#------------------------------------------------------------------------------
#$Date: 2016-03-23 00:13:45 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179099 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/61/4306156.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_4306156
loop_
_publ_author_name
'Tzung-Wen Chiou'
'Wen-Feng Liaw'
_publ_section_title
;
Mononuclear Nickel(III) Complexes [NiIII(OR)(P(C6H3-3-SiMe3-2-S)3)]- (R =
Me, Ph) Containing the Terminal Alkoxide Ligand: Relevance to the Nickel
Site of Oxidized-Form [NiFe] Hydrogenases
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              7908
_journal_page_last               7913
_journal_paper_doi               10.1021/ic801069t
_journal_volume                  47
_journal_year                    2008
_chemical_formula_moiety         'C69 H71 N Ni P3 S4 Si3'
_chemical_formula_sum            'C69 H71 N Ni P3 S4 Si3'
_chemical_formula_weight         1278.40
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 99.1520(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.0948(2)
_cell_length_b                   27.4679(4)
_cell_length_c                   17.3155(3)
_cell_measurement_reflns_used    30800
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      25.35
_cell_measurement_theta_min      2.037
_cell_volume                     6618.43(18)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Nonius BV, 1997-2000)'
_computing_data_reduction
'HKL Denzo and Scalepack (Otwinowski & Minor 19'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1986)'
_diffrn_ambient_temperature      200(2)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.976
_diffrn_measured_fraction_theta_max 0.976
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'CCD rotation images, thick slices'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0606
_diffrn_reflns_av_sigmaI/netI    0.0542
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            29608
_diffrn_reflns_theta_full        25.34
_diffrn_reflns_theta_max         25.34
_diffrn_reflns_theta_min         2.08
_exptl_absorpt_coefficient_mu    0.587
_exptl_absorpt_correction_T_max  0.8512
_exptl_absorpt_correction_T_min  0.7536
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 ?
;
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.283
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2684
_exptl_crystal_size_max          0.48
_exptl_crystal_size_mid          0.38
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.527
_refine_diff_density_min         -0.620
_refine_diff_density_rms         0.124
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.067
_refine_ls_hydrogen_treatment    fixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     730
_refine_ls_number_reflns         11808
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.067
_refine_ls_R_factor_all          0.0637
_refine_ls_R_factor_gt           0.0455
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0758P)²+2.7317P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1217
_refine_ls_wR_factor_ref         0.1373
_reflns_number_gt                9315
_reflns_number_total             11808
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic801069t-file003_2.cif
_cod_data_source_block           complex2
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4306156
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'
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 0.15139(3) 0.208884(14) 0.91605(2) 0.02410(11) Uani 1 1 d . . .
S1 S 0.18802(6) 0.13712(3) 0.85916(5) 0.03053(19) Uani 1 1 d . . .
S2 S 0.29028(6) 0.23750(3) 0.98565(5) 0.03021(18) Uani 1 1 d . . .
S3 S 0.01689(6) 0.25165(3) 0.89144(5) 0.03182(19) Uani 1 1 d . . .
S4 S 0.11598(6) 0.17138(3) 1.02315(5) 0.0406(2) Uani 1 1 d . . .
P1 P 0.19291(5) 0.24288(3) 0.81552(4) 0.02268(17) Uani 1 1 d . . .
P2 P 0.38214(5) 0.47360(3) 0.79935(5) 0.02486(18) Uani 1 1 d . . .
P3 P 0.30147(6) 0.56242(3) 0.71397(5) 0.02440(18) Uani 1 1 d . . .
Si1 Si 0.15590(7) 0.04675(3) 0.72018(6) 0.0334(2) Uani 1 1 d . . .
Si2 Si 0.50489(7) 0.28730(4) 1.04989(6) 0.0406(2) Uani 1 1 d . . .
Si3 Si -0.16615(7) 0.32496(4) 0.82115(6) 0.0414(2) Uani 1 1 d . . .
N1 N 0.35277(18) 0.52813(9) 0.78148(15) 0.0277(6) Uani 1 1 d . . .
C1 C 0.1804(2) 0.19989(10) 0.73585(17) 0.0236(6) Uani 1 1 d . . .
C2 C 0.1791(2) 0.15070(11) 0.75892(17) 0.0245(6) Uani 1 1 d . . .
C3 C 0.1672(2) 0.11374(11) 0.70057(18) 0.0289(7) Uani 1 1 d . . .
C4 C 0.0549(3) 0.03299(13) 0.7740(2) 0.0473(9) Uani 1 1 d . . .
H4A H 0.0520 -0.0015 0.7827 0.071 Uiso 1 1 calc R . .
H4B H -0.0044 0.0437 0.7437 0.071 Uiso 1 1 calc R . .
H4C H 0.0650 0.0496 0.8234 0.071 Uiso 1 1 calc R . .
