 1.541(3) . ? B1 C411 1.637(3) . ? B1 C431 1.640(3) . ? B1 C421 1.642(3) . ? B1 C441 1.644(3) . ? C411 C412 1.400(3) . ? C411 C418 1.415(3) . ? C412 C413 1.396(3) . ? C413 C415 1.390(3) . ? C413 C414 1.501(3) . ? C414 F13 1.338(2) . ? C414 F12 1.339(3) . ? C414 F11 1.346(2) . ? C415 C416 1.391(3) . ? C416 C418 1.390(3) . ? C416 C417 1.503(3) . ? C417 F15 1.339(2) . ? C417 F14 1.344(2) . ? C417 F16 1.345(2) . ? C421 C428 1.401(3) . ? C421 C422 1.407(3) . ? C422 C423 1.389(3) . ? C423 C425 1.391(3) . ? C423 C424 1.495(3) . ? C424 F23 1.339(3) . ? C424 F21 1.341(3) . ? C424 F22 1.347(3) . ? C425 C426 1.388(3) . ? C426 C428 1.396(3) . ? C426 C427 1.495(3) . ? C427 F24 1.325(3) . ? C427 F25 1.333(3) . ? C427 F26 1.346(3) . ? C431 C432 1.402(3) . ? C431 C438 1.408(3) . ? C432 C433 1.393(3) . ? C433 C435 1.389(3) . ? C433 C434 1.504(3) . ? C434 F33 1.339(3) . ? C434 F32 1.344(3) . ? C434 F31 1.348(3) . ? C435 C436 1.392(3) . ? C436 C438 1.393(3) . ? C436 C437 1.500(3) . ? C437 F34 1.335(2) . ? C437 F35 1.336(3) . ? C437 F36 1.336(3) . ? C441 C448 1.404(3) . ? C441 C442 1.408(3) . ? C442 C443 1.391(3) . ? C443 C445 1.393(3) . ? C443 C444 1.502(3) . ? C444 F41 1.325(3) . ? C444 F43 1.335(3) . ? C444 F42 1.343(3) . ? C445 C446 1.389(3) . ? C446 C448 1.397(3) . ? C446 C447 1.496(3) . ? C447 F46 1.332(3) . ? C447 F44 1.333(3) . ? C447 F45 1.341(3) . ? C11B C12B 1.346(7) . ? C11B C16B 1.354(7) . ? C12B C13B 1.357(7) . ? C13B C14B 1.357(7) . ? C14B C15B 1.391(7) . ? C15B C16B 1.373(7) . ? C21B C23B 1.385(4) 7_546 ? C21B C22B 1.386(4) . ? C22B C23B 1.388(4) . ? C23B C21B 1.385(4) 7_546 ? C31B C32B 1.3900 . ? C31B C36B 1.3900 . ? C32B C33B 1.3900 . ? C33B C34B 1.3900 . ? C34B C35B 1.3900 . ? C35B C36B 1.3900 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Ni1 Si1 178.63(5) . . ? N1 Ni1 P1 95.84(5) . . ? Si1 Ni1 P1 83.11(2) . . ? N1 Ni1 P3 98.53(5) . . ? Si1 Ni1 P3 82.757(19) . . ? P1 Ni1 P3 118.03(2) . . ? N1 Ni1 P2 97.18(5) . . ? Si1 Ni1 P2 82.613(19) . . ? P1 Ni1 P2 120.044(19) . . ? P3 Ni1 P2 117.31(2) . . ? N2 N1 Ni1 179.8(2) . . ? C16 Si1 C26 109.37(8) . . ? C16 Si1 C36 112.29(8) . . ? C26 Si1 C36 109.76(8) . . ? C16 Si1 Ni1 108.96(6) . . ? C26 Si1 Ni1 108.30(6) . . ? C36 Si1 Ni1 108.07(6) . . ? C11 P1 C121 105.23(9) . . ? C11 P1 C111 102.60(8) . . ? C121 P1 C111 101.27(8) . . ? C11 P1 Ni1 108.85(6) . . ? C121 P1 Ni1 116.35(6) . . ? C111 P1 Ni1 120.76(6) . . ? C12 C11 C16 120.05(17) . . ? C12 C11 P1 125.26(15) . . ? C16 C11 P1 114.68(14) . . ? C13 C12 C11 119.69(19) . . ? C14 C13 C12 120.61(19) . . ? C13 C14 C15 120.17(19) . . ? C14 C15 C16 120.55(19) . . ? C15 C16 C11 118.90(17) . . ? C15 C16 Si1 124.48(15) . . ? C11 C16 Si1 116.51(13) . . ? C112 C111 C113 109.36(15) . . ? C112 C111 P1 111.01(13) . . ? C113 C111 P1 114.59(14) . . ? C122 C121 C123 110.52(15) . . ? C122 C121 P1 112.13(13) . . ? C123 C121 P1 112.89(14) . . ? C21 P2 C221 105.95(9) . . ? C21 P2 C211 101.06(8) . . ? C221 P2 C211 100.56(9) . . ? C21 P2 Ni1 107.41(6) . . ? C221 P2 Ni1 115.16(7) . . ? C211 P2 Ni1 124.65(6) . . ? C22 C21 C26 120.10(17) . . ? C22 C21 P2 125.29(15) . . ? C26 C21 P2 114.62(14) . . ? C23 C22 C21 120.01(19) . . ? C22 C23 C24 120.34(19) . . ? C25 C24 C23 119.94(19) . . ? C24 C25 C26 120.54(19) . . ? C25 C26 C21 119.06(18) . . ? C25 C26 Si1 123.78(15) . . ? C21 C26 Si1 116.82(13) . . ? C212 C211 C213 108.49(16) . . ? C212 C211 P2 112.64(13) . . ? C213 C211 P2 113.35(14) . . ? C222 C221 C223 111.14(17) . . ? C222 C221 P2 113.18(14) . . ? C223 C221 P2 111.66(15) . . ? C31 P3 C321 105.48(9) . . ? C31 P3 C311 101.72(9) . . ? C321 P3 C311 102.02(9) . . ? C31 P3 Ni1 107.65(6) . . ? C321 P3 Ni1 114.52(7) . . ? C311 P3 Ni1 123.54(6) . . ? C32 C31 C36 120.30(17) . . ? C32 C31 P3 125.47(15) . . ? C36 C31 P3 114.23(14) . . ? C33 C32 C31 119.94(19) . . ? C32 C33 C34 120.20(19) . . ? C35 C34 C33 120.11(19) . . ? C34 C35 C36 120.43(19) . . ? C35 C36 C31 118.98(18) . . ? C35 C36 Si1 123.92(15) . . ? C31 C36 Si1 116.52(14) . . ? C312 C311 C313 108.64(16) . . ? C312 C311 P3 111.86(13) . . ? C313 C311 P3 113.09(14) . . ? C322 C321 C323 111.22(17) . . ? C322 C321 P3 111.44(13) . . ? C323 C321 P3 111.92(14) . . ? C411 B1 C431 110.06(16) . . ? C411 B1 C421 103.57(15) . . ? C431 B1 C421 114.45(15) . . ? C411 B1 C441 115.85(15) . . ? C431 B1 C441 103.43(15) . . ? C421 B1 C441 109.87(16) . . ? C412 C411 C418 115.14(17) . . ? C412 C411 B1 124.83(17) . . ? C418 C411 B1 119.73(16) . . ? C413 C412 C411 122.35(18) . . ? C415 C413 C412 121.25(17) . . ? C415 C413 C414 119.90(17) . . ? C412 C413 C414 118.84(17) . . ? F13 C414 F12 106.73(16) . . ? F13 C414 F11 106.50(16) . . ? F12 C414 F11 106.18(17) . . ? F13 C414 C413 112.93(16) . . ? F12 C414 C413 112.17(17) . . ? F11 C414 C413 111.87(17) . . ? C413 C415 C416 117.75(17) . . ? C418 C416 C415 120.80(18) . . ? C418 C416 C417 118.58(17) . . ? C415 C416 C417 120.61(17) . . ? F15 C417 F14 106.22(17) . . ? F15 C417 F16 107.04(18) . . ? F14 C417 F16 105.60(16) . . ? F15 C417 C416 112.70(16) . . ? F14 C417 C416 112.53(18) . . ? F16 C417 C416 112.24(17) . . ? C416 C418 C411 122.71(17) . . ? C428 C421 C422 115.71(18) . . ? C428 C421 B1 124.59(17) . . ? C422 C421 B1 119.37(16) . . ? C423 C422 C421 122.45(18) . . ? C422 C423 C425 120.80(19) . . ? C422 C423 C424 118.33(18) . . ? C425 C423 C424 120.85(19) . . ? F23 C424 F21 106.82(19) . . ? F23 C424 F22 106.6(2) . . ? F21 C424 F22 105.39(19) . . ? F23 C424 C423 113.17(19) . . ? F21 C424 C423 112.17(19) . . ? F22 C424 C423 112.18(19) . . ? C426 C425 C423 117.91(19) . . ? C425 C426 C428 121.13(18) . . ? C425 C426 C427 119.30(19) . . ? C428 C426 C427 119.57(19) . . ? F24 C427 F25 107.5(2) . . ? F24 C427 F26 106.0(2) . . ? F25 C427 F26 104.40(19) . . ? F24 C427 C426 112.68(19) . . ? F25 C427 C426 112.9(2) . . ? F26 C427 C426 112.7(2) . . ? C426 C428 C421 121.99(18) . . ? C432 C431 C438 115.45(18) . . ? C432 C431 B1 123.69(17) . . ? C438 C431 B1 120.77(16) . . ? C433 C432 C431 122.20(19) . . ? C435 C433 C432 121.30(18) . . ? C435 C433 C434 121.12(18) . . ? C432 C433 C434 117.53(19) . . ? F33 C434 F32 106.68(16) . . ? F33 C434 F31 107.24(18) . . ? F32 C434 F31 105.32(19) . . ? F33 C434 C433 112.97(19) . . ? F32 C434 C433 112.33(17) . . ? F31 C434 C433 111.83(17) . . ? C433 C435 C436 117.70(18) . . ? C435 C436 C438 120.81(19) . . ? C435 C436 C437 121.39(18) . . ? C438 C436 C437 117.69(17) . . ? F34 C437 F35 106.32(18) . . ? F34 C437 F36 105.88(18) . . ? F35 C437 F36 106.62(19) . . ? F34 C437 C436 113.31(18) . . ? F35 C437 C436 112.40(17) . . ? F36 C437 C436 111.82(18) . . ? C436 C438 C431 122.47(18) . . ? C448 C441 C442 115.53(18) . . ? C448 C441 B1 124.89(17) . . ? C442 C441 B1 119.24(16) . . ? C443 C442 C441 122.37(18) . . ? C442 C443 C445 120.99(18) . . ? C442 C443 C444 118.33(19) . . ? C445 C443 C444 120.68(19) . . ? F41 C444 F43 107.6(2) . . ? F41 C444 F42 105.8(2) . . ? F43 C444 F42 105.74(19) . . ? F41 C444 C443 112.08(19) . . ? F43 C444 C443 113.6(2) . . ? F42 C444 C443 111.6(2) . . ? C446 C445 C443 117.81(18) . . ? C445 C446 C448 121.05(18) . . ? C445 C446 C447 119.27(19) . . ? C448 C446 C447 119.65(18) . . ? F46 C447 F44 106.71(19) . . ? F46 C447 F45 105.3(2) . . ? F44 C447 F45 106.5(2) . . ? F46 C447 C446 112.57(19) . . ? F44 C447 C446 112.69(19) . . ? F45 C447 C446 112.53(18) . . ? C446 C448 C441 122.23(18) . . ? C12B C11B C16B 120.0(5) . . ? C11B C12B C13B 121.5(6) . . ? C14B C13B C12B 119.4(5) . . ? C13B C14B C15B 119.8(4) . . ? C16B C15B C14B 119.2(5) . . ? C11B C16B C15B 120.0(5) . . ? C23B C21B C22B 120.3(2) 7_546 . ? C21B C22B C23B 119.7(2) . . ? C21B C23B C22B 120.0(2) 7_546 . ? C32B C31B C36B 120.0 . . ? C33B C32B C31B 120.0 . . ? C34B C33B C32B 120.0 . . ? C33B C34B C35B 120.0 . . ? C36B C35B C34B 120.0 . . ? C35B C36B C31B 120.0 . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 30.03 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.202 _refine_diff_density_min -0.833 _refine_diff_density_rms 0.077 ####################################################### # Compound 3a: {[SiP(iPr)3]Ni-NCMe}{BArF} # ####################################################### data_09453 _database_code_depnum_ccdc_archive 'CCDC 844854' #TrackingRef 'Ni combined cif.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common {[SiP(iPr)3]Ni-NCMe}{BArF} _chemical_melting_point 'not measured' _chemical_formula_moiety 'C38 H57 N Ni P3 Si, C32 H12 B F24' _chemical_formula_sum 'C70 H69 B F24 N Ni P3 Si' _chemical_formula_weight 1570.78 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' N N 0.0061 0.0033 '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' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 12.8286(8) _cell_length_b 14.9103(10) _cell_length_c 38.095(3) _cell_angle_alpha 90.00 _cell_angle_beta 96.7790(10) _cell_angle_gamma 90.00 _cell_volume 7235.7(8) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9880 _cell_measurement_theta_min 2.21 _cell_measurement_theta_max 30.20 _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.442 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3216 _exptl_absorpt_coefficient_mu 0.454 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8047 _exptl_absorpt_correction_T_max 0.8949 _exptl_absorpt_process_details 'SADABS (Sheldrick, 2008)' _exptl_special_details ; 'Siemens three-circle diffractometer, Bruker APEX CCD' ; _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' _diffrn_measurement_method 'omega and phi scans' _diffrn_detector_area_resol_mean 8.3 _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 198282 _diffrn_reflns_av_R_equivalents 0.0664 _diffrn_reflns_av_sigmaI/netI 0.0384 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -53 _diffrn_reflns_limit_l_max 53 _diffrn_reflns_theta_min 1.08 _diffrn_reflns_theta_max 30.54 _reflns_number_total 22112 _reflns_number_gt 16620 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 3.0 (Bruker-AXS, 2008)' _computing_cell_refinement 'SAINT 7.46A (Bruker-AXS, 2008)' _computing_data_reduction 'SAINT 7.46A (Bruker-AXS, 2008)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. Disordered -CF3 groups on the BArF anion were modeled as an idealized disorder over two positions rotated 60\% from one another, with equivalent fluorine atoms constrained to have equal anisotropic displacement parameters. The disordered BArF anion was also refined with the help of similarity restraints on equivalent 1-2 and 1-3 distances within and between each aryl group. ; _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^)+(0.0468P)^2^+7.8725P] 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 22112 _refine_ls_number_parameters 943 _refine_ls_number_restraints 46 _refine_ls_R_factor_all 0.0708 _refine_ls_R_factor_gt 0.0479 _refine_ls_wR_factor_ref 0.1239 _refine_ls_wR_factor_gt 0.1096 _refine_ls_goodness_of_fit_ref 1.026 _refine_ls_restrained_S_all 1.038 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ni1 Ni 0.660563(18) 0.371550(16) 0.866983(6) 0.01597(6) Uani 1 1 d . . . N1 N 0.54393(12) 0.37255(11) 0.82977(4) 0.0194(3) Uani 1 1 d . . . C1 C 0.47427(15) 0.37163(14) 0.80822(5) 0.0224(4) Uani 1 1 d . . . C2 C 0.38399(18) 0.36874(17) 0.78099(6) 0.0324(5) Uani 1 1 d . . . H2A H 0.3894 0.3160 0.7660 0.049 Uiso 1 1 calc R . . H2B H 0.3828 0.4232 0.7665 0.049 Uiso 1 1 calc R . . H2C H 0.3192 0.3651 0.7922 0.049 Uiso 1 1 calc R . . Si1 Si 0.79360(4) 0.37128(3) 0.910303(13) 0.01672(10) Uani 1 1 d . . . P1 P 0.69631(4) 0.52429(3) 0.867274(13) 0.01846(10) Uani 1 1 d . . . C11 C 0.75219(15) 0.55571(13) 0.91212(5) 0.0203(4) Uani 1 1 d . . . C12 C 0.74487(17) 0.64036(14) 0.92747(6) 0.0254(4) Uani 1 1 d . . . H12 H 0.7085 0.6875 0.9145 0.030 Uiso 1 1 calc R . . C13 C 0.79116(18) 0.65498(15) 0.96187(6) 0.0299(5) Uani 1 1 d . . . H13 H 0.7847 0.7119 0.9726 0.036 Uiso 1 1 calc R . . C14 C 0.84666(18) 0.58709(15) 0.98064(6) 0.0295(4) Uani 1 1 d . . . H14 H 0.8796 0.5981 1.0039 0.035 Uiso 1 1 calc R . . C15 C 0.85424(15) 0.50286(14) 0.96544(5) 0.0241(4) Uani 1 1 d . . . H15 H 0.8923 0.4565 0.9784 0.029 Uiso 1 1 calc R . . C16 C 0.80612(14) 0.48585(13) 0.93115(5) 0.0193(3) Uani 1 1 d . . . C111 C 0.58118(16) 0.60004(14) 0.85645(6) 0.0258(4) Uani 1 1 d . . . H111 H 0.6045 0.6618 0.8640 0.031 Uiso 1 1 calc R . . C112 C 0.54645(18) 0.60419(16) 0.81644(6) 0.0316(5) Uani 1 1 d . . . H11A H 0.5247 0.5443 0.8078 0.047 Uiso 1 1 calc R . . H11B H 0.6051 0.6250 0.8043 0.047 Uiso 1 1 calc R . . H11C H 0.4874 0.6459 0.8118 0.047 Uiso 1 1 calc R . . C113 C 0.48927(17) 0.57623(16) 0.87667(7) 0.0323(5) Uani 1 1 d . . . H11D H 0.4327 0.6200 0.8711 0.048 Uiso 1 1 calc R . . H11E H 0.5125 0.5772 0.9021 0.048 Uiso 1 1 calc R . . H11F H 0.4635 0.5162 0.8698 0.048 Uiso 1 1 calc R . . C121 C 0.79261(16) 0.57816(14) 0.84016(6) 0.0246(4) Uani 1 1 d . . . H121 H 0.7692 0.5636 0.8148 0.029 Uiso 1 1 calc R . . C122 C 0.90400(16) 0.54098(15) 0.84883(6) 0.0291(4) Uani 1 1 d . . . H12A H 0.9504 0.5690 0.8333 0.044 Uiso 1 1 calc R . . H12B H 0.9032 0.4759 0.8452 0.044 Uiso 1 1 calc R . . H12C H 0.9297 0.5543 0.8735 0.044 Uiso 1 1 calc R . . C123 C 0.79798(19) 0.68066(15) 0.84327(7) 0.0326(5) Uani 1 1 d . . . H12D H 0.8198 0.6974 0.8679 0.049 Uiso 1 1 calc R . . H12E H 0.7286 0.7062 0.8356 0.049 Uiso 1 1 calc R . . H12F H 0.8489 0.7038 0.8283 0.049 Uiso 1 1 calc R . . P2 P 0.57066(4) 0.31147(3) 0.910373(12) 0.01662(9) Uani 1 1 d . . . C21 C 0.66372(15) 0.25683(13) 0.94380(5) 0.0189(3) Uani 1 1 d . . . C22 C 0.63861(16) 0.18875(14) 0.96690(5) 0.0237(4) Uani 1 1 d . . . H22 H 0.5683 0.1681 0.9661 0.028 Uiso 1 1 calc R . . C23 C 0.71661(17) 0.15167(14) 0.99088(6) 0.0264(4) Uani 1 1 d . . . H23 H 0.6999 0.1047 1.0061 0.032 Uiso 1 1 calc R . . C24 C 0.81878(17) 0.18286(14) 0.99270(5) 0.0262(4) Uani 1 1 d . . . H24 H 0.8715 0.1582 1.0096 0.031 Uiso 1 1 calc R . . C25 C 0.84466(15) 0.25008(14) 0.97002(5) 0.0221(4) Uani 1 1 d . . . H25 H 0.9150 0.2710 0.9714 0.026 Uiso 1 1 calc R . . C26 C 0.76755(15) 0.28728(13) 0.94507(5) 0.0188(3) Uani 1 1 d . . . C211 C 0.49373(15) 0.38593(13) 0.93760(5) 0.0215(4) Uani 1 1 d . . . H211 H 0.4436 0.4210 0.9208 0.026 Uiso 1 1 calc R . . C212 C 0.42844(18) 0.33701(16) 0.96298(6) 0.0303(5) Uani 1 1 d . . . H21A H 0.4749 0.3007 0.9796 0.045 Uiso 1 1 calc R . . H21B H 0.3770 0.2980 0.9494 0.045 Uiso 1 1 calc R . . H21C H 0.3918 0.3811 0.9761 0.045 Uiso 1 1 calc R . . C213 C 0.56530(16) 0.45364(14) 0.95885(6) 0.0252(4) Uani 1 1 d . . . H21D H 0.5223 0.4978 0.9696 0.038 Uiso 1 1 calc R . . H21E H 0.6089 0.4843 0.9431 0.038 Uiso 1 1 calc R . . H21F H 0.6105 0.4222 0.9774 0.038 Uiso 1 1 calc R . . C221 C 0.47194(15) 0.22233(13) 0.89669(5) 0.0217(4) Uani 1 1 d . . . H221 H 0.4501 0.1959 0.9188 0.026 Uiso 1 1 calc R . . C222 C 0.51670(18) 0.14614(16) 0.87640(7) 0.0349(5) Uani 1 1 d . . . H22A H 0.4626 0.1004 0.8706 0.052 Uiso 1 1 calc R . . H22B H 0.5768 0.1194 0.8910 0.052 Uiso 1 1 calc R . . H22C H 0.5395 0.1696 0.8545 0.052 Uiso 1 1 calc R . . C223 C 0.37299(16) 0.26001(16) 0.87538(6) 0.0279(4) Uani 1 1 d . . . H22D H 0.3893 0.2784 0.8519 0.042 Uiso 1 1 calc R . . H22E H 0.3480 0.3120 0.8877 0.042 Uiso 1 1 calc R . . H22F H 0.3183 0.2138 0.8728 0.042 Uiso 1 1 calc R . . P3 P 0.76988(4) 0.27759(3) 0.839619(13) 0.01901(10) Uani 1 1 d . . . C31 C 0.90521(15) 0.30557(13) 0.85650(5) 0.0203(4) Uani 1 1 d . . . C32 C 0.99311(16) 0.29204(14) 0.83855(6) 0.0249(4) Uani 1 1 d . . . H32 H 0.9849 0.2676 0.8154 0.030 Uiso 1 1 calc R . . C33 C 1.09232(16) 0.31449(15) 0.85477(6) 0.0274(4) Uani 1 1 d . . . H33 H 1.1518 0.3061 0.8424 0.033 Uiso 1 1 calc R . . C34 C 1.10541(15) 0.34914(14) 0.88880(6) 0.0256(4) Uani 1 1 d . . . H34 H 1.1737 0.3632 0.8999 0.031 Uiso 1 1 calc R . . C35 C 1.01842(15) 0.36319(14) 0.90663(6) 0.0229(4) Uani 1 1 d . . . H35 H 1.0276 0.3872 0.9299 0.027 Uiso 1 1 calc R . . C36 C 0.91723(14) 0.34226(13) 0.89063(5) 0.0195(4) Uani 1 1 d . . . C311 C 0.77230(17) 0.15250(13) 0.84511(6) 0.0243(4) Uani 1 1 d . . . H311 H 0.6997 0.1302 0.8374 0.029 Uiso 1 1 calc R . . C312 C 0.79969(18) 0.12497(14) 0.88378(6) 0.0285(4) Uani 1 1 d . . . H31A H 0.7910 0.0600 0.8860 0.043 Uiso 1 1 calc R . . H31B H 0.7530 0.1560 0.8984 0.043 Uiso 1 1 calc R . . H31C H 0.8727 0.1413 0.8917 0.043 Uiso 1 1 calc R . . C313 C 0.84689(19) 0.10295(16) 0.82286(7) 0.0336(5) Uani 1 1 d . . . H31D H 0.9194 0.1215 0.8304 0.050 Uiso 1 1 calc R . . H31E H 0.8284 0.1177 0.7978 0.050 Uiso 1 1 calc R . . H31F H 0.8404 0.0381 0.8262 0.050 Uiso 1 1 calc R . . C321 C 0.76269(16) 0.28779(15) 0.79059(5) 0.0253(4) Uani 1 1 d . . . H321 H 0.8269 0.2585 0.7833 0.030 Uiso 1 1 calc R . . C322 C 0.76396(19) 0.38566(16) 0.77893(6) 0.0315(5) Uani 1 1 d . . . H32A H 0.7627 0.3885 0.7532 0.047 Uiso 1 1 calc R . . H32B H 0.8278 0.4148 0.7902 0.047 Uiso 1 1 calc R . . H32C H 0.7022 0.4165 0.7859 0.047 Uiso 1 1 calc R . . C323 C 0.66709(18) 0.23839(17) 0.77168(6) 0.0327(5) Uani 1 1 d . . . H32D H 0.6027 0.2633 0.7793 0.049 Uiso 1 1 calc R . . H32E H 0.6720 0.1744 0.7776 0.049 Uiso 1 1 calc R . . H32F H 0.6656 0.2459 0.7461 0.049 Uiso 1 1 calc R . . B1 B 0.21956(16) -0.11694(14) 0.86965(5) 0.0178(4) Uani 1 1 d . . . C411 C 0.16297(15) -0.07408(13) 0.83255(5) 0.0193(3) Uani 1 1 d . . . C412 C 0.20016(16) 0.00328(13) 0.81752(5) 0.0214(4) Uani 1 1 d . . . H412 H 0.2635 0.0297 0.8282 0.026 Uiso 1 1 calc R . . C413 C 0.14743(16) 0.04294(13) 0.78741(5) 0.0218(4) Uani 1 1 d D . . C414 C 0.19490(19) 0.12346(14) 0.77196(6) 0.0290(4) Uani 1 1 d D . . F11 F -0.16211(10) -0.04666(9) 0.76087(3) 0.0309(3) Uani 1 1 d D . . F12 F -0.07330(12) -0.14887(10) 0.73836(4) 0.0396(3) Uani 1 1 d D . . F13 F -0.12792(11) -0.16880(10) 0.78919(4) 0.0385(3) Uani 1 1 d D . . C415 C 0.05402(16) 0.00776(13) 0.77135(5) 0.0233(4) Uani 1 1 d . . . H415 H 0.0182 0.0347 0.7508 0.028 Uiso 1 1 calc R . . C416 C 0.01395(15) -0.06833(13) 0.78625(5) 0.0209(4) Uani 1 1 d D . . C417 C -0.08638(17) -0.10821(14) 0.76887(5) 0.0253(4) Uani 1 1 d D . . F14 F 0.28913(15) 0.10546(12) 0.76195(6) 0.0651(6) Uani 1 1 d D . . F15 F 0.20812(15) 0.19172(10) 0.79442(4) 0.0496(4) Uani 1 1 d D . . F16 F 0.13858(16) 0.15387(11) 0.74285(4) 0.0594(5) Uani 1 1 d D . . C418 C 0.06745(15) -0.10814(13) 0.81606(5) 0.0204(4) Uani 1 1 d . . . H418 H 0.0385 -0.1601 0.8256 0.025 Uiso 1 1 calc R . . C421 C 0.16131(14) -0.06654(12) 0.89991(5) 0.0178(3) Uani 1 1 d . . . C422 C 0.19665(14) 0.01493(13) 0.91512(5) 0.0185(3) Uani 1 1 d . . . H422 H 0.2617 0.0385 0.9097 0.022 Uiso 1 1 calc R . . C423 C 0.13981(15) 0.06287(13) 0.93790(5) 0.0191(3) Uani 1 1 d . . . C424 C 0.18466(16) 0.14844(14) 0.95337(5) 0.0241(4) Uani 1 1 d . . . F21 F 0.22548(11) 0.19889(9) 0.92933(4) 0.0343(3) Uani 1 1 d . . . F22 F 0.26107(14) 0.13521(10) 0.97940(4) 0.0531(5) Uani 1 1 d . . . F23 F 0.11341(12) 0.20128(10) 0.96643(5) 0.0460(4) Uani 1 1 d . . . C425 C 0.04404(15) 0.03186(13) 0.94646(5) 0.0212(4) Uani 1 1 d . . . H425 H 0.0051 0.0645 0.9619 0.025 Uiso 1 1 calc R . . C426 C 0.00734(14) -0.04883(13) 0.93154(5) 0.0199(4) Uani 1 1 d . . . C427 C -0.09433(16) -0.08691(15) 0.94061(6) 0.0278(4) Uani 1 1 d . . . F24 F -0.15054(13) -0.02905(12) 0.95681(5) 0.0601(5) Uani 1 1 d . . . F25 F -0.15637(10) -0.11502(11) 0.91202(4) 0.0428(4) Uani 1 1 d . . . F26 F -0.07922(12) -0.15808(13) 0.96161(5) 0.0592(5) Uani 1 1 d . . . C428 C 0.06395(14) -0.09681(13) 0.90898(5) 0.0190(3) Uani 1 1 d . . . H428 H 0.0362 -0.1518 0.8993 0.023 Uiso 1 1 calc R . . C431 C 0.34706(14) -0.10367(12) 0.87482(5) 0.0185(3) Uani 1 1 d . A . C432 C 0.40749(16) -0.10178(13) 0.84649(5) 0.0217(4) Uani 1 1 d . . . H432 H 0.3728 -0.1017 0.8230 0.026 Uiso 1 1 calc R . . C433 C 0.51704(16) -0.10001(13) 0.85163(6) 0.0238(4) Uani 1 1 d . . . C434 C 0.57540(18) -0.09630(16) 0.81996(7) 0.0323(5) Uani 1 1 d . . . F31 F 0.55959(17) -0.16854(13) 0.79981(5) 0.0674(6) Uani 1 1 d . . . F32 F 0.55136(17) -0.02578(13) 0.79994(5) 0.0723(7) Uani 1 1 d . . . F33 F 0.67941(13) -0.09298(16) 0.82801(5) 0.0692(6) Uani 1 1 d . . . C435 C 0.57114(16) -0.10147(14) 0.88529(6) 0.0264(4) Uani 1 1 d . . . H435 H 0.6457 -0.1004 0.8888 0.032 Uiso 1 1 calc R . . C436 C 0.51275(15) -0.10453(14) 0.91375(6) 0.0239(4) Uani 1 1 d . A . C437 C 0.56918(17) -0.10721(17) 0.95042(6) 0.0315(5) Uani 1 1 d . . . F34A F 0.65585(19) -0.16028(18) 0.95154(6) 0.0538(6) Uani 0.779(2) 1 d PD A 1 F35A F 0.6100(3) -0.02921(15) 0.96011(7) 0.0702(8) Uani 0.779(2) 1 d PD A 1 F36A F 0.51439(17) -0.1366(3) 0.97382(6) 0.0848(12) Uani 0.779(2) 1 d PD A 1 F34B F 0.5171(7) -0.0550(6) 0.9739(2) 0.0538(6) Uani 0.221(2) 1 d PD A 2 F35B F 0.5765(9) -0.1860(5) 0.9647(2) 0.0702(8) Uani 0.221(2) 1 d PD A 2 F36B F 0.6589(6) -0.0769(10) 0.9563(2) 0.0848(12) Uani 0.221(2) 1 d PD A 2 C438 C 0.40380(15) -0.10498(13) 0.90862(5) 0.0214(4) Uani 1 1 d . . . H438 H 0.3664 -0.1062 0.9287 0.026 Uiso 1 1 calc R A . C441 C 0.20595(14) -0.22612(13) 0.87132(5) 0.0183(3) Uani 1 1 d . B . C442 C 0.20286(14) -0.27960(13) 0.84107(5) 0.0197(4) Uani 1 1 d . . . H442 H 0.2038 -0.2515 0.8187 0.024 Uiso 1 1 calc R . . C443 C 0.19838(15) -0.37285(13) 0.84269(5) 0.0204(4) Uani 1 1 d . B . C444 C 0.19453(17) -0.42567(14) 0.80932(6) 0.0257(4) Uani 1 1 d . . . F41A F 0.28655(14) -0.43005(16) 0.79688(5) 0.0544(6) Uani 0.901(2) 1 d PD B 1 F42A F 0.13229(18) -0.38673(14) 0.78245(5) 0.0588(6) Uani 0.901(2) 1 d PD B 1 F43A F 0.1581(2) -0.50710(12) 0.81171(5) 0.0654(7) Uani 0.901(2) 1 d PD B 1 F41B F 0.1088(12) -0.4514(12) 0.7990(4) 0.0544(6) Uani 0.099(2) 1 d PD B 2 F42B F 0.2616(13) -0.4993(11) 0.8156(4) 0.0588(6) Uani 0.099(2) 1 d PD B 2 F43B F 0.2200(15) -0.3901(10) 0.7847(4) 0.0654(7) Uani 0.099(2) 1 d PD B 2 C445 C 0.19866(15) -0.41719(13) 0.87476(5) 0.0222(4) Uani 1 1 d . . . H445 H 0.1947 -0.4807 0.8758 0.027 Uiso 1 1 calc R B . C446 C 0.20485(15) -0.36535(13) 0.90516(5) 0.0202(4) Uani 1 1 d . B . C447 C 0.20528(19) -0.41069(14) 0.94037(6) 0.0294(4) Uani 1 1 d . . . F44 F 0.24397(18) -0.49385(10) 0.94048(4) 0.0611(5) Uani 1 1 d . B . F45 F 0.10930(15) -0.41969(17) 0.94975(5) 0.0752(7) Uani 1 1 d . B . F46 F 0.26060(16) -0.36732(10) 0.96636(4) 0.0527(5) Uani 1 1 d . B . C448 C 0.20778(15) -0.27206(13) 0.90349(5) 0.0205(4) Uani 1 1 d . . . H448 H 0.2111 -0.2385 0.9248 0.025 Uiso 1 1 calc R B . 