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

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

data_Complex_6
_database_code_depnum_ccdc_archive 'CCDC 1476054'
_audit_update_record             
;
2016-05-13 deposited with the CCDC.
2016-06-21 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        'Complex 6'
_chemical_name_common            'Complex 6'
_chemical_melting_point          '463.2 (dec.)'
_chemical_formula_moiety         'C31 H28 B N6 Ni O'
_chemical_formula_sum            'C31 H28 B N6 Ni O'
_chemical_formula_weight         570.11

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   P2(1)/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                   11.481(5)
_cell_length_b                   15.958(5)
_cell_length_c                   15.833(5)
_cell_angle_alpha                90.000(5)
_cell_angle_beta                 100.343(5)
_cell_angle_gamma                90.000(5)
_cell_volume                     2853.7(18)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    8470
_cell_measurement_theta_min      2.21
_cell_measurement_theta_max      24.59

_exptl_crystal_description       plate
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.09
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.02
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.327
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1188
_exptl_absorpt_coefficient_mu    0.715
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6585
_exptl_absorpt_correction_T_max  0.8109
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean 8.366
_diffrn_reflns_number            53528
_diffrn_reflns_av_R_equivalents  0.1244
_diffrn_reflns_av_sigmaI/netI    0.0662
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         1.83
_diffrn_reflns_theta_max         25.42
_reflns_number_total             5259
_reflns_number_gt                3491
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker APEX2 v.2011.4'
_computing_cell_refinement       'Bruker APEX2 v.2011.4'
_computing_data_reduction        'Bruker APEX2 v.2011.4'
_computing_structure_solution    SIR-92
_computing_structure_refinement  SHELXL-97
_computing_molecular_graphics    ORTEP-32
_computing_publication_material  WinGX

_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)+(0.0327P)²+3.0717P] 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         5259
_refine_ls_number_parameters     368
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0889
_refine_ls_R_factor_gt           0.0484
_refine_ls_wR_factor_ref         0.1097
_refine_ls_wR_factor_gt          0.0951
_refine_ls_goodness_of_fit_ref   1.018
_refine_ls_restrained_S_all      1.018
_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
C1 C 0.1044(3) 0.0321(3) 0.7253(2) 0.0404(10) Uani 1 1 d . . .
C2 C 0.5690(3) -0.2381(2) 0.8450(2) 0.0370(9) Uani 1 1 d . . .
H2A H 0.5995 -0.2337 0.7926 0.056 Uiso 1 1 calc R . .
H2B H 0.5665 -0.2960 0.8610 0.056 Uiso 1 1 calc R . .
H2C H 0.6194 -0.2078 0.8896 0.056 Uiso 1 1 calc R . .
C3 C 0.4466(3) -0.2021(2) 0.8321(2) 0.0284(8) Uani 1 1 d . . .
C4 C 0.3412(3) -0.2423(2) 0.8314(2) 0.0291(8) Uani 1 1 d . . .
H4 H 0.3300 -0.2992 0.8399 0.035 Uiso 1 1 calc R . .
C5 C 0.2538(3) -0.1806(2) 0.8152(2) 0.0254(8) Uani 1 1 d . . .
C6 C 0.1262(3) -0.1906(2) 0.8121(2) 0.0293(8) Uani 1 1 d . . .
C7 C 0.0697(3) -0.2627(2) 0.7759(2) 0.0334(9) Uani 1 1 d . . .
H7 H 0.1124 -0.3022 0.7509 0.040 Uiso 1 1 calc R . .
C8 C -0.0490(4) -0.2763(3) 0.7765(3) 0.0454(11) Uani 1 1 d . . .
H8 H -0.0858 -0.3244 0.7516 0.055 Uiso 1 1 calc R . .
C9 C -0.1122(4) -0.2187(3) 0.8137(3) 0.0555(13) Uani 1 1 d . . .
H9 H -0.1919 -0.2282 0.8147 0.067 Uiso 1 1 calc R . .
C10 C -0.0581(4) -0.1464(3) 0.8501(3) 0.0510(12) Uani 1 1 d . . .
H10 H -0.1018 -0.1074 0.8749 0.061 Uiso 1 1 calc R . .
C11 C 0.0609(3) -0.1320(2) 0.8496(2) 0.0390(10) Uani 1 1 d . . .
H11 H 0.0971 -0.0836 0.8742 0.047 Uiso 1 1 calc R . .
C12 C 0.6760(3) 0.0576(2) 0.9597(2) 0.0369(9) Uani 1 1 d . . .
H12A H 0.6856 0.0009 0.9798 0.055 Uiso 1 1 calc R . .
H12B H 0.7075 0.0952 1.0055 0.055 Uiso 1 1 calc R . .
H12C H 0.7176 0.0653 0.9128 0.055 Uiso 1 1 calc R . .
C13 C 0.5480(3) 0.0756(2) 0.9302(2) 0.0293(8) Uani 1 1 d . . .
C14 C 0.4800(3) 0.1399(2) 0.9534(2) 0.0305(8) Uani 1 1 d . . .
H14 H 0.5053 0.1827 0.9922 0.037 Uiso 1 1 calc R . .
C15 C 0.3661(3) 0.1282(2) 0.9073(2) 0.0286(8) Uani 1 1 d . . .
C16 C 0.2588(3) 0.1791(2) 0.9072(2) 0.0320(9) Uani 1 1 d . . .
C17 C 0.1485(3) 0.1432(2) 0.9034(2) 0.0375(9) Uani 1 1 d . . .
H17 H 0.1412 0.0851 0.9036 0.045 Uiso 1 1 calc R . .
C18 C 0.0479(4) 0.1929(3) 0.8993(3) 0.0463(11) Uani 1 1 d . . .
H18 H -0.0258 0.1680 0.8972 0.056 Uiso 1 1 calc R . .
C19 C 0.0574(4) 0.2795(3) 0.8985(2) 0.0450(11) Uani 1 1 d . . .
H19 H -0.0100 0.3128 0.8941 0.054 Uiso 1 1 calc R . .
C20 C 0.1670(4) 0.3157(2) 0.9043(2) 0.0434(10) Uani 1 1 d . . .
H20 H 0.1738 0.3737 0.9055 0.052 Uiso 1 1 calc R . .
C21 C 0.2677(4) 0.2667(2) 0.9084(2) 0.0389(9) Uani 1 1 d . . .
H21 H 0.3413 0.2921 0.9119 0.047 Uiso 1 1 calc R . .
C22 C 0.7033(3) -0.0151(2) 0.6969(2) 0.0383(9) Uani 1 1 d . . .
H22A H 0.7436 -0.0016 0.6505 0.057 Uiso 1 1 calc R . .
H22B H 0.7115 -0.0740 0.7093 0.057 Uiso 1 1 calc R . .
H22C H 0.7371 0.0164 0.7469 0.057 Uiso 1 1 calc R . .
C23 C 0.5749(3) 0.0062(2) 0.6718(2) 0.0276(8) Uani 1 1 d . . .
C24 C 0.5169(3) 0.0463(2) 0.5988(2) 0.0295(8) Uani 1 1 d . . .
H24 H 0.5504 0.0658 0.5532 0.035 Uiso 1 1 calc R . .
C25 C 0.3986(3) 0.0516(2) 0.6070(2) 0.0244(8) Uani 1 1 d . . .
C26 C 0.2997(3) 0.0877(2) 0.5460(2) 0.0260(8) Uani 1 1 d . . .
C27 C 0.1907(3) 0.0477(2) 0.5249(2) 0.0304(8) Uani 1 1 d . . .
H27 H 0.1776 -0.0025 0.5516 0.036 Uiso 1 1 calc R . .
C28 C 0.1010(3) 0.0824(2) 0.4640(2) 0.0356(9) Uani 1 1 d . . .
H28 H 0.0285 0.0551 0.4501 0.043 Uiso 1 1 calc R . .
C29 C 0.1188(3) 0.1569(2) 0.4241(2) 0.0382(10) Uani 1 1 d . . .
H29 H 0.0588 0.1796 0.3832 0.046 Uiso 1 1 calc R . .
C30 C 0.2262(3) 0.1978(2) 0.4452(2) 0.0406(10) Uani 1 1 d . . .
H30 H 0.2385 0.2482 0.4186 0.049 Uiso 1 1 calc R . .
C31 C 0.3155(3) 0.1637(2) 0.5058(2) 0.0321(9) Uani 1 1 d . . .
H31 H 0.3872 0.1919 0.5200 0.039 Uiso 1 1 calc R . .
B1 B 0.5091(4) -0.0449(3) 0.8145(2) 0.0268(9) Uani 1 1 d . . .
N1 N 0.3037(2) -0.10551(17) 0.80570(17) 0.0263(7) Uani 1 1 d . . .
N2 N 0.4242(2) -0.11944(18) 0.81728(17) 0.0265(7) Uani 1 1 d . . .
N3 N 0.3638(2) 0.06027(17) 0.85646(17) 0.0271(7) Uani 1 1 d . . .
N4 N 0.4764(2) 0.02730(17) 0.87139(17) 0.0272(7) Uani 1 1 d . . .
N5 N 0.3840(2) 0.01690(17) 0.68193(17) 0.0246(6) Uani 1 1 d . . .
N6 N 0.4938(2) -0.01061(17) 0.72167(16) 0.0258(6) Uani 1 1 d . . .
O1 O 0.0060(3) 0.0485(2) 0.7140(2) 0.0637(9) Uani 1 1 d . . .
Ni1 Ni 0.25608(4) 0.00754(3) 0.75591(3) 0.02641(14) Uani 1 1 d . . .
H1 H 0.604(2) -0.0625(17) 0.8371(17) 0.013(7) 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
C1 O1 1.141(4) . ?
C1 Ni1 1.766(4) . ?
C2 C3 1.498(5) . ?
C2 H2A 0.9600 . ?
C2 H2B 0.9600 . ?
C2 H2C 0.9600 . ?
C3 N2 1.356(4) . ?
C3 C4 1.369(5) . ?
C4 C5 1.396(5) . ?
C4 H4 0.9300 . ?
C5 N1 1.349(4) . ?
C5 C6 1.466(5) . ?
C6 C7 1.392(5) . ?
C6 C11 1.396(5) . ?
C7 C8 1.381(5) . ?
C7 H7 0.9300 . ?
C8 C9 1.368(6) . ?
C8 H8 0.9300 . ?
C9 C10 1.386(6) . ?
C9 H9 0.9300 . ?
C10 C11 1.387(5) . ?
C10 H10 0.9300 . ?
C11 H11 0.9300 . ?
C12 C13 1.488(5) . ?
C12 H12A 0.9600 . ?
C12 H12B 0.9600 . ?
C12 H12C 0.9600 . ?
C13 N4 1.364(4) . ?
C13 C14 1.379(5) . ?
C14 C15 1.391(5) . ?
C14 H14 0.9300 . ?
C15 N3 1.347(4) . ?
C15 C16 1.475(5) . ?
C16 C17 1.382(5) . ?
C16 C21 1.402(5) . ?
C17 C18 1.394(5) . ?
C17 H17 0.9300 . ?
C18 C19 1.385(6) . ?
C18 H18 0.9300 . ?
C19 C20 1.373(6) . ?
C19 H19 0.9300 . ?
C20 C21 1.387(5) . ?
C20 H20 0.9300 . ?
C21 H21 0.9300 . ?
C22 C23 1.495(5) . ?
C22 H22A 0.9600 . ?
C22 H22B 0.9600 . ?
C22 H22C 0.9600 . ?
C23 N6 1.352(4) . ?
C23 C24 1.383(5) . ?
C24 C25 1.390(5) . ?
C24 H24 0.9300 . ?
C25 N5 1.346(4) . ?
C25 C26 1.470(5) . ?
C26 C27 1.391(5) . ?
C26 C31 1.397(5) . ?
C27 C28 1.394(5) . ?
C27 H27 0.9300 . ?
C28 C29 1.378(5) . ?
C28 H28 0.9300 . ?
C29 C30 1.382(5) . ?
C29 H29 0.9300 . ?
C30 C31 1.383(5) . ?
C30 H30 0.9300 . ?
C31 H31 0.9300 . ?
B1 N2 1.544(5) . ?
B1 N6 1.548(5) . ?
B1 N4 1.549(5) . ?
B1 H1 1.12(3) . ?
N1 N2 1.380(4) . ?
N1 Ni1 2.005(3) . ?
N3 N4 1.377(4) . ?
N3 Ni1 2.016(3) . ?
N5 N6 1.376(4) . ?
N5 Ni1 2.041(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
O1 C1 Ni1 173.2(4) . . ?
C3 C2 H2A 109.5 . . ?
C3 C2 H2B 109.5 . . ?
H2A C2 H2B 109.5 . . ?
C3 C2 H2C 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
N2 C3 C4 108.3(3) . . ?
N2 C3 C2 122.8(3) . . ?
C4 C3 C2 128.9(3) . . ?
C3 C4 C5 106.0(3) . . ?
C3 C4 H4 127.0 . . ?
C5 C4 H4 127.0 . . ?
N1 C5 C4 110.0(3) . . ?
N1 C5 C6 122.4(3) . . ?
C4 C5 C6 127.6(3) . . ?
C7 C6 C11 118.9(3) . . ?
C7 C6 C5 119.5(3) . . ?
C11 C6 C5 121.5(3) . . ?
C8 C7 C6 120.9(4) . . ?
C8 C7 H7 119.5 . . ?
C6 C7 H7 119.5 . . ?
C9 C8 C7 119.9(4) . . ?
C9 C8 H8 120.1 . . ?
C7 C8 H8 120.1 . . ?
C8 C9 C10 120.3(4) . . ?
C8 C9 H9 119.8 . . ?
C10 C9 H9 119.8 . . ?
C9 C10 C11 120.3(4) . . ?
C9 C10 H10 119.9 . . ?
C11 C10 H10 119.9 . . ?
C10 C11 C6 119.7(4) . . ?
C10 C11 H11 120.1 . . ?
C6 C11 H11 120.1 . . ?
C13 C12 H12A 109.5 . . ?
C13 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C13 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
N4 C13 C14 107.6(3) . . ?
N4 C13 C12 123.1(3) . . ?
C14 C13 C12 129.4(3) . . ?
C13 C14 C15 106.5(3) . . ?
C13 C14 H14 126.7 . . ?
C15 C14 H14 126.7 . . ?
N3 C15 C14 109.7(3) . . ?
N3 C15 C16 121.0(3) . . ?
C14 C15 C16 129.2(3) . . ?
C17 C16 C21 118.6(3) . . ?
C17 C16 C15 122.0(3) . . ?
C21 C16 C15 119.4(3) . . ?
C16 C17 C18 120.7(4) . . ?
C16 C17 H17 119.6 . . ?
C18 C17 H17 119.6 . . ?
C19 C18 C17 120.2(4) . . ?
C19 C18 H18 119.9 . . ?
C17 C18 H18 119.9 . . ?
C20 C19 C18 119.4(4) . . ?
C20 C19 H19 120.3 . . ?
C18 C19 H19 120.3 . . ?
C19 C20 C21 120.9(4) . . ?
C19 C20 H20 119.6 . . ?
C21 C20 H20 119.6 . . ?
C20 C21 C16 120.2(4) . . ?
C20 C21 H21 119.9 . . ?
C16 C21 H21 119.9 . . ?
C23 C22 H22A 109.5 . . ?
C23 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
C23 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
N6 C23 C24 107.6(3) . . ?
N6 C23 C22 123.3(3) . . ?
C24 C23 C22 129.1(3) . . ?
C23 C24 C25 106.3(3) . . ?
C23 C24 H24 126.8 . . ?
C25 C24 H24 126.8 . . ?
N5 C25 C24 109.7(3) . . ?
N5 C25 C26 122.4(3) . . ?
C24 C25 C26 127.9(3) . . ?
C27 C26 C31 118.3(3) . . ?
C27 C26 C25 122.3(3) . . ?
C31 C26 C25 119.4(3) . . ?
C26 C27 C28 120.3(3) . . ?
C26 C27 H27 119.8 . . ?
C28 C27 H27 119.8 . . ?
C29 C28 C27 120.5(4) . . ?
C29 C28 H28 119.7 . . ?
C27 C28 H28 119.7 . . ?
C28 C29 C30 119.7(3) . . ?
C28 C29 H29 120.1 . . ?
C30 C29 H29 120.1 . . ?
C29 C30 C31 120.0(4) . . ?
C29 C30 H30 120.0 . . ?
C31 C30 H30 120.0 . . ?
C30 C31 C26 121.1(4) . . ?
C30 C31 H31 119.4 . . ?
C26 C31 H31 119.4 . . ?
N2 B1 N6 109.6(3) . . ?
N2 B1 N4 109.6(3) . . ?
N6 B1 N4 107.0(3) . . ?
N2 B1 H1 112.4(14) . . ?
N6 B1 H1 109.2(14) . . ?
N4 B1 H1 108.9(14) . . ?
C5 N1 N2 106.1(3) . . ?
C5 N1 Ni1 138.8(2) . . ?
N2 N1 Ni1 113.2(2) . . ?
C3 N2 N1 109.5(3) . . ?
C3 N2 B1 130.8(3) . . ?
N1 N2 B1 119.7(3) . . ?
C15 N3 N4 106.7(3) . . ?
C15 N3 Ni1 138.7(2) . . ?
N4 N3 Ni1 113.6(2) . . ?
C13 N4 N3 109.5(3) . . ?
C13 N4 B1 129.6(3) . . ?
N3 N4 B1 120.1(3) . . ?
C25 N5 N6 106.6(3) . . ?
C25 N5 Ni1 138.8(2) . . ?
N6 N5 Ni1 114.12(19) . . ?
C23 N6 N5 109.9(3) . . ?
C23 N6 B1 130.7(3) . . ?
N5 N6 B1 119.0(3) . . ?
C1 Ni1 N1 119.59(16) . . ?
C1 Ni1 N3 123.97(15) . . ?
N1 Ni1 N3 88.83(11) . . ?
C1 Ni1 N5 127.00(15) . . ?
N1 Ni1 N5 96.77(11) . . ?
N3 Ni1 N5 91.15(11) . . ?

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 1.000
_refine_diff_density_max         0.366
_refine_diff_density_min         -0.450
_refine_diff_density_rms         0.067
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent'
_solvent_exptl_crystal_recrystallization_method Hexanes
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_Complex_8a
_database_code_depnum_ccdc_archive 'CCDC 1476055'
_audit_update_record             
;
2016-05-13 deposited with the CCDC.
2016-06-21 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        'Complex 8a'
_chemical_name_common            'Complex 8a'
_chemical_melting_point          385.2-387.2
_chemical_formula_moiety         'C39 H35 B N6 Ni O2'
_chemical_formula_sum            'C39 H35 B N6 Ni O2'
_chemical_formula_weight         689.25

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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 '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                   12.5248(8)
_cell_length_b                   15.0744(9)
_cell_length_c                   18.1859(10)
_cell_angle_alpha                90.00
_cell_angle_beta                 95.122(3)
_cell_angle_gamma                90.00
_cell_volume                     3419.9(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9099
_cell_measurement_theta_min      2.25
_cell_measurement_theta_max      25.45

_exptl_crystal_description       plate
_exptl_crystal_colour            red
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.02
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.339
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1440
_exptl_absorpt_coefficient_mu    0.612
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.8261
_exptl_absorpt_correction_T_max  0.9545
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean 8.366
_diffrn_reflns_number            39367
_diffrn_reflns_av_R_equivalents  0.0238
_diffrn_reflns_av_sigmaI/netI    0.0171
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         1.76
_diffrn_reflns_theta_max         25.48
_reflns_number_total             6334
_reflns_number_gt                5785
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker APEX2 v.2011.4'
_computing_cell_refinement       'Bruker APEX2 v.2011.4'
_computing_data_reduction        'Bruker APEX2 v.2011.4'
_computing_structure_solution    SIR-92
_computing_structure_refinement  SHELXL-97
_computing_molecular_graphics    ORTEP-32
_computing_publication_material  WinGX

_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)+(0.0423P)²+4.0404P] 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         6334
_refine_ls_number_parameters     449
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0301
_refine_ls_R_factor_gt           0.0268
_refine_ls_wR_factor_ref         0.0722
_refine_ls_wR_factor_gt          0.0695
_refine_ls_goodness_of_fit_ref   0.814
_refine_ls_restrained_S_all      0.814
_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
C2 C 0.36577(13) 0.37672(11) 0.03367(8) 0.0202(3) Uani 1 1 d . . .
C1 C 0.38073(12) 0.30342(10) 0.16390(8) 0.0167(3) Uani 1 1 d . . .
C3 C 0.38876(14) 0.22605(11) 0.21963(9) 0.0224(3) Uani 1 1 d . . .
H3A H 0.3304 0.1852 0.2064 0.027 Uiso 1 1 calc R . .
H3B H 0.4552 0.1945 0.2145 0.027 Uiso 1 1 calc R . .
C4 C 0.38535(13) 0.25102(10) 0.29959(8) 0.0162(3) Uani 1 1 d . . .
C9 C 0.47866(14) 0.27215(11) 0.34210(9) 0.0221(3) Uani 1 1 d . . .
H9 H 0.5426 0.2766 0.3200 0.027 Uiso 1 1 calc R . .
C8 C 0.47841(18) 0.28692(12) 0.41751(10) 0.0352(5) Uani 1 1 d . . .
H8 H 0.5419 0.3005 0.4457 0.042 Uiso 1 1 calc R . .
C7 C 0.3832(2) 0.28126(13) 0.45042(10) 0.0429(6) Uani 1 1 d . . .
H7 H 0.3825 0.2907 0.5009 0.052 Uiso 1 1 calc R . .
C6 C 0.28983(19) 0.26163(14) 0.40824(11) 0.0424(5) Uani 1 1 d . . .
H6 H 0.2257 0.2584 0.4302 0.051 Uiso 1 1 calc R . .
C5 C 0.29040(14) 0.24667(13) 0.33328(10) 0.0297(4) Uani 1 1 d . . .
H5 H 0.2266 0.2336 0.3052 0.036 Uiso 1 1 calc R . .
C10 C 0.13043(13) -0.00031(11) 0.16708(9) 0.0225(3) Uani 1 1 d . . .
H10A H 0.1143 -0.0353 0.1234 0.034 Uiso 1 1 calc R . .
H10B H 0.0742 -0.0071 0.1992 0.034 Uiso 1 1 calc R . .
H10C H 0.1971 -0.0198 0.1920 0.034 Uiso 1 1 calc R . .
C11 C 0.13939(12) 0.09516(10) 0.14619(8) 0.0168(3) Uani 1 1 d . . .
C12 C 0.08845(12) 0.16946(10) 0.17103(8) 0.0181(3) Uani 1 1 d . . .
H12 H 0.0364 0.1708 0.2044 0.022 Uiso 1 1 calc R . .
C13 C 0.13107(12) 0.24218(10) 0.13571(8) 0.0158(3) Uani 1 1 d . . .
C14 C 0.10460(12) 0.33744(10) 0.13953(8) 0.0173(3) Uani 1 1 d . . .
C15 C 0.11142(13) 0.39240(11) 0.07819(9) 0.0218(3) Uani 1 1 d . . .
H15 H 0.1316 0.3686 0.0343 0.026 Uiso 1 1 calc R . .
C16 C 0.08834(14) 0.48203(11) 0.08222(10) 0.0271(4) Uani 1 1 d . . .
H16 H 0.0942 0.5182 0.0414 0.032 Uiso 1 1 calc R . .
C17 C 0.05652(14) 0.51801(12) 0.14697(10) 0.0300(4) Uani 1 1 d . . .
H17 H 0.0414 0.5783 0.1497 0.036 Uiso 1 1 calc R . .
C18 C 0.04729(15) 0.46390(12) 0.20753(10) 0.0302(4) Uani 1 1 d . . .
H18 H 0.0247 0.4877 0.2507 0.036 Uiso 1 1 calc R . .
C19 C 0.07161(13) 0.37417(11) 0.20404(9) 0.0223(3) Uani 1 1 d . . .
H19 H 0.0658 0.3383 0.2451 0.027 Uiso 1 1 calc R . .
C20 C 0.16069(13) 0.00601(11) -0.10579(9) 0.0215(3) Uani 1 1 d . . .
H20A H 0.2029 -0.0413 -0.0830 0.032 Uiso 1 1 calc R . .
H20B H 0.1449 -0.0065 -0.1574 0.032 Uiso 1 1 calc R . .
H20C H 0.0949 0.0112 -0.0827 0.032 Uiso 1 1 calc R . .
C21 C 0.22186(12) 0.09114(10) -0.09685(8) 0.0164(3) Uani 1 1 d . . .
C22 C 0.24038(12) 0.15569(10) -0.14829(8) 0.0183(3) Uani 1 1 d . . .
H22 H 0.2211 0.1538 -0.1989 0.022 Uiso 1 1 calc R . .
C23 C 0.29417(12) 0.22452(10) -0.10848(8) 0.0160(3) Uani 1 1 d . . .
C24 C 0.33168(13) 0.31159(10) -0.13412(8) 0.0181(3) Uani 1 1 d . . .
C25 C 0.25761(14) 0.37581(11) -0.16002(8) 0.0227(3) Uani 1 1 d . . .
H25 H 0.1847 0.3632 -0.1626 0.027 Uiso 1 1 calc R . .
C26 C 0.29203(16) 0.45849(11) -0.18199(9) 0.0297(4) Uani 1 1 d . . .
H26 H 0.2420 0.5009 -0.1994 0.036 Uiso 1 1 calc R . .
C27 C 0.40031(16) 0.47814(12) -0.17810(9) 0.0306(4) Uani 1 1 d . . .
H27 H 0.4230 0.5338 -0.1922 0.037 Uiso 1 1 calc R . .
C28 C 0.47455(15) 0.41470(12) -0.15316(9) 0.0291(4) Uani 1 1 d . . .
H28 H 0.5474 0.4275 -0.1509 0.035 Uiso 1 1 calc R . .
C29 C 0.44040(14) 0.33156(11) -0.13142(9) 0.0235(3) Uani 1 1 d . . .
H29 H 0.4907 0.2890 -0.1149 0.028 Uiso 1 1 calc R . .
C30 C 0.44022(13) -0.08373(10) 0.09346(9) 0.0210(3) Uani 1 1 d . . .
H30A H 0.3806 -0.0935 0.1221 0.032 Uiso 1 1 calc R . .
H30B H 0.5007 -0.1175 0.1139 0.032 Uiso 1 1 calc R . .
H30C H 0.4214 -0.1021 0.0434 0.032 Uiso 1 1 calc R . .
C31 C 0.46830(12) 0.01276(10) 0.09480(8) 0.0170(3) Uani 1 1 d . . .
C32 C 0.56560(12) 0.05285(10) 0.11344(8) 0.0185(3) Uani 1 1 d . . .
H32 H 0.6294 0.0250 0.1303 0.022 Uiso 1 1 calc R . .
C33 C 0.54954(12) 0.14412(10) 0.10201(8) 0.0155(3) Uani 1 1 d . . .
C34 C 0.63108(12) 0.21499(10) 0.10867(8) 0.0165(3) Uani 1 1 d . . .
C35 C 0.62550(12) 0.28855(11) 0.06181(9) 0.0192(3) Uani 1 1 d . . .
H35 H 0.5663 0.2959 0.0277 0.023 Uiso 1 1 calc R . .
C36 C 0.70730(13) 0.35082(11) 0.06552(9) 0.0233(3) Uani 1 1 d . . .
H36 H 0.7024 0.3997 0.0342 0.028 Uiso 1 1 calc R . .
C37 C 0.79648(13) 0.34036(11) 0.11581(10) 0.0248(4) Uani 1 1 d . . .
H37 H 0.8521 0.3814 0.1176 0.030 Uiso 1 1 calc R . .
C38 C 0.80207(14) 0.26841(11) 0.16326(9) 0.0246(4) Uani 1 1 d . . .
H38 H 0.8610 0.2619 0.1978 0.029 Uiso 1 1 calc R . .
C39 C 0.72042(13) 0.20592(11) 0.15973(9) 0.0207(3) Uani 1 1 d . . .
H39 H 0.7253 0.1576 0.1916 0.025 Uiso 1 1 calc R . .
N2 N 0.20781(10) 0.12335(8) 0.09746(7) 0.0155(3) Uani 1 1 d . . .
N1 N 0.20495(10) 0.21406(8) 0.09151(7) 0.0156(3) Uani 1 1 d . . .
N4 N 0.26556(10) 0.11986(8) -0.03025(7) 0.0156(3) Uani 1 1 d . . .
N3 N 0.30878(10) 0.20292(8) -0.03692(7) 0.0157(3) Uani 1 1 d . . .
N6 N 0.39681(10) 0.07757(8) 0.07479(7) 0.0152(3) Uani 1 1 d . . .
N5 N 0.44620(10) 0.15883(8) 0.07939(7) 0.0150(3) Uani 1 1 d . . .
O2 O 0.37742(11) 0.44958(8) 0.02006(7) 0.0319(3) Uani 1 1 d . . .
O1 O 0.39150(13) 0.37836(8) 0.18306(6) 0.0383(3) Uani 1 1 d . . .
Ni1 Ni 0.349696(15) 0.264461(12) 0.061876(10) 0.01333(7) Uani 1 1 d . . .
B1 B 0.27704(14) 0.07215(11) 0.04545(9) 0.0161(3) Uani 1 1 d . . .
H1 H 0.2517(13) 0.0034(11) 0.0404(9) 0.015(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
C2 O2 1.138(2) . ?
C2 Ni1 1.7848(16) . ?
C1 O1 1.186(2) . ?
C1 C3 1.543(2) . ?
C1 Ni1 1.9518(15) . ?
C3 C4 1.506(2) . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C4 C9 1.380(2) . ?
C4 C5 1.387(2) . ?
C9 C8 1.390(2) . ?
C9 H9 0.9300 . ?
C8 C7 1.384(3) . ?
C8 H8 0.9300 . ?
C7 C6 1.373(3) . ?
C7 H7 0.9300 . ?
C6 C5 1.382(3) . ?
C6 H6 0.9300 . ?
C5 H5 0.9300 . ?
C10 C11 1.495(2) . ?
C10 H10A 0.9600 . ?
C10 H10B 0.9600 . ?
C10 H10C 0.9600 . ?
C11 N2 1.3548(19) . ?
C11 C12 1.385(2) . ?
C12 C13 1.400(2) . ?
C12 H12 0.9300 . ?
C13 N1 1.347(2) . ?
C13 C14 1.477(2) . ?
C14 C19 1.393(2) . ?
C14 C15 1.398(2) . ?
C15 C16 1.385(2) . ?
C15 H15 0.9300 . ?
C16 C17 1.387(3) . ?
C16 H16 0.9300 . ?
C17 C18 1.384(3) . ?
C17 H17 0.9300 . ?
C18 C19 1.389(2) . ?
C18 H18 0.9300 . ?
C19 H19 0.9300 . ?
C20 C21 1.496(2) . ?
C20 H20A 0.9600 . ?
C20 H20B 0.9600 . ?
C20 H20C 0.9600 . ?
C21 N4 1.3549(19) . ?
C21 C22 1.384(2) . ?
C22 C23 1.403(2) . ?
C22 H22 0.9300 . ?
C23 N3 1.3382(19) . ?
C23 C24 1.483(2) . ?
C24 C25 1.393(2) . ?
C24 C29 1.391(2) . ?
C25 C26 1.389(2) . ?
C25 H25 0.9300 . ?
C26 C27 1.384(3) . ?
C26 H26 0.9300 . ?
C27 C28 1.382(3) . ?
C27 H27 0.9300 . ?
C28 C29 1.393(2) . ?
C28 H28 0.9300 . ?
C29 H29 0.9300 . ?
C30 C31 1.496(2) . ?
C30 H30A 0.9600 . ?
C30 H30B 0.9600 . ?
C30 H30C 0.9600 . ?
C31 N6 1.353(2) . ?
C31 C32 1.375(2) . ?
C32 C33 1.403(2) . ?
C32 H32 0.9300 . ?
C33 N5 1.3411(19) . ?
C33 C34 1.475(2) . ?
C34 C39 1.395(2) . ?
C34 C35 1.396(2) . ?
C35 C36 1.387(2) . ?
C35 H35 0.9300 . ?
C36 C37 1.388(2) . ?
C36 H36 0.9300 . ?
C37 C38 1.384(2) . ?
C37 H37 0.9300 . ?
C38 C39 1.388(2) . ?
C38 H38 0.9300 . ?
C39 H39 0.9300 . ?
N2 N1 1.3719(17) . ?
N2 B1 1.546(2) . ?
N1 Ni1 2.0806(13) . ?
N4 N3 1.3738(18) . ?
N4 B1 1.548(2) . ?
N3 Ni1 2.0461(13) . ?
N6 N5 1.3715(17) . ?
N6 B1 1.549(2) . ?
N5 Ni1 2.0073(12) . ?
B1 H1 1.086(17) . ?