C5 C 0.2714(3) 0.02181(13) 0.7726(3) 0.0578(11) Uani 1 1 d . . .
H5A H 0.3222 0.0292 0.7435 0.087 Uiso 1 1 calc R . .
H5B H 0.2660 -0.0128 0.7776 0.087 Uiso 1 1 calc R . .
H5C H 0.2854 0.0362 0.8236 0.087 Uiso 1 1 calc R . .
C6 C 0.1271(3) 0.01430(14) 0.6240(2) 0.0532(10) Uani 1 1 d . . .
H6A H 0.1773 0.0201 0.5936 0.080 Uiso 1 1 calc R . .
H6B H 0.0673 0.0262 0.5961 0.080 Uiso 1 1 calc R . .
H6C H 0.1219 -0.0200 0.6330 0.080 Uiso 1 1 calc R . .
C7 C 0.1590(2) 0.12910(12) 0.62281(19) 0.0349(8) Uani 1 1 d . . .
H7 H 0.1528 0.1055 0.5839 0.042 Uiso 1 1 calc R . .
C8 C 0.1596(3) 0.17762(12) 0.60045(19) 0.0359(8) Uani 1 1 d . . .
H8 H 0.1531 0.1859 0.5478 0.043 Uiso 1 1 calc R . .
C9 C 0.1702(2) 0.21353(11) 0.65733(19) 0.0304(7) Uani 1 1 d . . .
H9 H 0.1704 0.2462 0.6434 0.036 Uiso 1 1 calc R . .
C10 C 0.3164(2) 0.26349(10) 0.83753(18) 0.0259(6) Uani 1 1 d . . .
C11 C 0.3553(2) 0.26326(10) 0.91730(18) 0.0255(6) Uani 1 1 d . . .
C12 C 0.4493(2) 0.28262(11) 0.9426(2) 0.0315(7) Uani 1 1 d . . .
C13 C 0.5216(3) 0.22710(16) 1.0985(3) 0.0604(11) Uani 1 1 d . . .
H13A H 0.5574 0.2062 1.0693 0.091 Uiso 1 1 calc R . .
H13B H 0.4600 0.2128 1.1010 0.091 Uiso 1 1 calc R . .
H13C H 0.5562 0.2311 1.1506 0.091 Uiso 1 1 calc R . .
C14 C 0.6280(3) 0.3132(2) 1.0551(3) 0.0806(16) Uani 1 1 d . . .
H14A H 0.6240 0.3446 1.0306 0.121 Uiso 1 1 calc R . .
H14B H 0.6662 0.2919 1.0284 0.121 Uiso 1 1 calc R . .
H14C H 0.6573 0.3163 1.1088 0.121 Uiso 1 1 calc R . .
C15 C 0.4341(4) 0.32867(19) 1.1035(3) 0.0822(16) Uani 1 1 d . . .
H15A H 0.4270 0.3596 1.0776 0.123 Uiso 1 1 calc R . .
H15B H 0.4670 0.3330 1.1560 0.123 Uiso 1 1 calc R . .
H15C H 0.3719 0.3148 1.1047 0.123 Uiso 1 1 calc R . .
C16 C 0.4987(2) 0.29930(11) 0.8840(2) 0.0358(8) Uani 1 1 d . . .
H16 H 0.5600 0.3120 0.8988 0.043 Uiso 1 1 calc R . .
C17 C 0.4613(2) 0.29797(12) 0.8049(2) 0.0367(8) Uani 1 1 d . . .
H17 H 0.4976 0.3089 0.7681 0.044 Uiso 1 1 calc R . .
C18 C 0.3692(2) 0.28013(12) 0.7813(2) 0.0353(8) Uani 1 1 d . . .
H18 H 0.3429 0.2793 0.7286 0.042 Uiso 1 1 calc R . .
C19 C 0.1146(2) 0.29357(11) 0.78415(17) 0.0251(6) Uani 1 1 d . . .
C20 C 0.0294(2) 0.29310(10) 0.81543(17) 0.0250(6) Uani 1 1 d . . .
C21 C -0.0449(2) 0.32688(11) 0.78855(18) 0.0304(7) Uani 1 1 d . . .
C22 C -0.2244(3) 0.26443(17) 0.8035(4) 0.0768(16) Uani 1 1 d . . .
H22A H -0.2309 0.2566 0.7488 0.115 Uiso 1 1 calc R . .
H22B H -0.2867 0.2652 0.8190 0.115 Uiso 1 1 calc R . .
H22C H -0.1855 0.2402 0.8334 0.115 Uiso 1 1 calc R . .
C23 C -0.1527(3) 0.34138(19) 0.9265(2) 0.0704(14) Uani 1 1 d . . .