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 0.01543(11) 0.01795(11) 0.01449(11) 0.00069(8) 0.00157(8) -0.00018(8) N1 0.0198(7) 0.0200(7) 0.0189(8) 0.0016(6) 0.0047(6) 0.0000(6) C1 0.0222(9) 0.0251(9) 0.0203(9) 0.0011(7) 0.0039(7) -0.0010(7) C2 0.0288(11) 0.0417(13) 0.0245(11) 0.0012(9) -0.0060(8) -0.0013(9) Si1 0.0151(2) 0.0192(2) 0.0160(2) 0.00077(18) 0.00183(17) 0.00026(18) P1 0.0188(2) 0.0181(2) 0.0184(2) 0.00207(17) 0.00159(17) -0.00065(17) C11 0.0190(8) 0.0210(9) 0.0210(9) -0.0006(7) 0.0032(7) -0.0035(7) C12 0.0300(10) 0.0211(9) 0.0254(10) -0.0002(8) 0.0046(8) -0.0037(8) C13 0.0375(12) 0.0236(10) 0.0290(11) -0.0070(8) 0.0063(9) -0.0071(9) C14 0.0350(11) 0.0307(11) 0.0221(10) -0.0066(8) 0.0007(8) -0.0084(9) C15 0.0218(9) 0.0286(10) 0.0212(9) 0.0000(8) 0.0000(7) -0.0028(8) C16 0.0177(8) 0.0217(9) 0.0190(9) -0.0002(7) 0.0039(7) -0.0031(7) C111 0.0255(10) 0.0213(9) 0.0301(11) 0.0042(8) 0.0008(8) 0.0016(8) C112 0.0321(11) 0.0291(11) 0.0315(12) 0.0086(9) -0.0047(9) 0.0010(9) C113 0.0241(10) 0.0331(11) 0.0400(13) 0.0071(10) 0.0057(9) 0.0048(9) C121 0.0270(10) 0.0227(9) 0.0245(10) 0.0054(8) 0.0049(8) -0.0031(8) C122 0.0250(10) 0.0301(11) 0.0334(12) 0.0083(9) 0.0079(8) -0.0025(8) C123 0.0385(12) 0.0242(10) 0.0363(12) 0.0072(9) 0.0096(10) -0.0055(9) P2 0.0158(2) 0.0186(2) 0.0157(2) 0.00067(17) 0.00281(16) -0.00060(17) C21 0.0212(8) 0.0203(8) 0.0150(8) 0.0005(7) 0.0017(7) 0.0016(7) C22 0.0261(9) 0.0238(9) 0.0215(9) 0.0038(7) 0.0045(7) -0.0032(8) C23 0.0341(11) 0.0253(10) 0.0199(9) 0.0067(8) 0.0038(8) 0.0013(8) C24 0.0294(10) 0.0290(10) 0.0193(9) 0.0051(8) -0.0008(8) 0.0049(8) C25 0.0212(9) 0.0258(9) 0.0189(9) 0.0007(7) 0.0010(7) 0.0027(7) C26 0.0205(8) 0.0207(9) 0.0155(8) -0.0005(7) 0.0031(7) 0.0016(7) C211 0.0201(8) 0.0241(9) 0.0214(9) -0.0005(7) 0.0066(7) 0.0000(7) C212 0.0318(11) 0.0312(11) 0.0307(11) -0.0035(9) 0.0160(9) -0.0070(9) C213 0.0274(10) 0.0273(10) 0.0223(10) -0.0042(8) 0.0086(8) -0.0025(8) C221 0.0193(8) 0.0236(9) 0.0225(9) -0.0008(7) 0.0040(7) -0.0029(7) C222 0.0258(10) 0.0324(12) 0.0470(14) -0.0165(10) 0.0066(10) -0.0060(9) C223 0.0196(9) 0.0385(12) 0.0253(10) 0.0035(9) 0.0007(8) -0.0035(8) P3 0.0188(2) 0.0215(2) 0.0172(2) -0.00141(18) 0.00430(17) 0.00070(18) C31 0.0187(8) 0.0189(8) 0.0236(9) 0.0029(7) 0.0041(7) 0.0019(7) C32 0.0237(9) 0.0265(10) 0.0259(10) 0.0008(8) 0.0084(8) 0.0024(8) C33 0.0190(9) 0.0283(10) 0.0366(12) 0.0031(9) 0.0101(8) 0.0031(8) C34 0.0168(8) 0.0265(10) 0.0337(11) 0.0047(8) 0.0034(8) 0.0016(7) C35 0.0195(9) 0.0253(9) 0.0237(10) 0.0031(8) 0.0019(7) 0.0002(7) C36 0.0179(8) 0.0200(8) 0.0211(9) 0.0034(7) 0.0037(7) 0.0001(7) C311 0.0269(10) 0.0212(9) 0.0258(10) -0.0034(7) 0.0075(8) 0.0006(8) C312 0.0336(11) 0.0230(10) 0.0294(11) 0.0011(8) 0.0059(9) 0.0042(8) C313 0.0379(12) 0.0275(11) 0.0380(13) -0.0059(9) 0.0147(10) 0.0051(9) C321 0.0261(10) 0.0311(10) 0.0194(9) -0.0025(8) 0.0057(7) 0.0004(8) C322 0.0392(12) 0.0371(12) 0.0186(10) 0.0032(8) 0.0052(8) -0.0032(10) C323 0.0329(11) 0.0423(13) 0.0229(10) -0.0092(9) 0.0028(9) 0.0000(10) B1 0.0190(9) 0.0190(9) 0.0154(9) 0.0008(7) 0.0026(7) -0.0014(7) C411 0.0229(9) 0.0196(8) 0.0157(8) -0.0004(7) 0.0030(7) 0.0010(7) C412 0.0258(9) 0.0196(9) 0.0191(9) -0.0023(7) 0.0039(7) -0.0011(7) C413 0.0308(10) 0.0170(8) 0.0185(9) 0.0002(7) 0.0060(7) 0.0005(7) C414 0.0414(12) 0.0220(10) 0.0239(10) 0.0045(8) 0.0055(9) -0.0013(9) F11 0.0287(6) 0.0322(7) 0.0298(7) 0.0008(5) -0.0054(5) 0.0030(5) F12 0.0438(8) 0.0437(8) 0.0300(7) -0.0175(6) -0.0015(6) 0.0014(6) F13 0.0377(7) 0.0396(8) 0.0347(7) 0.0143(6) -0.0103(6) -0.0136(6) C415 0.0319(10) 0.0213(9) 0.0162(9) 0.0024(7) 0.0006(7) 0.0033(8) C416 0.0243(9) 0.0226(9) 0.0155(8) -0.0002(7) 0.0014(7) 0.0005(7) C417 0.0321(10) 0.0239(9) 0.0185(9) 0.0015(7) -0.0022(8) -0.0015(8) F14 0.0644(11) 0.0443(9) 0.0961(15) 0.0230(10) 0.0487(11) 0.0010(8) F15 0.0871(13) 0.0266(7) 0.0360(8) -0.0057(6) 0.0112(8) -0.0208(8) F16 0.0914(14) 0.0419(9) 0.0391(9) 0.0219(7) -0.0166(9) -0.0252(9) C418 0.0259(9) 0.0200(8) 0.0153(8) 0.0015(7) 0.0022(7) -0.0007(7) C421 0.0177(8) 0.0202(8) 0.0150(8) 0.0025(7) 0.0004(6) -0.0009(7) C422 0.0169(8) 0.0213(9) 0.0174(8) 0.0016(7) 0.0026(6) -0.0023(7) C423 0.0228(9) 0.0195(8) 0.0148(8) 0.0002(7) 0.0013(7) -0.0026(7) C424 0.0284(10) 0.0243(9) 0.0197(9) -0.0031(7) 0.0038(8) -0.0046(8) F21 0.0469(8) 0.0244(6) 0.0338(7) -0.0018(5) 0.0136(6) -0.0125(6) F22 0.0677(11) 0.0363(8) 0.0457(9) -0.0015(7) -0.0333(8) -0.0089(7) F23 0.0475(9) 0.0350(8) 0.0605(10) -0.0244(7) 0.0276(8) -0.0106(7) C425 0.0220(9) 0.0228(9) 0.0194(9) 0.0022(7) 0.0051(7) 0.0009(7) C426 0.0173(8) 0.0221(9) 0.0204(9) 0.0041(7) 0.0029(7) -0.0021(7) C427 0.0223(9) 0.0285(10) 0.0337(11) 0.0003(9) 0.0084(8) -0.0029(8) F24 0.0396(8) 0.0555(10) 0.0936(14) -0.0329(10) 0.0438(9) -0.0166(8) F25 0.0231(6) 0.0599(10) 0.0451(9) -0.0085(7) 0.0027(6) -0.0154(6) F26 0.0347(8) 0.0685(11) 0.0750(12) 0.0451(10) 0.0087(8) -0.0129(8) C428 0.0185(8) 0.0197(8) 0.0185(9) 0.0015(7) 0.0005(7) -0.0020(7) C431 0.0198(8) 0.0174(8) 0.0185(9) -0.0001(7) 0.0035(7) -0.0018(7) C432 0.0243(9) 0.0199(9) 0.0216(9) -0.0003(7) 0.0054(7) -0.0006(7) C433 0.0246(9) 0.0208(9) 0.0281(10) 0.0013(8) 0.0116(8) 0.0001(7) C434 0.0318(11) 0.0307(11) 0.0377(13) 0.0021(9) 0.0177(10) 0.0021(9) F31 0.0977(15) 0.0584(11) 0.0565(11) -0.0242(9) 0.0519(11) -0.0241(10) F32 0.0948(15) 0.0669(12) 0.0670(12) 0.0409(10) 0.0583(11) 0.0391(11) F33 0.0339(8) 0.1205(18) 0.0579(11) 0.0016(11) 0.0252(8) -0.0038(10) C435 0.0192(9) 0.0258(10) 0.0347(11) 0.0029(8) 0.0058(8) -0.0005(8) C436 0.0201(9) 0.0251(9) 0.0259(10) 0.0035(8) 0.0009(7) -0.0020(7) C437 0.0233(10) 0.0389(12) 0.0309(11) 0.0034(9) -0.0027(8) -0.0018(9) F34A 0.0507(13) 0.0663(15) 0.0400(11) -0.0065(10) -0.0122(9) 0.0278(11) F35A 0.105(2) 0.0372(12) 0.0563(15) -0.0072(10) -0.0399(15) -0.0088(13) F36A 0.0292(10) 0.198(4) 0.0256(10) 0.0368(16) -0.0061(8) -0.0320(16) F34B 0.0507(13) 0.0663(15) 0.0400(11) -0.0065(10) -0.0122(9) 0.0278(11) F35B 0.105(2) 0.0372(12) 0.0563(15) -0.0072(10) -0.0399(15) -0.0088(13) F36B 0.0292(10) 0.198(4) 0.0256(10) 0.0368(16) -0.0061(8) -0.0320(16) C438 0.0198(8) 0.0240(9) 0.0207(9) 0.0016(7) 0.0040(7) -0.0017(7) C441 0.0171(8) 0.0200(8) 0.0174(8) 0.0003(7) 0.0010(6) -0.0009(7) C442 0.0188(8) 0.0233(9) 0.0169(9) 0.0004(7) 0.0016(7) -0.0019(7) C443 0.0189(8) 0.0219(9) 0.0205(9) -0.0041(7) 0.0022(7) -0.0029(7) C444 0.0272(10) 0.0269(10) 0.0235(10) -0.0053(8) 0.0046(8) -0.0052(8) F41A 0.0342(9) 0.0846(15) 0.0471(11) -0.0382(10) 0.0156(8) -0.0084(9) F42A 0.0800(15) 0.0539(12) 0.0342(10) -0.0200(8) -0.0276(9) 0.0214(10) F43A 0.137(2) 0.0322(9) 0.0333(10) -0.0164(7) 0.0339(11) -0.0428(12) F41B 0.0342(9) 0.0846(15) 0.0471(11) -0.0382(10) 0.0156(8) -0.0084(9) F42B 0.0800(15) 0.0539(12) 0.0342(10) -0.0200(8) -0.0276(9) 0.0214(10) F43B 0.137(2) 0.0322(9) 0.0333(10) -0.0164(7) 0.0339(11) -0.0428(12) C445 0.0233(9) 0.0197(9) 0.0236(10) -0.0012(7) 0.0025(7) -0.0015(7) C446 0.0206(8) 0.0212(9) 0.0188(9) 0.0018(7) 0.0017(7) -0.0001(7) C447 0.0438(13) 0.0225(10) 0.0214(10) 0.0035(8) 0.0021(9) 0.0002(9) F44 0.1255(17) 0.0258(7) 0.0303(8) 0.0068(6) 0.0024(9) 0.0202(9) F45 0.0530(11) 0.1227(18) 0.0527(11) 0.0519(12) 0.0179(9) -0.0006(11) F46 0.0969(14) 0.0355(8) 0.0211(7) 0.0041(6) -0.0121(8) -0.0131(8) C448 0.0222(9) 0.0208(9) 0.0179(9) -0.0014(7) -0.0004(7) -0.0005(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ni1 N1 1.9359(16) . ? Ni1 Si1 2.2297(6) . ? Ni1 P2 2.3054(5) . ? Ni1 P3 2.3154(5) . ? Ni1 P1 2.3229(6) . ? N1 C1 1.140(3) . ? C1 C2 1.461(3) . ? Si1 C26 1.881(2) . ? Si1 C36 1.8827(19) . ? Si1 C16 1.883(2) . ? P1 C11 1.834(2) . ? P1 C111 1.866(2) . ? P1 C121 1.881(2) . ? C11 C12 1.399(3) . ? C11 C16 1.404(3) . ? C12 C13 1.391(3) . ? C13 C14 1.387(3) . ? C14 C15 1.391(3) . ? C15 C16 1.401(3) . ? C111 C113 1.525(3) . ? C111 C112 1.538(3) . ? C121 C122 1.532(3) . ? C121 C123 1.534(3) . ? P2 C21 1.8308(19) . ? P2 C221 1.867(2) . ? P2 C211 1.877(2) . ? C21 C26 1.403(3) . ? C21 C22 1.405(3) . ? C22 C23 1.388(3) . ? C23 C24 1.385(3) . ? C24 C25 1.389(3) . ? C25 C26 1.403(3) . ? C211 C213 1.530(3) . ? C211 C212 1.536(3) . ? C221 C222 1.524(3) . ? C221 C223 1.531(3) . ? P3 C31 1.827(2) . ? P3 C321 1.865(2) . ? P3 C311 1.877(2) . ? C31 C32 1.401(3) . ? C31 C36 1.402(3) . ? C32 C33 1.389(3) . ? C33 C34 1.387(3) . ? C34 C35 1.389(3) . ? C35 C36 1.403(3) . ? C311 C312 1.530(3) . ? C311 C313 1.540(3) . ? C321 C322 1.526(3) . ? C321 C323 1.535(3) . ? B1 C421 1.630(3) . ? B1 C431 1.636(3) . ? B1 C441 1.639(3) . ? B1 C411 1.640(3) . ? C411 C412 1.396(3) . ? C411 C418 1.405(3) . ? C412 C413 1.393(3) . ? C413 C415 1.383(3) . ? C413 C414 1.498(3) . ? C414 F15 1.327(3) . ? C414 F16 1.330(3) . ? C414 F14 1.337(3) . ? F11 C417 1.345(2) . ? F12 C417 1.339(2) . ? F13 C417 1.340(2) . ? C415 C416 1.394(3) . ? C416 C418 1.389(3) . ? C416 C417 1.499(3) . ? C421 C422 1.398(3) . ? C421 C428 1.409(3) . ? C422 C423 1.395(3) . ? C423 C425 1.387(3) . ? C423 C424 1.492(3) . ? C424 F22 1.324(3) . ? C424 F21 1.339(2) . ? C424 F23 1.346(2) . ? C425 C426 1.389(3) . ? C426 C428 1.387(3) . ? C426 C427 1.500(3) . ? C427 F24 1.323(3) . ? C427 F26 1.329(3) . ? C427 F25 1.338(3) . ? C431 C432 1.401(3) . ? C431 C438 1.403(3) . ? C432 C433 1.396(3) . ? C433 C435 1.384(3) . ? C433 C434 1.494(3) . ? C434 F32 1.314(3) . ? C434 F31 1.324(3) . ? C434 F33 1.334(3) . ? C435 C436 1.389(3) . ? C436 C438 1.388(3) . ? C436 C437 1.496(3) . ? C437 F36B 1.232(8) . ? C437 F36A 1.276(3) . ? C437 F35B 1.293(9) . ? C437 F35A 1.310(3) . ? C437 F34A 1.361(3) . ? C437 F34B 1.412(8) . ? C441 C442 1.398(3) . ? C441 C448 1.402(3) . ? C442 C443 1.393(3) . ? C443 C445 1.389(3) . ? C443 C444 1.491(3) . ? C444 F43B 1.158(16) . ? C444 F41B 1.187(16) . ? C444 F43A 1.308(3) . ? C444 F41A 1.325(3) . ? C444 F42A 1.353(3) . ? C444 F42B 1.398(16) . ? C445 C446 1.387(3) . ? C446 C448 1.393(3) . ? C446 C447 1.501(3) . ? C447 F46 1.318(3) . ? C447 F45 1.329(3) . ? C447 F44 1.335(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Ni1 Si1 179.26(5) . . ? N1 Ni1 P2 96.85(5) . . ? Si1 Ni1 P2 82.68(2) . . ? N1 Ni1 P3 97.58(5) . . ? Si1 Ni1 P3 83.15(2) . . ? P2 Ni1 P3 117.94(2) . . ? N1 Ni1 P1 97.53(5) . . ? Si1 Ni1 P1 82.23(2) . . ? P2 Ni1 P1 119.52(2) . . ? P3 Ni1 P1 117.75(2) . . ? C1 N1 Ni1 178.49(17) . . ? N1 C1 C2 178.7(2) . . ? C26 Si1 C36 110.81(8) . . ? C26 Si1 C16 108.69(8) . . ? C36 Si1 C16 110.03(9) . . ? C26 Si1 Ni1 109.77(6) . . ? C36 Si1 Ni1 108.24(6) . . ? C16 Si1 Ni1 109.28(6) . . ? C11 P1 C111 105.27(10) . . ? C11 P1 C121 101.10(9) . . ? C111 P1 C121 100.03(9) . . ? C11 P1 Ni1 108.07(6) . . ? C111 P1 Ni1 116.21(7) . . ? C121 P1 Ni1 123.92(7) . . ? C12 C11 C16 120.46(18) . . ? C12 C11 P1 125.58(16) . . ? C16 C11 P1 113.96(14) . . ? C13 C12 C11 119.6(2) . . ? C14 C13 C12 120.5(2) . . ? C13 C14 C15 120.1(2) . . ? C14 C15 C16 120.5(2) . . ? C15 C16 C11 118.91(18) . . ? C15 C16 Si1 124.33(15) . . ? C11 C16 Si1 116.31(14) . . ? C113 C111 C112 111.05(18) . . ? C113 C111 P1 112.74(15) . . ? C112 C111 P1 111.87(16) . . ? C122 C121 C123 108.16(18) . . ? C122 C121 P1 112.55(14) . . ? C123 C121 P1 114.18(15) . . ? C21 P2 C221 104.03(9) . . ? C21 P2 C211 102.77(9) . . ? C221 P2 C211 101.05(9) . . ? C21 P2 Ni1 109.35(6) . . ? C221 P2 Ni1 117.17(7) . . ? C211 P2 Ni1 120.43(7) . . ? C26 C21 C22 119.94(17) . . ? C26 C21 P2 114.74(14) . . ? C22 C21 P2 125.31(15) . . ? C23 C22 C21 119.94(19) . . ? C24 C23 C22 120.26(19) . . ? C23 C24 C25 120.36(19) . . ? C24 C25 C26 120.37(19) . . ? C21 C26 C25 119.09(17) . . ? C21 C26 Si1 115.99(14) . . ? C25 C26 Si1 124.79(15) . . ? C213 C211 C212 108.53(17) . . ? C213 C211 P2 111.14(13) . . ? C212 C211 P2 115.36(14) . . ? C222 C221 C223 110.06(18) . . ? C222 C221 P2 112.86(14) . . ? C223 C221 P2 112.31(14) . . ? C31 P3 C321 105.45(9) . . ? C31 P3 C311 100.67(9) . . ? C321 P3 C311 101.00(10) . . ? C31 P3 Ni1 107.71(7) . . ? C321 P3 Ni1 116.14(7) . . ? C311 P3 Ni1 123.65(7) . . ? C32 C31 C36 120.14(18) . . ? C32 C31 P3 125.57(16) . . ? C36 C31 P3 114.29(14) . . ? C33 C32 C31 119.8(2) . . ? C34 C33 C32 120.61(19) . . ? C33 C34 C35 119.84(19) . . ? C34 C35 C36 120.6(2) . . ? C31 C36 C35 118.98(18) . . ? C31 C36 Si1 116.95(14) . . ? C35 C36 Si1 123.76(15) . . ? C312 C311 C313 108.31(18) . . ? C312 C311 P3 111.89(14) . . ? C313 C311 P3 114.75(15) . . ? C322 C321 C323 110.95(19) . . ? C322 C321 P3 111.61(14) . . ? C323 C321 P3 111.90(15) . . ? C421 B1 C431 113.23(15) . . ? C421 B1 C441 111.75(15) . . ? C431 B1 C441 103.00(15) . . ? C421 B1 C411 103.68(15) . . ? C431 B1 C411 113.03(15) . . ? C441 B1 C411 112.46(15) . . ? C412 C411 C418 115.95(17) . . ? C412 C411 B1 122.49(17) . . ? C418 C411 B1 121.24(17) . . ? C413 C412 C411 122.15(18) . . ? C415 C413 C412 120.97(18) . . ? C415 C413 C414 120.09(18) . . ? C412 C413 C414 118.92(19) . . ? F15 C414 F16 106.95(19) . . ? F15 C414 F14 106.7(2) . . ? F16 C414 F14 104.5(2) . . ? F15 C414 C413 112.84(18) . . ? F16 C414 C413 113.26(19) . . ? F14 C414 C413 111.98(18) . . ? C413 C415 C416 118.06(18) . . ? C418 C416 C415 120.70(18) . . ? C418 C416 C417 120.47(18) . . ? C415 C416 C417 118.80(18) . . ? F12 C417 F13 107.18(17) . . ? F12 C417 F11 105.85(16) . . ? F13 C417 F11 105.37(17) . . ? F12 C417 C416 111.96(18) . . ? F13 C417 C416 113.05(16) . . ? F11 C417 C416 112.89(17) . . ? C416 C418 C411 122.14(18) . . ? C422 C421 C428 115.49(17) . . ? C422 C421 B1 122.71(16) . . ? C428 C421 B1 121.30(16) . . ? C423 C422 C421 122.36(17) . . ? C425 C423 C422 121.20(18) . . ? C425 C423 C424 120.21(18) . . ? C422 C423 C424 118.58(17) . . ? F22 C424 F21 106.34(18) . . ? F22 C424 F23 106.59(18) . . ? F21 C424 F23 105.16(17) . . ? F22 C424 C423 112.66(17) . . ? F21 C424 C423 111.96(16) . . ? F23 C424 C423 113.55(17) . . ? C423 C425 C426 117.35(18) . . ? C428 C426 C425 121.55(17) . . ? C428 C426 C427 118.72(18) . . ? C425 C426 C427 119.71(18) . . ? F24 C427 F26 106.8(2) . . ? F24 C427 F25 106.22(19) . . ? F26 C427 F25 105.68(19) . . ? F24 C427 C426 113.41(18) . . ? F26 C427 C426 111.84(18) . . ? F25 C427 C426 112.38(18) . . ? C426 C428 C421 122.05(18) . . ? C432 C431 C438 115.66(17) . . ? C432 C431 B1 123.08(17) . . ? C438 C431 B1 120.79(16) . . ? C433 C432 C431 122.12(19) . . ? C435 C433 C432 121.06(18) . . ? C435 C433 C434 120.28(19) . . ? C432 C433 C434 118.7(2) . . ? F32 C434 F31 107.8(2) . . ? F32 C434 F33 105.3(2) . . ? F31 C434 F33 104.1(2) . . ? F32 C434 C433 113.11(19) . . ? F31 C434 C433 112.38(19) . . ? F33 C434 C433 113.5(2) . . ? C433 C435 C436 117.76(18) . . ? C438 C436 C435 121.13(19) . . ? C438 C436 C437 119.96(19) . . ? C435 C436 C437 118.92(19) . . ? F36B C437 F36A 125.3(4) . . ? F36B C437 F35B 103.6(7) . . ? F36A C437 F35B 54.1(5) . . ? F36B C437 F35A 44.7(6) . . ? F36A C437 F35A 110.0(3) . . ? F35B C437 F35A 132.9(4) . . ? F36B C437 F34A 57.7(7) . . ? F36A C437 F34A 107.1(3) . . ? F35B C437 F34A 55.9(6) . . ? F35A C437 F34A 102.1(2) . . ? F36B C437 F34B 100.6(7) . . ? F36A C437 F34B 53.5(4) . . ? F35B C437 F34B 104.6(6) . . ? F35A C437 F34B 62.3(4) . . ? F34A C437 F34B 138.3(4) . . ? F36B C437 C436 120.0(4) . . ? F36A C437 C436 114.56(19) . . ? F35B C437 C436 114.8(4) . . ? F35A C437 C436 111.9(2) . . ? F34A C437 C436 110.4(2) . . ? F34B C437 C436 111.3(3) . . ? C436 C438 C431 122.27(18) . . ? C442 C441 C448 115.97(17) . . ? C442 C441 B1 121.82(17) . . ? C448 C441 B1 121.89(17) . . ? C443 C442 C441 122.01(18) . . ? C445 C443 C442 121.21(18) . . ? C445 C443 C444 119.66(18) . . ? C442 C443 C444 119.12(18) . . ? F43B C444 F41B 102.7(12) . . ? F43B C444 F43A 128.2(8) . . ? F41B C444 F43A 53.0(9) . . ? F43B C444 F41A 52.0(9) . . ? F41B C444 F41A 134.1(8) . . ? F43A C444 F41A 108.6(2) . . ? F43B C444 F42A 52.3(9) . . ? F41B C444 F42A 56.5(9) . . ? F43A C444 F42A 105.5(2) . . ? F41A C444 F42A 102.8(2) . . ? F43B C444 F42B 105.7(12) . . ? F41B C444 F42B 109.3(11) . . ? F43A C444 F42B 58.4(7) . . ? F41A C444 F42B 57.7(8) . . ? F42A C444 F42B 139.7(6) . . ? F43B C444 C443 117.7(8) . . ? F41B C444 C443 112.8(7) . . ? F43A C444 C443 114.01(18) . . ? F41A C444 C443 112.94(17) . . ? F42A C444 C443 112.07(18) . . ? F42B C444 C443 108.1(6) . . ? C446 C445 C443 117.60(18) . . ? C445 C446 C448 121.15(18) . . ? C445 C446 C447 119.27(18) . . ? C448 C446 C447 119.55(18) . . ? F46 C447 F45 106.4(2) . . ? F46 C447 F44 106.64(19) . . ? F45 C447 F44 105.1(2) . . ? F46 C447 C446 113.27(18) . . ? F45 C447 C446 112.32(19) . . ? F44 C447 C446 112.52(18) . . ? C446 C448 C441 122.02(18) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 30.54 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.812 _refine_diff_density_min -0.563 _refine_diff_density_rms 0.075 ####################################################### # Compound 4a: {[SiP(iPr)3]Ni-CO}{BArF} # ####################################################### data_ct03 _database_code_depnum_ccdc_archive 'CCDC 844855' #TrackingRef 'Ni combined cif.