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
O2 C2 Ni1 175.86(14) . . ?
O1 C1 C3 121.86(14) . . ?
O1 C1 Ni1 125.00(12) . . ?
C3 C1 Ni1 113.13(10) . . ?
C4 C3 C1 116.07(13) . . ?
C4 C3 H3A 108.3 . . ?
C1 C3 H3A 108.3 . . ?
C4 C3 H3B 108.3 . . ?
C1 C3 H3B 108.3 . . ?
H3A C3 H3B 107.4 . . ?
C9 C4 C5 118.69(15) . . ?
C9 C4 C3 120.20(14) . . ?
C5 C4 C3 120.92(15) . . ?
C4 C9 C8 120.91(17) . . ?
C4 C9 H9 119.5 . . ?
C8 C9 H9 119.5 . . ?
C7 C8 C9 119.67(18) . . ?
C7 C8 H8 120.2 . . ?
C9 C8 H8 120.2 . . ?
C6 C7 C8 119.72(17) . . ?
C6 C7 H7 120.1 . . ?
C8 C7 H7 120.1 . . ?
C7 C6 C5 120.47(19) . . ?
C7 C6 H6 119.8 . . ?
C5 C6 H6 119.8 . . ?
C4 C5 C6 120.53(18) . . ?
C4 C5 H5 119.7 . . ?
C6 C5 H5 119.7 . . ?
C11 C10 H10A 109.5 . . ?
C11 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C11 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
N2 C11 C12 107.25(13) . . ?
N2 C11 C10 122.29(14) . . ?
C12 C11 C10 130.42(14) . . ?
C11 C12 C13 106.14(13) . . ?
C11 C12 H12 126.9 . . ?
C13 C12 H12 126.9 . . ?
N1 C13 C12 109.73(13) . . ?
N1 C13 C14 120.21(14) . . ?
C12 C13 C14 130.04(14) . . ?
C19 C14 C15 118.70(15) . . ?
C19 C14 C13 120.72(14) . . ?
C15 C14 C13 120.57(14) . . ?
C16 C15 C14 120.53(15) . . ?
C16 C15 H15 119.7 . . ?
C14 C15 H15 119.7 . . ?
C17 C16 C15 120.24(16) . . ?
C17 C16 H16 119.9 . . ?
C15 C16 H16 119.9 . . ?
C18 C17 C16 119.74(16) . . ?
C18 C17 H17 120.1 . . ?
C16 C17 H17 120.1 . . ?
C17 C18 C19 120.23(16) . . ?
C17 C18 H18 119.9 . . ?
C19 C18 H18 119.9 . . ?
C18 C19 C14 120.55(16) . . ?
C18 C19 H19 119.7 . . ?
C14 C19 H19 119.7 . . ?
C21 C20 H20A 109.5 . . ?
C21 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
C21 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
N4 C21 C22 107.51(13) . . ?
N4 C21 C20 122.24(14) . . ?
C22 C21 C20 130.16(14) . . ?
C21 C22 C23 105.85(13) . . ?
C21 C22 H22 127.1 . . ?
C23 C22 H22 127.1 . . ?
N3 C23 C22 109.86(13) . . ?
N3 C23 C24 120.09(13) . . ?
C22 C23 C24 130.04(14) . . ?
C25 C24 C29 118.79(15) . . ?
C25 C24 C23 120.08(14) . . ?
C29 C24 C23 121.12(14) . . ?
C26 C25 C24 120.42(16) . . ?
C26 C25 H25 119.8 . . ?
C24 C25 H25 119.8 . . ?
C27 C26 C25 120.35(17) . . ?
C27 C26 H26 119.8 . . ?
C25 C26 H26 119.8 . . ?
C28 C27 C26 119.76(16) . . ?
C28 C27 H27 120.1 . . ?
C26 C27 H27 120.1 . . ?
C27 C28 C29 120.08(17) . . ?
C27 C28 H28 120.0 . . ?
C29 C28 H28 120.0 . . ?
C28 C29 C24 120.61(16) . . ?
C28 C29 H29 119.7 . . ?
C24 C29 H29 119.7 . . ?
C31 C30 H30A 109.5 . . ?
C31 C30 H30B 109.5 . . ?
H30A C30 H30B 109.5 . . ?
C31 C30 H30C 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
N6 C31 C32 107.44(13) . . ?
N6 C31 C30 123.27(14) . . ?
C32 C31 C30 129.27(14) . . ?
C31 C32 C33 106.39(13) . . ?
C31 C32 H32 126.8 . . ?
C33 C32 H32 126.8 . . ?
N5 C33 C32 109.22(13) . . ?
N5 C33 C34 123.19(13) . . ?
C32 C33 C34 127.50(14) . . ?
C39 C34 C35 118.51(15) . . ?
C39 C34 C33 119.45(14) . . ?
C35 C34 C33 121.89(14) . . ?
C36 C35 C34 120.75(15) . . ?
C36 C35 H35 119.6 . . ?
C34 C35 H35 119.6 . . ?
C35 C36 C37 120.18(15) . . ?
C35 C36 H36 119.9 . . ?
C37 C36 H36 119.9 . . ?
C38 C37 C36 119.53(16) . . ?
C38 C37 H37 120.2 . . ?
C36 C37 H37 120.2 . . ?
C37 C38 C39 120.47(16) . . ?
C37 C38 H38 119.8 . . ?
C39 C38 H38 119.8 . . ?
C38 C39 C34 120.54(15) . . ?
C38 C39 H39 119.7 . . ?
C34 C39 H39 119.7 . . ?
C11 N2 N1 110.52(12) . . ?
C11 N2 B1 131.75(13) . . ?
N1 N2 B1 117.48(12) . . ?
C13 N1 N2 106.33(12) . . ?
C13 N1 Ni1 134.46(10) . . ?
N2 N1 Ni1 111.55(9) . . ?
C21 N4 N3 110.08(12) . . ?
C21 N4 B1 130.12(13) . . ?
N3 N4 B1 119.72(12) . . ?
C23 N3 N4 106.66(12) . . ?
C23 N3 Ni1 138.20(11) . . ?
N4 N3 Ni1 113.92(9) . . ?
C31 N6 N5 110.15(12) . . ?
C31 N6 B1 130.70(13) . . ?
N5 N6 B1 119.07(12) . . ?
C33 N5 N6 106.78(12) . . ?
C33 N5 Ni1 136.95(11) . . ?
N6 N5 Ni1 115.91(9) . . ?
C2 Ni1 C1 88.28(7) . . ?
C2 Ni1 N5 135.72(6) . . ?
C1 Ni1 N5 91.25(6) . . ?
C2 Ni1 N3 101.73(6) . . ?
C1 Ni1 N3 169.77(6) . . ?
N5 Ni1 N3 83.09(5) . . ?
C2 Ni1 N1 122.95(6) . . ?
C1 Ni1 N1 88.16(6) . . ?
N5 Ni1 N1 101.27(5) . . ?
N3 Ni1 N1 84.62(5) . . ?
N2 B1 N6 109.99(12) . . ?
N2 B1 N4 107.43(12) . . ?
N6 B1 N4 106.98(12) . . ?
N2 B1 H1 110.6(9) . . ?
N6 B1 H1 110.2(9) . . ?
N4 B1 H1 111.4(9) . . ?

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 1.000
_refine_diff_density_max         0.274
_refine_diff_density_min         -0.348
_refine_diff_density_rms         0.042
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent'
_solvent_exptl_crystal_recrystallization_method 'diethyl ether'
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_Complex_8b
_database_code_depnum_ccdc_archive 'CCDC 1476056'
_audit_update_record             
;
2016-05-13 deposited with the CCDC.
2016-06-21 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        'Complex 8b'
_chemical_name_common            'Complex 8b'
_chemical_melting_point          388.2-389.2
_chemical_formula_moiety         'C36 H39 B N6 Ni O2 Si'
_chemical_formula_sum            'C36 H39 B N6 Ni O2 Si'
_chemical_formula_weight         685.34

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'
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 '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'
B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   P2(1)/c

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

_cell_length_a                   11.1566(6)
_cell_length_b                   12.4011(7)
_cell_length_c                   25.4222(12)
_cell_angle_alpha                90.00
_cell_angle_beta                 100.042(4)
_cell_angle_gamma                90.00
_cell_volume                     3463.4(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    8481
_cell_measurement_theta_min      2.24
_cell_measurement_theta_max      25.47

_exptl_crystal_description       needle
_exptl_crystal_colour            orange
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.06
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.314
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1440
_exptl_absorpt_coefficient_mu    0.636
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.7520
_exptl_absorpt_correction_T_max  0.8204
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean 8.366
_diffrn_reflns_number            19381
_diffrn_reflns_av_R_equivalents  0.0395
_diffrn_reflns_av_sigmaI/netI    0.0517
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_theta_min         1.83
_diffrn_reflns_theta_max         25.54
_reflns_number_total             6447
_reflns_number_gt                4910
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker APEX2 v.2011.4'
_computing_cell_refinement       'Bruker APEX2 v.2011.4'
_computing_data_reduction        'Bruker APEX2 v.2011.4'
_computing_structure_solution    SIR-92
_computing_structure_refinement  SHELXL-97
_computing_molecular_graphics    ORTEP-32
_computing_publication_material  WinGX

_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)+(0.0613P)²+7.7419P] 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         6447
_refine_ls_number_parameters     434
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0672
_refine_ls_R_factor_gt           0.0452
_refine_ls_wR_factor_ref         0.1229
_refine_ls_wR_factor_gt          0.1103
_refine_ls_goodness_of_fit_ref   0.879
_refine_ls_restrained_S_all      0.879
_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
C1 C 0.2724(3) 0.2437(3) 0.86435(12) 0.0207(7) Uani 1 1 d . . .
C3 C 0.1982(3) 0.2171(3) 0.81023(12) 0.0219(7) Uani 1 1 d . . .
H3A H 0.1236 0.2591 0.8053 0.026 Uiso 1 1 calc R . .
H3B H 0.1758 0.1415 0.8097 0.026 Uiso 1 1 calc R . .
C4 C 0.3566(3) 0.3791(3) 0.76064(14) 0.0301(8) Uani 1 1 d . . .
H4A H 0.3871 0.3972 0.7287 0.045 Uiso 1 1 calc R . .
H4B H 0.4228 0.3767 0.7903 0.045 Uiso 1 1 calc R . .
H4C H 0.2989 0.4327 0.7672 0.045 Uiso 1 1 calc R . .
C5 C 0.3945(3) 0.1355(3) 0.74934(15) 0.0331(8) Uani 1 1 d . . .
H5A H 0.4429 0.1531 0.7228 0.050 Uiso 1 1 calc R . .
H5B H 0.3528 0.0686 0.7402 0.050 Uiso 1 1 calc R . .
H5C H 0.4463 0.1287 0.7835 0.050 Uiso 1 1 calc R . .
C6 C 0.1631(3) 0.2432(3) 0.69023(14) 0.0358(9) Uani 1 1 d . . .
H6A H 0.1104 0.3044 0.6901 0.054 Uiso 1 1 calc R . .
H6B H 0.1161 0.1782 0.6891 0.054 Uiso 1 1 calc R . .
H6C H 0.2024 0.2462 0.6595 0.054 Uiso 1 1 calc R . .
C2 C 0.2795(3) 0.3727(3) 0.93970(12) 0.0233(7) Uani 1 1 d . . .
C7 C -0.2150(3) 0.2969(3) 1.01847(13) 0.0277(8) Uani 1 1 d . . .
H7A H -0.2608 0.3300 0.9872 0.042 Uiso 1 1 calc R . .
H7B H -0.2324 0.3326 1.0498 0.042 Uiso 1 1 calc R . .
H7C H -0.2371 0.2222 1.0195 0.042 Uiso 1 1 calc R . .
C8 C -0.0822(3) 0.3058(3) 1.01686(12) 0.0201(7) Uani 1 1 d . . .
C9 C 0.0097(3) 0.3541(3) 1.05245(12) 0.0229(7) Uani 1 1 d . . .
H9 H 0.0019 0.3901 1.0838 0.028 Uiso 1 1 calc R . .
C10 C 0.1169(3) 0.3382(2) 1.03190(12) 0.0184(6) Uani 1 1 d . . .
C11 C 0.2407(3) 0.3702(2) 1.05717(12) 0.0184(7) Uani 1 1 d . . .
C12 C 0.2585(3) 0.4667(3) 1.08520(13) 0.0246(7) Uani 1 1 d . . .
H12 H 0.1927 0.5118 1.0868 0.030 Uiso 1 1 calc R . .
C13 C 0.3736(3) 0.4960(3) 1.11068(13) 0.0288(8) Uani 1 1 d . . .
H13 H 0.3848 0.5604 1.1297 0.035 Uiso 1 1 calc R . .
C14 C 0.4713(3) 0.4303(3) 1.10802(14) 0.0291(8) Uani 1 1 d . . .
H14 H 0.5486 0.4510 1.1248 0.035 Uiso 1 1 calc R . .
C15 C 0.4560(3) 0.3344(3) 1.08087(13) 0.0261(7) Uani 1 1 d . . .
H15 H 0.5228 0.2904 1.0792 0.031 Uiso 1 1 calc R . .
C16 C 0.3405(3) 0.3031(3) 1.05588(12) 0.0219(7) Uani 1 1 d . . .
H16 H 0.3297 0.2372 1.0382 0.026 Uiso 1 1 calc R . .
C17 C -0.3173(3) 0.2349(3) 0.83705(13) 0.0244(7) Uani 1 1 d . . .
H17A H -0.3059 0.1593 0.8317 0.037 Uiso 1 1 calc R . .
H17B H -0.3746 0.2632 0.8077 0.037 Uiso 1 1 calc R . .
H17C H -0.3479 0.2456 0.8697 0.037 Uiso 1 1 calc R . .
C18 C -0.1979(3) 0.2924(2) 0.84028(12) 0.0180(6) Uani 1 1 d . . .
C19 C -0.1637(3) 0.3700(2) 0.80719(12) 0.0192(7) Uani 1 1 d . . .
H19 H -0.2114 0.4002 0.7772 0.023 Uiso 1 1 calc R . .
C20 C -0.0419(3) 0.3941(2) 0.82811(11) 0.0172(6) Uani 1 1 d . . .
C21 C 0.0369(3) 0.4748(2) 0.80912(12) 0.0183(6) Uani 1 1 d . . .
C22 C 0.0204(3) 0.5032(3) 0.75506(13) 0.0238(7) Uani 1 1 d . . .
H22 H -0.0376 0.4673 0.7306 0.029 Uiso 1 1 calc R . .
C23 C 0.0897(3) 0.5844(3) 0.73760(13) 0.0273(8) Uani 1 1 d . . .
H23 H 0.0777 0.6026 0.7016 0.033 Uiso 1 1 calc R . .
C24 C 0.1763(3) 0.6381(3) 0.77350(13) 0.0260(8) Uani 1 1 d . . .
H24 H 0.2222 0.6930 0.7619 0.031 Uiso 1 1 calc R . .
C25 C 0.1945(3) 0.6095(3) 0.82714(13) 0.0236(7) Uani 1 1 d . . .
H25 H 0.2531 0.6450 0.8515 0.028 Uiso 1 1 calc R . .
C26 C 0.1255(3) 0.5283(2) 0.84432(12) 0.0194(7) Uani 1 1 d . . .
H26 H 0.1390 0.5093 0.8803 0.023 Uiso 1 1 calc R . .
C27 C -0.1544(3) -0.0461(3) 0.92940(14) 0.0277(8) Uani 1 1 d . . .
H27A H -0.1647 -0.0279 0.9650 0.042 Uiso 1 1 calc R . .
H27B H -0.1570 -0.1231 0.9252 0.042 Uiso 1 1 calc R . .
H27C H -0.2186 -0.0140 0.9042 0.042 Uiso 1 1 calc R . .
C28 C -0.0347(3) -0.0049(3) 0.91975(12) 0.0197(7) Uani 1 1 d . . .
C29 C 0.0650(3) -0.0602(3) 0.90939(12) 0.0221(7) Uani 1 1 d . . .
H29 H 0.0712 -0.1344 0.9052 0.027 Uiso 1 1 calc R . .
C30 C 0.1548(3) 0.0156(2) 0.90641(12) 0.0180(6) Uani 1 1 d . . .
C31 C 0.2790(3) -0.0084(3) 0.89690(12) 0.0198(7) Uani 1 1 d . . .
C32 C 0.2923(3) -0.0820(3) 0.85666(13) 0.0229(7) Uani 1 1 d . . .
H32 H 0.2236 -0.1134 0.8364 0.028 Uiso 1 1 calc R . .
C33 C 0.4067(3) -0.1086(3) 0.84669(14) 0.0283(8) Uani 1 1 d . . .
H33 H 0.4147 -0.1566 0.8194 0.034 Uiso 1 1 calc R . .
C34 C 0.5096(3) -0.0634(3) 0.87754(14) 0.0299(8) Uani 1 1 d . . .
H34 H 0.5867 -0.0812 0.8710 0.036 Uiso 1 1 calc R . .
C35 C 0.4969(3) 0.0082(3) 0.91791(14) 0.0314(8) Uani 1 1 d . . .
H35 H 0.5657 0.0383 0.9386 0.038 Uiso 1 1 calc R . .
C36 C 0.3825(3) 0.0354(3) 0.92781(14) 0.0269(8) Uani 1 1 d . . .
H36 H 0.3750 0.0831 0.9553 0.032 Uiso 1 1 calc R . .
N2 N -0.0309(2) 0.2629(2) 0.97743(10) 0.0171(5) Uani 1 1 d . . .
N1 N 0.0916(2) 0.2838(2) 0.98579(10) 0.0171(5) Uani 1 1 d . . .
N4 N -0.1009(2) 0.2719(2) 0.87883(10) 0.0168(5) Uani 1 1 d . . .
N3 N -0.0035(2) 0.3341(2) 0.87185(10) 0.0174(5) Uani 1 1 d . . .
N6 N -0.0057(2) 0.1014(2) 0.92166(10) 0.0174(5) Uani 1 1 d . . .
N5 N 0.1130(2) 0.1149(2) 0.91382(10) 0.0175(5) Uani 1 1 d . . .
O1 O 0.3813(2) 0.2483(2) 0.87201(9) 0.0304(6) Uani 1 1 d . . .
O2 O 0.3457(2) 0.4433(2) 0.95006(9) 0.0336(6) Uani 1 1 d . . .
Ni1 Ni 0.17753(3) 0.26503(3) 0.921144(15) 0.01815(12) Uani 1 1 d . . .
Si1 Si 0.28067(8) 0.24493(7) 0.75233(3) 0.0218(2) Uani 1 1 d . . .
B1 B -0.0887(3) 0.1982(3) 0.92822(14) 0.0182(7) Uani 1 1 d . . .
H1 H -0.181(3) 0.168(2) 0.9320(12) 0.017(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
C1 O1 1.198(4) . ?
C1 C3 1.513(4) . ?
C1 Ni1 1.951(3) . ?
C3 Si1 1.899(3) . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C4 Si1 1.863(3) . ?
C4 H4A 0.9600 . ?
C4 H4B 0.9600 . ?
C4 H4C 0.9600 . ?
C5 Si1 1.869(4) . ?
C5 H5A 0.9600 . ?
C5 H5B 0.9600 . ?
C5 H5C 0.9600 . ?
C6 Si1 1.869(3) . ?
C6 H6A 0.9600 . ?
C6 H6B 0.9600 . ?
C6 H6C 0.9600 . ?
C2 O2 1.146(4) . ?
C2 Ni1 1.764(3) . ?
C7 C8 1.493(4) . ?
C7 H7A 0.9600 . ?
C7 H7B 0.9600 . ?
C7 H7C 0.9600 . ?
C8 N2 1.348(4) . ?
C8 C9 1.381(4) . ?
C9 C10 1.401(4) . ?
C9 H9 0.9300 . ?
C10 N1 1.339(4) . ?
C10 C11 1.472(4) . ?
C11 C12 1.389(4) . ?
C11 C16 1.395(4) . ?
C12 C13 1.382(5) . ?
C12 H12 0.9300 . ?
C13 C14 1.372(5) . ?
C13 H13 0.9300 . ?
C14 C15 1.370(5) . ?
C14 H14 0.9300 . ?
C15 C16 1.389(4) . ?
C15 H15 0.9300 . ?
C16 H16 0.9300 . ?
C17 C18 1.500(4) . ?
C17 H17A 0.9600 . ?
C17 H17B 0.9600 . ?
C17 H17C 0.9600 . ?
C18 N4 1.351(4) . ?
C18 C19 1.375(4) . ?
C19 C20 1.403(4) . ?
C19 H19 0.9300 . ?
C20 N3 1.344(4) . ?
C20 C21 1.468(4) . ?
C21 C26 1.381(4) . ?
C21 C22 1.399(4) . ?
C22 C23 1.388(5) . ?
C22 H22 0.9300 . ?
C23 C24 1.380(5) . ?
C23 H23 0.9300 . ?
C24 C25 1.389(5) . ?
C24 H24 0.9300 . ?
C25 C26 1.384(4) . ?
C25 H25 0.9300 . ?
C26 H26 0.9300 . ?
C27 C28 1.490(4) . ?
C27 H27A 0.9600 . ?
C27 H27B 0.9600 . ?
C27 H27C 0.9600 . ?
C28 N6 1.356(4) . ?
C28 C29 1.371(4) . ?
C29 C30 1.386(4) . ?
C29 H29 0.9300 . ?
C30 N5 1.341(4) . ?
C30 C31 1.477(4) . ?
C31 C36 1.389(4) . ?
C31 C32 1.398(4) . ?
C32 C33 1.384(4) . ?
C32 H32 0.9300 . ?
C33 C34 1.391(5) . ?
C33 H33 0.9300 . ?
C34 C35 1.383(5) . ?
C34 H34 0.9300 . ?
C35 C36 1.385(5) . ?
C35 H35 0.9300 . ?
C36 H36 0.9300 . ?
N2 N1 1.371(3) . ?
N2 B1 1.530(4) . ?
N1 Ni1 2.055(2) . ?
N4 N3 1.369(3) . ?
N4 B1 1.540(4) . ?
N3 Ni1 2.346(2) . ?
N6 N5 1.383(3) . ?
N6 B1 1.544(4) . ?
N5 Ni1 1.993(3) . ?
B1 H1 1.12(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
O1 C1 C3 122.5(3) . . ?
O1 C1 Ni1 122.6(2) . . ?
C3 C1 Ni1 114.9(2) . . ?
C1 C3 Si1 113.8(2) . . ?
C1 C3 H3A 108.8 . . ?
Si1 C3 H3A 108.8 . . ?
C1 C3 H3B 108.8 . . ?
Si1 C3 H3B 108.8 . . ?
H3A C3 H3B 107.7 . . ?
Si1 C4 H4A 109.5 . . ?
Si1 C4 H4B 109.5 . . ?
H4A C4 H4B 109.5 . . ?
Si1 C4 H4C 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
Si1 C5 H5A 109.5 . . ?
Si1 C5 H5B 109.5 . . ?
H5A C5 H5B 109.5 . . ?
Si1 C5 H5C 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
Si1 C6 H6A 109.5 . . ?
Si1 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
Si1 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
O2 C2 Ni1 177.8(3) . . ?
C8 C7 H7A 109.5 . . ?
C8 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
C8 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
N2 C8 C9 107.2(3) . . ?
N2 C8 C7 122.9(3) . . ?
C9 C8 C7 129.9(3) . . ?
C8 C9 C10 106.2(3) . . ?
C8 C9 H9 126.9 . . ?
C10 C9 H9 126.9 . . ?
N1 C10 C9 109.5(3) . . ?
N1 C10 C11 123.8(3) . . ?
C9 C10 C11 126.6(3) . . ?
C12 C11 C16 118.8(3) . . ?
C12 C11 C10 119.7(3) . . ?
C16 C11 C10 121.4(3) . . ?
C13 C12 C11 120.4(3) . . ?
C13 C12 H12 119.8 . . ?
C11 C12 H12 119.8 . . ?
C14 C13 C12 120.1(3) . . ?
C14 C13 H13 120.0 . . ?
C12 C13 H13 120.0 . . ?
C15 C14 C13 120.7(3) . . ?
C15 C14 H14 119.7 . . ?
C13 C14 H14 119.7 . . ?
C14 C15 C16 119.8(3) . . ?
C14 C15 H15 120.1 . . ?
C16 C15 H15 120.1 . . ?
C11 C16 C15 120.2(3) . . ?
C11 C16 H16 119.9 . . ?
C15 C16 H16 119.9 . . ?
C18 C17 H17A 109.5 . . ?
C18 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
C18 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
N4 C18 C19 107.6(3) . . ?
N4 C18 C17 122.8(3) . . ?
C19 C18 C17 129.6(3) . . ?
C18 C19 C20 105.7(3) . . ?
C18 C19 H19 127.1 . . ?
C20 C19 H19 127.1 . . ?
N3 C20 C19 110.1(3) . . ?
N3 C20 C21 121.8(3) . . ?
C19 C20 C21 128.1(3) . . ?
C26 C21 C22 118.2(3) . . ?
C26 C21 C20 121.1(3) . . ?
C22 C21 C20 120.7(3) . . ?
C23 C22 C21 120.7(3) . . ?
C23 C22 H22 119.6 . . ?
C21 C22 H22 119.6 . . ?
C24 C23 C22 120.2(3) . . ?
C24 C23 H23 119.9 . . ?
C22 C23 H23 119.9 . . ?
C23 C24 C25 119.4(3) . . ?
C23 C24 H24 120.3 . . ?
C25 C24 H24 120.3 . . ?
C26 C25 C24 120.1(3) . . ?
C26 C25 H25 119.9 . . ?
C24 C25 H25 119.9 . . ?
C25 C26 C21 121.3(3) . . ?
C25 C26 H26 119.4 . . ?
C21 C26 H26 119.4 . . ?
C28 C27 H27A 109.5 . . ?
C28 C27 H27B 109.5 . . ?
H27A C27 H27B 109.5 . . ?
C28 C27 H27C 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
N6 C28 C29 107.2(3) . . ?
N6 C28 C27 122.9(3) . . ?
C29 C28 C27 129.8(3) . . ?
C28 C29 C30 106.8(3) . . ?
C28 C29 H29 126.6 . . ?
C30 C29 H29 126.6 . . ?
N5 C30 C29 110.0(3) . . ?
N5 C30 C31 124.5(3) . . ?
C29 C30 C31 125.4(3) . . ?
C36 C31 C32 119.0(3) . . ?
C36 C31 C30 122.7(3) . . ?
C32 C31 C30 118.2(3) . . ?
C33 C32 C31 120.6(3) . . ?
C33 C32 H32 119.7 . . ?
C31 C32 H32 119.7 . . ?
C34 C33 C32 119.9(3) . . ?
C34 C33 H33 120.1 . . ?
C32 C33 H33 120.1 . . ?
C33 C34 C35 119.7(3) . . ?
C33 C34 H34 120.1 . . ?
C35 C34 H34 120.1 . . ?
C36 C35 C34 120.6(3) . . ?
C36 C35 H35 119.7 . . ?
C34 C35 H35 119.7 . . ?
C35 C36 C31 120.3(3) . . ?
C35 C36 H36 119.9 . . ?
C31 C36 H36 119.9 . . ?
C8 N2 N1 110.6(2) . . ?
C8 N2 B1 129.9(2) . . ?
N1 N2 B1 119.5(2) . . ?
C10 N1 N2 106.5(2) . . ?
C10 N1 Ni1 134.4(2) . . ?
N2 N1 Ni1 116.48(18) . . ?
C18 N4 N3 110.7(2) . . ?
C18 N4 B1 130.4(3) . . ?
N3 N4 B1 118.7(2) . . ?
C20 N3 N4 105.9(2) . . ?
C20 N3 Ni1 139.82(19) . . ?
N4 N3 Ni1 110.75(17) . . ?
C28 N6 N5 110.0(2) . . ?
C28 N6 B1 128.0(2) . . ?
N5 N6 B1 122.0(2) . . ?
C30 N5 N6 105.9(2) . . ?
C30 N5 Ni1 137.9(2) . . ?
N6 N5 Ni1 116.03(18) . . ?
C2 Ni1 C1 83.85(14) . . ?
C2 Ni1 N5 159.62(13) . . ?
C1 Ni1 N5 92.16(12) . . ?
C2 Ni1 N1 93.99(12) . . ?
C1 Ni1 N1 174.79(12) . . ?
N5 Ni1 N1 88.23(10) . . ?
C2 Ni1 N3 108.79(12) . . ?
C1 Ni1 N3 100.48(11) . . ?
N5 Ni1 N3 91.59(9) . . ?
N1 Ni1 N3 84.70(9) . . ?
C4 Si1 C6 110.14(17) . . ?
C4 Si1 C5 110.76(16) . . ?
C6 Si1 C5 109.84(17) . . ?
C4 Si1 C3 110.28(15) . . ?
C6 Si1 C3 106.79(15) . . ?
C5 Si1 C3 108.94(16) . . ?
N2 B1 N4 108.7(3) . . ?
N2 B1 N6 108.7(2) . . ?
N4 B1 N6 110.0(2) . . ?
N2 B1 H1 111.8(16) . . ?
N4 B1 H1 108.5(16) . . ?
N6 B1 H1 109.1(16) . . ?