H23A H -0.1229 0.3728 0.9344 0.106 Uiso 1 1 calc R . .
H23B H -0.1133 0.3175 0.9569 0.106 Uiso 1 1 calc R . .
H23C H -0.2148 0.3423 0.9424 0.106 Uiso 1 1 calc R . .
C24 C -0.2458(3) 0.37128(16) 0.7643(3) 0.0596(11) Uani 1 1 d . . .
H24A H -0.2532 0.3636 0.7095 0.089 Uiso 1 1 calc R . .
H24B H -0.2175 0.4030 0.7731 0.089 Uiso 1 1 calc R . .
H24C H -0.3076 0.3710 0.7809 0.089 Uiso 1 1 calc R . .
C25 C -0.0243(2) 0.36184(12) 0.73515(19) 0.0341(7) Uani 1 1 d . . .
H25 H -0.0715 0.3845 0.7167 0.041 Uiso 1 1 calc R . .
C26 C 0.0630(2) 0.36436(11) 0.70837(19) 0.0333(7) Uani 1 1 d . . .
H26 H 0.0749 0.3894 0.6751 0.040 Uiso 1 1 calc R . .
C27 C 0.1320(2) 0.32948(11) 0.73138(18) 0.0296(7) Uani 1 1 d . . .
H27 H 0.1898 0.3299 0.7118 0.035 Uiso 1 1 calc R . .
C28 C -0.0078(2) 0.17585(12) 1.02962(18) 0.0336(7) Uani 1 1 d . . .
C29 C -0.0459(2) 0.21788(13) 1.0570(2) 0.0394(8) Uani 1 1 d . . .
H29 H -0.0072 0.2453 1.0671 0.047 Uiso 1 1 calc R . .
C30 C -0.1400(3) 0.21978(17) 1.0696(3) 0.0564(11) Uani 1 1 d . . .
H30 H -0.1642 0.2483 1.0880 0.068 Uiso 1 1 calc R . .
C31 C -0.1975(3) 0.1798(2) 1.0550(3) 0.0727(15) Uani 1 1 d . . .
H31 H -0.2610 0.1812 1.0633 0.087 Uiso 1 1 calc R . .
C32 C -0.1623(3) 0.1376(2) 1.0282(3) 0.0710(14) Uani 1 1 d . . .
H32 H -0.2014 0.1103 1.0192 0.085 Uiso 1 1 calc R . .
C33 C -0.0679(3) 0.13579(15) 1.0145(2) 0.0513(10) Uani 1 1 d . . .
H33 H -0.0447 0.1074 0.9949 0.062 Uiso 1 1 calc R . .
C34 C 0.2915(2) 0.44263(11) 0.84373(17) 0.0259(6) Uani 1 1 d . . .
C35 C 0.2033(2) 0.46481(12) 0.8428(2) 0.0358(8) Uani 1 1 d . . .
H35 H 0.1918 0.4951 0.8192 0.043 Uiso 1 1 calc R . .
C36 C 0.1316(2) 0.44240(13) 0.8765(2) 0.0392(8) Uani 1 1 d . . .
H36 H 0.0723 0.4575 0.8751 0.047 Uiso 1 1 calc R . .
C37 C 0.1485(2) 0.39772(12) 0.91207(19) 0.0350(8) Uani 1 1 d . . .
H37 H 0.1006 0.3826 0.9348 0.042 Uiso 1 1 calc R . .
C38 C 0.2358(2) 0.37556(12) 0.91397(19) 0.0340(7) Uani 1 1 d . . .
H38 H 0.2474 0.3456 0.9387 0.041 Uiso 1 1 calc R . .
C39 C 0.3070(2) 0.39735(11) 0.87930(19) 0.0323(7) Uani 1 1 d . . .
H39 H 0.3655 0.3816 0.8798 0.039 Uiso 1 1 calc R . .
C40 C 0.4038(2) 0.43927(11) 0.71591(19) 0.0294(7) Uani 1 1 d . . .
C41 C 0.3324(2) 0.41006(12) 0.6746(2) 0.0360(8) Uani 1 1 d . . .
H41 H 0.2748 0.4055 0.6934 0.043 Uiso 1 1 calc R . .
C42 C 0.3467(3) 0.38785(14) 0.6060(2) 0.0511(10) Uani 1 1 d . . .
H42 H 0.2989 0.3682 0.5789 0.061 Uiso 1 1 calc R . .
C43 C 0.4319(3) 0.39480(15) 0.5773(3) 0.0581(11) Uani 1 1 d . . .
H43 H 0.4411 0.3803 0.5305 0.070 Uiso 1 1 calc R . .
C44 C 0.5029(3) 0.42328(17) 0.6182(3) 0.0642(12) Uani 1 1 d . . .
H44 H 0.5604 0.4276 0.5992 0.077 Uiso 1 1 calc R . .
