# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2014

#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
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# 
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#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_compound_cis_4

_audit_creation_method           'SHELXL-97 + manual editing'
_chemical_name_systematic        
; 
?
;
_chemical_name_common            
;
?
;
_chemical_melting_point          ?
_chemical_formula_moiety         'C36 H48 N4 Ni Si'

_chemical_formula_sum            'C36 H48 N4 Ni Si'
_chemical_formula_weight         623.58

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'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   Cc
_symmetry_space_group_name_Hall  'C -2yc'

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

_cell_length_a                   11.8454(8)
_cell_length_b                   18.6420(13)
_cell_length_c                   16.1698(14)
_cell_angle_alpha                90.00
_cell_angle_beta                 103.264(3)
_cell_angle_gamma                90.00
_cell_volume                     3475.4(5)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    8523
_cell_measurement_theta_min      2.54
_cell_measurement_theta_max      26.74

_exptl_crystal_description       block
_exptl_crystal_colour            orange
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.09
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.192
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1336
_exptl_absorpt_coefficient_mu    0.622
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.5678
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_process_details   'Sadabs 2008/1 (Brucker 2008)'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_monochromator  'multi-layer mirror'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            20197
_diffrn_reflns_av_R_equivalents  0.0446
_diffrn_reflns_av_sigmaI/netI    0.0583
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         2.08
_diffrn_reflns_theta_max         26.76
_reflns_number_total             6715
_reflns_number_gt                6103
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'APEX2 ver. 2008.3 (Bruker AXS)'
_computing_cell_refinement       'Saint+ ver. 7.53A (Bruker AXS)'
_computing_data_reduction        'Saint+ ver. 7.53A (Bruker AXS)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'XP ver. 5.1 (Bruker AXS, 1998)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 2008)'

_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)+(0.0242P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.006(8)
_refine_ls_number_reflns         6715
_refine_ls_number_parameters     390
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0377
_refine_ls_R_factor_gt           0.0313
_refine_ls_wR_factor_ref         0.0644
_refine_ls_wR_factor_gt          0.0622
_refine_ls_goodness_of_fit_ref   0.996
_refine_ls_restrained_S_all      0.996
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni1 Ni 0.418749(18) 0.446753(12) 0.286769(15) 0.01366(7) Uani 1 1 d . . .
H1 H 0.4629(19) 0.4263(11) 0.3743(14) 0.020 Uiso 1 1 d . . .
Si1 Si 0.56995(5) 0.37483(3) 0.30571(3) 0.01590(13) Uani 1 1 d . . .
C1_1 C 0.50522(19) 0.28455(12) 0.32516(14) 0.0204(5) Uani 1 1 d . . .
C2_1 C 0.4494(2) 0.24039(12) 0.25840(16) 0.0261(5) Uani 1 1 d . . .
H2_1 H 0.4552 0.2520 0.2023 0.031 Uiso 1 1 calc R . .
C3_1 C 0.3860(2) 0.18034(14) 0.2704(2) 0.0394(7) Uani 1 1 d . . .
H3_1 H 0.3476 0.1526 0.2230 0.047 Uiso 1 1 calc R . .
C4_1 C 0.3790(2) 0.16093(15) 0.3518(2) 0.0431(8) Uani 1 1 d . . .
H4_1 H 0.3359 0.1199 0.3609 0.052 Uiso 1 1 calc R . .
C5_1 C 0.4358(2) 0.20220(15) 0.41935(19) 0.0397(7) Uani 1 1 d . . .
H5_1 H 0.4339 0.1885 0.4756 0.048 Uiso 1 1 calc R . .
C6_1 C 0.4954(2) 0.26332(14) 0.40618(15) 0.0279(6) Uani 1 1 d . . .
H6_1 H 0.5310 0.2918 0.4537 0.033 Uiso 1 1 calc R . .
C1_2 C 0.70185(19) 0.39162(11) 0.39611(13) 0.0195(5) Uani 1 1 d . . .
C2_2 C 0.7716(2) 0.33760(12) 0.44061(14) 0.0250(5) Uani 1 1 d . . .
H2_2 H 0.7509 0.2889 0.4278 0.030 Uiso 1 1 calc R . .
C3_2 C 0.8711(2) 0.35273(14) 0.50348(16) 0.0296(6) Uani 1 1 d . . .
H3_2 H 0.9166 0.3147 0.5330 0.035 Uiso 1 1 calc R . .
C4_2 C 0.9030(2) 0.42290(14) 0.52242(15) 0.0310(6) Uani 1 1 d . . .
H4_2 H 0.9712 0.4335 0.5645 0.037 Uiso 1 1 calc R . .
C5_2 C 0.8355(2) 0.47786(14) 0.47999(15) 0.0314(6) Uani 1 1 d . . .
H5_2 H 0.8571 0.5264 0.4928 0.038 Uiso 1 1 calc R . .
C6_2 C 0.7362(2) 0.46188(13) 0.41850(15) 0.0262(5) Uani 1 1 d . . .
H6_2 H 0.6898 0.5002 0.3906 0.031 Uiso 1 1 calc R . .
C1_3 C 0.6407(2) 0.35546(12) 0.21199(14) 0.0188(5) Uani 1 1 d . . .
C2_3 C 0.7601(2) 0.35080(13) 0.22046(16) 0.0267(5) Uani 1 1 d . . .
H2_3 H 0.8100 0.3564 0.2751 0.032 Uiso 1 1 calc R . .
C3_3 C 0.8083(2) 0.33819(14) 0.15094(17) 0.0358(6) Uani 1 1 d . . .
H3_3 H 0.8901 0.3353 0.1586 0.043 Uiso 1 1 calc R . .
C4_3 C 0.7373(3) 0.32991(14) 0.07095(17) 0.0380(7) Uani 1 1 d . . .
H4_3 H 0.7700 0.3218 0.0233 0.046 Uiso 1 1 calc R . .
C5_3 C 0.6194(2) 0.33341(13) 0.06062(15) 0.0306(6) Uani 1 1 d . . .
H5_3 H 0.5702 0.3270 0.0058 0.037 Uiso 1 1 calc R . .
C6_3 C 0.5719(2) 0.34621(12) 0.12977(14) 0.0237(5) Uani 1 1 d . . .
H6_3 H 0.4899 0.3488 0.1213 0.028 Uiso 1 1 calc R . .
C1_4 C 0.39770(19) 0.46756(11) 0.16936(13) 0.0160(5) Uani 1 1 d . . .
N2_4 N 0.46131(16) 0.50941(10) 0.12818(11) 0.0213(4) Uani 1 1 d . . .
C3_4 C 0.4197(3) 0.50554(17) 0.04086(18) 0.0305(5) Uani 1 1 d . . .
H3_4 H 0.4511 0.5291 -0.0009 0.037 Uiso 1 1 calc R . .
C4_4 C 0.3274(2) 0.46264(12) 0.02656(13) 0.0263(6) Uani 1 1 d . . .
H4_4 H 0.2797 0.4504 -0.0273 0.032 Uiso 1 1 calc R . .
N5_4 N 0.31408(16) 0.43929(9) 0.10494(11) 0.0189(4) Uani 1 1 d . . .
C6_4 C 0.5641(2) 0.55080(12) 0.17057(15) 0.0285(6) Uani 1 1 d . . .
H6_4 H 0.5842 0.5370 0.2320 0.034 Uiso 1 1 calc R . .
C7_4 C 0.6677(2) 0.53376(14) 0.13315(19) 0.0408(7) Uani 1 1 d . . .
H7A_4 H 0.6761 0.4816 0.1295 0.061 Uiso 1 1 calc R . .
H7B_4 H 0.7382 0.5540 0.1697 0.061 Uiso 1 1 calc R . .
H7C_4 H 0.6556 0.5547 0.0762 0.061 Uiso 1 1 calc R . .
C8_4 C 0.5382(3) 0.63125(14) 0.16482(18) 0.0403(7) Uani 1 1 d . . .
H8A_4 H 0.5188 0.6460 0.1050 0.060 Uiso 1 1 calc R . .
H8B_4 H 0.6066 0.6578 0.1952 0.060 Uiso 1 1 calc R . .
H8C_4 H 0.4727 0.6415 0.1905 0.060 Uiso 1 1 calc R . .
C9_4 C 0.2237(2) 0.39042(12) 0.11857(13) 0.0213(5) Uani 1 1 d . . .
H9_4 H 0.2434 0.3760 0.1798 0.026 Uiso 1 1 calc R . .
C10_4 C 0.2200(2) 0.32276(13) 0.06571(15) 0.0309(6) Uani 1 1 d . . .
H10A_4 H 0.1649 0.2887 0.0808 0.046 Uiso 1 1 calc R . .
H10B_4 H 0.2973 0.3010 0.0770 0.046 Uiso 1 1 calc R . .
H10C_4 H 0.1952 0.3349 0.0053 0.046 Uiso 1 1 calc R . .
C11_4 C 0.1074(2) 0.42807(14) 0.10121(16) 0.0303(6) Uani 1 1 d . . .
H11A_4 H 0.1101 0.4674 0.1419 0.046 Uiso 1 1 calc R . .
H11B_4 H 0.0470 0.3938 0.1072 0.046 Uiso 1 1 calc R . .
H11C_4 H 0.0897 0.4474 0.0433 0.046 Uiso 1 1 calc R . .
C1_5 C 0.27370(18) 0.47921(11) 0.30954(12) 0.0153(5) Uani 1 1 d . . .
N2_5 N 0.22352(16) 0.54531(9) 0.29789(11) 0.0200(4) Uani 1 1 d . . .
C3_5 C 0.1162(2) 0.54603(13) 0.31804(15) 0.0263(5) Uani 1 1 d . . .
H3_5 H 0.0658 0.5861 0.3150 0.032 Uiso 1 1 calc R . .
C4_5 C 0.0971(2) 0.47946(14) 0.34261(14) 0.0270(5) Uani 1 1 d . . .
H4_5 H 0.0302 0.4631 0.3601 0.032 Uiso 1 1 calc R . .
N5_5 N 0.19307(16) 0.43928(10) 0.33763(11) 0.0198(4) Uani 1 1 d . . .
C6_5 C 0.2790(2) 0.60708(11) 0.26681(14) 0.0231(5) Uani 1 1 d . . .
H6_5 H 0.3559 0.5912 0.2579 0.028 Uiso 1 1 calc R . .
C7_5 C 0.2066(3) 0.63314(15) 0.18229(16) 0.0400(7) Uani 1 1 d . . .
H7A_5 H 0.1991 0.5946 0.1402 0.060 Uiso 1 1 calc R . .
H7B_5 H 0.2445 0.6746 0.1630 0.060 Uiso 1 1 calc R . .
H7C_5 H 0.1295 0.6471 0.1890 0.060 Uiso 1 1 calc R . .
C8_5 C 0.2999(3) 0.66680(14) 0.33248(16) 0.0438(7) Uani 1 1 d . . .
H8A_5 H 0.2259 0.6815 0.3444 0.066 Uiso 1 1 calc R . .
H8B_5 H 0.3356 0.7079 0.3105 0.066 Uiso 1 1 calc R . .
H8C_5 H 0.3518 0.6495 0.3849 0.066 Uiso 1 1 calc R . .
C9_5 C 0.2089(2) 0.36281(13) 0.36150(15) 0.0236(6) Uani 1 1 d . . .
H9_5 H 0.2858 0.3472 0.3522 0.028 Uiso 1 1 calc R . .
C10_5 C 0.1161(2) 0.31577(14) 0.30721(17) 0.0363(6) Uani 1 1 d . . .
H10A_5 H 0.0403 0.3281 0.3180 0.054 Uiso 1 1 calc R . .
H10B_5 H 0.1334 0.2653 0.3216 0.054 Uiso 1 1 calc R . .
H10C_5 H 0.1147 0.3236 0.2470 0.054 Uiso 1 1 calc R . .
C11_5 C 0.2113(3) 0.35331(15) 0.45576(16) 0.0357(7) Uani 1 1 d . . .
H11A_5 H 0.1369 0.3685 0.4666 0.054 Uiso 1 1 calc R . .
H11B_5 H 0.2738 0.3826 0.4897 0.054 Uiso 1 1 calc R . .
H11C_5 H 0.2249 0.3027 0.4714 0.054 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 C1_4 1.897(2) . ?
Ni1 C1_5 1.935(2) . ?
Ni1 Si1 2.2017(6) . ?
Ni1 H1 1.44(2) . ?
Si1 C1_2 1.905(2) . ?
Si1 C1_1 1.905(2) . ?
Si1 C1_3 1.927(2) . ?
C1_1 C2_1 1.397(3) . ?
C1_1 C6_1 1.399(3) . ?
C2_1 C3_1 1.386(3) . ?
C2_1 H2_1 0.9500 . ?
C3_1 C4_1 1.385(4) . ?
C3_1 H3_1 0.9500 . ?
C4_1 C5_1 1.378(4) . ?
C4_1 H4_1 0.9500 . ?
C5_1 C6_1 1.383(4) . ?
C5_1 H5_1 0.9500 . ?
C6_1 H6_1 0.9500 . ?
C1_2 C2_2 1.394(3) . ?
C1_2 C6_2 1.394(3) . ?
C2_2 C3_2 1.397(3) . ?
C2_2 H2_2 0.9500 . ?
C3_2 C4_2 1.377(4) . ?
C3_2 H3_2 0.9500 . ?
C4_2 C5_2 1.381(4) . ?
C4_2 H4_2 0.9500 . ?
C5_2 C6_2 1.388(3) . ?
C5_2 H5_2 0.9500 . ?
C6_2 H6_2 0.9500 . ?
C1_3 C2_3 1.392(3) . ?
C1_3 C6_3 1.401(3) . ?
C2_3 C3_3 1.393(3) . ?
C2_3 H2_3 0.9500 . ?
C3_3 C4_3 1.380(4) . ?
C3_3 H3_3 0.9500 . ?
C4_3 C5_3 1.369(4) . ?
C4_3 H4_3 0.9500 . ?
C5_3 C6_3 1.383(3) . ?
C5_3 H5_3 0.9500 . ?
C6_3 H6_3 0.9500 . ?
C1_4 N2_4 1.360(3) . ?
C1_4 N5_4 1.368(3) . ?
N2_4 C3_4 1.387(3) . ?
N2_4 C6_4 1.471(3) . ?
C3_4 C4_4 1.332(4) . ?
C3_4 H3_4 0.9500 . ?
C4_4 N5_4 1.383(3) . ?
C4_4 H4_4 0.9500 . ?
N5_4 C9_4 1.460(3) . ?
C6_4 C7_4 1.521(4) . ?
C6_4 C8_4 1.529(3) . ?
C6_4 H6_4 1.0000 . ?
C7_4 H7A_4 0.9800 . ?
C7_4 H7B_4 0.9800 . ?
C7_4 H7C_4 0.9800 . ?
C8_4 H8A_4 0.9800 . ?
C8_4 H8B_4 0.9800 . ?
C8_4 H8C_4 0.9800 . ?
C9_4 C11_4 1.514(3) . ?
C9_4 C10_4 1.519(3) . ?
C9_4 H9_4 1.0000 . ?
C10_4 H10A_4 0.9800 . ?
C10_4 H10B_4 0.9800 . ?
C10_4 H10C_4 0.9800 . ?
C11_4 H11A_4 0.9800 . ?
C11_4 H11B_4 0.9800 . ?
C11_4 H11C_4 0.9800 . ?
C1_5 N2_5 1.362(3) . ?
C1_5 N5_5 1.368(3) . ?
N2_5 C3_5 1.383(3) . ?
N2_5 C6_5 1.470(3) . ?
C3_5 C4_5 1.338(3) . ?
C3_5 H3_5 0.9500 . ?
C4_5 N5_5 1.380(3) . ?
C4_5 H4_5 0.9500 . ?
N5_5 C9_5 1.478(3) . ?
C6_5 C7_5 1.517(3) . ?
C6_5 C8_5 1.519(3) . ?
C6_5 H6_5 1.0000 . ?
C7_5 H7A_5 0.9800 . ?
C7_5 H7B_5 0.9800 . ?
C7_5 H7C_5 0.9800 . ?
C8_5 H8A_5 0.9800 . ?
C8_5 H8B_5 0.9800 . ?
C8_5 H8C_5 0.9800 . ?
C9_5 C10_5 1.518(4) . ?
C9_5 C11_5 1.528(3) . ?
C9_5 H9_5 1.0000 . ?
C10_5 H10A_5 0.9800 . ?
C10_5 H10B_5 0.9800 . ?
C10_5 H10C_5 0.9800 . ?
C11_5 H11A_5 0.9800 . ?
C11_5 H11B_5 0.9800 . ?
C11_5 H11C_5 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C1_4 Ni1 C1_5 102.00(9) . . ?
C1_4 Ni1 Si1 100.35(7) . . ?
C1_5 Ni1 Si1 153.31(6) . . ?
C1_4 Ni1 H1 166.0(9) . . ?
C1_5 Ni1 H1 92.0(9) . . ?
Si1 Ni1 H1 66.6(9) . . ?
C1_2 Si1 C1_1 107.99(10) . . ?
C1_2 Si1 C1_3 101.90(10) . . ?
C1_1 Si1 C1_3 103.20(10) . . ?
C1_2 Si1 Ni1 120.31(7) . . ?
C1_1 Si1 Ni1 102.45(7) . . ?
C1_3 Si1 Ni1 119.43(8) . . ?
C2_1 C1_1 C6_1 115.5(2) . . ?
C2_1 C1_1 Si1 121.99(16) . . ?
C6_1 C1_1 Si1 121.84(18) . . ?
C3_1 C2_1 C1_1 122.9(2) . . ?
C3_1 C2_1 H2_1 118.6 . . ?
C1_1 C2_1 H2_1 118.6 . . ?
C4_1 C3_1 C2_1 119.8(3) . . ?
C4_1 C3_1 H3_1 120.1 . . ?
C2_1 C3_1 H3_1 120.1 . . ?
C5_1 C4_1 C3_1 118.8(2) . . ?
C5_1 C4_1 H4_1 120.6 . . ?
C3_1 C4_1 H4_1 120.6 . . ?
C4_1 C5_1 C6_1 120.8(2) . . ?
C4_1 C5_1 H5_1 119.6 . . ?
C6_1 C5_1 H5_1 119.6 . . ?
C5_1 C6_1 C1_1 122.2(3) . . ?
C5_1 C6_1 H6_1 118.9 . . ?
C1_1 C6_1 H6_1 118.9 . . ?
C2_2 C1_2 C6_2 116.2(2) . . ?
C2_2 C1_2 Si1 124.23(17) . . ?
C6_2 C1_2 Si1 119.51(17) . . ?
C1_2 C2_2 C3_2 122.1(2) . . ?
C1_2 C2_2 H2_2 119.0 . . ?
C3_2 C2_2 H2_2 119.0 . . ?
C4_2 C3_2 C2_2 119.8(2) . . ?
C4_2 C3_2 H3_2 120.1 . . ?
C2_2 C3_2 H3_2 120.1 . . ?
C3_2 C4_2 C5_2 119.8(2) . . ?
C3_2 C4_2 H4_2 120.1 . . ?
C5_2 C4_2 H4_2 120.1 . . ?
C4_2 C5_2 C6_2 119.7(2) . . ?
C4_2 C5_2 H5_2 120.1 . . ?
C6_2 C5_2 H5_2 120.1 . . ?
C5_2 C6_2 C1_2 122.5(2) . . ?
C5_2 C6_2 H6_2 118.8 . . ?
C1_2 C6_2 H6_2 118.8 . . ?
C2_3 C1_3 C6_3 116.2(2) . . ?
C2_3 C1_3 Si1 123.35(18) . . ?
C6_3 C1_3 Si1 120.41(18) . . ?
C1_3 C2_3 C3_3 121.8(2) . . ?
C1_3 C2_3 H2_3 119.1 . . ?
C3_3 C2_3 H2_3 119.1 . . ?
C4_3 C3_3 C2_3 120.0(2) . . ?
C4_3 C3_3 H3_3 120.0 . . ?
C2_3 C3_3 H3_3 120.0 . . ?
C5_3 C4_3 C3_3 119.6(2) . . ?
C5_3 C4_3 H4_3 120.2 . . ?
C3_3 C4_3 H4_3 120.2 . . ?
C4_3 C5_3 C6_3 120.2(2) . . ?
C4_3 C5_3 H5_3 119.9 . . ?
C6_3 C5_3 H5_3 119.9 . . ?
C5_3 C6_3 C1_3 122.1(2) . . ?
C5_3 C6_3 H6_3 118.9 . . ?
C1_3 C6_3 H6_3 118.9 . . ?
N2_4 C1_4 N5_4 103.53(17) . . ?
N2_4 C1_4 Ni1 130.30(16) . . ?
N5_4 C1_4 Ni1 126.11(16) . . ?
C1_4 N2_4 C3_4 111.2(2) . . ?
C1_4 N2_4 C6_4 124.40(17) . . ?
C3_4 N2_4 C6_4 124.4(2) . . ?
C4_4 C3_4 N2_4 107.1(2) . . ?
C4_4 C3_4 H3_4 126.5 . . ?
N2_4 C3_4 H3_4 126.5 . . ?
C3_4 C4_4 N5_4 107.0(2) . . ?
C3_4 C4_4 H4_4 126.5 . . ?
N5_4 C4_4 H4_4 126.5 . . ?
C1_4 N5_4 C4_4 111.22(19) . . ?
C1_4 N5_4 C9_4 123.59(17) . . ?
C4_4 N5_4 C9_4 125.19(19) . . ?
N2_4 C6_4 C7_4 111.2(2) . . ?
N2_4 C6_4 C8_4 110.7(2) . . ?
C7_4 C6_4 C8_4 110.5(2) . . ?
N2_4 C6_4 H6_4 108.1 . . ?
C7_4 C6_4 H6_4 108.1 . . ?
C8_4 C6_4 H6_4 108.1 . . ?
C6_4 C7_4 H7A_4 109.5 . . ?
C6_4 C7_4 H7B_4 109.5 . . ?
H7A_4 C7_4 H7B_4 109.5 . . ?
C6_4 C7_4 H7C_4 109.5 . . ?
H7A_4 C7_4 H7C_4 109.5 . . ?
H7B_4 C7_4 H7C_4 109.5 . . ?
C6_4 C8_4 H8A_4 109.5 . . ?
C6_4 C8_4 H8B_4 109.5 . . ?
H8A_4 C8_4 H8B_4 109.5 . . ?
C6_4 C8_4 H8C_4 109.5 . . ?
H8A_4 C8_4 H8C_4 109.5 . . ?
H8B_4 C8_4 H8C_4 109.5 . . ?
N5_4 C9_4 C11_4 110.51(19) . . ?
N5_4 C9_4 C10_4 111.15(19) . . ?
C11_4 C9_4 C10_4 111.89(19) . . ?
N5_4 C9_4 H9_4 107.7 . . ?
C11_4 C9_4 H9_4 107.7 . . ?
C10_4 C9_4 H9_4 107.7 . . ?
C9_4 C10_4 H10A_4 109.5 . . ?
C9_4 C10_4 H10B_4 109.5 . . ?
H10A_4 C10_4 H10B_4 109.5 . . ?
C9_4 C10_4 H10C_4 109.5 . . ?
H10A_4 C10_4 H10C_4 109.5 . . ?
H10B_4 C10_4 H10C_4 109.5 . . ?
C9_4 C11_4 H11A_4 109.5 . . ?
C9_4 C11_4 H11B_4 109.5 . . ?
H11A_4 C11_4 H11B_4 109.5 . . ?
C9_4 C11_4 H11C_4 109.5 . . ?
H11A_4 C11_4 H11C_4 109.5 . . ?
H11B_4 C11_4 H11C_4 109.5 . . ?
N2_5 C1_5 N5_5 102.84(18) . . ?
N2_5 C1_5 Ni1 129.41(16) . . ?
N5_5 C1_5 Ni1 127.67(15) . . ?
C1_5 N2_5 C3_5 111.83(18) . . ?
C1_5 N2_5 C6_5 122.72(19) . . ?
C3_5 N2_5 C6_5 125.45(18) . . ?
C4_5 C3_5 N2_5 106.8(2) . . ?
C4_5 C3_5 H3_5 126.6 . . ?
N2_5 C3_5 H3_5 126.6 . . ?
C3_5 C4_5 N5_5 106.7(2) . . ?
C3_5 C4_5 H4_5 126.6 . . ?
N5_5 C4_5 H4_5 126.6 . . ?
C1_5 N5_5 C4_5 111.82(18) . . ?
C1_5 N5_5 C9_5 123.72(18) . . ?
C4_5 N5_5 C9_5 124.44(19) . . ?
N2_5 C6_5 C7_5 110.7(2) . . ?
N2_5 C6_5 C8_5 110.44(19) . . ?
C7_5 C6_5 C8_5 111.3(2) . . ?
N2_5 C6_5 H6_5 108.1 . . ?
C7_5 C6_5 H6_5 108.1 . . ?
C8_5 C6_5 H6_5 108.1 . . ?
C6_5 C7_5 H7A_5 109.5 . . ?
C6_5 C7_5 H7B_5 109.5 . . ?
H7A_5 C7_5 H7B_5 109.5 . . ?
C6_5 C7_5 H7C_5 109.5 . . ?
H7A_5 C7_5 H7C_5 109.5 . . ?
H7B_5 C7_5 H7C_5 109.5 . . ?
C6_5 C8_5 H8A_5 109.5 . . ?
C6_5 C8_5 H8B_5 109.5 . . ?
H8A_5 C8_5 H8B_5 109.5 . . ?
C6_5 C8_5 H8C_5 109.5 . . ?
H8A_5 C8_5 H8C_5 109.5 . . ?
H8B_5 C8_5 H8C_5 109.5 . . ?
N5_5 C9_5 C10_5 112.0(2) . . ?
N5_5 C9_5 C11_5 110.2(2) . . ?
C10_5 C9_5 C11_5 110.8(2) . . ?
N5_5 C9_5 H9_5 107.9 . . ?
C10_5 C9_5 H9_5 107.9 . . ?
C11_5 C9_5 H9_5 107.9 . . ?
C9_5 C10_5 H10A_5 109.5 . . ?
C9_5 C10_5 H10B_5 109.5 . . ?
H10A_5 C10_5 H10B_5 109.5 . . ?
C9_5 C10_5 H10C_5 109.5 . . ?
H10A_5 C10_5 H10C_5 109.5 . . ?
H10B_5 C10_5 H10C_5 109.5 . . ?
C9_5 C11_5 H11A_5 109.5 . . ?
C9_5 C11_5 H11B_5 109.5 . . ?
H11A_5 C11_5 H11B_5 109.5 . . ?
C9_5 C11_5 H11C_5 109.5 . . ?
H11A_5 C11_5 H11C_5 109.5 . . ?
H11B_5 C11_5 H11C_5 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C1_4 Ni1 Si1 C1_2 129.48(10) . . . . ?
C1_5 Ni1 Si1 C1_2 -84.02(16) . . . . ?
C1_4 Ni1 Si1 C1_1 -110.83(10) . . . . ?
C1_5 Ni1 Si1 C1_1 35.67(16) . . . . ?
C1_4 Ni1 Si1 C1_3 2.32(11) . . . . ?
C1_5 Ni1 Si1 C1_3 148.82(16) . . . . ?
C1_2 Si1 C1_1 C2_1 -148.18(18) . . . . ?
C1_3 Si1 C1_1 C2_1 -40.8(2) . . . . ?
Ni1 Si1 C1_1 C2_1 83.87(18) . . . . ?
C1_2 Si1 C1_1 C6_1 41.4(2) . . . . ?
C1_3 Si1 C1_1 C6_1 148.84(19) . . . . ?
Ni1 Si1 C1_1 C6_1 -86.50(18) . . . . ?
C6_1 C1_1 C2_1 C3_1 1.4(3) . . . . ?
Si1 C1_1 C2_1 C3_1 -169.50(19) . . . . ?
C1_1 C2_1 C3_1 C4_1 -1.9(4) . . . . ?
C2_1 C3_1 C4_1 C5_1 0.0(4) . . . . ?
C3_1 C4_1 C5_1 C6_1 2.2(4) . . . . ?
C4_1 C5_1 C6_1 C1_1 -2.6(4) . . . . ?
C2_1 C1_1 C6_1 C5_1 0.8(3) . . . . ?
Si1 C1_1 C6_1 C5_1 171.75(19) . . . . ?
C1_1 Si1 C1_2 C2_2 29.6(2) . . . . ?
C1_3 Si1 C1_2 C2_2 -78.7(2) . . . . ?
Ni1 Si1 C1_2 C2_2 146.49(17) . . . . ?
C1_1 Si1 C1_2 C6_2 -153.25(17) . . . . ?
C1_3 Si1 C1_2 C6_2 98.46(19) . . . . ?
Ni1 Si1 C1_2 C6_2 -36.4(2) . . . . ?
C6_2 C1_2 C2_2 C3_2 -0.7(3) . . . . ?
Si1 C1_2 C2_2 C3_2 176.53(19) . . . . ?
C1_2 C2_2 C3_2 C4_2 -0.5(4) . . . . ?
C2_2 C3_2 C4_2 C5_2 0.9(4) . . . . ?
C3_2 C4_2 C5_2 C6_2 -0.1(4) . . . . ?
C4_2 C5_2 C6_2 C1_2 -1.2(4) . . . . ?
C2_2 C1_2 C6_2 C5_2 1.6(3) . . . . ?
Si1 C1_2 C6_2 C5_2 -175.80(19) . . . . ?
C1_2 Si1 C1_3 C2_3 4.7(2) . . . . ?
C1_1 Si1 C1_3 C2_3 -107.3(2) . . . . ?
Ni1 Si1 C1_3 C2_3 139.99(17) . . . . ?
C1_2 Si1 C1_3 C6_3 -174.40(18) . . . . ?
C1_1 Si1 C1_3 C6_3 73.7(2) . . . . ?
Ni1 Si1 C1_3 C6_3 -39.1(2) . . . . ?
C6_3 C1_3 C2_3 C3_3 0.5(3) . . . . ?
Si1 C1_3 C2_3 C3_3 -178.64(19) . . . . ?
C1_3 C2_3 C3_3 C4_3 0.0(4) . . . . ?
C2_3 C3_3 C4_3 C5_3 -0.7(4) . . . . ?
C3_3 C4_3 C5_3 C6_3 0.9(4) . . . . ?
C4_3 C5_3 C6_3 C1_3 -0.5(4) . . . . ?
C2_3 C1_3 C6_3 C5_3 -0.2(3) . . . . ?
Si1 C1_3 C6_3 C5_3 178.91(18) . . . . ?
C1_5 Ni1 C1_4 N2_4 122.0(2) . . . . ?
Si1 Ni1 C1_4 N2_4 -72.7(2) . . . . ?
C1_5 Ni1 C1_4 N5_4 -61.5(2) . . . . ?
Si1 Ni1 C1_4 N5_4 103.78(18) . . . . ?
N5_4 C1_4 N2_4 C3_4 -1.5(3) . . . . ?
Ni1 C1_4 N2_4 C3_4 175.62(19) . . . . ?
N5_4 C1_4 N2_4 C6_4 -178.9(2) . . . . ?
Ni1 C1_4 N2_4 C6_4 -1.8(3) . . . . ?
C1_4 N2_4 C3_4 C4_4 1.7(3) . . . . ?
C6_4 N2_4 C3_4 C4_4 179.1(2) . . . . ?
N2_4 C3_4 C4_4 N5_4 -1.1(3) . . . . ?
N2_4 C1_4 N5_4 C4_4 0.7(2) . . . . ?
Ni1 C1_4 N5_4 C4_4 -176.51(16) . . . . ?
N2_4 C1_4 N5_4 C9_4 -179.67(18) . . . . ?
Ni1 C1_4 N5_4 C9_4 3.1(3) . . . . ?
C3_4 C4_4 N5_4 C1_4 0.3(3) . . . . ?
C3_4 C4_4 N5_4 C9_4 -179.3(2) . . . . ?
C1_4 N2_4 C6_4 C7_4 126.6(2) . . . . ?
C3_4 N2_4 C6_4 C7_4 -50.5(3) . . . . ?
C1_4 N2_4 C6_4 C8_4 -110.2(2) . . . . ?
C3_4 N2_4 C6_4 C8_4 72.7(3) . . . . ?
C1_4 N5_4 C9_4 C11_4 107.8(2) . . . . ?
C4_4 N5_4 C9_4 C11_4 -72.7(3) . . . . ?
C1_4 N5_4 C9_4 C10_4 -127.4(2) . . . . ?
C4_4 N5_4 C9_4 C10_4 52.2(3) . . . . ?
C1_4 Ni1 C1_5 N2_5 -57.3(2) . . . . ?
Si1 Ni1 C1_5 N2_5 156.42(12) . . . . ?
C1_4 Ni1 C1_5 N5_5 118.96(18) . . . . ?
Si1 Ni1 C1_5 N5_5 -27.3(3) . . . . ?
N5_5 C1_5 N2_5 C3_5 0.0(2) . . . . ?
Ni1 C1_5 N2_5 C3_5 176.98(16) . . . . ?
N5_5 C1_5 N2_5 C6_5 -179.50(18) . . . . ?
Ni1 C1_5 N2_5 C6_5 -2.5(3) . . . . ?
C1_5 N2_5 C3_5 C4_5 -0.3(3) . . . . ?
C6_5 N2_5 C3_5 C4_5 179.2(2) . . . . ?
N2_5 C3_5 C4_5 N5_5 0.4(3) . . . . ?
N2_5 C1_5 N5_5 C4_5 0.2(2) . . . . ?
Ni1 C1_5 N5_5 C4_5 -176.81(15) . . . . ?
N2_5 C1_5 N5_5 C9_5 -178.45(19) . . . . ?
Ni1 C1_5 N5_5 C9_5 4.5(3) . . . . ?
C3_5 C4_5 N5_5 C1_5 -0.4(3) . . . . ?
C3_5 C4_5 N5_5 C9_5 178.3(2) . . . . ?
C1_5 N2_5 C6_5 C7_5 117.3(2) . . . . ?
C3_5 N2_5 C6_5 C7_5 -62.1(3) . . . . ?
C1_5 N2_5 C6_5 C8_5 -118.9(2) . . . . ?
C3_5 N2_5 C6_5 C8_5 61.6(3) . . . . ?
C1_5 N5_5 C9_5 C10_5 -119.7(2) . . . . ?
C4_5 N5_5 C9_5 C10_5 61.8(3) . . . . ?
C1_5 N5_5 C9_5 C11_5 116.5(2) . . . . ?
C4_5 N5_5 C9_5 C11_5 -62.0(3) . . . . ?