_diffrn_measured_fraction_theta_max 0.995
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         0.509
_refine_diff_density_min         -0.424
_refine_diff_density_rms         0.066
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent'
_solvent_exptl_crystal_recrystallization_method 'diethyl ether'
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_Complex_2a
_database_code_depnum_ccdc_archive 'CCDC 1476057'
_audit_update_record             
;
2016-05-13 deposited with the CCDC.
2016-06-21 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        'Complex 2a'
_chemical_name_common            'Complex 2a'
_chemical_melting_point          '428.2 - 429.1'
_chemical_formula_moiety         'C38 H35 B N6 Ni S2'
_chemical_formula_sum            'C38 H35 B N6 Ni S2'
_chemical_formula_weight         709.36

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Triclinic
_symmetry_space_group_name_H-M   P-1

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

_cell_length_a                   10.501(2)
_cell_length_b                   10.927(3)
_cell_length_c                   16.316(2)
_cell_angle_alpha                85.952(3)
_cell_angle_beta                 89.580(3)
_cell_angle_gamma                62.404(3)
_cell_volume                     1654.2(9)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9406
_cell_measurement_theta_min      2.19
_cell_measurement_theta_max      25.39

_exptl_crystal_description       rod
_exptl_crystal_colour            red
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.13
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.424
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             740
_exptl_absorpt_coefficient_mu    0.752
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.9520
_exptl_absorpt_correction_T_max  0.9804
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean 8.366
_diffrn_reflns_number            56120
_diffrn_reflns_av_R_equivalents  0.0262
_diffrn_reflns_av_sigmaI/netI    0.0137
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         2.11
_diffrn_reflns_theta_max         25.40
_reflns_number_total             6093
_reflns_number_gt                5618
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker APEX2 v.2011.4'
_computing_cell_refinement       'Bruker APEX2 v.2011.4'
_computing_data_reduction        'Bruker APEX2 v.2011.4'
_computing_structure_solution    SIR-92
_computing_structure_refinement  SHELXL-97
_computing_molecular_graphics    ORTEP-32
_computing_publication_material  WinGX

_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)+(0.0316P)²+1.2332P] 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         6093
_refine_ls_number_parameters     440
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0295
_refine_ls_R_factor_gt           0.0265
_refine_ls_wR_factor_ref         0.0681
_refine_ls_wR_factor_gt          0.0656
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_restrained_S_all      1.044
_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
C1 C 0.08131(17) 1.04635(16) 0.22417(10) 0.0171(3) Uani 1 1 d . . .
C2 C 0.03878(18) 1.27789(17) 0.12370(10) 0.0191(3) Uani 1 1 d . . .
H2A H 0.0801 1.2176 0.0795 0.023 Uiso 1 1 calc R . .
H2B H -0.0644 1.3110 0.1220 0.023 Uiso 1 1 calc R . .
C3 C 0.07149(17) 1.39858(16) 0.11338(9) 0.0171(3) Uani 1 1 d . . .
C4 C -0.03982(18) 1.53329(17) 0.10636(10) 0.0191(3) Uani 1 1 d . . .
H4 H -0.1347 1.5488 0.1073 0.023 Uiso 1 1 calc R . .
C5 C -0.01056(19) 1.64476(17) 0.09789(10) 0.0218(4) Uani 1 1 d . . .
H5 H -0.0859 1.7345 0.0927 0.026 Uiso 1 1 calc R . .
C6 C 0.13018(19) 1.62340(18) 0.09703(10) 0.0228(4) Uani 1 1 d . . .
H6 H 0.1497 1.6983 0.0920 0.027 Uiso 1 1 calc R . .
C7 C 0.24171(19) 1.48911(18) 0.10375(11) 0.0231(4) Uani 1 1 d . . .
H7 H 0.3365 1.4740 0.1031 0.028 Uiso 1 1 calc R . .
C8 C 0.21276(18) 1.37729(17) 0.11142(10) 0.0203(3) Uani 1 1 d . . .
H8 H 0.2882 1.2876 0.1153 0.024 Uiso 1 1 calc R . .
C9 C 0.00469(17) 0.67320(16) 0.30432(9) 0.0155(3) Uani 1 1 d . . .
C10 C 0.06703(17) 0.52835(16) 0.31476(9) 0.0169(3) Uani 1 1 d . . .
H10 H 0.0195 0.4745 0.3168 0.020 Uiso 1 1 calc R . .
C11 C 0.21335(17) 0.48205(16) 0.32131(9) 0.0162(3) Uani 1 1 d . . .
C12 C 0.33250(18) 0.33668(16) 0.32711(10) 0.0196(3) Uani 1 1 d . . .
H12A H 0.3843 0.3192 0.2769 0.029 Uiso 1 1 calc R . .
H12B H 0.2931 0.2734 0.3359 0.029 Uiso 1 1 calc R . .
H12C H 0.3966 0.3241 0.3722 0.029 Uiso 1 1 calc R . .
C13 C -0.14914(17) 0.77255(16) 0.29840(9) 0.0160(3) Uani 1 1 d . . .
C14 C -0.24920(18) 0.73118(17) 0.27281(10) 0.0187(3) Uani 1 1 d . . .
H14 H -0.2173 0.6416 0.2572 0.022 Uiso 1 1 calc R . .
C15 C -0.39521(18) 0.82176(18) 0.27044(10) 0.0216(4) Uani 1 1 d . . .
H15 H -0.4603 0.7926 0.2534 0.026 Uiso 1 1 calc R . .
C16 C -0.44459(18) 0.95559(18) 0.29339(10) 0.0215(3) Uani 1 1 d . . .
H16 H -0.5425 1.0165 0.2916 0.026 Uiso 1 1 calc R . .
C17 C -0.34652(18) 0.99788(17) 0.31904(10) 0.0210(3) Uani 1 1 d . . .
H17 H -0.3791 1.0878 0.3342 0.025 Uiso 1 1 calc R . .
C18 C -0.20103(17) 0.90781(17) 0.32230(10) 0.0178(3) Uani 1 1 d . . .
H18 H -0.1367 0.9372 0.3406 0.021 Uiso 1 1 calc R . .
C19 C 0.44258(17) 0.69494(16) 0.11835(10) 0.0165(3) Uani 1 1 d . . .
C20 C 0.56411(17) 0.56367(17) 0.12532(10) 0.0189(3) Uani 1 1 d . . .
H20 H 0.6312 0.5226 0.0853 0.023 Uiso 1 1 calc R . .
C21 C 0.56289(17) 0.50881(16) 0.20375(10) 0.0181(3) Uani 1 1 d . . .
C22 C 0.67047(18) 0.37517(17) 0.24675(11) 0.0241(4) Uani 1 1 d . . .
H22A H 0.7271 0.3933 0.2854 0.036 Uiso 1 1 calc R . .
H22B H 0.7322 0.3159 0.2071 0.036 Uiso 1 1 calc R . .
H22C H 0.6212 0.3306 0.2754 0.036 Uiso 1 1 calc R . .
C23 C 0.39994(16) 0.79982(17) 0.04841(10) 0.0178(3) Uani 1 1 d . . .
C24 C 0.41102(18) 0.76039(18) -0.03198(10) 0.0227(4) Uani 1 1 d . . .
H24 H 0.4391 0.6684 -0.0410 0.027 Uiso 1 1 calc R . .
C25 C 0.38074(19) 0.8564(2) -0.09834(11) 0.0257(4) Uani 1 1 d . . .
H25 H 0.3888 0.8286 -0.1515 0.031 Uiso 1 1 calc R . .
C26 C 0.33847(18) 0.99382(19) -0.08598(11) 0.0248(4) Uani 1 1 d . . .
H26 H 0.3185 1.0583 -0.1306 0.030 Uiso 1 1 calc R . .
C27 C 0.32610(19) 1.03444(18) -0.00652(11) 0.0248(4) Uani 1 1 d . . .
H27 H 0.2976 1.1267 0.0021 0.030 Uiso 1 1 calc R . .
C28 C 0.35593(17) 0.93842(17) 0.06038(10) 0.0209(3) Uani 1 1 d . . .
H28 H 0.3464 0.9669 0.1135 0.025 Uiso 1 1 calc R . .
C29 C 0.26597(17) 0.92378(16) 0.42154(9) 0.0156(3) Uani 1 1 d . . .
C30 C 0.39849(17) 0.84516(17) 0.46340(10) 0.0175(3) Uani 1 1 d . . .
H30 H 0.4381 0.8737 0.5041 0.021 Uiso 1 1 calc R . .
C31 C 0.45797(17) 0.71724(17) 0.43212(9) 0.0166(3) Uani 1 1 d . . .
C32 C 0.60208(17) 0.59602(17) 0.45108(10) 0.0201(3) Uani 1 1 d . . .
H32A H 0.5901 0.5175 0.4716 0.030 Uiso 1 1 calc R . .
H32B H 0.6520 0.6182 0.4919 0.030 Uiso 1 1 calc R . .
H32C H 0.6568 0.5744 0.4020 0.030 Uiso 1 1 calc R . .
C33 C 0.15677(17) 1.06475(16) 0.43714(9) 0.0161(3) Uani 1 1 d . . .
C34 C 0.00977(17) 1.10620(17) 0.42818(10) 0.0185(3) Uani 1 1 d . . .
H34 H -0.0204 1.0471 0.4066 0.022 Uiso 1 1 calc R . .
C35 C -0.09131(18) 1.23430(17) 0.45113(10) 0.0211(3) Uani 1 1 d . . .
H35 H -0.1888 1.2609 0.4446 0.025 Uiso 1 1 calc R . .
C36 C -0.04764(19) 1.32303(17) 0.48383(10) 0.0216(3) Uani 1 1 d . . .
H36 H -0.1156 1.4084 0.5002 0.026 Uiso 1 1 calc R . .
C37 C 0.09754(19) 1.28399(17) 0.49205(10) 0.0220(4) Uani 1 1 d . . .
H37 H 0.1270 1.3439 0.5131 0.026 Uiso 1 1 calc R . .
C38 C 0.19914(18) 1.15596(17) 0.46903(10) 0.0191(3) Uani 1 1 d . . .
H38 H 0.2964 1.1306 0.4749 0.023 Uiso 1 1 calc R . .
B1 B 0.38332(19) 0.59542(18) 0.32455(11) 0.0161(4) Uani 1 1 d . . .
N1 N 0.10874(14) 0.71208(13) 0.30425(8) 0.0149(3) Uani 1 1 d . . .
N2 N 0.23705(14) 0.59402(13) 0.31660(8) 0.0152(3) Uani 1 1 d . . .
N5 N 0.36929(14) 0.71917(13) 0.18772(8) 0.0164(3) Uani 1 1 d . . .
N6 N 0.44417(14) 0.60369(13) 0.23999(8) 0.0157(3) Uani 1 1 d . . .
N3 N 0.24729(14) 0.84720(13) 0.36654(8) 0.0158(3) Uani 1 1 d . . .
N4 N 0.36496(14) 0.71850(13) 0.37446(8) 0.0153(3) Uani 1 1 d . . .
S1 S -0.01020(4) 0.99807(4) 0.16546(2) 0.01907(9) Uani 1 1 d . . .
S2 S 0.11586(4) 1.18197(4) 0.22335(2) 0.01880(9) Uani 1 1 d . . .
Ni1 Ni 0.11610(2) 0.88367(2) 0.277281(12) 0.01489(7) Uani 1 1 d . . .
H1 H 0.4587(19) 0.4975(18) 0.3599(11) 0.017(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
C1 S1 1.6352(16) . ?
C1 S2 1.6802(16) . ?
C1 Ni1 1.7971(16) . ?
C2 C3 1.508(2) . ?
C2 S2 1.8411(16) . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C3 C4 1.389(2) . ?
C3 C8 1.391(2) . ?
C4 C5 1.386(2) . ?
C4 H4 0.9300 . ?
C5 C6 1.385(3) . ?
C5 H5 0.9300 . ?
C6 C7 1.387(3) . ?
C6 H6 0.9300 . ?
C7 C8 1.387(2) . ?
C7 H7 0.9300 . ?
C8 H8 0.9300 . ?
C9 N1 1.343(2) . ?
C9 C10 1.402(2) . ?
C9 C13 1.470(2) . ?
C10 C11 1.379(2) . ?
C10 H10 0.9300 . ?
C11 N2 1.354(2) . ?
C11 C12 1.495(2) . ?
C12 H12A 0.9600 . ?
C12 H12B 0.9600 . ?
C12 H12C 0.9600 . ?
C13 C14 1.399(2) . ?
C13 C18 1.402(2) . ?
C14 C15 1.386(2) . ?
C14 H14 0.9300 . ?
C15 C16 1.385(2) . ?
C15 H15 0.9300 . ?
C16 C17 1.387(2) . ?
C16 H16 0.9300 . ?
C17 C18 1.381(2) . ?
C17 H17 0.9300 . ?
C18 H18 0.9300 . ?
C19 N5 1.336(2) . ?
C19 C20 1.408(2) . ?
C19 C23 1.471(2) . ?
C20 C21 1.377(2) . ?
C20 H20 0.9300 . ?
C21 N6 1.363(2) . ?
C21 C22 1.496(2) . ?
C22 H22A 0.9600 . ?
C22 H22B 0.9600 . ?
C22 H22C 0.9600 . ?
C23 C28 1.392(2) . ?
C23 C24 1.397(2) . ?
C24 C25 1.382(2) . ?
C24 H24 0.9300 . ?
C25 C26 1.384(3) . ?
C25 H25 0.9300 . ?
C26 C27 1.386(3) . ?
C26 H26 0.9300 . ?
C27 C28 1.389(2) . ?
C27 H27 0.9300 . ?
C28 H28 0.9300 . ?
C29 N3 1.343(2) . ?
C29 C30 1.402(2) . ?
C29 C33 1.472(2) . ?
C30 C31 1.375(2) . ?
C30 H30 0.9300 . ?
C31 N4 1.356(2) . ?
C31 C32 1.494(2) . ?
C32 H32A 0.9600 . ?
C32 H32B 0.9600 . ?
C32 H32C 0.9600 . ?
C33 C38 1.396(2) . ?
C33 C34 1.398(2) . ?
C34 C35 1.385(2) . ?
C34 H34 0.9300 . ?
C35 C36 1.387(2) . ?
C35 H35 0.9300 . ?
C36 C37 1.384(2) . ?
C36 H36 0.9300 . ?
C37 C38 1.386(2) . ?
C37 H37 0.9300 . ?
C38 H38 0.9300 . ?
B1 N6 1.531(2) . ?
B1 N2 1.550(2) . ?
B1 N4 1.556(2) . ?
B1 H1 1.113(18) . ?
N1 N2 1.3699(18) . ?
N1 Ni1 1.9320(13) . ?
N5 N6 1.3698(18) . ?
N3 N4 1.3739(18) . ?
N3 Ni1 1.9017(13) . ?
S1 Ni1 2.1971(4) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
S1 C1 S2 135.75(10) . . ?
S1 C1 Ni1 79.45(7) . . ?
S2 C1 Ni1 144.78(10) . . ?
C3 C2 S2 108.56(11) . . ?
C3 C2 H2A 110.0 . . ?
S2 C2 H2A 110.0 . . ?
C3 C2 H2B 110.0 . . ?
S2 C2 H2B 110.0 . . ?
H2A C2 H2B 108.4 . . ?
C4 C3 C8 119.01(15) . . ?
C4 C3 C2 120.15(15) . . ?
C8 C3 C2 120.84(15) . . ?
C5 C4 C3 120.47(15) . . ?
C5 C4 H4 119.8 . . ?
C3 C4 H4 119.8 . . ?
C4 C5 C6 120.43(16) . . ?
C4 C5 H5 119.8 . . ?
C6 C5 H5 119.8 . . ?
C5 C6 C7 119.32(16) . . ?
C5 C6 H6 120.3 . . ?
C7 C6 H6 120.3 . . ?
C8 C7 C6 120.38(16) . . ?
C8 C7 H7 119.8 . . ?
C6 C7 H7 119.8 . . ?
C7 C8 C3 120.37(15) . . ?
C7 C8 H8 119.8 . . ?
C3 C8 H8 119.8 . . ?
N1 C9 C10 109.32(14) . . ?
N1 C9 C13 123.02(14) . . ?
C10 C9 C13 127.58(14) . . ?
C11 C10 C9 105.87(14) . . ?
C11 C10 H10 127.1 . . ?
C9 C10 H10 127.1 . . ?
N2 C11 C10 108.07(14) . . ?
N2 C11 C12 122.80(14) . . ?
C10 C11 C12 129.02(15) . . ?
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 . . ?
C14 C13 C18 118.02(15) . . ?
C14 C13 C9 120.19(14) . . ?
C18 C13 C9 121.69(14) . . ?
C15 C14 C13 120.93(15) . . ?
C15 C14 H14 119.5 . . ?
C13 C14 H14 119.5 . . ?
C16 C15 C14 120.31(15) . . ?
C16 C15 H15 119.8 . . ?
C14 C15 H15 119.8 . . ?
C15 C16 C17 119.36(15) . . ?
C15 C16 H16 120.3 . . ?
C17 C16 H16 120.3 . . ?
C18 C17 C16 120.65(16) . . ?
C18 C17 H17 119.7 . . ?
C16 C17 H17 119.7 . . ?
C17 C18 C13 120.73(15) . . ?
C17 C18 H18 119.6 . . ?
C13 C18 H18 119.6 . . ?
N5 C19 C20 110.79(14) . . ?
N5 C19 C23 121.76(14) . . ?
C20 C19 C23 127.35(14) . . ?
C21 C20 C19 105.58(14) . . ?
C21 C20 H20 127.2 . . ?
C19 C20 H20 127.2 . . ?
N6 C21 C20 106.99(14) . . ?
N6 C21 C22 123.74(15) . . ?
C20 C21 C22 129.22(15) . . ?
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 . . ?
C28 C23 C24 118.58(15) . . ?
C28 C23 C19 121.10(15) . . ?
C24 C23 C19 120.22(15) . . ?
C25 C24 C23 120.84(16) . . ?
C25 C24 H24 119.6 . . ?
C23 C24 H24 119.6 . . ?
C24 C25 C26 120.27(16) . . ?
C24 C25 H25 119.9 . . ?
C26 C25 H25 119.9 . . ?
C25 C26 C27 119.46(16) . . ?
C25 C26 H26 120.3 . . ?
C27 C26 H26 120.3 . . ?
C26 C27 C28 120.48(17) . . ?
C26 C27 H27 119.8 . . ?
C28 C27 H27 119.8 . . ?
C27 C28 C23 120.37(16) . . ?
C27 C28 H28 119.8 . . ?
C23 C28 H28 119.8 . . ?
N3 C29 C30 109.37(14) . . ?
N3 C29 C33 123.56(14) . . ?
C30 C29 C33 126.94(14) . . ?
C31 C30 C29 106.05(14) . . ?
C31 C30 H30 127.0 . . ?
C29 C30 H30 127.0 . . ?
N4 C31 C30 108.09(14) . . ?
N4 C31 C32 122.98(14) . . ?
C30 C31 C32 128.83(15) . . ?
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 . . ?
C38 C33 C34 118.48(15) . . ?
C38 C33 C29 119.63(14) . . ?
C34 C33 C29 121.61(14) . . ?
C35 C34 C33 120.69(15) . . ?
C35 C34 H34 119.7 . . ?
C33 C34 H34 119.7 . . ?
C34 C35 C36 120.20(16) . . ?
C34 C35 H35 119.9 . . ?
C36 C35 H35 119.9 . . ?
C37 C36 C35 119.68(16) . . ?
C37 C36 H36 120.2 . . ?
C35 C36 H36 120.2 . . ?
C36 C37 C38 120.33(15) . . ?
C36 C37 H37 119.8 . . ?
C38 C37 H37 119.8 . . ?
C37 C38 C33 120.61(15) . . ?
C37 C38 H38 119.7 . . ?
C33 C38 H38 119.7 . . ?
N6 B1 N2 111.18(13) . . ?
N6 B1 N4 111.04(13) . . ?
N2 B1 N4 109.58(13) . . ?
N6 B1 H1 109.4(9) . . ?
N2 B1 H1 107.4(9) . . ?
N4 B1 H1 108.1(9) . . ?
C9 N1 N2 107.19(12) . . ?
C9 N1 Ni1 134.81(11) . . ?
N2 N1 Ni1 117.36(10) . . ?
C11 N2 N1 109.51(12) . . ?
C11 N2 B1 127.38(13) . . ?
N1 N2 B1 123.10(12) . . ?
C19 N5 N6 105.51(12) . . ?
C21 N6 N5 111.11(13) . . ?
C21 N6 B1 130.18(13) . . ?
N5 N6 B1 118.63(12) . . ?
C29 N3 N4 107.01(12) . . ?
C29 N3 Ni1 135.22(11) . . ?
N4 N3 Ni1 117.14(10) . . ?
C31 N4 N3 109.43(12) . . ?
C31 N4 B1 126.74(13) . . ?
N3 N4 B1 123.82(12) . . ?
C1 S1 Ni1 53.52(6) . . ?
C1 S2 C2 103.58(8) . . ?
C1 Ni1 N3 108.37(6) . . ?
C1 Ni1 N1 160.02(6) . . ?
N3 Ni1 N1 91.60(5) . . ?
C1 Ni1 S1 47.03(5) . . ?
N3 Ni1 S1 155.18(4) . . ?
N1 Ni1 S1 113.01(4) . . ?

