# Electronic Supplementary Material (ESI) for Chemical Science.
# This journal is © The Royal Society of Chemistry 2016

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_091120lt
_audit_block_doi                 10.5517/ccvcdq9
_database_code_depnum_ccdc_archive 'CCDC 785531'
_audit_update_record             
;
2015-11-05 deposited with the CCDC.
2016-02-16 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C68 H74 N Ni O3 P3 S3 Si3'
_chemical_formula_weight         1285.35

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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'
S S 0.1246 0.1234 '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                   27.4702(8)
_cell_length_b                   17.1432(6)
_cell_length_c                   27.9778(8)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     13175.5(7)
_cell_formula_units_Z            8
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9936
_cell_measurement_theta_min      2.5
_cell_measurement_theta_max      25

_exptl_crystal_description       Columnar
_exptl_crystal_colour            Black
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.12
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_density_diffrn    1.296
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             5408
_exptl_absorpt_coefficient_mu    0.563
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.6754
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            76294
_diffrn_reflns_av_R_equivalents  0.0589
_diffrn_reflns_av_sigmaI/netI    0.0549
_diffrn_reflns_limit_h_min       -34
_diffrn_reflns_limit_h_max       34
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_theta_min         1.46
_diffrn_reflns_theta_max         26.45
_reflns_number_total             13499
_reflns_number_gt                9267
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker APEX2'
_computing_data_reduction        'Bruker Saint'
_computing_structure_solution    'Shelxtl-97 (Sheldrick, 2008)'
_computing_structure_refinement  'Shelxtl-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'Bruker APEX2'
_computing_publication_material  'Bruker APEX2'

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0852P)²+24.4055P] where P=(Fo²+2Fc²)/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         13499
_refine_ls_number_parameters     748
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0912
_refine_ls_R_factor_gt           0.0552
_refine_ls_wR_factor_ref         0.1725
_refine_ls_wR_factor_gt          0.1449
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_restrained_S_all      1.042
_refine_ls_shift/su_max          0.034
_refine_ls_shift/su_mean         0.001

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 0.290284(17) 0.96677(3) 0.180430(16) 0.01953(13) Uani 1 1 d . . .
P1 P 0.43834(3) 0.75930(6) 0.90357(3) 0.0193(2) Uani 1 1 d . . .
P2 P 0.52803(3) 0.68863(6) 0.94349(3) 0.0216(2) Uani 1 1 d . . .
P3 P 0.25679(3) 0.86050(6) 0.15964(3) 0.0182(2) Uani 1 1 d . . .
S1 S 0.35954(3) 0.90583(6) 0.15468(3) 0.0225(2) Uani 1 1 d . . .
S2 S 0.23886(3) 0.96993(6) 0.24164(3) 0.0225(2) Uani 1 1 d . . .
S3 S 0.25772(3) 1.02157(6) 0.11319(3) 0.0217(2) Uani 1 1 d . . .
Si1 Si 0.45273(4) 0.77315(7) 0.17099(4) 0.0251(3) Uani 1 1 d . . .
Si2 Si 0.14940(4) 0.94064(8) 0.32265(4) 0.0322(3) Uani 1 1 d . . .
Si3 Si 0.20901(4) 1.05517(7) 0.00531(4) 0.0278(3) Uani 1 1 d . . .
N1 N 0.47198(10) 0.7015(2) 0.93248(11) 0.0223(7) Uani 1 1 d . . .
O1 O 0.32630(12) 1.06425(19) 0.20136(11) 0.0372(7) Uani 1 1 d . . .
O2 O 0.38665(16) 1.0838(3) 0.26048(16) 0.0784(14) Uani 1 1 d . . .
O3 O 0.7041(2) 0.6424(3) 0.11395(17) 0.0911(16) Uani 1 1 d . . .
C1 C 0.47017(13) 0.8378(2) 0.87480(13) 0.0228(8) Uani 1 1 d . . .
C2 C 0.47785(15) 0.9079(3) 0.89878(17) 0.0323(10) Uani 1 1 d . . .
H2 H 0.4624 0.9170 0.9286 0.039 Uiso 1 1 calc R . .
C3 C 0.50760(17) 0.9640(3) 0.87959(19) 0.0425(12) Uani 1 1 d . . .
H3 H 0.5128 1.0115 0.8963 0.051 Uiso 1 1 calc R . .
C4 C 0.52998(17) 0.9516(3) 0.83611(19) 0.0427(13) Uani 1 1 d . . .
H4 H 0.5509 0.9905 0.8233 0.051 Uiso 1 1 calc R . .
C5 C 0.52227(15) 0.8834(3) 0.81112(16) 0.0365(11) Uani 1 1 d . . .
H5 H 0.5372 0.8756 0.7809 0.044 Uiso 1 1 calc R . .
C6 C 0.49256(14) 0.8263(3) 0.83060(14) 0.0289(9) Uani 1 1 d . . .
H6 H 0.4874 0.7789 0.8137 0.035 Uiso 1 1 calc R . .
C7 C 0.40554(13) 0.7063(3) 0.85879(13) 0.0250(9) Uani 1 1 d . . .
C8 C 0.38245(14) 0.7448(3) 0.82088(14) 0.0348(11) Uani 1 1 d . . .
H8 H 0.3854 0.7997 0.8172 0.042 Uiso 1 1 calc R . .
C9 C 0.35504(16) 0.7012(4) 0.78864(15) 0.0496(15) Uani 1 1 d . . .
H9 H 0.3387 0.7265 0.7631 0.060 Uiso 1 1 calc R . .
C10 C 0.35158(19) 0.6203(4) 0.79382(17) 0.0577(17) Uani 1 1 d . . .
H10 H 0.3330 0.5908 0.7716 0.069 Uiso 1 1 calc R . .
C11 C 0.3746(2) 0.5838(4) 0.83027(17) 0.0551(16) Uani 1 1 d . . .
H11 H 0.3724 0.5287 0.8330 0.066 Uiso 1 1 calc R . .
C12 C 0.40145(16) 0.6257(3) 0.86379(16) 0.0371(11) Uani 1 1 d . . .
H12 H 0.4168 0.5996 0.8897 0.045 Uiso 1 1 calc R . .
C13 C 0.39549(13) 0.8030(2) 0.94402(13) 0.0227(8) Uani 1 1 d . . .
C14 C 0.35323(15) 0.8387(3) 0.92751(14) 0.0344(11) Uani 1 1 d . . .
H14 H 0.3457 0.8374 0.8944 0.041 Uiso 1 1 calc R . .
C15 C 0.32234(16) 0.8758(3) 0.95871(16) 0.0408(12) Uani 1 1 d . . .
H15 H 0.2938 0.9007 0.9471 0.049 Uiso 1 1 calc R . .
C16 C 0.33288(15) 0.8768(3) 1.00686(15) 0.0354(11) Uani 1 1 d . . .
H16 H 0.3120 0.9036 1.0284 0.043 Uiso 1 1 calc R . .
C17 C 0.37342(15) 0.8394(3) 1.02391(15) 0.0372(11) Uani 1 1 d . . .
H17 H 0.3799 0.8387 1.0573 0.045 Uiso 1 1 calc R . .
C18 C 0.40502(14) 0.8023(3) 0.99232(14) 0.0307(10) Uani 1 1 d . . .
H18 H 0.4332 0.7765 1.0041 0.037 Uiso 1 1 calc R . .
C19 C 0.53232(15) 0.6418(3) 1.00080(14) 0.0295(10) Uani 1 1 d . . .
C20 C 0.49200(18) 0.6028(3) 1.01945(15) 0.0349(10) Uani 1 1 d . . .
H20 H 0.4621 0.6019 1.0024 0.042 Uiso 1 1 calc R . .
C21 C 0.4962(2) 0.5648(3) 1.06377(17) 0.0472(13) Uani 1 1 d . . .
H21 H 0.4692 0.5373 1.0765 0.057 Uiso 1 1 calc R . .
C22 C 0.5390(2) 0.5671(3) 1.08873(17) 0.0502(14) Uani 1 1 d . . .
H22 H 0.5414 0.5409 1.1186 0.060 Uiso 1 1 calc R . .
C23 C 0.5787(2) 0.6070(4) 1.07103(16) 0.0549(16) Uani 1 1 d . . .
H23 H 0.6080 0.6090 1.0890 0.066 Uiso 1 1 calc R . .
C24 C 0.57600(17) 0.6441(4) 1.02733(16) 0.0465(14) Uani 1 1 d . . .
H24 H 0.6035 0.6712 1.0151 0.056 Uiso 1 1 calc R . .
C25 C 0.56342(13) 0.7762(3) 0.94723(14) 0.0251(9) Uani 1 1 d . . .
C26 C 0.55864(16) 0.8255(3) 0.98683(15) 0.0372(11) Uani 1 1 d . . .
H26 H 0.5386 0.8108 1.0130 0.045 Uiso 1 1 calc R . .
C27 C 0.58367(19) 0.8967(3) 0.98749(18) 0.0481(13) Uani 1 1 d . . .
H27 H 0.5805 0.9303 1.0143 0.058 Uiso 1 1 calc R . .
C28 C 0.61274(16) 0.9185(3) 0.94996(18) 0.0440(12) Uani 1 1 d . . .
H28 H 0.6296 0.9669 0.9509 0.053 Uiso 1 1 calc R . .
C29 C 0.61743(15) 0.8703(3) 0.91077(17) 0.0371(11) Uani 1 1 d . . .
H29 H 0.6374 0.8858 0.8847 0.044 Uiso 1 1 calc R . .
C30 C 0.59328(13) 0.7995(3) 0.90913(15) 0.0265(9) Uani 1 1 d . . .
H30 H 0.5969 0.7665 0.8821 0.032 Uiso 1 1 calc R . .
C31 C 0.55547(13) 0.6270(2) 0.89879(13) 0.0219(8) Uani 1 1 d . . .
C32 C 0.60114(13) 0.5926(3) 0.90566(15) 0.0276(9) Uani 1 1 d . . .
H32 H 0.6184 0.6017 0.9345 0.033 Uiso 1 1 calc R . .
C33 C 0.62130(14) 0.5456(2) 0.87061(15) 0.0282(9) Uani 1 1 d . . .
H33 H 0.6520 0.5214 0.8758 0.034 Uiso 1 1 calc R . .
C34 C 0.59669(14) 0.5340(2) 0.82819(15) 0.0265(9) Uani 1 1 d . . .
H34 H 0.6109 0.5028 0.8038 0.032 Uiso 1 1 calc R . .
C35 C 0.55147(15) 0.5676(3) 0.82090(14) 0.0311(10) Uani 1 1 d . . .
H35 H 0.5346 0.5592 0.7917 0.037 Uiso 1 1 calc R . .
C36 C 0.53078(15) 0.6134(3) 0.85620(14) 0.0274(9) Uani 1 1 d . . .
H36 H 0.4995 0.6357 0.8513 0.033 Uiso 1 1 calc R . .
C37 C 0.29909(13) 0.7818(2) 0.16749(13) 0.0198(8) Uani 1 1 d . . .
C38 C 0.34811(13) 0.8056(2) 0.16379(12) 0.0202(8) Uani 1 1 d . . .
C39 C 0.38550(13) 0.7503(2) 0.16965(13) 0.0211(8) Uani 1 1 d . . .
C40 C 0.37113(14) 0.6731(3) 0.17797(14) 0.0275(9) Uani 1 1 d . . .
H40 H 0.3958 0.6347 0.1813 0.033 Uiso 1 1 calc R . .
C41 C 0.32343(15) 0.6496(3) 0.18160(15) 0.0298(9) Uani 1 1 d . . .
H41 H 0.3158 0.5964 0.1873 0.036 Uiso 1 1 calc R . .
C42 C 0.28657(14) 0.7041(3) 0.17680(14) 0.0265(9) Uani 1 1 d . . .
H42 H 0.2534 0.6891 0.1798 0.032 Uiso 1 1 calc R . .
C43 C 0.47356(15) 0.8058(3) 0.11076(15) 0.0372(11) Uani 1 1 d . . .
H43A H 0.4570 0.8546 0.1022 0.056 Uiso 1 1 calc R . .
H43B H 0.4658 0.7657 0.0870 0.056 Uiso 1 1 calc R . .
H43C H 0.5088 0.8145 0.1113 0.056 Uiso 1 1 calc R . .
C44 C 0.46712(14) 0.8456(3) 0.21882(15) 0.0311(10) Uani 1 1 d . . .
H44A H 0.5012 0.8620 0.2159 0.047 Uiso 1 1 calc R . .
H44B H 0.4619 0.8217 0.2502 0.047 Uiso 1 1 calc R . .
H44C H 0.4458 0.8911 0.2154 0.047 Uiso 1 1 calc R . .
C45 C 0.48633(15) 0.6812(3) 0.18587(16) 0.0375(11) Uani 1 1 d . . .
H45A H 0.4807 0.6424 0.1608 0.056 Uiso 1 1 calc R . .
H45B H 0.4746 0.6608 0.2165 0.056 Uiso 1 1 calc R . .
H45C H 0.5213 0.6923 0.1881 0.056 Uiso 1 1 calc R . .
C46 C 0.20379(12) 0.8409(2) 0.19579(13) 0.0209(8) Uani 1 1 d . . .
C47 C 0.19863(13) 0.8904(2) 0.23508(13) 0.0214(8) Uani 1 1 d . . .
C48 C 0.16043(13) 0.8774(2) 0.26858(13) 0.0242(9) Uani 1 1 d . . .
C49 C 0.12905(14) 0.8151(3) 0.25883(14) 0.0289(9) Uani 1 1 d . . .
H49 H 0.1035 0.8047 0.2808 0.035 Uiso 1 1 calc R . .
C50 C 0.13320(14) 0.7678(3) 0.21894(15) 0.0282(9) Uani 1 1 d . . .
H50 H 0.1104 0.7271 0.2134 0.034 Uiso 1 1 calc R . .
C51 C 0.17112(13) 0.7807(2) 0.18712(14) 0.0246(9) Uani 1 1 d . . .
H51 H 0.1747 0.7486 0.1596 0.030 Uiso 1 1 calc R . .
C52 C 0.20433(18) 0.9537(4) 0.36096(16) 0.0470(13) Uani 1 1 d . . .
H52A H 0.2305 0.9773 0.3421 0.071 Uiso 1 1 calc R . .
H52B H 0.2150 0.9028 0.3730 0.071 Uiso 1 1 calc R . .
H52C H 0.1963 0.9877 0.3880 0.071 Uiso 1 1 calc R . .
C53 C 0.10118(17) 0.8946(3) 0.36012(16) 0.0473(13) Uani 1 1 d . . .
H53A H 0.1120 0.8426 0.3703 0.071 Uiso 1 1 calc R . .
H53B H 0.0712 0.8898 0.3414 0.071 Uiso 1 1 calc R . .
H53C H 0.0951 0.9270 0.3883 0.071 Uiso 1 1 calc R . .
C54 C 0.1256(2) 1.0371(3) 0.30344(18) 0.0499(14) Uani 1 1 d . . .
H54A H 0.1195 1.0696 0.3316 0.075 Uiso 1 1 calc R . .
H54B H 0.0951 1.0298 0.2858 0.075 Uiso 1 1 calc R . .
H54C H 0.1495 1.0627 0.2828 0.075 Uiso 1 1 calc R . .
C55 C 0.23819(12) 0.8669(2) 0.09809(13) 0.0200(8) Uani 1 1 d . . .
C56 C 0.23581(12) 0.9432(2) 0.07937(13) 0.0197(8) Uani 1 1 d . . .
C57 C 0.21608(12) 0.9553(2) 0.03283(13) 0.0214(8) Uani 1 1 d . . .
C58 C 0.20181(13) 0.8885(3) 0.00730(13) 0.0241(9) Uani 1 1 d . . .
H58 H 0.1889 0.8951 -0.0239 0.029 Uiso 1 1 calc R . .
C59 C 0.20556(13) 0.8136(3) 0.02527(13) 0.0246(9) Uani 1 1 d . . .
H59 H 0.1959 0.7702 0.0064 0.030 Uiso 1 1 calc R . .
C60 C 0.22364(13) 0.8025(2) 0.07125(13) 0.0224(8) Uani 1 1 d . . .
H60 H 0.2261 0.7514 0.0842 0.027 Uiso 1 1 calc R . .
C61 C 0.26925(18) 1.1030(3) -0.00347(16) 0.0408(12) Uani 1 1 d . . .
H61A H 0.2913 1.0669 -0.0198 0.061 Uiso 1 1 calc R . .
H61B H 0.2830 1.1172 0.0277 0.061 Uiso 1 1 calc R . .
H61C H 0.2651 1.1501 -0.0229 0.061 Uiso 1 1 calc R . .
C62 C 0.16804(19) 1.1181(3) 0.04184(19) 0.0513(14) Uani 1 1 d . . .
H62A H 0.1648 1.1693 0.0266 0.077 Uiso 1 1 calc R . .
H62B H 0.1818 1.1245 0.0739 0.077 Uiso 1 1 calc R . .
H62C H 0.1359 1.0935 0.0443 0.077 Uiso 1 1 calc R . .
C63 C 0.18110(18) 1.0432(3) -0.05484(16) 0.0416(12) Uani 1 1 d . . .
H63A H 0.1473 1.0258 -0.0513 0.062 Uiso 1 1 calc R . .
H63B H 0.1995 1.0042 -0.0730 0.062 Uiso 1 1 calc R . .
H63C H 0.1818 1.0931 -0.0718 0.062 Uiso 1 1 calc R . .
C64 C 0.35514(19) 1.0686(4) 0.2301(2) 0.0555(15) Uani 1 1 d . . .
C65 C 0.6978(4) 0.6272(6) 0.1646(2) 0.107(3) Uani 1 1 d . . .
H65A H 0.6651 0.6442 0.1752 0.128 Uiso 1 1 calc R . .
H65B H 0.7013 0.5708 0.1713 0.128 Uiso 1 1 calc R . .
C66 C 0.7338(4) 0.6696(4) 0.1884(3) 0.108(3) Uani 1 1 d . . .
H66A H 0.7636 0.6378 0.1926 0.129 Uiso 1 1 calc R . .
H66B H 0.7222 0.6870 0.2201 0.129 Uiso 1 1 calc R . .
C67 C 0.7439(3) 0.7405(5) 0.1553(3) 0.081(2) Uani 1 1 d . . .
H67A H 0.7328 0.7895 0.1705 0.097 Uiso 1 1 calc R . .
H67B H 0.7790 0.7449 0.1481 0.097 Uiso 1 1 calc R . .
C68 C 0.7153(3) 0.7242(4) 0.1107(3) 0.079(2) Uani 1 1 d . . .
H68A H 0.6852 0.7559 0.1098 0.095 Uiso 1 1 calc R . .
H68B H 0.7349 0.7355 0.0819 0.095 Uiso 1 1 calc R . .