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        26.00
_diffrn_measured_fraction_theta_full 1.000
_refine_diff_density_max         0.361
_refine_diff_density_min         -0.215
_refine_diff_density_rms         0.045
_database_code_depnum_ccdc_archive 'CCDC 997522'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_compound_6

_audit_creation_method           'SHELXL-97 + manual editing'
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         C42H54N4Ni2Si2
_chemical_formula_sum            'C42 H54 N4 Ni2 Si2'
_chemical_formula_weight         788.49

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'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   P21/c

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

_cell_length_a                   10.480(5)
_cell_length_b                   16.614(7)
_cell_length_c                   12.530(6)
_cell_angle_alpha                90.00
_cell_angle_beta                 106.519(7)
_cell_angle_gamma                90.00
_cell_volume                     2091.6(16)
_cell_formula_units_Z            2
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    6552
_cell_measurement_theta_min      2.368
_cell_measurement_theta_max      25.470

_exptl_crystal_description       block
_exptl_crystal_colour            red
_exptl_crystal_size_max          0.29
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.06
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.252
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             836
_exptl_absorpt_coefficient_mu    0.990
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6382
_exptl_absorpt_correction_T_max  0.7453
_exptl_absorpt_process_details   'SadAbs-2008/1 (Bruker, 2008)'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      173(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_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            32458
_diffrn_reflns_av_R_equivalents  0.0587
_diffrn_reflns_av_sigmaI/netI    0.0369
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         2.03
_diffrn_reflns_theta_max         26.32
_reflns_number_total             4191
_reflns_number_gt                3326
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Smart-NT v. 5.63'
_computing_cell_refinement       'Saint-NT v. 7.23'
_computing_data_reduction        'Saint-NT v. 7.23'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'XP in ShelxTL-97'
_computing_publication_material  'XP in ShelxTL-97'