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         0.306
_refine_diff_density_min         -0.269
_refine_diff_density_rms         0.048

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

data_Complex_7b
_database_code_depnum_ccdc_archive 'CCDC 1476058'
_audit_update_record             
;
2016-05-13 deposited with the CCDC.
2016-06-21 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        'Complex 7b'
_chemical_name_common            'Complex 7b'
_chemical_melting_point          423.2-424.7
_chemical_formula_moiety         'C35 H39 B N6 Ni O Si, C4 H8 O'
_chemical_formula_sum            'C39 H47 B N6 Ni O2 Si'
_chemical_formula_weight         729.44

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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                   11.2799(17)
_cell_length_b                   11.6561(17)
_cell_length_c                   14.715(2)
_cell_angle_alpha                101.527(8)
_cell_angle_beta                 96.979(9)
_cell_angle_gamma                93.515(9)
_cell_volume                     1874.4(5)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9925
_cell_measurement_theta_min      2.16
_cell_measurement_theta_max      25.23

_exptl_crystal_description       rode
_exptl_crystal_colour            orange
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.08
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.292
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             772
_exptl_absorpt_coefficient_mu    0.592
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.9358
_exptl_absorpt_correction_T_max  0.9785
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean 8.366
_diffrn_reflns_number            19460
_diffrn_reflns_av_R_equivalents  0.0426
_diffrn_reflns_av_sigmaI/netI    0.0508
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         1.43
_diffrn_reflns_theta_max         25.26
_reflns_number_total             6652
_reflns_number_gt                5431
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker APEX2 v.2011.4'
_computing_cell_refinement       'Bruker APEX2 v.2011.4'
_computing_data_reduction        'Bruker APEX2 v.2011.4'
_computing_structure_solution    SIR-92
_computing_structure_refinement  SHELXL-97
_computing_molecular_graphics    ORTEP-32
_computing_publication_material  WinGX

_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)+(0.0595P)²+1.6298P] 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         6652
_refine_ls_number_parameters     461
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0604
_refine_ls_R_factor_gt           0.0471
_refine_ls_wR_factor_ref         0.1228
_refine_ls_wR_factor_gt          0.1147
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_restrained_S_all      1.037
_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
C1 C 0.1603(2) 0.1851(3) 0.25287(19) 0.0210(6) Uani 1 1 d . . .
C2 C 0.0953(3) 0.2266(3) 0.17476(19) 0.0245(7) Uani 1 1 d . . .
H2A H 0.0700 0.3036 0.1988 0.029 Uiso 1 1 calc R . .
H2B H 0.0236 0.1739 0.1505 0.029 Uiso 1 1 calc R . .
C3 C 0.1632(3) 0.0924(3) -0.0099(2) 0.0360(8) Uani 1 1 d . . .
H3A H 0.2060 0.0965 -0.0619 0.054 Uiso 1 1 calc R . .
H3B H 0.0795 0.0725 -0.0323 0.054 Uiso 1 1 calc R . .
H3C H 0.1936 0.0335 0.0215 0.054 Uiso 1 1 calc R . .
C4 C 0.1164(3) 0.3514(3) 0.0164(2) 0.0370(8) Uani 1 1 d . . .
H4A H 0.1187 0.4233 0.0620 0.056 Uiso 1 1 calc R . .
H4B H 0.0347 0.3251 -0.0095 0.056 Uiso 1 1 calc R . .
H4C H 0.1610 0.3647 -0.0327 0.056 Uiso 1 1 calc R . .
C5 C 0.3440(3) 0.2832(3) 0.1175(2) 0.0294(7) Uani 1 1 d . . .
H5A H 0.3774 0.2253 0.1487 0.044 Uiso 1 1 calc R . .
H5B H 0.3509 0.3576 0.1608 0.044 Uiso 1 1 calc R . .
H5C H 0.3866 0.2905 0.0661 0.044 Uiso 1 1 calc R . .
C6 C 0.6607(2) 0.5126(2) 0.4004(2) 0.0215(6) Uani 1 1 d . . .
H6A H 0.7001 0.4736 0.4456 0.032 Uiso 1 1 calc R . .
H6B H 0.6714 0.5961 0.4240 0.032 Uiso 1 1 calc R . .
H6C H 0.6946 0.4937 0.3430 0.032 Uiso 1 1 calc R . .
C7 C 0.5303(2) 0.4731(2) 0.38263(18) 0.0166(6) Uani 1 1 d . . .
C8 C 0.4346(2) 0.5373(2) 0.36477(18) 0.0182(6) Uani 1 1 d . . .
H8 H 0.4384 0.6162 0.3612 0.022 Uiso 1 1 calc R . .
C9 C 0.3314(2) 0.4610(2) 0.35304(18) 0.0175(6) Uani 1 1 d . . .
C10 C 0.2051(2) 0.4849(2) 0.33539(19) 0.0188(6) Uani 1 1 d . . .
C11 C 0.1687(3) 0.5500(3) 0.2685(2) 0.0253(7) Uani 1 1 d . . .
H11 H 0.2251 0.5812 0.2369 0.030 Uiso 1 1 calc R . .
C12 C 0.0489(3) 0.5681(3) 0.2492(2) 0.0321(7) Uani 1 1 d . . .
H12 H 0.0250 0.6100 0.2036 0.039 Uiso 1 1 calc R . .
C13 C -0.0355(3) 0.5243(3) 0.2972(2) 0.0325(8) Uani 1 1 d . . .
H13 H -0.1159 0.5359 0.2832 0.039 Uiso 1 1 calc R . .
C14 C -0.0002(3) 0.4634(3) 0.3660(2) 0.0250(7) Uani 1 1 d . . .
H14 H -0.0565 0.4354 0.3993 0.030 Uiso 1 1 calc R . .
C15 C 0.1194(2) 0.4440(2) 0.38519(19) 0.0199(6) Uani 1 1 d . . .
H15 H 0.1430 0.4033 0.4317 0.024 Uiso 1 1 calc R . .
C16 C 0.6806(3) 0.1629(3) 0.5663(2) 0.0226(6) Uani 1 1 d . . .
H16A H 0.7149 0.1286 0.5118 0.034 Uiso 1 1 calc R . .
H16B H 0.6996 0.1200 0.6147 0.034 Uiso 1 1 calc R . .
H16C H 0.7129 0.2433 0.5880 0.034 Uiso 1 1 calc R . .
C17 C 0.5475(2) 0.1583(2) 0.54238(18) 0.0174(6) Uani 1 1 d . . .
C18 C 0.4591(2) 0.1210(2) 0.58932(18) 0.0183(6) Uani 1 1 d . . .
H18 H 0.4696 0.0916 0.6438 0.022 Uiso 1 1 calc R . .
C19 C 0.3497(2) 0.1362(2) 0.53825(18) 0.0168(6) Uani 1 1 d . . .
C20 C 0.2281(2) 0.1193(2) 0.56318(18) 0.0179(6) Uani 1 1 d . . .
C21 C 0.1328(3) 0.1756(2) 0.5285(2) 0.0215(6) Uani 1 1 d . . .
H21 H 0.1440 0.2212 0.4847 0.026 Uiso 1 1 calc R . .
C22 C 0.0219(3) 0.1648(3) 0.5580(2) 0.0263(7) Uani 1 1 d . . .
H22 H -0.0407 0.2034 0.5342 0.032 Uiso 1 1 calc R . .
C23 C 0.0032(3) 0.0970(3) 0.6229(2) 0.0270(7) Uani 1 1 d . . .
H23 H -0.0716 0.0895 0.6426 0.032 Uiso 1 1 calc R . .
C24 C 0.0967(3) 0.0404(3) 0.6581(2) 0.0266(7) Uani 1 1 d . . .
H24 H 0.0848 -0.0050 0.7020 0.032 Uiso 1 1 calc R . .
C25 C 0.2075(3) 0.0506(2) 0.62866(19) 0.0218(6) Uani 1 1 d . . .
H25 H 0.2695 0.0114 0.6526 0.026 Uiso 1 1 calc R . .
C26 C 0.7521(3) 0.2161(3) 0.2636(2) 0.0281(7) Uani 1 1 d . . .
H26A H 0.7404 0.2966 0.2621 0.042 Uiso 1 1 calc R . .
H26B H 0.8005 0.1855 0.2165 0.042 Uiso 1 1 calc R . .
H26C H 0.7918 0.2115 0.3241 0.042 Uiso 1 1 calc R . .
C27 C 0.6329(2) 0.1452(2) 0.24492(19) 0.0188(6) Uani 1 1 d . . .
C28 C 0.5887(3) 0.0536(2) 0.17210(19) 0.0218(6) Uani 1 1 d . . .
H28 H 0.6272 0.0210 0.1219 0.026 Uiso 1 1 calc R . .
C29 C 0.4736(3) 0.0193(2) 0.18912(18) 0.0184(6) Uani 1 1 d . . .
C30 C 0.3880(3) -0.0772(2) 0.13301(19) 0.0216(6) Uani 1 1 d . . .
C31 C 0.2856(3) -0.1146(3) 0.1674(2) 0.0275(7) Uani 1 1 d . . .
H31 H 0.2698 -0.0777 0.2263 0.033 Uiso 1 1 calc R . .
C32 C 0.2072(3) -0.2065(3) 0.1140(2) 0.0361(8) Uani 1 1 d . . .
H32 H 0.1393 -0.2313 0.1374 0.043 Uiso 1 1 calc R . .
C33 C 0.2295(3) -0.2618(3) 0.0256(2) 0.0357(8) Uani 1 1 d . . .
H33 H 0.1770 -0.3236 -0.0099 0.043 Uiso 1 1 calc R . .
C34 C 0.3300(3) -0.2244(3) -0.0089(2) 0.0311(8) Uani 1 1 d . . .
H34 H 0.3448 -0.2610 -0.0682 0.037 Uiso 1 1 calc R . .
C35 C 0.4088(3) -0.1331(2) 0.0438(2) 0.0253(7) Uani 1 1 d . . .
H35 H 0.4763 -0.1086 0.0197 0.030 Uiso 1 1 calc R . .
C36 C 0.2678(3) 0.3165(3) -0.2072(2) 0.0392(8) Uani 1 1 d . . .
H36A H 0.2639 0.3047 -0.2747 0.047 Uiso 1 1 calc R . .
H36B H 0.1954 0.2787 -0.1929 0.047 Uiso 1 1 calc R . .
C37 C 0.3749(3) 0.2670(3) -0.1671(3) 0.0422(9) Uani 1 1 d . . .
H37A H 0.3948 0.1988 -0.2103 0.051 Uiso 1 1 calc R . .
H37B H 0.3628 0.2451 -0.1084 0.051 Uiso 1 1 calc R . .
C38 C 0.4710(3) 0.3674(3) -0.1520(3) 0.0410(9) Uani 1 1 d . . .
H38A H 0.5319 0.3642 -0.1003 0.049 Uiso 1 1 calc R . .
H38B H 0.5087 0.3666 -0.2080 0.049 Uiso 1 1 calc R . .
C39 C 0.4026(3) 0.4741(3) -0.1301(3) 0.0493(10) Uani 1 1 d . . .
H39A H 0.4114 0.5040 -0.0630 0.059 Uiso 1 1 calc R . .
H39B H 0.4326 0.5355 -0.1593 0.059 Uiso 1 1 calc R . .
N1 N 0.36275(19) 0.35408(19) 0.36224(15) 0.0161(5) Uani 1 1 d . . .
N2 N 0.48564(19) 0.36151(18) 0.38095(15) 0.0153(5) Uani 1 1 d . . .
N3 N 0.3711(2) 0.17852(19) 0.46273(15) 0.0167(5) Uani 1 1 d . . .
N4 N 0.4938(2) 0.19434(19) 0.46702(15) 0.0172(5) Uani 1 1 d . . .
N5 N 0.4480(2) 0.08594(19) 0.26837(15) 0.0182(5) Uani 1 1 d . . .
N6 N 0.5472(2) 0.16280(19) 0.30243(15) 0.0172(5) Uani 1 1 d . . .
O1 O 0.14369(17) 0.09260(17) 0.28020(13) 0.0238(5) Uani 1 1 d . . .
O2 O 0.2795(2) 0.4386(2) -0.16596(17) 0.0417(6) Uani 1 1 d . . .
Si1 Si 0.18385(8) 0.23767(8) 0.07316(6) 0.0254(2) Uani 1 1 d . . .
Ni01 Ni 0.27688(3) 0.20711(3) 0.34888(2) 0.01819(12) Uani 1 1 d . . .
B1 B 0.5521(3) 0.2526(3) 0.3960(2) 0.0181(7) Uani 1 1 d . . .
H1 H 0.646(2) 0.280(2) 0.4242(16) 0.003(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
C1 O1 1.235(3) . ?
C1 C2 1.468(4) . ?
C1 Ni01 1.776(3) . ?
C2 Si1 1.916(3) . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C3 Si1 1.863(3) . ?
C3 H3A 0.9600 . ?
C3 H3B 0.9600 . ?
C3 H3C 0.9600 . ?
C4 Si1 1.857(3) . ?
C4 H4A 0.9600 . ?
C4 H4B 0.9600 . ?
C4 H4C 0.9600 . ?
C5 Si1 1.851(3) . ?
C5 H5A 0.9600 . ?
C5 H5B 0.9600 . ?
C5 H5C 0.9600 . ?
C6 C7 1.490(4) . ?
C6 H6A 0.9600 . ?
C6 H6B 0.9600 . ?
C6 H6C 0.9600 . ?
C7 N2 1.360(3) . ?
C7 C8 1.379(4) . ?
C8 C9 1.393(4) . ?
C8 H8 0.9300 . ?
C9 N1 1.344(3) . ?
C9 C10 1.470(4) . ?
C10 C11 1.397(4) . ?
C10 C15 1.398(4) . ?
C11 C12 1.385(4) . ?
C11 H11 0.9300 . ?
C12 C13 1.383(5) . ?
C12 H12 0.9300 . ?
C13 C14 1.383(4) . ?
C13 H13 0.9300 . ?
C14 C15 1.386(4) . ?
C14 H14 0.9300 . ?
C15 H15 0.9300 . ?
C16 C17 1.496(4) . ?
C16 H16A 0.9600 . ?
C16 H16B 0.9600 . ?
C16 H16C 0.9600 . ?
C17 N4 1.352(4) . ?
C17 C18 1.377(4) . ?
C18 C19 1.405(4) . ?
C18 H18 0.9300 . ?
C19 N3 1.344(3) . ?
C19 C20 1.475(4) . ?
C20 C21 1.390(4) . ?
C20 C25 1.401(4) . ?
C21 C22 1.381(4) . ?
C21 H21 0.9300 . ?
C22 C23 1.383(4) . ?
C22 H22 0.9300 . ?
C23 C24 1.379(4) . ?
C23 H23 0.9300 . ?
C24 C25 1.379(4) . ?
C24 H24 0.9300 . ?
C25 H25 0.9300 . ?
C26 C27 1.500(4) . ?
C26 H26A 0.9600 . ?
C26 H26B 0.9600 . ?
C26 H26C 0.9600 . ?
C27 N6 1.358(3) . ?
C27 C28 1.373(4) . ?
C28 C29 1.401(4) . ?
C28 H28 0.9300 . ?
C29 N5 1.339(3) . ?
C29 C30 1.477(4) . ?
C30 C31 1.396(4) . ?
C30 C35 1.398(4) . ?
C31 C32 1.388(4) . ?
C31 H31 0.9300 . ?
C32 C33 1.391(5) . ?
C32 H32 0.9300 . ?
C33 C34 1.379(5) . ?
C33 H33 0.9300 . ?
C34 C35 1.383(4) . ?
C34 H34 0.9300 . ?
C35 H35 0.9300 . ?
C36 O2 1.423(4) . ?
C36 C37 1.480(5) . ?
C36 H36A 0.9700 . ?
C36 H36B 0.9700 . ?
C37 C38 1.508(5) . ?
C37 H37A 0.9700 . ?
C37 H37B 0.9700 . ?
C38 C39 1.505(5) . ?
C38 H38A 0.9700 . ?
C38 H38B 0.9700 . ?
C39 O2 1.428(4) . ?
C39 H39A 0.9700 . ?
C39 H39B 0.9700 . ?
N1 N2 1.374(3) . ?
N1 Ni01 1.878(2) . ?
N2 B1 1.552(4) . ?
N3 N4 1.376(3) . ?
N3 Ni01 1.970(2) . ?
N4 B1 1.544(4) . ?
N5 N6 1.366(3) . ?
N6 B1 1.546(4) . ?
O1 Ni01 1.9765(19) . ?
B1 H1 1.09(2) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 C1 C2 130.1(3) . . ?
O1 C1 Ni01 79.86(18) . . ?
C2 C1 Ni01 150.1(2) . . ?
C1 C2 Si1 115.4(2) . . ?
C1 C2 H2A 108.4 . . ?
Si1 C2 H2A 108.4 . . ?
C1 C2 H2B 108.4 . . ?
Si1 C2 H2B 108.4 . . ?
H2A C2 H2B 107.5 . . ?
Si1 C3 H3A 109.5 . . ?
Si1 C3 H3B 109.5 . . ?
H3A C3 H3B 109.5 . . ?
Si1 C3 H3C 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?
Si1 C4 H4A 109.5 . . ?
Si1 C4 H4B 109.5 . . ?
H4A C4 H4B 109.5 . . ?
Si1 C4 H4C 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
Si1 C5 H5A 109.5 . . ?
Si1 C5 H5B 109.5 . . ?
H5A C5 H5B 109.5 . . ?
Si1 C5 H5C 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
C7 C6 H6A 109.5 . . ?
C7 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
C7 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
N2 C7 C8 107.7(2) . . ?
N2 C7 C6 123.7(2) . . ?
C8 C7 C6 128.6(3) . . ?
C7 C8 C9 106.6(2) . . ?
C7 C8 H8 126.7 . . ?
C9 C8 H8 126.7 . . ?
N1 C9 C8 109.0(2) . . ?
N1 C9 C10 121.7(2) . . ?
C8 C9 C10 129.2(2) . . ?
C11 C10 C15 118.7(3) . . ?
C11 C10 C9 120.3(3) . . ?
C15 C10 C9 121.0(3) . . ?
C12 C11 C10 120.1(3) . . ?
C12 C11 H11 119.9 . . ?
C10 C11 H11 119.9 . . ?
C13 C12 C11 120.5(3) . . ?
C13 C12 H12 119.7 . . ?
C11 C12 H12 119.7 . . ?
C14 C13 C12 120.0(3) . . ?
C14 C13 H13 120.0 . . ?
C12 C13 H13 120.0 . . ?
C13 C14 C15 119.9(3) . . ?
C13 C14 H14 120.1 . . ?
C15 C14 H14 120.1 . . ?
C14 C15 C10 120.7(3) . . ?
C14 C15 H15 119.6 . . ?
C10 C15 H15 119.6 . . ?
C17 C16 H16A 109.5 . . ?
C17 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
C17 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
N4 C17 C18 107.9(2) . . ?
N4 C17 C16 123.1(2) . . ?
C18 C17 C16 129.0(3) . . ?
C17 C18 C19 106.1(2) . . ?
C17 C18 H18 127.0 . . ?
C19 C18 H18 127.0 . . ?
N3 C19 C18 109.4(2) . . ?
N3 C19 C20 122.6(2) . . ?
C18 C19 C20 127.8(2) . . ?
C21 C20 C25 117.8(3) . . ?
C21 C20 C19 122.3(2) . . ?
C25 C20 C19 119.8(3) . . ?
C22 C21 C20 121.2(3) . . ?
C22 C21 H21 119.4 . . ?
C20 C21 H21 119.4 . . ?
C21 C22 C23 120.3(3) . . ?
C21 C22 H22 119.8 . . ?
C23 C22 H22 119.8 . . ?
C24 C23 C22 119.4(3) . . ?
C24 C23 H23 120.3 . . ?
C22 C23 H23 120.3 . . ?
C25 C24 C23 120.5(3) . . ?
C25 C24 H24 119.7 . . ?
C23 C24 H24 119.7 . . ?
C24 C25 C20 120.8(3) . . ?
C24 C25 H25 119.6 . . ?
C20 C25 H25 119.6 . . ?
C27 C26 H26A 109.5 . . ?
C27 C26 H26B 109.5 . . ?
H26A C26 H26B 109.5 . . ?
C27 C26 H26C 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
N6 C27 C28 107.2(2) . . ?
N6 C27 C26 123.4(2) . . ?
C28 C27 C26 129.3(3) . . ?
C27 C28 C29 105.7(2) . . ?
C27 C28 H28 127.1 . . ?
C29 C28 H28 127.1 . . ?
N5 C29 C28 110.5(2) . . ?
N5 C29 C30 121.5(2) . . ?
C28 C29 C30 127.9(2) . . ?
C31 C30 C35 118.8(3) . . ?
C31 C30 C29 121.2(2) . . ?
C35 C30 C29 120.1(3) . . ?
C32 C31 C30 120.2(3) . . ?
C32 C31 H31 119.9 . . ?
C30 C31 H31 119.9 . . ?
C31 C32 C33 120.4(3) . . ?
C31 C32 H32 119.8 . . ?
C33 C32 H32 119.8 . . ?
C34 C33 C32 119.5(3) . . ?
C34 C33 H33 120.2 . . ?
C32 C33 H33 120.2 . . ?
C33 C34 C35 120.6(3) . . ?
C33 C34 H34 119.7 . . ?
C35 C34 H34 119.7 . . ?
C34 C35 C30 120.5(3) . . ?
C34 C35 H35 119.7 . . ?
C30 C35 H35 119.7 . . ?
O2 C36 C37 106.5(3) . . ?
O2 C36 H36A 110.4 . . ?
C37 C36 H36A 110.4 . . ?
O2 C36 H36B 110.4 . . ?
C37 C36 H36B 110.4 . . ?
H36A C36 H36B 108.6 . . ?
C36 C37 C38 102.8(3) . . ?
C36 C37 H37A 111.2 . . ?
C38 C37 H37A 111.2 . . ?
C36 C37 H37B 111.2 . . ?
C38 C37 H37B 111.2 . . ?
H37A C37 H37B 109.1 . . ?
C39 C38 C37 103.0(3) . . ?
C39 C38 H38A 111.2 . . ?
C37 C38 H38A 111.2 . . ?
C39 C38 H38B 111.2 . . ?
C37 C38 H38B 111.2 . . ?
H38A C38 H38B 109.1 . . ?
O2 C39 C38 107.2(3) . . ?
O2 C39 H39A 110.3 . . ?
C38 C39 H39A 110.3 . . ?
O2 C39 H39B 110.3 . . ?
C38 C39 H39B 110.3 . . ?
H39A C39 H39B 108.5 . . ?
C9 N1 N2 107.5(2) . . ?
C9 N1 Ni01 133.90(19) . . ?
N2 N1 Ni01 118.50(17) . . ?
C7 N2 N1 109.1(2) . . ?
C7 N2 B1 129.9(2) . . ?
N1 N2 B1 121.0(2) . . ?
C19 N3 N4 106.7(2) . . ?
C19 N3 Ni01 137.13(19) . . ?
N4 N3 Ni01 115.89(16) . . ?
C17 N4 N3 109.9(2) . . ?
C17 N4 B1 128.7(2) . . ?
N3 N4 B1 121.3(2) . . ?
C29 N5 N6 105.6(2) . . ?
C27 N6 N5 110.9(2) . . ?
C27 N6 B1 128.6(2) . . ?
N5 N6 B1 120.5(2) . . ?
C1 O1 Ni01 62.19(15) . . ?
C36 O2 C39 108.9(3) . . ?
C5 Si1 C4 110.03(16) . . ?
C5 Si1 C3 111.87(15) . . ?
C4 Si1 C3 110.33(16) . . ?
C5 Si1 C2 110.45(13) . . ?
C4 Si1 C2 105.75(14) . . ?
C3 Si1 C2 108.21(15) . . ?
C1 Ni01 N1 110.12(12) . . ?
C1 Ni01 N3 158.15(12) . . ?
N1 Ni01 N3 91.34(9) . . ?
C1 Ni01 O1 37.95(11) . . ?
N1 Ni01 O1 148.07(9) . . ?
N3 Ni01 O1 120.45(9) . . ?
N4 B1 N6 109.8(2) . . ?
N4 B1 N2 109.4(2) . . ?
N6 B1 N2 110.8(2) . . ?
N4 B1 H1 108.3(13) . . ?
N6 B1 H1 108.6(12) . . ?
N2 B1 H1 109.9(13) . . ?

_diffrn_measured_fraction_theta_max 0.979
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.983
_refine_diff_density_max         1.137
_refine_diff_density_min         -0.491
_refine_diff_density_rms         0.071
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent'
_solvent_exptl_crystal_recrystallization_method Hexanes/THF
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_Complex_4
_database_code_depnum_ccdc_archive 'CCDC 1476059'
_audit_update_record             
;
2016-05-13 deposited with the CCDC.
2016-06-21 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        'Complex 4'
_chemical_name_common            'Complex 4'
_chemical_melting_point          '469.5 (dec.)'
_chemical_formula_moiety         'C39 H38 B N7 Ni S2, C7 H8'
_chemical_formula_sum            'C46 H46 B N7 Ni S2'
_chemical_formula_weight         830.54

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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                   12.9610(18)
_cell_length_b                   20.401(3)
_cell_length_c                   16.044(2)
_cell_angle_alpha                90.00
_cell_angle_beta                 92.244(2)
_cell_angle_gamma                90.00
_cell_volume                     4239.1(10)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9886
_cell_measurement_theta_min      2.22
_cell_measurement_theta_max      25.34

_exptl_crystal_description       rode
_exptl_crystal_colour            green
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.09
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.301
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1744
_exptl_absorpt_coefficient_mu    0.598
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.8210
_exptl_absorpt_correction_T_max  0.8814
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean 8.366
_diffrn_reflns_number            28399
_diffrn_reflns_av_R_equivalents  0.0357
_diffrn_reflns_av_sigmaI/netI    0.0375
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         1.62
_diffrn_reflns_theta_max         25.35
_reflns_number_total             7751
_reflns_number_gt                5987
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker APEX2 v.2011.4'
_computing_cell_refinement       'Bruker APEX2 v.2011.4'
_computing_data_reduction        'Bruker APEX2 v.2011.4'
_computing_structure_solution    SIR-92
_computing_structure_refinement  SHELXL-97
_computing_molecular_graphics    ORTEP-32
_computing_publication_material  WinGX