_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 O1 2.028(3) . ?
Ni1 P3 2.1222(11) . ?
Ni1 S2 2.2208(10) . ?
Ni1 S3 2.2850(10) . ?
Ni1 S1 2.2869(11) . ?
P1 N1 1.578(3) . ?
P1 C7 1.791(4) . ?
P1 C1 1.795(4) . ?
P1 C13 1.796(4) . ?
P2 N1 1.585(3) . ?
P2 C25 1.792(4) . ?
P2 C19 1.797(4) . ?
P2 C31 1.803(4) . ?
P3 C37 1.794(4) . ?
P3 C55 1.800(4) . ?
P3 C46 1.805(4) . ?
S1 C38 1.766(4) . ?
S2 C47 1.765(4) . ?
S3 C56 1.750(4) . ?
Si1 C43 1.866(4) . ?
Si1 C44 1.868(4) . ?
Si1 C45 1.873(5) . ?
Si1 C39 1.889(4) . ?
Si2 C54 1.858(5) . ?
Si2 C52 1.864(5) . ?
Si2 C53 1.865(5) . ?
Si2 C48 1.886(4) . ?
Si3 C63 1.861(4) . ?
Si3 C61 1.863(5) . ?
Si3 C62 1.864(5) . ?
Si3 C57 1.887(4) . ?
O1 C64 1.132(6) . ?
O2 C64 1.240(7) . ?
O3 C68 1.439(8) . ?
O3 C65 1.451(8) . ?
C1 C2 1.393(6) . ?
C1 C6 1.395(5) . ?
C2 C3 1.371(6) . ?
C2 H2 0.9500 . ?
C3 C4 1.379(7) . ?
C3 H3 0.9500 . ?
C4 C5 1.379(7) . ?
C4 H4 0.9500 . ?
C5 C6 1.386(6) . ?
C5 H5 0.9500 . ?
C6 H6 0.9500 . ?
C7 C12 1.393(6) . ?
C7 C8 1.402(6) . ?
C8 C9 1.393(6) . ?
C8 H8 0.9500 . ?
C9 C10 1.397(8) . ?
C9 H9 0.9500 . ?
C10 C11 1.353(8) . ?
C10 H10 0.9500 . ?
C11 C12 1.392(6) . ?
C11 H11 0.9500 . ?
C12 H12 0.9500 . ?
C13 C18 1.377(5) . ?
C13 C14 1.392(5) . ?
C14 C15 1.374(6) . ?
C14 H14 0.9500 . ?
C15 C16 1.378(6) . ?
C15 H15 0.9500 . ?
C16 C17 1.371(6) . ?
C16 H16 0.9500 . ?
C17 C18 1.392(6) . ?
C17 H17 0.9500 . ?
C18 H18 0.9500 . ?
C19 C20 1.396(6) . ?
C19 C24 1.411(6) . ?
C20 C21 1.406(6) . ?
C20 H20 0.9500 . ?
C21 C22 1.367(8) . ?
C21 H21 0.9500 . ?
C22 C23 1.379(8) . ?
C22 H22 0.9500 . ?
C23 C24 1.380(6) . ?
C23 H23 0.9500 . ?
C24 H24 0.9500 . ?
C25 C26 1.399(6) . ?
C25 C30 1.403(5) . ?
C26 C27 1.400(7) . ?
C26 H26 0.9500 . ?
C27 C28 1.371(7) . ?
C27 H27 0.9500 . ?
C28 C29 1.379(7) . ?
C28 H28 0.9500 . ?
C29 C30 1.384(6) . ?
C29 H29 0.9500 . ?
C30 H30 0.9500 . ?
C31 C36 1.391(5) . ?
C31 C32 1.399(5) . ?
C32 C33 1.385(6) . ?
C32 H32 0.9500 . ?
C33 C34 1.380(6) . ?
C33 H33 0.9500 . ?
C34 C35 1.384(6) . ?
C34 H34 0.9500 . ?
C35 C36 1.384(6) . ?
C35 H35 0.9500 . ?
C36 H36 0.9500 . ?
C37 C42 1.399(6) . ?
C37 C38 1.411(5) . ?
C38 C39 1.407(5) . ?
C39 C40 1.399(6) . ?
C40 C41 1.375(6) . ?
C40 H40 0.9500 . ?
C41 C42 1.384(6) . ?
C41 H41 0.9500 . ?
C42 H42 0.9500 . ?
C43 H43A 0.9800 . ?
C43 H43B 0.9800 . ?
C43 H43C 0.9800 . ?
C44 H44A 0.9800 . ?
C44 H44B 0.9800 . ?
C44 H44C 0.9800 . ?
C45 H45A 0.9800 . ?
C45 H45B 0.9800 . ?
C45 H45C 0.9800 . ?
C46 C51 1.388(5) . ?
C46 C47 1.396(5) . ?
C47 C48 1.424(5) . ?
C48 C49 1.399(6) . ?
C49 C50 1.385(6) . ?
C49 H49 0.9500 . ?
C50 C51 1.388(5) . ?
C50 H50 0.9500 . ?
C51 H51 0.9500 . ?
C52 H52A 0.9800 . ?
C52 H52B 0.9800 . ?
C52 H52C 0.9800 . ?
C53 H53A 0.9800 . ?
C53 H53B 0.9800 . ?
C53 H53C 0.9800 . ?
C54 H54A 0.9800 . ?
C54 H54B 0.9800 . ?
C54 H54C 0.9800 . ?
C55 C60 1.393(5) . ?
C55 C56 1.410(5) . ?
C56 C57 1.425(5) . ?
C57 C58 1.406(6) . ?
C58 C59 1.383(6) . ?
C58 H58 0.9500 . ?
C59 C60 1.392(5) . ?
C59 H59 0.9500 . ?
C60 H60 0.9500 . ?
C61 H61A 0.9800 . ?
C61 H61B 0.9800 . ?
C61 H61C 0.9800 . ?
C62 H62A 0.9800 . ?
C62 H62B 0.9800 . ?
C62 H62C 0.9800 . ?
C63 H63A 0.9800 . ?
C63 H63B 0.9800 . ?
C63 H63C 0.9800 . ?
C65 C66 1.397(11) . ?
C65 H65A 0.9900 . ?
C65 H65B 0.9900 . ?
C66 C67 1.552(11) . ?
C66 H66A 0.9900 . ?
C66 H66B 0.9900 . ?
C67 C68 1.499(9) . ?
C67 H67A 0.9900 . ?
C67 H67B 0.9900 . ?
C68 H68A 0.9900 . ?
C68 H68B 0.9900 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Ni1 P3 176.22(10) . . ?
O1 Ni1 S2 93.87(9) . . ?
P3 Ni1 S2 87.50(4) . . ?
O1 Ni1 S3 95.16(10) . . ?
P3 Ni1 S3 87.57(4) . . ?
S2 Ni1 S3 112.08(4) . . ?
O1 Ni1 S1 93.53(9) . . ?
P3 Ni1 S1 83.23(4) . . ?
S2 Ni1 S1 141.56(4) . . ?
S3 Ni1 S1 104.72(4) . . ?
N1 P1 C7 109.5(2) . . ?
N1 P1 C1 114.54(17) . . ?
C7 P1 C1 108.17(18) . . ?
N1 P1 C13 108.83(17) . . ?
C7 P1 C13 108.82(17) . . ?
C1 P1 C13 106.81(19) . . ?
N1 P2 C25 114.95(18) . . ?
N1 P2 C19 107.40(18) . . ?
C25 P2 C19 106.6(2) . . ?
N1 P2 C31 110.66(18) . . ?
C25 P2 C31 107.77(18) . . ?
C19 P2 C31 109.25(19) . . ?
C37 P3 C55 110.29(17) . . ?
C37 P3 C46 108.27(18) . . ?
C55 P3 C46 108.58(16) . . ?
C37 P3 Ni1 109.35(13) . . ?
C55 P3 Ni1 109.46(14) . . ?
C46 P3 Ni1 110.88(14) . . ?
C38 S1 Ni1 104.55(13) . . ?
C47 S2 Ni1 107.42(13) . . ?
C56 S3 Ni1 105.32(13) . . ?
C43 Si1 C44 112.5(2) . . ?
C43 Si1 C45 107.6(2) . . ?
C44 Si1 C45 107.2(2) . . ?
C43 Si1 C39 110.14(18) . . ?
C44 Si1 C39 111.05(18) . . ?
C45 Si1 C39 108.2(2) . . ?
C54 Si2 C52 110.2(3) . . ?
C54 Si2 C53 106.8(2) . . ?
C52 Si2 C53 107.6(2) . . ?
C54 Si2 C48 109.6(2) . . ?
C52 Si2 C48 113.6(2) . . ?
C53 Si2 C48 108.8(2) . . ?
C63 Si3 C61 107.2(2) . . ?
C63 Si3 C62 108.1(2) . . ?
C61 Si3 C62 110.7(3) . . ?
C63 Si3 C57 108.1(2) . . ?
C61 Si3 C57 111.2(2) . . ?
C62 Si3 C57 111.3(2) . . ?
P1 N1 P2 139.1(2) . . ?
C64 O1 Ni1 127.0(4) . . ?
C68 O3 C65 105.1(6) . . ?
C2 C1 C6 118.8(4) . . ?
C2 C1 P1 120.3(3) . . ?
C6 C1 P1 120.4(3) . . ?
C3 C2 C1 120.4(4) . . ?
C3 C2 H2 119.8 . . ?
C1 C2 H2 119.8 . . ?
C2 C3 C4 120.2(5) . . ?
C2 C3 H3 119.9 . . ?
C4 C3 H3 119.9 . . ?
C5 C4 C3 120.6(4) . . ?
C5 C4 H4 119.7 . . ?
C3 C4 H4 119.7 . . ?
C4 C5 C6 119.4(4) . . ?
C4 C5 H5 120.3 . . ?
C6 C5 H5 120.3 . . ?
C5 C6 C1 120.5(4) . . ?
C5 C6 H6 119.7 . . ?
C1 C6 H6 119.7 . . ?
C12 C7 C8 120.5(4) . . ?
C12 C7 P1 118.3(3) . . ?
C8 C7 P1 121.2(4) . . ?
C9 C8 C7 118.8(5) . . ?
C9 C8 H8 120.6 . . ?
C7 C8 H8 120.6 . . ?
C8 C9 C10 120.2(5) . . ?
C8 C9 H9 119.9 . . ?
C10 C9 H9 119.9 . . ?
C11 C10 C9 120.4(5) . . ?
C11 C10 H10 119.8 . . ?
C9 C10 H10 119.8 . . ?
C10 C11 C12 121.1(6) . . ?
C10 C11 H11 119.4 . . ?
C12 C11 H11 119.4 . . ?
C11 C12 C7 119.1(5) . . ?
C11 C12 H12 120.5 . . ?
C7 C12 H12 120.5 . . ?
C18 C13 C14 119.2(4) . . ?
C18 C13 P1 119.4(3) . . ?
C14 C13 P1 121.4(3) . . ?
C15 C14 C13 120.5(4) . . ?
C15 C14 H14 119.7 . . ?
C13 C14 H14 119.7 . . ?
C14 C15 C16 119.8(4) . . ?
C14 C15 H15 120.1 . . ?
C16 C15 H15 120.1 . . ?
C17 C16 C15 120.3(4) . . ?
C17 C16 H16 119.8 . . ?
C15 C16 H16 119.8 . . ?
C16 C17 C18 120.0(4) . . ?
C16 C17 H17 120.0 . . ?
C18 C17 H17 120.0 . . ?
C13 C18 C17 120.0(4) . . ?
C13 C18 H18 120.0 . . ?
C17 C18 H18 120.0 . . ?
C20 C19 C24 119.4(4) . . ?
C20 C19 P2 119.7(3) . . ?
C24 C19 P2 120.8(3) . . ?
C19 C20 C21 119.1(5) . . ?
C19 C20 H20 120.4 . . ?
C21 C20 H20 120.4 . . ?
C22 C21 C20 120.6(5) . . ?
C22 C21 H21 119.7 . . ?
C20 C21 H21 119.7 . . ?
C21 C22 C23 120.7(5) . . ?
C21 C22 H22 119.7 . . ?
C23 C22 H22 119.7 . . ?
C22 C23 C24 120.3(5) . . ?
C22 C23 H23 119.8 . . ?
C24 C23 H23 119.8 . . ?
C23 C24 C19 119.9(5) . . ?
C23 C24 H24 120.0 . . ?
C19 C24 H24 120.0 . . ?
C26 C25 C30 119.0(4) . . ?
C26 C25 P2 120.1(3) . . ?
C30 C25 P2 120.7(3) . . ?
C25 C26 C27 119.4(4) . . ?
C25 C26 H26 120.3 . . ?
C27 C26 H26 120.3 . . ?
C28 C27 C26 120.9(5) . . ?
C28 C27 H27 119.5 . . ?
C26 C27 H27 119.5 . . ?
C27 C28 C29 120.0(5) . . ?
C27 C28 H28 120.0 . . ?
C29 C28 H28 120.0 . . ?
C28 C29 C30 120.5(4) . . ?
C28 C29 H29 119.8 . . ?
C30 C29 H29 119.8 . . ?
C29 C30 C25 120.3(4) . . ?
C29 C30 H30 119.9 . . ?
C25 C30 H30 119.9 . . ?
C36 C31 C32 119.0(4) . . ?
C36 C31 P2 119.2(3) . . ?
C32 C31 P2 121.8(3) . . ?
C33 C32 C31 120.4(4) . . ?
C33 C32 H32 119.8 . . ?
C31 C32 H32 119.8 . . ?
C34 C33 C32 119.8(4) . . ?
C34 C33 H33 120.1 . . ?
C32 C33 H33 120.1 . . ?
C33 C34 C35 120.4(4) . . ?
C33 C34 H34 119.8 . . ?
C35 C34 H34 119.8 . . ?
C34 C35 C36 120.0(4) . . ?
C34 C35 H35 120.0 . . ?
C36 C35 H35 120.0 . . ?
C35 C36 C31 120.4(4) . . ?
C35 C36 H36 119.8 . . ?
C31 C36 H36 119.8 . . ?
C42 C37 C38 121.5(4) . . ?
C42 C37 P3 125.4(3) . . ?
C38 C37 P3 113.1(3) . . ?
C39 C38 C37 119.6(4) . . ?
C39 C38 S1 122.9(3) . . ?
C37 C38 S1 117.5(3) . . ?
C40 C39 C38 116.7(3) . . ?
C40 C39 Si1 118.0(3) . . ?
C38 C39 Si1 125.2(3) . . ?
C41 C40 C39 123.9(4) . . ?
C41 C40 H40 118.0 . . ?
C39 C40 H40 118.0 . . ?
C40 C41 C42 119.5(4) . . ?
C40 C41 H41 120.3 . . ?
C42 C41 H41 120.3 . . ?
C41 C42 C37 118.7(4) . . ?
C41 C42 H42 120.6 . . ?
C37 C42 H42 120.6 . . ?
Si1 C43 H43A 109.5 . . ?
Si1 C43 H43B 109.5 . . ?
H43A C43 H43B 109.5 . . ?
Si1 C43 H43C 109.5 . . ?
H43A C43 H43C 109.5 . . ?
H43B C43 H43C 109.5 . . ?
Si1 C44 H44A 109.5 . . ?
Si1 C44 H44B 109.5 . . ?
H44A C44 H44B 109.5 . . ?
Si1 C44 H44C 109.5 . . ?
H44A C44 H44C 109.5 . . ?
H44B C44 H44C 109.5 . . ?
Si1 C45 H45A 109.5 . . ?
Si1 C45 H45B 109.5 . . ?
H45A C45 H45B 109.5 . . ?
Si1 C45 H45C 109.5 . . ?
H45A C45 H45C 109.5 . . ?
H45B C45 H45C 109.5 . . ?
C51 C46 C47 121.6(3) . . ?
C51 C46 P3 124.2(3) . . ?
C47 C46 P3 114.2(3) . . ?
C46 C47 C48 119.9(4) . . ?
C46 C47 S2 119.2(3) . . ?
C48 C47 S2 120.9(3) . . ?
C49 C48 C47 116.4(4) . . ?
C49 C48 Si2 119.7(3) . . ?
C47 C48 Si2 123.8(3) . . ?
C50 C49 C48 123.6(4) . . ?
C50 C49 H49 118.2 . . ?
C48 C49 H49 118.2 . . ?
C49 C50 C51 119.0(4) . . ?
C49 C50 H50 120.5 . . ?
C51 C50 H50 120.5 . . ?
C50 C51 C46 119.4(4) . . ?
C50 C51 H51 120.3 . . ?
C46 C51 H51 120.3 . . ?
Si2 C52 H52A 109.5 . . ?
Si2 C52 H52B 109.5 . . ?
H52A C52 H52B 109.5 . . ?
Si2 C52 H52C 109.5 . . ?
H52A C52 H52C 109.5 . . ?
H52B C52 H52C 109.5 . . ?
Si2 C53 H53A 109.5 . . ?
Si2 C53 H53B 109.5 . . ?
H53A C53 H53B 109.5 . . ?
Si2 C53 H53C 109.5 . . ?
H53A C53 H53C 109.5 . . ?
H53B C53 H53C 109.5 . . ?
Si2 C54 H54A 109.5 . . ?
Si2 C54 H54B 109.5 . . ?
H54A C54 H54B 109.5 . . ?
Si2 C54 H54C 109.5 . . ?
H54A C54 H54C 109.5 . . ?
H54B C54 H54C 109.5 . . ?
C60 C55 C56 121.4(3) . . ?
C60 C55 P3 123.3(3) . . ?
C56 C55 P3 115.1(3) . . ?
C55 C56 C57 119.5(3) . . ?
C55 C56 S3 119.7(3) . . ?
C57 C56 S3 120.8(3) . . ?
C58 C57 C56 116.8(4) . . ?
C58 C57 Si3 120.2(3) . . ?
C56 C57 Si3 122.9(3) . . ?
C59 C58 C57 123.4(3) . . ?
C59 C58 H58 118.3 . . ?
C57 C58 H58 118.3 . . ?
C58 C59 C60 119.3(4) . . ?
C58 C59 H59 120.3 . . ?
C60 C59 H59 120.3 . . ?
C59 C60 C55 119.5(4) . . ?
C59 C60 H60 120.3 . . ?
C55 C60 H60 120.3 . . ?
Si3 C61 H61A 109.5 . . ?
Si3 C61 H61B 109.5 . . ?
H61A C61 H61B 109.5 . . ?
Si3 C61 H61C 109.5 . . ?
H61A C61 H61C 109.5 . . ?
H61B C61 H61C 109.5 . . ?
Si3 C62 H62A 109.5 . . ?
Si3 C62 H62B 109.5 . . ?
H62A C62 H62B 109.5 . . ?
Si3 C62 H62C 109.5 . . ?
H62A C62 H62C 109.5 . . ?
H62B C62 H62C 109.5 . . ?
Si3 C63 H63A 109.5 . . ?
Si3 C63 H63B 109.5 . . ?
H63A C63 H63B 109.5 . . ?
Si3 C63 H63C 109.5 . . ?
H63A C63 H63C 109.5 . . ?
H63B C63 H63C 109.5 . . ?
O1 C64 O2 171.7(7) . . ?
C66 C65 O3 106.7(7) . . ?
C66 C65 H65A 110.4 . . ?
O3 C65 H65A 110.4 . . ?
C66 C65 H65B 110.4 . . ?
O3 C65 H65B 110.4 . . ?
H65A C65 H65B 108.6 . . ?
C65 C66 C67 104.4(7) . . ?
C65 C66 H66A 110.9 . . ?
C67 C66 H66A 110.9 . . ?
C65 C66 H66B 110.9 . . ?
C67 C66 H66B 110.9 . . ?
H66A C66 H66B 108.9 . . ?
C68 C67 C66 104.9(6) . . ?
C68 C67 H67A 110.8 . . ?
C66 C67 H67A 110.8 . . ?
C68 C67 H67B 110.8 . . ?
C66 C67 H67B 110.8 . . ?
H67A C67 H67B 108.8 . . ?
O3 C68 C67 104.0(6) . . ?
O3 C68 H68A 111.0 . . ?
C67 C68 H68A 111.0 . . ?
O3 C68 H68B 111.0 . . ?
C67 C68 H68B 111.0 . . ?
H68A C68 H68B 109.0 . . ?