_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)+(0.0391P)²+0.5469P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         4191
_refine_ls_number_parameters     234
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0450
_refine_ls_R_factor_gt           0.0310
_refine_ls_wR_factor_ref         0.0832
_refine_ls_wR_factor_gt          0.0758
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_restrained_S_all      1.038
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni Ni 0.49525(2) 0.075486(13) -0.006492(17) 0.02106(9) Uani 1 1 d . . .
Si Si 0.46101(5) 0.00251(3) 0.13309(4) 0.02200(13) Uani 1 1 d . . .
N1 N 0.61166(15) 0.22703(9) -0.05569(13) 0.0283(4) Uani 1 1 d . . .
N2 N 0.40251(16) 0.22125(9) -0.13827(14) 0.0303(4) Uani 1 1 d . . .
C1 C 0.50393(18) 0.17762(11) -0.07123(14) 0.0239(4) Uani 1 1 d . . .
C2 C 0.5766(2) 0.30023(12) -0.10946(19) 0.0408(5) Uani 1 1 d . . .
H2A H 0.6340 0.3445 -0.1093 0.049 Uiso 1 1 calc R . .
C3 C 0.4461(2) 0.29627(12) -0.16166(19) 0.0423(5) Uani 1 1 d . . .
H3A H 0.3933 0.3371 -0.2063 0.051 Uiso 1 1 calc R . .
C4 C 0.26336(19) 0.19338(13) -0.17307(17) 0.0353(5) Uani 1 1 d . . .
H4A H 0.2622 0.1364 -0.1478 0.042 Uiso 1 1 calc R . .
C5 C 0.74240(19) 0.20652(12) 0.02070(17) 0.0329(5) Uani 1 1 d . . .
H5A H 0.7537 0.1469 0.0180 0.039 Uiso 1 1 calc R . .
C6 C 0.2074(2) 0.19444(15) -0.29834(19) 0.0493(6) Uani 1 1 d . . .
H6A H 0.2640 0.1618 -0.3317 0.074 Uiso 1 1 calc R . .
H6B H 0.2049 0.2500 -0.3253 0.074 Uiso 1 1 calc R . .
H6C H 0.1171 0.1722 -0.3192 0.074 Uiso 1 1 calc R . .
C7 C 0.1804(2) 0.24282(17) -0.1160(2) 0.0608(7) Uani 1 1 d . . .
H7A H 0.2212 0.2414 -0.0353 0.091 Uiso 1 1 calc R . .
H7B H 0.0903 0.2204 -0.1336 0.091 Uiso 1 1 calc R . .
H7C H 0.1761 0.2986 -0.1421 0.091 Uiso 1 1 calc R . .
C8 C 0.8540(2) 0.24562(15) -0.0157(2) 0.0534(7) Uani 1 1 d . . .
H8A H 0.8439 0.2326 -0.0940 0.080 Uiso 1 1 calc R . .
H8B H 0.9399 0.2254 0.0303 0.080 Uiso 1 1 calc R . .
H8C H 0.8503 0.3041 -0.0071 0.080 Uiso 1 1 calc R . .
C9 C 0.7468(3) 0.22886(17) 0.1387(2) 0.0575(7) Uani 1 1 d . . .
H9A H 0.6751 0.2010 0.1597 0.086 Uiso 1 1 calc R . .
H9B H 0.7353 0.2872 0.1436 0.086 Uiso 1 1 calc R . .
H9C H 0.8329 0.2129 0.1894 0.086 Uiso 1 1 calc R . .
C21 C 0.2901(2) -0.00399(10) 0.15683(16) 0.0261(4) Uani 1 1 d . . .
C22 C 0.1964(2) 0.05606(14) 0.1189(2) 0.0489(6) Uani 1 1 d . . .
H22A H 0.2199 0.1023 0.0841 0.059 Uiso 1 1 calc R . .
C23 C 0.0686(3) 0.05013(17) 0.1307(3) 0.0710(9) Uani 1 1 d . . .
H23A H 0.0066 0.0923 0.1041 0.085 Uiso 1 1 calc R . .
C24 C 0.0316(3) -0.01550(16) 0.1799(2) 0.0552(7) Uani 1 1 d . . .
H24A H -0.0561 -0.0195 0.1868 0.066 Uiso 1 1 calc R . .
C25 C 0.1216(2) -0.07545(15) 0.2192(2) 0.0479(6) Uani 1 1 d . . .
H25A H 0.0974 -0.1210 0.2549 0.058 Uiso 1 1 calc R . .
C26 C 0.2489(2) -0.06975(13) 0.20672(19) 0.0397(5) Uani 1 1 d . . .
H26A H 0.3100 -0.1125 0.2334 0.048 Uiso 1 1 calc R . .
C31 C 0.5913(2) 0.00133(10) 0.27393(16) 0.0275(4) Uani 1 1 d . . .
C32 C 0.7190(2) 0.02851(13) 0.27781(18) 0.0354(5) Uani 1 1 d . . .
H32A H 0.7360 0.0461 0.2110 0.042 Uiso 1 1 calc R . .
C33 C 0.8216(2) 0.03043(16) 0.3766(2) 0.0507(6) Uani 1 1 d . . .
H33A H 0.9071 0.0497 0.3769 0.061 Uiso 1 1 calc R . .
C34 C 0.7992(3) 0.00442(15) 0.4739(2) 0.0600(8) Uani 1 1 d . . .
H34A H 0.8688 0.0063 0.5417 0.072 Uiso 1 1 calc R . .
C35 C 0.6756(3) -0.02431(17) 0.47281(19) 0.0563(7) Uani 1 1 d . . .
H35A H 0.6606 -0.0435 0.5396 0.068 Uiso 1 1 calc R . .
C36 C 0.5725(2) -0.02527(14) 0.37399(17) 0.0404(5) Uani 1 1 d . . .
H36A H 0.4874 -0.0445 0.3747 0.048 Uiso 1 1 calc R . .
H H 0.460(2) 0.0977(13) 0.1035(19) 0.050(6) Uiso 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
Ni C1 1.8941(19) . ?
Ni Si 2.1953(8) 3_655 ?
Ni Si 2.2393(9) . ?
Ni Ni 2.5136(12) 3_655 ?
Ni H 1.57(2) . ?
Si C31 1.900(2) . ?
Si C21 1.900(2) . ?
Si Ni 2.1953(8) 3_655 ?
Si H 1.62(2) . ?
N1 C1 1.364(2) . ?
N1 C2 1.388(2) . ?
N1 C5 1.471(2) . ?
N2 C1 1.361(2) . ?
N2 C3 1.387(2) . ?
N2 C4 1.473(2) . ?
C2 C3 1.339(3) . ?
C2 H2A 0.9500 . ?
C3 H3A 0.9500 . ?
C4 C6 1.511(3) . ?
C4 C7 1.515(3) . ?
C4 H4A 1.0000 . ?
C5 C9 1.513(3) . ?
C5 C8 1.517(3) . ?
C5 H5A 1.0000 . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C21 C22 1.386(3) . ?
C21 C26 1.387(3) . ?
C22 C23 1.391(3) . ?
C22 H22A 0.9500 . ?
C23 C24 1.363(4) . ?
C23 H23A 0.9500 . ?
C24 C25 1.364(3) . ?
C24 H24A 0.9500 . ?
C25 C26 1.389(3) . ?
C25 H25A 0.9500 . ?
C26 H26A 0.9500 . ?
C31 C36 1.395(3) . ?
C31 C32 1.400(3) . ?
C32 C33 1.390(3) . ?
C32 H32A 0.9500 . ?
C33 C34 1.375(4) . ?
C33 H33A 0.9500 . ?
C34 C35 1.377(4) . ?
C34 H34A 0.9500 . ?
C35 C36 1.393(3) . ?
C35 H35A 0.9500 . ?
C36 H36A 0.9500 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C1 Ni Si 100.02(6) . 3_655 ?
C1 Ni Si 149.02(6) . . ?
Si Ni Si 110.95(4) 3_655 . ?
C1 Ni Ni 156.32(6) . 3_655 ?
Si Ni Ni 56.30(2) 3_655 3_655 ?
Si Ni Ni 54.65(2) . 3_655 ?
C1 Ni H 102.6(8) . . ?
Si Ni H 157.4(8) 3_655 . ?
Si Ni H 46.5(8) . . ?
Ni Ni H 101.1(8) 3_655 . ?
C31 Si C21 108.34(9) . . ?
C31 Si Ni 114.99(7) . 3_655 ?
C21 Si Ni 118.64(6) . 3_655 ?
C31 Si Ni 119.91(7) . . ?
C21 Si Ni 121.37(6) . . ?
Ni Si Ni 69.05(4) 3_655 . ?
C31 Si H 100.3(8) . . ?
C21 Si H 98.3(8) . . ?
Ni Si H 113.5(8) 3_655 . ?
Ni Si H 44.5(8) . . ?
C1 N1 C2 111.31(16) . . ?
C1 N1 C5 122.23(15) . . ?
C2 N1 C5 126.01(16) . . ?
C1 N2 C3 111.27(16) . . ?
C1 N2 C4 123.29(16) . . ?
C3 N2 C4 125.28(16) . . ?
N2 C1 N1 103.71(15) . . ?
N2 C1 Ni 128.11(14) . . ?
N1 C1 Ni 128.06(13) . . ?
C3 C2 N1 106.67(18) . . ?
C3 C2 H2A 126.7 . . ?
N1 C2 H2A 126.7 . . ?
C2 C3 N2 107.02(18) . . ?
C2 C3 H3A 126.5 . . ?
N2 C3 H3A 126.5 . . ?
N2 C4 C6 111.29(18) . . ?
N2 C4 C7 110.02(18) . . ?
C6 C4 C7 112.26(19) . . ?
N2 C4 H4A 107.7 . . ?
C6 C4 H4A 107.7 . . ?
C7 C4 H4A 107.7 . . ?
N1 C5 C9 110.08(18) . . ?
N1 C5 C8 111.11(17) . . ?
C9 C5 C8 112.15(19) . . ?
N1 C5 H5A 107.8 . . ?
C9 C5 H5A 107.8 . . ?
C8 C5 H5A 107.8 . . ?
C4 C6 H6A 109.5 . . ?
C4 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
C4 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
C4 C7 H7A 109.5 . . ?
C4 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
C4 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
C5 C8 H8A 109.5 . . ?
C5 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C5 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C5 C9 H9A 109.5 . . ?
C5 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
C5 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C22 C21 C26 116.1(2) . . ?
C22 C21 Si 120.86(16) . . ?
C26 C21 Si 122.90(15) . . ?
C21 C22 C23 121.5(2) . . ?
C21 C22 H22A 119.3 . . ?
C23 C22 H22A 119.3 . . ?
C24 C23 C22 120.7(2) . . ?
C24 C23 H23A 119.6 . . ?
C22 C23 H23A 119.6 . . ?
C23 C24 C25 119.4(2) . . ?
C23 C24 H24A 120.3 . . ?
C25 C24 H24A 120.3 . . ?
C24 C25 C26 119.8(2) . . ?
C24 C25 H25A 120.1 . . ?
C26 C25 H25A 120.1 . . ?
C21 C26 C25 122.4(2) . . ?
C21 C26 H26A 118.8 . . ?
C25 C26 H26A 118.8 . . ?
C36 C31 C32 116.7(2) . . ?
C36 C31 Si 126.16(17) . . ?
C32 C31 Si 117.16(15) . . ?
C33 C32 C31 121.9(2) . . ?
C33 C32 H32A 119.1 . . ?
C31 C32 H32A 119.1 . . ?
C34 C33 C32 119.9(2) . . ?
C34 C33 H33A 120.0 . . ?
C32 C33 H33A 120.0 . . ?
C33 C34 C35 119.8(2) . . ?
C33 C34 H34A 120.1 . . ?
C35 C34 H34A 120.1 . . ?
C34 C35 C36 120.2(2) . . ?
C34 C35 H35A 119.9 . . ?
C36 C35 H35A 119.9 . . ?
C35 C36 C31 121.5(2) . . ?
C35 C36 H36A 119.2 . . ?
C31 C36 H36A 119.2 . . ?

_diffrn_measured_fraction_theta_max 0.986
_diffrn_reflns_theta_full        26.00
_diffrn_measured_fraction_theta_full 1.000
_refine_diff_density_max         0.443
_refine_diff_density_min         -0.212
_refine_diff_density_rms         0.056
_database_code_depnum_ccdc_archive 'CCDC 997523'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_compound_cis7

_audit_creation_method           'SHELXL-97 + manual editing'
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         C79H120N8Ni2Si2
_chemical_formula_sum            'C79 H120 N8 Ni2 Si2'
_chemical_formula_weight         1355.43

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'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   C2/c

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

_cell_length_a                   41.417(8)
_cell_length_b                   11.756(2)
_cell_length_c                   16.723(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 104.22(3)
_cell_angle_gamma                90.00
_cell_volume                     7893(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    8733
_cell_measurement_theta_min      2.695
_cell_measurement_theta_max      25.4435

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.10
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.141
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2936
_exptl_absorpt_coefficient_mu    0.552
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6628
_exptl_absorpt_correction_T_max  0.7453
_exptl_absorpt_process_details   'SadAbs-2008/1 (Bruker, 2008)'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      173(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_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            82571
_diffrn_reflns_av_R_equivalents  0.0497
_diffrn_reflns_av_sigmaI/netI    0.0228
_diffrn_reflns_limit_h_min       -50
_diffrn_reflns_limit_h_max       50
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         1.01
_diffrn_reflns_theta_max         26.09
_reflns_number_total             7787
_reflns_number_gt                6614
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Smart-NT v. 5.63'
_computing_cell_refinement       'Saint-NT v. 7.23'
_computing_data_reduction        'Saint-NT v. 7.23'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'XP in ShelxTL-97'
_computing_publication_material  'XP in ShelxTL-97'