_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)+(0.0511P)²+2.7755P] 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         7751
_refine_ls_number_parameters     523
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0593
_refine_ls_R_factor_gt           0.0408
_refine_ls_wR_factor_ref         0.1090
_refine_ls_wR_factor_gt          0.0978
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_restrained_S_all      1.034
_refine_ls_shift/su_max          0.005
_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
C1 C 0.57616(19) 0.18118(13) 0.17578(17) 0.0288(6) Uani 1 1 d . . .
C2 C 0.4739(3) 0.30004(16) 0.1615(3) 0.0795(15) Uani 1 1 d . . .
H2A H 0.4815 0.3014 0.2219 0.095 Uiso 1 1 calc R . .
H2B H 0.5334 0.3213 0.1385 0.095 Uiso 1 1 calc R . .
C3 C 0.3768(2) 0.33444(13) 0.1329(2) 0.0381(7) Uani 1 1 d . . .
C4 C 0.3597(2) 0.35509(14) 0.05107(19) 0.0379(7) Uani 1 1 d . . .
H4 H 0.4110 0.3487 0.0130 0.046 Uiso 1 1 calc R . .
C5 C 0.2704(3) 0.38427(14) 0.0253(2) 0.0438(8) Uani 1 1 d . . .
H5 H 0.2606 0.3971 -0.0301 0.053 Uiso 1 1 calc R . .
C6 C 0.1963(2) 0.39463(16) 0.0790(2) 0.0493(9) Uani 1 1 d . . .
H6 H 0.1352 0.4146 0.0603 0.059 Uiso 1 1 calc R . .
C7 C 0.2079(3) 0.37681(17) 0.1601(2) 0.0540(9) Uani 1 1 d . . .
H7 H 0.1554 0.3851 0.1965 0.065 Uiso 1 1 calc R . .
C8 C 0.2979(3) 0.34631(16) 0.18878(19) 0.0505(9) Uani 1 1 d . . .
H8 H 0.3061 0.3338 0.2444 0.061 Uiso 1 1 calc R . .
C9 C 0.51381(19) 0.07382(13) 0.13865(17) 0.0286(6) Uani 1 1 d . . .
H9A H 0.4478 0.0794 0.1629 0.043 Uiso 1 1 calc R . .
H9B H 0.5371 0.0296 0.1473 0.043 Uiso 1 1 calc R . .
H9C H 0.5076 0.0827 0.0799 0.043 Uiso 1 1 calc R . .
C10 C 1.07021(19) 0.01274(13) 0.39754(16) 0.0285(6) Uani 1 1 d . . .
H10A H 1.0301 -0.0154 0.4316 0.043 Uiso 1 1 calc R . .
H10B H 1.1279 0.0297 0.4301 0.043 Uiso 1 1 calc R . .
H10C H 1.0949 -0.0117 0.3513 0.043 Uiso 1 1 calc R . .
C11 C 1.00461(18) 0.06810(12) 0.36589(15) 0.0231(5) Uani 1 1 d . . .
C12 C 1.02242(19) 0.13441(13) 0.36815(16) 0.0279(6) Uani 1 1 d . . .
H12 H 1.0806 0.1554 0.3909 0.033 Uiso 1 1 calc R . .
C13 C 0.93599(18) 0.16426(12) 0.32953(15) 0.0219(5) Uani 1 1 d . . .
C14 C 0.91674(18) 0.23505(12) 0.31558(16) 0.0255(6) Uani 1 1 d . . .
C15 C 0.9489(2) 0.26515(14) 0.24343(18) 0.0345(6) Uani 1 1 d . . .
H15 H 0.9816 0.2406 0.2034 0.041 Uiso 1 1 calc R . .
C16 C 0.9325(2) 0.33143(15) 0.2309(2) 0.0420(8) Uani 1 1 d . . .
H16 H 0.9535 0.3512 0.1822 0.050 Uiso 1 1 calc R . .
C17 C 0.8856(2) 0.36782(15) 0.2896(2) 0.0452(8) Uani 1 1 d . . .
H17 H 0.8750 0.4124 0.2809 0.054 Uiso 1 1 calc R . .
C18 C 0.8539(2) 0.33893(15) 0.3619(2) 0.0467(8) Uani 1 1 d . . .
H18 H 0.8223 0.3640 0.4020 0.056 Uiso 1 1 calc R . .
C19 C 0.8693(2) 0.27227(14) 0.37472(19) 0.0375(7) Uani 1 1 d . . .
H19 H 0.8476 0.2527 0.4234 0.045 Uiso 1 1 calc R . .
C20 C 0.9209(2) -0.11338(14) 0.17343(18) 0.0395(7) Uani 1 1 d . . .
H20A H 0.9853 -0.1019 0.2012 0.059 Uiso 1 1 calc R . .
H20B H 0.9340 -0.1379 0.1239 0.059 Uiso 1 1 calc R . .
H20C H 0.8808 -0.1395 0.2100 0.059 Uiso 1 1 calc R . .
C21 C 0.8629(2) -0.05273(13) 0.15050(16) 0.0292(6) Uani 1 1 d . . .
C22 C 0.8266(2) -0.03169(13) 0.07364(16) 0.0307(6) Uani 1 1 d . . .
H22 H 0.8330 -0.0532 0.0230 0.037 Uiso 1 1 calc R . .
C23 C 0.77817(19) 0.02814(13) 0.08636(15) 0.0261(6) Uani 1 1 d . . .
C24 C 0.73040(19) 0.07259(13) 0.02277(16) 0.0276(6) Uani 1 1 d . . .
C25 C 0.6789(2) 0.04647(15) -0.04715(16) 0.0335(6) Uani 1 1 d . . .
H25 H 0.6745 0.0013 -0.0537 0.040 Uiso 1 1 calc R . .
C26 C 0.6338(2) 0.08751(16) -0.10734(18) 0.0401(7) Uani 1 1 d . . .
H26 H 0.5994 0.0697 -0.1540 0.048 Uiso 1 1 calc R . .
C27 C 0.6399(2) 0.15449(16) -0.09817(19) 0.0420(7) Uani 1 1 d . . .
H27 H 0.6094 0.1818 -0.1385 0.050 Uiso 1 1 calc R . .
C28 C 0.6914(2) 0.18116(15) -0.02876(18) 0.0397(7) Uani 1 1 d . . .
H28 H 0.6952 0.2264 -0.0222 0.048 Uiso 1 1 calc R . .
C29 C 0.7370(2) 0.14015(14) 0.03073(17) 0.0331(6) Uani 1 1 d . . .
H29 H 0.7726 0.1582 0.0767 0.040 Uiso 1 1 calc R . .
C30 C 0.7541(2) -0.11015(13) 0.42394(18) 0.0350(7) Uani 1 1 d . . .
H30A H 0.7592 -0.1395 0.3775 0.053 Uiso 1 1 calc R . .
H30B H 0.7143 -0.1304 0.4661 0.053 Uiso 1 1 calc R . .
H30C H 0.8220 -0.1003 0.4465 0.053 Uiso 1 1 calc R . .
C31 C 0.7023(2) -0.04817(12) 0.39532(15) 0.0270(6) Uani 1 1 d . . .
C32 C 0.6058(2) -0.02495(13) 0.41138(16) 0.0288(6) Uani 1 1 d . . .
H32 H 0.5574 -0.0446 0.4447 0.035 Uiso 1 1 calc R . .
C33 C 0.59460(19) 0.03422(13) 0.36757(15) 0.0256(6) Uani 1 1 d . . .
C34 C 0.5069(2) 0.08062(13) 0.36388(15) 0.0276(6) Uani 1 1 d . . .
C35 C 0.4062(2) 0.05806(16) 0.34929(17) 0.0363(7) Uani 1 1 d . . .
H35 H 0.3937 0.0134 0.3433 0.044 Uiso 1 1 calc R . .
C36 C 0.3244(2) 0.10209(17) 0.3437(2) 0.0459(8) Uani 1 1 d . . .
H36 H 0.2575 0.0867 0.3340 0.055 Uiso 1 1 calc R . .
C37 C 0.3417(2) 0.16806(17) 0.35222(19) 0.0451(8) Uani 1 1 d . . .
H37 H 0.2870 0.1975 0.3473 0.054 Uiso 1 1 calc R . .
C38 C 0.4406(2) 0.19041(16) 0.3682(2) 0.0450(8) Uani 1 1 d . . .
H38 H 0.4523 0.2351 0.3751 0.054 Uiso 1 1 calc R . .
C39 C 0.5226(2) 0.14735(14) 0.37413(18) 0.0356(7) Uani 1 1 d . . .
H39 H 0.5890 0.1633 0.3851 0.043 Uiso 1 1 calc R . .
C40 C 0.6145(3) 0.46542(17) 0.6647(2) 0.0534(9) Uani 1 1 d . . .
H40A H 0.6805 0.4696 0.6934 0.080 Uiso 1 1 calc R . .
H40B H 0.5607 0.4706 0.7037 0.080 Uiso 1 1 calc R . .
H40C H 0.6077 0.4986 0.6224 0.080 Uiso 1 1 calc R . .
C41 C 0.6060(3) 0.39927(17) 0.6250(2) 0.0482(8) Uani 1 1 d . . .
C42 C 0.6887(3) 0.35689(18) 0.6243(2) 0.0501(8) Uani 1 1 d . . .
H42 H 0.7507 0.3682 0.6516 0.060 Uiso 1 1 calc R . .
C43 C 0.6795(3) 0.29710(18) 0.5828(2) 0.0535(9) Uani 1 1 d . . .
H43 H 0.7358 0.2688 0.5826 0.064 Uiso 1 1 calc R . .
C44 C 0.5887(3) 0.27922(18) 0.5420(2) 0.0534(9) Uani 1 1 d . . .
H44 H 0.5832 0.2388 0.5154 0.064 Uiso 1 1 calc R . .
C45 C 0.5070(3) 0.3208(2) 0.5407(2) 0.0575(9) Uani 1 1 d . . .
H45 H 0.4458 0.3096 0.5120 0.069 Uiso 1 1 calc R . .
C46 C 0.5155(2) 0.37996(18) 0.5825(2) 0.0510(9) Uani 1 1 d . . .
H46 H 0.4587 0.4078 0.5821 0.061 Uiso 1 1 calc R . .
N1 N 0.86827(15) 0.11824(10) 0.30441(12) 0.0218(4) Uani 1 1 d . . .
N2 N 0.91075(15) 0.05882(10) 0.32723(12) 0.0225(4) Uani 1 1 d . . .
N3 N 0.78395(15) 0.04327(10) 0.16790(13) 0.0244(5) Uani 1 1 d . . .
N4 N 0.83642(15) -0.00724(10) 0.20748(12) 0.0236(5) Uani 1 1 d . . .
N5 N 0.68087(15) 0.04626(10) 0.32663(12) 0.0233(5) Uani 1 1 d . . .
N6 N 0.74715(15) -0.00477(10) 0.34411(12) 0.0236(5) Uani 1 1 d . . .
N7 N 0.58797(15) 0.11890(10) 0.17785(13) 0.0240(5) Uani 1 1 d . . .
S1 S 0.67530(5) 0.22589(3) 0.22485(5) 0.03731(19) Uani 1 1 d . . .
S2 S 0.46566(5) 0.21564(4) 0.12606(5) 0.0408(2) Uani 1 1 d . . .
Ni1 Ni 0.72665(2) 0.113292(15) 0.242052(19) 0.02150(10) Uani 1 1 d . . .
B1 B 0.8537(2) -0.00525(14) 0.30322(18) 0.0250(6) Uani 1 1 d . . .
H1 H 0.8971(17) -0.0478(12) 0.3240(14) 0.017(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
C1 N7 1.280(3) . ?
C1 S1 1.739(3) . ?
C1 S2 1.758(3) . ?
C2 C3 1.498(4) . ?
C2 S2 1.815(3) . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C3 C4 1.388(4) . ?
C3 C8 1.408(5) . ?
C4 C5 1.352(4) . ?
C4 H4 0.9300 . ?
C5 C6 1.331(5) . ?
C5 H5 0.9300 . ?
C6 C7 1.354(5) . ?
C6 H6 0.9300 . ?
C7 C8 1.384(5) . ?
C7 H7 0.9300 . ?
C8 H8 0.9300 . ?
C9 N7 1.455(3) . ?
C9 H9A 0.9600 . ?
C9 H9B 0.9600 . ?
C9 H9C 0.9600 . ?
C10 C11 1.491(3) . ?
C10 H10A 0.9600 . ?
C10 H10B 0.9600 . ?
C10 H10C 0.9600 . ?
C11 N2 1.357(3) . ?
C11 C12 1.373(4) . ?
C12 C13 1.398(3) . ?
C12 H12 0.9300 . ?
C13 N1 1.337(3) . ?
C13 C14 1.481(3) . ?
C14 C19 1.378(4) . ?
C14 C15 1.389(4) . ?
C15 C16 1.382(4) . ?
C15 H15 0.9300 . ?
C16 C17 1.360(5) . ?
C16 H16 0.9300 . ?
C17 C18 1.378(5) . ?
C17 H17 0.9300 . ?
C18 C19 1.389(4) . ?
C18 H18 0.9300 . ?
C19 H19 0.9300 . ?
C20 C21 1.487(4) . ?
C20 H20A 0.9600 . ?
C20 H20B 0.9600 . ?
C20 H20C 0.9600 . ?
C21 N4 1.356(3) . ?
C21 C22 1.371(4) . ?
C22 C23 1.391(4) . ?
C22 H22 0.9300 . ?
C23 N3 1.343(3) . ?
C23 C24 1.482(3) . ?
C24 C25 1.389(4) . ?
C24 C29 1.387(4) . ?
C25 C26 1.389(4) . ?
C25 H25 0.9300 . ?
C26 C27 1.376(4) . ?
C26 H26 0.9300 . ?
C27 C28 1.387(4) . ?
C27 H27 0.9300 . ?
C28 C29 1.385(4) . ?
C28 H28 0.9300 . ?
C29 H29 0.9300 . ?
C30 C31 1.496(4) . ?
C30 H30A 0.9600 . ?
C30 H30B 0.9600 . ?
C30 H30C 0.9600 . ?
C31 N6 1.354(3) . ?
C31 C32 1.371(4) . ?
C32 C33 1.402(4) . ?
C32 H32 0.9300 . ?
C33 N5 1.342(3) . ?
C33 C34 1.478(4) . ?
C34 C39 1.385(4) . ?
C34 C35 1.396(4) . ?
C35 C36 1.389(4) . ?
C35 H35 0.9300 . ?
C36 C37 1.370(5) . ?
C36 H36 0.9300 . ?
C37 C38 1.375(4) . ?
C37 H37 0.9300 . ?
C38 C39 1.380(4) . ?
C38 H38 0.9300 . ?
C39 H39 0.9300 . ?
C40 C41 1.494(5) . ?
C40 H40A 0.9600 . ?
C40 H40B 0.9600 . ?
C40 H40C 0.9600 . ?
C41 C42 1.377(5) . ?
C41 C46 1.390(5) . ?
C42 C43 1.393(5) . ?
C42 H42 0.9300 . ?
C43 C44 1.374(5) . ?
C43 H43 0.9300 . ?
C44 C45 1.356(5) . ?
C44 H44 0.9300 . ?
C45 C46 1.383(5) . ?
C45 H45 0.9300 . ?
C46 H46 0.9300 . ?
N1 N2 1.375(3) . ?
N1 Ni1 2.058(2) . ?
N2 B1 1.543(4) . ?
N3 N4 1.376(3) . ?
N3 Ni1 2.019(2) . ?
N4 B1 1.544(3) . ?
N5 N6 1.372(3) . ?
N5 Ni1 2.031(2) . ?
N6 B1 1.553(4) . ?
N7 Ni1 2.040(2) . ?
S1 Ni1 2.4045(8) . ?
B1 H1 1.08(2) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N7 C1 S1 115.05(19) . . ?
N7 C1 S2 120.20(19) . . ?
S1 C1 S2 124.75(16) . . ?
C3 C2 S2 108.0(2) . . ?
C3 C2 H2A 110.1 . . ?
S2 C2 H2A 110.1 . . ?
C3 C2 H2B 110.1 . . ?
S2 C2 H2B 110.1 . . ?
H2A C2 H2B 108.4 . . ?
C4 C3 C8 117.2(3) . . ?
C4 C3 C2 122.3(3) . . ?
C8 C3 C2 120.5(3) . . ?
C5 C4 C3 121.7(3) . . ?
C5 C4 H4 119.1 . . ?
C3 C4 H4 119.1 . . ?
C6 C5 C4 120.2(3) . . ?
C6 C5 H5 119.9 . . ?
C4 C5 H5 119.9 . . ?
C5 C6 C7 121.5(3) . . ?
C5 C6 H6 119.2 . . ?
C7 C6 H6 119.2 . . ?
C6 C7 C8 120.1(3) . . ?
C6 C7 H7 120.0 . . ?
C8 C7 H7 120.0 . . ?
C7 C8 C3 119.3(3) . . ?
C7 C8 H8 120.4 . . ?
C3 C8 H8 120.4 . . ?
N7 C9 H9A 109.5 . . ?
N7 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
N7 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C11 C10 H10A 109.5 . . ?
C11 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C11 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
N2 C11 C12 107.2(2) . . ?
N2 C11 C10 122.6(2) . . ?
C12 C11 C10 130.1(2) . . ?
C11 C12 C13 106.6(2) . . ?
C11 C12 H12 126.7 . . ?
C13 C12 H12 126.7 . . ?
N1 C13 C12 109.5(2) . . ?
N1 C13 C14 122.3(2) . . ?
C12 C13 C14 128.2(2) . . ?
C19 C14 C15 119.1(3) . . ?
C19 C14 C13 120.7(2) . . ?
C15 C14 C13 120.2(2) . . ?
C16 C15 C14 120.3(3) . . ?
C16 C15 H15 119.9 . . ?
C14 C15 H15 119.9 . . ?
C17 C16 C15 120.3(3) . . ?
C17 C16 H16 119.9 . . ?
C15 C16 H16 119.9 . . ?
C16 C17 C18 120.3(3) . . ?
C16 C17 H17 119.8 . . ?
C18 C17 H17 119.8 . . ?
C17 C18 C19 119.8(3) . . ?
C17 C18 H18 120.1 . . ?
C19 C18 H18 120.1 . . ?
C14 C19 C18 120.2(3) . . ?
C14 C19 H19 119.9 . . ?
C18 C19 H19 119.9 . . ?
C21 C20 H20A 109.5 . . ?
C21 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
C21 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
N4 C21 C22 107.8(2) . . ?
N4 C21 C20 122.8(2) . . ?
C22 C21 C20 129.4(2) . . ?
C21 C22 C23 106.5(2) . . ?
C21 C22 H22 126.8 . . ?
C23 C22 H22 126.8 . . ?
N3 C23 C22 109.6(2) . . ?
N3 C23 C24 122.4(2) . . ?
C22 C23 C24 127.9(2) . . ?
C25 C24 C29 118.8(2) . . ?
C25 C24 C23 119.7(2) . . ?
C29 C24 C23 121.5(2) . . ?
C24 C25 C26 120.4(3) . . ?
C24 C25 H25 119.8 . . ?
C26 C25 H25 119.8 . . ?
C27 C26 C25 120.2(3) . . ?
C27 C26 H26 119.9 . . ?
C25 C26 H26 119.9 . . ?
C26 C27 C28 119.9(3) . . ?
C26 C27 H27 120.0 . . ?
C28 C27 H27 120.0 . . ?
C29 C28 C27 119.7(3) . . ?
C29 C28 H28 120.1 . . ?
C27 C28 H28 120.1 . . ?
C28 C29 C24 120.9(3) . . ?
C28 C29 H29 119.5 . . ?
C24 C29 H29 119.5 . . ?
C31 C30 H30A 109.5 . . ?
C31 C30 H30B 109.5 . . ?
H30A C30 H30B 109.5 . . ?
C31 C30 H30C 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
N6 C31 C32 107.8(2) . . ?
N6 C31 C30 122.7(2) . . ?
C32 C31 C30 129.5(2) . . ?
C31 C32 C33 106.3(2) . . ?
C31 C32 H32 126.9 . . ?
C33 C32 H32 126.9 . . ?
N5 C33 C32 109.4(2) . . ?
N5 C33 C34 121.1(2) . . ?
C32 C33 C34 129.5(2) . . ?
C39 C34 C35 118.4(3) . . ?
C39 C34 C33 121.0(2) . . ?
C35 C34 C33 120.5(2) . . ?
C36 C35 C34 120.3(3) . . ?
C36 C35 H35 119.9 . . ?
C34 C35 H35 119.9 . . ?
C37 C36 C35 120.5(3) . . ?
C37 C36 H36 119.8 . . ?
C35 C36 H36 119.8 . . ?
C36 C37 C38 119.5(3) . . ?
C36 C37 H37 120.3 . . ?
C38 C37 H37 120.3 . . ?
C37 C38 C39 120.8(3) . . ?
C37 C38 H38 119.6 . . ?
C39 C38 H38 119.6 . . ?
C38 C39 C34 120.5(3) . . ?
C38 C39 H39 119.7 . . ?
C34 C39 H39 119.7 . . ?
C41 C40 H40A 109.5 . . ?
C41 C40 H40B 109.5 . . ?
H40A C40 H40B 109.5 . . ?
C41 C40 H40C 109.5 . . ?
H40A C40 H40C 109.5 . . ?
H40B C40 H40C 109.5 . . ?
C42 C41 C46 117.4(3) . . ?
C42 C41 C40 121.8(3) . . ?
C46 C41 C40 120.8(3) . . ?
C41 C42 C43 120.1(3) . . ?
C41 C42 H42 119.9 . . ?
C43 C42 H42 119.9 . . ?
C44 C43 C42 121.0(3) . . ?
C44 C43 H43 119.5 . . ?
C42 C43 H43 119.5 . . ?
C45 C44 C43 119.7(4) . . ?
C45 C44 H44 120.1 . . ?
C43 C44 H44 120.1 . . ?
C44 C45 C46 119.4(4) . . ?
C44 C45 H45 120.3 . . ?
C46 C45 H45 120.3 . . ?
C45 C46 C41 122.3(3) . . ?
C45 C46 H46 118.8 . . ?
C41 C46 H46 118.8 . . ?
C13 N1 N2 106.70(19) . . ?
C13 N1 Ni1 138.05(17) . . ?
N2 N1 Ni1 115.24(14) . . ?
C11 N2 N1 109.96(19) . . ?
C11 N2 B1 130.1(2) . . ?
N1 N2 B1 119.83(19) . . ?
C23 N3 N4 106.6(2) . . ?
C23 N3 Ni1 136.77(17) . . ?
N4 N3 Ni1 116.39(15) . . ?
C21 N4 N3 109.6(2) . . ?
C21 N4 B1 131.1(2) . . ?
N3 N4 B1 119.29(19) . . ?
C33 N5 N6 106.8(2) . . ?
C33 N5 Ni1 136.15(17) . . ?
N6 N5 Ni1 116.78(15) . . ?
C31 N6 N5 109.9(2) . . ?
C31 N6 B1 131.5(2) . . ?
N5 N6 B1 118.61(19) . . ?
C1 N7 C9 122.7(2) . . ?
C1 N7 Ni1 99.84(16) . . ?
C9 N7 Ni1 137.46(17) . . ?
C1 S1 Ni1 75.36(9) . . ?
C1 S2 C2 101.53(14) . . ?
N3 Ni1 N5 92.36(8) . . ?
N3 Ni1 N7 94.55(8) . . ?
N5 Ni1 N7 95.77(8) . . ?
N3 Ni1 N1 88.83(8) . . ?
N5 Ni1 N1 89.23(8) . . ?
N7 Ni1 N1 173.84(8) . . ?
N3 Ni1 S1 135.63(6) . . ?
N5 Ni1 S1 129.28(6) . . ?
N7 Ni1 S1 69.75(6) . . ?
N1 Ni1 S1 104.27(6) . . ?
N2 B1 N4 108.7(2) . . ?
N2 B1 N6 108.3(2) . . ?
N4 B1 N6 108.9(2) . . ?
N2 B1 H1 111.5(12) . . ?
N4 B1 H1 109.8(12) . . ?
N6 B1 H1 109.6(12) . . ?

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 1.000
_refine_diff_density_max         0.900
_refine_diff_density_min         -0.620
_refine_diff_density_rms         0.058
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent'
_solvent_exptl_crystal_recrystallization_method Hexanes
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_Complex_5a
_database_code_depnum_ccdc_archive 'CCDC 1476060'
_audit_update_record             
;
2016-05-13 deposited with the CCDC.
2016-06-21 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        'Complex 5a'
_chemical_name_common            'Complex 5a'
_chemical_melting_point          '448.4 - 449.7'
_chemical_formula_moiety         'C42 H44 B N7 Ni, C4 H10 O'
_chemical_formula_sum            'C46 H54 B N7 Ni O'
_chemical_formula_weight         790.48

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'
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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                   16.2356(14)
_cell_length_b                   10.7693(10)
_cell_length_c                   24.309(2)
_cell_angle_alpha                90.00
_cell_angle_beta                 91.729(4)
_cell_angle_gamma                90.00
_cell_volume                     4248.5(7)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9957
_cell_measurement_theta_min      2.41
_cell_measurement_theta_max      25.41

_exptl_crystal_description       rode
_exptl_crystal_colour            yellow-orange
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.15
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.236
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1680
_exptl_absorpt_coefficient_mu    0.500
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.8769
_exptl_absorpt_correction_T_max  0.9288
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean 8.366
_diffrn_reflns_number            65820
_diffrn_reflns_av_R_equivalents  0.0314
_diffrn_reflns_av_sigmaI/netI    0.0189
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_theta_min         1.49
_diffrn_reflns_theta_max         25.45
_reflns_number_total             7831
_reflns_number_gt                6886
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker APEX2 v.2011.4'
_computing_cell_refinement       'Bruker APEX2 v.2011.4'
_computing_data_reduction        'Bruker APEX2 v.2011.4'
_computing_structure_solution    SIR-92
_computing_structure_refinement  SHELXL-97
_computing_molecular_graphics    ORTEP-32
_computing_publication_material  WinGX