_diffrn_measured_fraction_theta_max 0.993
_diffrn_reflns_theta_full        26.45
_diffrn_measured_fraction_theta_full 0.993
_refine_diff_density_max         2.517
_refine_diff_density_min         -0.964
_refine_diff_density_rms         0.111
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_100652lt
_audit_block_doi                 10.5517/cc1k5gz5
_database_code_depnum_ccdc_archive 'CCDC 1435237'
_audit_update_record             
;
2015-11-05 deposited with the CCDC.
2016-02-16 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C68 H74 N2 Ni O2 P3 S3 Si3'
_chemical_formula_weight         1283.36

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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'
S S 0.1246 0.1234 '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   'P b c a'
_symmetry_space_group_name_hall  '-P 2ac 2ab'

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                   27.5733(7)
_cell_length_b                   17.0409(5)
_cell_length_c                   27.8585(8)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     13090.0(6)
_cell_formula_units_Z            8
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9966
_cell_measurement_theta_min      2.3977
_cell_measurement_theta_max      26.3511

_exptl_crystal_description       Lump
_exptl_crystal_colour            Black
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.18
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_density_diffrn    1.302
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             5400
_exptl_absorpt_coefficient_mu    0.566
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.7083
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_process_details   'SADABS V2008/1 (Bruker AXS)'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean 8.333
_diffrn_reflns_number            113110
_diffrn_reflns_av_R_equivalents  0.0359
_diffrn_reflns_av_sigmaI/netI    0.0216
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_h_max       34
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_theta_min         1.46
_diffrn_reflns_theta_max         26.39
_reflns_number_total             13383
_reflns_number_gt                11346
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'APEX2 (Bruker AXS, 2010)'
_computing_cell_refinement       'SAINT V7.34A (Bruker AXS, 2006)'
_computing_data_reduction        'SAINT V7.34A (Bruker AXS, 2006)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  SHELXTL