C45 C 0.4898(3) 0.44541(14) 0.6870(2) 0.0469(9) Uani 1 1 d . . .
H45 H 0.5384 0.4645 0.7143 0.056 Uiso 1 1 calc R . .
C46 C 0.4932(2) 0.47508(11) 0.86708(19) 0.0292(7) Uani 1 1 d . . .
C47 C 0.5255(2) 0.51869(12) 0.90210(19) 0.0348(8) Uani 1 1 d . . .
H47 H 0.4896 0.5470 0.8910 0.042 Uiso 1 1 calc R . .
C48 C 0.6115(3) 0.52003(15) 0.9538(2) 0.0468(9) Uani 1 1 d . . .
H48 H 0.6333 0.5493 0.9771 0.056 Uiso 1 1 calc R . .
C49 C 0.6645(3) 0.47859(16) 0.9706(2) 0.0485(10) Uani 1 1 d . . .
H49 H 0.7214 0.4797 1.0061 0.058 Uiso 1 1 calc R . .
C50 C 0.6344(3) 0.43577(16) 0.9356(3) 0.0541(11) Uani 1 1 d . . .
H50 H 0.6716 0.4079 0.9466 0.065 Uiso 1 1 calc R . .
C51 C 0.5487(2) 0.43322(13) 0.8836(2) 0.0447(9) Uani 1 1 d . . .
H51 H 0.5284 0.4038 0.8600 0.054 Uiso 1 1 calc R . .
C52 C 0.3878(2) 0.60316(11) 0.68391(19) 0.0304(7) Uani 1 1 d . . .
C53 C 0.4848(2) 0.59288(13) 0.7019(2) 0.0459(9) Uani 1 1 d . . .
H53 H 0.5052 0.5662 0.7333 0.055 Uiso 1 1 calc R . .
C54 C 0.5513(3) 0.62182(15) 0.6738(3) 0.0581(12) Uani 1 1 d . . .
H54 H 0.6164 0.6147 0.6863 0.070 Uiso 1 1 calc R . .
C55 C 0.5218(3) 0.66115(14) 0.6273(3) 0.0548(11) Uani 1 1 d . . .
H55 H 0.5666 0.6803 0.6073 0.066 Uiso 1 1 calc R . .
C56 C 0.4260(3) 0.67207(15) 0.6106(3) 0.0605(12) Uani 1 1 d . . .
H56 H 0.4060 0.6992 0.5802 0.073 Uiso 1 1 calc R . .
C57 C 0.3595(3) 0.64351(14) 0.6381(2) 0.0493(10) Uani 1 1 d . . .
H57 H 0.2946 0.6512 0.6260 0.059 Uiso 1 1 calc R . .
C58 C 0.2109(2) 0.59703(10) 0.75114(19) 0.0272(7) Uani 1 1 d . . .
C59 C 0.2131(2) 0.59984(13) 0.8314(2) 0.0388(8) Uani 1 1 d . . .
H59 H 0.2604 0.5833 0.8650 0.047 Uiso 1 1 calc R . .
C60 C 0.1451(3) 0.62716(15) 0.8617(2) 0.0521(10) Uani 1 1 d . . .
H60 H 0.1466 0.6286 0.9156 0.063 Uiso 1 1 calc R . .
C61 C 0.0754(3) 0.65209(14) 0.8129(3) 0.0514(11) Uani 1 1 d . . .
H61 H 0.0304 0.6707 0.8336 0.062 Uiso 1 1 calc R . .
C62 C 0.0725(3) 0.64957(13) 0.7339(3) 0.0495(10) Uani 1 1 d . . .
H62 H 0.0252 0.6665 0.7010 0.059 Uiso 1 1 calc R . .
C63 C 0.1398(2) 0.62191(13) 0.7016(2) 0.0388(8) Uani 1 1 d . . .
H63 H 0.1370 0.6202 0.6477 0.047 Uiso 1 1 calc R . .
C64 C 0.2460(2) 0.53022(11) 0.62765(19) 0.0328(7) Uani 1 1 d . . .
C65 C 0.1560(3) 0.50984(12) 0.6260(2) 0.0395(8) Uani 1 1 d . . .
H65 H 0.1212 0.5162 0.6662 0.047 Uiso 1 1 calc R . .
C66 C 0.1175(3) 0.47997(14) 0.5642(3) 0.0558(11) Uani 1 1 d . . .
H66 H 0.0573 0.4660 0.5634 0.067 Uiso 1 1 calc R . .
C67 C 0.1681(4) 0.47102(16) 0.5041(3) 0.0647(13) Uani 1 1 d . . .
H67 H 0.1423 0.4510 0.4628 0.078 Uiso 1 1 calc R . .
C68 C 0.2568(4) 0.49175(16) 0.5055(2) 0.0658(13) Uani 1 1 d . . .