_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)+(0.0282P)²+3.6588P] 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         7831
_refine_ls_number_parameters     517
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0367
_refine_ls_R_factor_gt           0.0308
_refine_ls_wR_factor_ref         0.0759
_refine_ls_wR_factor_gt          0.0727
_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
C1 C 0.77758(10) 0.34107(15) 0.12928(7) 0.0158(3) Uani 1 1 d . . .
C2 C 0.75022(10) 0.45037(16) 0.16171(7) 0.0185(3) Uani 1 1 d . . .
H2A H 0.7850 0.5228 0.1528 0.022 Uiso 1 1 calc R . .
H2B H 0.7586 0.4323 0.2014 0.022 Uiso 1 1 calc R . .
C3 C 0.66072(10) 0.48363(15) 0.15055(7) 0.0179(3) Uani 1 1 d . . .
C4 C 0.63650(11) 0.53649(16) 0.10053(7) 0.0225(4) Uani 1 1 d . . .
H4 H 0.6760 0.5486 0.0730 0.027 Uiso 1 1 calc R . .
C5 C 0.55543(12) 0.57172(18) 0.09034(8) 0.0277(4) Uani 1 1 d . . .
H5 H 0.5396 0.6077 0.0559 0.033 Uiso 1 1 calc R . .
C6 C 0.49748(11) 0.55449(18) 0.13027(8) 0.0295(4) Uani 1 1 d . . .
H6 H 0.4421 0.5800 0.1236 0.035 Uiso 1 1 calc R . .
C7 C 0.52054(11) 0.50018(18) 0.17970(8) 0.0285(4) Uani 1 1 d . . .
H7 H 0.4806 0.4867 0.2069 0.034 Uiso 1 1 calc R . .
C8 C 0.60205(11) 0.46491(16) 0.19003(7) 0.0226(4) Uani 1 1 d . . .
H8 H 0.6175 0.4279 0.2243 0.027 Uiso 1 1 calc R . .
C9 C 0.89836(10) 0.38921(16) 0.06781(7) 0.0191(4) Uani 1 1 d . . .
C10 C 0.96393(11) 0.42980(18) 0.11014(8) 0.0289(4) Uani 1 1 d . . .
H10A H 0.9391 0.4845 0.1373 0.043 Uiso 1 1 calc R . .
H10B H 1.0078 0.4746 0.0916 0.043 Uiso 1 1 calc R . .
H10C H 0.9872 0.3565 0.1288 0.043 Uiso 1 1 calc R . .
C11 C 0.93363(11) 0.30093(17) 0.02552(8) 0.0245(4) Uani 1 1 d . . .
H11A H 0.9629 0.2330 0.0446 0.037 Uiso 1 1 calc R . .
H11B H 0.9720 0.3462 0.0025 0.037 Uiso 1 1 calc R . .
H11C H 0.8887 0.2668 0.0023 0.037 Uiso 1 1 calc R . .
C12 C 0.85801(11) 0.50082(16) 0.03915(8) 0.0243(4) Uani 1 1 d . . .
H12A H 0.8116 0.4726 0.0157 0.036 Uiso 1 1 calc R . .
H12B H 0.8985 0.5427 0.0165 0.036 Uiso 1 1 calc R . .
H12C H 0.8381 0.5588 0.0668 0.036 Uiso 1 1 calc R . .
C13 C 0.74258(11) -0.22418(16) -0.01940(7) 0.0225(4) Uani 1 1 d . . .
H13A H 0.7005 -0.2666 0.0017 0.034 Uiso 1 1 calc R . .
H13B H 0.7808 -0.2856 -0.0339 0.034 Uiso 1 1 calc R . .
H13C H 0.7160 -0.1787 -0.0500 0.034 Uiso 1 1 calc R . .
C14 C 0.78897(10) -0.13514(15) 0.01718(6) 0.0166(3) Uani 1 1 d . . .
C15 C 0.87075(10) -0.13642(15) 0.03439(7) 0.0176(3) Uani 1 1 d . . .
H15 H 0.9114 -0.1956 0.0249 0.021 Uiso 1 1 calc R . .
C16 C 0.88166(10) -0.03280(15) 0.06861(6) 0.0152(3) Uani 1 1 d . . .
C17 C 0.95595(10) 0.00838(15) 0.09962(7) 0.0162(3) Uani 1 1 d . . .
C18 C 1.03410(10) -0.00756(16) 0.07814(7) 0.0192(4) Uani 1 1 d . . .
H18 H 1.0396 -0.0485 0.0438 0.023 Uiso 1 1 calc R . .
C19 C 1.10353(10) 0.03565(17) 0.10637(8) 0.0234(4) Uani 1 1 d . . .
H19 H 1.1563 0.0252 0.0911 0.028 Uiso 1 1 calc R . .
C20 C 1.09648(11) 0.09425(18) 0.15684(8) 0.0261(4) Uani 1 1 d . . .
H20 H 1.1442 0.1243 0.1761 0.031 Uiso 1 1 calc R . .
C21 C 1.01936(11) 0.10872(17) 0.17908(8) 0.0247(4) Uani 1 1 d . . .
H21 H 1.0143 0.1485 0.2137 0.030 Uiso 1 1 calc R . .
C22 C 0.94990(10) 0.06534(16) 0.15100(7) 0.0197(4) Uani 1 1 d . . .
H22 H 0.8974 0.0743 0.1668 0.024 Uiso 1 1 calc R . .
C23 C 0.50513(11) -0.10182(17) 0.08904(7) 0.0234(4) Uani 1 1 d . . .
H23A H 0.4777 -0.0498 0.0609 0.035 Uiso 1 1 calc R . .
H23B H 0.4641 -0.1339 0.1142 0.035 Uiso 1 1 calc R . .
H23C H 0.5327 -0.1714 0.0713 0.035 Uiso 1 1 calc R . .
C24 C 0.56751(10) -0.02602(15) 0.12072(7) 0.0164(3) Uani 1 1 d . . .
C25 C 0.56814(10) 0.01054(15) 0.17491(7) 0.0174(3) Uani 1 1 d . . .
H25 H 0.5289 -0.0105 0.2016 0.021 Uiso 1 1 calc R . .
C26 C 0.63827(10) 0.08516(15) 0.18291(7) 0.0149(3) Uani 1 1 d . . .
C27 C 0.66507(10) 0.15113(15) 0.23346(7) 0.0156(3) Uani 1 1 d . . .
C28 C 0.60643(10) 0.18346(15) 0.27200(7) 0.0189(4) Uani 1 1 d . . .
H28 H 0.5505 0.1601 0.2658 0.023 Uiso 1 1 calc R . .
C29 C 0.62900(11) 0.24921(16) 0.31920(7) 0.0221(4) Uani 1 1 d . . .
H29 H 0.5885 0.2700 0.3451 0.027 Uiso 1 1 calc R . .
C30 C 0.71031(11) 0.28467(16) 0.32881(7) 0.0225(4) Uani 1 1 d . . .
H30 H 0.7254 0.3317 0.3606 0.027 Uiso 1 1 calc R . .
C31 C 0.76947(11) 0.25084(16) 0.29163(7) 0.0210(4) Uani 1 1 d . . .
H31 H 0.8254 0.2735 0.2983 0.025 Uiso 1 1 calc R . .
C32 C 0.74710(10) 0.18392(15) 0.24466(7) 0.0174(3) Uani 1 1 d . . .
H32 H 0.7882 0.1601 0.2198 0.021 Uiso 1 1 calc R . .
C33 C 0.54268(10) 0.24666(16) 0.05595(7) 0.0209(4) Uani 1 1 d . . .
H33A H 0.5075 0.1742 0.0487 0.031 Uiso 1 1 calc R . .
H33B H 0.5105 0.3227 0.0500 0.031 Uiso 1 1 calc R . .
H33C H 0.5638 0.2440 0.0941 0.031 Uiso 1 1 calc R . .
C34 C 0.61339(10) 0.24524(15) 0.01773(7) 0.0166(3) Uani 1 1 d . . .
C35 C 0.63835(10) 0.33738(16) -0.01707(7) 0.0178(3) Uani 1 1 d . . .
H35 H 0.6151 0.4178 -0.0215 0.021 Uiso 1 1 calc R . .
C36 C 0.70557(10) 0.28762(16) -0.04477(7) 0.0169(3) Uani 1 1 d . . .
C37 C 0.75580(10) 0.34555(16) -0.08732(7) 0.0179(3) Uani 1 1 d . . .
C38 C 0.73984(11) 0.46584(17) -0.10615(7) 0.0234(4) Uani 1 1 d . . .
H38 H 0.6967 0.5127 -0.0907 0.028 Uiso 1 1 calc R . .
C39 C 0.78648(12) 0.51769(18) -0.14732(8) 0.0292(4) Uani 1 1 d . . .
H39 H 0.7748 0.5995 -0.1599 0.035 Uiso 1 1 calc R . .
C40 C 0.84974(12) 0.45119(19) -0.17014(8) 0.0294(4) Uani 1 1 d . . .
H40 H 0.8810 0.4866 -0.1986 0.035 Uiso 1 1 calc R . .
C41 C 0.86714(11) 0.33267(18) -0.15125(8) 0.0271(4) Uani 1 1 d . . .
H41 H 0.9109 0.2868 -0.1665 0.033 Uiso 1 1 calc R . .
C42 C 0.82104(11) 0.28037(17) -0.11005(7) 0.0229(4) Uani 1 1 d . . .
H42 H 0.8340 0.1992 -0.0971 0.028 Uiso 1 1 calc R . .
C43 C 0.65072(14) 0.21081(19) -0.21347(8) 0.0343(5) Uani 1 1 d . . .
H43A H 0.6475 0.1936 -0.2531 0.051 Uiso 1 1 calc R . .
H43B H 0.6868 0.2824 -0.2065 0.051 Uiso 1 1 calc R . .
H43C H 0.5955 0.2291 -0.2005 0.051 Uiso 1 1 calc R . .
C44 C 0.68482(12) 0.10008(19) -0.18364(9) 0.0347(5) Uani 1 1 d . . .
H44A H 0.7412 0.0825 -0.1960 0.042 Uiso 1 1 calc R . .
H44B H 0.6879 0.1170 -0.1436 0.042 Uiso 1 1 calc R . .
C45 C 0.65585(16) -0.1077(2) -0.16226(13) 0.0620(8) Uani 1 1 d . . .
H45A H 0.6452 -0.0900 -0.1232 0.074 Uiso 1 1 calc R . .
H45B H 0.7156 -0.1234 -0.1655 0.074 Uiso 1 1 calc R . .
C46 C 0.60894(13) -0.2205(2) -0.17993(10) 0.0386(5) Uani 1 1 d . . .
H46A H 0.5498 -0.2056 -0.1762 0.058 Uiso 1 1 calc R . .
H46B H 0.6259 -0.2910 -0.1567 0.058 Uiso 1 1 calc R . .
H46C H 0.6203 -0.2392 -0.2184 0.058 Uiso 1 1 calc R . .
N7 N 0.83349(8) 0.31917(12) 0.09652(6) 0.0154(3) Uani 1 1 d . . .
N1 N 0.81033(8) 0.02896(12) 0.07163(5) 0.0144(3) Uani 1 1 d . . .
N2 N 0.75345(8) -0.03452(12) 0.03998(5) 0.0147(3) Uani 1 1 d . . .
N4 N 0.63486(8) 0.02351(12) 0.09737(5) 0.0143(3) Uani 1 1 d . . .
N3 N 0.67877(8) 0.09258(12) 0.13560(5) 0.0140(3) Uani 1 1 d . . .
N6 N 0.66483(8) 0.14649(13) 0.01131(5) 0.0150(3) Uani 1 1 d . . .
N5 N 0.72141(8) 0.17168(13) -0.02783(6) 0.0167(3) Uani 1 1 d . . .
O1 O 0.63325(7) -0.00432(12) -0.19438(5) 0.0251(3) Uani 1 1 d . . .
Ni1 Ni 0.772829(12) 0.177283(18) 0.109198(8) 0.01287(6) Uani 1 1 d . . .
B1 B 0.66414(11) 0.01453(17) 0.03730(8) 0.0153(4) Uani 1 1 d . . .
H1 H 0.6245(10) -0.0501(16) 0.0134(7) 0.011(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
C1 N7 1.248(2) . ?
C1 C2 1.492(2) . ?
C1 Ni1 1.8312(16) . ?
C2 C3 1.513(2) . ?
C3 C8 1.387(2) . ?
C3 C4 1.389(2) . ?
C4 C5 1.385(3) . ?
C5 C6 1.385(3) . ?
C6 C7 1.378(3) . ?
C7 C8 1.392(3) . ?
C9 N7 1.486(2) . ?
C9 C10 1.522(2) . ?
C9 C11 1.525(2) . ?
C9 C12 1.527(2) . ?
C13 C14 1.496(2) . ?
C14 N2 1.354(2) . ?
C14 C15 1.380(2) . ?
C15 C16 1.400(2) . ?
C16 N1 1.339(2) . ?
C16 C17 1.471(2) . ?
C17 C18 1.397(2) . ?
C17 C22 1.398(2) . ?
C18 C19 1.383(3) . ?
C19 C20 1.388(3) . ?
C20 C21 1.388(3) . ?
C21 C22 1.382(2) . ?
C23 C24 1.496(2) . ?
C24 N4 1.356(2) . ?
C24 C25 1.375(2) . ?
C25 C26 1.402(2) . ?
C26 N3 1.344(2) . ?
C26 C27 1.474(2) . ?
C27 C32 1.397(2) . ?
C27 C28 1.400(2) . ?
C28 C29 1.388(2) . ?
C29 C30 1.387(3) . ?
C30 C31 1.387(2) . ?
C31 C32 1.389(2) . ?
C33 C34 1.499(2) . ?
C34 N6 1.364(2) . ?
C34 C35 1.373(2) . ?
C35 C36 1.406(2) . ?
C36 N5 1.337(2) . ?
C36 C37 1.475(2) . ?
C37 C38 1.396(2) . ?
C37 C42 1.398(2) . ?
C38 C39 1.390(3) . ?
C39 C40 1.382(3) . ?
C40 C41 1.383(3) . ?
C41 C42 1.388(3) . ?
C43 C44 1.493(3) . ?
C44 O1 1.421(2) . ?
C45 O1 1.402(3) . ?
C45 C46 1.490(3) . ?
N7 Ni1 1.8487(13) . ?
N1 N2 1.3672(19) . ?
N1 Ni1 1.9468(13) . ?
N2 B1 1.543(2) . ?
N4 N3 1.3731(18) . ?
N4 B1 1.552(2) . ?
N3 Ni1 1.9066(13) . ?
N6 N5 1.3696(18) . ?
N6 B1 1.555(2) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N7 C1 C2 136.07(15) . . ?
N7 C1 Ni1 70.94(10) . . ?
C2 C1 Ni1 152.89(13) . . ?
C1 C2 C3 113.06(14) . . ?
C8 C3 C4 118.89(16) . . ?
C8 C3 C2 121.16(16) . . ?
C4 C3 C2 119.94(15) . . ?
C5 C4 C3 120.76(17) . . ?
C6 C5 C4 120.01(18) . . ?
C7 C6 C5 119.71(17) . . ?
C6 C7 C8 120.32(17) . . ?
C3 C8 C7 120.30(17) . . ?
N7 C9 C10 108.62(14) . . ?
N7 C9 C11 106.62(13) . . ?
C10 C9 C11 111.45(15) . . ?
N7 C9 C12 108.27(13) . . ?
C10 C9 C12 111.35(15) . . ?
C11 C9 C12 110.35(15) . . ?
N2 C14 C15 107.56(14) . . ?
N2 C14 C13 122.92(15) . . ?
C15 C14 C13 129.52(15) . . ?
C14 C15 C16 106.00(14) . . ?
N1 C16 C15 109.52(14) . . ?
N1 C16 C17 121.27(14) . . ?
C15 C16 C17 129.18(15) . . ?
C18 C17 C22 118.49(15) . . ?
C18 C17 C16 120.75(15) . . ?
C22 C17 C16 120.76(14) . . ?
C19 C18 C17 120.61(16) . . ?
C18 C19 C20 120.28(16) . . ?
C21 C20 C19 119.68(17) . . ?
C22 C21 C20 120.14(17) . . ?
C21 C22 C17 120.76(15) . . ?
N4 C24 C25 107.80(14) . . ?
N4 C24 C23 122.74(15) . . ?
C25 C24 C23 129.41(15) . . ?
C24 C25 C26 106.23(14) . . ?
N3 C26 C25 109.36(14) . . ?
N3 C26 C27 123.03(14) . . ?
C25 C26 C27 127.58(14) . . ?
C32 C27 C28 118.07(15) . . ?
C32 C27 C26 122.70(14) . . ?
C28 C27 C26 119.23(15) . . ?
C29 C28 C27 120.81(16) . . ?
C30 C29 C28 120.38(16) . . ?
C31 C30 C29 119.47(16) . . ?
C30 C31 C32 120.18(16) . . ?
C31 C32 C27 121.03(16) . . ?
N6 C34 C35 107.45(14) . . ?
N6 C34 C33 124.20(15) . . ?
C35 C34 C33 128.35(15) . . ?
C34 C35 C36 105.52(15) . . ?
N5 C36 C35 110.69(14) . . ?
N5 C36 C37 120.37(15) . . ?
C35 C36 C37 128.94(15) . . ?
C38 C37 C42 118.14(16) . . ?
C38 C37 C36 121.44(16) . . ?
C42 C37 C36 120.42(15) . . ?
C39 C38 C37 120.62(17) . . ?
C40 C39 C38 120.56(18) . . ?
C39 C40 C41 119.46(17) . . ?
C40 C41 C42 120.34(18) . . ?
C41 C42 C37 120.86(17) . . ?
O1 C44 C43 109.56(16) . . ?
O1 C45 C46 111.34(19) . . ?
C1 N7 C9 137.99(15) . . ?
C1 N7 Ni1 69.42(10) . . ?
C9 N7 Ni1 152.40(11) . . ?
C16 N1 N2 106.94(13) . . ?
C16 N1 Ni1 135.75(11) . . ?
N2 N1 Ni1 117.31(10) . . ?
C14 N2 N1 109.98(13) . . ?
C14 N2 B1 131.92(14) . . ?
N1 N2 B1 118.07(13) . . ?
C24 N4 N3 109.78(13) . . ?
C24 N4 B1 130.01(13) . . ?
N3 N4 B1 120.20(12) . . ?
C26 N3 N4 106.83(13) . . ?
C26 N3 Ni1 137.21(11) . . ?
N4 N3 Ni1 115.85(10) . . ?
C34 N6 N5 110.54(13) . . ?
C34 N6 B1 130.83(13) . . ?
N5 N6 B1 118.45(13) . . ?
C36 N5 N6 105.79(13) . . ?
C45 O1 C44 112.51(15) . . ?
C1 Ni1 N7 39.64(7) . . ?
C1 Ni1 N3 113.50(6) . . ?
N7 Ni1 N3 152.58(6) . . ?
C1 Ni1 N1 154.71(6) . . ?
N7 Ni1 N1 115.10(6) . . ?
N3 Ni1 N1 91.74(6) . . ?
N2 B1 N4 107.20(13) . . ?
N2 B1 N6 108.16(13) . . ?
N4 B1 N6 109.35(13) . . ?

_diffrn_measured_fraction_theta_max 0.996
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 1.000
_refine_diff_density_max         0.629
_refine_diff_density_min         -0.562
_refine_diff_density_rms         0.045
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent'
_solvent_exptl_crystal_recrystallization_method Hexanes
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_Complex_3
_database_code_depnum_ccdc_archive 'CCDC 1476061'
_audit_update_record             
;
2016-05-13 deposited with the CCDC.
2016-06-21 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        'Complex 3'
_chemical_name_common            'Complex 3'
_chemical_melting_point          '433.2 (dec.)'
_chemical_formula_moiety         'C39 H38 B N7 Ni'
_chemical_formula_sum            'C39 H38 B N7 Ni'
_chemical_formula_weight         674.28

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'
C C 0.0033 0.0016 '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'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Orthorhombic
_symmetry_space_group_name_H-M   Pbca

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

_cell_length_a                   11.0031(10)
_cell_length_b                   22.283(2)
_cell_length_c                   28.239(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     6923.6(11)
_cell_formula_units_Z            8
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9399
_cell_measurement_theta_min      2.19
_cell_measurement_theta_max      25.35

_exptl_crystal_description       rode
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.30
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.294
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2832
_exptl_absorpt_coefficient_mu    0.599
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.7955
_exptl_absorpt_correction_T_max  0.8407
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean 8.366
_diffrn_reflns_number            114898
_diffrn_reflns_av_R_equivalents  0.0363
_diffrn_reflns_av_sigmaI/netI    0.0127
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_theta_min         1.83
_diffrn_reflns_theta_max         25.37
_reflns_number_total             6355
_reflns_number_gt                5646
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker APEX2 v.2011.4'
_computing_cell_refinement       'Bruker APEX2 v.2011.4'
_computing_data_reduction        'Bruker APEX2 v.2011.4'
_computing_structure_solution    SIR-92
_computing_structure_refinement  SHELXL-97
_computing_molecular_graphics    ORTEP-32
_computing_publication_material  WinGX

_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)+(0.0571P)²+7.2977P] 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         6355
_refine_ls_number_parameters     441
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0331
_refine_ls_R_factor_gt           0.0280
_refine_ls_wR_factor_ref         0.0835
_refine_ls_wR_factor_gt          0.0778
_refine_ls_goodness_of_fit_ref   0.824
_refine_ls_restrained_S_all      0.824
_refine_ls_shift/su_max          0.032
_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
C9 C -0.08450(18) 0.20683(8) 0.69972(6) 0.0291(4) Uani 1 1 d . . .
H1A H -0.0100 0.2076 0.7174 0.044 Uiso 1 1 calc R . .
H1B H -0.1406 0.1796 0.7145 0.044 Uiso 1 1 calc R . .
H1C H -0.1191 0.2464 0.6990 0.044 Uiso 1 1 calc R . .
C1 C -0.05685(15) 0.20933(7) 0.61098(5) 0.0192(3) Uani 1 1 d . . .
C2 C -0.07481(17) 0.27005(7) 0.58933(6) 0.0259(4) Uani 1 1 d . . .
H2A H -0.1431 0.2678 0.5677 0.031 Uiso 1 1 calc R . .
H2B H -0.0033 0.2796 0.5707 0.031 Uiso 1 1 calc R . .
C3 C -0.09738(16) 0.32139(7) 0.62323(6) 0.0224(3) Uani 1 1 d . . .
C4 C -0.00147(16) 0.34742(8) 0.64754(7) 0.0275(4) Uani 1 1 d . . .
H4 H 0.0769 0.3328 0.6431 0.033 Uiso 1 1 calc R . .
C5 C -0.02043(17) 0.39484(8) 0.67837(7) 0.0304(4) Uani 1 1 d . . .
H5 H 0.0448 0.4114 0.6947 0.036 Uiso 1 1 calc R . .
C6 C -0.13612(19) 0.41766(8) 0.68494(7) 0.0340(4) Uani 1 1 d . . .
H6 H -0.1491 0.4497 0.7054 0.041 Uiso 1 1 calc R . .
C7 C -0.23190(19) 0.39219(9) 0.66078(8) 0.0402(5) Uani 1 1 d . . .
H7 H -0.3100 0.4072 0.6650 0.048 Uiso 1 1 calc R . .
C8 C -0.21326(17) 0.34424(9) 0.63007(7) 0.0333(4) Uani 1 1 d . . .
H8 H -0.2788 0.3274 0.6141 0.040 Uiso 1 1 calc R . .
C11 C 0.21381(15) -0.07955(8) 0.62615(6) 0.0251(4) Uani 1 1 d . . .
H11A H 0.2068 -0.0920 0.5937 0.038 Uiso 1 1 calc R . .
H11B H 0.2051 -0.1138 0.6465 0.038 Uiso 1 1 calc R . .
H11C H 0.2920 -0.0616 0.6312 0.038 Uiso 1 1 calc R . .
C12 C 0.11645(14) -0.03484(7) 0.63721(5) 0.0187(3) Uani 1 1 d . . .
C13 C 0.03453(14) -0.03386(7) 0.67392(5) 0.0183(3) Uani 1 1 d . . .
H13 H 0.0253 -0.0626 0.6975 0.022 Uiso 1 1 calc R . .
C14 C -0.03220(13) 0.01914(7) 0.66857(5) 0.0165(3) Uani 1 1 d . . .
C15 C -0.12996(14) 0.04192(7) 0.69935(5) 0.0170(3) Uani 1 1 d . . .
C16 C -0.23372(14) 0.07004(7) 0.68153(5) 0.0202(3) Uani 1 1 d . . .
H16 H -0.2433 0.0746 0.6490 0.024 Uiso 1 1 calc R . .
C17 C -0.32283(15) 0.09125(7) 0.71213(6) 0.0239(3) Uani 1 1 d . . .
H17 H -0.3916 0.1100 0.6999 0.029 Uiso 1 1 calc R . .
C18 C -0.31001(15) 0.08472(7) 0.76073(6) 0.0246(4) Uani 1 1 d . . .
H18 H -0.3692 0.0997 0.7811 0.030 Uiso 1 1 calc R . .
C19 C -0.20835(15) 0.05576(7) 0.77880(6) 0.0231(3) Uani 1 1 d . . .
H19 H -0.2000 0.0506 0.8113 0.028 Uiso 1 1 calc R . .
C20 C -0.11931(14) 0.03462(7) 0.74839(6) 0.0203(3) Uani 1 1 d . . .
H20 H -0.0514 0.0153 0.7607 0.024 Uiso 1 1 calc R . .
C21 C 0.20221(15) 0.02586(8) 0.45952(6) 0.0249(4) Uani 1 1 d . . .
H21A H 0.2819 0.0414 0.4659 0.037 Uiso 1 1 calc R . .
H21B H 0.1877 0.0262 0.4260 0.037 Uiso 1 1 calc R . .
H21C H 0.1966 -0.0146 0.4711 0.037 Uiso 1 1 calc R . .
C22 C 0.10943(14) 0.06398(7) 0.48379(5) 0.0181(3) Uani 1 1 d . . .
C23 C 0.02089(14) 0.09952(7) 0.46378(5) 0.0183(3) Uani 1 1 d . . .
H23 H 0.0066 0.1055 0.4317 0.022 Uiso 1 1 calc R . .
C24 C -0.04309(14) 0.12475(7) 0.50157(5) 0.0159(3) Uani 1 1 d . . .
C25 C -0.14863(13) 0.16546(7) 0.49991(5) 0.0162(3) Uani 1 1 d . . .
C26 C -0.15158(14) 0.21210(7) 0.46686(5) 0.0211(3) Uani 1 1 d . . .
H26 H -0.0886 0.2160 0.4451 0.025 Uiso 1 1 calc R . .
C27 C -0.24716(15) 0.25257(8) 0.46610(6) 0.0247(3) Uani 1 1 d . . .
H27 H -0.2476 0.2838 0.4442 0.030 Uiso 1 1 calc R . .
C28 C -0.34218(15) 0.24647(8) 0.49798(6) 0.0252(4) Uani 1 1 d . . .
H28 H -0.4052 0.2743 0.4982 0.030 Uiso 1 1 calc R . .
C29 C -0.34321(15) 0.19888(8) 0.52955(6) 0.0246(3) Uani 1 1 d . . .
H29 H -0.4086 0.1939 0.5500 0.030 Uiso 1 1 calc R . .
C30 C -0.24699(14) 0.15870(7) 0.53069(5) 0.0201(3) Uani 1 1 d . . .
H30 H -0.2480 0.1270 0.5521 0.024 Uiso 1 1 calc R . .
C31 C 0.46464(18) 0.01664(12) 0.56319(8) 0.0494(6) Uani 1 1 d . . .
H31A H 0.4500 -0.0192 0.5812 0.074 Uiso 1 1 calc R . .
H31B H 0.5505 0.0238 0.5613 0.074 Uiso 1 1 calc R . .
H31C H 0.4322 0.0119 0.5319 0.074 Uiso 1 1 calc R . .
C32 C 0.40430(15) 0.06860(9) 0.58694(6) 0.0310(4) Uani 1 1 d . . .
C33 C 0.45699(17) 0.11529(10) 0.61133(6) 0.0332(4) Uani 1 1 d . . .
H33 H 0.5396 0.1219 0.6161 0.040 Uiso 1 1 calc R . .
C34 C 0.36063(16) 0.15086(8) 0.62747(6) 0.0258(4) Uani 1 1 d . . .
C35 C 0.36457(17) 0.20566(8) 0.65651(6) 0.0311(4) Uani 1 1 d . . .
C36 C 0.4743(2) 0.23633(10) 0.66360(7) 0.0420(5) Uani 1 1 d . . .
H36 H 0.5452 0.2227 0.6492 0.050 Uiso 1 1 calc R . .
C37 C 0.4772(2) 0.28727(10) 0.69225(8) 0.0513(7) Uani 1 1 d . . .
H37 H 0.5501 0.3075 0.6968 0.062 Uiso 1 1 calc R . .
C38 C 0.3733(3) 0.30795(9) 0.71391(7) 0.0499(6) Uani 1 1 d . . .
H38 H 0.3762 0.3417 0.7333 0.060 Uiso 1 1 calc R . .
C39 C 0.2645(2) 0.27821(9) 0.70674(7) 0.0435(5) Uani 1 1 d . . .
H39 H 0.1940 0.2921 0.7212 0.052 Uiso 1 1 calc R . .
C40 C 0.26017(19) 0.22762(8) 0.67789(6) 0.0337(4) Uani 1 1 d . . .
H40 H 0.1864 0.2083 0.6729 0.040 Uiso 1 1 calc R . .
N7 N -0.05995(12) 0.18689(6) 0.65141(5) 0.0205(3) Uani 1 1 d . . .
N1 N 0.00774(11) 0.04928(6) 0.63046(4) 0.0161(3) Uani 1 1 d . . .
N2 N 0.09880(11) 0.01531(6) 0.61092(4) 0.0162(3) Uani 1 1 d . . .
N3 N 0.00595(11) 0.10645(6) 0.54263(4) 0.0155(3) Uani 1 1 d . . .
N4 N 0.09962(11) 0.06849(6) 0.53149(4) 0.0162(3) Uani 1 1 d . . .
N5 N 0.25337(13) 0.12783(6) 0.61365(5) 0.0219(3) Uani 1 1 d . . .
N6 N 0.28114(12) 0.07741(6) 0.58848(4) 0.0214(3) Uani 1 1 d . . .
Ni01 Ni -0.021961(18) 0.129389(8) 0.606255(6) 0.01575(8) Uani 1 1 d . . .
B1 B 0.17895(16) 0.03676(8) 0.56923(6) 0.0186(4) Uani 1 1 d . . .
H1 H 0.2219(15) -0.0032(8) 0.5538(6) 0.018(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
C9 N7 1.460(2) . ?
C1 N7 1.247(2) . ?
C1 C2 1.498(2) . ?
C1 Ni01 1.8271(16) . ?
C2 C3 1.512(2) . ?
C3 C8 1.387(2) . ?
C3 C4 1.386(2) . ?
C4 C5 1.385(3) . ?
C5 C6 1.383(3) . ?
C6 C7 1.378(3) . ?
C7 C8 1.391(3) . ?
C11 C12 1.496(2) . ?
C12 N2 1.356(2) . ?
C12 C13 1.374(2) . ?
C13 C14 1.399(2) . ?
C14 N1 1.343(2) . ?
C14 C15 1.473(2) . ?
C15 C16 1.396(2) . ?
C15 C20 1.399(2) . ?
C16 C17 1.390(2) . ?
C17 C18 1.387(2) . ?
C18 C19 1.389(2) . ?
C19 C20 1.385(2) . ?
C21 C22 1.494(2) . ?
C22 N4 1.3550(19) . ?
C22 C23 1.377(2) . ?
C23 C24 1.397(2) . ?
C24 N3 1.342(2) . ?
C24 C25 1.474(2) . ?
C25 C30 1.396(2) . ?
C25 C26 1.397(2) . ?
C26 C27 1.386(2) . ?
C27 C28 1.386(2) . ?
C28 C29 1.385(2) . ?
C29 C30 1.387(2) . ?
C31 C32 1.494(3) . ?
C32 N6 1.370(2) . ?
C32 C33 1.376(3) . ?
C33 C34 1.400(3) . ?
C34 N5 1.345(2) . ?
C34 C35 1.472(3) . ?
C35 C40 1.387(3) . ?
C35 C36 1.402(3) . ?
C36 C37 1.394(3) . ?
C37 C38 1.376(4) . ?
C38 C39 1.383(3) . ?
C39 C40 1.392(3) . ?
N7 Ni01 1.8554(13) . ?
N1 N2 1.3716(18) . ?
N1 Ni01 1.9392(13) . ?
N2 B1 1.547(2) . ?
N3 N4 1.3699(17) . ?
N3 Ni01 1.8932(13) . ?
N4 B1 1.549(2) . ?
N5 N6 1.3642(19) . ?
N6 B1 1.543(2) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N7 C1 C2 137.09(15) . . ?
N7 C1 Ni01 71.44(10) . . ?
C2 C1 Ni01 151.47(12) . . ?
C1 C2 C3 116.52(14) . . ?
C8 C3 C4 118.52(16) . . ?
C8 C3 C2 121.14(16) . . ?
C4 C3 C2 120.33(15) . . ?
C3 C4 C5 121.06(17) . . ?
C6 C5 C4 120.23(17) . . ?
C7 C6 C5 119.08(17) . . ?
C6 C7 C8 120.82(18) . . ?
C3 C8 C7 120.29(18) . . ?
N2 C12 C13 107.82(13) . . ?
N2 C12 C11 122.50(14) . . ?
C13 C12 C11 129.64(14) . . ?
C12 C13 C14 106.04(14) . . ?
N1 C14 C13 109.71(13) . . ?
N1 C14 C15 122.66(14) . . ?
C13 C14 C15 127.62(14) . . ?
C16 C15 C20 118.52(14) . . ?
C16 C15 C14 122.62(13) . . ?
C20 C15 C14 118.86(14) . . ?
C17 C16 C15 120.36(14) . . ?
C18 C17 C16 120.51(16) . . ?
C17 C18 C19 119.62(15) . . ?
C20 C19 C18 119.99(15) . . ?
C19 C20 C15 120.98(15) . . ?
N4 C22 C23 107.99(13) . . ?
N4 C22 C21 123.53(14) . . ?
C23 C22 C21 128.48(14) . . ?
C22 C23 C24 105.94(13) . . ?
N3 C24 C23 109.58(13) . . ?
N3 C24 C25 122.08(13) . . ?
C23 C24 C25 128.34(14) . . ?
C30 C25 C26 118.57(14) . . ?
C30 C25 C24 121.62(14) . . ?
C26 C25 C24 119.81(14) . . ?
C27 C26 C25 120.80(15) . . ?
C28 C27 C26 119.91(15) . . ?
C27 C28 C29 119.94(15) . . ?
C30 C29 C28 120.19(15) . . ?
C29 C30 C25 120.49(14) . . ?
N6 C32 C33 107.02(17) . . ?
N6 C32 C31 124.40(18) . . ?
C33 C32 C31 128.58(17) . . ?
C32 C33 C34 105.78(16) . . ?
N5 C34 C33 110.74(16) . . ?
N5 C34 C35 120.28(16) . . ?
C33 C34 C35 128.97(16) . . ?
C40 C35 C36 118.64(19) . . ?
C40 C35 C34 120.73(16) . . ?
C36 C35 C34 120.63(19) . . ?
C37 C36 C35 119.9(2) . . ?
C38 C37 C36 120.8(2) . . ?
C37 C38 C39 119.6(2) . . ?
C38 C39 C40 120.2(2) . . ?
C35 C40 C39 120.82(19) . . ?
C1 N7 C9 137.62(15) . . ?
C1 N7 Ni01 68.99(9) . . ?
C9 N7 Ni01 153.39(12) . . ?
C14 N1 N2 106.59(12) . . ?
C14 N1 Ni01 133.46(11) . . ?
N2 N1 Ni01 119.30(10) . . ?
C12 N2 N1 109.84(12) . . ?
C12 N2 B1 126.15(13) . . ?
N1 N2 B1 123.51(12) . . ?
C24 N3 N4 106.96(12) . . ?
C24 N3 Ni01 132.26(11) . . ?
N4 N3 Ni01 120.44(9) . . ?
C22 N4 N3 109.51(12) . . ?
C22 N4 B1 127.27(13) . . ?
N3 N4 B1 123.23(12) . . ?
C34 N5 N6 105.60(14) . . ?
N5 N6 C32 110.86(14) . . ?
N5 N6 B1 120.25(12) . . ?
C32 N6 B1 128.73(15) . . ?
C1 Ni01 N7 39.57(6) . . ?
C1 Ni01 N3 111.51(6) . . ?
N7 Ni01 N3 151.08(6) . . ?
C1 Ni01 N1 155.11(6) . . ?
N7 Ni01 N1 115.56(6) . . ?
N3 Ni01 N1 93.36(5) . . ?
N6 B1 N4 112.65(13) . . ?
N6 B1 N2 109.21(12) . . ?
N4 B1 N2 110.10(12) . . ?