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common {[SiP(iPr)3]Ni-CO}{BArF} _chemical_melting_point 'not measured' _chemical_formula_moiety 'C37 H54 Ni O P3 Si, C32 H12 B F24' _chemical_formula_sum 'C69 H66 B Cl F24 Ni O P3 Si' _chemical_formula_weight 1593.19 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 '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' 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' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pbca loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 26.3375(11) _cell_length_b 19.5435(8) _cell_length_c 27.2078(10) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 14004.6(10) _cell_formula_units_Z 8 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9953 _cell_measurement_theta_min 2.35 _cell_measurement_theta_max 27.28 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.511 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 6504 _exptl_absorpt_coefficient_mu 0.508 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8792 _exptl_absorpt_correction_T_max 0.9277 _exptl_absorpt_process_details 'SADABS v2008/1 (Bruker-AXS, 2008)' _exptl_special_details ; 'Bruker KAPPA APEX II' ; _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 KAPPA APEX II' _diffrn_measurement_method '\w and \f scans' _diffrn_detector_area_resol_mean 8.3 _diffrn_reflns_number 190453 _diffrn_reflns_av_R_equivalents 0.0698 _diffrn_reflns_av_sigmaI/netI 0.0401 _diffrn_reflns_limit_h_min -35 _diffrn_reflns_limit_h_max 37 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_min -33 _diffrn_reflns_limit_l_max 38 _diffrn_reflns_theta_min 1.86 _diffrn_reflns_theta_max 30.54 _reflns_number_total 21390 _reflns_number_gt 15341 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 v2009.7-0 (Bruker-AXS, 2009)' _computing_cell_refinement 'SAINT-Plus v7.66A (Bruker-AXS, 2009)' _computing_data_reduction 'SAINT-Plus v7.66A (Bruker-AXS, 2009)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. The BArF anion was refined with the help of similarity restraints on equivalent 1-2 and 1-3 distances within and between each aryl group. The bound CO molecule was refined to an 87% occupancy; the balance is made up by a partial chlorine atom with a 13% occupancy. When the occupancy of the BArF anion was allowed to refine freely, it refined to very near full occupancy, suggesting that the minor nickel species present is the nickel (III) chloride [SiP(iPr)3]Ni-Cl BArF, which has been observed as a decomposition product of the dinitrogen adduct and has also been seperately crystallographically characterized. The residual electron density peak of 2.02 electrons near P2 arises from the minor part of a disorder of that ligand arm; this disorder has not been modeled, as the minor part comprises only ca. 3% occupation. ; _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^)+(0.0590P)^2^+22.3720P] 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 21390 _refine_ls_number_parameters 923 _refine_ls_number_restraints 970 _refine_ls_R_factor_all 0.0832 _refine_ls_R_factor_gt 0.0540 _refine_ls_wR_factor_ref 0.1443 _refine_ls_wR_factor_gt 0.1278 _refine_ls_goodness_of_fit_ref 1.003 _refine_ls_restrained_S_all 0.989 _refine_ls_shift/su_max 0.034 _refine_ls_shift/su_mean 0.002 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ni1 Ni 0.857348(10) 0.704555(14) -0.001351(10) 0.01561(6) Uani 1 1 d . . . Si1 Si 0.78592(2) 0.75632(3) -0.02824(2) 0.01453(11) Uani 1 1 d . . . C1 C 0.91349(17) 0.6621(2) 0.01932(17) 0.0218(8) Uani 0.873(16) 1 d P . . O1 O 0.95009(14) 0.6357(3) 0.03328(13) 0.0344(7) Uani 0.873(16) 1 d P . . Cl1 Cl 0.9326(5) 0.6597(9) 0.0273(5) 0.066(7) Uani 0.127(16) 1 d P . . P1 P 0.88930(2) 0.74652(3) -0.07363(2) 0.01850(11) Uani 1 1 d . . . C11 C 0.85230(9) 0.82041(11) -0.09378(7) 0.0179(4) Uani 1 1 d . . . C12 C 0.86860(10) 0.86912(12) -0.12802(8) 0.0228(5) Uani 1 1 d . . . H12 H 0.9028 0.8692 -0.1390 0.027 Uiso 1 1 calc R . . C13 C 0.83472(11) 0.91711(12) -0.14574(8) 0.0267(5) Uani 1 1 d . . . H13 H 0.8457 0.9497 -0.1694 0.032 Uiso 1 1 calc R . . C14 C 0.78480(11) 0.91815(12) -0.12933(9) 0.0271(5) Uani 1 1 d . . . H14 H 0.7616 0.9506 -0.1424 0.032 Uiso 1 1 calc R . . C15 C 0.76873(9) 0.87178(12) -0.09380(8) 0.0225(4) Uani 1 1 d . . . H15 H 0.7349 0.8737 -0.0817 0.027 Uiso 1 1 calc R . . C16 C 0.80235(9) 0.82220(10) -0.07578(7) 0.0173(4) Uani 1 1 d . . . C111 C 0.88734(9) 0.69235(12) -0.13037(8) 0.0228(5) Uani 1 1 d . . . H111 H 0.9047 0.6482 -0.1226 0.027 Uiso 1 1 calc R . . C112 C 0.91486(11) 0.72425(13) -0.17448(9) 0.0301(5) Uani 1 1 d . . . H11A H 0.9139 0.6924 -0.2023 0.045 Uiso 1 1 calc R . . H11B H 0.9503 0.7336 -0.1656 0.045 Uiso 1 1 calc R . . H11C H 0.8980 0.7671 -0.1837 0.045 Uiso 1 1 calc R . . C113 C 0.83269(10) 0.67542(13) -0.14530(9) 0.0279(5) Uani 1 1 d . . . H11D H 0.8146 0.7178 -0.1534 0.042 Uiso 1 1 calc R . . H11E H 0.8155 0.6524 -0.1180 0.042 Uiso 1 1 calc R . . H11F H 0.8330 0.6453 -0.1741 0.042 Uiso 1 1 calc R . . C121 C 0.95670(9) 0.77421(13) -0.07311(9) 0.0262(5) Uani 1 1 d . . . H121 H 0.9625 0.8009 -0.1040 0.031 Uiso 1 1 calc R . . C122 C 0.99324(10) 0.71276(15) -0.07442(11) 0.0338(6) Uani 1 1 d . . . H12A H 1.0283 0.7293 -0.0759 0.051 Uiso 1 1 calc R . . H12B H 0.9860 0.6848 -0.1035 0.051 Uiso 1 1 calc R . . H12C H 0.9886 0.6851 -0.0447 0.051 Uiso 1 1 calc R . . C123 C 0.96903(10) 0.82150(16) -0.03052(10) 0.0348(6) Uani 1 1 d . . . H12D H 0.9627 0.7977 0.0006 0.052 Uiso 1 1 calc R . . H12E H 0.9476 0.8624 -0.0324 0.052 Uiso 1 1 calc R . . H12F H 1.0048 0.8350 -0.0322 0.052 Uiso 1 1 calc R . . P2 P 0.80542(2) 0.60868(3) -0.00264(2) 0.02115(12) Uani 1 1 d . . . C21 C 0.75248(9) 0.62283(12) -0.04481(9) 0.0226(4) Uani 1 1 d . . . C22 C 0.72342(10) 0.57125(13) -0.06675(11) 0.0322(6) Uani 1 1 d . . . H22 H 0.7285 0.5248 -0.0577 0.039 Uiso 1 1 calc R . . C23 C 0.68724(10) 0.58804(15) -0.10170(12) 0.0367(6) Uani 1 1 d . . . H23 H 0.6677 0.5528 -0.1166 0.044 Uiso 1 1 calc R . . C24 C 0.67915(10) 0.65469(14) -0.11517(10) 0.0305(5) Uani 1 1 d . . . H24 H 0.6548 0.6655 -0.1397 0.037 Uiso 1 1 calc R . . C25 C 0.70676(9) 0.70612(13) -0.09273(8) 0.0230(4) Uani 1 1 d . . . H25 H 0.7007 0.7525 -0.1015 0.028 Uiso 1 1 calc R . . C26 C 0.74358(8) 0.69080(11) -0.05717(8) 0.0185(4) Uani 1 1 d . . . C211 C 0.77395(11) 0.58074(13) 0.05553(10) 0.0305(5) Uani 1 1 d . . . H211 H 0.8006 0.5780 0.0816 0.037 Uiso 1 1 calc R . . C212 C 0.73433(11) 0.63293(15) 0.07224(10) 0.0350(6) Uani 1 1 d . . . H21A H 0.7065 0.6345 0.0483 0.053 Uiso 1 1 calc R . . H21B H 0.7501 0.6782 0.0747 0.053 Uiso 1 1 calc R . . H21C H 0.7209 0.6195 0.1044 0.053 Uiso 1 1 calc R . . C213 C 0.74768(15) 0.51100(16) 0.05290(13) 0.0496(8) Uani 1 1 d . . . H21D H 0.7319 0.5007 0.0847 0.074 Uiso 1 1 calc R . . H21E H 0.7728 0.4756 0.0451 0.074 Uiso 1 1 calc R . . H21F H 0.7215 0.5120 0.0273 0.074 Uiso 1 1 calc R . . C221 C 0.83343(10) 0.52656(12) -0.02462(10) 0.0275(5) Uani 1 1 d . . . H221 H 0.8049 0.4929 -0.0263 0.033 Uiso 1 1 calc R . . C222 C 0.85627(13) 0.52994(15) -0.07559(12) 0.0416(7) Uani 1 1 d . . . H22A H 0.8844 0.5628 -0.0758 0.062 Uiso 1 1 calc R . . H22B H 0.8303 0.5445 -0.0991 0.062 Uiso 1 1 calc R . . H22C H 0.8690 0.4846 -0.0849 0.062 Uiso 1 1 calc R . . C223 C 0.87189(12) 0.49762(15) 0.01185(12) 0.0403(7) Uani 1 1 d . . . H22D H 0.8783 0.4494 0.0042 0.060 Uiso 1 1 calc R . . H22E H 0.8583 0.5015 0.0453 0.060 Uiso 1 1 calc R . . H22F H 0.9037 0.5234 0.0095 0.060 Uiso 1 1 calc R . . P3 P 0.84809(2) 0.77969(3) 0.06312(2) 0.01920(11) Uani 1 1 d . . . C31 C 0.78063(8) 0.80095(11) 0.06971(8) 0.0186(4) Uani 1 1 d . . . C32 C 0.75688(9) 0.82173(13) 0.11315(8) 0.0239(5) Uani 1 1 d . . . H32 H 0.7760 0.8264 0.1425 0.029 Uiso 1 1 calc R . . C33 C 0.70509(10) 0.83559(13) 0.11321(9) 0.0272(5) Uani 1 1 d . . . H33 H 0.6888 0.8487 0.1429 0.033 Uiso 1 1 calc R . . C34 C 0.67705(9) 0.83050(14) 0.07032(9) 0.0281(5) Uani 1 1 d . . . H34 H 0.6418 0.8408 0.0706 0.034 Uiso 1 1 calc R . . C35 C 0.70049(9) 0.81030(13) 0.02685(8) 0.0245(5) Uani 1 1 d . . . H35 H 0.6812 0.8072 -0.0026 0.029 Uiso 1 1 calc R . . C36 C 0.75229(8) 0.79453(11) 0.02620(7) 0.0178(4) Uani 1 1 d . . . C311 C 0.87880(10) 0.86572(13) 0.06147(9) 0.0282(5) Uani 1 1 d . . . H311 H 0.9161 0.8584 0.0570 0.034 Uiso 1 1 calc R . . C312 C 0.87160(12) 0.90704(16) 0.10917(10) 0.0385(7) Uani 1 1 d . . . H31A H 0.8886 0.9514 0.1060 0.058 Uiso 1 1 calc R . . H31B H 0.8864 0.8818 0.1368 0.058 Uiso 1 1 calc R . . H31C H 0.8353 0.9142 0.1151 0.058 Uiso 1 1 calc R . . C313 C 0.86017(11) 0.90796(13) 0.01809(10) 0.0308(5) Uani 1 1 d . . . H31D H 0.8234 0.9143 0.0206 0.046 Uiso 1 1 calc R . . H31E H 0.8682 0.8841 -0.0126 0.046 Uiso 1 1 calc R . . H31F H 0.8770 0.9527 0.0183 0.046 Uiso 1 1 calc R . . C321 C 0.86939(9) 0.74798(15) 0.12415(9) 0.0279(5) Uani 1 1 d . . . H321 H 0.8554 0.7803 0.1492 0.033 Uiso 1 1 calc R . . C322 C 0.84869(11) 0.67696(16) 0.13691(10) 0.0357(6) Uani 1 1 d . . . H32A H 0.8628 0.6431 0.1141 0.054 Uiso 1 1 calc R . . H32B H 0.8116 0.6772 0.1342 0.054 Uiso 1 1 calc R . . H32C H 0.8584 0.6651 0.1706 0.054 Uiso 1 1 calc R . . C323 C 0.92728(11) 0.74991(19) 0.12956(10) 0.0418(7) Uani 1 1 d . . . H32D H 0.9367 0.7346 0.1626 0.063 Uiso 1 1 calc R . . H32E H 0.9394 0.7968 0.1244 0.063 Uiso 1 1 calc R . . H32F H 0.9427 0.7196 0.1051 0.063 Uiso 1 1 calc R . . B1 B 0.56580(9) 0.81289(13) 0.25612(9) 0.0193(5) Uani 1 1 d D . . C411 C 0.54959(8) 0.73999(12) 0.23021(8) 0.0202(4) Uani 1 1 d D . . C412 C 0.50914(8) 0.70065(11) 0.24782(8) 0.0203(4) Uani 1 1 d D . . H412 H 0.4917 0.7157 0.2764 0.024 Uiso 1 1 calc R . . C413 C 0.49331(9) 0.64043(12) 0.22522(8) 0.0221(4) Uani 1 1 d D . . C414 C 0.45040(10) 0.60129(12) 0.24753(9) 0.0262(5) Uani 1 1 d D . . F11 F 0.45803(7) 0.58740(9) 0.29514(6) 0.0412(4) Uani 1 1 d D . . F12 F 0.40628(6) 0.63593(8) 0.24614(6) 0.0306(3) Uani 1 1 d D . . F13 F 0.44140(7) 0.54154(9) 0.22498(7) 0.0470(5) Uani 1 1 d D . . C415 C 0.51750(9) 0.61668(12) 0.18325(9) 0.0242(5) Uani 1 1 d D . . H415 H 0.5070 0.5754 0.1678 0.029 Uiso 1 1 calc R . . C416 C 0.55735(9) 0.65496(12) 0.16453(8) 0.0232(5) Uani 1 1 d D . . C417 C 0.58700(10) 0.62840(13) 0.12146(9) 0.0295(5) Uani 1 1 d D . . F14 F 0.56011(7) 0.58471(10) 0.09374(6) 0.0470(5) Uani 1 1 d D . . F15 F 0.60237(8) 0.67846(9) 0.09113(6) 0.0452(5) Uani 1 1 d D . . F16 F 0.62868(6) 0.59467(9) 0.13543(6) 0.0410(4) Uani 1 1 d D . . C418 C 0.57300(9) 0.71544(12) 0.18737(8) 0.0213(4) Uani 1 1 d D . . H418 H 0.6003 0.7407 0.1735 0.026 Uiso 1 1 calc R . . C421 C 0.52999(8) 0.87066(11) 0.22970(8) 0.0177(4) Uani 1 1 d D . . C422 C 0.48382(8) 0.89421(11) 0.24885(8) 0.0196(4) Uani 1 1 d D . . H422 H 0.4733 0.8786 0.2803 0.024 Uiso 1 1 calc R . . C423 C 0.45285(8) 0.93957(12) 0.22346(8) 0.0216(4) Uani 1 1 d D . . C424 C 0.40393(10) 0.96236(14) 0.24678(10) 0.0311(5) Uani 1 1 d D . . F21 F 0.41118(7) 0.99349(10) 0.28985(7) 0.0498(5) Uani 1 1 d D . . F22 F 0.37377(7) 0.90922(10) 0.25863(7) 0.0491(5) Uani 1 1 d D . . F23 F 0.37648(9) 1.00210(17) 0.21855(9) 0.0988(12) Uani 1 1 d D . . C425 C 0.46634(9) 0.96388(12) 0.17737(8) 0.0229(4) Uani 1 1 d D . . H425 H 0.4454 0.9954 0.1602 0.027 Uiso 1 1 calc R . . C426 C 0.51172(9) 0.94050(12) 0.15718(8) 0.0210(4) Uani 1 1 d D . . C427 C 0.52804(11) 0.96675(13) 0.10788(9) 0.0290(5) Uani 1 1 d D . . F24 F 0.55855(7) 0.92320(8) 0.08413(6) 0.0366(4) Uani 1 1 d D . . F25 F 0.48873(8) 0.97734(14) 0.07746(7) 0.0647(7) Uani 1 1 d D . . F26 F 0.55246(10) 1.02552(9) 0.11051(7) 0.0642(7) Uani 1 1 d D . . C428 C 0.54268(9) 0.89540(11) 0.18261(8) 0.0200(4) Uani 1 1 d D . . H428 H 0.5735 0.8807 0.1678 0.024 Uiso 1 1 calc R . . C431 C 0.55883(8) 0.81052(12) 0.31606(8) 0.0192(4) Uani 1 1 d D . . C432 C 0.55131(8) 0.87008(12) 0.34403(8) 0.0197(4) Uani 1 1 d D . . H432 H 0.5464 0.9123 0.3274 0.024 Uiso 1 1 calc R . . C433 C 0.55082(8) 0.86933(12) 0.39532(8) 0.0207(4) Uani 1 1 d D . . C434 C 0.54142(10) 0.93424(13) 0.42317(9) 0.0265(5) Uani 1 1 d D . . F31 F 0.55769(8) 0.98939(9) 0.39916(7) 0.0491(5) Uani 1 1 d D . . F32 F 0.49250(7) 0.94433(10) 0.43234(9) 0.0575(6) Uani 1 1 d D . . F33 F 0.56434(9) 0.93514(10) 0.46676(7) 0.0581(6) Uani 1 1 d D . . C435 C 0.55829(8) 0.80876(12) 0.42116(8) 0.0219(4) Uani 1 1 d D . . H435 H 0.5580 0.8081 0.4561 0.026 Uiso 1 1 calc R . . C436 C 0.56619(8) 0.74935(12) 0.39438(8) 0.0215(4) Uani 1 1 d D . . C437 C 0.57592(9) 0.68278(13) 0.41992(9) 0.0261(5) Uani 1 1 d D . . F34 F 0.56947(8) 0.68602(9) 0.46855(6) 0.0441(4) Uani 1 1 d D . . F35 F 0.62416(6) 0.66085(8) 0.41308(6) 0.0366(4) Uani 1 1 d D . . F36 F 0.54632(6) 0.63234(8) 0.40349(6) 0.0381(4) Uani 1 1 d D . . C438 C 0.56641(8) 0.75025(12) 0.34302(8) 0.0206(4) Uani 1 1 d D . . H438 H 0.5719 0.7086 0.3258 0.025 Uiso 1 1 calc R . . C441 C 0.62679(9) 0.82868(13) 0.24868(8) 0.0231(5) Uani 1 1 d D . . C442 C 0.64637(9) 0.89506(14) 0.24357(8) 0.0257(5) Uani 1 1 d D . . H442 H 0.6234 0.9325 0.2420 0.031 Uiso 1 1 calc R . . C443 C 0.69838(9) 0.90815(15) 0.24069(9) 0.0326(6) Uani 1 1 d D . . C444 C 0.71771(12) 0.97947(19) 0.23274(12) 0.0485(9) Uani 1 1 d D . . F41 F 0.68292(9) 1.02703(12) 0.23543(10) 0.0716(7) Uani 1 1 d D . . F42 F 0.75202(10) 0.99688(16) 0.26732(11) 0.0950(10) Uani 1 1 d D . . F43 F 0.74246(13) 0.98499(14) 0.19084(10) 0.1010(12) Uani 1 1 d D . . C445 C 0.73324(10) 0.85510(17) 0.24340(9) 0.0366(7) Uani 1 1 d D . . H445 H 0.7687 0.8639 0.2418 0.044 Uiso 1 1 calc R . . C446 C 0.71522(10) 0.78976(17) 0.24850(9) 0.0349(6) Uani 1 1 d D . . C447 C 0.75059(11) 0.72945(19) 0.25006(10) 0.0446(8) Uani 1 1 d D . . F44 F 0.79946(7) 0.74832(13) 0.24257(8) 0.0591(6) Uani 1 1 d D . . F45 F 0.74961(9) 0.69828(13) 0.29328(7) 0.0663(7) Uani 1 1 d D . . F46 F 0.73966(7) 0.68234(11) 0.21547(7) 0.0540(5) Uani 1 1 d D . . C448 C 0.66277(9) 0.77623(15) 0.25130(8) 0.0280(5) Uani 1 1 d D . . H448 H 0.6516 0.7303 0.2551 0.034 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ni1 0.01474(12) 0.01641(12) 0.01569(12) 0.00307(10) -0.00011(10) 0.00106(10) Si1 0.0159(3) 0.0138(2) 0.0139(2) -0.0010(2) -0.0014(2) 0.0004(2) C1 0.0175(18) 0.0234(15) 0.0245(16) 0.0071(12) -0.0016(14) -0.0017(14) O1 0.0202(13) 0.0373(18) 0.0457(15) 0.0180(12) -0.0055(11) 0.0068(12) Cl1 0.051(15) 0.079(9) 0.068(7) 0.044(6) 0.004(7) -0.007(9) P1 0.0199(3) 0.0186(3) 0.0170(2) 0.0028(2) 0.0033(2) 0.0022(2) C11 0.0250(11) 0.0141(9) 0.0147(9) -0.0012(7) -0.0008(8) 0.0011(8) C12 0.0334(12) 0.0171(10) 0.0180(10) -0.0007(8) 0.0050(9) -0.0017(9) C13 0.0448(15) 0.0161(10) 0.0191(10) 0.0036(8) 0.0012(10) 0.0005(10) C14 0.0415(14) 0.0187(11) 0.0211(10) 0.0003(8) -0.0040(10) 0.0067(10) C15 0.0268(11) 0.0202(10) 0.0205(10) -0.0005(8) -0.0042(9) 0.0031(9) C16 0.0248(10) 0.0128(9) 0.0143(9) -0.0019(7) -0.0032(8) 0.0004(8) C111 0.0317(12) 0.0161(10) 0.0205(10) 0.0012(8) 0.0084(9) 0.0035(9) C112 0.0432(15) 0.0246(12) 0.0226(11) -0.0010(9) 0.0134(10) 0.0011(11) C113 0.0350(13) 0.0246(12) 0.0243(11) -0.0074(9) 0.0052(10) 0.0003(10) C121 0.0216(11) 0.0316(12) 0.0255(11) 0.0052(9) 0.0054(9) -0.0023(9) C122 0.0253(12) 0.0402(15) 0.0359(14) 0.0080(12) 0.0064(10) 0.0056(11) C123 0.0260(12) 0.0441(16) 0.0344(13) -0.0034(12) 0.0012(10) -0.0093(12) P2 0.0200(3) 0.0159(2) 0.0275(3) 0.0037(2) -0.0018(2) -0.0006(2) C21 0.0184(10) 0.0200(10) 0.0293(11) -0.0032(9) -0.0009(9) -0.0009(8) C22 0.0272(12) 0.0198(11) 0.0497(16) -0.0059(11) -0.0069(11) 0.0002(10) C23 0.0253(12) 0.0309(14) 0.0539(17) -0.0133(12) -0.0148(12) -0.0014(11) C24 0.0221(12) 0.0344(14) 0.0351(13) -0.0126(11) -0.0073(10) 0.0044(10) C25 0.0194(10) 0.0272(12) 0.0223(10) -0.0059(9) -0.0010(8) 0.0021(9) C26 0.0168(9) 0.0189(10) 0.0199(9) -0.0053(8) 0.0019(8) -0.0007(8) C211 0.0350(14) 0.0269(12) 0.0298(12) 0.0069(10) 0.0024(10) -0.0041(11) C212 0.0315(14) 0.0381(15) 0.0355(14) 0.0025(12) 0.0082(11) -0.0060(12) C213 0.061(2) 0.0325(16) 0.0551(19) 0.0077(14) 0.0140(17) -0.0180(15) C221 0.0286(12) 0.0167(10) 0.0371(13) 0.0021(9) -0.0034(10) 0.0012(9) C222 0.0531(18) 0.0251(13) 0.0467(16) 0.0052(12) 0.0124(14) 0.0162(13) C223 0.0418(16) 0.0268(13) 0.0523(18) 0.0037(12) -0.0115(14) 0.0097(12) P3 0.0175(3) 0.0251(3) 0.0150(2) -0.0016(2) -0.00184(19) -0.0028(2) C31 0.0197(10) 0.0188(10) 0.0172(9) -0.0019(8) 0.0003(8) -0.0012(8) C32 0.0264(12) 0.0291(12) 0.0163(9) -0.0032(9) -0.0010(8) 0.0008(10) C33 0.0300(12) 0.0318(13) 0.0199(10) -0.0033(9) 0.0052(9) 0.0067(10) C34 0.0217(11) 0.0351(13) 0.0276(12) -0.0023(10) 0.0024(9) 0.0098(10) C35 0.0220(11) 0.0324(13) 0.0190(10) -0.0024(9) -0.0025(8) 0.0064(9) C36 0.0205(10) 0.0163(9) 0.0164(9) -0.0016(7) 0.0000(8) 0.0018(8) C311 0.0298(12) 0.0302(13) 0.0247(11) -0.0070(10) 0.0006(9) -0.0115(10) C312 0.0481(17) 0.0373(15) 0.0300(13) -0.0130(11) -0.0012(12) -0.0125(13) C313 0.0412(15) 0.0228(12) 0.0286(12) -0.0047(10) 0.0010(11) -0.0078(11) C321 0.0242(11) 0.0410(14) 0.0184(10) 0.0008(10) -0.0065(9) -0.0002(10) C322 0.0361(14) 0.0447(16) 0.0265(12) 0.0083(11) -0.0056(11) 0.0009(12) C323 0.0274(13) 0.068(2) 0.0304(13) 0.0032(14) -0.0135(11) -0.0011(14) B1 0.0166(11) 0.0227(12) 0.0185(11) 0.0019(9) 0.0003(9) 0.0008(9) C411 0.0187(10) 0.0220(11) 0.0198(10) 0.0024(8) -0.0016(8) 0.0048(8) C412 0.0203(10) 0.0219(10) 0.0187(9) 0.0011(8) -0.0007(8) 0.0038(8) C413 0.0220(11) 0.0200(10) 0.0243(10) 0.0041(8) -0.0003(9) 0.0042(9) C414 0.0286(12) 0.0221(11) 0.0279(11) 0.0024(9) -0.0002(9) 0.0011(10) F11 0.0401(9) 0.0489(10) 0.0346(8) 0.0249(8) -0.0052(7) -0.0063(8) F12 0.0239(7) 0.0344(8) 0.0335(8) 0.0100(6) 0.0044(6) 0.0028(6) F13 0.0495(11) 0.0267(8) 0.0647(12) -0.0137(8) 0.0196(9) -0.0127(8) C415 0.0278(12) 0.0194(10) 0.0253(11) 0.0003(8) -0.0022(9) 0.0049(9) C416 0.0255(11) 0.0224(11) 0.0216(10) 0.0005(8) 0.0011(9) 0.0079(9) C417 0.0323(13) 0.0271(12) 0.0290(12) -0.0024(10) 0.0061(10) 0.0054(10) F14 0.0480(10) 0.0544(11) 0.0385(9) -0.0232(8) 0.0079(8) -0.0026(9) F15 0.0701(13) 0.0326(9) 0.0328(8) 0.0031(7) 0.0241(8) 0.0094(9) F16 0.0354(9) 0.0456(10) 0.0420(9) 0.0007(8) 0.0113(7) 0.0162(8) C418 0.0222(10) 0.0217(11) 0.0198(10) 0.0020(8) 0.0017(8) 0.0034(9) C421 0.0164(9) 0.0190(10) 0.0178(9) -0.0015(8) -0.0014(7) -0.0037(8) C422 0.0189(10) 0.0207(10) 0.0193(9) 0.0010(8) -0.0012(8) -0.0021(8) C423 0.0186(10) 0.0241(11) 0.0221(10) -0.0005(8) -0.0014(8) 0.0013(9) C424 0.0245(12) 0.0374(14) 0.0315(13) 0.0030(11) 0.0006(10) 0.0084(11) F21 0.0371(9) 0.0508(11) 0.0615(12) -0.0332(9) 0.0145(8) -0.0075(8) F22 0.0290(9) 0.0584(12) 0.0599(12) -0.0251(10) 0.0163(8) -0.0119(8) F23 0.0663(15) 0.156(3) 0.0742(16) 0.0675(17) 0.0344(13) 0.0799(18) C425 0.0253(11) 0.0210(11) 0.0224(10) 0.0002(8) -0.0050(9) 0.0031(9) C426 0.0273(11) 0.0190(10) 0.0169(9) 0.0009(8) -0.0003(8) -0.0019(9) C427 0.0415(15) 0.0246(12) 0.0209(11) 0.0031(9) 0.0037(10) 0.0030(11) F24 0.0505(10) 0.0310(8) 0.0283(8) 0.0038(6) 0.0153(7) 0.0050(7) F25 0.0546(12) 0.1118(19) 0.0278(9) 0.0249(11) -0.0008(8) 0.0262(12) F26 0.126(2) 0.0317(9) 0.0344(9) -0.0022(7) 0.0278(11) -0.0313(11) C428 0.0217(10) 0.0197(10) 0.0188(9) -0.0005(8) -0.0001(8) -0.0015(8) C431 0.0139(9) 0.0243(11) 0.0193(9) 0.0014(8) 0.0000(7) 0.0006(8) C432 0.0158(10) 0.0239(11) 0.0193(10) 0.0017(8) -0.0004(8) 0.0002(8) C433 0.0176(10) 0.0249(11) 0.0198(10) -0.0015(8) 0.0011(8) -0.0024(8) C434 0.0301(12) 0.0261(12) 0.0233(11) -0.0028(9) 0.0024(9) -0.0030(10) F31 0.0808(14) 0.0256(8) 0.0409(9) -0.0043(7) 0.0199(9) -0.0136(9) F32 