H68 H 0.2907 0.4857 0.4647 0.079 Uiso 1 1 calc R . .
C69 C 0.2972(3) 0.52172(13) 0.5669(2) 0.0451(9) Uani 1 1 d . . .
H69 H 0.3572 0.5358 0.5671 0.054 Uiso 1 1 calc R . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 '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'
Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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
P1 Ni1 S3 87.04(3) . . ?
P1 Ni1 S4 176.82(3) . . ?
S3 Ni1 S4 96.11(3) . . ?
P1 Ni1 S2 87.50(3) . . ?
S3 Ni1 S2 123.94(4) . . ?
S4 Ni1 S2 90.38(4) . . ?
P1 Ni1 S1 85.21(3) . . ?
S3 Ni1 S1 128.06(4) . . ?
S4 Ni1 S1 93.16(3) . . ?
S2 Ni1 S1 106.92(3) . . ?
C2 S1 Ni1 104.78(10) . . ?
C11 S2 Ni1 106.25(10) . . ?
C20 S3 Ni1 107.50(10) . . ?
C28 S4 Ni1 111.78(11) . . ?
C1 P1 C19 107.09(14) . . ?
C1 P1 C10 109.84(13) . . ?
C19 P1 C10 110.07(14) . . ?
C1 P1 Ni1 109.31(10) . . ?
C19 P1 Ni1 110.39(10) . . ?
C10 P1 Ni1 110.08(10) . . ?
N1 P2 C40 114.60(14) . . ?
N1 P2 C46 106.34(14) . . ?
C40 P2 C46 107.14(15) . . ?
N1 P2 C34 110.53(14) . . ?
C40 P2 C34 108.56(14) . . ?
C46 P2 C34 109.53(14) . . ?
N1 P3 C52 109.55(15) . . ?
N1 P3 C58 108.55(14) . . ?
C52 P3 C58 109.21(14) . . ?
N1 P3 C64 114.00(14) . . ?
C52 P3 C64 106.89(15) . . ?
C58 P3 C64 108.55(15) . . ?
C4 Si1 C5 111.1(2) . . ?
C4 Si1 C6 105.87(18) . . ?
C5 Si1 C6 107.9(2) . . ?
C4 Si1 C3 112.48(15) . . ?
C5 Si1 C3 110.80(16) . . ?
C6 Si1 C3 108.48(17) . . ?
C13 Si2 C15 111.0(2) . . ?
C13 Si2 C14 105.5(2) . . ?
C15 Si2 C14 108.2(3) . . ?
C13 Si2 C12 112.73(18) . . ?
C15 Si2 C12 111.06(19) . . ?
C14 Si2 C12 107.98(19) . . ?
C22 Si3 C23 110.6(3) . . ?
C22 Si3 C24 108.0(2) . . ?
C23 Si3 C24 108.1(2) . . ?
C22 Si3 C21 111.93(18) . . ?
C23 Si3 C21 109.33(18) . . ?
C24 Si3 C21 108.70(17) . . ?
P2 N1 P3 141.93(18) . . ?
C9 C1 C2 122.0(3) . . ?
C9 C1 P1 123.5(2) . . ?
C2 C1 P1 114.5(2) . . ?
C1 C2 C3 119.2(3) . . ?
C1 C2 S1 118.7(2) . . ?
C3 C2 S1 122.1(2) . . ?
C7 C3 C2 116.8(3) . . ?
C7 C3 Si1 118.2(2) . . ?
C2 C3 Si1 125.0(2) . . ?
Si1 C4 H4A 109.5 . . ?
Si1 C4 H4B 109.5 . . ?
H4A C4 H4B 109.5 . . ?
Si1 C4 H4C 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
Si1 C5 H5A 109.5 . . ?
Si1 C5 H5B 109.5 . . ?
H5A C5 H5B 109.5 . . ?
Si1 C5 H5C 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
Si1 C6 H6A 109.5 . . ?
Si1 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
Si1 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
C8 C7 C3 123.7(3) . . ?
C8 C7 H7 118.1 . . ?
C3 C7 H7 118.1 . . ?
C9 C8 C7 119.4(3) . . ?
C9 C8 H8 120.3 . . ?
C7 C8 H8 120.3 . . ?
C8 C9 C1 119.0(3) . . ?
C8 C9 H9 120.5 . . ?
C1 C9 H9 120.5 . . ?
C18 C10 C11 121.4(3) . . ?
C18 C10 P1 123.9(3) . . ?
C11 C10 P1 114.7(2) . . ?
C10 C11 C12 119.9(3) . . ?
C10 C11 S2 120.1(2) . . ?
C12 C11 S2 120.0(2) . . ?
C16 C12 C11 116.3(3) . . ?
C16 C12 Si2 120.8(2) . . ?