_diffrn_measured_fraction_theta_max 1.000
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 1.000
_refine_diff_density_max         0.638
_refine_diff_density_min         -0.386
_refine_diff_density_rms         0.043
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent'
_solvent_exptl_crystal_recrystallization_method Toluene/Hexanes
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_Complex_5b
_database_code_depnum_ccdc_archive 'CCDC 1476064'
_audit_update_record             
;
2016-06-07 deposited with the CCDC.
2016-06-21 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_CHEMW03_Complex_5b          
;
PROBLEM: WARNING: The ratio of given/expected molecular weight as
RESPONSE: The solvent-mask program of Olex was used to refine the solvent disorder. Such refinement automatically result in a discrepancy between the given and expected molecular weight.
;
# Added during the CSD deposition process: Tuesday 07 June 2016 04:20 PM
# end Validation Reply Form

_audit_creation_date             2016-06-07
_audit_creation_method           
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_shelxl_version_number           2014/6
_chemical_name_common            ?
_chemical_name_systematic        'Conplex 5b'
_chemical_formula_moiety         'C39 H48 B N7 Ni Si, C3.84 H8.96'
_chemical_formula_sum            'C42.84 H56.96 B N7 Ni Si'
_chemical_formula_weight         767.60
_chemical_melting_point          '478.9 - 479.9'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 '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'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/n 1'
_space_group_name_Hall           '-P 2yn'
loop_
_space_group_symop_operation_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                   13.930(3)
_cell_length_b                   11.256(3)
_cell_length_c                   26.727(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 96.631(19)
_cell_angle_gamma                90.00
_cell_volume                     4162.6(9)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    9799
_cell_measurement_temperature    100(2)
_cell_measurement_theta_min      2.33
_cell_measurement_theta_max      25.41
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    0.532
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.6837
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.0977 before and 0.0428 after correction.
The Ratio of minimum to maximum transmission is 0.9175.
The λ/2 correction factor is 0.0000.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.225
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1640
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.07
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0413
_diffrn_reflns_av_unetI/netI     0.0330
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            45312
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.431
_diffrn_reflns_theta_min         1.534
_diffrn_reflns_v_R_equivalents   ?
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.366
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                6314
_reflns_number_total             7674
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_data_collection       'Bruker APEX2 v.2011.4'
_computing_cell_refinement       'Bruker APEX2 v.2011.4'
_computing_data_reduction        'Bruker APEX2 v.2011.4'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_refine_diff_density_max         0.268
_refine_diff_density_min         -0.247
_refine_diff_density_rms         0.046
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     463
_refine_ls_number_reflns         7674
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0426
_refine_ls_R_factor_gt           0.0316
_refine_ls_restrained_S_all      1.055
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0310P)²+1.7504P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0728
_refine_ls_wR_factor_ref         0.0759
_refine_special_details          ', SQUEEZE'
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C1AA(H1AA,H1AB)
2.b Aromatic/amide H refined with riding coordinates:
 C12(H12), C15(H15), C16(H16), C17(H17), C18(H18), C19(H19), C22(H22),
 C25(H25), C26(H26), C27(H27), C28(H28), C29(H29), C32(H32), C35(H35), C36(H36),
  C37(H37), C38(H38), C39(H39)
2.c Idealised Me refined as rotating group:
 C2AA(H2AA,H2AB,H2AC), C3AA(H3AA,H3AB,H3AC), C4AA(H4AA,H4AB,H4AC), C7(H7A,H7B,
 H7C), C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C10(H10A,H10B,H10C), C20(H20A,H20B,
 H20C)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C0AA C 0.75629(12) 0.29124(16) 0.14730(6) 0.0189(4) Uani 1 1 d . . . . .
C1AA C 0.80918(12) 0.38079(17) 0.18010(6) 0.0204(4) Uani 1 1 d . . . . .
H1AA H 0.8167 0.3512 0.2144 0.024 Uiso 1 1 calc R . . . .
H1AB H 0.7704 0.4525 0.1795 0.024 Uiso 1 1 calc R . . . .
C2AA C 0.91724(15) 0.5029(2) 0.10150(7) 0.0323(5) Uani 1 1 d . . . . .
H2AA H 0.9791 0.5299 0.0937 0.048 Uiso 1 1 calc GR . . . .
H2AB H 0.8756 0.5700 0.1043 0.048 Uiso 1 1 calc GR . . . .
H2AC H 0.8890 0.4513 0.0752 0.048 Uiso 1 1 calc GR . . . .
C3AA C 0.99123(14) 0.51460(18) 0.21422(7) 0.0282(4) Uani 1 1 d . . . . .
H3AA H 0.9968 0.4703 0.2451 0.042 Uiso 1 1 calc GR . . . .
H3AB H 0.9528 0.5843 0.2176 0.042 Uiso 1 1 calc GR . . . .
H3AC H 1.0544 0.5377 0.2068 0.042 Uiso 1 1 calc GR . . . .
C4AA C 1.00536(14) 0.28490(19) 0.15605(7) 0.0302(5) Uani 1 1 d . . . . .
H4AA H 0.9721 0.2334 0.1312 0.045 Uiso 1 1 calc GR . . . .
H4AB H 1.0148 0.2445 0.1879 0.045 Uiso 1 1 calc GR . . . .
H4AC H 1.0670 0.3064 0.1460 0.045 Uiso 1 1 calc GR . . . .
C5AA C 0.60601(13) 0.37278(18) 0.09637(7) 0.0251(4) Uani 1 1 d . . . . .
C7 C 0.65184(15) 0.48311(19) 0.07624(8) 0.0336(5) Uani 1 1 d . . . . .
H7A H 0.6926 0.5209 0.1030 0.050 Uiso 1 1 calc GR . . . .
H7B H 0.6020 0.5373 0.0630 0.050 Uiso 1 1 calc GR . . . .
H7C H 0.6898 0.4608 0.0500 0.050 Uiso 1 1 calc GR . . . .
C8 C 0.54078(14) 0.31203(19) 0.05456(7) 0.0318(5) Uani 1 1 d . . . . .
H8A H 0.5783 0.2884 0.0283 0.048 Uiso 1 1 calc GR . . . .
H8B H 0.4910 0.3661 0.0412 0.048 Uiso 1 1 calc GR . . . .
H8C H 0.5119 0.2431 0.0678 0.048 Uiso 1 1 calc GR . . . .
C9 C 0.55054(14) 0.4032(2) 0.14085(8) 0.0334(5) Uani 1 1 d . . . . .
H9A H 0.5219 0.3324 0.1526 0.050 Uiso 1 1 calc GR . . . .
H9B H 0.5007 0.4598 0.1303 0.050 Uiso 1 1 calc GR . . . .
H9C H 0.5942 0.4366 0.1676 0.050 Uiso 1 1 calc GR . . . .
C10 C 1.01920(14) -0.19237(18) 0.14381(7) 0.0288(4) Uani 1 1 d . . . . .
H10A H 0.9783 -0.2522 0.1270 0.043 Uiso 1 1 calc GR . . . .
H10B H 1.0575 -0.2269 0.1723 0.043 Uiso 1 1 calc GR . . . .
H10C H 1.0609 -0.1606 0.1209 0.043 Uiso 1 1 calc GR . . . .
C11 C 0.95831(12) -0.09493(17) 0.16131(6) 0.0203(4) Uani 1 1 d . . . . .
C12 C 0.95867(13) -0.04897(17) 0.20908(6) 0.0223(4) Uani 1 1 d . . . . .
H12 H 0.9992 -0.0708 0.2377 0.027 Uiso 1 1 calc R . . . .
C13 C 0.88579(12) 0.03727(16) 0.20594(6) 0.0193(4) Uani 1 1 d . . . . .
C14 C 0.85705(13) 0.11439(16) 0.24616(6) 0.0201(4) Uani 1 1 d . . . . .
C15 C 0.92845(14) 0.16719(17) 0.28002(6) 0.0251(4) Uani 1 1 d . . . . .
H15 H 0.9933 0.1512 0.2776 0.030 Uiso 1 1 calc R . . . .
C16 C 0.90323(15) 0.24331(19) 0.31714(7) 0.0310(5) Uani 1 1 d . . . . .
H16 H 0.9512 0.2778 0.3396 0.037 Uiso 1 1 calc R . . . .
C17 C 0.80764(15) 0.26808(18) 0.32096(7) 0.0298(5) Uani 1 1 d . . . . .
H17 H 0.7910 0.3204 0.3455 0.036 Uiso 1 1 calc R . . . .
C18 C 0.73638(14) 0.21485(17) 0.28816(6) 0.0264(4) Uani 1 1 d . . . . .
H18 H 0.6717 0.2309 0.2909 0.032 Uiso 1 1 calc R . . . .
C19 C 0.76069(13) 0.13773(17) 0.25112(6) 0.0220(4) Uani 1 1 d . . . . .
H19 H 0.7122 0.1015 0.2295 0.026 Uiso 1 1 calc R . . . .
C20 C 0.74663(14) -0.25585(17) 0.01251(6) 0.0239(4) Uani 1 1 d . . . . .
H20A H 0.7785 -0.2196 -0.0136 0.036 Uiso 1 1 calc GR . . . .
H20B H 0.6983 -0.3102 -0.0023 0.036 Uiso 1 1 calc GR . . . .
H20C H 0.7931 -0.2981 0.0352 0.036 Uiso 1 1 calc GR . . . .
C21 C 0.69984(13) -0.16200(16) 0.04083(6) 0.0190(4) Uani 1 1 d . . . . .
C22 C 0.60404(13) -0.14891(17) 0.04715(6) 0.0202(4) Uani 1 1 d . . . . .
H22 H 0.5534 -0.1982 0.0345 0.024 Uiso 1 1 calc R . . . .
C23 C 0.59778(12) -0.04696(16) 0.07621(6) 0.0173(4) Uani 1 1 d . . . . .
C24 C 0.50992(12) 0.00202(16) 0.09387(6) 0.0186(4) Uani 1 1 d . . . . .
C25 C 0.42166(13) -0.01305(17) 0.06408(6) 0.0228(4) Uani 1 1 d . . . . .
H25 H 0.4200 -0.0517 0.0332 0.027 Uiso 1 1 calc R . . . .
C26 C 0.33662(13) 0.02860(19) 0.07968(7) 0.0284(5) Uani 1 1 d . . . . .
H26 H 0.2783 0.0177 0.0595 0.034 Uiso 1 1 calc R . . . .
C27 C 0.33846(14) 0.0865(2) 0.12544(7) 0.0311(5) Uani 1 1 d . . . . .
H27 H 0.2815 0.1150 0.1360 0.037 Uiso 1 1 calc R . . . .
C28 C 0.42519(14) 0.10179(19) 0.15536(7) 0.0286(5) Uani 1 1 d . . . . .
H28 H 0.4263 0.1411 0.1860 0.034 Uiso 1 1 calc R . . . .
C29 C 0.51052(13) 0.05919(18) 0.14020(6) 0.0239(4) Uani 1 1 d . . . . .
H29 H 0.5683 0.0687 0.1610 0.029 Uiso 1 1 calc R . . . .
C30 C 1.06374(14) 0.0581(2) 0.06779(7) 0.0249(4) Uani 1 1 d . . . . .
H30A H 1.0663(14) 0.0554(19) 0.1043(8) 0.037 Uiso 1 1 d R . . . .
H30B H 1.1186(16) 0.104(2) 0.0605(7) 0.037 Uiso 1 1 d R . . . .
H30C H 1.0703(15) -0.023(2) 0.0552(8) 0.037 Uiso 1 1 d R . . . .
C31 C 0.97294(12) 0.11444(17) 0.04372(6) 0.0205(4) Uani 1 1 d . . . . .
C32 C 0.96133(12) 0.21626(17) 0.01567(6) 0.0212(4) Uani 1 1 d . . . . .
H32 H 1.0095 0.2680 0.0078 0.025 Uiso 1 1 calc R . . . .
C33 C 0.86148(12) 0.22620(16) 0.00118(6) 0.0195(4) Uani 1 1 d . . . . .
C34 C 0.80936(13) 0.31918(18) -0.02948(6) 0.0229(4) Uani 1 1 d . . . . .
C35 C 0.71371(15) 0.3039(2) -0.04976(8) 0.0390(5) Uani 1 1 d . . . . .
H35 H 0.6822 0.2328 -0.0446 0.047 Uiso 1 1 calc R . . . .
C36 C 0.66511(17) 0.3935(2) -0.07755(10) 0.0520(7) Uani 1 1 d . . . . .
H36 H 0.6009 0.3821 -0.0906 0.062 Uiso 1 1 calc R . . . .
C37 C 0.71021(16) 0.4995(2) -0.08626(9) 0.0425(6) Uani 1 1 d . . . . .
H37 H 0.6769 0.5594 -0.1049 0.051 Uiso 1 1 calc R . . . .
C38 C 0.80539(15) 0.51512(19) -0.06693(7) 0.0309(5) Uani 1 1 d . . . . .
H38 H 0.8371 0.5854 -0.0730 0.037 Uiso 1 1 calc R . . . .
C39 C 0.85364(14) 0.42660(18) -0.03856(6) 0.0246(4) Uani 1 1 d . . . . .
H39 H 0.9175 0.4390 -0.0251 0.029 Uiso 1 1 calc R . . . .
B1 B 0.85846(15) -0.0486(2) 0.07300(7) 0.0196(4) Uani 1 1 d . . . . .
N1 N 0.84362(10) 0.04447(13) 0.15820(5) 0.0177(3) Uani 1 1 d . . . . .
N2 N 0.88905(10) -0.03747(13) 0.13087(5) 0.0181(3) Uani 1 1 d . . . . .
N3 N 0.68616(10) 0.00136(13) 0.08716(5) 0.0175(3) Uani 1 1 d . . . . .
N4 N 0.74916(10) -0.07099(13) 0.06505(5) 0.0176(3) Uani 1 1 d . . . . .
N5 N 0.88362(10) 0.06756(13) 0.04609(5) 0.0177(3) Uani 1 1 d . . . . .
N6 N 0.81411(10) 0.13570(14) 0.01946(5) 0.0196(3) Uani 1 1 d . . . . .
N7 N 0.68344(10) 0.28709(13) 0.11524(5) 0.0200(3) Uani 1 1 d . . . . .
Ni1 Ni 0.74230(2) 0.13829(2) 0.12533(2) 0.01639(7) Uani 1 1 d . . . . .
Si1 Si 0.93251(4) 0.42058(5) 0.16211(2) 0.02127(12) Uani 1 1 d . . . . .
H1 H 0.8955(12) -0.1259(16) 0.0597(6) 0.014(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
C0AA C1AA 1.476(2) . ?
C0AA N7 1.251(2) . ?
C0AA Ni1 1.8221(18) . ?
C1AA Si1 1.8905(17) . ?
C2AA Si1 1.8571(19) . ?
C3AA Si1 1.8616(19) . ?
C4AA Si1 1.851(2) . ?
C5AA C7 1.523(3) . ?
C5AA C8 1.519(3) . ?
C5AA C9 1.530(3) . ?
C5AA N7 1.491(2) . ?
C10 C11 1.494(3) . ?
C11 C12 1.377(2) . ?
C11 N2 1.353(2) . ?
C12 C13 1.400(3) . ?
C13 C14 1.473(2) . ?
C13 N1 1.344(2) . ?
C14 C15 1.398(2) . ?
C14 C19 1.389(3) . ?
C15 C16 1.387(3) . ?
C16 C17 1.376(3) . ?
C17 C18 1.383(3) . ?
C18 C19 1.388(2) . ?
C20 C21 1.493(2) . ?
C21 C22 1.372(2) . ?
C21 N4 1.356(2) . ?
C22 C23 1.394(2) . ?
C23 C24 1.469(2) . ?
C23 N3 1.347(2) . ?
C24 C25 1.396(2) . ?
C24 C29 1.394(2) . ?
C25 C26 1.382(3) . ?
C26 C27 1.383(3) . ?
C27 C28 1.380(3) . ?
C28 C29 1.385(3) . ?
C30 C31 1.493(3) . ?
C31 C32 1.369(3) . ?
C31 N5 1.360(2) . ?
C32 C33 1.404(2) . ?
C33 C34 1.469(3) . ?
C33 N6 1.337(2) . ?
C34 C35 1.390(3) . ?
C34 C39 1.391(3) . ?
C35 C36 1.382(3) . ?
C36 C37 1.381(3) . ?
C37 C38 1.377(3) . ?
C38 C39 1.379(3) . ?
B1 N2 1.561(2) . ?
B1 N4 1.534(2) . ?
B1 N5 1.552(3) . ?
N1 N2 1.3754(19) . ?
N1 Ni1 1.8955(14) . ?
N3 N4 1.3794(19) . ?
N3 Ni1 1.9605(15) . ?
N5 N6 1.369(2) . ?
N7 Ni1 1.8706(15) . ?

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
C1AA C0AA Ni1 149.79(14) . . ?
N7 C0AA C1AA 137.90(18) . . ?
N7 C0AA Ni1 72.30(11) . . ?
C0AA C1AA Si1 114.62(11) . . ?
C7 C5AA C9 111.22(17) . . ?
C8 C5AA C7 110.29(16) . . ?
C8 C5AA C9 111.08(16) . . ?
N7 C5AA C7 109.32(15) . . ?
N7 C5AA C8 107.79(16) . . ?
N7 C5AA C9 107.02(14) . . ?
C12 C11 C10 128.66(16) . . ?
N2 C11 C10 123.63(15) . . ?
N2 C11 C12 107.70(16) . . ?
C11 C12 C13 106.27(15) . . ?
C12 C13 C14 128.43(15) . . ?
N1 C13 C12 109.45(15) . . ?
N1 C13 C14 122.10(16) . . ?
C15 C14 C13 119.34(16) . . ?
C19 C14 C13 121.90(16) . . ?
C19 C14 C15 118.75(16) . . ?
C16 C15 C14 120.39(18) . . ?
C17 C16 C15 120.39(18) . . ?
C16 C17 C18 119.68(18) . . ?
C17 C18 C19 120.46(18) . . ?
C18 C19 C14 120.31(17) . . ?
C22 C21 C20 128.77(17) . . ?
N4 C21 C20 123.37(16) . . ?
N4 C21 C22 107.86(15) . . ?
C21 C22 C23 106.33(16) . . ?
C22 C23 C24 126.59(16) . . ?
N3 C23 C22 109.82(15) . . ?
N3 C23 C24 123.58(16) . . ?
C25 C24 C23 118.86(15) . . ?
C29 C24 C23 122.60(16) . . ?
C29 C24 C25 118.50(16) . . ?
C26 C25 C24 121.05(17) . . ?
C25 C26 C27 119.82(18) . . ?
C28 C27 C26 119.77(18) . . ?
C27 C28 C29 120.70(18) . . ?
C28 C29 C24 120.15(17) . . ?
C32 C31 C30 129.23(17) . . ?
N5 C31 C30 123.33(17) . . ?
N5 C31 C32 107.44(15) . . ?
C31 C32 C33 105.56(16) . . ?
C32 C33 C34 128.37(16) . . ?
N6 C33 C32 110.70(16) . . ?
N6 C33 C34 120.93(15) . . ?
C35 C34 C33 121.27(18) . . ?
C35 C34 C39 117.65(18) . . ?
C39 C34 C33 121.07(17) . . ?
C36 C35 C34 120.5(2) . . ?
C37 C36 C35 121.1(2) . . ?
C38 C37 C36 118.9(2) . . ?
C37 C38 C39 120.1(2) . . ?
C38 C39 C34 121.74(18) . . ?
N4 B1 N2 107.66(13) . . ?
N4 B1 N5 110.37(15) . . ?
N5 B1 N2 109.95(15) . . ?
C13 N1 N2 106.63(14) . . ?
C13 N1 Ni1 133.95(12) . . ?
N2 N1 Ni1 119.41(10) . . ?
C11 N2 B1 130.66(15) . . ?
C11 N2 N1 109.95(13) . . ?
N1 N2 B1 119.36(14) . . ?
C23 N3 N4 106.22(14) . . ?
C23 N3 Ni1 136.91(12) . . ?
N4 N3 Ni1 116.86(10) . . ?
C21 N4 B1 129.10(15) . . ?
C21 N4 N3 109.77(13) . . ?
N3 N4 B1 120.95(14) . . ?
C31 N5 B1 127.27(15) . . ?
C31 N5 N6 110.76(14) . . ?
N6 N5 B1 121.95(14) . . ?
C33 N6 N5 105.53(14) . . ?
C0AA N7 C5AA 134.87(16) . . ?
C0AA N7 Ni1 68.12(11) . . ?
C5AA N7 Ni1 156.35(12) . . ?
C0AA Ni1 N1 109.32(7) . . ?
C0AA Ni1 N3 158.73(7) . . ?
C0AA Ni1 N7 39.58(7) . . ?
N1 Ni1 N3 91.95(6) . . ?
N7 Ni1 N1 148.89(6) . . ?
N7 Ni1 N3 119.15(6) . . ?
C2AA Si1 C1AA 108.91(9) . . ?
C2AA Si1 C3AA 111.42(10) . . ?
C3AA Si1 C1AA 106.15(8) . . ?
C4AA Si1 C1AA 110.50(9) . . ?
C4AA Si1 C2AA 110.12(9) . . ?
C4AA Si1 C3AA 109.67(9) . . ?

_smtbx_masks_special_details     ?
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 0.250 -0.946 0.250 325.0 63.9 ?
2 0.750 -0.198 0.750 325.0 63.9 ?