_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)+(0.0535P)²+6.3641P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         7787
_refine_ls_number_parameters     434
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0463
_refine_ls_R_factor_gt           0.0373
_refine_ls_wR_factor_ref         0.1019
_refine_ls_wR_factor_gt          0.0930
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_restrained_S_all      1.056
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni Ni 0.135877(5) 0.667789(18) 0.459373(13) 0.02219(8) Uani 1 1 d . . .
Si Si 0.158780(12) 0.82380(4) 0.52401(3) 0.02301(12) Uani 1 1 d . . .
N1 N 0.17738(4) 0.66641(14) 0.33807(10) 0.0324(4) Uani 1 1 d . . .
N2 N 0.12549(4) 0.67902(14) 0.27837(10) 0.0338(4) Uani 1 1 d . . .
N3 N 0.11239(4) 0.42701(13) 0.44466(10) 0.0327(4) Uani 1 1 d . . .
N4 N 0.07366(4) 0.54154(14) 0.45643(10) 0.0329(4) Uani 1 1 d . . .
C1 C 0.14696(5) 0.67317(14) 0.35533(11) 0.0256(4) Uani 1 1 d . . .
C2 C 0.17474(6) 0.6676(2) 0.25358(14) 0.0499(6) Uani 1 1 d . . .
H2A H 0.1926 0.6639 0.2272 0.060 Uiso 1 1 calc R . .
C3 C 0.14233(6) 0.6749(2) 0.21650(13) 0.0491(6) Uani 1 1 d . . .
H3 H 0.1327 0.6768 0.1588 0.059 Uiso 1 1 calc R . .
C4 C 0.20936(5) 0.66482(17) 0.40075(13) 0.0341(4) Uani 1 1 d . . .
H4A H 0.2045 0.6718 0.4562 0.041 Uiso 1 1 calc R . .
C5 C 0.08905(5) 0.68643(19) 0.26338(13) 0.0408(5) Uani 1 1 d . . .
H5A H 0.0835 0.6977 0.3178 0.049 Uiso 1 1 calc R . .
C6 C 0.23039(6) 0.7669(2) 0.38914(15) 0.0470(6) Uani 1 1 d . . .
H6A H 0.2184 0.8372 0.3945 0.070 Uiso 1 1 calc R . .
H6B H 0.2348 0.7637 0.3342 0.070 Uiso 1 1 calc R . .
H6C H 0.2515 0.7654 0.4312 0.070 Uiso 1 1 calc R . .
C7 C 0.22758(6) 0.5529(2) 0.39868(16) 0.0505(6) Uani 1 1 d . . .
H7A H 0.2131 0.4896 0.4058 0.076 Uiso 1 1 calc R . .
H7B H 0.2479 0.5517 0.4434 0.076 Uiso 1 1 calc R . .
H7C H 0.2334 0.5452 0.3455 0.076 Uiso 1 1 calc R . .
C8 C 0.07567(8) 0.7883(3) 0.2092(2) 0.0772(9) Uani 1 1 d . . .
H8A H 0.0518 0.7967 0.2053 0.116 Uiso 1 1 calc R . .
H8B H 0.0792 0.7765 0.1539 0.116 Uiso 1 1 calc R . .
H8C H 0.0874 0.8572 0.2334 0.116 Uiso 1 1 calc R . .
C9 C 0.07277(6) 0.5781(2) 0.22643(19) 0.0637(7) Uani 1 1 d . . .
H9A H 0.0486 0.5850 0.2172 0.096 Uiso 1 1 calc R . .
H9B H 0.0807 0.5148 0.2642 0.096 Uiso 1 1 calc R . .
H9C H 0.0784 0.5639 0.1737 0.096 Uiso 1 1 calc R . .
C11 C 0.10604(4) 0.54013(15) 0.45073(11) 0.0262(4) Uani 1 1 d . . .
C12 C 0.08499(6) 0.36090(19) 0.44788(16) 0.0482(6) Uani 1 1 d . . .
H12A H 0.0837 0.2803 0.4454 0.058 Uiso 1 1 calc R . .
C13 C 0.06074(5) 0.43288(19) 0.45511(16) 0.0475(6) Uani 1 1 d . . .
H13A H 0.0389 0.4130 0.4586 0.057 Uiso 1 1 calc R . .
C14 C 0.14406(5) 0.38305(17) 0.43172(13) 0.0360(5) Uani 1 1 d . . .
H14A H 0.1599 0.4483 0.4367 0.043 Uiso 1 1 calc R . .
C15 C 0.05588(5) 0.64743(18) 0.46701(13) 0.0361(5) Uani 1 1 d . . .
H15A H 0.0708 0.7130 0.4635 0.043 Uiso 1 1 calc R . .
C16 C 0.15928(6) 0.2962(2) 0.49749(16) 0.0559(6) Uani 1 1 d . . .
H16A H 0.1632 0.3316 0.5521 0.084 Uiso 1 1 calc R . .
H16B H 0.1805 0.2693 0.4884 0.084 Uiso 1 1 calc R . .
H16C H 0.1440 0.2318 0.4944 0.084 Uiso 1 1 calc R . .
C17 C 0.13879(7) 0.3341(2) 0.34525(16) 0.0579(7) Uani 1 1 d . . .
H17A H 0.1311 0.3944 0.3045 0.087 Uiso 1 1 calc R . .
H17B H 0.1220 0.2737 0.3374 0.087 Uiso 1 1 calc R . .
H17C H 0.1598 0.3028 0.3381 0.087 Uiso 1 1 calc R . .
C18 C 0.02418(6) 0.6607(2) 0.39824(16) 0.0586(7) Uani 1 1 d . . .
H18A H 0.0296 0.6539 0.3446 0.088 Uiso 1 1 calc R . .
H18B H 0.0143 0.7356 0.4025 0.088 Uiso 1 1 calc R . .
H18C H 0.0083 0.6012 0.4034 0.088 Uiso 1 1 calc R . .
C19 C 0.04850(6) 0.6503(2) 0.55147(15) 0.0474(6) Uani 1 1 d . . .
H19A H 0.0693 0.6414 0.5941 0.071 Uiso 1 1 calc R . .
H19B H 0.0332 0.5882 0.5558 0.071 Uiso 1 1 calc R . .
H19C H 0.0382 0.7233 0.5590 0.071 Uiso 1 1 calc R . .
C21 C 0.12108(4) 0.92206(15) 0.51561(11) 0.0249(4) Uani 1 1 d . . .
C22 C 0.10181(4) 0.92269(16) 0.57506(11) 0.0284(4) Uani 1 1 d . . .
C23 C 0.07244(5) 0.98625(16) 0.56137(13) 0.0338(4) Uani 1 1 d . . .
H23A H 0.0599 0.9851 0.6018 0.041 Uiso 1 1 calc R . .
C24 C 0.06097(5) 1.05119(17) 0.49054(14) 0.0379(5) Uani 1 1 d . . .
C25 C 0.07976(5) 1.05015(16) 0.43206(13) 0.0358(5) Uani 1 1 d . . .
H25 H 0.0723 1.0933 0.3830 0.043 Uiso 1 1 calc R . .
C26 C 0.10919(5) 0.98788(15) 0.44305(11) 0.0300(4) Uani 1 1 d . . .
C27 C 0.11243(5) 0.85753(19) 0.65522(12) 0.0355(4) Uani 1 1 d . . .
H27A H 0.1194 0.7807 0.6441 0.053 Uiso 1 1 calc R . .
H27B H 0.0937 0.8526 0.6812 0.053 Uiso 1 1 calc R . .
H27C H 0.1311 0.8970 0.6923 0.053 Uiso 1 1 calc R . .
C28 C 0.02942(6) 1.1218(2) 0.47789(17) 0.0532(6) Uani 1 1 d . . .
H28A H 0.0291 1.1614 0.5293 0.080 Uiso 1 1 calc R . .
H28B H 0.0099 1.0718 0.4622 0.080 Uiso 1 1 calc R . .
H28C H 0.0288 1.1777 0.4341 0.080 Uiso 1 1 calc R . .
C29 C 0.12785(6) 0.99268(18) 0.37566(12) 0.0419(5) Uani 1 1 d . . .
H29A H 0.1330 0.9152 0.3610 0.063 Uiso 1 1 calc R . .
H29B H 0.1486 1.0353 0.3955 0.063 Uiso 1 1 calc R . .
H29C H 0.1140 1.0306 0.3270 0.063 Uiso 1 1 calc R . .
C31 C 0.18612(4) 0.82652(15) 0.63569(11) 0.0259(4) Uani 1 1 d . . .
C32 C 0.19764(4) 0.72678(17) 0.68127(12) 0.0318(4) Uani 1 1 d . . .
C33 C 0.21634(5) 0.7348(2) 0.76336(13) 0.0427(5) Uani 1 1 d . . .
H33A H 0.2237 0.6667 0.7929 0.051 Uiso 1 1 calc R . .
C34 C 0.22451(6) 0.8381(2) 0.80291(13) 0.0469(6) Uani 1 1 d . . .
C35 C 0.21447(5) 0.9358(2) 0.75737(13) 0.0433(5) Uani 1 1 d . . .
H35A H 0.2204 1.0077 0.7827 0.052 Uiso 1 1 calc R . .
C36 C 0.19588(5) 0.93222(17) 0.67531(12) 0.0332(4) Uani 1 1 d . . .
C37 C 0.19149(6) 0.60855(18) 0.64558(15) 0.0440(5) Uani 1 1 d . . .
H37A H 0.2096 0.5581 0.6735 0.066 Uiso 1 1 calc R . .
H37B H 0.1906 0.6109 0.5865 0.066 Uiso 1 1 calc R . .
H37C H 0.1703 0.5798 0.6535 0.066 Uiso 1 1 calc R . .
C38 C 0.24391(8) 0.8438(3) 0.89285(16) 0.0794(10) Uani 1 1 d . . .
H38A H 0.2518 0.7676 0.9119 0.119 Uiso 1 1 calc R . .
H38B H 0.2294 0.8728 0.9265 0.119 Uiso 1 1 calc R . .
H38C H 0.2630 0.8948 0.8980 0.119 Uiso 1 1 calc R . .
C39 C 0.18667(6) 1.04445(17) 0.63152(14) 0.0439(5) Uani 1 1 d . . .
H39A H 0.2000 1.1055 0.6635 0.066 Uiso 1 1 calc R . .
H39B H 0.1630 1.0598 0.6261 0.066 Uiso 1 1 calc R . .
H39C H 0.1911 1.0408 0.5766 0.066 Uiso 1 1 calc R . .
C100 C 0.0000 0.9802(4) 0.2500 0.1049(18) Uani 1 2 d S . .
H10A H 0.0212 0.9525 0.2416 0.157 Uiso 0.50 1 calc PR . .
H10B H -0.0183 0.9525 0.2054 0.157 Uiso 0.50 1 calc PR . .
H10C H -0.0029 0.9525 0.3030 0.157 Uiso 0.50 1 calc PR . .
C101 C 0.0000 1.1071(3) 0.2500 0.0495(8) Uani 1 2 d S . .
C102 C 0.02716(6) 1.1680(3) 0.23875(15) 0.0557(7) Uani 1 1 d . . .
H10D H 0.0461 1.1284 0.2307 0.067 Uiso 1 1 calc R . .
C103 C 0.02705(9) 1.2841(3) 0.23913(17) 0.0776(10) Uani 1 1 d . . .
H10E H 0.0460 1.3246 0.2318 0.093 Uiso 1 1 calc R . .
C104 C 0.0000 1.3424(4) 0.2500 0.0911(17) Uani 1 2 d S . .
H10F H 0.0000 1.4232 0.2500 0.109 Uiso 1 2 calc SR . .
H1 H 0.1796(5) 0.8858(18) 0.4838(12) 0.037(5) Uiso 1 1 d . . .
H2 H 0.1325(5) 0.6899(18) 0.5386(13) 0.040(6) Uiso 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
Ni C1 1.9065(19) . ?
Ni C11 1.9268(18) . ?
Ni Si 2.2199(7) . ?
Ni H2 1.39(2) . ?
Si C21 1.9193(18) . ?
Si C31 1.932(2) . ?
Si H1 1.42(2) . ?
Si H2 1.96(2) . ?
N1 C1 1.362(2) . ?
N1 C2 1.390(3) . ?
N1 C4 1.474(3) . ?
N2 C1 1.375(2) . ?
N2 C3 1.384(3) . ?
N2 C5 1.471(3) . ?
N3 C11 1.364(2) . ?
N3 C12 1.387(3) . ?
N3 C14 1.474(2) . ?
N4 C11 1.368(2) . ?
N4 C13 1.383(3) . ?
N4 C15 1.479(2) . ?
C2 C3 1.336(3) . ?
C2 H2A 0.9500 . ?
C3 H3 0.9500 . ?
C4 C7 1.522(3) . ?
C4 C6 1.523(3) . ?
C4 H4A 1.0000 . ?
C5 C9 1.501(3) . ?
C5 C8 1.522(3) . ?
C5 H5A 1.0000 . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C12 C13 1.341(3) . ?
C12 H12A 0.9500 . ?
C13 H13A 0.9500 . ?
C14 C16 1.519(3) . ?
C14 C17 1.521(3) . ?
C14 H14A 1.0000 . ?
C15 C19 1.517(3) . ?
C15 C18 1.526(3) . ?
C15 H15A 1.0000 . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
C21 C22 1.420(3) . ?
C21 C26 1.421(3) . ?
C22 C23 1.398(3) . ?
C22 C27 1.512(3) . ?
C23 C24 1.391(3) . ?
C23 H23A 0.9500 . ?
C24 C25 1.391(3) . ?
C24 C28 1.518(3) . ?
C25 C26 1.395(3) . ?
C25 H25 0.9500 . ?
C26 C29 1.516(3) . ?
C27 H27A 0.9800 . ?
C27 H27B 0.9800 . ?
C27 H27C 0.9800 . ?
C28 H28A 0.9800 . ?
C28 H28B 0.9800 . ?
C28 H28C 0.9800 . ?
C29 H29A 0.9800 . ?
C29 H29B 0.9800 . ?
C29 H29C 0.9800 . ?
C31 C32 1.416(3) . ?
C31 C36 1.419(3) . ?
C32 C33 1.404(3) . ?
C32 C37 1.509(3) . ?
C33 C34 1.384(3) . ?
C33 H33A 0.9500 . ?
C34 C35 1.384(3) . ?
C34 C38 1.523(3) . ?
C35 C36 1.400(3) . ?
C35 H35A 0.9500 . ?
C36 C39 1.512(3) . ?
C37 H37A 0.9800 . ?
C37 H37B 0.9800 . ?
C37 H37C 0.9800 . ?
C38 H38A 0.9800 . ?
C38 H38B 0.9800 . ?
C38 H38C 0.9800 . ?
C39 H39A 0.9800 . ?
C39 H39B 0.9800 . ?
C39 H39C 0.9800 . ?
C100 C101 1.491(6) . ?
C100 H10A 0.9800 . ?
C100 H10B 0.9800 . ?
C100 H10C 0.9800 . ?
C101 C102 1.385(3) 2 ?
C101 C102 1.385(3) . ?
C102 C103 1.365(4) . ?
C102 H10D 0.9500 . ?
C103 C104 1.363(4) . ?
C103 H10E 0.9500 . ?
C104 C103 1.363(4) 2 ?
C104 H10F 0.9500 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C1 Ni C11 104.55(8) . . ?
C1 Ni Si 104.30(5) . . ?
C11 Ni Si 150.40(6) . . ?
C1 Ni H2 165.2(9) . . ?
C11 Ni H2 90.2(9) . . ?
Si Ni H2 60.9(9) . . ?
C21 Si C31 109.50(8) . . ?
C21 Si Ni 102.65(6) . . ?
C31 Si Ni 124.28(6) . . ?
C21 Si H1 103.6(8) . . ?
C31 Si H1 99.8(8) . . ?
Ni Si H1 115.5(8) . . ?
C21 Si H2 91.5(6) . . ?
C31 Si H2 96.0(6) . . ?
Ni Si H2 38.2(6) . . ?
H1 Si H2 153.1(10) . . ?
C1 N1 C2 111.65(17) . . ?
C1 N1 C4 124.50(16) . . ?
C2 N1 C4 123.76(17) . . ?
C1 N2 C3 111.67(17) . . ?
C1 N2 C5 124.30(17) . . ?
C3 N2 C5 124.02(18) . . ?
C11 N3 C12 111.63(16) . . ?
C11 N3 C14 123.18(15) . . ?
C12 N3 C14 125.10(17) . . ?
C11 N4 C13 111.70(16) . . ?
C11 N4 C15 122.96(16) . . ?
C13 N4 C15 125.27(16) . . ?
N1 C1 N2 102.94(16) . . ?
N1 C1 Ni 129.36(14) . . ?
N2 C1 Ni 127.63(14) . . ?
C3 C2 N1 106.95(19) . . ?
C3 C2 H2A 126.5 . . ?
N1 C2 H2A 126.5 . . ?
C2 C3 N2 106.78(19) . . ?
C2 C3 H3 126.6 . . ?
N2 C3 H3 126.6 . . ?
N1 C4 C7 111.04(17) . . ?
N1 C4 C6 109.99(18) . . ?
C7 C4 C6 112.08(18) . . ?
N1 C4 H4A 107.9 . . ?
C7 C4 H4A 107.9 . . ?
C6 C4 H4A 107.9 . . ?
N2 C5 C9 111.00(19) . . ?
N2 C5 C8 110.9(2) . . ?
C9 C5 C8 111.2(2) . . ?
N2 C5 H5A 107.9 . . ?
C9 C5 H5A 107.9 . . ?
C8 C5 H5A 107.9 . . ?
C4 C6 H6A 109.5 . . ?
C4 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
C4 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
C4 C7 H7A 109.5 . . ?
C4 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
C4 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
C5 C8 H8A 109.5 . . ?
C5 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C5 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C5 C9 H9A 109.5 . . ?
C5 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
C5 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
N3 C11 N4 103.14(15) . . ?
N3 C11 Ni 129.27(13) . . ?
N4 C11 Ni 127.38(13) . . ?
C13 C12 N3 106.73(19) . . ?
C13 C12 H12A 126.6 . . ?
N3 C12 H12A 126.6 . . ?
C12 C13 N4 106.79(18) . . ?
C12 C13 H13A 126.6 . . ?
N4 C13 H13A 126.6 . . ?
N3 C14 C16 110.80(18) . . ?
N3 C14 C17 110.30(18) . . ?
C16 C14 C17 111.80(19) . . ?
N3 C14 H14A 107.9 . . ?
C16 C14 H14A 107.9 . . ?
C17 C14 H14A 107.9 . . ?
N4 C15 C19 110.50(17) . . ?
N4 C15 C18 110.95(18) . . ?
C19 C15 C18 111.49(19) . . ?
N4 C15 H15A 107.9 . . ?
C19 C15 H15A 107.9 . . ?
C18 C15 H15A 107.9 . . ?
C14 C16 H16A 109.5 . . ?
C14 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
C14 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C14 C17 H17A 109.5 . . ?
C14 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
C14 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C15 C18 H18A 109.5 . . ?
C15 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
C15 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C15 C19 H19A 109.5 . . ?
C15 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
C15 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C22 C21 C26 117.29(16) . . ?
C22 C21 Si 122.62(14) . . ?
C26 C21 Si 119.68(14) . . ?
C23 C22 C21 120.30(17) . . ?
C23 C22 C27 117.88(17) . . ?
C21 C22 C27 121.80(16) . . ?
C24 C23 C22 122.29(19) . . ?
C24 C23 H23A 118.9 . . ?
C22 C23 H23A 118.9 . . ?
C23 C24 C25 117.44(18) . . ?
C23 C24 C28 121.4(2) . . ?
C25 C24 C28 121.2(2) . . ?
C24 C25 C26 122.24(18) . . ?
C24 C25 H25 118.9 . . ?
C26 C25 H25 118.9 . . ?
C25 C26 C21 120.43(18) . . ?
C25 C26 C29 118.11(17) . . ?
C21 C26 C29 121.46(17) . . ?
C22 C27 H27A 109.5 . . ?
C22 C27 H27B 109.5 . . ?
H27A C27 H27B 109.5 . . ?
C22 C27 H27C 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
C24 C28 H28A 109.5 . . ?
C24 C28 H28B 109.5 . . ?
H28A C28 H28B 109.5 . . ?
C24 C28 H28C 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
C26 C29 H29A 109.5 . . ?
C26 C29 H29B 109.5 . . ?
H29A C29 H29B 109.5 . . ?
C26 C29 H29C 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
C32 C31 C36 117.00(17) . . ?
C32 C31 Si 123.14(14) . . ?
C36 C31 Si 119.85(14) . . ?
C33 C32 C31 120.20(19) . . ?
C33 C32 C37 116.57(18) . . ?
C31 C32 C37 123.22(18) . . ?
C34 C33 C32 122.5(2) . . ?
C34 C33 H33A 118.7 . . ?
C32 C33 H33A 118.7 . . ?
C35 C34 C33 117.4(2) . . ?
C35 C34 C38 121.4(2) . . ?
C33 C34 C38 121.2(2) . . ?
C34 C35 C36 122.2(2) . . ?
C34 C35 H35A 118.9 . . ?
C36 C35 H35A 118.9 . . ?
C35 C36 C31 120.58(19) . . ?
C35 C36 C39 117.48(19) . . ?
C31 C36 C39 121.94(17) . . ?
C32 C37 H37A 109.5 . . ?
C32 C37 H37B 109.5 . . ?
H37A C37 H37B 109.5 . . ?
C32 C37 H37C 109.5 . . ?
H37A C37 H37C 109.5 . . ?
H37B C37 H37C 109.5 . . ?
C34 C38 H38A 109.5 . . ?
C34 C38 H38B 109.5 . . ?
H38A C38 H38B 109.5 . . ?
C34 C38 H38C 109.5 . . ?
H38A C38 H38C 109.5 . . ?
H38B C38 H38C 109.5 . . ?
C36 C39 H39A 109.5 . . ?
C36 C39 H39B 109.5 . . ?
H39A C39 H39B 109.5 . . ?
C36 C39 H39C 109.5 . . ?
H39A C39 H39C 109.5 . . ?
H39B C39 H39C 109.5 . . ?
C101 C100 H10A 109.5 . . ?
C101 C100 H10B 109.5 . . ?
H10A C100 H10B 109.5 . . ?
C101 C100 H10C 109.5 . . ?
H10A C100 H10C 109.5 . . ?
H10B C100 H10C 109.5 . . ?
C102 C101 C102 117.7(4) 2 . ?
C102 C101 C100 121.14(18) 2 . ?
C102 C101 C100 121.14(18) . . ?
C103 C102 C101 120.8(3) . . ?
C103 C102 H10D 119.6 . . ?
C101 C102 H10D 119.6 . . ?
C104 C103 C102 120.5(3) . . ?
C104 C103 H10E 119.8 . . ?
C102 C103 H10E 119.8 . . ?
C103 C104 C103 119.6(5) 2 . ?
C103 C104 H10F 120.2 2 . ?
C103 C104 H10F 120.2 . . ?