C11 C12 Si2 122.9(2) . . ?
Si2 C13 H13A 109.5 . . ?
Si2 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
Si2 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
Si2 C14 H14A 109.5 . . ?
Si2 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
Si2 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
Si2 C15 H15A 109.5 . . ?
Si2 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
Si2 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C17 C16 C12 123.6(3) . . ?
C17 C16 H16 118.2 . . ?
C12 C16 H16 118.2 . . ?
C16 C17 C18 119.4(3) . . ?
C16 C17 H17 120.3 . . ?
C18 C17 H17 120.3 . . ?
C17 C18 C10 119.3(3) . . ?
C17 C18 H18 120.4 . . ?
C10 C18 H18 120.4 . . ?
C27 C19 C20 121.0(3) . . ?
C27 C19 P1 125.5(2) . . ?
C20 C19 P1 113.5(2) . . ?
C19 C20 C21 120.1(3) . . ?
C19 C20 S3 119.3(2) . . ?
C21 C20 S3 120.5(2) . . ?
C25 C21 C20 116.5(3) . . ?
C25 C21 Si3 120.8(2) . . ?
C20 C21 Si3 122.7(2) . . ?
Si3 C22 H22A 109.5 . . ?
Si3 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
Si3 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
Si3 C23 H23A 109.5 . . ?
Si3 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
Si3 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
Si3 C24 H24A 109.5 . . ?
Si3 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
Si3 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C26 C25 C21 123.1(3) . . ?
C26 C25 H25 118.4 . . ?
C21 C25 H25 118.4 . . ?
C27 C26 C25 119.5(3) . . ?
C27 C26 H26 120.2 . . ?
C25 C26 H26 120.2 . . ?
C26 C27 C19 119.5(3) . . ?
C26 C27 H27 120.3 . . ?
C19 C27 H27 120.3 . . ?
C33 C28 C29 117.8(3) . . ?
C33 C28 S4 120.7(3) . . ?
C29 C28 S4 121.2(3) . . ?
C30 C29 C28 121.3(4) . . ?
C30 C29 H29 119.4 . . ?
C28 C29 H29 119.4 . . ?
C31 C30 C29 119.9(4) . . ?
C31 C30 H30 120.0 . . ?
C29 C30 H30 120.0 . . ?
C30 C31 C32 120.4(4) . . ?
C30 C31 H31 119.8 . . ?
C32 C31 H31 119.8 . . ?
C31 C32 C33 119.9(4) . . ?
C31 C32 H32 120.1 . . ?
C33 C32 H32 120.1 . . ?
C32 C33 C28 120.7(4) . . ?
C32 C33 H33 119.6 . . ?
C28 C33 H33 119.6 . . ?
C35 C34 C39 118.5(3) . . ?
C35 C34 P2 118.9(2) . . ?
C39 C34 P2 122.6(2) . . ?
C34 C35 C36 120.8(3) . . ?
C34 C35 H35 119.6 . . ?
C36 C35 H35 119.6 . . ?
C37 C36 C35 119.9(3) . . ?
C37 C36 H36 120.1 . . ?
C35 C36 H36 120.1 . . ?
C38 C37 C36 119.9(3) . . ?
C38 C37 H37 120.1 . . ?
C36 C37 H37 120.1 . . ?
C37 C38 C39 120.6(3) . . ?
C37 C38 H38 119.7 . . ?
C39 C38 H38 119.7 . . ?
C38 C39 C34 120.3(3) . . ?
C38 C39 H39 119.8 . . ?
C34 C39 H39 119.8 . . ?
C41 C40 C45 119.0(3) . . ?
C41 C40 P2 121.0(2) . . ?
C45 C40 P2 119.7(2) . . ?
C42 C41 C40 120.3(3) . . ?
C42 C41 H41 119.9 . . ?
C40 C41 H41 119.9 . . ?
C41 C42 C43 120.2(4) . . ?
C41 C42 H42 119.9 . . ?
C43 C42 H42 119.9 . . ?
C44 C43 C42 119.7(4) . . ?
C44 C43 H43 120.1 . . ?
C42 C43 H43 120.1 . . ?
C45 C44 C43 120.7(4) . . ?
C45 C44 H44 119.7 . . ?
C43 C44 H44 119.7 . . ?
C44 C45 C40 120.2(3) . . ?
C44 C45 H45 119.9 . . ?
C40 C45 H45 119.9 . . ?
C47 C46 C51 119.3(3) . . ?
C47 C46 P2 119.7(2) . . ?
C51 C46 P2 121.1(3) . . ?
C46 C47 C48 119.8(3) . . ?
C46 C47 H47 120.1 . . ?
C48 C47 H47 120.1 . . ?
C49 C48 C47 120.5(4) . . ?