0.0340(9) 0.0451(11) 0.0933(16) -0.0322(11) 0.0195(10) -0.0020(8) F33 0.0951(16) 0.0443(11) 0.0349(9) -0.0154(8) -0.0249(10) 0.0095(11) C435 0.0181(10) 0.0297(12) 0.0179(10) 0.0024(8) 0.0005(8) -0.0028(9) C436 0.0164(10) 0.0257(11) 0.0225(10) 0.0048(9) -0.0011(8) -0.0004(9) C437 0.0230(11) 0.0305(12) 0.0247(11) 0.0064(9) -0.0001(9) -0.0009(10) F34 0.0677(12) 0.0407(10) 0.0241(8) 0.0116(7) 0.0053(8) 0.0072(9) F35 0.0257(8) 0.0327(8) 0.0514(10) 0.0164(7) 0.0009(7) 0.0052(6) F36 0.0373(9) 0.0296(8) 0.0474(9) 0.0118(7) -0.0086(7) -0.0118(7) C438 0.0176(10) 0.0250(11) 0.0194(10) 0.0005(8) 0.0007(8) 0.0012(8) C441 0.0179(10) 0.0367(13) 0.0146(9) -0.0015(9) -0.0005(8) 0.0002(10) C442 0.0201(11) 0.0382(13) 0.0188(10) -0.0085(9) 0.0016(8) -0.0041(10) C443 0.0221(12) 0.0538(17) 0.0219(11) -0.0150(11) 0.0034(9) -0.0106(11) C444 0.0343(15) 0.064(2) 0.0470(17) -0.0281(16) 0.0167(13) -0.0263(16) F41 0.0547(13) 0.0521(13) 0.108(2) -0.0114(13) 0.0248(13) -0.0230(11) F42 0.0699(16) 0.105(2) 0.110(2) -0.0548(18) -0.0151(15) -0.0383(16) F43 0.148(3) 0.0739(17) 0.0810(17) -0.0356(14) 0.0823(18) -0.0628(18) C445 0.0183(11) 0.070(2) 0.0210(11) -0.0150(12) 0.0008(9) -0.0047(12) C446 0.0227(12) 0.067(2) 0.0150(10) -0.0045(11) -0.0020(9) 0.0126(13) C447 0.0280(14) 0.077(2) 0.0292(13) -0.0005(14) -0.0041(11) 0.0192(15) F44 0.0237(8) 0.0948(17) 0.0587(12) -0.0114(12) -0.0020(8) 0.0163(10) F45 0.0604(13) 0.0915(17) 0.0470(11) 0.0238(11) 0.0045(10) 0.0391(12) F46 0.0376(10) 0.0683(14) 0.0561(12) -0.0152(10) -0.0089(9) 0.0196(10) C448 0.0227(11) 0.0429(14) 0.0183(10) 0.0015(10) -0.0012(9) 0.0063(11) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ni1 C1 1.787(4) . ? Ni1 Si1 2.2578(6) . ? Ni1 P1 2.2909(6) . ? Ni1 P3 2.3006(6) . ? Ni1 Cl1 2.303(15) . ? Ni1 P2 2.3201(6) . ? Si1 C26 1.872(2) . ? Si1 C16 1.876(2) . ? Si1 C36 1.880(2) . ? C1 Cl1 0.549(13) . ? C1 O1 1.157(8) . ? O1 Cl1 0.678(13) . ? P1 C11 1.826(2) . ? P1 C121 1.856(2) . ? P1 C111 1.872(2) . ? C11 C12 1.399(3) . ? C11 C16 1.404(3) . ? C12 C13 1.382(3) . ? C13 C14 1.389(4) . ? C14 C15 1.391(3) . ? C15 C16 1.401(3) . ? C111 C113 1.532(4) . ? C111 C112 1.535(3) . ? C121 C123 1.517(4) . ? C121 C122 1.539(4) . ? P2 C21 1.827(2) . ? P2 C221 1.865(3) . ? P2 C211 1.868(3) . ? C21 C26 1.390(3) . ? C21 C22 1.399(3) . ? C22 C23 1.386(4) . ? C23 C24 1.370(4) . ? C24 C25 1.383(3) . ? C25 C26 1.402(3) . ? C211 C212 1.528(4) . ? C211 C213 1.530(4) . ? C221 C222 1.513(4) . ? C221 C223 1.527(4) . ? P3 C31 1.833(2) . ? P3 C321 1.859(2) . ? P3 C311 1.866(3) . ? C31 C32 1.398(3) . ? C31 C36 1.405(3) . ? C32 C33 1.391(3) . ? C33 C34 1.385(4) . ? C34 C35 1.391(3) . ? C35 C36 1.399(3) . ? C311 C313 1.521(4) . ? C311 C312 1.540(4) . ? C321 C322 1.531(4) . ? C321 C323 1.532(4) . ? B1 C421 1.637(3) . ? B1 C431 1.642(3) . ? B1 C411 1.646(3) . ? B1 C441 1.648(3) . ? C411 C412 1.398(3) . ? C411 C418 1.403(3) . ? C412 C413 1.392(3) . ? C413 C415 1.387(3) . ? C413 C414 1.494(3) . ? C414 F11 1.339(3) . ? C414 F13 1.340(3) . ? C414 F12 1.345(3) . ? C415 C416 1.386(3) . ? C416 C418 1.398(3) . ? C416 C417 1.501(3) . ? C417 F16 1.335(3) . ? C417 F14 1.341(3) . ? C417 F15 1.342(3) . ? C421 C422 1.401(3) . ? C421 C428 1.410(3) . ? C422 C423 1.389(3) . ? C423 C425 1.387(3) . ? C423 C424 1.503(3) . ? C424 F23 1.310(3) . ? C424 F21 1.334(3) . ? C424 F22 1.347(3) . ? C425 C426 1.393(3) . ? C426 C428 1.386(3) . ? C426 C427 1.499(3) . ? C427 F26 1.318(3) . ? C427 F24 1.337(3) . ? C427 F25 1.342(3) . ? C431 C438 1.402(3) . ? C431 C432 1.405(3) . ? C432 C433 1.396(3) . ? C433 C435 1.391(3) . ? C433 C434 1.498(3) . ? C434 F32 1.327(3) . ? C434 F33 1.331(3) . ? C434 F31 1.331(3) . ? C435 C436 1.387(3) . ? C436 C438 1.398(3) . ? C436 C437 1.497(3) . ? C437 F36 1.334(3) . ? C437 F34 1.335(3) . ? C437 F35 1.354(3) . ? C441 C448 1.398(3) . ? C441 C442 1.403(4) . ? C442 C443 1.396(3) . ? C443 C445 1.387(4) . ? C443 C444 1.500(4) . ? C444 F41 1.307(4) . ? C444 F43 1.318(3) . ? C444 F42 1.348(4) . ? C445 C446 1.369(4) . ? C446 C448 1.409(4) . ? C446 C447 1.503(4) . ? C447 F45 1.325(3) . ? C447 F46 1.348(4) . ? C447 F44 1.354(4) . ? 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 Ni1 Si1 178.87(15) . . ? C1 Ni1 P1 97.61(15) . . ? Si1 Ni1 P1 82.39(2) . . ? C1 Ni1 P3 98.29(14) . . ? Si1 Ni1 P3 82.69(2) . . ? P1 Ni1 P3 117.71(2) . . ? C1 Ni1 Cl1 5.3(5) . . ? Si1 Ni1 Cl1 175.8(4) . . ? P1 Ni1 Cl1 96.4(3) . . ? P3 Ni1 Cl1 94.4(4) . . ? C1 Ni1 P2 96.75(15) . . ? Si1 Ni1 P2 82.29(2) . . ? P1 Ni1 P2 119.52(2) . . ? P3 Ni1 P2 117.68(2) . . ? Cl1 Ni1 P2 101.8(4) . . ? C26 Si1 C16 108.48(10) . . ? C26 Si1 C36 108.81(10) . . ? C16 Si1 C36 112.29(10) . . ? C26 Si1 Ni1 109.03(7) . . ? C16 Si1 Ni1 109.80(7) . . ? C36 Si1 Ni1 108.38(7) . . ? Cl1 C1 O1 22(2) . . ? Cl1 C1 Ni1 157(2) . . ? O1 C1 Ni1 178.7(4) . . ? Cl1 O1 C1 17.3(14) . . ? C1 Cl1 O1 141(3) . . ? C1 Cl1 Ni1 17.5(17) . . ? O1 Cl1 Ni1 158.6(18) . . ? C11 P1 C121 106.39(11) . . ? C11 P1 C111 100.65(10) . . ? C121 P1 C111 101.40(11) . . ? C11 P1 Ni1 110.16(7) . . ? C121 P1 Ni1 116.69(8) . . ? C111 P1 Ni1 119.68(7) . . ? C12 C11 C16 120.2(2) . . ? C12 C11 P1 125.03(18) . . ? C16 C11 P1 114.52(16) . . ? C13 C12 C11 119.7(2) . . ? C12 C13 C14 120.6(2) . . ? C13 C14 C15 120.1(2) . . ? C14 C15 C16 120.1(2) . . ? C15 C16 C11 119.2(2) . . ? C15 C16 Si1 124.75(18) . . ? C11 C16 Si1 116.08(16) . . ? C113 C111 C112 108.9(2) . . ? C113 C111 P1 111.52(16) . . ? C112 C111 P1 113.71(17) . . ? C123 C121 C122 111.1(2) . . ? C123 C121 P1 112.85(17) . . ? C122 C121 P1 111.73(18) . . ? C21 P2 C221 103.35(11) . . ? C21 P2 C211 103.75(12) . . ? C221 P2 C211 101.28(12) . . ? C21 P2 Ni1 109.71(8) . . ? C221 P2 Ni1 117.82(9) . . ? C211 P2 Ni1 119.00(9) . . ? C26 C21 C22 119.5(2) . . ? C26 C21 P2 115.17(17) . . ? C22 C21 P2 125.19(19) . . ? C23 C22 C21 119.9(2) . . ? C24 C23 C22 121.1(2) . . ? C23 C24 C25 119.4(2) . . ? C24 C25 C26 120.9(2) . . ? C21 C26 C25 119.2(2) . . ? C21 C26 Si1 116.85(17) . . ? C25 C26 Si1 123.79(18) . . ? C212 C211 C213 107.4(2) . . ? C212 C211 P2 111.09(18) . . ? C213 C211 P2 114.9(2) . . ? C222 C221 C223 110.4(2) . . ? C222 C221 P2 114.43(18) . . ? C223 C221 P2 111.88(19) . . ? C31 P3 C321 106.31(11) . . ? C31 P3 C311 102.60(11) . . ? C321 P3 C311 101.02(12) . . ? C31 P3 Ni1 108.78(7) . . ? C321 P3 Ni1 115.87(9) . . ? C311 P3 Ni1 120.71(8) . . ? C32 C31 C36 120.1(2) . . ? C32 C31 P3 125.61(17) . . ? C36 C31 P3 114.34(16) . . ? C33 C32 C31 119.8(2) . . ? C34 C33 C32 120.6(2) . . ? C33 C34 C35 120.0(2) . . ? C34 C35 C36 120.4(2) . . ? C35 C36 C31 119.18(19) . . ? C35 C36 Si1 123.85(16) . . ? C31 C36 Si1 116.68(16) . . ? C313 C311 C312 109.2(2) . . ? C313 C311 P3 111.58(17) . . ? C312 C311 P3 113.49(18) . . ? C322 C321 C323 110.8(2) . . ? C322 C321 P3 113.41(17) . . ? C323 C321 P3 112.20(18) . . ? C421 B1 C431 113.02(18) . . ? C421 B1 C411 105.04(17) . . ? C431 B1 C411 111.84(18) . . ? C421 B1 C441 112.23(18) . . ? C431 B1 C441 103.66(17) . . ? C411 B1 C441 111.24(18) . . ? C412 C411 C418 115.6(2) . . ? C412 C411 B1 121.79(19) . . ? C418 C411 B1 122.5(2) . . ? C413 C412 C411 122.8(2) . . ? C415 C413 C412 120.6(2) . . ? C415 C413 C414 120.7(2) . . ? C412 C413 C414 118.7(2) . . ? F11 C414 F13 107.0(2) . . ? F11 C414 F12 105.0(2) . . ? F13 C414 F12 105.8(2) . . ? F11 C414 C413 112.5(2) . . ? F13 C414 C413 113.2(2) . . ? F12 C414 C413 112.61(19) . . ? C416 C415 C413 118.0(2) . . ? C415 C416 C418 121.1(2) . . ? C415 C416 C417 119.6(2) . . ? C418 C416 C417 119.1(2) . . ? F16 C417 F14 106.3(2) . . ? F16 C417 F15 106.7(2) . . ? F14 C417 F15 106.1(2) . . ? F16 C417 C416 112.1(2) . . ? F14 C417 C416 112.6(2) . . ? F15 C417 C416 112.6(2) . . ? C416 C418 C411 121.9(2) . . ? C422 C421 C428 115.5(2) . . ? C422 C421 B1 124.29(19) . . ? C428 C421 B1 119.93(19) . . ? C423 C422 C421 122.3(2) . . ? C425 C423 C422 121.2(2) . . ? C425 C423 C424 120.0(2) . . ? C422 C423 C424 118.9(2) . . ? F23 C424 F21 108.9(3) . . ? F23 C424 F22 105.8(3) . . ? F21 C424 F22 103.0(2) . . ? F23 C424 C423 113.7(2) . . ? F21 C424 C423 112.5(2) . . ? F22 C424 C423 112.2(2) . . ? C423 C425 C426 117.6(2) . . ? C428 C426 C425 121.1(2) . . ? C428 C426 C427 119.7(2) . . ? C425 C426 C427 119.1(2) . . ? F26 C427 F24 106.7(2) . . ? F26 C427 F25 106.0(2) . . ? F24 C427 F25 105.3(2) . . ? F26 C427 C426 112.9(2) . . ? F24 C427 C426 112.8(2) . . ? F25 C427 C426 112.6(2) . . ? C426 C428 C421 122.2(2) . . ? C438 C431 C432 115.65(19) . . ? C438 C431 B1 121.8(2) . . ? C432 C431 B1 122.04(19) . . ? C433 C432 C431 122.3(2) . . ? C435 C433 C432 120.9(2) . . ? C435 C433 C434 119.2(2) . . ? C432 C433 C434 119.9(2) . . ? F32 C434 F33 105.7(2) . . ? F32 C434 F31 106.5(2) . . ? F33 C434 F31 106.3(2) . . ? F32 C434 C433 112.4(2) . . ? F33 C434 C433 112.8(2) . . ? F31 C434 C433 112.6(2) . . ? C436 C435 C433 117.9(2) . . ? C435 C436 C438 121.0(2) . . ? C435 C436 C437 120.6(2) . . ? C438 C436 C437 118.3(2) . . ? F36 C437 F34 107.0(2) . . ? F36 C437 F35 105.6(2) . . ? F34 C437 F35 105.7(2) . . ? F36 C437 C436 112.75(19) . . ? F34 C437 C436 113.4(2) . . ? F35 C437 C436 111.83(19) . . ? C436 C438 C431 122.2(2) . . ? C448 C441 C442 115.7(2) . . ? C448 C441 B1 121.1(2) . . ? C442 C441 B1 122.9(2) . . ? C443 C442 C441 122.4(3) . . ? C445 C443 C442 120.6(3) . . ? C445 C443 C444 118.5(2) . . ? C442 C443 C444 120.8(3) . . ? F41 C444 F43 109.7(4) . . ? F41 C444 F42 104.6(3) . . ? F43 C444 F42 104.6(3) . . ? F41 C444 C443 114.5(2) . . ? F43 C444 C443 111.6(2) . . ? F42 C444 C443 111.2(3) . . ? C446 C445 C443 118.2(2) . . ? C445 C446 C448 121.4(3) . . ? C445 C446 C447 121.3(3) . . ? C448 C446 C447 117.3(3) . . ? F45 C447 F46 107.6(3) . . ? F45 C447 F44 106.1(2) . . ? F46 C447 F44 106.5(2) . . ? F45 C447 C446 111.9(2) . . ? F46 C447 C446 112.6(2) . . ? F44 C447 C446 111.8(3) . . ? C441 C448 C446 121.6(3) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 30.54 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 2.027 _refine_diff_density_min -0.826 _refine_diff_density_rms 0.084 ####################################################### # Compound 6a: [SiP(iPr)3]Ni-H # ####################################################### data_ct15 _database_code_depnum_ccdc_archive 'CCDC 844856' #TrackingRef 'Ni combined cif.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common '[SiP(iPr)3]Ni-H' _chemical_melting_point 'not measured' _chemical_formula_moiety 'C36 H55 Ni P3 Si' _chemical_formula_sum 'C36 H55 Cl Ni P3 Si' _chemical_formula_weight 702.96 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' Si Si 0.0817 0.0704 '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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.9905(7) _cell_length_b 11.1304(7) _cell_length_c 16.8144(11) _cell_angle_alpha 78.237(3) _cell_angle_beta 79.052(3) _cell_angle_gamma 61.648(2) _cell_volume 1761.8(2) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9920 _cell_measurement_theta_min 2.27 _cell_measurement_theta_max 36.99 _exptl_crystal_description plate _exptl_crystal_colour orange _exptl_crystal_size_max 0.36 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.325 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 750 _exptl_absorpt_coefficient_mu 0.821 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7564 _exptl_absorpt_correction_T_max 0.9679 _exptl_absorpt_process_details 'SADABS v2008/1 (Bruker-AXS, 2008)' _exptl_special_details ; 'Bruker KAPPA APEX II' ; _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 KAPPA APEX II' _diffrn_measurement_method '\w and \f scans' _diffrn_detector_area_resol_mean 8.3 _diffrn_reflns_number 82069 _diffrn_reflns_av_R_equivalents 0.0631 _diffrn_reflns_av_sigmaI/netI 0.0560 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 1.24 _diffrn_reflns_theta_max 36.32 _reflns_number_total 16765 _reflns_number_gt 12147 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 v2010.7-0 (Bruker-AXS, 2010)' _computing_cell_refinement 'SAINT-Plus v7.66A (Bruker-AXS, 2009)' _computing_data_reduction 'SAINT-Plus v7.66A (Bruker-AXS, 2009)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. The hydride bound to the nickel center was located in the difference map and refined semi-freely, with the Ueq of the hydride constrained to be 1.2 times that of the nickel to which it is bound. The difference map indicated that the hydride position is partially occup- ied by chloride. The chloride occupancy refines to about 2.6 %, which is consistent with what is seen in the corresponding NMR spectra. ; _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^)+(0.0485P)^2^+1.1686P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 16765 _refine_ls_number_parameters 390 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0750 _refine_ls_R_factor_gt 0.0462 _refine_ls_wR_factor_ref 0.1168 _refine_ls_wR_factor_gt 0.1045 _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 Ni1 Ni 0.372451(19) 0.195843(18) 0.302492(11) 0.00783(4) Uani 1 1 d . . . Cl1 Cl 0.4439(16) 0.0775(16) 0.4306(9) 0.017(5) Uiso 0.026(2) 1 d P A 1 H100 H 0.401(3) 0.133(3) 0.3884(16) 0.021 Uiso 0.974(2) 1 d P A 2 Si1 Si 0.31062(4) 0.30423(4) 0.18082(2) 0.00874(7) Uani 1 1 d . A . P1 P 0.16939(4) 0.19345(4) 0.32334(2) 0.00891(7) Uani 1 1 d . A . C11 C 0.11710(16) 0.20039(15) 0.22397(9) 0.0113(2) Uani 1 1 d . . . C12 C 0.02643(17) 0.15100(17) 0.21261(10) 0.0157(3) Uani 1 1 d . A . H12 H -0.0110 0.1079 0.2581 0.019 Uiso 1 1 calc R . . C13 C -0.00890(19) 0.16516(19) 0.13454(11) 0.0197(3) Uani 1 1 d . . . H13 H -0.0700 0.1313 0.1269 0.024 Uiso 1 1 calc R A . C14 C 0.0456(2) 0.22923(19) 0.06761(11) 0.0210(3) Uani 1 1 d . A . H14 H 0.0215 0.2389 0.0145 0.025 Uiso 1 1 calc R . . C15 C 0.13516(18) 0.27876(17) 0.07879(10) 0.0167(3) Uani 1 1 d . . . H15 H 0.1710 0.3231 0.0332 0.020 Uiso 1 1 calc R A . C16 C 0.17323(16) 0.26408(15) 0.15648(9) 0.0114(2) Uani 1 1 d . A . C111 C 0.00274(16) 0.33429(15) 0.36698(9) 0.0123(2) Uani 1 1 d . . . H111 H 0.0221 0.3486 0.4192 0.015 Uiso 1 1 calc R A . C112 C -0.03884(17) 0.47093(16) 0.31023(10) 0.0161(3) Uani 1 1 d . A . H11A H -0.0586 0.4611 0.2581 0.024 Uiso 1 1 calc R . . H11B H 0.0375 0.4960 0.3005 0.024 Uiso 1 1 calc R . . H11C H -0.1221 0.5431 0.3358 0.024 Uiso 1 1 calc R . . C113 C -0.12264(17) 0.30247(18) 0.38776(12) 0.0200(3) Uani 1 1 d . A . H11D H -0.2036 0.3810 0.4097 0.030 Uiso 1 1 calc R . . H11E H -0.1003 0.2205 0.4286 0.030 Uiso 1 1 calc R . . H11F H -0.1436 0.2857 0.3382 0.030 Uiso 1 1 calc R . . C121 C 0.16128(17) 0.04001(15) 0.38957(9) 0.0128(3) Uani 1 1 d . . . H121 H 0.0705 0.0426 0.3855 0.015 Uiso 1 1 calc R A . C122 C 0.27863(19) -0.09532(16) 0.36355(11) 0.0172(3) Uani 1 1 d . A . H12A H 0.3685 -0.0990 0.3667 0.026 Uiso 1 1 calc R . . H12B H 0.2718 -0.1011 0.3073 0.026 Uiso 1 1 calc R . . H12C H 0.2709 -0.1728 0.4000 0.026 Uiso 1 1 calc R . . C123 C 0.1680(2) 0.04627(18) 0.47878(10) 0.0186(3) Uani 1 1 d . A . H12D H 0.1660 -0.0354 0.5131 0.028 Uiso 1 1 calc R . . H12E H 0.0881 0.1293 0.4969 0.028 Uiso 1 1 calc R . . H12F H 0.2543 0.0489 0.4833 0.028 Uiso 1 1 calc R . . P2 P 0.38469(4) 0.38272(4) 0.31671(2) 0.00912(7) Uani 1 1 d . A . C21 C 0.26203(15) 0.53045(14) 0.25278(9) 0.0106(2) Uani 1 1 d . . . C22 C 0.19603(17) 0.66792(15) 0.26831(10) 0.0146(3) Uani 1 1 d . A . H22 H 0.2149 0.6911 0.3144 0.018 Uiso 1 1 calc R . . C23 C 0.10287(17) 0.77035(16) 0.21615(11) 0.0165(3) Uani 1 1 d . . . H23 H 0.0575 0.8632 0.2270 0.020 Uiso 1 1 calc R A . C24 C 0.07618(17) 0.73702(16) 0.14835(10) 0.0159(3) Uani 1 1 d . A . H24 H 0.0128 0.8072 0.1129 0.019 Uiso 1 1 calc R . . C25 C 0.14190(16) 0.60118(15) 0.13203(9) 0.0133(3) Uani 1 1 d . . . H25 H 0.1237 0.5796 0.0851 0.016 Uiso 1 1 calc R A . C26 C 0.23435(15) 0.49628(15) 0.18405(9) 0.0106(2) Uani 1 1 d . A . C211 C 0.54522(16) 0.41042(15) 0.28613(9) 0.0121(2) Uani 1 1 d . . . H211 H 0.6207 0.3332 0.3170 0.015 Uiso 1 1 calc R A . C212 C 0.59610(17) 0.40254(17) 0.19523(10) 0.0161(3) Uani 1 1 d . A . H21A H 0.5279 0.4808 0.1627 0.024 Uiso 1 1 calc R . . H21B H 0.6075 0.3164 0.1811 0.024 Uiso 1 1 calc R . . H21C H 0.6855 0.4055 0.1836 0.024 Uiso 1 1 calc R . . C213 C 0.53054(18) 0.54500(17) 0.30716(11) 0.0176(3) Uani 1 1 d . A . H21D H 0.6185 0.5501 0.2901 0.026 Uiso 1 1 calc R . . H21E H 0.5073 0.5471 0.3662 0.026 Uiso 1 1 calc R . . H21F H 0.4565 0.6236 0.2785 0.026 Uiso 1 1 calc R . . C221 C 0.33547(17) 0.43315(16) 0.42186(9) 0.0134(3) Uani 1 1 d . . . H221 H 0.3243 0.5286 0.4182 0.016 Uiso 1 1 calc R A . C222 C 0.19791(18) 0.43255(18) 0.45950(10) 0.0178(3) Uani 1 1 d . A . H22A H 0.2064 0.3401 0.4623 0.027 Uiso 1 1 calc R . . H22B H 0.1241 0.4985 0.4257 0.027 Uiso 1 1 calc R . . H22C H 0.1749 0.4587 0.5147 0.027 Uiso 1 1 calc R . . C223 C 0.45149(19) 0.33556(19) 0.47603(10) 0.0189(3) Uani 1 1 d . A . H22D H 0.4198 0.3545 0.5327 0.028 Uiso 1 1 calc R . . H22E H 0.5342 0.3499 0.4570 0.028 Uiso 1 1 calc R . . H22F H 0.4745 0.2400 0.4729 0.028 Uiso 1 1 calc R . . P3 P 0.54704(4) 0.03809(4) 0.23397(2) 0.00909(7) Uani 1 1 d . A . C31 C 0.58392(16) 0.12185(15) 0.13234(9) 0.0110(2) Uani 1 1 d . . . C32 C 0.71274(16) 0.07415(16) 0.08450(10) 0.0145(3) Uani 1 1 d . A . H32 H 0.7890 -0.0086 0.1036 0.017 Uiso 1 1 calc R . . C33 C 0.72957(18) 0.14710(18) 0.00922(10) 0.0172(3) Uani 1 1 d . . . H33 H 0.8175 0.1145 -0.0227 0.021 Uiso 1 1 calc R A . C34 C 0.61788(18) 0.26790(17) -0.01964(10) 0.0165(3) Uani 1 1 d . A . H34 H 0.6298 0.3180 -0.0709 0.020 Uiso 1 1 calc R . . C35 C 0.48894(17) 0.31488(16) 0.02677(9) 0.0138(3) Uani 1 1 d . . . H35 H 0.4127 0.3962 0.0063 0.017 Uiso 1 1 calc R A . C36 C 0.46972(15) 0.24415(15) 0.10327(9) 0.0106(2) Uani 1 1 d . A . C311 C 0.54373(17) -0.11461(15) 0.20376(10) 0.0135(3) Uani 1 1 d . . . H311 H 0.5196 -0.1661 0.2551 0.016 Uiso 1 1 calc R A . C312 C 0.68155(19) -0.21764(17) 0.16277(11) 0.0191(3) Uani 1 1 d . A . H31A H 0.6700 -0.2942 0.1511 0.029 Uiso 1 1 calc R . . H31B H 0.7541 -0.2532 0.1995 0.029 Uiso 1 1 calc R . . H31C H 0.7085 -0.1713 0.1116 0.029 Uiso 1 1 calc R . . C313 C 0.42931(19) -0.06919(17) 0.14818(11) 0.0194(3) Uani 1 1 d . A . H31D H 0.4533 -0.0253 0.0951 0.029 Uiso 1 1 calc R . . H31E H 0.3406 -0.0035 0.1736 0.029 Uiso 1 1 calc R . . H31F H 0.4210 -0.1498 0.1404 0.029 Uiso 1 1 calc R . . C321 C 0.71402(16) -0.05146(15) 0.28069(9) 0.0126(3) Uani 1 1 d . . . H321 H 0.7897 -0.1045 0.2396 0.015 Uiso 1 1 calc R A . C322 C 0.75127(17) 0.05034(17) 0.30575(10) 0.0157(3) Uani 1 1 d . A . H32A H 0.6792 0.1014 0.3472 0.024 Uiso 1 1 calc R . . H32B H 0.7575 0.1150 0.2578 0.024 Uiso 1 1 calc R . . H32C H 0.8410 0.0001 0.3283 0.024 Uiso 1 1 calc R . . C323 C 0.70480(18) -0.15273(16) 0.35560(10) 0.0176(3) Uani 1 1 d . A . H32D H 0.7926 -0.1985 0.3801 0.026 Uiso 1 1 calc R . . H32E H 0.6871 -0.2219 0.3389 0.026 Uiso 1 1 calc R . . H32F H 0.6287 -0.1026 0.3957 0.026 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ni1 0.00731(8) 0.00694(7) 0.00843(8) 0.00055(5) -0.00254(6) -0.00257(6) Si1 0.00823(17) 0.00778(15) 0.00906(16) 0.00026(12) -0.00279(13) -0.00256(14) P1 0.00805(15) 0.00856(14) 0.01013(15) -0.00019(11) -0.00197(12) -0.00384(13) C11 0.0096(6) 0.0100(5) 0.0128(6) -0.0018(4) -0.0034(5) -0.0025(5) C12 0.0126(7) 0.0167(7) 0.0199(7) -0.0021(5) -0.0046(5) -0.0075(6) C13 0.0188(8) 0.0218(8) 0.0236(8) -0.0036(6) -0.0091(6) -0.0107(7) C14 0.0253(9) 0.0214(8) 0.0194(7) -0.0011(6) -0.0140(6) -0.0094(7) C15 0.0187(7) 0.0160(7) 0.0144(7) 0.0012(5) -0.0073(6) -0.0063(6) C16 0.0106(6) 0.0100(5) 0.0125(6) -0.0012(4) -0.0036(5) -0.0030(5) C111 