_diffrn_measured_fraction_theta_max 0.992
_diffrn_reflns_theta_full        26.00
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         0.492
_refine_diff_density_min         -0.186
_refine_diff_density_rms         0.058
_database_code_depnum_ccdc_archive 'CCDC 997524'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_cis_9

_audit_creation_method           'SHELXL-97 + manual editing'
_chemical_name_systematic        
; 

;
_chemical_formula_moiety         C22H46N4NiSi2
_chemical_formula_sum            'C22 H46 N4 Ni Si2'
_chemical_formula_weight         481.52

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'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   C2/c

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

_cell_length_a                   32.548(7)
_cell_length_b                   9.6502(19)
_cell_length_c                   18.368(4)
_cell_angle_alpha                90.00
_cell_angle_beta                 99.54(3)
_cell_angle_gamma                90.00
_cell_volume                     5689(2)
_cell_formula_units_Z            8
_cell_measurement_temperature    203(2)
_cell_measurement_reflns_used    8000
_cell_measurement_theta_min      2.25
_cell_measurement_theta_max      25.85

_exptl_crystal_description       prism
_exptl_crystal_colour            orange
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.20
_exptl_crystal_density_diffrn    1.124
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2096
_exptl_absorpt_coefficient_mu    0.780
_exptl_absorpt_correction_type   none

_diffrn_ambient_temperature      203(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  'STOE IPDS 1'
_diffrn_measurement_method       rotation
_diffrn_detector_area_resol_mean 6.67
_diffrn_reflns_number            17280
_diffrn_reflns_av_R_equivalents  0.0448
_diffrn_reflns_av_sigmaI/netI    0.0388
_diffrn_reflns_limit_h_min       -37
_diffrn_reflns_limit_h_max       39
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         2.20
_diffrn_reflns_theta_max         25.95
_reflns_number_total             5357
_reflns_number_gt                4120
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'STOE X-AREA'
_computing_cell_refinement       'STOE X-AREA'
_computing_data_reduction        'STOE X-RED'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'SHELXL-97 (Sheldrick, 1997)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'

_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)+(0.0585P)²+0.3934P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         5357
_refine_ls_number_parameters     270
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0563
_refine_ls_R_factor_gt           0.0371
_refine_ls_wR_factor_ref         0.0952
_refine_ls_wR_factor_gt          0.0872
_refine_ls_goodness_of_fit_ref   1.000
_refine_ls_restrained_S_all      1.000
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni1 Ni 0.124195(9) 0.32585(3) 0.059868(14) 0.02764(10) Uani 1 1 d . . .
Si1 Si 0.08322(2) 0.38383(7) -0.04621(3) 0.03397(16) Uani 1 1 d . . .
Si2 Si 0.16308(2) 0.49780(7) 0.02492(4) 0.03631(17) Uani 1 1 d . . .
C1 C 0.10437(8) 0.1372(2) 0.05453(12) 0.0311(5) Uani 1 1 d . . .
C2 C 0.09940(9) -0.0911(3) 0.02413(17) 0.0486(7) Uani 1 1 d . . .
H2A H 0.1045 -0.1766 0.0028 0.058 Uiso 1 1 calc R . .
C3 C 0.07179(9) -0.0664(3) 0.06860(17) 0.0506(7) Uani 1 1 d . . .
H3A H 0.0536 -0.1311 0.0844 0.061 Uiso 1 1 calc R . .
C4 C 0.05145(9) 0.1440(3) 0.13750(15) 0.0493(7) Uani 1 1 d . . .
H4A H 0.0572 0.2443 0.1339 0.059 Uiso 1 1 calc R . .
C5 C 0.06729(14) 0.1013(6) 0.21654(19) 0.1012(16) Uani 1 1 d . . .
H5A H 0.0971 0.1176 0.2280 0.152 Uiso 1 1 calc R . .
H5B H 0.0617 0.0036 0.2226 0.152 Uiso 1 1 calc R . .
H5C H 0.0533 0.1553 0.2496 0.152 Uiso 1 1 calc R . .
C6 C 0.00514(10) 0.1248(4) 0.1142(2) 0.0724(10) Uani 1 1 d . . .
H6A H -0.0029 0.1542 0.0634 0.109 Uiso 1 1 calc R . .
H6B H -0.0096 0.1800 0.1457 0.109 Uiso 1 1 calc R . .
H6C H -0.0019 0.0278 0.1187 0.109 Uiso 1 1 calc R . .
C7 C 0.15059(10) 0.0522(3) -0.03208(15) 0.0499(7) Uani 1 1 d . . .
H7A H 0.1613 0.1481 -0.0252 0.060 Uiso 1 1 calc R . .
C8 C 0.13153(15) 0.0349(5) -0.11289(19) 0.0947(15) Uani 1 1 d . . .
H8A H 0.1086 0.0995 -0.1254 0.142 Uiso 1 1 calc R . .
H8B H 0.1213 -0.0591 -0.1214 0.142 Uiso 1 1 calc R . .
H8C H 0.1525 0.0533 -0.1435 0.142 Uiso 1 1 calc R . .
C9 C 0.18692(10) -0.0457(4) -0.01099(19) 0.0657(9) Uani 1 1 d . . .
H9A H 0.1990 -0.0312 0.0404 0.099 Uiso 1 1 calc R . .
H9B H 0.2078 -0.0279 -0.0419 0.099 Uiso 1 1 calc R . .
H9C H 0.1773 -0.1406 -0.0179 0.099 Uiso 1 1 calc R . .
C10 C 0.14747(8) 0.3390(2) 0.16281(12) 0.0341(5) Uani 1 1 d . . .
C11 C 0.18060(9) 0.2997(3) 0.27963(13) 0.0456(7) Uani 1 1 d . . .
H11A H 0.1991 0.2612 0.3192 0.055 Uiso 1 1 calc R . .
C12 C 0.15260(10) 0.3983(3) 0.28375(13) 0.0512(7) Uani 1 1 d . . .
H12A H 0.1474 0.4427 0.3269 0.061 Uiso 1 1 calc R . .
C13 C 0.10199(14) 0.5340(4) 0.19232(17) 0.0910(15) Uani 1 1 d . . .
H13A H 0.0957 0.5391 0.1378 0.109 Uiso 1 1 calc R . .
C14 C 0.06166(14) 0.5015(5) 0.2209(3) 0.119(2) Uani 1 1 d . . .
H14A H 0.0508 0.4132 0.2010 0.178 Uiso 1 1 calc R . .
H14B H 0.0414 0.5738 0.2055 0.178 Uiso 1 1 calc R . .
H14C H 0.0672 0.4966 0.2744 0.178 Uiso 1 1 calc R . .
C15 C 0.11972(18) 0.6743(4) 0.2215(2) 0.1099(19) Uani 1 1 d . . .
H15A H 0.1451 0.6933 0.2022 0.165 Uiso 1 1 calc R . .
H15B H 0.1258 0.6717 0.2750 0.165 Uiso 1 1 calc R . .
H15C H 0.0995 0.7465 0.2059 0.165 Uiso 1 1 calc R . .
C16 C 0.20264(9) 0.1599(3) 0.17596(13) 0.0415(6) Uani 1 1 d . . .
H16A H 0.1946 0.1600 0.1216 0.050 Uiso 1 1 calc R . .
C17 C 0.24841(10) 0.1966(4) 0.19347(19) 0.0678(9) Uani 1 1 d . . .
H17A H 0.2527 0.2886 0.1748 0.102 Uiso 1 1 calc R . .
H17B H 0.2644 0.1299 0.1703 0.102 Uiso 1 1 calc R . .
H17C H 0.2574 0.1948 0.2465 0.102 Uiso 1 1 calc R . .
C18 C 0.19365(13) 0.0167(3) 0.2033(2) 0.0716(10) Uani 1 1 d . . .
H18A H 0.1641 -0.0025 0.1906 0.107 Uiso 1 1 calc R . .
H18B H 0.2020 0.0126 0.2564 0.107 Uiso 1 1 calc R . .
H18C H 0.2092 -0.0517 0.1802 0.107 Uiso 1 1 calc R . .
C19 C 0.05217(13) 0.5472(4) -0.0368(3) 0.1088(18) Uani 1 1 d . . .
H19A H 0.0349 0.5685 -0.0837 0.163 Uiso 1 1 calc R . .
H19B H 0.0711 0.6236 -0.0221 0.163 Uiso 1 1 calc R . .
H19C H 0.0346 0.5331 0.0004 0.163 Uiso 1 1 calc R . .
C20 C 0.03958(10) 0.2591(3) -0.08303(17) 0.0582(8) Uani 1 1 d . . .
H20A H 0.0241 0.2949 -0.1288 0.087 Uiso 1 1 calc R . .
H20B H 0.0210 0.2491 -0.0471 0.087 Uiso 1 1 calc R . .
H20C H 0.0513 0.1695 -0.0920 0.087 Uiso 1 1 calc R . .
C21 C 0.20032(10) 0.4111(3) -0.02982(19) 0.0607(8) Uani 1 1 d . . .
H21A H 0.2181 0.4806 -0.0466 0.091 Uiso 1 1 calc R . .
H21B H 0.1846 0.3640 -0.0721 0.091 Uiso 1 1 calc R . .
H21C H 0.2173 0.3444 0.0012 0.091 Uiso 1 1 calc R . .
C22 C 0.19937(11) 0.5999(3) 0.09736(19) 0.0678(9) Uani 1 1 d . . .
H22A H 0.2138 0.6700 0.0733 0.102 Uiso 1 1 calc R . .
H22B H 0.2196 0.5376 0.1250 0.102 Uiso 1 1 calc R . .
H22C H 0.1833 0.6443 0.1308 0.102 Uiso 1 1 calc R . .
N1 N 0.11917(7) 0.03358(19) 0.01546(11) 0.0363(5) Uani 1 1 d . . .
N2 N 0.07499(7) 0.0728(2) 0.08718(11) 0.0386(5) Uani 1 1 d . . .
N3 N 0.17727(6) 0.26428(19) 0.20533(10) 0.0338(4) Uani 1 1 d . . .
N4 N 0.13252(8) 0.4231(2) 0.21272(10) 0.0489(6) Uani 1 1 d . . .
H2 H 0.1460(9) 0.607(3) -0.0248(15) 0.052(8) Uiso 1 1 d . . .
H1 H 0.1033(9) 0.408(3) -0.1068(15) 0.053(8) Uiso 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
Ni1 C10 1.921(2) . ?
Ni1 C1 1.928(2) . ?
Ni1 Si1 2.2419(10) . ?
Ni1 Si2 2.2442(8) . ?
Si1 C19 1.896(4) . ?
Si1 C20 1.899(3) . ?
Si1 H1 1.40(3) . ?
Si2 C21 1.893(3) . ?
Si2 C22 1.902(3) . ?
Si2 H2 1.44(3) . ?
C1 N2 1.360(3) . ?
C1 N1 1.364(3) . ?
C2 C3 1.332(4) . ?
C2 N1 1.386(3) . ?
C2 H2A 0.9400 . ?
C3 N2 1.385(3) . ?
C3 H3A 0.9400 . ?
C4 N2 1.466(3) . ?
C4 C6 1.508(4) . ?
C4 C5 1.515(4) . ?
C4 H4A 0.9900 . ?
C5 H5A 0.9700 . ?
C5 H5B 0.9700 . ?
C5 H5C 0.9700 . ?
C6 H6A 0.9700 . ?
C6 H6B 0.9700 . ?
C6 H6C 0.9700 . ?
C7 N1 1.462(3) . ?
C7 C9 1.513(4) . ?
C7 C8 1.520(5) . ?
C7 H7A 0.9900 . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C8 H8C 0.9700 . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C9 H9C 0.9700 . ?
C10 N3 1.349(3) . ?
C10 N4 1.373(3) . ?
C11 C12 1.328(4) . ?
C11 N3 1.394(3) . ?
C11 H11A 0.9400 . ?
C12 N4 1.380(3) . ?
C12 H12A 0.9400 . ?
C13 N4 1.466(4) . ?
C13 C14 1.525(7) . ?
C13 C15 1.533(6) . ?
C13 H13A 0.9900 . ?
C14 H14A 0.9700 . ?
C14 H14B 0.9700 . ?
C14 H14C 0.9700 . ?
C15 H15A 0.9700 . ?
C15 H15B 0.9700 . ?
C15 H15C 0.9700 . ?
C16 N3 1.461(3) . ?
C16 C17 1.513(4) . ?
C16 C18 1.515(4) . ?
C16 H16A 0.9900 . ?
C17 H17A 0.9700 . ?
C17 H17B 0.9700 . ?
C17 H17C 0.9700 . ?
C18 H18A 0.9700 . ?
C18 H18B 0.9700 . ?
C18 H18C 0.9700 . ?
C19 H19A 0.9700 . ?
C19 H19B 0.9700 . ?
C19 H19C 0.9700 . ?
C20 H20A 0.9700 . ?
C20 H20B 0.9700 . ?
C20 H20C 0.9700 . ?
C21 H21A 0.9700 . ?
C21 H21B 0.9700 . ?
C21 H21C 0.9700 . ?
C22 H22A 0.9700 . ?
C22 H22B 0.9700 . ?
C22 H22C 0.9700 . ?

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
C10 Ni1 C1 100.74(9) . . ?
C10 Ni1 Si1 156.87(7) . . ?
C1 Ni1 Si1 92.61(7) . . ?
C10 Ni1 Si2 94.80(8) . . ?
C1 Ni1 Si2 152.03(7) . . ?
Si1 Ni1 Si2 81.33(3) . . ?
C19 Si1 C20 100.43(16) . . ?
C19 Si1 Ni1 112.16(16) . . ?
C20 Si1 Ni1 116.96(10) . . ?
C19 Si1 H1 105.0(11) . . ?
C20 Si1 H1 104.1(12) . . ?
Ni1 Si1 H1 116.3(12) . . ?
C21 Si2 C22 102.86(16) . . ?
C21 Si2 Ni1 105.45(10) . . ?
C22 Si2 Ni1 119.82(11) . . ?
C21 Si2 H2 101.4(11) . . ?
C22 Si2 H2 101.3(11) . . ?
Ni1 Si2 H2 123.0(11) . . ?
N2 C1 N1 103.42(19) . . ?
N2 C1 Ni1 131.51(17) . . ?
N1 C1 Ni1 125.05(17) . . ?
C3 C2 N1 106.7(2) . . ?
C3 C2 H2A 126.6 . . ?
N1 C2 H2A 126.6 . . ?
C2 C3 N2 107.1(2) . . ?
C2 C3 H3A 126.5 . . ?
N2 C3 H3A 126.5 . . ?
N2 C4 C6 111.5(3) . . ?
N2 C4 C5 110.2(3) . . ?
C6 C4 C5 113.8(3) . . ?
N2 C4 H4A 107.0 . . ?
C6 C4 H4A 107.0 . . ?
C5 C4 H4A 107.0 . . ?
C4 C5 H5A 109.5 . . ?
C4 C5 H5B 109.5 . . ?
H5A C5 H5B 109.5 . . ?
C4 C5 H5C 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
C4 C6 H6A 109.5 . . ?
C4 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
C4 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
N1 C7 C9 111.4(2) . . ?
N1 C7 C8 110.9(3) . . ?
C9 C7 C8 110.9(3) . . ?
N1 C7 H7A 107.8 . . ?
C9 C7 H7A 107.8 . . ?
C8 C7 H7A 107.8 . . ?
C7 C8 H8A 109.5 . . ?
C7 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C7 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C7 C9 H9A 109.5 . . ?
C7 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
C7 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
N3 C10 N4 103.29(19) . . ?
N3 C10 Ni1 131.53(17) . . ?
N4 C10 Ni1 124.80(18) . . ?
C12 C11 N3 106.8(2) . . ?
C12 C11 H11A 126.6 . . ?
N3 C11 H11A 126.6 . . ?
C11 C12 N4 107.0(2) . . ?
C11 C12 H12A 126.5 . . ?
N4 C12 H12A 126.5 . . ?
N4 C13 C14 110.3(4) . . ?
N4 C13 C15 110.8(4) . . ?
C14 C13 C15 110.9(3) . . ?
N4 C13 H13A 108.2 . . ?
C14 C13 H13A 108.2 . . ?
C15 C13 H13A 108.2 . . ?
C13 C14 H14A 109.5 . . ?
C13 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C13 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C13 C15 H15A 109.5 . . ?
C13 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
C13 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
N3 C16 C17 110.9(2) . . ?
N3 C16 C18 110.8(2) . . ?
C17 C16 C18 112.4(3) . . ?
N3 C16 H16A 107.5 . . ?
C17 C16 H16A 107.5 . . ?
C18 C16 H16A 107.5 . . ?
C16 C17 H17A 109.5 . . ?
C16 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
C16 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C16 C18 H18A 109.5 . . ?
C16 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
C16 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
Si1 C19 H19A 109.5 . . ?
Si1 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
Si1 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
Si1 C20 H20A 109.5 . . ?
Si1 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
Si1 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
Si2 C21 H21A 109.5 . . ?
Si2 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
Si2 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
Si2 C22 H22A 109.5 . . ?
Si2 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
Si2 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C1 N1 C2 111.4(2) . . ?
C1 N1 C7 124.54(19) . . ?
C2 N1 C7 124.0(2) . . ?
C1 N2 C3 111.4(2) . . ?
C1 N2 C4 122.9(2) . . ?
C3 N2 C4 125.7(2) . . ?
C10 N3 C11 111.6(2) . . ?
C10 N3 C16 123.41(19) . . ?
C11 N3 C16 125.0(2) . . ?
C10 N4 C12 111.3(2) . . ?
C10 N4 C13 124.1(2) . . ?
C12 N4 C13 124.3(2) . . ?