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0743P)²+5.8765P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     SHELXL
_refine_ls_extinction_coef       0.00282(13)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         13383
_refine_ls_number_parameters     749
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0499
_refine_ls_R_factor_gt           0.0382
_refine_ls_wR_factor_ref         0.1276
_refine_ls_wR_factor_gt          0.1060
_refine_ls_goodness_of_fit_ref   1.171
_refine_ls_restrained_S_all      1.171
_refine_ls_shift/su_max          0.003
_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 0.289945(10) 0.468059(15) 0.182749(10) 0.01497(9) Uani 1 1 d . . .
P1 P 0.470261(19) 0.81006(3) 0.054889(19) 0.01535(13) Uani 1 1 d . . .
P2 P 0.560595(19) 0.74113(3) 0.094400(19) 0.01497(13) Uani 1 1 d . . .
P3 P 0.256454(19) 0.36149(3) 0.161752(19) 0.01373(12) Uani 1 1 d . . .
S1 S 0.25721(2) 0.52338(3) 0.115389(19) 0.01812(13) Uani 1 1 d . . .
S2 S 0.238753(19) 0.47043(3) 0.244532(19) 0.01826(13) Uani 1 1 d . . .
S3 S 0.358726(19) 0.40655(3) 0.156060(19) 0.01779(13) Uani 1 1 d . . .
Si1 Si 0.20877(3) 0.55749(4) 0.00684(3) 0.02655(16) Uani 1 1 d . . .
Si2 Si 0.14819(3) 0.44071(4) 0.32518(2) 0.02812(17) Uani 1 1 d . . .
Si3 Si 0.45182(2) 0.27222(4) 0.17280(2) 0.02210(15) Uani 1 1 d . . .
N1 N 0.52618(6) 0.79714(11) 0.06437(6) 0.0172(4) Uani 1 1 d . . .
N2 N 0.32380(7) 0.55998(11) 0.20578(7) 0.0226(4) Uani 1 1 d . . .
O1 O 0.38780(7) 0.58643(12) 0.26080(7) 0.0380(5) Uani 1 1 d . . .
O2 O 0.29511(9) 0.64218(14) 0.38677(7) 0.0507(6) Uani 1 1 d . . .
C1 C 0.43473(8) 0.72168(13) 0.05322(8) 0.0190(4) Uani 1 1 d . . .
C2 C 0.43857(9) 0.67057(15) 0.01382(9) 0.0269(5) Uani 1 1 d . . .
H2 H 0.4582 0.6842 -0.0129 0.032 Uiso 1 1 calc R . .
C3 C 0.41349(10) 0.60006(16) 0.01427(10) 0.0341(6) Uani 1 1 d . . .
H3 H 0.4158 0.5656 -0.0125 0.041 Uiso 1 1 calc R . .
C4 C 0.38514(9) 0.57933(16) 0.05329(10) 0.0326(6) Uani 1 1 d . . .
H4 H 0.3685 0.5305 0.0534 0.039 Uiso 1 1 calc R . .
C5 C 0.38099(9) 0.62939(15) 0.09218(9) 0.0273(5) Uani 1 1 d . . .
H5 H 0.3613 0.6152 0.1188 0.033 Uiso 1 1 calc R . .
C6 C 0.40577(8) 0.70053(14) 0.09222(8) 0.0211(5) Uani 1 1 d . . .
H6 H 0.4030 0.7349 0.1189 0.025 Uiso 1 1 calc R . .
C7 C 0.46461(8) 0.85600(13) -0.00294(8) 0.0191(4) Uani 1 1 d . . .
C8 C 0.42155(9) 0.85152(15) -0.02906(8) 0.0263(5) Uani 1 1 d . . .
H8 H 0.3947 0.8233 -0.0165 0.032 Uiso 1 1 calc R . .
C9 C 0.41797(9) 0.88841(16) -0.07342(9) 0.0313(6) Uani 1 1 d . . .
H9 H 0.3885 0.8858 -0.0911 0.038 Uiso 1 1 calc R . .
C10 C 0.45717(10) 0.92890(15) -0.09185(9) 0.0301(6) Uani 1 1 d . . .
H10 H 0.4547 0.9537 -0.1223 0.036 Uiso 1 1 calc R . .
C11 C 0.49992(10) 0.93354(15) -0.06617(9) 0.0290(5) Uani 1 1 d . . .
H11 H 0.5267 0.9617 -0.0790 0.035 Uiso 1 1 calc R . .
C12 C 0.50405(9) 0.89740(14) -0.02178(8) 0.0234(5) Uani 1 1 d . . .
H12 H 0.5335 0.9007 -0.0042 0.028 Uiso 1 1 calc R . .
C13 C 0.44378(7) 0.87327(13) 0.09969(8) 0.0166(4) Uani 1 1 d . . .
C14 C 0.39916(8) 0.91021(14) 0.09244(8) 0.0224(5) Uani 1 1 d . . .
H14 H 0.3823 0.9034 0.0630 0.027 Uiso 1 1 calc R . .
C15 C 0.37946(8) 0.95687(14) 0.12828(9) 0.0239(5) Uani 1 1 d . . .
H15 H 0.3493 0.9826 0.1231 0.029 Uiso 1 1 calc R . .
C16 C 0.40342(9) 0.96622(13) 0.17152(9) 0.0218(5) Uani 1 1 d . . .
H16 H 0.3893 0.9972 0.1962 0.026 Uiso 1 1 calc R . .
C17 C 0.44768(9) 0.93067(14) 0.17878(8) 0.0253(5) Uani 1 1 d . . .
H17 H 0.4643 0.9378 0.2083 0.030 Uiso 1 1 calc R . .
C18 C 0.46806(8) 0.88461(14) 0.14315(8) 0.0221(5) Uani 1 1 d . . .
H18 H 0.4987 0.8606 0.1483 0.027 Uiso 1 1 calc R . .
C19 C 0.59282(7) 0.79618(13) 0.13909(8) 0.0182(4) Uani 1 1 d . . .
C20 C 0.59574(8) 0.87767(14) 0.13423(8) 0.0233(5) Uani 1 1 d . . .
H20 H 0.5798 0.9032 0.1083 0.028 Uiso 1 1 calc R . .
C21 C 0.62209(9) 0.92135(16) 0.16739(9) 0.0304(6) Uani 1 1 d . . .
H21 H 0.6235 0.9769 0.1646 0.036 Uiso 1 1 calc R . .
C22 C 0.64613(9) 0.88416(17) 0.20422(9) 0.0332(6) Uani 1 1 d . . .
H22 H 0.6646 0.9141 0.2264 0.040 Uiso 1 1 calc R . .
C23 C 0.64356(9) 0.80349(17) 0.20922(9) 0.0297(6) Uani 1 1 d . . .
H23 H 0.6604 0.7784 0.2347 0.036 Uiso 1 1 calc R . .
C24 C 0.61646(8) 0.75916(15) 0.17718(8) 0.0231(5) Uani 1 1 d . . .
H24 H 0.6140 0.7039 0.1811 0.028 Uiso 1 1 calc R . .
C25 C 0.60419(8) 0.69781(13) 0.05449(8) 0.0189(4) Uani 1 1 d . . .
C26 C 0.64695(9) 0.66462(16) 0.07191(9) 0.0299(6) Uani 1 1 d . . .
H26 H 0.6542 0.6672 0.1052 0.036 Uiso 1 1 calc R . .
C27 C 0.67882(9) 0.62784(17) 0.04068(10) 0.0336(6) Uani 1 1 d . . .
H27 H 0.7081 0.6056 0.0525 0.040 Uiso 1 1 calc R . .
C28 C 0.66785(9) 0.62365(16) -0.00769(9) 0.0316(6) Uani 1 1 d . . .
H28 H 0.6893 0.5975 -0.0290 0.038 Uiso 1 1 calc R . .
C29 C 0.62624(10) 0.65704(18) -0.02504(10) 0.0379(7) Uani 1 1 d . . .
H29 H 0.6193 0.6547 -0.0584 0.045 Uiso 1 1 calc R . .
C30 C 0.59410(9) 0.69432(17) 0.00589(9) 0.0310(6) Uani 1 1 d . . .
H30 H 0.5653 0.7174 -0.0063 0.037 Uiso 1 1 calc R . .
C31 C 0.52943(8) 0.66170(13) 0.12387(8) 0.0200(5) Uani 1 1 d . . .
C32 C 0.52190(9) 0.59179(14) 0.09917(10) 0.0295(6) Uani 1 1 d . . .
H32 H 0.5369 0.5834 0.0689 0.035 Uiso 1 1 calc R . .
C33 C 0.49241(11) 0.53445(16) 0.11897(12) 0.0417(7) Uani 1 1 d . . .
H33 H 0.4872 0.4866 0.1022 0.050 Uiso 1 1 calc R . .
C34 C 0.47071(10) 0.54653(17) 0.16278(12) 0.0418(8) Uani 1 1 d . . .
H34 H 0.4501 0.5073 0.1758 0.050 Uiso 1 1 calc R . .
C35 C 0.47852(9) 0.61499(18) 0.18815(10) 0.0353(6) Uani 1 1 d . . .
H35 H 0.4640 0.6223 0.2187 0.042 Uiso 1 1 calc R . .
C36 C 0.50785(8) 0.67299(15) 0.16852(9) 0.0245(5) Uani 1 1 d . . .
H36 H 0.5132 0.7205 0.1856 0.029 Uiso 1 1 calc R . .
C37 C 0.23827(7) 0.36804(13) 0.09992(7) 0.0159(4) Uani 1 1 d . . .
C38 C 0.23577(7) 0.44445(13) 0.08106(8) 0.0151(4) Uani 1 1 d . . .
C39 C 0.21636(8) 0.45658(13) 0.03459(8) 0.0183(4) Uani 1 1 d . . .
C40 C 0.20245(8) 0.38991(14) 0.00863(8) 0.0199(5) Uani 1 1 d . . .
H40 H 0.1897 0.3967 -0.0228 0.024 Uiso 1 1 calc R . .
C41 C 0.20645(8) 0.31392(14) 0.02684(8) 0.0207(5) Uani 1 1 d . . .
H41 H 0.1970 0.2702 0.0079 0.025 Uiso 1 1 calc R . .
C42 C 0.22437(8) 0.30290(13) 0.07274(8) 0.0192(4) Uani 1 1 d . . .
H42 H 0.2272 0.2515 0.0857 0.023 Uiso 1 1 calc R . .
C43 C 0.16849(12) 0.62179(19) 0.04383(12) 0.0484(8) Uani 1 1 d . . .
H43A H 0.1690 0.6753 0.0309 0.073 Uiso 1 1 calc R . .
H43B H 0.1801 0.6224 0.0771 0.073 Uiso 1 1 calc R . .
H43C H 0.1353 0.6014 0.0429 0.073 Uiso 1 1 calc R . .
C44 C 0.26907(11) 0.60450(17) -0.00236(10) 0.0389(7) Uani 1 1 d . . .
H44A H 0.2910 0.5672 -0.0180 0.058 Uiso 1 1 calc R . .
H44B H 0.2826 0.6199 0.0288 0.058 Uiso 1 1 calc R . .
H44C H 0.2653 0.6511 -0.0226 0.058 Uiso 1 1 calc R . .
C45 C 0.18029(12) 0.54482(18) -0.05332(10) 0.0414(7) Uani 1 1 d . . .
H45A H 0.1474 0.5241 -0.0495 0.062 Uiso 1 1 calc R . .
H45B H 0.1996 0.5081 -0.0724 0.062 Uiso 1 1 calc R . .
H45C H 0.1789 0.5957 -0.0697 0.062 Uiso 1 1 calc R . .
C46 C 0.20345(7) 0.34185(13) 0.19763(8) 0.0165(4) Uani 1 1 d . . .
C47 C 0.19799(7) 0.39128(13) 0.23752(8) 0.0168(4) Uani 1 1 d . . .
C48 C 0.15991(8) 0.37774(13) 0.27087(8) 0.0207(5) Uani 1 1 d . . .
C49 C 0.12861(8) 0.31512(14) 0.26075(8) 0.0231(5) Uani 1 1 d . . .
H49 H 0.1031 0.3042 0.2827 0.028 Uiso 1 1 calc R . .
C50 C 0.13292(8) 0.26812(14) 0.22020(9) 0.0232(5) Uani 1 1 d . . .
H50 H 0.1102 0.2274 0.2142 0.028 Uiso 1 1 calc R . .
C51 C 0.17081(8) 0.28155(13) 0.18859(8) 0.0200(5) Uani 1 1 d . . .
H51 H 0.1744 0.2497 0.1608 0.024 Uiso 1 1 calc R . .
C52 C 0.12466(12) 0.53808(17) 0.30544(11) 0.0436(7) Uani 1 1 d . . .
H52A H 0.1183 0.5709 0.3336 0.065 Uiso 1 1 calc R . .
H52B H 0.0945 0.5307 0.2873 0.065 Uiso 1 1 calc R . .
H52C H 0.1488 0.5638 0.2850 0.065 Uiso 1 1 calc R . .
C53 C 0.20242(11) 0.4536(2) 0.36431(11) 0.0445(7) Uani 1 1 d . . .
H53A H 0.2283 0.4794 0.3461 0.067 Uiso 1 1 calc R . .
H53B H 0.2137 0.4021 0.3753 0.067 Uiso 1 1 calc R . .
H53C H 0.1938 0.4859 0.3921 0.067 Uiso 1 1 calc R . .
C54 C 0.09944(11) 0.39361(19) 0.36195(10) 0.0411(7) Uani 1 1 d . . .
H54A H 0.1090 0.3398 0.3699 0.062 Uiso 1 1 calc R . .
H54B H 0.0691 0.3928 0.3436 0.062 Uiso 1 1 calc R . .
H54C H 0.0947 0.4236 0.3916 0.062 Uiso 1 1 calc R . .
C55 C 0.29853(7) 0.28190(13) 0.17014(7) 0.0154(4) Uani 1 1 d . . .
C56 C 0.34729(8) 0.30590(12) 0.16608(7) 0.0163(4) Uani 1 1 d . . .
C57 C 0.38475(8) 0.24982(13) 0.17217(8) 0.0191(4) Uani 1 1 d . . .
C58 C 0.37030(8) 0.17239(14) 0.18175(8) 0.0227(5) Uani 1 1 d . . .
H58 H 0.3948 0.1336 0.1855 0.027 Uiso 1 1 calc R . .
C59 C 0.32232(9) 0.14945(13) 0.18606(8) 0.0227(5) Uani 1 1 d . . .
H59 H 0.3145 0.0963 0.1929 0.027 Uiso 1 1 calc R . .
C60 C 0.28589(8) 0.20435(13) 0.18041(8) 0.0179(4) Uani 1 1 d . . .
H60 H 0.2528 0.1896 0.1835 0.021 Uiso 1 1 calc R . .
C61 C 0.46734(9) 0.34573(15) 0.22034(9) 0.0278(5) Uani 1 1 d . . .
H61A H 0.4635 0.3217 0.2521 0.042 Uiso 1 1 calc R . .
H61B H 0.4457 0.3911 0.2176 0.042 Uiso 1 1 calc R . .
H61C H 0.5010 0.3629 0.2162 0.042 Uiso 1 1 calc R . .
C62 C 0.47205(9) 0.30508(17) 0.11205(9) 0.0324(6) Uani 1 1 d . . .
H62A H 0.5069 0.3160 0.1127 0.049 Uiso 1 1 calc R . .
H62B H 0.4544 0.3528 0.1030 0.049 Uiso 1 1 calc R . .
H62C H 0.4654 0.2637 0.0885 0.049 Uiso 1 1 calc R . .
C63 C 0.48478(9) 0.17991(16) 0.18779(10) 0.0335(6) Uani 1 1 d . . .
H63A H 0.4767 0.1394 0.1641 0.050 Uiso 1 1 calc R . .
H63B H 0.4752 0.1621 0.2199 0.050 Uiso 1 1 calc R . .
H63C H 0.5198 0.1897 0.1872 0.050 Uiso 1 1 calc R . .
C64 C 0.35555(8) 0.57147(13) 0.23336(9) 0.0227(5) Uani 1 1 d . . .
C65 C 0.28477(15) 0.7225(2) 0.38860(13) 0.0588(9) Uani 1 1 d . . .
H65A H 0.3152 0.7532 0.3897 0.071 Uiso 1 1 calc R . .
H65B H 0.2655 0.7348 0.4176 0.071 Uiso 1 1 calc R . .
C66 C 0.25656(13) 0.7426(2) 0.34428(12) 0.0519(8) Uani 1 1 d . . .
H66A H 0.2706 0.7892 0.3282 0.062 Uiso 1 1 calc R . .
H66B H 0.2222 0.7536 0.3522 0.062 Uiso 1 1 calc R . .
C67 C 0.26064(16) 0.6713(2) 0.31291(14) 0.0683(12) Uani 1 1 d . . .
H67A H 0.2292 0.6437 0.3105 0.082 Uiso 1 1 calc R . .
H67B H 0.2718 0.6856 0.2803 0.082 Uiso 1 1 calc R . .
C68 C 0.29727(15) 0.6222(2) 0.33798(13) 0.0605(10) Uani 1 1 d . . .
H68A H 0.2899 0.5658 0.3335 0.073 Uiso 1 1 calc R . .
H68B H 0.3301 0.6327 0.3250 0.073 Uiso 1 1 calc R . .