0.0094(6) 0.0125(6) 0.0142(6) -0.0012(5) 0.0004(5) -0.0051(5) C112 0.0131(7) 0.0116(6) 0.0189(7) -0.0018(5) -0.0003(5) -0.0025(5) C113 0.0103(7) 0.0178(7) 0.0311(9) -0.0052(6) 0.0027(6) -0.0067(6) C121 0.0135(6) 0.0124(6) 0.0138(6) 0.0008(5) -0.0022(5) -0.0076(5) C122 0.0193(7) 0.0115(6) 0.0202(7) 0.0005(5) -0.0033(6) -0.0071(6) C123 0.0246(8) 0.0183(7) 0.0140(7) 0.0017(5) -0.0017(6) -0.0121(7) P2 0.00932(15) 0.00783(14) 0.01033(15) -0.00020(11) -0.00308(12) -0.00366(13) C21 0.0089(6) 0.0085(5) 0.0134(6) 0.0005(4) -0.0017(5) -0.0037(5) C22 0.0143(7) 0.0096(6) 0.0193(7) -0.0023(5) -0.0027(5) -0.0044(5) C23 0.0136(7) 0.0081(6) 0.0225(7) -0.0012(5) -0.0021(6) -0.0009(5) C24 0.0102(6) 0.0117(6) 0.0188(7) 0.0020(5) -0.0030(5) -0.0004(5) C25 0.0120(6) 0.0117(6) 0.0131(6) 0.0019(5) -0.0028(5) -0.0039(5) C26 0.0083(6) 0.0095(5) 0.0115(6) 0.0008(4) -0.0016(4) -0.0027(5) C211 0.0114(6) 0.0100(5) 0.0156(6) 0.0000(5) -0.0039(5) -0.0052(5) C212 0.0139(7) 0.0176(7) 0.0175(7) -0.0006(5) -0.0006(5) -0.0089(6) C213 0.0159(7) 0.0143(6) 0.0261(8) -0.0028(6) -0.0028(6) -0.0095(6) C221 0.0158(7) 0.0138(6) 0.0125(6) -0.0025(5) -0.0036(5) -0.0072(6) C222 0.0185(7) 0.0213(7) 0.0153(7) -0.0054(6) 0.0001(6) -0.0099(6) C223 0.0219(8) 0.0235(8) 0.0142(7) -0.0004(6) -0.0078(6) -0.0113(7) P3 0.00802(15) 0.00742(14) 0.00990(15) 0.00041(11) -0.00191(12) -0.00221(13) C31 0.0107(6) 0.0102(5) 0.0106(6) -0.0009(4) -0.0016(5) -0.0037(5) C32 0.0111(6) 0.0135(6) 0.0145(6) -0.0009(5) -0.0001(5) -0.0029(5) C33 0.0137(7) 0.0208(7) 0.0149(7) -0.0014(5) 0.0019(5) -0.0077(6) C34 0.0168(7) 0.0195(7) 0.0117(6) 0.0017(5) -0.0007(5) -0.0088(6) C35 0.0146(7) 0.0146(6) 0.0110(6) 0.0017(5) -0.0030(5) -0.0065(6) C36 0.0108(6) 0.0107(5) 0.0098(6) -0.0005(4) -0.0018(4) -0.0046(5) C311 0.0136(7) 0.0104(6) 0.0161(6) -0.0030(5) -0.0022(5) -0.0044(5) C312 0.0178(7) 0.0127(6) 0.0243(8) -0.0070(6) 0.0005(6) -0.0041(6) C313 0.0209(8) 0.0151(7) 0.0239(8) -0.0050(6) -0.0080(6) -0.0066(6) C321 0.0104(6) 0.0100(6) 0.0135(6) 0.0012(5) -0.0033(5) -0.0018(5) C322 0.0130(7) 0.0162(7) 0.0169(7) 0.0017(5) -0.0048(5) -0.0063(6) C323 0.0181(7) 0.0123(6) 0.0184(7) 0.0050(5) -0.0077(6) -0.0043(6) _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 Si1 2.2014(5) . ? Ni1 P1 2.2045(5) . ? Ni1 P3 2.2085(4) . ? Ni1 P2 2.2096(4) . ? Ni1 Cl1 2.345(16) . ? Ni1 H100 1.49(3) . ? Cl1 H100 0.88(3) . ? Si1 C36 1.8931(15) . ? Si1 C16 1.8966(16) . ? Si1 C26 1.8981(15) . ? P1 C11 1.8433(15) . ? P1 C121 1.8698(15) . ? P1 C111 1.8927(15) . ? C11 C12 1.403(2) . ? C11 C16 1.412(2) . ? C12 C13 1.396(2) . ? C12 H12 0.9500 . ? C13 C14 1.399(3) . ? C13 H13 0.9500 . ? C14 C15 1.391(3) . ? C14 H14 0.9500 . ? C15 C16 1.401(2) . ? C15 H15 0.9500 . ? C111 C112 1.532(2) . ? C111 C113 1.542(2) . ? C111 H111 1.0000 . ? C112 H11A 0.9800 . ? C112 H11B 0.9800 . ? C112 H11C 0.9800 . ? C113 H11D 0.9800 . ? C113 H11E 0.9800 . ? C113 H11F 0.9800 . ? C121 C122 1.527(2) . ? C121 C123 1.533(2) . ? C121 H121 1.0000 . ? C122 H12A 0.9800 . ? C122 H12B 0.9800 . ? C122 H12C 0.9800 . ? C123 H12D 0.9800 . ? C123 H12E 0.9800 . ? C123 H12F 0.9800 . ? P2 C21 1.8442(15) . ? P2 C221 1.8672(16) . ? P2 C211 1.8919(16) . ? C21 C22 1.404(2) . ? C21 C26 1.412(2) . ? C22 C23 1.394(2) . ? C22 H22 0.9500 . ? C23 C24 1.388(2) . ? C23 H23 0.9500 . ? C24 C25 1.393(2) . ? C24 H24 0.9500 . ? C25 C26 1.398(2) . ? C25 H25 0.9500 . ? C211 C212 1.530(2) . ? C211 C213 1.536(2) . ? C211 H211 1.0000 . ? C212 H21A 0.9800 . ? C212 H21B 0.9800 . ? C212 H21C 0.9800 . ? C213 H21D 0.9800 . ? C213 H21E 0.9800 . ? C213 H21F 0.9800 . ? C221 C222 1.527(2) . ? C221 C223 1.536(2) . ? C221 H221 1.0000 . ? C222 H22A 0.9800 . ? C222 H22B 0.9800 . ? C222 H22C 0.9800 . ? C223 H22D 0.9800 . ? C223 H22E 0.9800 . ? C223 H22F 0.9800 . ? P3 C31 1.8438(15) . ? P3 C321 1.8628(16) . ? P3 C311 1.8883(15) . ? C31 C32 1.400(2) . ? C31 C36 1.416(2) . ? C32 C33 1.389(2) . ? C32 H32 0.9500 . ? C33 C34 1.394(2) . ? C33 H33 0.9500 . ? C34 C35 1.390(2) . ? C34 H34 0.9500 . ? C35 C36 1.400(2) . ? C35 H35 0.9500 . ? C311 C312 1.536(2) . ? C311 C313 1.536(2) . ? C311 H311 1.0000 . ? C312 H31A 0.9800 . ? C312 H31B 0.9800 . ? C312 H31C 0.9800 . ? C313 H31D 0.9800 . ? C313 H31E 0.9800 . ? C313 H31F 0.9800 . ? C321 C322 1.526(2) . ? C321 C323 1.532(2) . ? C321 H321 1.0000 . ? C322 H32A 0.9800 . ? C322 H32B 0.9800 . ? C322 H32C 0.9800 . ? C323 H32D 0.9800 . ? C323 H32E 0.9800 . ? C323 H32F 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Si1 Ni1 P1 85.076(16) . . ? Si1 Ni1 P3 84.652(16) . . ? P1 Ni1 P3 118.269(17) . . ? Si1 Ni1 P2 84.776(16) . . ? P1 Ni1 P2 119.831(16) . . ? P3 Ni1 P2 119.496(17) . . ? Si1 Ni1 Cl1 178.6(4) . . ? P1 Ni1 Cl1 96.0(4) . . ? P3 Ni1 Cl1 94.1(4) . . ? P2 Ni1 Cl1 95.4(4) . . ? Si1 Ni1 H100 174.3(9) . . ? P1 Ni1 H100 91.3(9) . . ? P3 Ni1 H100 101.0(9) . . ? P2 Ni1 H100 93.2(9) . . ? Cl1 Ni1 H100 7.1(10) . . ? Ni1 Cl1 H100 12.1(17) . . ? C36 Si1 C16 111.00(7) . . ? C36 Si1 C26 110.78(7) . . ? C16 Si1 C26 109.48(7) . . ? C36 Si1 Ni1 108.71(5) . . ? C16 Si1 Ni1 108.55(5) . . ? C26 Si1 Ni1 108.24(5) . . ? C11 P1 C121 106.39(7) . . ? C11 P1 C111 99.38(7) . . ? C121 P1 C111 99.38(7) . . ? C11 P1 Ni1 108.73(5) . . ? C121 P1 Ni1 116.51(5) . . ? C111 P1 Ni1 124.11(5) . . ? C12 C11 C16 120.08(14) . . ? C12 C11 P1 125.04(12) . . ? C16 C11 P1 114.87(11) . . ? C13 C12 C11 120.08(16) . . ? C13 C12 H12 120.0 . . ? C11 C12 H12 120.0 . . ? C12 C13 C14 120.00(16) . . ? C12 C13 H13 120.0 . . ? C14 C13 H13 120.0 . . ? C15 C14 C13 120.02(15) . . ? C15 C14 H14 120.0 . . ? C13 C14 H14 120.0 . . ? C14 C15 C16 120.87(16) . . ? C14 C15 H15 119.6 . . ? C16 C15 H15 119.6 . . ? C15 C16 C11 118.95(14) . . ? C15 C16 Si1 126.41(12) . . ? C11 C16 Si1 114.30(11) . . ? C112 C111 C113 108.88(13) . . ? C112 C111 P1 111.20(10) . . ? C113 C111 P1 115.42(11) . . ? C112 C111 H111 107.0 . . ? C113 C111 H111 107.0 . . ? P1 C111 H111 107.0 . . ? C111 C112 H11A 109.5 . . ? C111 C112 H11B 109.5 . . ? H11A C112 H11B 109.5 . . ? C111 C112 H11C 109.5 . . ? H11A C112 H11C 109.5 . . ? H11B C112 H11C 109.5 . . ? C111 C113 H11D 109.5 . . ? C111 C113 H11E 109.5 . . ? H11D C113 H11E 109.5 . . ? C111 C113 H11F 109.5 . . ? H11D C113 H11F 109.5 . . ? H11E C113 H11F 109.5 . . ? C122 C121 C123 109.50(13) . . ? C122 C121 P1 112.19(11) . . ? C123 C121 P1 109.69(11) . . ? C122 C121 H121 108.5 . . ? C123 C121 H121 108.5 . . ? P1 C121 H121 108.5 . . ? C121 C122 H12A 109.5 . . ? C121 C122 H12B 109.5 . . ? H12A C122 H12B 109.5 . . ? C121 C122 H12C 109.5 . . ? H12A C122 H12C 109.5 . . ? H12B C122 H12C 109.5 . . ? C121 C123 H12D 109.5 . . ? C121 C123 H12E 109.5 . . ? H12D C123 H12E 109.5 . . ? C121 C123 H12F 109.5 . . ? H12D C123 H12F 109.5 . . ? H12E C123 H12F 109.5 . . ? C21 P2 C221 105.20(7) . . ? C21 P2 C211 100.02(7) . . ? C221 P2 C211 99.81(7) . . ? C21 P2 Ni1 108.47(5) . . ? C221 P2 Ni1 116.12(5) . . ? C211 P2 Ni1 124.74(5) . . ? C22 C21 C26 119.93(13) . . ? C22 C21 P2 125.40(12) . . ? C26 C21 P2 114.66(10) . . ? C23 C22 C21 119.99(15) . . ? C23 C22 H22 120.0 . . ? C21 C22 H22 120.0 . . ? C24 C23 C22 120.13(14) . . ? C24 C23 H23 119.9 . . ? C22 C23 H23 119.9 . . ? C23 C24 C25 120.33(14) . . ? C23 C24 H24 119.8 . . ? C25 C24 H24 119.8 . . ? C24 C25 C26 120.63(15) . . ? C24 C25 H25 119.7 . . ? C26 C25 H25 119.7 . . ? C25 C26 C21 118.98(13) . . ? C25 C26 Si1 126.11(12) . . ? C21 C26 Si1 114.34(10) . . ? C212 C211 C213 108.52(13) . . ? C212 C211 P2 112.35(11) . . ? C213 C211 P2 114.95(11) . . ? C212 C211 H211 106.9 . . ? C213 C211 H211 106.9 . . ? P2 C211 H211 106.9 . . ? C211 C212 H21A 109.5 . . ? C211 C212 H21B 109.5 . . ? H21A C212 H21B 109.5 . . ? C211 C212 H21C 109.5 . . ? H21A C212 H21C 109.5 . . ? H21B C212 H21C 109.5 . . ? C211 C213 H21D 109.5 . . ? C211 C213 H21E 109.5 . . ? H21D C213 H21E 109.5 . . ? C211 C213 H21F 109.5 . . ? H21D C213 H21F 109.5 . . ? H21E C213 H21F 109.5 . . ? C222 C221 C223 110.41(14) . . ? C222 C221 P2 111.16(11) . . ? C223 C221 P2 109.93(11) . . ? C222 C221 H221 108.4 . . ? C223 C221 H221 108.4 . . ? P2 C221 H221 108.4 . . ? C221 C222 H22A 109.5 . . ? C221 C222 H22B 109.5 . . ? H22A C222 H22B 109.5 . . ? C221 C222 H22C 109.5 . . ? H22A C222 H22C 109.5 . . ? H22B C222 H22C 109.5 . . ? C221 C223 H22D 109.5 . . ? C221 C223 H22E 109.5 . . ? H22D C223 H22E 109.5 . . ? C221 C223 H22F 109.5 . . ? H22D C223 H22F 109.5 . . ? H22E C223 H22F 109.5 . . ? C31 P3 C321 105.98(7) . . ? C31 P3 C311 100.03(7) . . ? C321 P3 C311 99.61(7) . . ? C31 P3 Ni1 108.66(5) . . ? C321 P3 Ni1 115.41(5) . . ? C311 P3 Ni1 124.89(5) . . ? C32 C31 C36 119.77(14) . . ? C32 C31 P3 125.21(11) . . ? C36 C31 P3 115.01(11) . . ? C33 C32 C31 120.36(14) . . ? C33 C32 H32 119.8 . . ? C31 C32 H32 119.8 . . ? C32 C33 C34 120.21(15) . . ? C32 C33 H33 119.9 . . ? C34 C33 H33 119.9 . . ? C35 C34 C33 119.87(15) . . ? C35 C34 H34 120.1 . . ? C33 C34 H34 120.1 . . ? C34 C35 C36 121.02(14) . . ? C34 C35 H35 119.5 . . ? C36 C35 H35 119.5 . . ? C35 C36 C31 118.75(14) . . ? C35 C36 Si1 126.94(11) . . ? C31 C36 Si1 113.88(10) . . ? C312 C311 C313 108.49(14) . . ? C312 C311 P3 115.69(12) . . ? C313 C311 P3 111.57(11) . . ? C312 C311 H311 106.9 . . ? C313 C311 H311 106.9 . . ? P3 C311 H311 106.9 . . ? C311 C312 H31A 109.5 . . ? C311 C312 H31B 109.5 . . ? H31A C312 H31B 109.5 . . ? C311 C312 H31C 109.5 . . ? H31A C312 H31C 109.5 . . ? H31B C312 H31C 109.5 . . ? C311 C313 H31D 109.5 . . ? C311 C313 H31E 109.5 . . ? H31D C313 H31E 109.5 . . ? C311 C313 H31F 109.5 . . ? H31D C313 H31F 109.5 . . ? H31E C313 H31F 109.5 . . ? C322 C321 C323 109.43(13) . . ? C322 C321 P3 111.68(10) . . ? C323 C321 P3 110.08(11) . . ? C322 C321 H321 108.5 . . ? C323 C321 H321 108.5 . . ? P3 C321 H321 108.5 . . ? C321 C322 H32A 109.5 . . ? C321 C322 H32B 109.5 . . ? H32A C322 H32B 109.5 . . ? C321 C322 H32C 109.5 . . ? H32A C322 H32C 109.5 . . ? H32B C322 H32C 109.5 . . ? C321 C323 H32D 109.5 . . ? C321 C323 H32E 109.5 . . ? H32D C323 H32E 109.5 . . ? C321 C323 H32F 109.5 . . ? H32D C323 H32F 109.5 . . ? H32E C323 H32F 109.5 . . ? _diffrn_measured_fraction_theta_max 0.980 _diffrn_reflns_theta_full 36.32 _diffrn_measured_fraction_theta_full 0.980 _refine_diff_density_max 1.065 _refine_diff_density_min -0.544 _refine_diff_density_rms 0.118 ####################################################### # Compound 2b: {[SiP(Ph)3]Ni-N2}{BArF} # ####################################################### data_ct07 _database_code_depnum_ccdc_archive 'CCDC 844857' #TrackingRef 'Ni combined cif.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common {[SiP(Ph)3]Ni-N2}{BArF} _chemical_melting_point 'not measured' _chemical_formula_moiety 'C54 H42 N2 Ni P3 Si, C32 H12 B F24' _chemical_formula_sum 'C86 H54 B F24 N2 Ni P3 Si' _chemical_formula_weight 1761.83 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' N N 0.0061 0.0033 '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' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 13.2952(6) _cell_length_b 15.4595(7) _cell_length_c 20.2687(10) _cell_angle_alpha 74.996(3) _cell_angle_beta 84.981(3) _cell_angle_gamma 83.775(3) _cell_volume 3992.6(3) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 8871 _cell_measurement_theta_min 2.43 _cell_measurement_theta_max 29.39 _exptl_crystal_description plate _exptl_crystal_colour red _exptl_crystal_size_max 0.23 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.466 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1784 _exptl_absorpt_coefficient_mu 0.422 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9093 _exptl_absorpt_correction_T_max 0.9671 _exptl_absorpt_process_details 'SADABS v2008/1 (Bruker-AXS, 2008)' _exptl_special_details ; 'Bruker KAPPA APEX II' ; _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 KAPPA APEX II' _diffrn_measurement_method '\w and \f scans' _diffrn_detector_area_resol_mean 8.3 _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 72851 _diffrn_reflns_av_R_equivalents 0.0712 _diffrn_reflns_av_sigmaI/netI 0.0802 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 1.81 _diffrn_reflns_theta_max 28.28 _reflns_number_total 19649 _reflns_number_gt 12927 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 v2010.7-0 (Bruker-AXS, 2010)' _computing_cell_refinement 'SAINT-Plus v7.66A (Bruker-AXS, 2009)' _computing_data_reduction 'SAINT-Plus v7.66A (Bruker-AXS, 2009)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. Disordered -CF3 groups on the BArF anion were modeled as an idealized disorder over two positions rotated 60\% from one another, with equivalent fluorine atoms constrained to have equal anisotropic displacement parameters. The disordered BArF anion was also refined with the help of similarity restraints on equivalent 1-2 and 1-3 distances within and between each aryl group. ; _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^)+(0.0401P)^2^+3.3273P] 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 19649 _refine_ls_number_parameters 1073 _refine_ls_number_restraints 1036 _refine_ls_R_factor_all 0.0963 _refine_ls_R_factor_gt 0.0526 _refine_ls_wR_factor_ref 0.1203 _refine_ls_wR_factor_gt 0.1037 _refine_ls_goodness_of_fit_ref 1.011 _refine_ls_restrained_S_all 1.028 _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 0.33794(2) 0.67018(2) 0.292103(17) 0.01377(8) Uani 1 1 d . . . N1 N 0.45598(18) 0.59627(15) 0.32322(12) 0.0211(5) Uani 1 1 d . . . N2 N 0.5195(2) 0.55061(19) 0.34440(15) 0.0360(7) Uani 1 1 d . . . Si1 Si 0.18836(5) 0.74874(5) 0.26742(4) 0.01553(16) Uani 1 1 d . . . P1 P 0.36104(5) 0.78090(4) 0.34006(4) 0.01627(15) Uani 1 1 d . . . C11 C 0.2779(2) 0.88155(17) 0.30657(14) 0.0200(6) Uani 1 1 d . . . C12 C 0.2900(2) 0.96687(18) 0.31451(16) 0.0270(7) Uani 1 1 d . . . H12 H 0.3467 0.9761 0.3365 0.032 Uiso 1 1 calc R . . C13 C 0.2188(2) 1.03799(19) 0.29009(17) 0.0299(7) Uani 1 1 d . . . H13 H 0.2264 1.0961 0.2955 0.036 Uiso 1 1 calc R . . C14 C 0.1364(2) 1.02408(19) 0.25778(15) 0.0269(7) Uani 1 1 d . . . H14 H 0.0874 1.0728 0.2416 0.032 Uiso 1 1 calc R . . C15 C 0.1247(2) 0.94014(18) 0.24888(15) 0.0223(6) Uani 1 1 d . . . H15 H 0.0681 0.9318 0.2263 0.027 Uiso 1 1 calc R . . C16 C 0.1958(2) 0.86725(17) 0.27294(14) 0.0180(6) Uani 1 1 d . . . C111 C 0.4893(2) 0.81635(17) 0.33121(15) 0.0200(6) Uani 1 1 d . . . C112 C 0.5553(2) 0.79794(18) 0.27864(15) 0.0220(6) Uani 1 1 d . . . H112 H 0.5343 0.7643 0.2500 0.026 Uiso 1 1 calc R . . C113 C 0.6520(2) 0.8279(2) 0.26718(17) 0.0305(7) Uani 1 1 d . . . H113 H 0.6966 0.8150 0.2310 0.037 Uiso 1 1 calc R . . C114 C 0.6822(2) 0.8767(2) 0.30899(18) 0.0372(8) Uani 1 1 d . . . H114 H 0.7478 0.8978 0.3013 0.045 Uiso 1 1 calc R . . C115 C 0.6179(2) 0.8951(2) 0.36212(18) 0.0353(8) Uani 1 1 d . . . H115 H 0.6396 0.9285 0.3907 0.042 Uiso 1 1 calc R . . C116 C 0.5218(2) 0.86494(19) 0.37373(16) 0.0266(7) Uani 1 1 d . . . H116 H 0.4781 0.8772 0.4105 0.032 Uiso 1 1 calc R . . C121 C 0.3293(2) 0.75564(18) 0.43204(15) 0.0219(6) Uani 1 1 d . . . C122 C 0.4007(2) 0.7075(2) 0.47762(16) 0.0289(7) Uani 1 1 d . . . H122 H 0.4681 0.6939 0.4611 0.035 Uiso 1 1 calc R . . C123 C 0.3733(3) 0.6795(2) 0.54695(17) 0.0405(9) Uani 1 1 d . . . H123 H 0.4222 0.6474 0.5779 0.049 Uiso 1 1 calc R . . C124 C 0.2754(4) 0.6984(2) 0.57097(19) 0.0498(11) Uani 1 1 d . . . H124 H 0.2568 0.6788 0.6184 0.060 Uiso 1 1 calc R . . C125 C 0.2045(3) 0.7455(2) 0.5265(2) 0.0496(10) Uani 1 1 d . . . H125 H 0.1371 0.7583 0.5434 0.060 Uiso 1 1 calc R . . C126 C 0.2309(3) 0.7746(2) 0.45706(17) 0.0328(7) Uani 1 1 d . . . H126 H 0.1816 0.8074 0.4266 0.039 Uiso 1 1 calc R . . P2 P 0.36604(5) 0.69971(4) 0.17631(4) 0.01508(14) Uani 1 1 d . . . C21 C 0.2465(2) 0.73196(16) 0.13546(14) 0.0171(6) Uani 1 1 d . . . C22 C 0.2364(2) 0.74281(18) 0.06554(15) 0.0227(6) Uani 1 1 d . . . H22 H 0.2946 0.7384 0.0355 0.027 Uiso 1 1 calc R . . C23 C 0.1407(2) 0.76000(19) 0.04054(16) 0.0273(7) Uani 1 1 d . . . H23 H 0.1332 0.7669 -0.0068 0.033 Uiso 1 1 calc R . . C24 C 0.0559(2) 0.7672(2) 0.08410(16) 0.0278(7) Uani 1 1 d . . . H24 H -0.0098 0.7755 0.0671 0.033 Uiso 1 1 calc R . . C25 C 0.0660(2) 0.76236(18) 0.15241(15) 0.0226(6) Uani 1 1 d . . . H25 H 0.0076 0.7705 0.1814 0.027 Uiso 1 1 calc R . . C26 C 0.1619(2) 0.74555(17) 0.17902(14) 0.0180(6) Uani 1 1 d . . . C211 C 0.42624(19) 0.60388(17) 0.14684(14) 0.0167(6) Uani 1 1 d . . . C212 C 0.5227(2) 0.56953(18) 0.16943(15) 0.0218(6) Uani 1 1 d . . . H212 H 0.5524 0.5952 0.2000 0.026 Uiso 1 1 calc R . . C213 C 0.5750(2) 0.49866(19) 0.14756(16) 0.0271(7) Uani 1 1 d . . . H213 H 0.6404 0.4759 0.1630 0.032 Uiso 1 1 calc R . . C214 C 0.5319(2) 0.46082(19) 0.10298(15) 0.0260(7) Uani 1 1 d . . . H214 H 0.5686 0.4135 0.0867 0.031 Uiso 1 1 calc R . . C215 C 0.4355(2) 0.49206(18) 0.08238(15) 0.0251(6) Uani 1 1 d . . . H215 H 0.4055 0.4651 0.0527 0.030 Uiso 1 1 calc R . . C216 C 0.3825(2) 0.56215(18) 0.10452(14) 0.0202(6) Uani 1 1 d . . . H216 H 0.3156 0.5821 0.0908 0.024 Uiso 1 1 calc R . . C221 C 0.4419(2) 0.79227(17) 0.13245(14) 0.0185(6) Uani 1 1 d . . . C222 C 0.5354(2) 0.78132(19) 0.09777(15) 0.0244(6) Uani 1 1 d . . . H222 H 0.5621 0.7233 0.0937 0.029 Uiso 1 1 calc R . . C223 C 0.5900(2) 0.8555(2) 0.06901(17) 0.0322(8) Uani 1 1 d . . . H223 H 0.6544 0.8477 0.0459 0.039 Uiso 1 1 calc R . . C224 C 0.5513(2) 0.9400(2) 0.07394(16) 0.0323(8) Uani 1 1 d . . . H224 H 0.5891 0.9903 0.0546 0.039 Uiso 1 1 calc R . . C225 C 0.4575(2) 0.9518(2) 0.10697(17) 0.0330(8) Uani 1 1 d . . . H225 H 0.4301 1.0102 0.1097 0.040 Uiso 1 1 calc R . . C226 C 0.4031(2) 0.87806(18) 0.13612(16) 0.0260(7) Uani 1 1 d . . . H226 H 0.3386 0.8864 0.1589 0.031 Uiso 1 1 calc R . . P3 P 0.23595(5) 0.55985(4) 0.33616(4) 0.01513(15) Uani 1 1 d . . . C31 C 0.10969(19) 0.60403(17) 0.35952(13) 0.0159(5) Uani 1 1 d . . . C32 C 0.0387(2) 0.55392(19) 0.40447(14) 0.0229(6) Uani 1 1 d . . . H32 H 0.0536 0.4914 0.4236 0.028 Uiso 1 1 calc R . . C33 C -0.0535(2) 0.5969(2) 0.42054(15) 0.0280(7) Uani 1 1 d . . . H33 H -0.1017 0.5636 0.4514 0.034 Uiso 1 1 calc R . . C34 C -0.0764(2) 0.6880(2) 0.39213(16) 0.0285(7) Uani 1 1 d . . . H34 H -0.1397 0.7168 0.4040 0.034 Uiso 1 1 calc R . . C35 C -0.0069(2) 0.73706(19) 0.34644(15) 0.0230(6) Uani 1 1 d . . . H35 H -0.0233 0.7992 0.3264 0.028 Uiso 1 1 calc R . . C36 C 0.08689(19) 0.69553(17) 0.32977(14) 0.0176(6) Uani 1 1 d . . . C311 C 0.27483(19) 0.48096(17) 0.41567(13) 0.0162(5) Uani 1 1 d . . . C312 C 0.2887(2) 0.51775(19) 0.47004(15) 0.0235(6) Uani 1 1 d . . . H312 H 0.2806 0.5811 0.4637 0.028 Uiso 1 1 calc R . . C313 C 0.3140(2) 0.4628(2) 0.53297(15) 0.0265(7) Uani 1 1 d . . . H313 H 0.3227 0.4885 0.5697 0.032 Uiso 1 1 calc R . . C314 C 0.3269(2) 0.3702(2) 0.54257(15) 0.0247(7) Uani 1 1 d . . . H314 H 0.3442 0.3325 0.5858 0.030 Uiso 1 1 calc R . . C315 C 0.3143(2) 0.33314(19) 0.48914(15) 0.0239(6) Uani 1 1 d . . . H315 H 0.3236 0.2698 0.4956 0.029 Uiso 1 1 calc R . . C316 C 0.2881(2) 0.38779(18) 0.42584(14) 0.0210(6) Uani 1 1 d . . . H316 H 0.2792 0.3616 0.3894 0.025 Uiso 1 1 calc R . . C321 C 0.2194(2) 0.49139(17) 0.27782(13) 0.0171(6) Uani 1 1 d . . . C322 C 0.3006(2) 0.43509(17) 0.26028(14) 0.0208(6) Uani 1 1 d . . . H322 H 0.3638 0.4316 0.2797 0.025 Uiso 1 1 calc R . . C323 C 0.2900(2) 0.38423(18) 0.21482(15) 0.0268(7) Uani 1 1 d . . . H323 H 0.3450 0.3443 0.2045 0.032 Uiso 1 1 calc R . . C324 C 0.1989(3) 0.39159(19) 0.18428(15) 0.0296(7) Uani 1 1 d . . . H324 H 0.1916 0.3569 0.1528 0.036 Uiso 1 1 calc R . . C325 C 0.1194(2) 0.44901(19) 0.19965(15) 0.0269(7) Uani 1 1 d . . . H325 H 0.0576 0.4548 0.1780 