_diffrn_measured_fraction_theta_max 0.965
_diffrn_reflns_theta_full        25.95
_diffrn_measured_fraction_theta_full 0.965
_refine_diff_density_max         0.411
_refine_diff_density_min         -0.323
_refine_diff_density_rms         0.055
_database_code_depnum_ccdc_archive 'CCDC 997525'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_compound_cis_10

_audit_creation_method           'SHELXL-97 + manual editing'
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         C26H54N4NiSi2
_chemical_formula_sum            'C26 H54 N4 Ni Si2'
_chemical_formula_weight         537.62

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'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   C2/c

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

_cell_length_a                   36.437(3)
_cell_length_b                   9.9652(8)
_cell_length_c                   18.8125(14)
_cell_angle_alpha                90.00
_cell_angle_beta                 111.354(2)
_cell_angle_gamma                90.00
_cell_volume                     6361.9(8)
_cell_formula_units_Z            8
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9958
_cell_measurement_theta_min      2.3195
_cell_measurement_theta_max      26.0755

_exptl_crystal_description       block
_exptl_crystal_colour            orange
_exptl_crystal_size_max          0.48
_exptl_crystal_size_mid          0.45
_exptl_crystal_size_min          0.35
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.123
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2352
_exptl_absorpt_coefficient_mu    0.704
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_correction_T_min  0.6472
_exptl_absorpt_correction_T_max  0.7453
_exptl_absorpt_process_details   'Sadabs 2008/1 (Bruker 2008)'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker X8-APEX II'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            39789
_diffrn_reflns_av_R_equivalents  0.0291
_diffrn_reflns_av_sigmaI/netI    0.0175
_diffrn_reflns_limit_h_min       -44
_diffrn_reflns_limit_h_max       44
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_theta_min         2.13
_diffrn_reflns_theta_max         26.08
_reflns_number_total             6304
_reflns_number_gt                5762
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'APEX2 ver. 2010.3 (Bruker AXS)'
_computing_cell_refinement       'Saint+ ver. 7.68A (Bruker AXS)'
_computing_data_reduction        'Saint+ ver. 7.68A (Bruker AXS)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'XP ver. 5.1 (Bruker AXS, 1998)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 2008)'

_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)+(0.0344P)²+5.2707P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         6304
_refine_ls_number_parameters     318
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0283
_refine_ls_R_factor_gt           0.0250
_refine_ls_wR_factor_ref         0.0672
_refine_ls_wR_factor_gt          0.0652
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_restrained_S_all      1.052
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni Ni 0.125465(4) 0.724842(16) 0.062489(9) 0.01436(6) Uani 1 1 d . . .
N1 N 0.07119(3) 0.94737(11) -0.01659(6) 0.0194(2) Uani 1 1 d . . .
N2 N 0.11092(3) 1.00518(11) 0.09421(6) 0.0193(2) Uani 1 1 d . . .
N3 N 0.14016(3) 0.65121(12) -0.07738(6) 0.0216(2) Uani 1 1 d . . .
N4 N 0.17354(3) 0.82533(12) -0.02564(6) 0.0199(2) Uani 1 1 d . . .
Si1 Si 0.164145(10) 0.54692(4) 0.11732(2) 0.01807(9) Uani 1 1 d . . .
Si2 Si 0.090103(10) 0.66233(4) 0.13373(2) 0.01668(8) Uani 1 1 d . . .
C1 C 0.10069(4) 0.89786(13) 0.04546(7) 0.0164(2) Uani 1 1 d . . .
C2 C 0.06336(4) 1.08104(14) -0.00677(8) 0.0259(3) Uani 1 1 d . . .
H2A H 0.0441 1.1363 -0.0424 0.031 Uiso 1 1 calc R . .
C3 C 0.08833(4) 1.11701(14) 0.06270(8) 0.0262(3) Uani 1 1 d . . .
H3A H 0.0902 1.2027 0.0858 0.031 Uiso 1 1 calc R . .
C4 C 0.14017(4) 0.99936(14) 0.17266(8) 0.0237(3) Uani 1 1 d . . .
H4A H 0.1540 0.9110 0.1792 0.028 Uiso 1 1 calc R . .
C5 C 0.05163(4) 0.86869(14) -0.08629(7) 0.0222(3) Uani 1 1 d . . .
H5A H 0.0611 0.7739 -0.0756 0.027 Uiso 1 1 calc R . .
C6 C 0.17099(5) 1.10953(16) 0.18677(9) 0.0318(3) Uani 1 1 d . . .
H6A H 0.1833 1.1034 0.1485 0.048 Uiso 1 1 calc R . .
H6B H 0.1911 1.0987 0.2378 0.048 Uiso 1 1 calc R . .
H6C H 0.1583 1.1974 0.1831 0.048 Uiso 1 1 calc R . .
C7 C 0.11986(5) 1.00606(18) 0.23024(9) 0.0357(4) Uani 1 1 d . . .
H7A H 0.1005 0.9333 0.2202 0.054 Uiso 1 1 calc R . .
H7B H 0.1064 1.0927 0.2257 0.054 Uiso 1 1 calc R . .
H7C H 0.1395 0.9965 0.2819 0.054 Uiso 1 1 calc R . .
C8 C 0.06351(5) 0.92081(18) -0.15084(8) 0.0329(3) Uani 1 1 d . . .
H8A H 0.0922 0.9144 -0.1360 0.049 Uiso 1 1 calc R . .
H8B H 0.0553 1.0147 -0.1614 0.049 Uiso 1 1 calc R . .
H8C H 0.0507 0.8668 -0.1968 0.049 Uiso 1 1 calc R . .
C9 C 0.00716(4) 0.86818(17) -0.10755(9) 0.0319(3) Uani 1 1 d . . .
H9A H 0.0009 0.8419 -0.0630 0.048 Uiso 1 1 calc R . .
H9B H -0.0048 0.8041 -0.1491 0.048 Uiso 1 1 calc R . .
H9C H -0.0033 0.9582 -0.1242 0.048 Uiso 1 1 calc R . .
C11 C 0.14806(4) 0.73418(13) -0.01563(7) 0.0173(3) Uani 1 1 d . . .
C12 C 0.16055(5) 0.69050(16) -0.12338(8) 0.0281(3) Uani 1 1 d . . .
H12A H 0.1598 0.6483 -0.1692 0.034 Uiso 1 1 calc R . .
C13 C 0.18146(4) 0.79918(15) -0.09098(8) 0.0268(3) Uani 1 1 d . . .
H13A H 0.1985 0.8489 -0.1092 0.032 Uiso 1 1 calc R . .
C14 C 0.18957(4) 0.93944(14) 0.02561(8) 0.0239(3) Uani 1 1 d . . .
H14A H 0.1811 0.9294 0.0703 0.029 Uiso 1 1 calc R . .
C15 C 0.11463(5) 0.53217(15) -0.09106(8) 0.0300(3) Uani 1 1 d . . .
H15A H 0.1044 0.5263 -0.0486 0.036 Uiso 1 1 calc R . .
C16 C 0.17249(5) 1.07056(15) -0.01420(10) 0.0331(3) Uani 1 1 d . . .
H16A H 0.1437 1.0689 -0.0297 0.050 Uiso 1 1 calc R . .
H16B H 0.1796 1.0816 -0.0594 0.050 Uiso 1 1 calc R . .
H16C H 0.1832 1.1457 0.0209 0.050 Uiso 1 1 calc R . .
C17 C 0.23441(5) 0.93809(19) 0.05579(10) 0.0390(4) Uani 1 1 d . . .
H17A H 0.2440 0.8515 0.0801 0.058 Uiso 1 1 calc R . .
H17B H 0.2445 1.0102 0.0933 0.058 Uiso 1 1 calc R . .
H17C H 0.2436 0.9517 0.0134 0.058 Uiso 1 1 calc R . .
C18 C 0.07943(5) 0.54440(19) -0.16541(10) 0.0418(4) Uani 1 1 d . . .
H18A H 0.0648 0.6266 -0.1646 0.063 Uiso 1 1 calc R . .
H18B H 0.0621 0.4665 -0.1713 0.063 Uiso 1 1 calc R . .
H18C H 0.0886 0.5479 -0.2083 0.063 Uiso 1 1 calc R . .
C19 C 0.13790(6) 0.40457(17) -0.08960(10) 0.0424(4) Uani 1 1 d . . .
H19A H 0.1607 0.4002 -0.0417 0.064 Uiso 1 1 calc R . .
H19B H 0.1469 0.4051 -0.1327 0.064 Uiso 1 1 calc R . .
H19C H 0.1210 0.3263 -0.0935 0.064 Uiso 1 1 calc R . .
C21 C 0.17974(4) 0.52454(15) 0.22513(8) 0.0242(3) Uani 1 1 d . . .
H21A H 0.1561 0.5058 0.2377 0.029 Uiso 1 1 calc R . .
H21B H 0.1975 0.4461 0.2413 0.029 Uiso 1 1 calc R . .
C22 C 0.20075(5) 0.64832(17) 0.26960(9) 0.0351(4) Uani 1 1 d . . .
H22A H 0.2063 0.6349 0.3241 0.053 Uiso 1 1 calc R . .
H22B H 0.1839 0.7273 0.2517 0.053 Uiso 1 1 calc R . .
H22C H 0.2256 0.6620 0.2615 0.053 Uiso 1 1 calc R . .
C23 C 0.21395(4) 0.55090(15) 0.10418(9) 0.0277(3) Uani 1 1 d . . .
H23A H 0.2090 0.5595 0.0491 0.033 Uiso 1 1 calc R . .
H23B H 0.2285 0.6319 0.1299 0.033 Uiso 1 1 calc R . .
C24 C 0.24002(5) 0.42797(17) 0.13512(11) 0.0378(4) Uani 1 1 d . . .
H24A H 0.2645 0.4372 0.1251 0.057 Uiso 1 1 calc R . .
H24B H 0.2260 0.3470 0.1099 0.057 Uiso 1 1 calc R . .
H24C H 0.2463 0.4209 0.1902 0.057 Uiso 1 1 calc R . .
C31 C 0.07110(4) 0.48123(14) 0.11909(8) 0.0244(3) Uani 1 1 d . . .
H31A H 0.0933 0.4195 0.1449 0.029 Uiso 1 1 calc R . .
H31B H 0.0513 0.4700 0.1432 0.029 Uiso 1 1 calc R . .
C32 C 0.05252(4) 0.44291(15) 0.03452(9) 0.0293(3) Uani 1 1 d . . .
H32A H 0.0368 0.3611 0.0292 0.044 Uiso 1 1 calc R . .
H32B H 0.0734 0.4271 0.0142 0.044 Uiso 1 1 calc R . .
H32C H 0.0355 0.5161 0.0061 0.044 Uiso 1 1 calc R . .
C33 C 0.04196(4) 0.75985(14) 0.11477(8) 0.0209(3) Uani 1 1 d . . .
H33A H 0.0474 0.8570 0.1132 0.025 Uiso 1 1 calc R . .
H33B H 0.0228 0.7340 0.0640 0.025 Uiso 1 1 calc R . .
C34 C 0.02328(5) 0.73553(18) 0.17453(10) 0.0370(4) Uani 1 1 d . . .
H34A H -0.0006 0.7902 0.1623 0.056 Uiso 1 1 calc R . .
H34B H 0.0420 0.7604 0.2251 0.056 Uiso 1 1 calc R . .
H34C H 0.0164 0.6404 0.1744 0.056 Uiso 1 1 calc R . .
H1 H 0.1076(5) 0.6765(17) 0.2129(9) 0.029(4) Uiso 1 1 d . . .
H2 H 0.1491(5) 0.4165(17) 0.0881(9) 0.031(4) Uiso 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
Ni C1 1.9182(13) . ?
Ni C11 1.9306(13) . ?
Ni Si2 2.2588(4) . ?
Ni Si1 2.2661(4) . ?
N1 C1 1.3593(17) . ?
N1 C2 1.3887(18) . ?
N1 C5 1.4702(17) . ?
N2 C1 1.3693(17) . ?
N2 C3 1.3841(18) . ?
N2 C4 1.4738(17) . ?
N3 C11 1.3684(17) . ?
N3 C12 1.3867(18) . ?
N3 C15 1.4712(19) . ?
N4 C11 1.3600(17) . ?
N4 C13 1.3858(17) . ?
N4 C14 1.4675(18) . ?
Si1 C21 1.9097(14) . ?
Si1 C23 1.9191(14) . ?
Si1 H2 1.440(17) . ?
Si2 C31 1.9165(14) . ?
Si2 C33 1.9218(14) . ?
Si2 H1 1.398(16) . ?
C2 C3 1.341(2) . ?
C2 H2A 0.9500 . ?
C3 H3A 0.9500 . ?
C4 C7 1.520(2) . ?
C4 C6 1.523(2) . ?
C4 H4A 1.0000 . ?
C5 C9 1.5209(19) . ?
C5 C8 1.521(2) . ?
C5 H5A 1.0000 . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C12 C13 1.337(2) . ?
C12 H12A 0.9500 . ?
C13 H13A 0.9500 . ?
C14 C16 1.522(2) . ?
C14 C17 1.522(2) . ?
C14 H14A 1.0000 . ?
C15 C18 1.520(2) . ?
C15 C19 1.523(2) . ?
C15 H15A 1.0000 . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
C21 C22 1.530(2) . ?
C21 H21A 0.9900 . ?
C21 H21B 0.9900 . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C23 C24 1.529(2) . ?
C23 H23A 0.9900 . ?
C23 H23B 0.9900 . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?
C31 C32 1.533(2) . ?
C31 H31A 0.9900 . ?
C31 H31B 0.9900 . ?
C32 H32A 0.9800 . ?
C32 H32B 0.9800 . ?
C32 H32C 0.9800 . ?
C33 C34 1.5308(19) . ?
C33 H33A 0.9900 . ?
C33 H33B 0.9900 . ?
C34 H34A 0.9800 . ?
C34 H34B 0.9800 . ?
C34 H34C 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C1 Ni C11 97.74(5) . . ?
C1 Ni Si2 90.66(4) . . ?
C11 Ni Si2 163.42(4) . . ?
C1 Ni Si1 162.97(4) . . ?
C11 Ni Si1 90.99(4) . . ?
Si2 Ni Si1 84.763(14) . . ?
C1 N1 C2 111.75(11) . . ?
C1 N1 C5 123.18(11) . . ?
C2 N1 C5 125.01(11) . . ?
C1 N2 C3 111.57(11) . . ?
C1 N2 C4 124.14(11) . . ?
C3 N2 C4 124.13(11) . . ?
C11 N3 C12 111.37(12) . . ?
C11 N3 C15 124.05(11) . . ?
C12 N3 C15 124.53(12) . . ?
C11 N4 C13 111.74(12) . . ?
C11 N4 C14 123.71(11) . . ?
C13 N4 C14 124.52(12) . . ?
C21 Si1 C23 102.10(6) . . ?
C21 Si1 Ni 118.03(5) . . ?
C23 Si1 Ni 112.69(5) . . ?
C21 Si1 H2 103.0(7) . . ?
C23 Si1 H2 102.5(6) . . ?
Ni Si1 H2 116.4(7) . . ?
C31 Si2 C33 101.07(6) . . ?
C31 Si2 Ni 115.39(5) . . ?
C33 Si2 Ni 115.45(4) . . ?
C31 Si2 H1 104.4(7) . . ?
C33 Si2 H1 100.2(7) . . ?
Ni Si2 H1 117.9(7) . . ?
N1 C1 N2 103.23(11) . . ?
N1 C1 Ni 130.29(10) . . ?
N2 C1 Ni 126.40(9) . . ?
C3 C2 N1 106.66(12) . . ?
C3 C2 H2A 126.7 . . ?
N1 C2 H2A 126.7 . . ?
C2 C3 N2 106.79(12) . . ?
C2 C3 H3A 126.6 . . ?
N2 C3 H3A 126.6 . . ?
N2 C4 C7 110.47(12) . . ?
N2 C4 C6 111.38(12) . . ?
C7 C4 C6 111.31(12) . . ?
N2 C4 H4A 107.8 . . ?
C7 C4 H4A 107.8 . . ?
C6 C4 H4A 107.8 . . ?
N1 C5 C9 111.12(11) . . ?
N1 C5 C8 110.08(12) . . ?
C9 C5 C8 112.14(12) . . ?
N1 C5 H5A 107.8 . . ?
C9 C5 H5A 107.8 . . ?
C8 C5 H5A 107.8 . . ?
C4 C6 H6A 109.5 . . ?
C4 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
C4 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
C4 C7 H7A 109.5 . . ?
C4 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
C4 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
C5 C8 H8A 109.5 . . ?
C5 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C5 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C5 C9 H9A 109.5 . . ?
C5 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
C5 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
N4 C11 N3 103.25(11) . . ?
N4 C11 Ni 129.75(10) . . ?
N3 C11 Ni 126.93(10) . . ?
C13 C12 N3 106.86(12) . . ?
C13 C12 H12A 126.6 . . ?
N3 C12 H12A 126.6 . . ?
C12 C13 N4 106.78(13) . . ?
C12 C13 H13A 126.6 . . ?
N4 C13 H13A 126.6 . . ?
N4 C14 C16 110.39(12) . . ?
N4 C14 C17 110.77(12) . . ?
C16 C14 C17 112.47(13) . . ?
N4 C14 H14A 107.7 . . ?
C16 C14 H14A 107.7 . . ?
C17 C14 H14A 107.7 . . ?
N3 C15 C18 111.36(13) . . ?
N3 C15 C19 110.96(13) . . ?
C18 C15 C19 111.17(13) . . ?
N3 C15 H15A 107.7 . . ?
C18 C15 H15A 107.7 . . ?
C19 C15 H15A 107.7 . . ?
C14 C16 H16A 109.5 . . ?
C14 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
C14 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C14 C17 H17A 109.5 . . ?
C14 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
C14 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C15 C18 H18A 109.5 . . ?
C15 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
C15 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C15 C19 H19A 109.5 . . ?
C15 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
C15 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C22 C21 Si1 112.50(10) . . ?
C22 C21 H21A 109.1 . . ?
Si1 C21 H21A 109.1 . . ?
C22 C21 H21B 109.1 . . ?
Si1 C21 H21B 109.1 . . ?
H21A C21 H21B 107.8 . . ?
C21 C22 H22A 109.5 . . ?
C21 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
C21 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C24 C23 Si1 114.82(10) . . ?
C24 C23 H23A 108.6 . . ?
Si1 C23 H23A 108.6 . . ?
C24 C23 H23B 108.6 . . ?
Si1 C23 H23B 108.6 . . ?
H23A C23 H23B 107.5 . . ?
C23 C24 H24A 109.5 . . ?
C23 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
C23 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C32 C31 Si2 112.55(10) . . ?
C32 C31 H31A 109.1 . . ?
Si2 C31 H31A 109.1 . . ?
C32 C31 H31B 109.1 . . ?
Si2 C31 H31B 109.1 . . ?
H31A C31 H31B 107.8 . . ?
C31 C32 H32A 109.5 . . ?
C31 C32 H32B 109.5 . . ?
H32A C32 H32B 109.5 . . ?
C31 C32 H32C 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
C34 C33 Si2 113.80(10) . . ?
C34 C33 H33A 108.8 . . ?
Si2 C33 H33A 108.8 . . ?
C34 C33 H33B 108.8 . . ?
Si2 C33 H33B 108.8 . . ?
H33A C33 H33B 107.7 . . ?
C33 C34 H34A 109.5 . . ?
C33 C34 H34B 109.5 . . ?
H34A C34 H34B 109.5 . . ?
C33 C34 H34C 109.5 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 109.5 . . ?