_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 N2 1.9330(19) . ?
Ni1 P3 2.1197(6) . ?
Ni1 S2 2.2263(6) . ?
Ni1 S1 2.2857(6) . ?
Ni1 S3 2.2909(6) . ?
P1 N1 1.5797(18) . ?
P1 C1 1.797(2) . ?
P1 C7 1.798(2) . ?
P1 C13 1.803(2) . ?
P2 N1 1.5849(18) . ?
P2 C19 1.794(2) . ?
P2 C25 1.796(2) . ?
P2 C31 1.801(2) . ?
P3 C37 1.797(2) . ?
P3 C55 1.800(2) . ?
P3 C46 1.802(2) . ?
S1 C38 1.753(2) . ?
S2 C47 1.767(2) . ?
S3 C56 1.766(2) . ?
Si1 C44 1.863(3) . ?
Si1 C45 1.863(3) . ?
Si1 C43 1.870(3) . ?
Si1 C39 1.897(2) . ?
Si2 C53 1.863(3) . ?
Si2 C52 1.865(3) . ?
Si2 C54 1.871(3) . ?
Si2 C48 1.883(2) . ?
Si3 C63 1.864(3) . ?
Si3 C62 1.868(3) . ?
Si3 C61 1.873(3) . ?
Si3 C57 1.888(2) . ?
N2 C64 1.181(3) . ?
O1 C64 1.200(3) . ?
O2 C65 1.399(4) . ?
O2 C68 1.403(4) . ?
C1 C6 1.396(3) . ?
C1 C2 1.405(3) . ?
C2 C3 1.386(4) . ?
C2 H2 0.9500 . ?
C3 C4 1.385(4) . ?
C3 H3 0.9500 . ?
C4 C5 1.384(4) . ?
C4 H4 0.9500 . ?
C5 C6 1.392(3) . ?
C5 H5 0.9500 . ?
C6 H6 0.9500 . ?
C7 C8 1.395(3) . ?
C7 C12 1.399(3) . ?
C8 C9 1.390(3) . ?
C8 H8 0.9500 . ?
C9 C10 1.381(4) . ?
C9 H9 0.9500 . ?
C10 C11 1.381(4) . ?
C10 H10 0.9500 . ?
C11 C12 1.386(3) . ?
C11 H11 0.9500 . ?
C12 H12 0.9500 . ?
C13 C14 1.397(3) . ?
C13 C18 1.397(3) . ?
C14 C15 1.387(3) . ?
C14 H14 0.9500 . ?
C15 C16 1.383(3) . ?
C15 H15 0.9500 . ?
C16 C17 1.377(3) . ?
C16 H16 0.9500 . ?
C17 C18 1.384(3) . ?
C17 H17 0.9500 . ?
C18 H18 0.9500 . ?
C19 C24 1.396(3) . ?
C19 C20 1.398(3) . ?
C20 C21 1.391(3) . ?
C20 H20 0.9500 . ?
C21 C22 1.376(4) . ?
C21 H21 0.9500 . ?
C22 C23 1.384(4) . ?
C22 H22 0.9500 . ?
C23 C24 1.388(3) . ?
C23 H23 0.9500 . ?
C24 H24 0.9500 . ?
C25 C30 1.383(3) . ?
C25 C26 1.395(3) . ?
C26 C27 1.386(3) . ?
C26 H26 0.9500 . ?
C27 C28 1.383(4) . ?
C27 H27 0.9500 . ?
C28 C29 1.369(4) . ?
C28 H28 0.9500 . ?
C29 C30 1.390(3) . ?
C29 H29 0.9500 . ?
C30 H30 0.9500 . ?
C31 C32 1.391(3) . ?
C31 C36 1.392(3) . ?
C32 C33 1.386(4) . ?
C32 H32 0.9500 . ?
C33 C34 1.375(5) . ?
C33 H33 0.9500 . ?
C34 C35 1.381(4) . ?
C34 H34 0.9500 . ?
C35 C36 1.389(3) . ?
C35 H35 0.9500 . ?
C36 H36 0.9500 . ?
C37 C42 1.397(3) . ?
C37 C38 1.406(3) . ?
C38 C39 1.416(3) . ?
C39 C40 1.400(3) . ?
C40 C41 1.395(3) . ?
C40 H40 0.9500 . ?
C41 C42 1.384(3) . ?
C41 H41 0.9500 . ?
C42 H42 0.9500 . ?
C43 H43A 0.9800 . ?
C43 H43B 0.9800 . ?
C43 H43C 0.9800 . ?
C44 H44A 0.9800 . ?
C44 H44B 0.9800 . ?
C44 H44C 0.9800 . ?
C45 H45A 0.9800 . ?
C45 H45B 0.9800 . ?
C45 H45C 0.9800 . ?
C46 C51 1.389(3) . ?
C46 C47 1.403(3) . ?
C47 C48 1.421(3) . ?
C48 C49 1.401(3) . ?
C49 C50 1.390(3) . ?
C49 H49 0.9500 . ?
C50 C51 1.386(3) . ?
C50 H50 0.9500 . ?
C51 H51 0.9500 . ?
C52 H52A 0.9800 . ?
C52 H52B 0.9800 . ?
C52 H52C 0.9800 . ?
C53 H53A 0.9800 . ?
C53 H53B 0.9800 . ?
C53 H53C 0.9800 . ?
C54 H54A 0.9800 . ?
C54 H54B 0.9800 . ?
C54 H54C 0.9800 . ?
C55 C60 1.396(3) . ?
C55 C56 1.410(3) . ?
C56 C57 1.417(3) . ?
C57 C58 1.404(3) . ?
C58 C59 1.385(3) . ?
C58 H58 0.9500 . ?
C59 C60 1.382(3) . ?
C59 H59 0.9500 . ?
C60 H60 0.9500 . ?
C61 H61A 0.9800 . ?
C61 H61B 0.9800 . ?
C61 H61C 0.9800 . ?
C62 H62A 0.9800 . ?
C62 H62B 0.9800 . ?
C62 H62C 0.9800 . ?
C63 H63A 0.9800 . ?
C63 H63B 0.9800 . ?
C63 H63C 0.9800 . ?
C65 C66 1.499(5) . ?
C65 H65A 0.9900 . ?
C65 H65B 0.9900 . ?
C66 C67 1.501(5) . ?
C66 H66A 0.9900 . ?
C66 H66B 0.9900 . ?
C67 C68 1.486(5) . ?
C67 H67A 0.9900 . ?
C67 H67B 0.9900 . ?
C68 H68A 0.9900 . ?
C68 H68B 0.9900 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N2 Ni1 P3 175.03(6) . . ?
N2 Ni1 S2 92.00(6) . . ?
P3 Ni1 S2 87.29(2) . . ?
N2 Ni1 S1 97.41(6) . . ?
P3 Ni1 S1 87.41(2) . . ?
S2 Ni1 S1 112.14(2) . . ?
N2 Ni1 S3 94.51(6) . . ?
P3 Ni1 S3 83.06(2) . . ?
S2 Ni1 S3 141.64(2) . . ?
S1 Ni1 S3 104.42(2) . . ?
N1 P1 C1 114.81(10) . . ?
N1 P1 C7 107.16(10) . . ?
C1 P1 C7 107.12(11) . . ?
N1 P1 C13 111.27(10) . . ?
C1 P1 C13 107.33(10) . . ?
C7 P1 C13 108.97(10) . . ?
N1 P2 C19 110.36(10) . . ?
N1 P2 C25 108.75(10) . . ?
C19 P2 C25 108.24(10) . . ?
N1 P2 C31 114.05(10) . . ?
C19 P2 C31 108.23(10) . . ?
C25 P2 C31 107.02(11) . . ?
C37 P3 C55 110.54(10) . . ?
C37 P3 C46 108.47(10) . . ?
C55 P3 C46 108.11(10) . . ?
C37 P3 Ni1 109.43(7) . . ?
C55 P3 Ni1 109.20(7) . . ?
C46 P3 Ni1 111.06(7) . . ?
C38 S1 Ni1 105.34(7) . . ?
C47 S2 Ni1 107.70(7) . . ?
C56 S3 Ni1 104.19(7) . . ?
C44 Si1 C45 107.59(13) . . ?
C44 Si1 C43 110.72(15) . . ?
C45 Si1 C43 108.26(15) . . ?
C44 Si1 C39 110.32(12) . . ?
C45 Si1 C39 107.94(12) . . ?
C43 Si1 C39 111.85(13) . . ?
C53 Si2 C52 110.31(16) . . ?
C53 Si2 C54 107.86(14) . . ?
C52 Si2 C54 107.06(14) . . ?
C53 Si2 C48 113.53(12) . . ?
C52 Si2 C48 109.26(12) . . ?
C54 Si2 C48 108.59(12) . . ?
C63 Si3 C62 108.08(13) . . ?
C63 Si3 C61 107.13(12) . . ?
C62 Si3 C61 111.85(12) . . ?
C63 Si3 C57 108.00(11) . . ?
C62 Si3 C57 110.17(11) . . ?
C61 Si3 C57 111.44(10) . . ?
P1 N1 P2 139.16(12) . . ?
C64 N2 Ni1 135.08(18) . . ?
C65 O2 C68 106.3(3) . . ?
C6 C1 C2 119.4(2) . . ?
C6 C1 P1 120.53(17) . . ?
C2 C1 P1 119.90(17) . . ?
C3 C2 C1 119.5(2) . . ?
C3 C2 H2 120.2 . . ?
C1 C2 H2 120.2 . . ?
C4 C3 C2 120.7(2) . . ?
C4 C3 H3 119.7 . . ?
C2 C3 H3 119.7 . . ?
C5 C4 C3 120.3(2) . . ?
C5 C4 H4 119.9 . . ?
C3 C4 H4 119.9 . . ?
C4 C5 C6 119.8(2) . . ?
C4 C5 H5 120.1 . . ?
C6 C5 H5 120.1 . . ?
C5 C6 C1 120.3(2) . . ?
C5 C6 H6 119.8 . . ?
C1 C6 H6 119.8 . . ?
C8 C7 C12 119.6(2) . . ?
C8 C7 P1 121.16(18) . . ?
C12 C7 P1 119.24(17) . . ?
C9 C8 C7 120.0(2) . . ?
C9 C8 H8 120.0 . . ?
C7 C8 H8 120.0 . . ?
C10 C9 C8 120.1(2) . . ?
C10 C9 H9 120.0 . . ?
C8 C9 H9 120.0 . . ?
C9 C10 C11 120.2(2) . . ?
C9 C10 H10 119.9 . . ?
C11 C10 H10 119.9 . . ?
C10 C11 C12 120.5(2) . . ?
C10 C11 H11 119.8 . . ?
C12 C11 H11 119.8 . . ?
C11 C12 C7 119.7(2) . . ?
C11 C12 H12 120.2 . . ?
C7 C12 H12 120.2 . . ?
C14 C13 C18 119.0(2) . . ?
C14 C13 P1 121.72(17) . . ?
C18 C13 P1 119.24(16) . . ?
C15 C14 C13 119.9(2) . . ?
C15 C14 H14 120.0 . . ?
C13 C14 H14 120.0 . . ?
C16 C15 C14 120.4(2) . . ?
C16 C15 H15 119.8 . . ?
C14 C15 H15 119.8 . . ?
C17 C16 C15 120.0(2) . . ?
C17 C16 H16 120.0 . . ?
C15 C16 H16 120.0 . . ?
C16 C17 C18 120.2(2) . . ?
C16 C17 H17 119.9 . . ?
C18 C17 H17 119.9 . . ?
C17 C18 C13 120.3(2) . . ?
C17 C18 H18 119.8 . . ?
C13 C18 H18 119.8 . . ?
C24 C19 C20 119.7(2) . . ?
C24 C19 P2 121.49(18) . . ?
C20 C19 P2 118.74(17) . . ?
C21 C20 C19 119.8(2) . . ?
C21 C20 H20 120.1 . . ?
C19 C20 H20 120.1 . . ?
C22 C21 C20 120.0(2) . . ?
C22 C21 H21 120.0 . . ?
C20 C21 H21 120.0 . . ?
C21 C22 C23 120.5(2) . . ?
C21 C22 H22 119.7 . . ?
C23 C22 H22 119.7 . . ?
C22 C23 C24 120.2(2) . . ?
C22 C23 H23 119.9 . . ?
C24 C23 H23 119.9 . . ?
C23 C24 C19 119.6(2) . . ?
C23 C24 H24 120.2 . . ?
C19 C24 H24 120.2 . . ?
C30 C25 C26 119.5(2) . . ?
C30 C25 P2 119.26(17) . . ?
C26 C25 P2 121.14(17) . . ?
C27 C26 C25 120.1(2) . . ?
C27 C26 H26 120.0 . . ?
C25 C26 H26 120.0 . . ?
C28 C27 C26 119.8(2) . . ?
C28 C27 H27 120.1 . . ?
C26 C27 H27 120.1 . . ?
C29 C28 C27 120.4(2) . . ?
C29 C28 H28 119.8 . . ?
C27 C28 H28 119.8 . . ?
C28 C29 C30 120.4(2) . . ?
C28 C29 H29 119.8 . . ?
C30 C29 H29 119.8 . . ?
C25 C30 C29 119.9(2) . . ?
C25 C30 H30 120.1 . . ?
C29 C30 H30 120.1 . . ?
C32 C31 C36 119.8(2) . . ?
C32 C31 P2 119.29(19) . . ?
C36 C31 P2 120.49(18) . . ?
C33 C32 C31 119.6(3) . . ?
C33 C32 H32 120.2 . . ?
C31 C32 H32 120.2 . . ?
C34 C33 C32 120.2(3) . . ?
C34 C33 H33 119.9 . . ?
C32 C33 H33 119.9 . . ?
C33 C34 C35 120.9(2) . . ?
C33 C34 H34 119.6 . . ?
C35 C34 H34 119.6 . . ?
C34 C35 C36 119.4(3) . . ?
C34 C35 H35 120.3 . . ?
C36 C35 H35 120.3 . . ?
C35 C36 C31 120.2(2) . . ?
C35 C36 H36 119.9 . . ?
C31 C36 H36 119.9 . . ?
C42 C37 C38 121.32(19) . . ?
C42 C37 P3 123.13(17) . . ?
C38 C37 P3 115.43(16) . . ?
C37 C38 C39 119.70(19) . . ?
C37 C38 S1 119.35(16) . . ?
C39 C38 S1 120.95(17) . . ?
C40 C39 C38 117.2(2) . . ?
C40 C39 Si1 119.65(17) . . ?
C38 C39 Si1 123.13(17) . . ?
C41 C40 C39 122.9(2) . . ?
C41 C40 H40 118.5 . . ?
C39 C40 H40 118.5 . . ?
C42 C41 C40 119.4(2) . . ?
C42 C41 H41 120.3 . . ?
C40 C41 H41 120.3 . . ?
C41 C42 C37 119.4(2) . . ?
C41 C42 H42 120.3 . . ?
C37 C42 H42 120.3 . . ?
Si1 C43 H43A 109.5 . . ?
Si1 C43 H43B 109.5 . . ?
H43A C43 H43B 109.5 . . ?
Si1 C43 H43C 109.5 . . ?
H43A C43 H43C 109.5 . . ?
H43B C43 H43C 109.5 . . ?
Si1 C44 H44A 109.5 . . ?
Si1 C44 H44B 109.5 . . ?
H44A C44 H44B 109.5 . . ?
Si1 C44 H44C 109.5 . . ?
H44A C44 H44C 109.5 . . ?
H44B C44 H44C 109.5 . . ?
Si1 C45 H45A 109.5 . . ?
Si1 C45 H45B 109.5 . . ?
H45A C45 H45B 109.5 . . ?
Si1 C45 H45C 109.5 . . ?
H45A C45 H45C 109.5 . . ?
H45B C45 H45C 109.5 . . ?
C51 C46 C47 121.2(2) . . ?
C51 C46 P3 124.22(17) . . ?
C47 C46 P3 114.52(16) . . ?
C46 C47 C48 120.0(2) . . ?
C46 C47 S2 118.54(16) . . ?
C48 C47 S2 121.45(17) . . ?
C49 C48 C47 116.6(2) . . ?
C49 C48 Si2 119.34(17) . . ?
C47 C48 Si2 124.04(17) . . ?
C50 C49 C48 123.4(2) . . ?
C50 C49 H49 118.3 . . ?
C48 C49 H49 118.3 . . ?
C51 C50 C49 119.1(2) . . ?
C51 C50 H50 120.5 . . ?
C49 C50 H50 120.5 . . ?
C50 C51 C46 119.7(2) . . ?
C50 C51 H51 120.1 . . ?
C46 C51 H51 120.1 . . ?
Si2 C52 H52A 109.5 . . ?
Si2 C52 H52B 109.5 . . ?
H52A C52 H52B 109.5 . . ?
Si2 C52 H52C 109.5 . . ?
H52A C52 H52C 109.5 . . ?
H52B C52 H52C 109.5 . . ?
Si2 C53 H53A 109.5 . . ?
Si2 C53 H53B 109.5 . . ?
H53A C53 H53B 109.5 . . ?
Si2 C53 H53C 109.5 . . ?
H53A C53 H53C 109.5 . . ?
H53B C53 H53C 109.5 . . ?
Si2 C54 H54A 109.5 . . ?
Si2 C54 H54B 109.5 . . ?
H54A C54 H54B 109.5 . . ?
Si2 C54 H54C 109.5 . . ?
H54A C54 H54C 109.5 . . ?
H54B C54 H54C 109.5 . . ?
C60 C55 C56 121.9(2) . . ?
C60 C55 P3 125.36(16) . . ?
C56 C55 P3 112.68(16) . . ?
C55 C56 C57 119.3(2) . . ?
C55 C56 S3 117.69(16) . . ?
C57 C56 S3 122.93(16) . . ?
C58 C57 C56 116.7(2) . . ?
C58 C57 Si3 117.79(17) . . ?
C56 C57 Si3 125.34(17) . . ?
C59 C58 C57 123.6(2) . . ?
C59 C58 H58 118.2 . . ?
C57 C58 H58 118.2 . . ?
C60 C59 C58 119.6(2) . . ?
C60 C59 H59 120.2 . . ?
C58 C59 H59 120.2 . . ?
C59 C60 C55 118.9(2) . . ?
C59 C60 H60 120.6 . . ?
C55 C60 H60 120.6 . . ?
Si3 C61 H61A 109.5 . . ?
Si3 C61 H61B 109.5 . . ?
H61A C61 H61B 109.5 . . ?
Si3 C61 H61C 109.5 . . ?
H61A C61 H61C 109.5 . . ?
H61B C61 H61C 109.5 . . ?
Si3 C62 H62A 109.5 . . ?
Si3 C62 H62B 109.5 . . ?
H62A C62 H62B 109.5 . . ?
Si3 C62 H62C 109.5 . . ?
H62A C62 H62C 109.5 . . ?
H62B C62 H62C 109.5 . . ?
Si3 C63 H63A 109.5 . . ?
Si3 C63 H63B 109.5 . . ?
H63A C63 H63B 109.5 . . ?
Si3 C63 H63C 109.5 . . ?
H63A C63 H63C 109.5 . . ?
H63B C63 H63C 109.5 . . ?
N2 C64 O1 177.2(3) . . ?
O2 C65 C66 107.4(3) . . ?
O2 C65 H65A 110.2 . . ?
C66 C65 H65A 110.2 . . ?
O2 C65 H65B 110.2 . . ?
C66 C65 H65B 110.2 . . ?
H65A C65 H65B 108.5 . . ?
C65 C66 C67 104.8(3) . . ?
C65 C66 H66A 110.8 . . ?
C67 C66 H66A 110.8 . . ?
C65 C66 H66B 110.8 . . ?
C67 C66 H66B 110.8 . . ?
H66A C66 H66B 108.9 . . ?
C68 C67 C66 103.5(3) . . ?
C68 C67 H67A 111.1 . . ?
C66 C67 H67A 111.1 . . ?
C68 C67 H67B 111.1 . . ?
C66 C67 H67B 111.1 . . ?
H67A C67 H67B 109.0 . . ?
O2 C68 C67 106.8(3) . . ?
O2 C68 H68A 110.4 . . ?
C67 C68 H68A 110.4 . . ?
O2 C68 H68B 110.4 . . ?
C67 C68 H68B 110.4 . . ?
H68A C68 H68B 108.6 . . ?