0.032 Uiso 1 1 calc R . . C326 C 0.1284(2) 0.49862(18) 0.24637(14) 0.0224(6) Uani 1 1 d . . . H326 H 0.0726 0.5376 0.2571 0.027 Uiso 1 1 calc R . . B1 B -0.1684(2) 0.25193(18) 0.20958(15) 0.0152(6) Uani 1 1 d D . . C411 C -0.10773(19) 0.19294(16) 0.15942(13) 0.0153(5) Uani 1 1 d D . . C412 C -0.1441(2) 0.11544(16) 0.15067(14) 0.0176(6) Uani 1 1 d D . . H412 H -0.2102 0.1013 0.1692 0.021 Uiso 1 1 calc R . . C413 C -0.0875(2) 0.05832(17) 0.11598(14) 0.0205(6) Uani 1 1 d D . . C414 C -0.1346(2) -0.0230(2) 0.10981(18) 0.0335(8) Uani 1 1 d D . . F11 F -0.08754(17) -0.05922(12) 0.06159(10) 0.0472(5) Uani 1 1 d D . . F12 F -0.13153(16) -0.08900(12) 0.16801(11) 0.0491(6) Uani 1 1 d D . . F13 F -0.23143(16) -0.00579(15) 0.09702(16) 0.0741(8) Uani 1 1 d D . . C415 C 0.0101(2) 0.07420(18) 0.08973(14) 0.0220(6) Uani 1 1 d D . . H415 H 0.0494 0.0345 0.0668 0.026 Uiso 1 1 calc R . . C416 C 0.04904(19) 0.15061(17) 0.09812(14) 0.0188(6) Uani 1 1 d D . . C417 C 0.1553(2) 0.16902(19) 0.07113(15) 0.0242(6) Uani 1 1 d D . . F14 F 0.21494(13) 0.09367(12) 0.07075(11) 0.0414(5) Uani 1 1 d D . . F15 F 0.15987(13) 0.21956(13) 0.00612(9) 0.0378(5) Uani 1 1 d D . . F16 F 0.19976(13) 0.21256(14) 0.10752(10) 0.0401(5) Uani 1 1 d D . . C418 C -0.00883(19) 0.20896(17) 0.13117(13) 0.0173(6) Uani 1 1 d D . . H418 H 0.0192 0.2614 0.1349 0.021 Uiso 1 1 calc R . . C421 C -0.11244(19) 0.20841(16) 0.28122(13) 0.0150(5) Uani 1 1 d D . . C422 C -0.1283(2) 0.11998(17) 0.31810(14) 0.0185(6) Uani 1 1 d D . . H422 H -0.1796 0.0905 0.3051 0.022 Uiso 1 1 calc R . . C423 C -0.0716(2) 0.07445(17) 0.37281(14) 0.0194(6) Uani 1 1 d D . . C424 C -0.0915(2) -0.01977(18) 0.41012(15) 0.0258(7) Uani 1 1 d D . . F21 F -0.00786(13) -0.06969(10) 0.43463(9) 0.0336(4) Uani 1 1 d D . . F22 F -0.15757(15) -0.02239(12) 0.46410(10) 0.0489(6) Uani 1 1 d D . . F23 F -0.12940(18) -0.06395(11) 0.37066(11) 0.0529(6) Uani 1 1 d D . . C425 C 0.0022(2) 0.11520(17) 0.39490(14) 0.0194(6) Uani 1 1 d D . . H425 H 0.0407 0.0839 0.4326 0.023 Uiso 1 1 calc R . . C426 C 0.0184(2) 0.20306(17) 0.36049(14) 0.0178(6) Uani 1 1 d D . . C427 C 0.0972(2) 0.24884(18) 0.38305(15) 0.0249(7) Uani 1 1 d D . . F24 F 0.12012(19) 0.21299(14) 0.44699(10) 0.0622(8) Uani 1 1 d D . . F25 F 0.06960(15) 0.33541(12) 0.37817(11) 0.0454(5) Uani 1 1 d D . . F26 F 0.18359(15) 0.24782(15) 0.34442(12) 0.0545(6) Uani 1 1 d D . . C428 C -0.03707(19) 0.24793(17) 0.30410(13) 0.0167(6) Uani 1 1 d D . . H428 H -0.0230 0.3074 0.2805 0.020 Uiso 1 1 calc R . . C431 C -0.28955(19) 0.23531(16) 0.21671(14) 0.0160(5) Uani 1 1 d D . . C432 C -0.3477(2) 0.21452(17) 0.27861(15) 0.0194(6) Uani 1 1 d D . . H432 H -0.3177 0.2134 0.3197 0.023 Uiso 1 1 calc R . . C433 C -0.4488(2) 0.19535(18) 0.28202(15) 0.0226(6) Uani 1 1 d D . . C434 C -0.5066(2) 0.1741(2) 0.35008(17) 0.0319(7) Uani 1 1 d D . . F31 F -0.45093(16) 0.12890(16) 0.40112(11) 0.0598(7) Uani 1 1 d D . . F32 F -0.54603(17) 0.24834(14) 0.36820(11) 0.0558(6) Uani 1 1 d D . . F33 F -0.58510(17) 0.12674(17) 0.35095(12) 0.0666(8) Uani 1 1 d D . . C435 C -0.4952(2) 0.19617(18) 0.22367(15) 0.0238(6) Uani 1 1 d D . . H435 H -0.5632 0.1815 0.2262 0.029 Uiso 1 1 calc R . . C436 C -0.4404(2) 0.21888(18) 0.16106(15) 0.0227(6) Uani 1 1 d D . . C437 C -0.4859(2) 0.2166(2) 0.09645(17) 0.0318(7) Uani 1 1 d D . . F34 F -0.58184(18) 0.2063(3) 0.10385(13) 0.1215(15) Uani 1 1 d D . . F35 F -0.4426(2) 0.14834(14) 0.07154(13) 0.0737(8) Uani 1 1 d D . . F36 F -0.46967(18) 0.28735(13) 0.04485(10) 0.0514(6) Uani 1 1 d D . . C438 C -0.34044(19) 0.23859(17) 0.15836(15) 0.0200(6) Uani 1 1 d D . . H438 H -0.3049 0.2551 0.1149 0.024 Uiso 1 1 calc R . . C441 C -0.16066(18) 0.36025(16) 0.17954(13) 0.0146(5) Uani 1 1 d D A . C442 C -0.17174(19) 0.41968(17) 0.22190(14) 0.0176(6) Uani 1 1 d D . . H442 H -0.1796 0.3959 0.2700 0.021 Uiso 1 1 calc R . . C443 C -0.1716(2) 0.51238(17) 0.19606(14) 0.0190(6) Uani 1 1 d D A . C444 C -0.1853(2) 0.57256(19) 0.24402(16) 0.0280(7) Uani 1 1 d D . . F41A F -0.1592(4) 0.5308(2) 0.30721(16) 0.0923(15) Uani 0.843(4) 1 d PD A 1 F42A F -0.27829(19) 0.6046(3) 0.2526(2) 0.0892(15) Uani 0.843(4) 1 d PD A 1 F43A F -0.1297(3) 0.6402(2) 0.22656(18) 0.0811(14) Uani 0.843(4) 1 d PD A 1 F41B F -0.2195(16) 0.6545(10) 0.2093(8) 0.0923(15) Uani 0.157(4) 1 d PD A 2 F42B F -0.1108(10) 0.5793(13) 0.2680(10) 0.0892(15) Uani 0.157(4) 1 d PD A 2 F43B F -0.2461(13) 0.5508(11) 0.2914(9) 0.0811(14) Uani 0.157(4) 1 d PD A 2 C445 C -0.1635(2) 0.55020(17) 0.12623(15) 0.0230(6) Uani 1 1 d D . . H445 H -0.1636 0.6134 0.1085 0.028 Uiso 1 1 calc R A . C446 C -0.1552(2) 0.49313(17) 0.08271(14) 0.0208(6) Uani 1 1 d D A . C447 C -0.1534(2) 0.53375(19) 0.00719(15) 0.0295(7) Uani 1 1 d D . . F44 F -0.07680(14) 0.58562(12) -0.01573(9) 0.0416(5) Uani 1 1 d D A . F45 F -0.23813(14) 0.58763(13) -0.01057(10) 0.0424(5) Uani 1 1 d D A . F46 F -0.14530(19) 0.47253(12) -0.02928(9) 0.0530(6) Uani 1 1 d D A . C448 C -0.1528(2) 0.40049(17) 0.10901(14) 0.0189(6) Uani 1 1 d D . . H448 H -0.1457 0.3631 0.0781 0.023 Uiso 1 1 calc R A . 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 0.01194(16) 0.01532(16) 0.01428(18) -0.00429(13) -0.00145(13) -0.00034(12) N1 0.0190(12) 0.0207(11) 0.0229(13) -0.0050(10) -0.0018(10) 0.0001(10) N2 0.0295(15) 0.0403(16) 0.0361(17) -0.0065(13) -0.0080(13) 0.0032(13) Si1 0.0129(3) 0.0166(3) 0.0165(4) -0.0035(3) -0.0010(3) 0.0002(3) P1 0.0143(3) 0.0182(3) 0.0180(4) -0.0076(3) -0.0013(3) -0.0010(3) C11 0.0197(14) 0.0190(13) 0.0216(15) -0.0071(11) 0.0001(12) 0.0001(11) C12 0.0269(16) 0.0221(14) 0.0360(19) -0.0127(13) -0.0054(14) -0.0030(12) C13 0.0338(17) 0.0181(14) 0.0390(19) -0.0112(13) 0.0002(15) 0.0000(12) C14 0.0286(16) 0.0228(14) 0.0271(17) -0.0063(12) 0.0016(13) 0.0043(12) C15 0.0220(14) 0.0228(14) 0.0206(15) -0.0035(11) -0.0027(12) 0.0004(11) C16 0.0197(14) 0.0184(12) 0.0146(14) -0.0034(10) 0.0026(11) -0.0006(10) C111 0.0168(13) 0.0210(13) 0.0232(16) -0.0057(11) -0.0045(11) -0.0031(10) C112 0.0172(14) 0.0266(14) 0.0236(16) -0.0082(12) -0.0034(12) -0.0019(11) C113 0.0210(15) 0.0422(18) 0.0303(18) -0.0121(14) 0.0031(13) -0.0083(13) C114 0.0227(16) 0.049(2) 0.046(2) -0.0177(17) -0.0011(15) -0.0157(15) C115 0.0308(18) 0.0406(18) 0.044(2) -0.0218(16) -0.0063(16) -0.0143(14) C116 0.0266(16) 0.0308(15) 0.0285(17) -0.0165(13) -0.0027(13) -0.0055(12) C121 0.0247(15) 0.0221(13) 0.0224(16) -0.0111(12) 0.0006(12) -0.0055(11) C122 0.0325(17) 0.0315(16) 0.0249(17) -0.0071(13) -0.0058(14) -0.0092(13) C123 0.064(3) 0.0403(19) 0.0221(18) -0.0080(15) -0.0114(17) -0.0184(18) C124 0.086(3) 0.046(2) 0.0227(19) -0.0152(16) 0.013(2) -0.023(2) C125 0.058(3) 0.047(2) 0.044(2) -0.0194(18) 0.027(2) -0.0094(19) C126 0.0359(18) 0.0330(16) 0.0297(18) -0.0128(14) 0.0097(15) -0.0015(14) P2 0.0138(3) 0.0168(3) 0.0145(4) -0.0039(3) -0.0005(3) -0.0012(3) C21 0.0179(13) 0.0166(12) 0.0165(14) -0.0043(10) -0.0027(11) 0.0007(10) C22 0.0269(15) 0.0226(14) 0.0175(15) -0.0048(11) -0.0023(12) 0.0035(11) C23 0.0332(17) 0.0299(15) 0.0192(16) -0.0080(12) -0.0118(13) 0.0081(13) C24 0.0235(16) 0.0335(16) 0.0274(18) -0.0083(13) -0.0149(13) 0.0057(12) C25 0.0166(14) 0.0260(14) 0.0248(17) -0.0072(12) -0.0029(12) 0.0037(11) C26 0.0202(14) 0.0166(12) 0.0172(14) -0.0042(10) -0.0026(11) -0.0010(10) C211 0.0155(13) 0.0186(12) 0.0159(14) -0.0051(10) 0.0028(11) -0.0018(10) C212 0.0177(14) 0.0260(14) 0.0240(16) -0.0107(12) -0.0023(12) 0.0002(11) C213 0.0181(14) 0.0295(15) 0.0333(18) -0.0093(13) -0.0024(13) 0.0031(12) C214 0.0273(16) 0.0240(14) 0.0267(17) -0.0097(12) 0.0040(13) 0.0014(12) C215 0.0289(16) 0.0233(14) 0.0256(17) -0.0097(12) -0.0024(13) -0.0047(12) C216 0.0201(14) 0.0243(14) 0.0166(15) -0.0042(11) -0.0046(11) -0.0023(11) C221 0.0201(14) 0.0221(13) 0.0135(14) -0.0035(11) 0.0001(11) -0.0057(11) C222 0.0241(15) 0.0256(14) 0.0239(16) -0.0070(12) 0.0028(12) -0.0053(12) C223 0.0251(16) 0.0358(17) 0.0342(19) -0.0057(14) 0.0064(14) -0.0099(13) C224 0.0320(17) 0.0301(16) 0.0330(19) -0.0014(14) 0.0004(14) -0.0132(13) C225 0.0359(18) 0.0213(14) 0.040(2) -0.0042(13) 0.0010(15) -0.0053(13) C226 0.0247(15) 0.0230(14) 0.0294(17) -0.0068(12) 0.0052(13) -0.0033(12) P3 0.0146(3) 0.0165(3) 0.0142(4) -0.0033(3) -0.0015(3) -0.0017(3) C31 0.0150(13) 0.0216(13) 0.0119(13) -0.0056(10) -0.0018(10) -0.0016(10) C32 0.0204(14) 0.0278(14) 0.0191(15) -0.0024(12) -0.0001(12) -0.0051(12) C33 0.0205(15) 0.0408(17) 0.0207(16) -0.0044(13) 0.0051(12) -0.0068(13) C34 0.0154(14) 0.0388(17) 0.0289(18) -0.0079(14) 0.0062(13) 0.0011(12) C35 0.0181(14) 0.0248(14) 0.0258(16) -0.0082(12) 0.0006(12) 0.0033(11) C36 0.0152(13) 0.0226(13) 0.0158(14) -0.0063(11) -0.0015(11) -0.0020(10) C311 0.0136(12) 0.0191(12) 0.0152(14) -0.0020(10) -0.0028(10) -0.0025(10) C312 0.0253(15) 0.0233(14) 0.0219(16) -0.0047(12) -0.0024(12) -0.0037(12) C313 0.0277(16) 0.0348(16) 0.0185(16) -0.0072(13) -0.0059(13) -0.0054(13) C314 0.0180(14) 0.0341(16) 0.0178(15) 0.0021(12) -0.0046(12) -0.0016(12) C315 0.0226(15) 0.0230(14) 0.0220(16) 0.0013(12) -0.0043(12) 0.0007(11) C316 0.0210(14) 0.0237(13) 0.0190(15) -0.0056(11) -0.0039(12) -0.0028(11) C321 0.0219(14) 0.0175(12) 0.0112(13) -0.0007(10) -0.0007(11) -0.0058(10) C322 0.0226(14) 0.0199(13) 0.0197(15) -0.0047(11) -0.0001(12) -0.0030(11) C323 0.0373(18) 0.0193(13) 0.0229(16) -0.0055(12) 0.0039(14) -0.0032(12) C324 0.048(2) 0.0259(15) 0.0179(16) -0.0077(12) -0.0006(14) -0.0121(14) C325 0.0327(17) 0.0313(15) 0.0192(16) -0.0061(12) -0.0045(13) -0.0118(13) C326 0.0225(15) 0.0263(14) 0.0190(15) -0.0054(12) -0.0026(12) -0.0047(12) B1 0.0118(14) 0.0175(14) 0.0161(16) -0.0046(12) -0.0005(12) -0.0001(11) C411 0.0151(13) 0.0174(12) 0.0117(13) -0.0012(10) -0.0032(10) 0.0027(10) C412 0.0158(13) 0.0195(13) 0.0173(14) -0.0050(11) -0.0014(11) 0.0006(10) C413 0.0197(14) 0.0200(13) 0.0217(16) -0.0054(11) -0.0057(12) 0.0030(11) C414 0.0278(17) 0.0292(16) 0.049(2) -0.0216(15) -0.0009(16) 0.0023(13) F11 0.0685(15) 0.0343(10) 0.0481(13) -0.0293(9) 0.0117(11) -0.0111(10) F12 0.0629(14) 0.0319(10) 0.0537(14) -0.0135(10) 0.0176(11) -0.0200(10) F13 0.0366(13) 0.0540(14) 0.156(3) -0.0634(16) -0.0357(15) 0.0056(10) C415 0.0225(15) 0.0237(14) 0.0202(15) -0.0092(11) -0.0031(12) 0.0068(11) C416 0.0157(13) 0.0256(14) 0.0139(14) -0.0041(11) -0.0026(11) 0.0029(11) C417 0.0179(14) 0.0312(15) 0.0250(17) -0.0120(13) -0.0032(12) 0.0041(12) F14 0.0224(9) 0.0356(10) 0.0619(14) -0.0132(9) 0.0084(9) 0.0087(8) F15 0.0274(10) 0.0529(12) 0.0277(10) -0.0006(9) 0.0035(8) -0.0073(9) F16 0.0181(9) 0.0686(13) 0.0445(12) -0.0332(10) 0.0023(8) -0.0081(9) C418 0.0169(13) 0.0196(13) 0.0162(14) -0.0048(11) -0.0060(11) 0.0001(10) C421 0.0136(12) 0.0180(12) 0.0130(14) -0.0044(10) 0.0002(10) 0.0015(10) C422 0.0185(13) 0.0209(13) 0.0185(15) -0.0082(11) -0.0025(11) -0.0037(10) C423 0.0237(14) 0.0185(13) 0.0166(15) -0.0040(11) -0.0036(12) -0.0034(11) C424 0.0279(16) 0.0229(14) 0.0263(17) -0.0023(12) -0.0092(13) -0.0051(12) F21 0.0380(11) 0.0211(8) 0.0373(11) 0.0027(8) -0.0129(9) 0.0007(7) F22 0.0457(12) 0.0345(10) 0.0513(13) 0.0104(9) 0.0173(10) -0.0051(9) F23 0.0856(17) 0.0216(9) 0.0550(14) 0.0021(9) -0.0458(12) -0.0155(10) C425 0.0215(14) 0.0218(13) 0.0153(14) -0.0052(11) -0.0042(11) -0.0006(11) C426 0.0180(13) 0.0198(13) 0.0165(14) -0.0056(11) -0.0037(11) -0.0015(10) C427 0.0259(16) 0.0228(14) 0.0243(17) 0.0009(12) -0.0092(13) -0.0048(12) F24 0.0941(18) 0.0581(13) 0.0346(12) 0.0180(10) -0.0421(12) -0.0503(13) F25 0.0453(12) 0.0267(9) 0.0729(15) -0.0203(10) -0.0299(11) -0.0013(8) F26 0.0286(11) 0.0723(15) 0.0780(17) -0.0433(13) 0.0081(11) -0.0218(10) C428 0.0167(13) 0.0171(12) 0.0157(14) -0.0036(10) 0.0007(11) -0.0010(10) C431 0.0150(13) 0.0124(11) 0.0202(15) -0.0042(10) -0.0025(11) 0.0016(10) C432 0.0179(14) 0.0197(13) 0.0223(15) -0.0094(11) 0.0001(11) -0.0008(10) C433 0.0201(14) 0.0203(13) 0.0281(17) -0.0105(12) 0.0065(12) -0.0009(11) C434 0.0224(16) 0.0390(18) 0.038(2) -0.0166(15) 0.0069(14) -0.0064(13) F31 0.0433(13) 0.0872(17) 0.0332(12) 0.0058(11) 0.0141(10) -0.0007(12) F32 0.0594(14) 0.0580(13) 0.0538(14) -0.0315(11) 0.0223(12) 0.0001(11) F33 0.0588(15) 0.1036(19) 0.0544(15) -0.0411(14) 0.0311(12) -0.0583(14) C435 0.0140(13) 0.0235(14) 0.0351(18) -0.0103(13) 0.0002(12) -0.0009(11) C436 0.0173(14) 0.0230(14) 0.0277(17) -0.0058(12) -0.0046(12) 0.0000(11) C437 0.0234(16) 0.0384(18) 0.0353(19) -0.0098(15) -0.0081(14) -0.0040(13) F34 0.0310(14) 0.291(5) 0.0494(17) -0.038(2) -0.0087(12) -0.051(2) F35 0.128(2) 0.0375(12) 0.0685(17) -0.0256(12) -0.0575(17) 0.0081(13) F36 0.0863(17) 0.0357(11) 0.0355(12) -0.0041(9) -0.0280(12) -0.0129(11) C438 0.0153(13) 0.0197(13) 0.0236(16) -0.0034(11) 0.0000(11) -0.0016(10) C441 0.0102(12) 0.0184(12) 0.0148(14) -0.0035(10) -0.0030(10) 0.0013(10) C442 0.0135(13) 0.0214(13) 0.0182(15) -0.0059(11) -0.0016(11) -0.0006(10) C443 0.0162(13) 0.0197(13) 0.0232(16) -0.0091(11) -0.0032(11) -0.0002(10) C444 0.0288(17) 0.0254(15) 0.0323(19) -0.0109(13) -0.0038(14) -0.0030(12) F41A 0.194(5) 0.0484(17) 0.0441(19) -0.0320(14) -0.051(2) 0.031(2) F42A 0.0212(13) 0.150(4) 0.145(4) -0.133(3) -0.0220(17) 0.0271(17) F43A 0.116(3) 0.069(2) 0.085(3) -0.0612(19) 0.055(2) -0.071(2) F41B 0.194(5) 0.0484(17) 0.0441(19) -0.0320(14) -0.051(2) 0.031(2) F42B 0.0212(13) 0.150(4) 0.145(4) -0.133(3) -0.0220(17) 0.0271(17) F43B 0.116(3) 0.069(2) 0.085(3) -0.0612(19) 0.055(2) -0.071(2) C445 0.0215(14) 0.0153(12) 0.0313(17) -0.0040(12) -0.0039(13) -0.0001(11) C446 0.0214(14) 0.0199(13) 0.0191(15) -0.0007(11) -0.0041(12) -0.0019(11) C447 0.0382(18) 0.0233(14) 0.0233(17) -0.0001(13) 0.0008(14) -0.0026(13) F44 0.0405(11) 0.0396(11) 0.0331(11) 0.0099(9) 0.0070(9) -0.0070(9) F45 0.0360(11) 0.0476(11) 0.0334(11) 0.0088(9) -0.0114(9) 0.0026(9) F46 0.1061(19) 0.0332(10) 0.0168(10) -0.0024(8) -0.0025(11) -0.0042(11) C448 0.0179(13) 0.0199(13) 0.0198(15) -0.0066(11) -0.0022(11) -0.0009(10) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ni1 N1 1.891(2) . ? Ni1 P1 2.2352(8) . ? Ni1 Si1 2.2396(8) . ? Ni1 P3 2.2465(7) . ? Ni1 P2 2.2770(8) . ? N1 N2 1.083(3) . ? Si1 C26 1.870(3) . ? Si1 C36 1.870(3) . ? Si1 C16 1.878(3) . ? P1 C11 1.821(3) . ? P1 C121 1.824(3) . ? P1 C111 1.828(3) . ? C11 C12 1.397(4) . ? C11 C16 1.402(4) . ? C12 C13 1.387(4) . ? C13 C14 1.388(4) . ? C14 C15 1.382(4) . ? C15 C16 1.403(4) . ? C111 C112 1.388(4) . ? C111 C116 1.402(4) . ? C112 C113 1.394(4) . ? C113 C114 1.379(4) . ? C114 C115 1.384(5) . ? C115 C116 1.387(4) . ? C121 C126 1.391(4) . ? C121 C122 1.397(4) . ? C122 C123 1.387(4) . ? C123 C124 1.377(5) . ? C124 C125 1.376(6) . ? C125 C126 1.387(5) . ? P2 C21 1.818(3) . ? P2 C211 1.819(3) . ? P2 C221 1.831(2) . ? C21 C26 1.400(4) . ? C21 C22 1.400(4) . ? C22 C23 1.384(4) . ? C23 C24 1.383(4) . ? C24 C25 1.385(4) . ? C25 C26 1.400(4) . ? C211 C216 1.395(4) . ? C211 C212 1.402(4) . ? C212 C213 1.383(4) . ? C213 C214 1.388(4) . ? C214 C215 1.379(4) . ? C215 C216 1.380(4) . ? C221 C226 1.388(4) . ? C221 C222 1.390(4) . ? C222 C223 1.393(4) . ? C223 C224 1.377(4) . ? C224 C225 1.380(4) . ? C225 C226 1.387(4) . ? P3 C31 1.813(3) . ? P3 C321 1.820(3) . ? P3 C311 1.828(3) . ? C31 C36 1.398(3) . ? C31 C32 1.401(3) . ? C32 C33 1.384(4) . ? C33 C34 1.388(4) . ? C34 C35 1.387(4) . ? C35 C36 1.395(4) . ? C311 C316 1.395(4) . ? C311 C312 1.398(4) . ? C312 C313 1.384(4) . ? C313 C314 1.386(4) . ? C314 C315 1.380(4) . ? C315 C316 1.391(4) . ? C321 C322 1.392(4) . ? C321 C326 1.397(4) . ? C322 C323 1.382(4) . ? C323 C324 1.389(4) . ? C324 C325 1.372(4) . ? C325 C326 1.384(4) . ? B1 C441 1.638(3) . ? B1 C421 1.640(4) . ? B1 C411 1.641(4) . ? B1 C431 1.646(4) . ? C411 C412 1.397(3) . ? C411 C418 1.408(3) . ? C412 C413 1.388(4) . ? C413 C415 1.381(4) . ? C413 C414 1.502(4) . ? C414 F13 1.320(4) . ? C414 F11 1.327(4) . ? C414 F12 1.346(4) . ? C415 C416 1.394(4) . ? C416 C418 1.388(4) . ? C416 C417 1.499(4) . ? C417 F16 1.329(3) . ? C417 F14 1.338(3) . ? C417 F15 1.347(3) . ? C421 C428 1.398(3) . ? C421 C422 1.407(3) . ? C422 C423 1.386(4) . ? C423 C425 1.385(4) . ? C423 C424 1.497(3) . ? C424 F22 1.336(3) . ? C424 F23 1.337(3) . ? C424 F21 1.339(3) . ? C425 C426 1.387(3) . ? C426 C428 1.399(4) . ? C426 C427 1.490(4) . ? C427 F24 1.319(3) . ? C427 F25 1.329(3) . ? C427 F26 1.333(3) . ? C431 C432 1.397(4) . ? C431 C438 1.400(4) . ? C432 C433 1.399(4) . ? C433 C435 1.378(4) . ? C433 C434 1.495(4) . ? C434 F31 1.324(4) . ? C434 F32 1.334(4) . ? C434 F33 1.335(3) . ? C435 C436 1.388(4) . ? C436 C438 1.389(3) . ? C436 C437 1.500(4) . ? C437 F34 1.293(3) . ? C437 F36 1.325(3) . ? C437 F35 1.339(4) . ? C441 C442 1.400(4) . ? C441 C448 1.403(4) . ? C442 C443 1.393(3) . ? C443 C445 1.384(4) . ? C443 C444 1.498(4) . ? C444 F42B 1.166(14) . ? C444 F43B 1.202(15) . ? C444 F42A 1.295(4) . ? C444 F43A 1.303(3) . ? C444 F41B 1.333(14) . ? C444 F41A 1.333(4) . ? C445 C446 1.390(4) . ? C446 C448 1.391(3) . ? C446 C447 1.496(4) . ? C447 F46 1.334(3) . ? C447 F44 1.341(3) . ? C447 F45 1.343(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Ni1 P1 96.32(7) . . ? N1 Ni1 Si1 172.87(7) . . ? P1 Ni1 Si1 83.64(3) . . ? N1 Ni1 P3 93.14(7) . . ? P1 Ni1 P3 125.29(3) . . ? Si1 Ni1 P3 81.16(3) . . ? N1 Ni1 P2 102.30(8) . . ? P1 Ni1 P2 116.33(3) . . ? Si1 Ni1 P2 84.02(3) . . ? P3 Ni1 P2 113.84(3) . . ? N2 N1 Ni1 175.2(2) . . ? C26 Si1 C36 109.59(12) . . ? C26 Si1 C16 111.14(12) . . ? C36 Si1 C16 110.04(12) . . ? C26 Si1 Ni1 107.67(9) . . ? C36 Si1 Ni1 109.45(9) . . ? C16 Si1 Ni1 108.92(9) . . ? C11 P1 C121 103.35(13) . . ? C11 P1 C111 106.42(12) . . ? C121 P1 C111 103.85(13) . . ? C11 P1 Ni1 111.47(10) . . ? C121 P1 Ni1 114.10(9) . . ? C111 P1 Ni1 116.47(10) . . ? C12 C11 C16 120.8(3) . . ? C12 C11 P1 124.6(2) . . ? C16 C11 P1 114.59(19) . . ? C13 C12 C11 119.7(3) . . ? C12 C13 C14 119.9(3) . . ? C15 C14 C13 120.8(3) . . ? C14 C15 C16 120.4(3) . . ? C11 C16 C15 118.5(2) . . ? C11 C16 Si1 116.03(19) . . ? C15 C16 Si1 125.5(2) . . ? C112 C111 C116 118.9(2) . . ? C112 C111 P1 118.8(2) . . ? C116 C111 P1 122.3(2) . . ? C111 C112 C113 121.1(3) . . ? C114 C113 C112 119.2(3) . . ? C113 C114 C115 120.7(3) . . ? C114 C115 C116 120.2(3) . . ? C115 C116 C111 120.0(3) . . ? C126 C121 C122 119.2(3) . . ? C126 C121 P1 120.4(2) . . ? C122 C121 P1 120.0(2) . . ? C123 C122 C121 120.1(3) . . ? C124 C123 C122 120.1(4) . . ? C125 C124 C123 120.2(3) . . ? C124 C125 C126 120.4(4) . . ? C125 C126 C121 120.0(3) . . ? C21 P2 C211 106.73(13) . . ? C21 P2 C221 102.43(12) . . ? C211 P2 C221 104.15(12) . . ? C21 P2 Ni1 110.02(9) . . ? C211 P2 Ni1 113.47(9) . . ? C221 P2 Ni1 118.88(9) . . ? C26 C21 C22 120.6(3) . . ? C26 C21 P2 115.4(2) . . ? C22 C21 P2 124.0(2) . . ? C23 C22 C21 119.4(3) . . ? C24 C23 C22 120.3(3) . . ? C23 C24 C25 120.4(3) . . ? C24 C25 C26 120.4(3) . . ? C25 C26 C21 118.5(3) . . ? C25 C26 Si1 125.0(2) . . ? C21 C26 Si1 116.2(2) . . ? C216 C211 C212 118.4(3) . . ? C216 C211 P2 124.5(2) . . ? C212 C211 P2 117.0(2) . . ? C213 C212 C211 120.6(3) . . ? C212 C213 C214 119.9(3) . . ? C215 C214 C213 119.9(3) . . ? C214 C215 C216 120.5(3) . . ? C215 C216 C211 120.5(3) . . ? C226 C221 C222 119.0(2) . . ? C226 C221 P2 116.8(2) . . ? C222 C221 P2 124.2(2) . . ? C221 C222 C223 120.0(3) . . ? C224 C223 C222 120.4(3) . . ? C223 C224 C225 120.0(3) . . ? C224 C225 C226 119.9(3) . . ? C225 C226 C221 120.8(3) . . ? C31 P3 C321 106.03(12) . . ? C31 P3 C311 103.20(12) . . ? C321 P3 C311 105.91(12) . . ? C31 P3 Ni1 111.69(8) . . ? C321 P3 Ni1 113.72(8) . . ? C311 P3 Ni1 115.34(8) . . ? C36 C31 C32 120.6(2) . . ? C36 C31 P3 114.53(18) . . ? C32 