C49 C48 H48 119.8 . . ?
C47 C48 H48 119.8 . . ?
C50 C49 C48 120.3(3) . . ?
C50 C49 H49 119.9 . . ?
C48 C49 H49 119.9 . . ?
C49 C50 C51 120.7(4) . . ?
C49 C50 H50 119.7 . . ?
C51 C50 H50 119.7 . . ?
C50 C51 C46 119.5(4) . . ?
C50 C51 H51 120.2 . . ?
C46 C51 H51 120.2 . . ?
C53 C52 C57 118.6(3) . . ?
C53 C52 P3 120.0(3) . . ?
C57 C52 P3 121.3(3) . . ?
C54 C53 C52 120.5(4) . . ?
C54 C53 H53 119.8 . . ?
C52 C53 H53 119.8 . . ?
C55 C54 C53 120.2(4) . . ?
C55 C54 H54 119.9 . . ?
C53 C54 H54 119.9 . . ?
C56 C55 C54 119.6(3) . . ?
C56 C55 H55 120.2 . . ?
C54 C55 H55 120.2 . . ?
C55 C56 C57 120.7(4) . . ?
C55 C56 H56 119.7 . . ?
C57 C56 H56 119.7 . . ?
C56 C57 C52 120.5(4) . . ?
C56 C57 H57 119.7 . . ?
C52 C57 H57 119.7 . . ?
C59 C58 C63 119.3(3) . . ?
C59 C58 P3 119.1(2) . . ?
C63 C58 P3 121.6(3) . . ?
C60 C59 C58 120.3(3) . . ?
C60 C59 H59 119.9 . . ?
C58 C59 H59 119.9 . . ?
C61 C60 C59 120.5(4) . . ?
C61 C60 H60 119.8 . . ?
C59 C60 H60 119.8 . . ?
C62 C61 C60 119.8(4) . . ?
C62 C61 H61 120.1 . . ?
C60 C61 H61 120.1 . . ?
C61 C62 C63 120.9(4) . . ?
C61 C62 H62 119.5 . . ?
C63 C62 H62 119.5 . . ?
C58 C63 C62 119.3(3) . . ?
C58 C63 H63 120.4 . . ?
C62 C63 H63 120.4 . . ?
C65 C64 C69 120.1(3) . . ?
C65 C64 P3 119.4(3) . . ?
C69 C64 P3 120.1(3) . . ?
C64 C65 C66 120.0(4) . . ?
C64 C65 H65 120.0 . . ?
C66 C65 H65 120.0 . . ?
C67 C66 C65 120.2(4) . . ?
C67 C66 H66 119.9 . . ?
C65 C66 H66 119.9 . . ?
C68 C67 C66 119.6(4) . . ?
C68 C67 H67 120.2 . . ?
C66 C67 H67 120.2 . . ?
C67 C68 C69 121.3(4) . . ?
C67 C68 H68 119.3 . . ?
C69 C68 H68 119.3 . . ?
C64 C69 C68 118.7(4) . . ?
C64 C69 H69 120.7 . . ?
C68 C69 H69 120.7 . . ?
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 P1 2.1375(8) . ?
Ni1 S3 2.2133(8) . ?
Ni1 S4 2.2459(9) . ?
Ni1 S2 2.2698(9) . ?
Ni1 S1 2.2986(8) . ?
S1 C2 1.760(3) . ?
S2 C11 1.756(3) . ?
S3 C20 1.770(3) . ?
S4 C28 1.771(3) . ?
P1 C1 1.803(3) . ?
P1 C19 1.806(3) . ?
P1 C10 1.812(3) . ?
P2 N1 1.571(2) . ?
P2 C40 1.792(3) . ?
P2 C46 1.801(3) . ?
P2 C34 1.806(3) . ?
P3 N1 1.584(3) . ?
P3 C52 1.791(3) . ?
P3 C58 1.792(3) . ?
P3 C64 1.804(3) . ?
Si1 C4 1.860(4) . ?
Si1 C5 1.863(4) . ?
Si1 C6 1.876(4) . ?
Si1 C3 1.882(3) . ?
Si2 C13 1.854(4) . ?
Si2 C15 1.855(4) . ?
Si2 C14 1.864(4) . ?
Si2 C12 1.902(4) . ?
Si3 C22 1.858(5) . ?
Si3 C23 1.859(4) . ?
Si3 C24 1.870(4) . ?
Si3 C21 1.884(3) . ?
C1 C9 1.396(4) . ?
C1 C2 1.410(4) . ?
C2 C3 1.423(4) . ?
C3 C7 1.398(4) . ?
C4 H4A 0.9600 . ?
C4 H4B 0.9600 . ?
C4 H4C 0.9600 . ?
C5 H5A 0.9600 . ?
C5 H5B 0.9600 . ?