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        26.39
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         0.829
_refine_diff_density_min         -0.629
_refine_diff_density_rms         0.190
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_a11745
_audit_block_doi                 10.5517/cc1k5h07
_database_code_depnum_ccdc_archive 'CCDC 1435238'
_audit_update_record             
;
2015-11-05 deposited with the CCDC.
2016-02-16 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C67 H78 N3 Ni O P3 S3 Si3'
_chemical_formula_sum            'C67 H78 N3 Ni O P3 S3 Si3'
_chemical_formula_weight         1273.39

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 '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'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21/n'

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   14.3160(4)
_cell_length_b                   26.0756(6)
_cell_length_c                   18.0992(4)
_cell_angle_alpha                90.00
_cell_angle_beta                 97.069(2)
_cell_angle_gamma                90.00
_cell_volume                     6705.0(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    200(2)
_cell_measurement_reflns_used    0
_cell_measurement_theta_min      0
_cell_measurement_theta_max      0

_exptl_crystal_description       prism
_exptl_crystal_colour            brown(dark)
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.22
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.261
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2688
_exptl_absorpt_coefficient_mu    0.551
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.8348
_exptl_absorpt_correction_T_max  0.8884
_exptl_absorpt_process_details   ?

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      200(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  'CCD area detector'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            38140
_diffrn_reflns_av_R_equivalents  0.0348
_diffrn_reflns_av_sigmaI/netI    0.0420
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         1.56
_diffrn_reflns_theta_max         25.07
_reflns_number_total             11712
_reflns_number_gt                9139
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1986)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'

_refine_special_details          
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and
 goodness of fit S are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The threshold expression of
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
 not relevant to the choice of reflections for refinement.  R-factors based
 on F² are statistically about twice as large as those based on F, and R-
 factors based on ALL data will be even larger.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0860P)²+1.5042P] where P=(Fo²+2Fc²)/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         11712
_refine_ls_number_parameters     730
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0547
_refine_ls_R_factor_gt           0.0398
_refine_ls_wR_factor_ref         0.1229
_refine_ls_wR_factor_gt          0.1124
_refine_ls_goodness_of_fit_ref   0.923
_refine_ls_restrained_S_all      0.923
_refine_ls_shift/su_max          0.038
_refine_ls_shift/su_mean         0.001