C31 P3 124.8(2) . . ? C33 C32 C31 119.0(3) . . ? C32 C33 C34 120.9(3) . . ? C35 C34 C33 120.0(3) . . ? C34 C35 C36 120.3(3) . . ? C35 C36 C31 119.2(2) . . ? C35 C36 Si1 126.7(2) . . ? C31 C36 Si1 114.10(19) . . ? C316 C311 C312 118.7(2) . . ? C316 C311 P3 124.5(2) . . ? C312 C311 P3 116.7(2) . . ? C313 C312 C311 120.7(3) . . ? C312 C313 C314 120.1(3) . . ? C315 C314 C313 119.8(3) . . ? C314 C315 C316 120.5(3) . . ? C315 C316 C311 120.2(3) . . ? C322 C321 C326 118.9(3) . . ? C322 C321 P3 119.8(2) . . ? C326 C321 P3 121.2(2) . . ? C323 C322 C321 120.5(3) . . ? C322 C323 C324 119.9(3) . . ? C325 C324 C323 119.9(3) . . ? C324 C325 C326 120.7(3) . . ? C325 C326 C321 120.0(3) . . ? C441 B1 C421 114.1(2) . . ? C441 B1 C411 112.7(2) . . ? C421 B1 C411 101.2(2) . . ? C441 B1 C431 107.0(2) . . ? C421 B1 C431 112.6(2) . . ? C411 B1 C431 109.2(2) . . ? C412 C411 C418 115.4(2) . . ? C412 C411 B1 121.9(2) . . ? C418 C411 B1 121.9(2) . . ? C413 C412 C411 122.5(2) . . ? C415 C413 C412 121.2(2) . . ? C415 C413 C414 121.0(3) . . ? C412 C413 C414 117.8(2) . . ? F13 C414 F11 107.9(3) . . ? F13 C414 F12 105.4(3) . . ? F11 C414 F12 105.6(2) . . ? F13 C414 C413 112.7(2) . . ? F11 C414 C413 112.7(3) . . ? F12 C414 C413 112.0(3) . . ? C413 C415 C416 117.7(3) . . ? C418 C416 C415 121.0(2) . . ? C418 C416 C417 120.0(2) . . ? C415 C416 C417 119.0(2) . . ? F16 C417 F14 106.7(2) . . ? F16 C417 F15 106.2(2) . . ? F14 C417 F15 105.7(2) . . ? F16 C417 C416 112.6(2) . . ? F14 C417 C416 112.4(2) . . ? F15 C417 C416 112.7(2) . . ? C416 C418 C411 122.1(2) . . ? C428 C421 C422 115.7(2) . . ? C428 C421 B1 124.3(2) . . ? C422 C421 B1 119.4(2) . . ? C423 C422 C421 122.1(2) . . ? C425 C423 C422 121.2(2) . . ? C425 C423 C424 118.9(2) . . ? C422 C423 C424 119.9(2) . . ? F22 C424 F23 106.6(2) . . ? F22 C424 F21 105.8(2) . . ? F23 C424 F21 106.2(2) . . ? F22 C424 C423 112.1(2) . . ? F23 C424 C423 112.8(2) . . ? F21 C424 C423 112.8(2) . . ? C423 C425 C426 118.2(2) . . ? C425 C426 C428 120.5(2) . . ? C425 C426 C427 119.5(2) . . ? C428 C426 C427 120.1(2) . . ? F24 C427 F25 106.5(3) . . ? F24 C427 F26 106.9(3) . . ? F25 C427 F26 104.8(2) . . ? F24 C427 C426 113.5(2) . . ? F25 C427 C426 112.5(2) . . ? F26 C427 C426 112.2(3) . . ? C421 C428 C426 122.4(2) . . ? C432 C431 C438 115.3(2) . . ? C432 C431 B1 124.6(2) . . ? C438 C431 B1 120.0(2) . . ? C431 C432 C433 122.1(3) . . ? C435 C433 C432 120.8(3) . . ? C435 C433 C434 120.0(2) . . ? C432 C433 C434 119.2(3) . . ? F31 C434 F32 105.1(3) . . ? F31 C434 F33 106.9(3) . . ? F32 C434 F33 105.4(3) . . ? F31 C434 C433 113.9(2) . . ? F32 C434 C433 112.0(3) . . ? F33 C434 C433 112.8(3) . . ? C433 C435 C436 118.6(2) . . ? C435 C436 C438 120.0(3) . . ? C435 C436 C437 120.6(2) . . ? C438 C436 C437 119.3(3) . . ? F34 C437 F36 108.9(3) . . ? F34 C437 F35 105.5(3) . . ? F36 C437 F35 102.3(3) . . ? F34 C437 C436 113.9(3) . . ? F36 C437 C436 113.6(2) . . ? F35 C437 C436 111.6(3) . . ? C436 C438 C431 123.1(3) . . ? C442 C441 C448 115.5(2) . . ? C442 C441 B1 122.3(2) . . ? C448 C441 B1 121.8(2) . . ? C443 C442 C441 122.4(2) . . ? C445 C443 C442 120.8(3) . . ? C445 C443 C444 119.3(2) . . ? C442 C443 C444 119.9(2) . . ? F42B C444 F43B 105.8(11) . . ? F42B C444 F42A 132.5(8) . . ? F43B C444 F42A 50.4(9) . . ? F42B C444 F43A 53.1(9) . . ? F43B C444 F43A 131.1(8) . . ? F42A C444 F43A 107.5(3) . . ? F42B C444 F41B 107.6(11) . . ? F43B C444 F41B 106.0(11) . . ? F42A C444 F41B 58.2(8) . . ? F43A C444 F41B 56.8(8) . . ? F42B C444 F41A 54.1(9) . . ? F43B C444 F41A 56.8(9) . . ? F42A C444 F41A 104.0(3) . . ? F43A C444 F41A 103.5(3) . . ? F41B C444 F41A 138.5(7) . . ? F42B C444 C443 113.8(8) . . ? F43B C444 C443 114.8(8) . . ? F42A C444 C443 113.6(3) . . ? F43A C444 C443 114.1(3) . . ? F41B C444 C443 108.3(7) . . ? F41A C444 C443 113.1(3) . . ? C443 C445 C446 118.2(2) . . ? C445 C446 C448 120.6(3) . . ? C445 C446 C447 118.5(2) . . ? C448 C446 C447 120.8(3) . . ? F46 C447 F44 106.6(3) . . ? F46 C447 F45 106.9(3) . . ? F44 C447 F45 105.4(2) . . ? F46 C447 C446 113.1(2) . . ? F44 C447 C446 112.9(3) . . ? F45 C447 C446 111.4(3) . . ? C446 C448 C441 122.4(3) . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 28.28 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 1.215 _refine_diff_density_min -0.987 _refine_diff_density_rms 0.078 ####################################################### # Compound 4b: {[SiP(Ph)3]Ni-CO}{BArF} # ####################################################### data_ct10 _database_code_depnum_ccdc_archive 'CCDC 844858' #TrackingRef 'Ni combined cif.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common {[SiP(Ph)3]Ni-CO}{BArF} _chemical_melting_point 'not measured' _chemical_formula_moiety 'C55 H42 N2 Ni O P3 Si, C32 H12 B F24' _chemical_formula_sum 'C87 H54 B F24 Ni O P3 Si' _chemical_formula_weight 1761.82 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 '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' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 13.2892(5) _cell_length_b 15.4570(6) _cell_length_c 20.2883(7) _cell_angle_alpha 74.8510(10) _cell_angle_beta 85.1070(10) _cell_angle_gamma 83.8420(10) _cell_volume 3992.3(3) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9902 _cell_measurement_theta_min 2.28 _cell_measurement_theta_max 31.09 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.466 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1784 _exptl_absorpt_coefficient_mu 0.422 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8768 _exptl_absorpt_correction_T_max 0.9670 _exptl_absorpt_process_details 'SADABS v2008/1 (Bruker-AXS, 2008)' _exptl_special_details ; 'Bruker KAPPA APEX II' ; _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 KAPPA APEX II' _diffrn_measurement_method '\w and \f scans' _diffrn_detector_area_resol_mean 8.3 _diffrn_reflns_number 93327 _diffrn_reflns_av_R_equivalents 0.0490 _diffrn_reflns_av_sigmaI/netI 0.0503 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 1.91 _diffrn_reflns_theta_max 30.47 _reflns_number_total 24174 _reflns_number_gt 17722 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 v2010.7-0 (Bruker-AXS, 2010)' _computing_cell_refinement 'SAINT-Plus v7.66A (Bruker-AXS, 2009)' _computing_data_reduction 'SAINT-Plus v7.66A (Bruker-AXS, 2009)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. Disordered -CF3 groups on the BArF anion were modeled as an idealized disorder over two positions rotated 60\% from one another, with equivalent fluorine atoms constrained to have equal anisotropic displacement parameters. The disordered BArF anion was also refined with the help of similarity restraints on equivalent 1-2 and 1-3 distances within and between each aryl group. ; _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^)+(0.0639P)^2^+2.0555P] 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 24174 _refine_ls_number_parameters 1090 _refine_ls_number_restraints 1147 _refine_ls_R_factor_all 0.0733 _refine_ls_R_factor_gt 0.0470 _refine_ls_wR_factor_ref 0.1289 _refine_ls_wR_factor_gt 0.1140 _refine_ls_goodness_of_fit_ref 1.019 _refine_ls_restrained_S_all 1.088 _refine_ls_shift/su_max 0.027 _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 0.659901(18) 0.830930(16) -0.292616(12) 0.01277(6) Uani 1 1 d . . . C1 C 0.54767(15) 0.90039(14) -0.32304(11) 0.0194(4) Uani 1 1 d . . . O1 O 0.47986(12) 0.94647(12) -0.34578(9) 0.0324(4) Uani 1 1 d . . . Si1 Si 0.81136(4) 0.75206(4) -0.26745(3) 0.01450(10) Uani 1 1 d . . . P1 P 0.63821(4) 0.71965(3) -0.33959(3) 0.01561(10) Uani 1 1 d . . . C11 C 0.72156(15) 0.61886(14) -0.30571(11) 0.0198(4) Uani 1 1 d . . . C12 C 0.70953(18) 0.53362(15) -0.31385(13) 0.0274(5) Uani 1 1 d . . . H12 H 0.6527 0.5243 -0.3358 0.033 Uiso 1 1 calc R . . C13 C 0.78118(19) 0.46266(15) -0.28970(14) 0.0304(5) Uani 1 1 d . . . H13 H 0.7733 0.4045 -0.2949 0.037 Uiso 1 1 calc R . . C14 C 0.86474(18) 0.47642(15) -0.25776(12) 0.0269(5) Uani 1 1 d . . . H14 H 0.9142 0.4279 -0.2420 0.032 Uiso 1 1 calc R . . C15 C 0.87581(16) 0.56068(15) -0.24888(11) 0.0228(4) Uani 1 1 d . . . H15 H 0.9324 0.5693 -0.2264 0.027 Uiso 1 1 calc R . . C16 C 0.80419(15) 0.63349(13) -0.27274(10) 0.0177(4) Uani 1 1 d . . . C111 C 0.66979(16) 0.74560(15) -0.43159(11) 0.0213(4) Uani 1 1 d . . . C112 C 0.7685(2) 0.72593(18) -0.45629(14) 0.0338(6) Uani 1 1 d . . . H112 H 0.8178 0.6933 -0.4258 0.041 Uiso 1 1 calc R . . C113 C 0.7942(3) 0.7546(2) -0.52599(16) 0.0497(8) Uani 1 1 d . . . H113 H 0.8613 0.7411 -0.5430 0.060 Uiso 1 1 calc R . . C114 C 0.7228(3) 0.8024(2) -0.57076(14) 0.0483(8) Uani 1 1 d . . . H114 H 0.7411 0.8221 -0.6182 0.058 Uiso 1 1 calc R . . C115 C 0.6252(2) 0.8216(2) -0.54637(13) 0.0409(7) Uani 1 1 d . . . H115 H 0.5760 0.8537 -0.5772 0.049 Uiso 1 1 calc R . . C116 C 0.59845(19) 0.79406(17) -0.47695(12) 0.0293(5) Uani 1 1 d . . . H116 H 0.5314 0.8083 -0.4603 0.035 Uiso 1 1 calc R . . C121 C 0.51039(15) 0.68329(14) -0.33096(11) 0.0193(4) Uani 1 1 d . . . C122 C 0.47915(17) 0.63399(16) -0.37326(12) 0.0261(5) Uani 1 1 d . . . H122 H 0.5234 0.6218 -0.4097 0.031 Uiso 1 1 calc R . . C123 C 0.38324(19) 0.60289(18) -0.36189(14) 0.0344(6) Uani 1 1 d . . . H123 H 0.3624 0.5690 -0.3904 0.041 Uiso 1 1 calc R . . C124 C 0.31773(19) 0.62092(19) -0.30921(14) 0.0354(6) Uani 1 1 d . . . H124 H 0.2523 0.5994 -0.3018 0.042 Uiso 1 1 calc R . . C125 C 0.34739(17) 0.67025(17) -0.26740(13) 0.0301(5) Uani 1 1 d . . . H125 H 0.3025 0.6826 -0.2313 0.036 Uiso 1 1 calc R . . C126 C 0.44320(16) 0.70170(15) -0.27854(11) 0.0227(4) Uani 1 1 d . . . H126 H 0.4632 0.7361 -0.2501 0.027 Uiso 1 1 calc R . . P2 P 0.76162(4) 0.94077(3) -0.33733(2) 0.01393(10) Uani 1 1 d . . . C21 C 0.75282(15) 0.76898(13) -0.13571(10) 0.0161(4) Uani 1 1 d . . . C22 C 0.76238(17) 0.75741(14) -0.06572(11) 0.0222(4) Uani 1 1 d . . . H22 H 0.7038 0.7617 -0.0360 0.027 Uiso 1 1 calc R . . C23 C 0.85793(18) 0.73969(16) -0.04002(12) 0.0271(5) Uani 1 1 d . . . H23 H 0.8650 0.7324 0.0074 0.033 Uiso 1 1 calc R . . C24 C 0.94329(18) 0.73261(16) -0.08352(12) 0.0283(5) Uani 1 1 d . . . H24 H 1.0088 0.7241 -0.0661 0.034 Uiso 1 1 calc R . . C25 C 0.93387(16) 0.73785(15) -0.15192(11) 0.0225(4) Uani 1 1 d . . . H25 H 0.9926 0.7297 -0.1806 0.027 Uiso 1 1 calc R . . C26 C 0.83788(15) 0.75518(13) -0.17905(10) 0.0168(4) Uani 1 1 d . . . C211 C 0.55722(15) 0.71000(14) -0.13359(10) 0.0178(4) Uani 1 1 d . . . C212 C 0.59687(18) 0.62353(15) -0.13609(12) 0.0260(5) Uani 1 1 d . . . H212 H 0.6617 0.6149 -0.1582 0.031 Uiso 1 1 calc R . . C213 C 0.5422(2) 0.55001(16) -0.10648(14) 0.0323(5) Uani 1 1 d . . . H213 H 0.5697 0.4913 -0.1085 0.039 Uiso 1 1 calc R . . C214 C 0.44751(19) 0.56213(17) -0.07399(13) 0.0316(5) Uani 1 1 d . . . H214 H 0.4096 0.5120 -0.0542 0.038 Uiso 1 1 calc R . . C215 C 0.40872(18) 0.64746(17) -0.07057(13) 0.0312(5) Uani 1 1 d . . . H215 H 0.3442 0.6557 -0.0479 0.037 Uiso 1 1 calc R . . C216 C 0.46310(17) 0.72164(15) -0.09997(11) 0.0240(4) Uani 1 1 d . . . H216 H 0.4359 0.7800 -0.0971 0.029 Uiso 1 1 calc R . . C221 C 0.57386(14) 0.89816(13) -0.14827(10) 0.0158(4) Uani 1 1 d . . . C222 C 0.61765(16) 0.93797(14) -0.10431(10) 0.0187(4) Uani 1 1 d . . . H222 H 0.6840 0.9168 -0.0898 0.022 Uiso 1 1 calc R . . C223 C 0.56424(17) 1.00835(15) -0.08192(11) 0.0229(4) Uani 1 1 d . . . H223 H 0.5940 1.0345 -0.0517 0.027 Uiso 1 1 calc R . . C224 C 0.46817(17) 1.04066(15) -0.10328(12) 0.0247(4) Uani 1 1 d . . . H224 H 0.4312 1.0874 -0.0865 0.030 Uiso 1 1 calc R . . C225 C 0.42592(16) 1.00456(15) -0.14932(12) 0.0252(4) Uani 1 1 d . . . H225 H 0.3610 1.0283 -0.1655 0.030 Uiso 1 1 calc R . . C226 C 0.47812(15) 0.93409(14) -0.17173(11) 0.0203(4) Uani 1 1 d . . . H226 H 0.4488 0.9098 -0.2033 0.024 Uiso 1 1 calc R . . P3 P 0.63384(4) 0.80214(3) -0.17738(3) 0.01381(10) Uani 1 1 d . . . C31 C 0.88865(14) 0.89710(14) -0.36015(10) 0.0164(4) Uani 1 1 d . . . C32 C 0.95922(16) 0.94812(16) -0.40488(11) 0.0226(4) Uani 1 1 d . . . H32 H 0.9434 1.0105 -0.4246 0.027 Uiso 1 1 calc R . . C33 C 1.05269(16) 0.90591(17) -0.41980(12) 0.0271(5) Uani 1 1 d . . . H33 H 1.1010 0.9398 -0.4502 0.033 Uiso 1 1 calc R . . C34 C 1.07645(16) 0.81517(17) -0.39103(12) 0.0282(5) Uani 1 1 d . . . H34 H 1.1404 0.7871 -0.4023 0.034 Uiso 1 1 calc R . . C35 C 1.00724(15) 0.76493(15) -0.34570(11) 0.0228(4) Uani 1 1 d . . . H35 H 1.0243 0.7029 -0.3256 0.027 Uiso 1 1 calc R . . C36 C 0.91222(14) 0.80585(14) -0.32970(10) 0.0167(4) Uani 1 1 d . . . C311 C 0.77746(15) 1.00854(13) -0.27861(10) 0.0165(4) Uani 1 1 d . . . C312 C 0.86809(16) 1.00091(15) -0.24670(11) 0.0213(4) Uani 1 1 d . . . H312 H 0.9237 0.9616 -0.2569 0.026 Uiso 1 1 calc R . . C313 C 0.87714(19) 1.05108(16) -0.19974(12) 0.0272(5) Uani 1 1 d . . . H313 H 0.9387 1.0453 -0.1777 0.033 Uiso 1 1 calc R . . C314 C 0.7969(2) 1.10907(15) -0.18519(11) 0.0284(5) Uani 1 1 d . . . H314 H 0.8038 1.1440 -0.1539 0.034 Uiso 1 1 calc R . . C315 C 0.70635(19) 1.11642(15) -0.21607(12) 0.0265(5) Uani 1 1 d . . . H315 H 0.6514 1.1564 -0.2059 0.032 Uiso 1 1 calc R . . C316 C 0.69547(16) 1.06546(14) -0.26196(11) 0.0207(4) Uani 1 1 d . . . H316 H 0.6325 1.0693 -0.2819 0.025 Uiso 1 1 calc R . . C321 C 0.72333(14) 1.02032(14) -0.41699(10) 0.0170(4) Uani 1 1 d . . . C322 C 0.71218(16) 1.11324(14) -0.42705(11) 0.0204(4) Uani 1 1 d . . . H322 H 0.7221 1.1389 -0.3906 0.024 Uiso 1 1 calc R . . C323 C 0.68645(17) 1.16884(15) -0.49043(11) 0.0241(4) Uani 1 1 d . . . H323 H 0.6783 1.2323 -0.4968 0.029 Uiso 1 1 calc R . . C324 C 0.67275(16) 1.13228(16) -0.54414(11) 0.0246(4) Uani 1 1 d . . . H324 H 0.6554 1.1704 -0.5873 0.029 Uiso 1 1 calc R . . C325 C 0.68445(18) 1.03965(17) -0.53461(11) 0.0267(5) Uani 1 1 d . . . H325 H 0.6754 1.0143 -0.5714 0.032 Uiso 1 1 calc R . . C326 C 0.70933(17) 0.98391(15) -0.47157(11) 0.0238(4) Uani 1 1 d . . . H326 H 0.7169 0.9205 -0.4654 0.029 Uiso 1 1 calc R . . B1 B 0.83117(15) 0.75144(14) 0.20944(11) 0.0140(4) Uani 1 1 d D . . C411 C 0.89267(14) 0.69254(13) 0.15934(9) 0.0145(3) Uani 1 1 d D . . C412 C 0.85609(15) 0.61487(13) 0.15072(10) 0.0178(4) Uani 1 1 d D . . H412 H 0.7901 0.6005 0.1693 0.021 Uiso 1 1 calc R . . C413 C 0.91275(16) 0.55789(14) 0.11589(11) 0.0198(4) Uani 1 1 d D . . C414 C 0.86605(18) 0.47662(16) 0.10971(14) 0.0312(5) Uani 1 1 d D . . F11 F 0.91306(14) 0.44032(11) 0.06157(9) 0.0457(4) Uani 1 1 d D . . F12 F 0.76864(14) 0.49393(13) 0.09714(14) 0.0712(7) Uani 1 1 d D . . F13 F 0.86905(14) 0.41033(11) 0.16815(9) 0.0470(4) Uani 1 1 d D . . C415 C 1.01062(16) 0.57449(14) 0.08950(11) 0.0217(4) Uani 1 1 d D . . H415 H 1.0499 0.5350 0.0665 0.026 Uiso 1 1 calc R . . C416 C 1.04932(14) 0.65066(14) 0.09784(10) 0.0187(4) Uani 1 1 d D . . C417 C 1.15545(16) 0.66967(16) 0.07092(12) 0.0245(4) Uani 1 1 d D . . F14 F 1.21540(11) 0.59431(10) 0.07049(9) 0.0407(4) Uani 1 1 d D . . F15 F 1.15995(11) 0.72031(11) 0.00612(7) 0.0362(3) Uani 1 1 d D . . F16 F 1.19997(10) 0.71305(12) 0.10759(8) 0.0389(4) Uani 1 1 d D . . C418 C 0.99136(14) 0.70910(13) 0.13130(10) 0.0166(4) Uani 1 1 d D . . H418 H 1.0194 0.7614 0.1352 0.020 Uiso 1 1 calc R . . C421 C 0.88771(14) 0.70822(13) 0.28121(10) 0.0147(3) Uani 1 1 d D A . C422 C 0.87231(15) 0.61956(13) 0.31791(10) 0.0170(4) Uani 1 1 d D . . H422 H 0.8210 0.5901 0.3048 0.020 Uiso 1 1 calc R . . C423 C 0.92940(16) 0.57355(13) 0.37261(10) 0.0185(4) Uani 1 1 d D . . C424 C 0.91009(18) 0.47919(15) 0.40961(12) 0.0264(5) Uani 1 1 d D . . F21 F 0.87416(16) 0.43452(10) 0.36969(9) 0.0537(5) Uani 1 1 d D . . F22 F 0.84275(13) 0.47599(11) 0.46300(9) 0.0491(5) Uani 1 1 d D . . F23 F 0.99338(11) 0.42993(9) 0.43532(8) 0.0329(3) Uani 1 1 d D . . C425 C 1.00309(16) 0.61467(14) 0.39498(10) 0.0195(4) Uani 1 1 d D . . H425 H 1.0417 0.5834 0.4327 0.023 Uiso 1 1 calc R . . C426 C 1.01848(15) 0.70279(14) 0.36048(10) 0.0178(4) Uani 1 1 d D A . C427 C 1.09735(17) 0.74903(15) 0.38310(11) 0.0236(4) Uani 1 1 d D . . F24A F 1.11889(17) 0.71379(13) 0.44754(9) 0.0596(7) Uani 0.974(3) 1 d PD A 1 F25A F 1.18423(12) 0.74732(14) 0.34506(11) 0.0524(6) Uani 0.974(3) 1 d PD A 1 F26A F 1.07044(13) 0.83586(10) 0.37712(10) 0.0427(5) Uani 0.974(3) 1 d PD A 1 F25B F 1.061(3) 0.783(2) 0.4326(19) 0.0524(6) Uani 0.026(3) 1 d PD A 2 F26B F 1.177(3) 0.699(3) 0.3997(15) 0.0427(5) Uani 0.026(3) 1 d PD A 2 C428 C 0.96311(15) 0.74804(13) 0.30403(10) 0.0163(4) Uani 1 1 d . . . H428 H 0.9771 0.8076 0.2805 0.020 Uiso 1 1 calc R A . C431 C 0.71037(14) 0.73450(13) 0.21658(10) 0.0155(4) Uani 1 1 d D B . C432 C 0.65970(15) 0.73774(14) 0.15789(11) 0.0189(4) Uani 1 1 d D . . H432 H 0.6950 0.7546 0.1144 0.023 Uiso 1 1 calc R . . C433 C 0.55958(15) 0.71709(14) 0.16109(12) 0.0218(4) Uani 1 1 d D B . C434 C 0.51445(17) 0.71453(18) 0.09639(13) 0.0317(5) Uani 1 1 d D . . F31A F 0.41817(15) 0.7012(3) 0.10408(12) 0.0966(12) Uani 0.913(2) 1 d PD B 1 F32A F 0.56133(19) 0.64703(12) 0.07028(11) 0.0562(6) Uani 0.913(2) 1 d PD B 1 F33A F 0.52904(16) 0.78625(11) 0.04492(9) 0.0417(5) Uani 0.913(2) 1 d PD B 1 F31B F 0.5726(12) 0.7215(8) 0.0381(10) 0.0966(12) Uani 0.087(2) 1 d PD B 2 F32B F 0.4436(12) 0.7796(9) 0.0849(9) 0.0562(6) Uani 0.087(2) 1 d PD B 2 F33B F 0.4842(10) 0.6474(9) 0.0964(8) 0.0417(5) Uani 0.087(2) 1 d PD B 2 C435 C 0.50451(16) 0.69441(14) 0.22364(12) 0.0233(4) Uani 1 1 d D . . H435 H 0.4366 0.6793 0.2263 0.028 Uiso 1 1 calc R B . C436 C 0.55148(16) 0.69443(14) 0.28183(11) 0.0219(4) Uani 1 1 d D B . C437 C 0.49340(18) 0.67322(17) 0.34998(13) 0.0314(5) Uani 1 1 d D . . F34 F 0.41495(15) 0.62585(15) 0.35099(10) 0.0651(6) Uani 1 1 d D B . F35 F 0.45441(14) 0.74785(12) 0.36781(9) 0.0518(5) Uani 1 1 d D B . F36 F 0.54971(14) 0.62793(14) 0.40082(9) 0.0587(5) Uani 1 1 d D B . C438 C 0.65226(15) 0.71396(13) 0.27847(11) 0.0185(4) Uani 1 1 d D . . H438 H 0.6822 0.7133 0.3195 0.022 Uiso 1 1 calc R B . C441 C 0.83916(14) 0.85976(13) 0.17924(10) 0.0143(3) Uani 1 1 d D C . C442 C 0.84669(15) 0.89992(13) 0.10859(10) 0.0169(4) Uani 1 1 d D . . H442 H 0.8536 0.8624 0.0778 0.020 Uiso 1 1 calc R . . C443 C 0.84442(16) 0.99259(14) 0.08215(10) 0.0198(4) Uani 1 1 d D . . C444 C 0.84570(19) 1.03345(16) 0.00631(12) 0.0283(5) Uani 1 1 d D . . F41 F 0.85364(17) 0.97193(11) -0.02971(7) 0.0518(5) Uani 1 1 d D . . F42 F 0.76132(12) 1.08757(11) -0.01143(8) 0.0411(4) Uani 1 1 d D . . F43 F 0.92265(12) 1.08500(10) -0.01656(8) 0.0394(4) Uani 1 1 d D . . C445 C 0.83585(16) 1.05000(14) 0.12515(11) 0.0218(4) Uani 1 1 d D . . H445 H 0.8354 1.1133 0.1071 0.026 Uiso 1 1 calc R . . C446 C 0.82804(15) 1.01236(14) 0.19517(11) 0.0191(4) Uani 1 1 d D C . C447 C 0.81528(17) 1.07278(15) 0.24289(12) 0.0258(5) Uani 1 1 d D . . F44A F 0.8175(5) 1.0290(2) 0.30874(16) 0.0737(12) Uani 0.604(4) 1 d PD C 1 F45A F 0.8842(3) 1.1285(3) 0.2340(2) 0.0489(8) Uani 0.604(4) 1 d PD C 1 F46A F 0.7282(3) 1.1232(4) 0.2373(3) 0.0721(13) Uani 0.604(4) 1 d PD C 1 F44B F 0.8318(7) 1.1584(3) 0.2100(3) 0.0737(12) Uani 0.396(4) 1 d PD C 2 F45B F 0.7249(4) 1.0755(4) 0.2721(3) 0.0489(8) Uani 0.396(4) 1 d PD C 2 F46B F 0.8773(4) 1.0478(5) 0.2910(4) 0.0721(13) Uani 0.396(4) 1 d PD C 2 C448 C 0.82831(14) 0.91967(13) 0.22125(10) 0.0167(4) Uani 1 1 d . . . H448 H 0.8209 0.8960 0.2694 0.020 Uiso 1 1 calc R C . 