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        26.00
_diffrn_measured_fraction_theta_full 1.000
_refine_diff_density_max         0.421
_refine_diff_density_min         -0.202
_refine_diff_density_rms         0.046
_database_code_depnum_ccdc_archive 'CCDC 997526'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_compound_cis_11

_audit_creation_method           'SHELXL-97 + manual editing'
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         C30H58N4NiSi2
_chemical_formula_sum            'C30 H58 N4 Ni Si2'
_chemical_formula_weight         589.69

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'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   C2/c

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

_cell_length_a                   15.655(4)
_cell_length_b                   11.439(3)
_cell_length_c                   19.648(5)
_cell_angle_alpha                90.00
_cell_angle_beta                 106.741(9)
_cell_angle_gamma                90.00
_cell_volume                     3369.3(16)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    4538
_cell_measurement_theta_min      2.2395
_cell_measurement_theta_max      26.014

_exptl_crystal_description       block
_exptl_crystal_colour            orange
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.29
_exptl_crystal_size_min          0.25
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.163
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1288
_exptl_absorpt_coefficient_mu    0.671
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_correction_T_min  0.6397
_exptl_absorpt_correction_T_max  0.7453
_exptl_absorpt_process_details   'Sadabs 2008/1 (Bruker 2008)'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_monochromator  'multi-layer mirror'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            12233
_diffrn_reflns_av_R_equivalents  0.0355
_diffrn_reflns_av_sigmaI/netI    0.0366
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_theta_min         2.16
_diffrn_reflns_theta_max         26.16
_reflns_number_total             3332
_reflns_number_gt                2882
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'APEX2 ver. 2010.3 (Bruker AXS)'
_computing_cell_refinement       'Saint+ ver. 7.68A (Bruker AXS)'
_computing_data_reduction        'Saint+ ver. 7.68A (Bruker AXS)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'XP ver. 5.1 (Bruker AXS, 1998)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 2008)'

_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)+(0.0278P)²+2.7739P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         3332
_refine_ls_number_parameters     180
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0384
_refine_ls_R_factor_gt           0.0300
_refine_ls_wR_factor_ref         0.0691
_refine_ls_wR_factor_gt          0.0658
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_restrained_S_all      1.026
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni Ni 0.0000 0.64543(2) 0.7500 0.01159(9) Uani 1 2 d S . .
N1 N -0.15688(9) 0.76440(12) 0.77601(7) 0.0141(3) Uani 1 1 d . . .
N2 N -0.03489(9) 0.83362(11) 0.84411(7) 0.0144(3) Uani 1 1 d . . .
Si Si 0.03729(3) 0.49296(4) 0.69211(2) 0.01457(11) Uani 1 1 d . . .
C1 C -0.06588(10) 0.75166(14) 0.79239(8) 0.0128(3) Uani 1 1 d . . .
C2 C -0.18021(12) 0.85213(15) 0.81603(9) 0.0191(4) Uani 1 1 d . . .
H2A H -0.2389 0.8768 0.8137 0.023 Uiso 1 1 calc R . .
C3 C -0.10372(12) 0.89537(15) 0.85861(9) 0.0190(4) Uani 1 1 d . . .
H3A H -0.0979 0.9567 0.8923 0.023 Uiso 1 1 calc R . .
C4 C 0.06060(11) 0.85631(15) 0.87721(9) 0.0176(4) Uani 1 1 d . . .
H4A H 0.0948 0.7924 0.8621 0.021 Uiso 1 1 calc R . .
C5 C -0.22256(11) 0.68928(15) 0.72675(9) 0.0190(4) Uani 1 1 d . . .
H5A H -0.1898 0.6227 0.7128 0.023 Uiso 1 1 calc R . .
C6 C 0.08376(13) 0.85285(17) 0.95773(9) 0.0263(4) Uani 1 1 d . . .
H6A H 0.0640 0.7784 0.9727 0.039 Uiso 1 1 calc R . .
H6B H 0.0538 0.9175 0.9743 0.039 Uiso 1 1 calc R . .
H6C H 0.1485 0.8605 0.9782 0.039 Uiso 1 1 calc R . .
C7 C 0.08726(13) 0.97118(16) 0.85006(10) 0.0269(4) Uani 1 1 d . . .
H7A H 0.0743 0.9677 0.7982 0.040 Uiso 1 1 calc R . .
H7B H 0.1512 0.9845 0.8715 0.040 Uiso 1 1 calc R . .
H7C H 0.0534 1.0354 0.8629 0.040 Uiso 1 1 calc R . .
C8 C -0.28736(12) 0.63904(16) 0.76408(10) 0.0252(4) Uani 1 1 d . . .
H8A H -0.3272 0.5830 0.7326 0.038 Uiso 1 1 calc R . .
H8B H -0.3227 0.7025 0.7759 0.038 Uiso 1 1 calc R . .
H8C H -0.2538 0.5993 0.8078 0.038 Uiso 1 1 calc R . .
C9 C -0.27217(12) 0.75489(17) 0.65937(9) 0.0257(4) Uani 1 1 d . . .
H9A H -0.3154 0.7024 0.6279 0.039 Uiso 1 1 calc R . .
H9B H -0.2294 0.7824 0.6350 0.039 Uiso 1 1 calc R . .
H9C H -0.3035 0.8220 0.6719 0.039 Uiso 1 1 calc R . .
C21 C -0.05954(11) 0.42620(15) 0.62007(9) 0.0172(4) Uani 1 1 d . . .
H21A H -0.1069 0.4050 0.6428 0.021 Uiso 1 1 calc R . .
C22 C -0.10093(12) 0.51158(16) 0.55980(10) 0.0249(4) Uani 1 1 d . . .
H22A H -0.0542 0.5391 0.5388 0.030 Uiso 1 1 calc R . .
H22B H -0.1240 0.5805 0.5795 0.030 Uiso 1 1 calc R . .
C23 C -0.17714(13) 0.45657(18) 0.50129(10) 0.0319(5) Uani 1 1 d . . .
H23A H -0.2278 0.4397 0.5204 0.038 Uiso 1 1 calc R . .
H23B H -0.1979 0.5128 0.4617 0.038 Uiso 1 1 calc R . .
C24 C -0.14762(13) 0.34377(17) 0.47333(10) 0.0288(4) Uani 1 1 d . . .
H24A H -0.1995 0.3074 0.4385 0.035 Uiso 1 1 calc R . .
H24B H -0.1024 0.3621 0.4485 0.035 Uiso 1 1 calc R . .
C25 C -0.10854(13) 0.25830(17) 0.53308(10) 0.0266(4) Uani 1 1 d . . .
H25A H -0.0870 0.1880 0.5137 0.032 Uiso 1 1 calc R . .
H25B H -0.1555 0.2335 0.5546 0.032 Uiso 1 1 calc R . .
C26 C -0.03148(12) 0.31306(15) 0.59005(9) 0.0216(4) Uani 1 1 d . . .
H26A H 0.0179 0.3306 0.5695 0.026 Uiso 1 1 calc R . .
H26B H -0.0091 0.2564 0.6292 0.026 Uiso 1 1 calc R . .
H1 H 0.1022(12) 0.5173(16) 0.6555(9) 0.022(5) Uiso 1 1 d . . .
H2 H 0.0797(13) 0.3919(17) 0.7328(10) 0.028(5) Uiso 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
Ni C1 1.9309(16) . ?
Ni C1 1.9310(16) 2_556 ?
Ni Si 2.2491(7) 2_556 ?
Ni Si 2.2492(6) . ?
N1 C1 1.375(2) . ?
N1 C2 1.387(2) . ?
N1 C5 1.469(2) . ?
N2 C1 1.365(2) . ?
N2 C3 1.385(2) . ?
N2 C4 1.471(2) . ?
Si C21 1.9102(17) . ?
Si H1 1.431(18) . ?
Si H2 1.453(19) . ?
C2 C3 1.342(3) . ?
C2 H2A 0.9500 . ?
C3 H3A 0.9500 . ?
C4 C6 1.518(2) . ?
C4 C7 1.521(2) . ?
C4 H4A 1.0000 . ?
C5 C8 1.525(2) . ?
C5 C9 1.525(2) . ?
C5 H5A 1.0000 . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C21 C22 1.528(2) . ?
C21 C26 1.538(2) . ?
C21 H21A 1.0000 . ?
C22 C23 1.533(3) . ?
C22 H22A 0.9900 . ?
C22 H22B 0.9900 . ?
C23 C24 1.525(3) . ?
C23 H23A 0.9900 . ?
C23 H23B 0.9900 . ?
C24 C25 1.515(3) . ?
C24 H24A 0.9900 . ?
C24 H24B 0.9900 . ?
C25 C26 1.524(2) . ?
C25 H25A 0.9900 . ?
C25 H25B 0.9900 . ?
C26 H26A 0.9900 . ?
C26 H26B 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
C1 Ni C1 102.01(9) . 2_556 ?
C1 Ni Si 91.21(5) . 2_556 ?
C1 Ni Si 162.70(5) 2_556 2_556 ?
C1 Ni Si 162.70(5) . . ?
C1 Ni Si 91.21(5) 2_556 . ?
Si Ni Si 78.32(3) 2_556 . ?
C1 N1 C2 111.61(14) . . ?
C1 N1 C5 124.99(13) . . ?
C2 N1 C5 123.23(14) . . ?
C1 N2 C3 111.89(14) . . ?
C1 N2 C4 123.24(13) . . ?
C3 N2 C4 124.81(14) . . ?
C21 Si Ni 114.74(6) . . ?
C21 Si H1 103.4(7) . . ?
Ni Si H1 115.4(7) . . ?
C21 Si H2 103.2(8) . . ?
Ni Si H2 118.9(7) . . ?
H1 Si H2 98.8(10) . . ?
N2 C1 N1 102.91(13) . . ?
N2 C1 Ni 129.35(12) . . ?
N1 C1 Ni 127.73(12) . . ?
C3 C2 N1 106.66(15) . . ?
C3 C2 H2A 126.7 . . ?
N1 C2 H2A 126.7 . . ?
C2 C3 N2 106.92(15) . . ?
C2 C3 H3A 126.5 . . ?
N2 C3 H3A 126.5 . . ?
N2 C4 C6 111.30(14) . . ?
N2 C4 C7 110.11(14) . . ?
C6 C4 C7 112.37(15) . . ?
N2 C4 H4A 107.6 . . ?
C6 C4 H4A 107.6 . . ?
C7 C4 H4A 107.6 . . ?
N1 C5 C8 109.86(13) . . ?
N1 C5 C9 111.64(14) . . ?
C8 C5 C9 111.09(14) . . ?
N1 C5 H5A 108.0 . . ?
C8 C5 H5A 108.0 . . ?
C9 C5 H5A 108.0 . . ?
C4 C6 H6A 109.5 . . ?
C4 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
C4 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
C4 C7 H7A 109.5 . . ?
C4 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
C4 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
C5 C8 H8A 109.5 . . ?
C5 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C5 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C5 C9 H9A 109.5 . . ?
C5 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
C5 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C22 C21 C26 110.17(14) . . ?
C22 C21 Si 112.81(12) . . ?
C26 C21 Si 111.55(12) . . ?
C22 C21 H21A 107.3 . . ?
C26 C21 H21A 107.3 . . ?
Si C21 H21A 107.3 . . ?
C21 C22 C23 112.55(16) . . ?
C21 C22 H22A 109.1 . . ?
C23 C22 H22A 109.1 . . ?
C21 C22 H22B 109.1 . . ?
C23 C22 H22B 109.1 . . ?
H22A C22 H22B 107.8 . . ?
C24 C23 C22 111.48(16) . . ?
C24 C23 H23A 109.3 . . ?
C22 C23 H23A 109.3 . . ?
C24 C23 H23B 109.3 . . ?
C22 C23 H23B 109.3 . . ?
H23A C23 H23B 108.0 . . ?
C25 C24 C23 111.30(15) . . ?
C25 C24 H24A 109.4 . . ?
C23 C24 H24A 109.4 . . ?
C25 C24 H24B 109.4 . . ?
C23 C24 H24B 109.4 . . ?
H24A C24 H24B 108.0 . . ?
C24 C25 C26 111.19(15) . . ?
C24 C25 H25A 109.4 . . ?
C26 C25 H25A 109.4 . . ?
C24 C25 H25B 109.4 . . ?
C26 C25 H25B 109.4 . . ?
H25A C25 H25B 108.0 . . ?
C25 C26 C21 111.99(15) . . ?
C25 C26 H26A 109.2 . . ?
C21 C26 H26A 109.2 . . ?
C25 C26 H26B 109.2 . . ?
C21 C26 H26B 109.2 . . ?
H26A C26 H26B 107.9 . . ?

_diffrn_measured_fraction_theta_max 0.990
_diffrn_reflns_theta_full        26.00
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         0.336
_refine_diff_density_min         -0.224
_refine_diff_density_rms         0.050
_database_code_depnum_ccdc_archive 'CCDC 997527'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_compound_trans_12

_audit_creation_method           'SHELXL-97 + manual editing'
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         C30H62N4NiO6Si2
_chemical_formula_sum            'C30 H62 N4 Ni O6 Si2'
_chemical_formula_weight         689.73

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'
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   P2(1)/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                   10.576(2)
_cell_length_b                   12.144(2)
_cell_length_c                   14.883(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 102.49(3)
_cell_angle_gamma                90.00
_cell_volume                     1866.3(6)
_cell_formula_units_Z            2
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    4933
_cell_measurement_theta_min      2.7335
_cell_measurement_theta_max      25.3335

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.12
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.227
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             748
_exptl_absorpt_coefficient_mu    0.627
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6295
_exptl_absorpt_correction_T_max  0.7453
_exptl_absorpt_process_details   'SadAbs-2008/1 (Bruker, 2008)'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      173(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_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            7173
_diffrn_reflns_av_R_equivalents  0.0339
_diffrn_reflns_av_sigmaI/netI    0.0459
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         2.16
_diffrn_reflns_theta_max         26.23
_reflns_number_total             3736
_reflns_number_gt                3102
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Smart-NT v. 5.63'
_computing_cell_refinement       'Saint-NT v. 7.23'
_computing_data_reduction        'Saint-NT v. 7.23'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'XP in ShelxTL-97'
_computing_publication_material  'XP in ShelxTL-97'

_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)+(0.0758P)²+0.1791P] 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         3736
_refine_ls_number_parameters     203
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0574
_refine_ls_R_factor_gt           0.0426
_refine_ls_wR_factor_ref         0.1363
_refine_ls_wR_factor_gt          0.1159
_refine_ls_goodness_of_fit_ref   1.149
_refine_ls_restrained_S_all      1.149
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni Ni 0.0000 0.5000 0.0000 0.02063(16) Uani 1 2 d S . .
N2 N -0.05177(19) 0.70833(15) 0.08083(13) 0.0252(4) Uani 1 1 d . . .
Si Si -0.09101(7) 0.41401(5) 0.10673(5) 0.0278(2) Uani 1 1 d . . .
O1 O -0.24232(18) 0.45868(17) 0.09845(13) 0.0408(5) Uani 1 1 d . . .
N1 N 0.14763(19) 0.66031(15) 0.12640(13) 0.0250(4) Uani 1 1 d . . .
O3 O -0.02414(19) 0.42066(15) 0.21944(12) 0.0396(5) Uani 1 1 d . . .
C1 C 0.0330(2) 0.62665(18) 0.07239(15) 0.0226(5) Uani 1 1 d . . .
C4 C 0.2683(2) 0.5979(2) 0.13585(17) 0.0292(5) Uani 1 1 d . . .
H4A H 0.2571 0.5447 0.0834 0.035 Uiso 1 1 calc R . .
C2 C 0.1339(3) 0.7610(2) 0.16632(18) 0.0332(6) Uani 1 1 d . . .
H2A H 0.2000 0.8011 0.2064 0.040 Uiso 1 1 calc R . .
O2 O -0.0991(2) 0.27885(15) 0.09111(15) 0.0507(6) Uani 1 1 d . . .
C3 C 0.0104(3) 0.7913(2) 0.13808(18) 0.0348(6) Uani 1 1 d . . .
H3A H -0.0278 0.8572 0.1541 0.042 Uiso 1 1 calc R . .
C6 C 0.3791(3) 0.6744(3) 0.1291(2) 0.0506(8) Uani 1 1 d . . .
H6A H 0.3553 0.7187 0.0729 0.076 Uiso 1 1 calc R . .
H6B H 0.4565 0.6308 0.1271 0.076 Uiso 1 1 calc R . .
H6C H 0.3972 0.7232 0.1828 0.076 Uiso 1 1 calc R . .
C5 C -0.1869(2) 0.7105(2) 0.03035(17) 0.0307(6) Uani 1 1 d . . .
H5A H -0.2105 0.6342 0.0075 0.037 Uiso 1 1 calc R . .
C15 C -0.0280(3) 0.5159(2) 0.27349(19) 0.0412(7) Uani 1 1 d . . .
H15A H -0.1186 0.5417 0.2654 0.049 Uiso 1 1 calc R . .
H15B H 0.0233 0.5753 0.2530 0.049 Uiso 1 1 calc R . .
C9 C -0.2764(3) 0.7425(3) 0.0925(2) 0.0489(8) Uani 1 1 d . . .
H9A H -0.2605 0.6946 0.1468 0.073 Uiso 1 1 calc R . .
H9B H -0.3665 0.7344 0.0591 0.073 Uiso 1 1 calc R . .
H9C H -0.2603 0.8193 0.1119 0.073 Uiso 1 1 calc R . .
C13 C -0.1453(4) 0.1965(2) 0.1401(2) 0.0553(8) Uani 1 1 d . . .
H13A H -0.2330 0.2167 0.1478 0.066 Uiso 1 1 calc R . .
H13B H -0.0883 0.1909 0.2022 0.066 Uiso 1 1 calc R . .
C11 C -0.3254(3) 0.4302(3) 0.1592(2) 0.0444(7) Uani 1 1 d . . .
H11A H -0.3500 0.4978 0.1884 0.053 Uiso 1 1 calc R . .
H11B H -0.2781 0.3814 0.2085 0.053 Uiso 1 1 calc R . .
C7 C 0.2947(3) 0.5322(3) 0.2240(2) 0.0518(8) Uani 1 1 d . . .
H7A H 0.2220 0.4822 0.2243 0.078 Uiso 1 1 calc R . .
H7B H 0.3049 0.5825 0.2766 0.078 Uiso 1 1 calc R . .
H7C H 0.3742 0.4893 0.2284 0.078 Uiso 1 1 calc R . .
C8 C -0.2019(3) 0.7857(3) -0.0534(2) 0.0499(8) Uani 1 1 d . . .
H8A H -0.1402 0.7637 -0.0906 0.075 Uiso 1 1 calc R . .
H8B H -0.1848 0.8620 -0.0329 0.075 Uiso 1 1 calc R . .
H8C H -0.2903 0.7798 -0.0904 0.075 Uiso 1 1 calc R . .
C16 C 0.0258(4) 0.4907(3) 0.3729(2) 0.0620(11) Uani 1 1 d . . .
H16A H 0.0218 0.5569 0.4099 0.093 Uiso 1 1 calc R . .
H16B H 0.1161 0.4669 0.3810 0.093 Uiso 1 1 calc R . .
H16C H -0.0251 0.4319 0.3930 0.093 Uiso 1 1 calc R . .
C12 C -0.4455(3) 0.3728(3) 0.1086(2) 0.0590(9) Uani 1 1 d . . .
H12A H -0.5010 0.3555 0.1516 0.088 Uiso 1 1 calc R . .
H12B H -0.4215 0.3045 0.0814 0.088 Uiso 1 1 calc R . .
H12C H -0.4924 0.4210 0.0598 0.088 Uiso 1 1 calc R . .
C14 C -0.1510(4) 0.0904(3) 0.0950(3) 0.0708(11) Uani 1 1 d . . .
H14A H -0.1928 0.0369 0.1284 0.106 Uiso 1 1 calc R . .
H14B H -0.0631 0.0656 0.0944 0.106 Uiso 1 1 calc R . .
H14C H -0.2011 0.0970 0.0317 0.106 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
Ni C1 1.867(2) . ?
Ni C1 1.867(2) 3_565 ?
Ni Si 2.2806(8) 3_565 ?
Ni Si 2.2806(8) . ?
N2 C1 1.361(3) . ?
N2 C3 1.389(3) . ?
N2 C5 1.464(3) . ?
Si O2 1.657(2) . ?
Si O1 1.669(2) . ?
Si O3 1.6755(19) . ?
O1 C11 1.433(3) . ?
N1 C1 1.364(3) . ?
N1 C2 1.380(3) . ?
N1 C4 1.465(3) . ?
O3 C15 1.414(3) . ?
C4 C7 1.509(4) . ?
C4 C6 1.516(4) . ?
C4 H4A 1.0000 . ?
C2 C3 1.334(4) . ?
C2 H2A 0.9500 . ?
O2 C13 1.388(3) . ?
C3 H3A 0.9500 . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?
C5 C9 1.511(4) . ?
C5 C8 1.525(4) . ?
C5 H5A 1.0000 . ?
C15 C16 1.498(4) . ?
C15 H15A 0.9900 . ?
C15 H15B 0.9900 . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C13 C14 1.448(5) . ?
C13 H13A 0.9900 . ?
C13 H13B 0.9900 . ?
C11 C12 1.500(4) . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C1 Ni C1 180.0 . 3_565 ?
C1 Ni Si 88.30(7) . 3_565 ?
C1 Ni Si 91.70(7) 3_565 3_565 ?
C1 Ni Si 91.70(7) . . ?
C1 Ni Si 88.30(7) 3_565 . ?
Si Ni Si 180.00(3) 3_565 . ?
C1 N2 C3 110.6(2) . . ?
C1 N2 C5 123.72(19) . . ?
C3 N2 C5 125.6(2) . . ?
O2 Si O1 106.98(11) . . ?
O2 Si O3 100.71(11) . . ?
O1 Si O3 104.40(10) . . ?
O2 Si Ni 111.87(7) . . ?
O1 Si Ni 110.01(7) . . ?
O3 Si Ni 121.66(8) . . ?
C11 O1 Si 125.73(19) . . ?
C1 N1 C2 110.8(2) . . ?
C1 N1 C4 123.11(19) . . ?
C2 N1 C4 126.0(2) . . ?
C15 O3 Si 123.43(17) . . ?
N2 C1 N1 104.27(18) . . ?
N2 C1 Ni 127.51(17) . . ?
N1 C1 Ni 128.19(17) . . ?
N1 C4 C7 110.5(2) . . ?
N1 C4 C6 110.3(2) . . ?
C7 C4 C6 112.4(2) . . ?
N1 C4 H4A 107.8 . . ?
C7 C4 H4A 107.8 . . ?
C6 C4 H4A 107.8 . . ?
C3 C2 N1 107.2(2) . . ?
C3 C2 H2A 126.4 . . ?
N1 C2 H2A 126.4 . . ?
C13 O2 Si 130.8(2) . . ?
C2 C3 N2 107.1(2) . . ?
C2 C3 H3A 126.4 . . ?
N2 C3 H3A 126.4 . . ?
C4 C6 H6A 109.5 . . ?
C4 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
C4 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
N2 C5 C9 111.2(2) . . ?
N2 C5 C8 110.3(2) . . ?
C9 C5 C8 112.2(2) . . ?
N2 C5 H5A 107.6 . . ?
C9 C5 H5A 107.6 . . ?
C8 C5 H5A 107.6 . . ?
O3 C15 C16 110.1(3) . . ?
O3 C15 H15A 109.6 . . ?
C16 C15 H15A 109.6 . . ?
O3 C15 H15B 109.6 . . ?
C16 C15 H15B 109.6 . . ?
H15A C15 H15B 108.2 . . ?
C5 C9 H9A 109.5 . . ?
C5 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
C5 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
O2 C13 C14 112.4(3) . . ?
O2 C13 H13A 109.1 . . ?
C14 C13 H13A 109.1 . . ?
O2 C13 H13B 109.1 . . ?
C14 C13 H13B 109.1 . . ?
H13A C13 H13B 107.8 . . ?
O1 C11 C12 111.3(2) . . ?
O1 C11 H11A 109.4 . . ?
C12 C11 H11A 109.4 . . ?
O1 C11 H11B 109.4 . . ?
C12 C11 H11B 109.4 . . ?
H11A C11 H11B 108.0 . . ?
C4 C7 H7A 109.5 . . ?
C4 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
C4 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
C5 C8 H8A 109.5 . . ?
C5 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C5 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C15 C16 H16A 109.5 . . ?
C15 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
C15 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C11 C12 H12A 109.5 . . ?
C11 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C11 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C13 C14 H14A 109.5 . . ?
C13 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C13 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?