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
C1 C 1.02473(16) 0.19242(10) 0.14236(13) 0.0263(5) Uani 1 1 d . . .
C2 C 1.03710(16) 0.18899(9) 0.06624(13) 0.0258(5) Uani 1 1 d . . .
C3 C 1.11949(16) 0.20991(10) 0.04156(14) 0.0286(5) Uani 1 1 d . . .
C4 C 1.1370(2) 0.14450(13) -0.10034(19) 0.0541(9) Uani 1 1 d . . .
H4A H 1.1838 0.1232 -0.0704 0.081 Uiso 1 1 calc R . .
H4B H 1.1523 0.1464 -0.1516 0.081 Uiso 1 1 calc R . .
H4C H 1.0744 0.1293 -0.1002 0.081 Uiso 1 1 calc R . .
C5 C 1.2576(2) 0.23834(16) -0.0665(2) 0.0665(11) Uani 1 1 d . . .
H5A H 1.3056 0.2174 -0.0373 0.100 Uiso 1 1 calc R . .
H5B H 1.2602 0.2734 -0.0469 0.100 Uiso 1 1 calc R . .
H5C H 1.2695 0.2388 -0.1187 0.100 Uiso 1 1 calc R . .
C6 C 1.0490(3) 0.25158(15) -0.1156(2) 0.0685(10) Uani 1 1 d . . .
H6A H 1.0504 0.2860 -0.0939 0.103 Uiso 1 1 calc R . .
H6B H 0.9862 0.2367 -0.1151 0.103 Uiso 1 1 calc R . .
H6C H 1.0636 0.2537 -0.1670 0.103 Uiso 1 1 calc R . .
C7 C 1.18643(17) 0.23136(10) 0.09531(15) 0.0337(6) Uani 1 1 d . . .
H7 H 1.2426 0.2449 0.0799 0.040 Uiso 1 1 calc R . .
C8 C 1.17476(17) 0.23382(10) 0.16992(15) 0.0346(6) Uani 1 1 d . . .
H8 H 1.2223 0.2485 0.2048 0.041 Uiso 1 1 calc R . .
C9 C 1.09361(17) 0.21472(10) 0.19323(15) 0.0324(6) Uani 1 1 d . . .
H9 H 1.0846 0.2168 0.2443 0.039 Uiso 1 1 calc R . .
C10 C 0.93858(16) 0.13374(10) 0.25404(14) 0.0287(6) Uani 1 1 d . . .
C11 C 0.94003(15) 0.07996(10) 0.24702(13) 0.0250(5) Uani 1 1 d . . .
C12 C 0.95748(16) 0.04858(10) 0.31057(14) 0.0307(6) Uani 1 1 d . . .
C13 C 1.0369(2) -0.05551(13) 0.26112(19) 0.0560(9) Uani 1 1 d . . .
H13A H 1.0992 -0.0448 0.2846 0.084 Uiso 1 1 calc R . .
H13B H 1.0295 -0.0458 0.2084 0.084 Uiso 1 1 calc R . .
H13C H 1.0309 -0.0928 0.2654 0.084 Uiso 1 1 calc R . .
C14 C 0.8234(2) -0.04207(12) 0.2662(2) 0.0528(8) Uani 1 1 d . . .
H14A H 0.7766 -0.0246 0.2925 0.079 Uiso 1 1 calc R . .
H14B H 0.8157 -0.0793 0.2703 0.079 Uiso 1 1 calc R . .
H14C H 0.8144 -0.0321 0.2136 0.079 Uiso 1 1 calc R . .
C15 C 0.9562(2) -0.04731(13) 0.40682(17) 0.0540(8) Uani 1 1 d . . .
H15A H 0.9084 -0.0311 0.4334 0.081 Uiso 1 1 calc R . .
H15B H 1.0190 -0.0387 0.4317 0.081 Uiso 1 1 calc R . .
H15C H 0.9477 -0.0846 0.4068 0.081 Uiso 1 1 calc R . .
C16 C 0.97717(18) 0.07337(12) 0.37904(15) 0.0368(6) Uani 1 1 d . . .
H16 H 0.9926 0.0532 0.4225 0.044 Uiso 1 1 calc R . .
C17 C 0.9751(2) 0.12630(12) 0.38611(15) 0.0430(7) Uani 1 1 d . . .
H17 H 0.9879 0.1416 0.4339 0.052 Uiso 1 1 calc R . .
C18 C 0.95445(19) 0.15673(11) 0.32423(15) 0.0383(7) Uani 1 1 d . . .
H18 H 0.9510 0.1929 0.3291 0.046 Uiso 1 1 calc R . .
C19 C 0.83618(17) 0.21975(10) 0.18068(14) 0.0294(6) Uani 1 1 d . . .
C20 C 0.74383(17) 0.21484(9) 0.14474(14) 0.0280(5) Uani 1 1 d . . .
C21 C 0.67519(18) 0.25201(10) 0.15899(15) 0.0330(6) Uani 1 1 d . . .
C22 C 0.5361(2) 0.25243(15) 0.01592(19) 0.0628(10) Uani 1 1 d . . .
H22A H 0.5652 0.2845 0.0021 0.094 Uiso 1 1 calc R . .
H22B H 0.4692 0.2524 -0.0040 0.094 Uiso 1 1 calc R . .
H22C H 0.5676 0.2233 -0.0047 0.094 Uiso 1 1 calc R . .
C23 C 0.4937(2) 0.18684(12) 0.1481(2) 0.0550(9) Uani 1 1 d . . .
H23A H 0.5008 0.1848 0.2026 0.083 Uiso 1 1 calc R . .
H23B H 0.5249 0.1574 0.1281 0.083 Uiso 1 1 calc R . .
H23C H 0.4266 0.1865 0.1289 0.083 Uiso 1 1 calc R . .
C24 C 0.4808(2) 0.30134(14) 0.1561(2) 0.0667(10) Uani 1 1 d . . .
H24A H 0.5075 0.3340 0.1421 0.100 Uiso 1 1 calc R . .
H24B H 0.4856 0.2990 0.2105 0.100 Uiso 1 1 calc R . .
H24C H 0.4145 0.2994 0.1350 0.100 Uiso 1 1 calc R . .
C25 C 0.7049(2) 0.29291(11) 0.20471(16) 0.0392(7) Uani 1 1 d . . .
H25 H 0.6599 0.3180 0.2145 0.047 Uiso 1 1 calc R . .
C26 C 0.7973(2) 0.29893(11) 0.23697(17) 0.0430(7) Uani 1 1 d . . .
H26 H 0.8152 0.3281 0.2669 0.052 Uiso 1 1 calc R . .
C27 C 0.86256(19) 0.26215(11) 0.22505(15) 0.0367(6) Uani 1 1 d . . .
H27 H 0.9259 0.2657 0.2472 0.044 Uiso 1 1 calc R . .
C28 C 0.51205(16) 0.88070(10) 0.37324(13) 0.0272(5) Uani 1 1 d . . .
C29 C 0.59696(17) 0.90669(11) 0.38034(15) 0.0349(6) Uani 1 1 d . . .
H29 H 0.6000 0.9405 0.3610 0.042 Uiso 1 1 calc R . .
C30 C 0.67767(19) 0.88352(12) 0.41560(17) 0.0439(7) Uani 1 1 d . . .
H30 H 0.7362 0.9011 0.4196 0.053 Uiso 1 1 calc R . .
C31 C 0.67289(19) 0.83480(12) 0.44487(16) 0.0431(7) Uani 1 1 d . . .
H31 H 0.7282 0.8191 0.4691 0.052 Uiso 1 1 calc R . .
C32 C 0.58855(19) 0.80878(11) 0.43916(15) 0.0385(6) Uani 1 1 d . . .
H32 H 0.5857 0.7754 0.4599 0.046 Uiso 1 1 calc R . .
C33 C 0.50775(18) 0.83142(10) 0.40297(15) 0.0333(6) Uani 1 1 d . . .
H33 H 0.4496 0.8134 0.3984 0.040 Uiso 1 1 calc R . .
C34 C 0.32623(17) 0.91926(10) 0.39410(14) 0.0312(6) Uani 1 1 d . . .
C35 C 0.27442(19) 0.87830(12) 0.41689(16) 0.0406(7) Uani 1 1 d . . .
H35 H 0.2804 0.8453 0.3958 0.049 Uiso 1 1 calc R . .
C36 C 0.2147(2) 0.88553(13) 0.46985(18) 0.0513(8) Uani 1 1 d . . .
H36 H 0.1785 0.8577 0.4846 0.062 Uiso 1 1 calc R . .
C37 C 0.2074(2) 0.93273(15) 0.50139(19) 0.0573(9) Uani 1 1 d . . .
H37 H 0.1666 0.9374 0.5385 0.069 Uiso 1 1 calc R . .
C38 C 0.2585(3) 0.97361(14) 0.4799(2) 0.0638(10) Uani 1 1 d . . .
H38 H 0.2534 1.0063 0.5022 0.077 Uiso 1 1 calc R . .
C39 C 0.3176(2) 0.96672(12) 0.42546(18) 0.0476(8) Uani 1 1 d . . .
H39 H 0.3523 0.9949 0.4098 0.057 Uiso 1 1 calc R . .
C40 C 0.35546(17) 0.86990(10) 0.25420(14) 0.0294(6) Uani 1 1 d . . .
C41 C 0.41206(19) 0.84021(10) 0.21471(15) 0.0357(6) Uani 1 1 d . . .
H41 H 0.4777 0.8380 0.2306 0.043 Uiso 1 1 calc R . .
C42 C 0.3735(2) 0.81363(12) 0.15210(16) 0.0511(8) Uani 1 1 d . . .
H42 H 0.4126 0.7928 0.1257 0.061 Uiso 1 1 calc R . .
C43 C 0.2784(3) 0.81737(14) 0.12794(17) 0.0560(9) Uani 1 1 d . . .
H43 H 0.2524 0.7999 0.0841 0.067 Uiso 1 1 calc R . .
C44 C 0.2215(2) 0.84631(14) 0.16730(18) 0.0560(9) Uani 1 1 d . . .
H44 H 0.1558 0.8481 0.1514 0.067 Uiso 1 1 calc R . .
C45 C 0.25951(19) 0.87277(12) 0.22998(17) 0.0444(7) Uani 1 1 d . . .
H45 H 0.2199 0.8930 0.2567 0.053 Uiso 1 1 calc R . .
C46 C 0.49541(17) 0.95813(10) 0.15669(14) 0.0303(6) Uani 1 1 d . . .
C47 C 0.58218(19) 0.93325(12) 0.16944(16) 0.0434(7) Uani 1 1 d . . .
H47 H 0.6215 0.9384 0.2151 0.052 Uiso 1 1 calc R . .
C48 C 0.6110(2) 0.90130(14) 0.11611(17) 0.0548(9) Uani 1 1 d . . .
H48 H 0.6707 0.8850 0.1246 0.066 Uiso 1 1 calc R . .
C49 C 0.5535(2) 0.89283(13) 0.05044(18) 0.0533(8) Uani 1 1 d . . .
H49 H 0.5731 0.8701 0.0143 0.064 Uiso 1 1 calc R . .
C50 C 0.4679(2) 0.91699(13) 0.03694(17) 0.0504(8) Uani 1 1 d . . .
H50 H 0.4287 0.9112 -0.0086 0.061 Uiso 1 1 calc R . .
C51 C 0.43863(19) 0.94984(12) 0.08970(16) 0.0412(7) Uani 1 1 d . . .
H51 H 0.3796 0.9668 0.0801 0.049 Uiso 1 1 calc R . .
C52 C 0.35343(16) 1.03150(10) 0.18758(15) 0.0296(6) Uani 1 1 d . . .
C53 C 0.26620(19) 1.02046(13) 0.2083(2) 0.0572(9) Uani 1 1 d . . .
H53 H 0.2600 0.9952 0.2452 0.069 Uiso 1 1 calc R . .
C54 C 0.1875(2) 1.04638(14) 0.1749(2) 0.0662(11) Uani 1 1 d . . .
H54 H 0.1274 1.0383 0.1889 0.079 Uiso 1 1 calc R . .
C55 C 0.19488(19) 1.08334(12) 0.12243(19) 0.0494(8) Uani 1 1 d . . .
H55 H 0.1405 1.1008 0.0999 0.059 Uiso 1 1 calc R . .
C56 C 0.2821(2) 1.09480(12) 0.10275(19) 0.0492(8) Uani 1 1 d . . .
H56 H 0.2882 1.1207 0.0668 0.059 Uiso 1 1 calc R . .
C57 C 0.36096(19) 1.06904(11) 0.13476(17) 0.0431(7) Uani 1 1 d . . .
H57 H 0.4209 1.0771 0.1204 0.052 Uiso 1 1 calc R . .
C58 C 0.54762(16) 1.04160(10) 0.25968(15) 0.0318(6) Uani 1 1 d . . .
C59 C 0.61441(18) 1.05747(12) 0.21501(17) 0.0416(7) Uani 1 1 d . . .
H59 H 0.6122 1.0448 0.1656 0.050 Uiso 1 1 calc R . .
C60 C 0.6843(2) 1.09177(13) 0.2424(2) 0.0529(9) Uani 1 1 d . . .
H60 H 0.7306 1.1021 0.2121 0.063 Uiso 1 1 calc R . .
C61 C 0.6866(2) 1.11066(14) 0.3130(2) 0.0636(10) Uani 1 1 d . . .
H61 H 0.7348 1.1340 0.3316 0.076 Uiso 1 1 calc R . .
C62 C 0.6195(2) 1.09602(15) 0.3577(2) 0.0629(10) Uani 1 1 d . . .
H62 H 0.6206 1.1101 0.4062 0.075 Uiso 1 1 calc R . .
C63 C 0.5507(2) 1.06093(13) 0.33161(18) 0.0479(8) Uani 1 1 d . . .
H63 H 0.5056 1.0501 0.3627 0.057 Uiso 1 1 calc R . .
C64 C 0.6345(5) 0.8590(2) 0.6521(5) 0.171(4) Uani 1 1 d . . .
H64A H 0.5767 0.8493 0.6194 0.205 Uiso 1 1 calc R . .
H64B H 0.6175 0.8643 0.7029 0.205 Uiso 1 1 calc R . .
C65 C 0.6982(4) 0.8204(3) 0.6534(4) 0.147(3) Uani 1 1 d . . .
H65A H 0.6823 0.7970 0.6106 0.177 Uiso 1 1 calc R . .
H65B H 0.7003 0.8004 0.7001 0.177 Uiso 1 1 calc R . .
C66 C 0.7873(4) 0.8456(4) 0.6487(5) 0.219(5) Uani 1 1 d . . .
H66A H 0.8261 0.8455 0.6980 0.263 Uiso 1 1 calc R . .
H66B H 0.8225 0.8276 0.6127 0.263 Uiso 1 1 calc R . .
C67 C 0.7659(4) 0.8997(3) 0.6236(3) 0.136(2) Uani 1 1 d . . .
H67A H 0.8023 0.9244 0.6574 0.163 Uiso 1 1 calc R . .
H67B H 0.7819 0.9050 0.5725 0.163 Uiso 1 1 calc R . .
N1 N 0.80160(15) 0.06876(9) 0.00514(12) 0.0360(5) Uani 1 1 d . . .
H1A H 0.7643 0.0866 -0.0311 0.043 Uiso 1 1 calc R . .
H1B H 0.8511 0.0554 -0.0166 0.043 Uiso 1 1 calc R . .
N2 N 0.74726(17) 0.02673(10) 0.02876(16) 0.0518(7) Uani 1 1 d . . .
H2A H 0.7383 0.0239 0.0758 0.062 Uiso 1 1 calc R . .
H2B H 0.7230 0.0039 -0.0039 0.062 Uiso 1 1 calc R . .
N3 N 0.43206(15) 0.96633(8) 0.29935(12) 0.0333(5) Uani 1 1 d . . .
Si1 Si 1.13798(5) 0.21033(3) -0.05997(4) 0.0393(2) Uani 1 1 d . . .
Si2 Si 0.94405(5) -0.02343(3) 0.30853(4) 0.03455(18) Uani 1 1 d . . .
Si3 Si 0.54779(5) 0.24688(3) 0.11932(5) 0.0393(2) Uani 1 1 d . . .
P1 P 0.91387(4) 0.16712(3) 0.16573(3) 0.02591(15) Uani 1 1 d . . .
P2 P 0.40810(4) 0.91127(3) 0.32719(4) 0.02598(15) Uani 1 1 d . . .
P3 P 0.45574(4) 0.99684(3) 0.22890(4) 0.02699(16) Uani 1 1 d . . .
S1 S 0.95055(4) 0.15930(3) 0.00391(4) 0.03506(17) Uani 1 1 d . . .
S2 S 0.91734(4) 0.05386(3) 0.15681(3) 0.03074(16) Uani 1 1 d . . .
S3 S 0.71644(4) 0.16354(3) 0.08303(4) 0.03164(16) Uani 1 1 d . . .
Ni1 Ni 0.85310(2) 0.118023(12) 0.082952(17) 0.02720(10) Uani 1 1 d . . .
O1 O 0.6707(3) 0.90628(17) 0.6256(3) 0.1438(16) Uani 1 1 d . . .


_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
C1 C9 1.391(3) . ?
C1 C2 1.413(3) . ?
C1 P1 1.816(2) . ?
C2 C3 1.421(3) . ?
C2 S1 1.750(2) . ?
C3 C7 1.396(4) . ?
C3 Si1 1.889(3) . ?
C4 Si1 1.865(3) . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C4 H4C 0.9800 . ?
C5 Si1 1.879(3) . ?
C5 H5A 0.9800 . ?
C5 H5B 0.9800 . ?
C5 H5C 0.9800 . ?
C6 Si1 1.865(4) . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?
C7 C8 1.382(4) . ?
C7 H7 0.9500 . ?
C8 C9 1.377(3) . ?
C8 H8 0.9500 . ?
C9 H9 0.9500 . ?
C10 C18 1.398(4) . ?
C10 C11 1.409(4) . ?
C10 P1 1.816(3) . ?
C11 C12 1.409(4) . ?
C11 S2 1.762(2) . ?
C12 C16 1.395(4) . ?
C12 Si2 1.887(3) . ?
C13 Si2 1.867(3) . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C14 Si2 1.866(3) . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C15 Si2 1.872(3) . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
C16 C17 1.387(4) . ?
C16 H16 0.9500 . ?
C17 C18 1.375(4) . ?
C17 H17 0.9500 . ?
C18 H18 0.9500 . ?
C19 C27 1.391(4) . ?
C19 C20 1.406(3) . ?
C19 P1 1.808(3) . ?
C20 C21 1.426(3) . ?
C20 S3 1.756(3) . ?
C21 C25 1.384(4) . ?
C21 Si3 1.881(3) . ?
C22 Si3 1.864(3) . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C23 Si3 1.850(3) . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 H23C 0.9800 . ?
C24 Si3 1.880(3) . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?
C25 C26 1.388(4) . ?
C25 H25 0.9500 . ?
C26 C27 1.374(4) . ?
C26 H26 0.9500 . ?
C27 H27 0.9500 . ?
C28 C29 1.384(3) . ?
C28 C33 1.397(4) . ?
C28 P2 1.800(2) . ?
C29 C30 1.388(4) . ?
C29 H29 0.9500 . ?
C30 C31 1.381(4) . ?
C30 H30 0.9500 . ?
C31 C32 1.378(4) . ?
C31 H31 0.9500 . ?
C32 C33 1.389(4) . ?
C32 H32 0.9500 . ?
C33 H33 0.9500 . ?
C34 C39 1.373(4) . ?
C34 C35 1.391(4) . ?
C34 P2 1.798(2) . ?
C35 C36 1.373(4) . ?
C35 H35 0.9500 . ?
C36 C37 1.366(5) . ?
C36 H36 0.9500 . ?
C37 C38 1.376(5) . ?
C37 H37 0.9500 . ?
C38 C39 1.387(4) . ?
C38 H38 0.9500 . ?
C39 H39 0.9500 . ?
C40 C41 1.382(4) . ?
C40 C45 1.392(4) . ?
C40 P2 1.798(3) . ?
C41 C42 1.384(4) . ?
C41 H41 0.9500 . ?
C42 C43 1.382(5) . ?
C42 H42 0.9500 . ?
C43 C44 1.372(5) . ?
C43 H43 0.9500 . ?
C44 C45 1.381(4) . ?
C44 H44 0.9500 . ?
C45 H45 0.9500 . ?
C46 C51 1.391(4) . ?
C46 C47 1.395(4) . ?
C46 P3 1.798(3) . ?
C47 C48 1.376(4) . ?
C47 H47 0.9500 . ?
C48 C49 1.378(5) . ?
C48 H48 0.9500 . ?
C49 C50 1.373(4) . ?
C49 H49 0.9500 . ?
C50 C51 1.385(4) . ?
C50 H50 0.9500 . ?
C51 H51 0.9500 . ?
C52 C53 1.378(4) . ?
C52 C57 1.382(4) . ?
C52 P3 1.803(2) . ?
C53 C54 1.386(4) . ?
C53 H53 0.9500 . ?
C54 C55 1.367(5) . ?
C54 H54 0.9500 . ?
C55 C56 1.373(4) . ?
C55 H55 0.9500 . ?
C56 C57 1.379(4) . ?
C56 H56 0.9500 . ?
C57 H57 0.9500 . ?
C58 C59 1.389(4) . ?
C58 C63 1.392(4) . ?
C58 P3 1.795(3) . ?
C59 C60 1.388(4) . ?
C59 H59 0.9500 . ?
C60 C61 1.366(5) . ?
C60 H60 0.9500 . ?
C61 C62 1.384(5) . ?
C61 H61 0.9500 . ?
C62 C63 1.384(4) . ?
C62 H62 0.9500 . ?
C63 H63 0.9500 . ?
C64 O1 1.441(7) . ?
C64 C65 1.358(8) . ?
C64 H64A 0.9900 . ?
C64 H64B 0.9900 . ?
C65 C66 1.447(8) . ?
C65 H65A 0.9900 . ?
C65 H65B 0.9900 . ?
C66 C67 1.503(9) . ?
C66 H66A 0.9900 . ?
C66 H66B 0.9900 . ?
C67 O1 1.378(6) . ?
C67 H67A 0.9900 . ?
C67 H67B 0.9900 . ?
N1 N2 1.439(3) . ?
N1 Ni1 1.980(2) . ?
N1 H1A 0.9200 . ?
N1 H1B 0.9200 . ?
N2 H2A 0.8800 . ?
N2 H2B 0.8800 . ?
N3 P2 1.573(2) . ?
N3 P3 1.575(2) . ?
P1 Ni1 2.0784(7) . ?
S1 Ni1 2.3753(7) . ?
S2 Ni1 2.2649(7) . ?
S3 Ni1 2.2885(7) . ?