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 0.01056(11) 0.01499(12) 0.01318(12) -0.00439(9) -0.00112(8) -0.00072(8) C1 0.0169(9) 0.0212(10) 0.0204(10) -0.0050(8) -0.0026(7) -0.0029(7) O1 0.0219(8) 0.0403(10) 0.0319(9) -0.0054(8) -0.0094(7) 0.0074(7) Si1 0.0117(2) 0.0166(3) 0.0149(2) -0.0040(2) -0.00088(19) 0.00004(18) P1 0.0132(2) 0.0182(2) 0.0174(2) -0.00794(19) -0.00051(18) -0.00188(17) C11 0.0181(9) 0.0188(10) 0.0234(10) -0.0078(8) 0.0004(8) -0.0011(7) C12 0.0264(11) 0.0220(11) 0.0378(13) -0.0143(10) -0.0035(10) -0.0023(8) C13 0.0350(13) 0.0178(10) 0.0395(14) -0.0102(10) 0.0008(10) -0.0018(9) C14 0.0287(11) 0.0200(10) 0.0288(12) -0.0039(9) 0.0005(9) 0.0050(8) C15 0.0221(10) 0.0225(10) 0.0217(10) -0.0037(8) -0.0021(8) 0.0027(8) C16 0.0166(9) 0.0181(9) 0.0175(9) -0.0047(7) 0.0025(7) 0.0001(7) C111 0.0236(10) 0.0242(10) 0.0200(10) -0.0118(8) 0.0032(8) -0.0069(8) C112 0.0352(13) 0.0338(13) 0.0329(13) -0.0137(11) 0.0125(11) -0.0029(10) C113 0.0591(19) 0.0487(17) 0.0409(17) -0.0196(14) 0.0295(15) -0.0085(15) C114 0.080(2) 0.0494(17) 0.0210(13) -0.0165(12) 0.0136(14) -0.0245(16) C115 0.0618(19) 0.0454(16) 0.0201(12) -0.0080(11) -0.0093(12) -0.0209(14) C116 0.0324(12) 0.0365(13) 0.0223(11) -0.0093(10) -0.0036(9) -0.0113(10) C121 0.0150(9) 0.0214(10) 0.0232(10) -0.0073(8) -0.0029(7) -0.0045(7) C122 0.0232(10) 0.0309(12) 0.0296(12) -0.0157(10) -0.0022(9) -0.0055(9) C123 0.0302(12) 0.0402(14) 0.0417(15) -0.0202(12) -0.0055(11) -0.0147(11) C124 0.0230(11) 0.0455(15) 0.0428(15) -0.0157(12) -0.0007(10) -0.0158(10) C125 0.0198(10) 0.0407(14) 0.0321(13) -0.0123(11) 0.0040(9) -0.0094(9) C126 0.0182(9) 0.0279(11) 0.0240(10) -0.0090(9) -0.0014(8) -0.0049(8) P2 0.0131(2) 0.0163(2) 0.0124(2) -0.00314(18) -0.00132(17) -0.00208(17) C21 0.0163(9) 0.0157(9) 0.0158(9) -0.0027(7) -0.0035(7) 0.0000(7) C22 0.0254(10) 0.0235(10) 0.0157(9) -0.0037(8) -0.0030(8) 0.0043(8) C23 0.0342(12) 0.0276(11) 0.0193(10) -0.0065(9) -0.0121(9) 0.0077(9) C24 0.0246(11) 0.0324(12) 0.0293(12) -0.0105(10) -0.0140(9) 0.0082(9) C25 0.0171(9) 0.0259(11) 0.0246(11) -0.0070(9) -0.0061(8) 0.0036(8) C26 0.0167(9) 0.0158(9) 0.0179(9) -0.0041(7) -0.0027(7) -0.0005(7) C211 0.0192(9) 0.0193(9) 0.0148(9) -0.0033(7) -0.0001(7) -0.0050(7) C212 0.0261(11) 0.0218(11) 0.0281(12) -0.0039(9) 0.0039(9) -0.0046(8) C213 0.0356(13) 0.0206(11) 0.0392(14) -0.0043(10) 0.0014(11) -0.0070(9) C214 0.0321(12) 0.0293(12) 0.0309(13) 0.0007(10) 0.0005(10) -0.0146(10) C215 0.0235(11) 0.0358(13) 0.0330(13) -0.0061(10) 0.0081(10) -0.0112(10) C216 0.0225(10) 0.0254(11) 0.0240(11) -0.0065(9) 0.0051(8) -0.0064(8) C221 0.0153(8) 0.0171(9) 0.0152(9) -0.0052(7) 0.0008(7) -0.0011(7) C222 0.0198(9) 0.0194(10) 0.0173(9) -0.0047(8) -0.0028(7) -0.0017(7) C223 0.0283(11) 0.0220(10) 0.0213(10) -0.0096(8) -0.0022(8) -0.0038(8) C224 0.0265(11) 0.0209(10) 0.0276(11) -0.0106(9) 0.0030(9) 0.0016(8) C225 0.0183(10) 0.0257(11) 0.0313(12) -0.0088(9) -0.0017(8) 0.0032(8) C226 0.0165(9) 0.0241(10) 0.0225(10) -0.0100(8) -0.0024(8) 0.0004(7) P3 0.0124(2) 0.0159(2) 0.0132(2) -0.00410(18) -0.00006(17) -0.00096(17) C31 0.0127(8) 0.0237(10) 0.0135(9) -0.0060(7) 0.0007(7) -0.0028(7) C32 0.0189(9) 0.0277(11) 0.0189(10) -0.0010(8) 0.0008(8) -0.0058(8) C33 0.0166(10) 0.0407(13) 0.0211(10) -0.0034(9) 0.0050(8) -0.0062(9) C34 0.0154(9) 0.0396(13) 0.0278(12) -0.0084(10) 0.0048(8) 0.0007(9) C35 0.0161(9) 0.0266(11) 0.0249(11) -0.0069(9) 0.0016(8) 0.0008(8) C36 0.0141(8) 0.0220(10) 0.0147(9) -0.0061(7) 0.0007(7) -0.0024(7) C311 0.0201(9) 0.0175(9) 0.0122(8) -0.0029(7) -0.0008(7) -0.0056(7) C312 0.0228(10) 0.0242(10) 0.0176(10) -0.0044(8) -0.0042(8) -0.0048(8) C313 0.0340(12) 0.0310(12) 0.0190(10) -0.0057(9) -0.0058(9) -0.0116(10) C314 0.0477(14) 0.0230(11) 0.0167(10) -0.0064(8) 0.0005(9) -0.0119(10) C315 0.0392(13) 0.0184(10) 0.0219(11) -0.0065(8) 0.0039(9) -0.0029(9) C316 0.0232(10) 0.0191(10) 0.0188(10) -0.0030(8) 0.0002(8) -0.0026(8) C321 0.0141(8) 0.0221(10) 0.0139(9) -0.0019(7) -0.0019(7) -0.0040(7) C322 0.0203(9) 0.0229(10) 0.0171(9) -0.0032(8) -0.0022(7) -0.0025(8) C323 0.0241(10) 0.0225(10) 0.0214(10) 0.0016(8) -0.0036(8) 0.0002(8) C324 0.0186(10) 0.0331(12) 0.0171(10) 0.0027(9) -0.0044(8) -0.0008(8) C325 0.0294(11) 0.0345(12) 0.0169(10) -0.0049(9) -0.0073(8) -0.0049(9) C326 0.0293(11) 0.0240(11) 0.0188(10) -0.0045(8) -0.0045(8) -0.0047(9) B1 0.0135(9) 0.0147(10) 0.0138(9) -0.0039(8) -0.0011(7) -0.0005(7) C411 0.0145(8) 0.0161(9) 0.0116(8) -0.0017(7) -0.0034(6) 0.0021(7) C412 0.0178(9) 0.0182(9) 0.0172(9) -0.0043(7) -0.0029(7) 0.0000(7) C413 0.0220(10) 0.0172(9) 0.0210(10) -0.0063(8) -0.0040(8) 0.0014(7) C414 0.0276(11) 0.0258(12) 0.0458(15) -0.0199(11) -0.0027(10) 0.0009(9) F11 0.0660(11) 0.0335(8) 0.0469(10) -0.0281(8) 0.0091(8) -0.0108(8) F12 0.0374(9) 0.0512(11) 0.149(2) -0.0631(13) -0.0363(12) 0.0068(8) F13 0.0592(11) 0.0300(8) 0.0531(11) -0.0140(7) 0.0190(9) -0.0189(7) C415 0.0227(10) 0.0217(10) 0.0210(10) -0.0088(8) -0.0026(8) 0.0058(8) C416 0.0140(9) 0.0240(10) 0.0167(9) -0.0041(8) -0.0025(7) 0.0027(7) C417 0.0169(9) 0.0313(12) 0.0258(11) -0.0103(9) -0.0001(8) 0.0028(8) F14 0.0207(7) 0.0366(8) 0.0614(11) -0.0141(8) 0.0080(7) 0.0087(6) F15 0.0249(7) 0.0502(9) 0.0284(8) -0.0015(7) 0.0040(6) -0.0064(6) F16 0.0170(6) 0.0655(11) 0.0444(9) -0.0313(8) 0.0015(6) -0.0078(6) C418 0.0157(9) 0.0185(9) 0.0152(9) -0.0032(7) -0.0033(7) -0.0003(7) C421 0.0142(8) 0.0168(9) 0.0122(8) -0.0026(7) -0.0004(7) -0.0001(7) C422 0.0184(9) 0.0180(9) 0.0153(9) -0.0045(7) -0.0030(7) -0.0016(7) C423 0.0223(9) 0.0169(9) 0.0156(9) -0.0022(7) -0.0029(7) -0.0022(7) C424 0.0307(11) 0.0224(11) 0.0247(11) -0.0008(9) -0.0105(9) -0.0032(9) F21 0.0888(14) 0.0218(7) 0.0545(11) 0.0007(7) -0.0465(10) -0.0155(8) F22 0.0434(9) 0.0357(9) 0.0514(11) 0.0138(8) 0.0154(8) -0.0061(7) F23 0.0379(8) 0.0209(7) 0.0357(8) 0.0031(6) -0.0135(6) 0.0003(6) C425 0.0219(10) 0.0211(10) 0.0146(9) -0.0022(8) -0.0041(7) -0.0013(8) C426 0.0176(9) 0.0202(10) 0.0164(9) -0.0044(7) -0.0036(7) -0.0032(7) C427 0.0271(11) 0.0221(10) 0.0209(10) -0.0003(8) -0.0075(8) -0.0070(8) F24A 0.0909(15) 0.0554(12) 0.0320(9) 0.0182(8) -0.0395(10) -0.0493(11) F25A 0.0271(8) 0.0715(13) 0.0749(14) -0.0443(11) 0.0102(8) -0.0234(8) F26A 0.0451(9) 0.0228(8) 0.0677(12) -0.0165(8) -0.0299(9) -0.0019(6) F25B 0.0271(8) 0.0715(13) 0.0749(14) -0.0443(11) 0.0102(8) -0.0234(8) F26B 0.0451(9) 0.0228(8) 0.0677(12) -0.0165(8) -0.0299(9) -0.0019(6) C428 0.0168(9) 0.0169(9) 0.0145(9) -0.0024(7) -0.0012(7) -0.0017(7) C431 0.0141(8) 0.0126(8) 0.0196(9) -0.0044(7) -0.0006(7) 0.0004(6) C432 0.0148(9) 0.0195(10) 0.0216(10) -0.0041(8) -0.0025(7) 0.0001(7) C433 0.0161(9) 0.0221(10) 0.0277(11) -0.0063(8) -0.0058(8) -0.0002(7) C434 0.0197(10) 0.0418(14) 0.0357(13) -0.0094(11) -0.0093(9) -0.0073(10) F31A 0.0212(10) 0.226(4) 0.0495(13) -0.0342(18) -0.0062(9) -0.0395(15) F32A 0.0884(17) 0.0344(10) 0.0569(13) -0.0250(9) -0.0389(12) 0.0068(10) F33A 0.0723(13) 0.0277(8) 0.0280(9) -0.0046(7) -0.0223(8) -0.0086(8) F31B 0.0212(10) 0.226(4) 0.0495(13) -0.0342(18) -0.0062(9) -0.0395(15) F32B 0.0884(17) 0.0344(10) 0.0569(13) -0.0250(9) -0.0389(12) 0.0068(10) F33B 0.0723(13) 0.0277(8) 0.0280(9) -0.0046(7) -0.0223(8) -0.0086(8) C435 0.0145(9) 0.0212(10) 0.0355(12) -0.0101(9) 0.0013(8) -0.0027(7) C436 0.0182(9) 0.0204(10) 0.0275(11) -0.0089(8) 0.0068(8) -0.0030(8) C437 0.0244(11) 0.0369(13) 0.0361(13) -0.0157(11) 0.0101(10) -0.0103(10) F34 0.0581(12) 0.0982(16) 0.0554(12) -0.0401(11) 0.0329(9) -0.0568(11) F35 0.0543(11) 0.0542(11) 0.0510(11) -0.0297(9) 0.0206(9) -0.0012(8) F36 0.0438(10) 0.0822(14) 0.0334(9) 0.0074(9) 0.0158(8) -0.0016(9) C438 0.0179(9) 0.0177(9) 0.0215(10) -0.0085(8) 0.0013(7) -0.0023(7) C441 0.0116(8) 0.0168(9) 0.0147(9) -0.0040(7) -0.0024(6) -0.0003(6) C442 0.0164(9) 0.0191(9) 0.0156(9) -0.0049(7) -0.0030(7) -0.0009(7) C443 0.0217(10) 0.0188(10) 0.0170(9) -0.0003(8) -0.0014(8) -0.0031(7) C444 0.0363(13) 0.0239(11) 0.0208(11) 0.0013(9) -0.0014(9) -0.0026(9) F41 0.1051(16) 0.0320(8) 0.0157(7) -0.0014(6) -0.0049(8) -0.0051(9) F42 0.0387(8) 0.0445(9) 0.0300(8) 0.0099(7) -0.0118(7) 0.0007(7) F43 0.0388(8) 0.0370(8) 0.0315(8) 0.0096(6) 0.0070(7) -0.0076(7) C445 0.0208(10) 0.0169(10) 0.0266(11) -0.0030(8) -0.0028(8) -0.0027(7) C446 0.0168(9) 0.0193(10) 0.0238(10) -0.0104(8) -0.0012(8) -0.0009(7) C447 0.0254(11) 0.0238(11) 0.0310(12) -0.0122(9) -0.0018(9) -0.0020(8) F44A 0.167(4) 0.0291(13) 0.0288(14) -0.0146(11) 0.003(2) -0.017(2) F45A 0.0506(16) 0.0573(17) 0.0557(18) -0.0396(14) 0.0169(13) -0.0325(14) F46A 0.0354(14) 0.096(3) 0.119(3) -0.093(3) -0.0360(17) 0.0313(16) F44B 0.167(4) 0.0291(13) 0.0288(14) -0.0146(11) 0.003(2) -0.017(2) F45B 0.0506(16) 0.0573(17) 0.0557(18) -0.0396(14) 0.0169(13) -0.0325(14) F46B 0.0354(14) 0.096(3) 0.119(3) -0.093(3) -0.0360(17) 0.0313(16) C448 0.0150(8) 0.0201(9) 0.0155(9) -0.0059(7) -0.0020(7) -0.0002(7) _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 C1 1.796(2) . ? Ni1 P1 2.2271(6) . ? Ni1 P2 2.2385(5) . ? Ni1 Si1 2.2631(6) . ? Ni1 P3 2.2661(6) . ? C1 O1 1.137(3) . ? Si1 C36 1.866(2) . ? Si1 C26 1.871(2) . ? Si1 C16 1.877(2) . ? P1 C11 1.824(2) . ? P1 C111 1.825(2) . ? P1 C121 1.826(2) . ? C11 C12 1.397(3) . ? C11 C16 1.401(3) . ? C12 C13 1.387(3) . ? C13 C14 1.394(4) . ? C14 C15 1.385(3) . ? C15 C16 1.404(3) . ? C111 C116 1.394(3) . ? C111 C112 1.395(3) . ? C112 C113 1.391(4) . ? C113 C114 1.385(5) . ? C114 C115 1.378(5) . ? C115 C116 1.387(3) . ? C121 C126 1.397(3) . ? C121 C122 1.400(3) . ? C122 C123 1.390(3) . ? C123 C124 1.387(4) . ? C124 C125 1.384(4) . ? C125 C126 1.391(3) . ? P2 C311 1.818(2) . ? P2 C31 1.8180(19) . ? P2 C321 1.830(2) . ? C21 C22 1.399(3) . ? C21 C26 1.405(3) . ? C21 P3 1.818(2) . ? C22 C23 1.387(3) . ? C23 C24 1.389(3) . ? C24 C25 1.385(3) . ? C25 C26 1.404(3) . ? C211 C216 1.390(3) . ? C211 C212 1.395(3) . ? C211 P3 1.830(2) . ? C212 C213 1.387(3) . ? C213 C214 1.388(4) . ? C214 C215 1.381(4) . ? C215 C216 1.393(3) . ? C221 C222 1.402(3) . ? C221 C226 1.403(3) . ? C221 P3 1.820(2) . ? C222 C223 1.390(3) . ? C223 C224 1.383(3) . ? C224 C225 1.389(3) . ? C225 C226 1.385(3) . ? C31 C36 1.397(3) . ? C31 C32 1.402(3) . ? C32 C33 1.388(3) . ? C33 C34 1.384(3) . ? C34 C35 1.389(3) . ? C35 C36 1.402(3) . ? C311 C312 1.395(3) . ? C311 C316 1.401(3) . ? C312 C313 1.396(3) . ? C313 C314 1.381(4) . ? C314 C315 1.383(4) . ? C315 C316 1.392(3) . ? C321 C322 1.390(3) . ? C321 C326 1.400(3) . ? C322 C323 1.394(3) . ? C323 C324 1.385(3) . ? C324 C325 1.387(3) . ? C325 C326 1.387(3) . ? B1 C441 1.637(3) . ? B1 C431 1.642(3) . ? B1 C421 1.644(3) . ? B1 C411 1.647(3) . ? C411 C412 1.399(3) . ? C411 C418 1.406(3) . ? C412 C413 1.391(3) . ? C413 C415 1.387(3) . ? C413 C414 1.497(3) . ? C414 F12 1.326(3) . ? C414 F11 1.329(3) . ? C414 F13 1.350(3) . ? C415 C416 1.389(3) . ? C416 C418 1.397(3) . ? C416 C417 1.499(3) . ? C417 F16 1.332(3) . ? C417 F14 1.340(2) . ? C417 F15 1.343(3) . ? C421 C428 1.399(3) . ? C421 C422 1.405(3) . ? C422 C423 1.389(3) . ? C423 C425 1.389(3) . ? C423 C424 1.494(3) . ? C424 F23 1.337(3) . ? C424 F21 1.338(3) . ? C424 F22 1.339(3) . ? C425 C426 1.387(3) . ? C426 C428 1.399(3) . ? C426 C427 1.495(3) . ? C427 F26B 1.26(4) . ? C427 F25B 1.29(4) . ? C427 F24A 1.321(3) . ? C427 F26A 1.328(3) . ? C427 F25A 1.335(3) . ? C431 C438 1.397(3) . ? C431 C432 1.404(3) . ? C432 C433 1.394(3) . ? C433 C435 1.390(3) . ? C433 C434 1.500(3) . ? C434 F33B 1.152(15) . ? C434 F32B 1.290(16) . ? C434 F31A 1.307(3) . ? C434 F33A 1.328(3) . ? C434 F31B 1.342(17) . ? C434 F32A 1.360(3) . ? C435 C436 1.382(3) . ? C436 C438 1.396(3) . ? C436 C437 1.500(3) . ? C437 F36 1.325(3) . ? C437 F34 1.333(3) . ? C437 F35 1.337(3) . ? C441 C448 1.403(3) . ? C441 C442 1.405(3) . ? C442 C443 1.390(3) . ? C443 C445 1.388(3) . ? C443 C444 1.502(3) . ? C444 F41 1.334(3) . ? C444 F43 1.340(3) . ? C444 F42 1.341(3) . ? C445 C446 1.387(3) . ? C446 C448 1.391(3) . ? C446 C447 1.500(3) . ? C447 F46B 1.286(6) . ? C447 F45A 1.294(3) . ? C447 F45B 1.294(5) . ? C447 F46A 1.320(4) . ? C447 F44A 1.332(4) . ? C447 F44B 1.350(5) . ? 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 Ni1 P1 96.32(7) . . ? C1 Ni1 P2 93.33(7) . . ? P1 Ni1 P2 124.87(2) . . ? C1 Ni1 Si1 172.56(7) . . ? P1 Ni1 Si1 83.23(2) . . ? P2 Ni1 Si1 80.95(2) . . ? C1 Ni1 P3 103.13(7) . . ? P1 Ni1 P3 116.53(2) . . ? P2 Ni1 P3 113.63(2) . . ? Si1 Ni1 P3 83.62(2) . . ? O1 C1 Ni1 175.9(2) . . ? C36 Si1 C26 109.64(9) . . ? C36 Si1 C16 110.18(9) . . ? C26 Si1 C16 111.07(9) . . ? C36 Si1 Ni1 109.34(7) . . ? C26 Si1 Ni1 107.72(6) . . ? C16 Si1 Ni1 108.84(7) . . ? C11 P1 C111 103.64(10) . . ? C11 P1 C121 106.11(10) . . ? C111 P1 C121 103.79(10) . . ? C11 P1 Ni1 111.99(7) . . ? C111 P1 Ni1 113.62(7) . . ? C121 P1 Ni1 116.51(7) . . ? C12 C11 C16 121.0(2) . . ? C12 C11 P1 124.35(17) . . ? C16 C11 P1 114.59(15) . . ? C13 C12 C11 119.5(2) . . ? C12 C13 C14 120.2(2) . . ? C15 C14 C13 120.2(2) . . ? C14 C15 C16 120.6(2) . . ? C11 C16 C15 118.44(19) . . ? C11 C16 Si1 115.97(15) . . ? C15 C16 Si1 125.54(16) . . ? C116 C111 C112 119.6(2) . . ? C116 C111 P1 119.93(17) . . ? C112 C111 P1 120.06(19) . . ? C113 C112 C111 119.4(3) . . ? C114 C113 C112 120.6(3) . . ? C115 C114 C113 120.0(3) . . ? C114 C115 C116 120.2(3) . . ? C115 C116 C111 120.2(2) . . ? C126 C121 C122 118.95(19) . . ? C126 C121 P1 118.95(16) . . ? C122 C121 P1 122.04(16) . . ? C123 C122 C121 119.9(2) . . ? C124 C123 C122 120.5(2) . . ? C125 C124 C123 120.2(2) . . ? C124 C125 C126 119.7(2) . . ? C125 C126 C121 120.8(2) . . ? C311 P2 C31 105.85(9) . . ? C311 P2 C321 105.95(9) . . ? C31 P2 C321 103.16(9) . . ? C311 P2 Ni1 112.76(6) . . ? C31 P2 Ni1 112.18(7) . . ? C321 P2 Ni1 116.00(7) . . ? C22 C21 C26 120.65(18) . . ? C22 C21 P3 124.11(16) . . ? C26 C21 P3 115.23(15) . . ? C23 C22 C21 119.5(2) . . ? C22 C23 C24 120.1(2) . . ? C25 C24 C23 120.7(2) . . ? C24 C25 C26 120.2(2) . . ? C25 C26 C21 118.53(19) . . ? C25 C26 Si1 125.17(16) . . ? C21 C26 Si1 116.09(14) . . ? C216 C211 C212 119.29(19) . . ? C216 C211 P3 124.16(16) . . ? C212 C211 P3 116.53(15) . . ? C213 C212 C211 120.5(2) . . ? C212 C213 C214 120.0(2) . . ? C215 C214 C213 119.6(2) . . ? C214 C215 C216 120.7(2) . . ? C211 C216 C215 119.8(2) . . ? C222 C221 C226 118.57(18) . . ? C222 C221 P3 123.99(15) . . ? C226 C221 P3 117.44(15) . . ? C223 C222 C221 120.13(19) . . ? C224 C223 C222 120.6(2) . . ? C223 C224 C225 119.8(2) . . ? C226 C225 C224 120.2(2) . . ? C225 C226 C221 120.7(2) . . ? C21 P3 C221 106.78(9) . . ? C21 P3 C211 102.18(9) . . ? C221 P3 C211 103.98(9) . . ? C21 P3 Ni1 111.04(7) . . ? C221 P3 Ni1 113.45(7) . . ? C211 P3 Ni1 118.24(7) . . ? C36 C31 C32 120.97(18) . . ? C36 C31 P2 114.54(14) . . ? C32 C31 P2 124.49(16) . . ? C33 C32 C31 118.8(2) . . ? C34 C33 C32 120.9(2) . . ? C33 C34 C35 120.3(2) . . ? C34 C35 C36 120.0(2) . . ? C31 C36 C35 119.01(18) . . ? C31 C36 Si1 114.26(14) . . ? C35 C36 Si1 126.68(16) . . ? C312 C311 C316 119.32(19) . . ? C312 C311 P2 121.07(16) . . ? C316 C311 P2 119.51(15) . . ? C311 C312 C313 120.0(2) . . ? C314 C313 C312 120.2(2) . . ? C313 C314 C315 120.2(2) . . ? C314 C315 C316 120.3(2) . . ? C315 C316 C311 119.9(2) . . ? C322 C321 C326 118.97(19) . . ? C322 C321 P2 124.20(16) . . ? C326 C321 P2 116.76(16) . . ? C321 C322 C323 120.2(2) . . ? C324 C323 C322 120.5(2) . . ? C323 C324 C325 119.7(2) . . ? C326 C325 C324 120.2(2) . . ? C325 C326 C321 120.5(2) . . ? C441 B1 C431 107.27(15) . . ? C441 B1 C421 113.79(15) . . ? C431 B1 C421 112.69(15) . . ? C441 B1 C411 112.44(15) . . ? C431 B1 C411 109.50(15) . . ? C421 B1 C411 101.11(14) . . ? C412 C411 C418 115.82(17) . . ? C412 C411 B1 121.56(17) . . ? C418 C411 B1 121.95(17) . . ? C413 C412 C411 122.44(19) . . ? C415 C413 C412 120.96(19) . . ? C415 C413 C414 121.10(19) . . ? C412 C413 C414 117.92(19) . . ? F12 C414 F11 108.2(2) . . ? F12 C414 F13 105.1(2) . . ? F11 C414 F13 105.58(19) . . ? F12 C414 C413 112.45(19) . . ? F11 C414 C413 113.0(2) . . ? F13 C414 C413 112.0(2) . . ? C413 C415 C416 117.87(18) . . ? C415 C416 C418 121.11(18) . . ? C415 C416 C417 119.17(18) . . ? C418 C416 C417 119.72(19) . . ? F16 C417 F14 106.62(18) . . ? F16 C417 F15 106.39(19) . . ? F14 C417 F15 105.61(18) . . ? F16 C417 C416 112.64(18) . . ? F14 C417 C416 112.29(19) . . ? F15 C417 C416 112.77(18) . . ? C416 C418 C411 121.77(18) . . ? C428 C421 C422 115.78(17) . . ? C428 C421 B1 124.46(17) . . ? C422 C421 B1 119.03(17) . . ? C423 C422 C421 122.30(18) . . ? C422 C423 C425 121.01(19) . . ? C422 C423 C424 120.04(19) . . ? C425 C423 C424 118.94(18) . . ? F23 C424 F21 106.20(19) . . ? F23 C424 F22 105.57(18) . . ? F21 C424 F22 106.7(2) . . ? F23 C424 C423 112.90(19) . . ? F21 C424 C423 112.83(19) . . ? F22 C424 C423 112.11(19) . . ? C426 C425 C423 117.86(19) . . ? C425 C426 C428 121.01(18) . . ? C425 C426 C427 119.27(18) . . ? C428 C426 C427 119.70(18) . . ? F26B C427 F25B 110(2) . . ? F26B C427 F24A 57.4(12) . . ? F25B C427 F24A 56.4(12) . . ? F26B C427 F26A 134(2) . . ? F25B C427 F26A 55.0(12) . . ? F24A C427 F26A 106.5(2) . . ? F26B C427 F25A 53.4(12) . . ? F25B C427 F25A 137(2) . . ? F24A C427 F25A 107.2(2) . . ? F26A C427 F25A 104.56(19) . . ? F26B C427 C426 114(2) . . ? F25B C427 C426 111(2) . . ? F24A C427 C426 113.21(18) . . ? F26A C427 C426 112.70(18) . . ? F25A C427 C426 112.12(19) . . ? C426 C428 C421 121.99(18) . . ? C438 C431 C432 115.69(18) . . ? C438 C431 B1 124.56(18) . . ? C432 C431 B1 119.72(17) . . ? C433 C432 C431 122.45(19) . . ? C435 C433 C432 120.5(2) . . ? C435 C433 C434 120.65(19) . . ? C432 C433 C434 118.8(2) . . ? F33B C434 F32B 111.0(9) . . ? F33B C434 F31A 56.5(6) . . ? F32B C434 F31A 57.3(6) . . ? F33B C434 F33A 129.8(9) . . ? F32B C434 F33A 61.3(6) . . ? F31A C434 F33A 109.4(2) . . ? F33B C434 F31B 95.7(9) . . ? F32B C434 F31B 107.1(9) . . ? F31A C434 F31B 125.5(9) . . ? F33A C434 F31B 50.3(5) . . ? F33B C434 F32A 51.8(6) . . ? F32B C434 F32A 142.1(9) . . ? F31A C434 F32A 105.8(2) . . ? F33A C434 F32A 101.6(2) . . ? F31B C434 F32A 52.0(5) . . ? F33B C434 C433 115.7(9) . . ? F32B C434 C433 106.4(9) . . ? F31A C434 C433 113.8(2) . . ? F33A C434 C433 113.7(2) . . ? F31B C434 C433 120.5(9) . . ? F32A C434 C433 111.5(2) . . ? C436 C435 C433 118.06(19) . . ? C435 C436 C438 121.23(19) . . ? C435 C436 C437 119.6(2) . . ? C438 C436 C437 119.2(2) . . ? F36 C437 F34 107.1(2) . . ? F36 C437 F35 105.3(2) . . ? F34 C437 F35 105.7(2) . . ? F36 C437 C436 113.4(2) . . ? F34 C437 C436 113.0(2) . . ? F35 C437 C436 111.8(2) . . ? C436 C438 C431 122.0(2) . . ? C448 C441 C442 115.39(17) . . ? C448 C441 B1 122.60(17) . . ? C442 C441 B1 121.69(17) . . ? C443 C442 C441 122.31(19) . . ? C445 C443 C442 120.91(19) . . ? C445 C443 C444 118.23(19) . . ? C442 C443 C444 120.79(19) . . ? F41 C444 F43 106.6(2) . . ? F41 C444 F42 107.3(2) . . ? F43 C444 F42 105.51(18) . . ? F41 C444 C443 112.85(18) . . ? F43 C444 C443 112.6(2) . . ? F42 C444 C443 111.55(19) . . ? C446 C445 C443 118.12(19) . . ? C445 C446 C448 120.66(19) . . ? C445 C446 C447 119.39(19) . . ? C448 C446 C447 119.92(19) . . ? F46B C447 F45A 69.3(4) . . ? F46B C447 F45B 106.9(4) . . ? F45A C447 F45B 130.2(3) . . ? F46B C447 F46A 132.3(3) . . ? F45A C447 F46A 105.4(3) . . ? F45B C447 F46A 39.2(3) . . ? F46B C447 F44A 39.7(3) . . ? F45A C447 F44A 104.2(3) . . ? F45B C447 F44A 70.0(4) . . ? F46A C447 F44A 105.3(3) . . ? F46B C447 F44B 106.7(5) . . ? F45A C447 F44B 39.7(3) . . ? F45B C447 F44B 106.5(4) . . ? F46A C447 F44B 70.5(4) . . ? F44A C447 F44B 131.4(3) . . ? F46B C447 C446 112.2(3) . . ? F45A C447 C446 114.5(2) . . ? F45B C447 C446 112.5(3) . . ? F46A C447 C446 112.6(2) . . ? F44A C447 C446 113.9(2) . . ? F44B C447 C446 111.7(3) . . ? C446 C448 C441 122.58(18) . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 30.47 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 1.423 _refine_diff_density_min -0.857 _refine_diff_density_rms 0.091