_diffrn_measured_fraction_theta_max 0.994
_diffrn_reflns_theta_full        26.00
_diffrn_measured_fraction_theta_full 1.000
_refine_diff_density_max         0.767
_refine_diff_density_min         -0.651
_refine_diff_density_rms         0.210
_database_code_depnum_ccdc_archive 'CCDC 997528'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_Ph6Si3H2

_audit_creation_method           'SHELXL-97 + manual editing'
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C36 H32 Si3'
_chemical_formula_weight         548.89

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   P-1

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   9.9470(12)
_cell_length_b                   10.5252(13)
_cell_length_c                   16.903(2)
_cell_angle_alpha                102.664(2)
_cell_angle_beta                 98.563(1)
_cell_angle_gamma                110.928(2)
_cell_volume                     1561.8(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    9903
_cell_measurement_theta_min      2.1675
_cell_measurement_theta_max      25.943

_exptl_crystal_description       plate
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.03
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.167
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             580
_exptl_absorpt_coefficient_mu    0.175
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6189
_exptl_absorpt_correction_T_max  0.7453
_exptl_absorpt_process_details   'SadAbs-2008/1 (Bruker, 2008)'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      173(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_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            5327
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0388
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         2.17
_diffrn_reflns_theta_max         24.71
_reflns_number_total             5327
_reflns_number_gt                4851
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Smart-NT v. 5.63'
_computing_cell_refinement       'Saint-NT v. 7.23'
_computing_data_reduction        'Saint-NT v. 7.23'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'XP in ShelxTL-97'
_computing_publication_material  'XP in ShelxTL-97'

_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)+(0.0636P)²+0.5968P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         5327
_refine_ls_number_parameters     360
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0465
_refine_ls_R_factor_gt           0.0430
_refine_ls_wR_factor_ref         0.1211
_refine_ls_wR_factor_gt          0.1175
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_restrained_S_all      1.029
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Si1 Si 0.13517(6) 0.29292(5) 0.14371(3) 0.04672(16) Uani 1 1 d . . .
H1 H 0.156(2) 0.178(2) 0.1695(14) 0.065(6) Uiso 1 1 d . . .
Si2 Si 0.26036(5) 0.50729(5) 0.25364(3) 0.03497(15) Uani 1 1 d . . .
Si3 Si 0.15007(5) 0.48156(5) 0.36667(3) 0.03672(15) Uani 1 1 d . . .
H3 H 0.006(2) 0.474(2) 0.3443(12) 0.045(5) Uiso 1 1 d . . .
C1 C -0.0700(2) 0.2470(2) 0.12068(13) 0.0511(5) Uani 1 1 d . . .
C2 C -0.1485(3) 0.2013(3) 0.17769(15) 0.0697(7) Uani 1 1 d . . .
H2A H -0.0979 0.1921 0.2270 0.084 Uiso 1 1 calc R . .
C3 C -0.2992(3) 0.1690(3) 0.16369(19) 0.0830(9) Uani 1 1 d . . .
H3A H -0.3504 0.1404 0.2042 0.100 Uiso 1 1 calc R . .
C4 C -0.3750(3) 0.1778(3) 0.0922(2) 0.0817(8) Uani 1 1 d . . .
H4A H -0.4789 0.1536 0.0824 0.098 Uiso 1 1 calc R . .
C5 C -0.3007(3) 0.2214(3) 0.03505(19) 0.0785(8) Uani 1 1 d . . .
H5A H -0.3530 0.2283 -0.0146 0.094 Uiso 1 1 calc R . .
C6 C -0.1489(3) 0.2561(3) 0.04877(15) 0.0642(6) Uani 1 1 d . . .
H6A H -0.0986 0.2864 0.0084 0.077 Uiso 1 1 calc R . .
C11 C 0.2085(2) 0.2982(2) 0.04750(13) 0.0503(5) Uani 1 1 d . . .
C12 C 0.2495(3) 0.4173(3) 0.02005(15) 0.0694(7) Uani 1 1 d . . .
H12A H 0.2365 0.4986 0.0491 0.083 Uiso 1 1 calc R . .
C13 C 0.3092(4) 0.4213(3) -0.04897(17) 0.0850(8) Uani 1 1 d . . .
H13A H 0.3379 0.5052 -0.0662 0.102 Uiso 1 1 calc R . .
C14 C 0.3268(3) 0.3046(4) -0.09222(18) 0.0859(9) Uani 1 1 d . . .
H14A H 0.3678 0.3069 -0.1394 0.103 Uiso 1 1 calc R . .
C15 C 0.2848(4) 0.1851(4) -0.06676(19) 0.0909(9) Uani 1 1 d . . .
H15A H 0.2961 0.1035 -0.0968 0.109 Uiso 1 1 calc R . .
C16 C 0.2260(3) 0.1810(3) 0.00222(16) 0.0726(7) Uani 1 1 d . . .
H16A H 0.1972 0.0965 0.0188 0.087 Uiso 1 1 calc R . .
C21 C 0.2326(2) 0.65844(18) 0.22127(10) 0.0374(4) Uani 1 1 d . . .
C22 C 0.0916(2) 0.6599(2) 0.20619(14) 0.0566(5) Uani 1 1 d . . .
H22A H 0.0098 0.5827 0.2108 0.068 Uiso 1 1 calc R . .
C23 C 0.0679(3) 0.7708(3) 0.18470(17) 0.0753(7) Uani 1 1 d . . .
H23A H -0.0291 0.7698 0.1750 0.090 Uiso 1 1 calc R . .
C24 C 0.1845(4) 0.8820(3) 0.17750(17) 0.0812(9) Uani 1 1 d . . .
H24A H 0.1687 0.9590 0.1633 0.097 Uiso 1 1 calc R . .
C25 C 0.3236(3) 0.8828(2) 0.19068(17) 0.0798(8) Uani 1 1 d . . .
H25A H 0.4041 0.9600 0.1850 0.096 Uiso 1 1 calc R . .
C26 C 0.3486(2) 0.7714(2) 0.21244(13) 0.0537(5) Uani 1 1 d . . .
H26A H 0.4458 0.7730 0.2213 0.064 Uiso 1 1 calc R . .
C31 C 0.46553(19) 0.55149(18) 0.28591(11) 0.0366(4) Uani 1 1 d . . .
C32 C 0.5346(2) 0.4790(2) 0.23982(13) 0.0494(5) Uani 1 1 d . . .
H32A H 0.4768 0.4026 0.1907 0.059 Uiso 1 1 calc R . .
C33 C 0.6868(2) 0.5164(2) 0.26427(15) 0.0595(6) Uani 1 1 d . . .
H33A H 0.7317 0.4656 0.2318 0.071 Uiso 1 1 calc R . .
C34 C 0.7722(2) 0.6262(2) 0.33519(14) 0.0521(5) Uani 1 1 d . . .
H34A H 0.8764 0.6524 0.3513 0.062 Uiso 1 1 calc R . .
C35 C 0.7068(2) 0.6982(2) 0.38271(13) 0.0491(5) Uani 1 1 d . . .
H35A H 0.7654 0.7733 0.4323 0.059 Uiso 1 1 calc R . .
C36 C 0.5554(2) 0.6615(2) 0.35843(12) 0.0455(4) Uani 1 1 d . . .
H36A H 0.5115 0.7122 0.3918 0.055 Uiso 1 1 calc R . .
C41 C 0.25105(19) 0.64171(19) 0.46145(11) 0.0381(4) Uani 1 1 d . . .
C42 C 0.3098(2) 0.6314(2) 0.53864(13) 0.0484(5) Uani 1 1 d . . .
H42A H 0.3002 0.5410 0.5445 0.058 Uiso 1 1 calc R . .
C43 C 0.3822(2) 0.7516(3) 0.60698(14) 0.0596(6) Uani 1 1 d . . .
H43A H 0.4215 0.7431 0.6594 0.072 Uiso 1 1 calc R . .
C44 C 0.3976(2) 0.8835(2) 0.59959(14) 0.0571(5) Uani 1 1 d . . .
H44A H 0.4472 0.9657 0.6468 0.069 Uiso 1 1 calc R . .
C45 C 0.3408(2) 0.8960(2) 0.52370(14) 0.0509(5) Uani 1 1 d . . .
H45A H 0.3519 0.9869 0.5183 0.061 Uiso 1 1 calc R . .
C46 C 0.2676(2) 0.7764(2) 0.45534(12) 0.0443(4) Uani 1 1 d . . .
H46A H 0.2280 0.7859 0.4033 0.053 Uiso 1 1 calc R . .
C51 C 0.13324(19) 0.30926(18) 0.38731(11) 0.0372(4) Uani 1 1 d . . .
C52 C 0.0027(2) 0.2228(2) 0.40270(13) 0.0473(5) Uani 1 1 d . . .
H52A H -0.0722 0.2573 0.4100 0.057 Uiso 1 1 calc R . .
C53 C -0.0197(2) 0.0876(2) 0.40752(15) 0.0561(5) Uani 1 1 d . . .
H53A H -0.1097 0.0299 0.4176 0.067 Uiso 1 1 calc R . .
C54 C 0.0875(2) 0.0363(2) 0.39775(14) 0.0536(5) Uani 1 1 d . . .
H54A H 0.0711 -0.0573 0.4001 0.064 Uiso 1 1 calc R . .
C55 C 0.2184(2) 0.1204(2) 0.38452(14) 0.0545(5) Uani 1 1 d . . .
H55A H 0.2936 0.0858 0.3788 0.065 Uiso 1 1 calc R . .
C56 C 0.2412(2) 0.2559(2) 0.37948(13) 0.0477(5) Uani 1 1 d . . .
H56A H 0.3325 0.3133 0.3705 0.057 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
Si1 C1 1.878(2) . ?
Si1 C11 1.883(2) . ?
Si1 Si2 2.3578(7) . ?
Si2 C21 1.8858(17) . ?
Si2 C31 1.8862(17) . ?
Si2 Si3 2.3592(7) . ?
Si3 C51 1.8753(17) . ?
Si3 C41 1.8826(19) . ?
C1 C6 1.387(3) . ?
C1 C2 1.388(3) . ?
C2 C3 1.383(4) . ?
C3 C4 1.366(4) . ?
C4 C5 1.362(4) . ?
C5 C6 1.390(3) . ?
C11 C12 1.379(3) . ?
C11 C16 1.384(3) . ?
C12 C13 1.388(4) . ?
C13 C14 1.368(4) . ?
C14 C15 1.363(4) . ?
C15 C16 1.382(4) . ?
C21 C26 1.384(3) . ?
C21 C22 1.394(3) . ?
C22 C23 1.381(3) . ?
C23 C24 1.365(4) . ?
C24 C25 1.366(4) . ?
C25 C26 1.394(3) . ?
C31 C32 1.391(3) . ?
C31 C36 1.398(3) . ?
C32 C33 1.390(3) . ?
C33 C34 1.372(3) . ?
C34 C35 1.373(3) . ?
C35 C36 1.384(3) . ?
C41 C42 1.392(3) . ?
C41 C46 1.396(3) . ?
C42 C43 1.384(3) . ?
C43 C44 1.378(3) . ?
C44 C45 1.376(3) . ?
C45 C46 1.381(3) . ?
C51 C56 1.389(3) . ?
C51 C52 1.394(2) . ?
C52 C53 1.382(3) . ?
C53 C54 1.371(3) . ?
C54 C55 1.371(3) . ?
C55 C56 1.385(3) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C1 Si1 C11 112.21(9) . . ?
C1 Si1 Si2 109.38(7) . . ?
C11 Si1 Si2 112.80(7) . . ?
C21 Si2 C31 109.38(8) . . ?
C21 Si2 Si1 110.33(6) . . ?
C31 Si2 Si1 111.47(6) . . ?
C21 Si2 Si3 106.81(6) . . ?
C31 Si2 Si3 111.03(6) . . ?
Si1 Si2 Si3 107.71(3) . . ?
C51 Si3 C41 113.69(8) . . ?
C51 Si3 Si2 109.81(6) . . ?
C41 Si3 Si2 111.47(6) . . ?
C6 C1 C2 117.5(2) . . ?
C6 C1 Si1 123.24(17) . . ?
C2 C1 Si1 119.23(17) . . ?
C3 C2 C1 120.9(2) . . ?
C4 C3 C2 120.6(3) . . ?
C5 C4 C3 119.6(2) . . ?
C4 C5 C6 120.5(3) . . ?
C1 C6 C5 120.9(2) . . ?
C12 C11 C16 117.3(2) . . ?
C12 C11 Si1 122.32(16) . . ?
C16 C11 Si1 120.35(19) . . ?
C11 C12 C13 121.5(2) . . ?
C14 C13 C12 120.1(3) . . ?
C15 C14 C13 119.2(3) . . ?
C14 C15 C16 120.9(3) . . ?
C15 C16 C11 121.0(3) . . ?
C26 C21 C22 117.56(18) . . ?
C26 C21 Si2 122.41(15) . . ?
C22 C21 Si2 120.03(14) . . ?
C23 C22 C21 121.6(2) . . ?
C24 C23 C22 119.7(2) . . ?
C23 C24 C25 120.1(2) . . ?
C24 C25 C26 120.6(2) . . ?
C21 C26 C25 120.4(2) . . ?
C32 C31 C36 117.02(16) . . ?
C32 C31 Si2 122.67(14) . . ?
C36 C31 Si2 120.31(13) . . ?
C33 C32 C31 121.26(19) . . ?
C34 C33 C32 120.26(19) . . ?
C33 C34 C35 119.81(18) . . ?
C34 C35 C36 120.05(19) . . ?
C35 C36 C31 121.58(18) . . ?
C42 C41 C46 118.03(18) . . ?
C42 C41 Si3 122.38(14) . . ?
C46 C41 Si3 119.59(14) . . ?
C43 C42 C41 120.58(19) . . ?
C44 C43 C42 120.5(2) . . ?
C45 C44 C43 119.8(2) . . ?
C44 C45 C46 120.06(19) . . ?
C45 C46 C41 121.05(19) . . ?
C56 C51 C52 117.41(17) . . ?
C56 C51 Si3 122.17(13) . . ?
C52 C51 Si3 120.09(13) . . ?
C53 C52 C51 121.09(18) . . ?
C54 C53 C52 120.29(18) . . ?
C55 C54 C53 119.80(18) . . ?
C54 C55 C56 120.12(18) . . ?
C55 C56 C51 121.26(18) . . ?

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        24.71
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         0.437
_refine_diff_density_min         -0.215
_refine_diff_density_rms         0.050



#===END
_database_code_depnum_ccdc_archive 'CCDC 997529'