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
C9 C1 C2 120.5(2) . . ?
C9 C1 P1 124.50(18) . . ?
C2 C1 P1 114.96(17) . . ?
C1 C2 C3 119.4(2) . . ?
C1 C2 S1 119.51(17) . . ?
C3 C2 S1 121.10(18) . . ?
C7 C3 C2 117.4(2) . . ?
C7 C3 Si1 120.62(18) . . ?
C2 C3 Si1 121.97(19) . . ?
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 123.0(2) . . ?
C8 C7 H7 118.5 . . ?
C3 C7 H7 118.5 . . ?
C9 C8 C7 119.4(2) . . ?
C9 C8 H8 120.3 . . ?
C7 C8 H8 120.3 . . ?
C8 C9 C1 120.3(2) . . ?
C8 C9 H9 119.9 . . ?
C1 C9 H9 119.9 . . ?
C18 C10 C11 120.4(2) . . ?
C18 C10 P1 125.9(2) . . ?
C11 C10 P1 113.65(18) . . ?
C10 C11 C12 120.5(2) . . ?
C10 C11 S2 117.72(19) . . ?
C12 C11 S2 121.8(2) . . ?
C16 C12 C11 116.9(2) . . ?
C16 C12 Si2 119.2(2) . . ?
C11 C12 Si2 123.68(19) . . ?
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 122.6(3) . . ?
C17 C16 H16 118.7 . . ?
C12 C16 H16 118.7 . . ?
C18 C17 C16 120.3(3) . . ?
C18 C17 H17 119.9 . . ?
C16 C17 H17 119.9 . . ?
C17 C18 C10 119.2(3) . . ?
C17 C18 H18 120.4 . . ?
C10 C18 H18 120.4 . . ?
C27 C19 C20 120.8(2) . . ?
C27 C19 P1 124.2(2) . . ?
C20 C19 P1 115.00(19) . . ?
C19 C20 C21 119.0(2) . . ?
C19 C20 S3 119.18(19) . . ?
C21 C20 S3 121.86(19) . . ?
C25 C21 C20 117.6(2) . . ?
C25 C21 Si3 119.7(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 123.0(3) . . ?
C26 C25 H25 118.5 . . ?
C21 C25 H25 118.5 . . ?
C27 C26 C25 119.1(3) . . ?
C27 C26 H26 120.5 . . ?
C25 C26 H26 120.5 . . ?
C26 C27 C19 120.3(3) . . ?
C26 C27 H27 119.9 . . ?
C19 C27 H27 119.9 . . ?
C29 C28 C33 119.6(2) . . ?
C29 C28 P2 119.5(2) . . ?
C33 C28 P2 120.84(18) . . ?
C28 C29 C30 120.1(3) . . ?
C28 C29 H29 120.0 . . ?
C30 C29 H29 120.0 . . ?
C31 C30 C29 119.9(3) . . ?
C31 C30 H30 120.0 . . ?
C29 C30 H30 120.0 . . ?
C32 C31 C30 120.6(3) . . ?
C32 C31 H31 119.7 . . ?
C30 C31 H31 119.7 . . ?
C31 C32 C33 119.8(3) . . ?
C31 C32 H32 120.1 . . ?
C33 C32 H32 120.1 . . ?
C32 C33 C28 119.9(2) . . ?
C32 C33 H33 120.0 . . ?
C28 C33 H33 120.0 . . ?
C39 C34 C35 119.4(2) . . ?
C39 C34 P2 118.8(2) . . ?
C35 C34 P2 121.7(2) . . ?
C36 C35 C34 120.1(3) . . ?
C36 C35 H35 119.9 . . ?
C34 C35 H35 119.9 . . ?
C35 C36 C37 120.1(3) . . ?
C35 C36 H36 119.9 . . ?
C37 C36 H36 119.9 . . ?
C36 C37 C38 120.6(3) . . ?
C36 C37 H37 119.7 . . ?
C38 C37 H37 119.7 . . ?
C37 C38 C39 119.5(3) . . ?
C37 C38 H38 120.3 . . ?
C39 C38 H38 120.3 . . ?
C34 C39 C38 120.2(3) . . ?
C34 C39 H39 119.9 . . ?
C38 C39 H39 119.9 . . ?
C41 C40 C45 119.1(3) . . ?
C41 C40 P2 119.8(2) . . ?
C45 C40 P2 120.5(2) . . ?
C42 C41 C40 120.3(3) . . ?
C42 C41 H41 119.9 . . ?
C40 C41 H41 119.9 . . ?
C41 C42 C43 120.1(3) . . ?
C41 C42 H42 119.9 . . ?
C43 C42 H42 119.9 . . ?
C44 C43 C42 120.0(3) . . ?
C44 C43 H43 120.0 . . ?
C42 C43 H43 120.0 . . ?
C43 C44 C45 120.2(3) . . ?
C43 C44 H44 119.9 . . ?
C45 C44 H44 119.9 . . ?
C44 C45 C40 120.4(3) . . ?
C44 C45 H45 119.8 . . ?
C40 C45 H45 119.8 . . ?
C51 C46 C47 119.0(3) . . ?
C51 C46 P3 121.2(2) . . ?
C47 C46 P3 119.7(2) . . ?
C48 C47 C46 120.2(3) . . ?
C48 C47 H47 119.9 . . ?
C46 C47 H47 119.9 . . ?
C49 C48 C47 120.2(3) . . ?
C49 C48 H48 119.9 . . ?
C47 C48 H48 119.9 . . ?
C48 C49 C50 120.4(3) . . ?
C48 C49 H49 119.8 . . ?
C50 C49 H49 119.8 . . ?
C49 C50 C51 120.0(3) . . ?
C49 C50 H50 120.0 . . ?
C51 C50 H50 120.0 . . ?
C50 C51 C46 120.2(3) . . ?
C50 C51 H51 119.9 . . ?
C46 C51 H51 119.9 . . ?
C53 C52 C57 119.1(2) . . ?
C53 C52 P3 120.0(2) . . ?
C57 C52 P3 120.89(19) . . ?
C54 C53 C52 119.7(3) . . ?
C54 C53 H53 120.2 . . ?
C52 C53 H53 120.2 . . ?
C55 C54 C53 121.2(3) . . ?
C55 C54 H54 119.4 . . ?
C53 C54 H54 119.4 . . ?
C54 C55 C56 119.0(3) . . ?
C54 C55 H55 120.5 . . ?
C56 C55 H55 120.5 . . ?
C55 C56 C57 120.6(3) . . ?
C55 C56 H56 119.7 . . ?
C57 C56 H56 119.7 . . ?
C56 C57 C52 120.4(3) . . ?
C56 C57 H57 119.8 . . ?
C52 C57 H57 119.8 . . ?
C59 C58 C63 119.5(3) . . ?
C59 C58 P3 122.9(2) . . ?
C63 C58 P3 117.6(2) . . ?
C60 C59 C58 120.1(3) . . ?
C60 C59 H59 119.9 . . ?
C58 C59 H59 119.9 . . ?
C61 C60 C59 120.0(3) . . ?
C61 C60 H60 120.0 . . ?
C59 C60 H60 120.0 . . ?
C60 C61 C62 120.6(3) . . ?
C60 C61 H61 119.7 . . ?
C62 C61 H61 119.7 . . ?
C61 C62 C63 120.0(3) . . ?
C61 C62 H62 120.0 . . ?
C63 C62 H62 120.0 . . ?
C62 C63 C58 119.8(3) . . ?
C62 C63 H63 120.1 . . ?
C58 C63 H63 120.1 . . ?
O1 C64 C65 111.9(6) . . ?
O1 C64 H64A 109.2 . . ?
C65 C64 H64A 109.2 . . ?
O1 C64 H64B 109.2 . . ?
C65 C64 H64B 109.3 . . ?
H64A C64 H64B 107.9 . . ?
C64 C65 C66 104.8(7) . . ?
C64 C65 H65A 110.8 . . ?
C66 C65 H65A 110.8 . . ?
C64 C65 H65B 110.8 . . ?
C66 C65 H65B 110.8 . . ?
H65A C65 H65B 108.9 . . ?
C67 C66 C65 107.2(5) . . ?
C67 C66 H66A 110.3 . . ?
C65 C66 H66A 110.3 . . ?
C67 C66 H66B 110.3 . . ?
C65 C66 H66B 110.3 . . ?
H66A C66 H66B 108.5 . . ?
O1 C67 C66 105.9(5) . . ?
O1 C67 H67A 110.5 . . ?
C66 C67 H67A 110.5 . . ?
O1 C67 H67B 110.5 . . ?
C66 C67 H67B 110.5 . . ?
H67A C67 H67B 108.7 . . ?
N2 N1 Ni1 116.77(17) . . ?
N2 N1 H1A 108.1 . . ?
Ni1 N1 H1A 108.1 . . ?
N2 N1 H1B 108.1 . . ?
Ni1 N1 H1B 108.1 . . ?
H1A N1 H1B 107.3 . . ?
N1 N2 H2A 120.0 . . ?
N1 N2 H2B 120.0 . . ?
H2A N2 H2B 120.0 . . ?
P2 N3 P3 142.89(16) . . ?
C6 Si1 C4 110.34(17) . . ?
C6 Si1 C5 108.01(19) . . ?
C4 Si1 C5 107.22(15) . . ?
C6 Si1 C3 111.14(14) . . ?
C4 Si1 C3 112.37(13) . . ?
C5 Si1 C3 107.54(14) . . ?
C13 Si2 C14 111.73(17) . . ?
C13 Si2 C15 107.42(15) . . ?
C14 Si2 C15 106.06(15) . . ?
C13 Si2 C12 112.23(13) . . ?
C14 Si2 C12 110.74(13) . . ?
C15 Si2 C12 108.36(14) . . ?
C23 Si3 C22 111.07(18) . . ?
C23 Si3 C21 111.89(14) . . ?
C22 Si3 C21 109.95(14) . . ?
C23 Si3 C24 106.84(16) . . ?
C22 Si3 C24 108.08(17) . . ?
C21 Si3 C24 108.88(15) . . ?
C19 P1 C10 106.79(12) . . ?
C19 P1 C1 109.30(11) . . ?
C10 P1 C1 107.33(11) . . ?
C19 P1 Ni1 111.40(9) . . ?
C10 P1 Ni1 110.99(9) . . ?
C1 P1 Ni1 110.87(8) . . ?
N3 P2 C34 107.22(12) . . ?
N3 P2 C40 113.61(12) . . ?
C34 P2 C40 108.38(12) . . ?
N3 P2 C28 110.62(12) . . ?
C34 P2 C28 108.04(11) . . ?
C40 P2 C28 108.81(12) . . ?
N3 P3 C58 107.43(12) . . ?
N3 P3 C46 115.06(12) . . ?
C58 P3 C46 107.80(12) . . ?
N3 P3 C52 110.13(12) . . ?
C58 P3 C52 109.25(12) . . ?
C46 P3 C52 107.04(12) . . ?
C2 S1 Ni1 103.53(8) . . ?
C11 S2 Ni1 106.07(9) . . ?
C20 S3 Ni1 105.75(8) . . ?
N1 Ni1 P1 176.76(7) . . ?
N1 Ni1 S2 91.67(7) . . ?
P1 Ni1 S2 85.76(3) . . ?
N1 Ni1 S3 95.36(7) . . ?
P1 Ni1 S3 87.83(3) . . ?
S2 Ni1 S3 131.90(3) . . ?
N1 Ni1 S1 93.47(7) . . ?
P1 Ni1 S1 86.00(3) . . ?
S2 Ni1 S1 117.66(3) . . ?
S3 Ni1 S1 109.32(3) . . ?
C67 O1 C64 107.4(5) . . ?

_diffrn_measured_fraction_theta_max 0.984
_diffrn_reflns_theta_full        25.07
_diffrn_measured_fraction_theta_full 0.984
_refine_diff_density_max         0.393
_refine_diff_density_min         -0.432
_refine_diff_density_rms         0.093