C5 H5C 0.9600 . ?
C6 H6A 0.9600 . ?
C6 H6B 0.9600 . ?
C6 H6C 0.9600 . ?
C7 C8 1.388(5) . ?
C7 H7 0.9300 . ?
C8 C9 1.385(4) . ?
C8 H8 0.9300 . ?
C9 H9 0.9300 . ?
C10 C18 1.393(4) . ?
C10 C11 1.403(4) . ?
C11 C12 1.431(4) . ?
C12 C16 1.396(5) . ?
C13 H13A 0.9600 . ?
C13 H13B 0.9600 . ?
C13 H13C 0.9600 . ?
C14 H14A 0.9600 . ?
C14 H14B 0.9600 . ?
C14 H14C 0.9600 . ?
C15 H15A 0.9600 . ?
C15 H15B 0.9600 . ?
C15 H15C 0.9600 . ?
C16 C17 1.388(5) . ?
C16 H16 0.9300 . ?
C17 C18 1.387(5) . ?
C17 H17 0.9300 . ?
C18 H18 0.9300 . ?
C19 C27 1.393(4) . ?
C19 C20 1.393(4) . ?
C20 C21 1.421(4) . ?
C21 C25 1.395(4) . ?
C22 H22A 0.9600 . ?
C22 H22B 0.9600 . ?
C22 H22C 0.9600 . ?
C23 H23A 0.9600 . ?
C23 H23B 0.9600 . ?
C23 H23C 0.9600 . ?
C24 H24A 0.9600 . ?
C24 H24B 0.9600 . ?
C24 H24C 0.9600 . ?
C25 C26 1.383(5) . ?
C25 H25 0.9300 . ?
C26 C27 1.379(4) . ?
C26 H26 0.9300 . ?
C27 H27 0.9300 . ?
C28 C33 1.388(5) . ?
C28 C29 1.388(5) . ?
C29 C30 1.379(5) . ?
C29 H29 0.9300 . ?
C30 C31 1.365(7) . ?
C30 H30 0.9300 . ?
C31 C32 1.370(7) . ?
C31 H31 0.9300 . ?
C32 C33 1.389(6) . ?
C32 H32 0.9300 . ?
C33 H33 0.9300 . ?
C34 C35 1.382(4) . ?
C34 C39 1.390(4) . ?
C35 C36 1.389(5) . ?
C35 H35 0.9300 . ?
C36 C37 1.377(5) . ?
C36 H36 0.9300 . ?
C37 C38 1.369(5) . ?
C37 H37 0.9300 . ?
C38 C39 1.384(4) . ?
C38 H38 0.9300 . ?
C39 H39 0.9300 . ?
C40 C41 1.393(4) . ?
C40 C45 1.392(4) . ?
C41 C42 1.379(5) . ?
C41 H41 0.9300 . ?
C42 C43 1.384(6) . ?
C42 H42 0.9300 . ?
C43 C44 1.375(6) . ?
C43 H43 0.9300 . ?
C44 C45 1.376(5) . ?
C44 H44 0.9300 . ?
C45 H45 0.9300 . ?
C46 C47 1.386(4) . ?
C46 C51 1.394(4) . ?
C47 C48 1.389(5) . ?
C47 H47 0.9300 . ?
C48 C49 1.367(5) . ?
C48 H48 0.9300 . ?
C49 C50 1.360(6) . ?
C49 H49 0.9300 . ?
C50 C51 1.389(5) . ?
C50 H50 0.9300 . ?
C51 H51 0.9300 . ?
C52 C53 1.381(5) . ?
C52 C57 1.384(5) . ?
C53 C54 1.376(5) . ?
C53 H53 0.9300 . ?
C54 C55 1.372(6) . ?
C54 H54 0.9300 . ?
C55 C56 1.368(6) . ?
C55 H55 0.9300 . ?
C56 C57 1.365(5) . ?
C56 H56 0.9300 . ?
C57 H57 0.9300 . ?
C58 C59 1.387(5) . ?
C58 C63 1.390(4) . ?
C59 C60 1.385(5) . ?
C59 H59 0.9300 . ?
C60 C61 1.372(6) . ?
C60 H60 0.9300 . ?
C61 C62 1.365(6) . ?
C61 H61 0.9300 . ?
C62 C63 1.398(5) . ?
C62 H62 0.9300 . ?
C63 H63 0.9300 . ?
C64 C65 1.383(5) . ?
C64 C69 1.386(5) . ?
C65 C66 1.388(5) . ?
C65 H65 0.9300 . ?
C66 C67 1.373(6) . ?
C66 H66 0.9300 . ?
C67 C68 1.371(7) . ?
C67 H67 0.9300 . ?
C68 C69 1.392(6) . ?
C68 H68 0.9300 . ?
C69 H69 0.9300 . ?