_olex2_submission_special_instructions 'No special instructions were received'

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

data_Complex_2b
_database_code_depnum_ccdc_archive 'CCDC 1476065'
_audit_update_record             
;
2016-06-07 deposited with the CCDC.
2016-06-21 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_CHEMW03_Complex_2b          
;
PROBLEM: WARNING: The ratio of given/expected molecular weight as
RESPONSE: The solvent-mask program of Olex was used to refine the solvent disorder. Such refinement automatically result in a discrepancy between the given and expected molecular weight.
;
# Added during the CSD deposition process: Tuesday 07 June 2016 04:17 PM
# end Validation Reply Form

_audit_creation_date             2016-06-07
_audit_creation_method           
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_shelxl_version_number           2014/6
_chemical_name_common            ?
_chemical_name_systematic        'Complex 2b'
_chemical_formula_moiety         
'C35 H39 B N6 Ni S2 Si, C5.97 H17.91 O0.995 Si1.99'
_chemical_formula_sum            'C40.97 H56.91 B N6 Ni O S2 Si2.99'
_chemical_formula_weight         867.02
_chemical_melting_point          '448.2 - 449.2'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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'
S S 0.1246 0.1234 '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'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   10.534(9)
_cell_length_b                   15.566(7)
_cell_length_c                   17.689(9)
_cell_angle_alpha                112.175(4)
_cell_angle_beta                 101.588(4)
_cell_angle_gamma                98.702(4)
_cell_volume                     2547.9(23)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    8049
_cell_measurement_temperature    100(2)
_cell_measurement_theta_min      2.33
_cell_measurement_theta_max      25.41
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    0.567
_exptl_absorpt_correction_T_min  0.8261
_exptl_absorpt_correction_T_max  0.9235
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.0977 before and 0.0428 after correction.
The Ratio of minimum to maximum transmission is 0.9175.
The λ/2 correction factor is 0.0000.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.130
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rode
_exptl_crystal_F_000             919
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.11
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0714
_diffrn_reflns_av_unetI/netI     0.0878
_diffrn_reflns_Laue_measured_fraction_full 0.937
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            30732
_diffrn_reflns_point_group_measured_fraction_full 0.937
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         25.387
_diffrn_reflns_theta_min         1.488
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.366
_diffrn_measured_fraction_theta_full 0.937
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed tube'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                5732
_reflns_number_total             9357
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_data_collection       'Bruker APEX2 v.2011.4'
_computing_cell_refinement       'Bruker APEX2 v.2011.4'
_computing_data_reduction        'Bruker APEX2 v.2011.4'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_refine_diff_density_max         1.480
_refine_diff_density_min         -0.741
_refine_diff_density_rms         0.085
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     523
_refine_ls_number_reflns         9357
_refine_ls_number_restraints     91
_refine_ls_R_factor_all          0.1084
_refine_ls_R_factor_gt           0.0660
_refine_ls_restrained_S_all      1.117
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1053P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1804
_refine_ls_wR_factor_ref         0.1978
_refine_special_details          
'The crystal structure contains large solvent accessible voids. The solvent (hexamethyl-disiloxane) situated in the voids is strongly disordered. We were able to find and freely refine one position of a HMDSO molecule with an occupancy of about 62 percent (PART 1), corresponding to 1.239 HMDS-molecules per unit cell. Still, several relatively strong residual peaks up to 4 electrons/A^^3 remained close to this position. We described the two strongest peaks as Si atoms with occupancies of about 22.1 and 21.3 percent, corresponding in total to 12.15 electrons or 0.135 HMDSO-molecules per unit cell (PART 2). However, attempts to describe the electron density by three complete, partially occupied rigid group HMDSO molecules were not successful. Also, for a part of the electron density in the void, all attempts for describing with partially occupied HMDSO-molecules failed, and the masked refinement routine in Olex2 has been employed. The electron density in the masked area sums up to 55.4 electrons corresponding to 0.616 HMDSO-molecules per unit cell. All contributions together (the partially occupied HMDSO-molecule, the residual electron density described by Si-atom equivalents and the electron density in the masked volume) sum up to 1.99 HMDSO-molecule per unit cell, SQUEEZE'
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All B(H) groups, All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 Si1A-C41 \\sim Si1A-C42 \\sim Si1A-O0AA \\sim Si1A-C40 \\sim Si3-C38 \\sim
Si3-C37 \\sim Si3-C36
 with sigma of 0.02
 Si1A-O0AA \\sim Si3-O0AA
 with sigma of 0.02
3. Rigid body (RIGU) restrains
 C42, C41, Si1A, C40, O0AA, Si3, C38, C37, C36
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C42, C41, Si1A, O0AA, Si3, C38, C37, C36, C40
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Others
 Sof(C36)=Sof(H36A)=Sof(H36B)=Sof(H36C)=Sof(C37)=Sof(H37A)=Sof(H37B)=Sof(H37C)=
 Sof(C41)=Sof(H41A)=Sof(H41B)=Sof(H41C)=Sof(C42)=Sof(H42A)=Sof(H42B)=Sof(H42C)=
 Sof(Si1A)=Sof(O0AA)=Sof(Si3)=Sof(C38)=Sof(H38A)=Sof(H38B)=Sof(H38C)=Sof(C40)=
 Sof(H40A)=Sof(H40B)=Sof(H40C)=FVAR(1)
5.a Ternary CH refined with riding coordinates:
 B1(H1)
5.b Secondary CH2 refined with riding coordinates:
 C1AA(H1AA,H1AB)
5.c Me refined with riding coordinates:
 C36(H36A,H36B,H36C), C37(H37A,H37B,H37C), C41(H41A,H41B,H41C), C42(H42A,H42B,
 H42C), C38(H38A,H38B,H38C), C40(H40A,H40B,H40C)
5.d Aromatic/amide H refined with riding coordinates:
 C6AA(H6AA), C8AA(H8AA), C12(H12), C13(H13), C14(H14), C15(H15), C18(H18),
 C21(H21), C22(H22), C23(H23), C24(H24), C25(H25), C28(H28), C31(H31), C32(H32),
  C33(H33), C34(H34), C35(H35)
5.e Idealised Me refined as rotating group:
 C2AA(H2AA,H2AB,H2AC), C3AA(H3AA,H3AB,H3AC), C4AA(H4AA,H4AB,H4AC), C5AA(H5AA,
 H5AB,H5AC), C16(H16A,H16B,H16C), C26(H26A,H26B,H26C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C0AA C 0.8703(4) 0.0396(4) 0.2185(3) 0.0356(12) Uani 1 1 d . . . . .
C1AA C 0.9406(4) 0.0123(4) 0.1511(3) 0.0412(13) Uani 1 1 d . . . . .
H1AA H 1.0343 0.0465 0.1758 0.049 Uiso 1 1 calc R . . . .
H1AB H 0.9030 0.0323 0.1076 0.049 Uiso 1 1 calc R . . . .
C2AA C 0.9804(5) -0.1430(5) 0.0002(4) 0.0588(16) Uani 1 1 d . . . . .
H2AA H 0.9714 -0.2104 -0.0304 0.088 Uiso 1 1 calc GR . . . .
H2AB H 1.0720 -0.1089 0.0149 0.088 Uiso 1 1 calc GR . . . .
H2AC H 0.9246 -0.1210 -0.0348 0.088 Uiso 1 1 calc GR . . . .
C3AA C 0.7512(4) -0.1912(4) 0.0702(3) 0.0527(15) Uani 1 1 d . . . . .
H3AA H 0.7473 -0.2585 0.0485 0.079 Uiso 1 1 calc GR . . . .
H3AB H 0.6959 -0.1784 0.0275 0.079 Uiso 1 1 calc GR . . . .
H3AC H 0.7196 -0.1727 0.1199 0.079 Uiso 1 1 calc GR . . . .
C4AA C 1.0444(5) -0.1526(5) 0.1732(4) 0.0607(17) Uani 1 1 d . . . . .
H4AA H 1.0193 -0.1370 0.2252 0.091 Uiso 1 1 calc GR . . . .
H4AB H 1.1343 -0.1169 0.1853 0.091 Uiso 1 1 calc GR . . . .
H4AC H 1.0393 -0.2199 0.1475 0.091 Uiso 1 1 calc GR . . . .
C5AA C 0.6454(5) 0.1264(4) 0.6416(3) 0.0443(13) Uani 1 1 d . . . . .
H5AA H 0.6998 0.1906 0.6748 0.066 Uiso 1 1 calc GR . . . .
H5AB H 0.6531 0.0903 0.6752 0.066 Uiso 1 1 calc GR . . . .
H5AC H 0.5537 0.1279 0.6241 0.066 Uiso 1 1 calc GR . . . .
C0BA C 0.6920(4) 0.0798(3) 0.5641(3) 0.0326(11) Uani 1 1 d . . . . .
C6AA C 0.7458(4) 0.0033(3) 0.5424(3) 0.0327(11) Uani 1 1 d . . . . .
H6AA H 0.7660 -0.0308 0.5746 0.039 Uiso 1 1 calc R . . . .
C7AA C 0.7653(4) -0.0148(3) 0.4625(3) 0.0272(10) Uani 1 1 d . . . . .
C9AA C 0.8147(4) -0.0934(3) 0.4105(3) 0.0278(10) Uani 1 1 d . . . . .
C8AA C 0.9119(4) -0.1260(3) 0.4505(3) 0.0327(11) Uani 1 1 d . . . . .
H8AA H 0.9500 -0.0935 0.5090 0.039 Uiso 1 1 calc R . . . .
C12 C 0.9527(5) -0.2049(4) 0.4055(3) 0.0422(13) Uani 1 1 d . . . . .
H12 H 1.0183 -0.2250 0.4335 0.051 Uiso 1 1 calc R . . . .
C13 C 0.8972(5) -0.2536(4) 0.3201(3) 0.0482(13) Uani 1 1 d . . . . .
H13 H 0.9227 -0.3083 0.2900 0.058 Uiso 1 1 calc R . . . .
C14 C 0.8020(5) -0.2218(4) 0.2777(3) 0.0484(13) Uani 1 1 d . . . . .
H14 H 0.7672 -0.2535 0.2189 0.058 Uiso 1 1 calc R . . . .
C15 C 0.7592(4) -0.1433(4) 0.3227(3) 0.0402(12) Uani 1 1 d . . . . .
H15 H 0.6933 -0.1236 0.2944 0.048 Uiso 1 1 calc R . . . .
C16 C 0.3437(5) 0.2325(4) 0.4710(3) 0.0431(12) Uani 1 1 d . . . . .
H16A H 0.3620 0.2118 0.5159 0.065 Uiso 1 1 calc GR . . . .
H16B H 0.2490 0.2241 0.4511 0.065 Uiso 1 1 calc GR . . . .
H16C H 0.3885 0.2989 0.4921 0.065 Uiso 1 1 calc GR . . . .
C17 C 0.3919(4) 0.1754(3) 0.4008(3) 0.0337(11) Uani 1 1 d . . . . .
C18 C 0.3258(4) 0.1273(3) 0.3146(3) 0.0365(12) Uani 1 1 d . . . . .
H18 H 0.2395 0.1263 0.2881 0.044 Uiso 1 1 calc R . . . .
C19 C 0.4146(4) 0.0804(3) 0.2752(3) 0.0295(11) Uani 1 1 d . . . . .
C20 C 0.3943(4) 0.0197(4) 0.1856(3) 0.0337(11) Uani 1 1 d . . . . .
C21 C 0.3583(4) 0.0549(4) 0.1244(3) 0.0464(14) Uani 1 1 d . . . . .
H21 H 0.3439 0.1160 0.1410 0.056 Uiso 1 1 calc R . . . .
C22 C 0.3441(5) -0.0001(5) 0.0399(3) 0.0514(15) Uani 1 1 d . . . . .
H22 H 0.3223 0.0249 0.0002 0.062 Uiso 1 1 calc R . . . .
C23 C 0.3614(4) -0.0899(5) 0.0140(3) 0.0523(16) Uani 1 1 d . . . . .
H23 H 0.3521 -0.1260 -0.0433 0.063 Uiso 1 1 calc R . . . .
C24 C 0.3934(4) -0.1292(4) 0.0729(3) 0.0498(14) Uani 1 1 d . . . . .
H24 H 0.4029 -0.1917 0.0550 0.060 Uiso 1 1 calc R . . . .
C25 C 0.4108(4) -0.0722(4) 0.1593(3) 0.0399(13) Uani 1 1 d . . . . .
H25 H 0.4337 -0.0967 0.1992 0.048 Uiso 1 1 calc R . . . .
C26 C 0.7872(6) 0.4042(4) 0.6253(3) 0.0568(15) Uani 1 1 d . . . . .
H26A H 0.6990 0.4146 0.6151 0.085 Uiso 1 1 calc GR . . . .
H26B H 0.8519 0.4648 0.6571 0.085 Uiso 1 1 calc GR . . . .
H26C H 0.7931 0.3661 0.6571 0.085 Uiso 1 1 calc GR . . . .
C27 C 0.8147(5) 0.3529(3) 0.5418(3) 0.0386(12) Uani 1 1 d . . . . .
C28 C 0.9075(4) 0.3821(4) 0.5061(3) 0.0398(12) Uani 1 1 d . . . . .
H28 H 0.9695 0.4412 0.5300 0.048 Uiso 1 1 calc R . . . .
C29 C 0.8919(4) 0.3074(3) 0.4279(3) 0.0359(12) Uani 1 1 d . . . . .
C30 C 0.9666(4) 0.3056(3) 0.3661(3) 0.0370(12) Uani 1 1 d . . . . .
C31 C 0.9025(5) 0.2691(4) 0.2802(3) 0.0502(15) Uani 1 1 d . . . . .
H31 H 0.8098 0.2469 0.2616 0.060 Uiso 1 1 calc R . . . .
C32 C 0.9727(6) 0.2648(4) 0.2216(4) 0.0618(17) Uani 1 1 d . . . . .
H32 H 0.9279 0.2379 0.1639 0.074 Uiso 1 1 calc R . . . .
C33 C 1.1096(6) 0.3006(4) 0.2489(4) 0.0580(16) Uani 1 1 d . . . . .
H33 H 1.1577 0.2971 0.2095 0.070 Uiso 1 1 calc R . . . .
C34 C 1.1748(6) 0.3413(4) 0.3340(5) 0.0631(18) Uani 1 1 d . . . . .
H34 H 1.2669 0.3669 0.3523 0.076 Uiso 1 1 calc R . . . .
C35 C 1.1037(5) 0.3448(4) 0.3947(4) 0.0507(14) Uani 1 1 d . . . . .
H35 H 1.1481 0.3728 0.4525 0.061 Uiso 1 1 calc R . . . .
B1 B 0.6311(5) 0.1936(4) 0.4926(3) 0.0329(12) Uani 1 1 d . . . . .
H1 H 0.6010 0.2271 0.5422 0.040 Uiso 1 1 calc R . . . .
N1 N 0.7268(3) 0.0517(2) 0.4374(2) 0.0258(8) Uani 1 1 d . . . . .
N2 N 0.6791(3) 0.1088(3) 0.5003(2) 0.0291(8) Uani 1 1 d . . . . .
N3 N 0.5143(3) 0.1567(3) 0.4111(2) 0.0318(9) Uani 1 1 d . . . . .
N4 N 0.5305(3) 0.0993(3) 0.3352(2) 0.0297(9) Uani 1 1 d . . . . .
N5 N 0.7932(3) 0.2334(3) 0.4161(2) 0.0325(9) Uani 1 1 d . . . . .
N6 N 0.7459(3) 0.2632(3) 0.4869(2) 0.0324(9) Uani 1 1 d . . . . .
Si0A Si 0.92846(12) -0.12141(12) 0.09887(9) 0.0443(4) Uani 1 1 d . . . . .
S1 S 0.70894(11) 0.04236(11) 0.19320(8) 0.0488(4) Uani 1 1 d . . . . .
S2 S 0.94449(10) 0.06393(9) 0.32020(7) 0.0338(3) Uani 1 1 d . . . . .
Ni1 Ni 0.72605(5) 0.08968(4) 0.33895(3) 0.0292(2) Uani 1 1 d . . . . .
C36 C 0.5009(14) 0.4541(13) 0.1236(9) 0.153(6) Uani 0.619(4) 1 d D U P A 1
H36A H 0.4786 0.4737 0.0783 0.230 Uiso 0.619(4) 1 calc R . P A 1
H36B H 0.5961 0.4736 0.1485 0.230 Uiso 0.619(4) 1 calc R . P A 1
H36C H 0.4711 0.3856 0.1015 0.230 Uiso 0.619(4) 1 calc R . P A 1
C37 C 0.4665(10) 0.6381(6) 0.2512(6) 0.073(3) Uani 0.619(4) 1 d D U P A 1
H37A H 0.4435 0.6607 0.2080 0.110 Uiso 0.619(4) 1 calc R . P A 1
H37B H 0.4197 0.6618 0.2930 0.110 Uiso 0.619(4) 1 calc R . P A 1
H37C H 0.5612 0.6606 0.2780 0.110 Uiso 0.619(4) 1 calc R . P A 1
C41 C 0.5616(12) 0.4633(9) 0.4404(6) 0.114(4) Uani 0.619(4) 1 d D U P A 1
H41A H 0.6280 0.4410 0.4686 0.171 Uiso 0.619(4) 1 calc R . P A 1
H41B H 0.5762 0.5312 0.4715 0.171 Uiso 0.619(4) 1 calc R . P A 1
H41C H 0.4742 0.4315 0.4377 0.171 Uiso 0.619(4) 1 calc R . P A 1
C42 C 0.5387(10) 0.3106(7) 0.2785(9) 0.121(5) Uani 0.619(4) 1 d D U P A 1
H42A H 0.6018 0.2872 0.3078 0.181 Uiso 0.619(4) 1 calc R . P A 1
H42B H 0.4497 0.2825 0.2764 0.181 Uiso 0.619(4) 1 calc R . P A 1
H42C H 0.5456 0.2938 0.2216 0.181 Uiso 0.619(4) 1 calc R . P A 1
Si1A Si 0.5737(3) 0.4371(3) 0.3333(3) 0.0925(15) Uani 0.619(4) 1 d D U P A 1
O0AA O 0.4608(6) 0.4737(5) 0.2794(5) 0.088(2) Uani 0.619(4) 1 d D U P A 1
Si3 Si 0.4199(2) 0.50907(19) 0.20369(17) 0.0549(9) Uani 0.619(4) 1 d D U P A 1
C38 C 0.2359(8) 0.4637(7) 0.1562(6) 0.066(3) Uani 0.619(4) 1 d D U P A 1
H38A H 0.2087 0.4834 0.1114 0.099 Uiso 0.619(4) 1 calc R . P A 1
H38B H 0.2121 0.3951 0.1335 0.099 Uiso 0.619(4) 1 calc R . P A 1
H38C H 0.1918 0.4894 0.1992 0.099 Uiso 0.619(4) 1 calc R . P A 1
C40 C 0.7452(7) 0.4939(7) 0.3378(7) 0.082(3) Uani 0.619(4) 1 d D U P A 1
H40A H 0.8096 0.4728 0.3687 0.123 Uiso 0.619(4) 1 calc R . P A 1
H40B H 0.7530 0.4760 0.2810 0.123 Uiso 0.619(4) 1 calc R . P A 1
H40C H 0.7614 0.5623 0.3659 0.123 Uiso 0.619(4) 1 calc R . P A 1
Si1B Si 0.6339(6) 0.4584(6) 0.2424(4) 0.043(3) Uani 0.221(8) 1 d . . . B 2
Si2B Si 0.5875(9) 0.4057(8) 0.2549(7) 0.065(4) Uani 0.213(9) 1 d . . . B 2


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C0AA C1AA 1.490(6) . ?
C0AA S1 1.680(4) . ?
C0AA S2 1.680(4) . ?
C1AA H1AA 0.9700 . ?
C1AA H1AB 0.9700 . ?
C1AA Si0A 1.903(5) . ?
C2AA H2AA 0.9600 . ?
C2AA H2AB 0.9600 . ?
C2AA H2AC 0.9600 . ?
C2AA Si0A 1.858(5) . ?
C3AA H3AA 0.9600 . ?
C3AA H3AB 0.9600 . ?
C3AA H3AC 0.9600 . ?
C3AA Si0A 1.875(4) . ?
C4AA H4AA 0.9600 . ?
C4AA H4AB 0.9600 . ?
C4AA H4AC 0.9600 . ?
C4AA Si0A 1.863(5) . ?
C5AA H5AA 0.9600 . ?
C5AA H5AB 0.9600 . ?
C5AA H5AC 0.9600 . ?
C5AA C0BA 1.508(6) . ?
C0BA C6AA 1.354(6) . ?
C0BA N2 1.355(5) . ?
C6AA H6AA 0.9300 . ?
C6AA C7AA 1.397(6) . ?
C7AA C9AA 1.467(6) . ?
C7AA N1 1.353(5) . ?
C9AA C8AA 1.394(6) . ?
C9AA C15 1.395(6) . ?
C8AA H8AA 0.9300 . ?
C8AA C12 1.373(7) . ?
C12 H12 0.9300 . ?
C12 C13 1.358(7) . ?
C13 H13 0.9300 . ?
C13 C14 1.395(7) . ?
C14 H14 0.9300 . ?
C14 C15 1.381(7) . ?
C15 H15 0.9300 . ?
C16 H16A 0.9600 . ?
C16 H16B 0.9600 . ?
C16 H16C 0.9600 . ?
C16 C17 1.466(7) . ?
C17 C18 1.387(6) . ?
C17 N3 1.356(5) . ?
C18 H18 0.9300 . ?
C18 C19 1.407(6) . ?
C19 C20 1.456(6) . ?
C19 N4 1.357(5) . ?
C20 C21 1.401(6) . ?
C20 C25 1.377(7) . ?
C21 H21 0.9300 . ?
C21 C22 1.376(7) . ?
C22 H22 0.9300 . ?
C22 C23 1.352(8) . ?
C23 H23 0.9300 . ?
C23 C24 1.406(7) . ?
C24 H24 0.9300 . ?
C24 C25 1.405(7) . ?
C25 H25 0.9300 . ?
C26 H26A 0.9600 . ?
C26 H26B 0.9600 . ?
C26 H26C 0.9600 . ?
C26 C27 1.503(7) . ?
C27 C28 1.375(6) . ?
C27 N6 1.344(6) . ?
C28 H28 0.9300 . ?
C28 C29 1.389(7) . ?
C29 C30 1.464(6) . ?
C29 N5 1.350(5) . ?
C30 C31 1.381(7) . ?
C30 C35 1.386(6) . ?
C31 H31 0.9300 . ?
C31 C32 1.377(7) . ?
C32 H32 0.9300 . ?
C32 C33 1.378(7) . ?
C33 H33 0.9300 . ?
C33 C34 1.369(8) . ?
C34 H34 0.9300 . ?
C34 C35 1.416(8) . ?
C35 H35 0.9300 . ?
B1 H1 0.9800 . ?
B1 N2 1.525(6) . ?
B1 N3 1.540(6) . ?
B1 N6 1.543(6) . ?
N1 N2 1.376(5) . ?
N1 Ni1 2.039(3) . ?
N3 N4 1.364(5) . ?
N4 Ni1 2.077(3) . ?
N5 N6 1.384(5) . ?
N5 Ni1 2.048(4) . ?
S1 Ni1 2.3585(13) . ?
S2 Ni1 2.4600(12) . ?
C36 H36A 0.9600 . ?
C36 H36B 0.9600 . ?
C36 H36C 0.9600 . ?
C36 Si3 1.805(10) . ?
C37 H37A 0.9600 . ?
C37 H37B 0.9600 . ?
C37 H37C 0.9600 . ?
C37 Si3 1.801(9) . ?
C41 H41A 0.9600 . ?
C41 H41B 0.9600 . ?
C41 H41C 0.9600 . ?
C41 Si1A 1.817(10) . ?
C42 H42A 0.9600 . ?
C42 H42B 0.9600 . ?
C42 H42C 0.9600 . ?
C42 Si1A 1.774(10) . ?
Si1A O0AA 1.676(6) . ?
Si1A C40 1.860(8) . ?
O0AA Si3 1.637(7) . ?
Si3 C38 1.856(8) . ?
C38 H38A 0.9600 . ?
C38 H38B 0.9600 . ?
C38 H38C 0.9600 . ?
C40 H40A 0.9600 . ?
C40 H40B 0.9600 . ?
C40 H40C 0.9600 . ?
Si1B Si2B 1.009(10) . ?

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
C1AA C0AA S1 120.0(3) . . ?
C1AA C0AA S2 122.4(3) . . ?
S2 C0AA S1 117.5(3) . . ?
C0AA C1AA H1AA 108.8 . . ?
C0AA C1AA H1AB 108.8 . . ?
C0AA C1AA Si0A 113.7(3) . . ?
H1AA C1AA H1AB 107.7 . . ?
Si0A C1AA H1AA 108.8 . . ?
Si0A C1AA H1AB 108.8 . . ?
H2AA C2AA H2AB 109.5 . . ?
H2AA C2AA H2AC 109.5 . . ?
H2AB C2AA H2AC 109.5 . . ?
Si0A C2AA H2AA 109.5 . . ?
Si0A C2AA H2AB 109.5 . . ?
Si0A C2AA H2AC 109.5 . . ?
H3AA C3AA H3AB 109.5 . . ?
H3AA C3AA H3AC 109.5 . . ?
H3AB C3AA H3AC 109.5 . . ?
Si0A C3AA H3AA 109.5 . . ?
Si0A C3AA H3AB 109.5 . . ?
Si0A C3AA H3AC 109.5 . . ?
H4AA C4AA H4AB 109.5 . . ?
H4AA C4AA H4AC 109.5 . . ?
H4AB C4AA H4AC 109.5 . . ?
Si0A C4AA H4AA 109.5 . . ?
Si0A C4AA H4AB 109.5 . . ?
Si0A C4AA H4AC 109.5 . . ?
H5AA C5AA H5AB 109.5 . . ?
H5AA C5AA H5AC 109.5 . . ?
H5AB C5AA H5AC 109.5 . . ?
C0BA C5AA H5AA 109.5 . . ?
C0BA C5AA H5AB 109.5 . . ?
C0BA C5AA H5AC 109.5 . . ?
C6AA C0BA C5AA 129.2(4) . . ?
C6AA C0BA N2 108.0(4) . . ?
N2 C0BA C5AA 122.7(4) . . ?
C0BA C6AA H6AA 126.4 . . ?
C0BA C6AA C7AA 107.1(4) . . ?
C7AA C6AA H6AA 126.4 . . ?
C6AA C7AA C9AA 127.5(4) . . ?
N1 C7AA C6AA 108.8(4) . . ?
N1 C7AA C9AA 123.7(4) . . ?
C8AA C9AA C7AA 119.3(4) . . ?
C8AA C9AA C15 118.1(4) . . ?
C15 C9AA C7AA 122.3(4) . . ?
C9AA C8AA H8AA 119.2 . . ?
C12 C8AA C9AA 121.6(4) . . ?
C12 C8AA H8AA 119.2 . . ?
C8AA C12 H12 120.0 . . ?
C13 C12 C8AA 119.9(5) . . ?
C13 C12 H12 120.0 . . ?
C12 C13 H13 120.0 . . ?
C12 C13 C14 120.1(5) . . ?
C14 C13 H13 120.0 . . ?
C13 C14 H14 119.9 . . ?
C15 C14 C13 120.2(5) . . ?
C15 C14 H14 119.9 . . ?
C9AA C15 H15 120.0 . . ?
C14 C15 C9AA 120.0(4) . . ?
C14 C15 H15 120.0 . . ?
H16A C16 H16B 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C17 C16 H16A 109.5 . . ?
C17 C16 H16B 109.5 . . ?
C17 C16 H16C 109.5 . . ?
C18 C17 C16 129.3(4) . . ?
N3 C17 C16 124.0(4) . . ?
N3 C17 C18 106.6(4) . . ?
C17 C18 H18 126.7 . . ?
C17 C18 C19 106.6(4) . . ?
C19 C18 H18 126.7 . . ?
C18 C19 C20 128.9(4) . . ?
N4 C19 C18 109.0(4) . . ?
N4 C19 C20 122.0(4) . . ?
C21 C20 C19 119.9(5) . . ?
C25 C20 C19 121.4(4) . . ?
C25 C20 C21 118.7(5) . . ?
C20 C21 H21 119.6 . . ?
C22 C21 C20 120.7(6) . . ?
C22 C21 H21 119.6 . . ?
C21 C22 H22 119.6 . . ?
C23 C22 C21 120.7(5) . . ?
C23 C22 H22 119.6 . . ?
C22 C23 H23 119.8 . . ?
C22 C23 C24 120.5(5) . . ?
C24 C23 H23 119.8 . . ?
C23 C24 H24 120.7 . . ?
C25 C24 C23 118.6(5) . . ?
C25 C24 H24 120.7 . . ?
C20 C25 C24 120.8(5) . . ?
C20 C25 H25 119.6 . . ?
C24 C25 H25 119.6 . . ?
H26A C26 H26B 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
C27 C26 H26A 109.5 . . ?
C27 C26 H26B 109.5 . . ?
C27 C26 H26C 109.5 . . ?
C28 C27 C26 130.5(5) . . ?
N6 C27 C26 122.4(4) . . ?
N6 C27 C28 107.1(4) . . ?
C27 C28 H28 126.2 . . ?
C27 C28 C29 107.6(4) . . ?
C29 C28 H28 126.2 . . ?
C28 C29 C30 127.6(4) . . ?
N5 C29 C28 108.7(4) . . ?
N5 C29 C30 123.7(4) . . ?
C31 C30 C29 121.3(4) . . ?
C31 C30 C35 119.3(5) . . ?
C35 C30 C29 119.3(4) . . ?
C30 C31 H31 119.2 . . ?
C32 C31 C30 121.5(5) . . ?
C32 C31 H31 119.2 . . ?
C31 C32 H32 120.1 . . ?
C31 C32 C33 119.7(6) . . ?
C33 C32 H32 120.1 . . ?
C32 C33 H33 120.1 . . ?
C34 C33 C32 119.8(5) . . ?
C34 C33 H33 120.1 . . ?
C33 C34 H34 119.6 . . ?
C33 C34 C35 120.8(5) . . ?
C35 C34 H34 119.6 . . ?
C30 C35 C34 118.7(5) . . ?
C30 C35 H35 120.7 . . ?
C34 C35 H35 120.7 . . ?
N2 B1 H1 109.6 . . ?
N2 B1 N3 109.2(4) . . ?
N2 B1 N6 109.9(4) . . ?
N3 B1 H1 109.6 . . ?
N3 B1 N6 108.8(3) . . ?
N6 B1 H1 109.6 . . ?
C7AA N1 N2 106.4(3) . . ?
C7AA N1 Ni1 138.3(3) . . ?
N2 N1 Ni1 115.3(2) . . ?
C0BA N2 B1 130.7(4) . . ?
C0BA N2 N1 109.6(4) . . ?
N1 N2 B1 119.6(3) . . ?
C17 N3 B1 129.4(4) . . ?
C17 N3 N4 111.4(3) . . ?
N4 N3 B1 119.2(4) . . ?
C19 N4 N3 106.3(3) . . ?
C19 N4 Ni1 137.4(3) . . ?
N3 N4 Ni1 114.6(2) . . ?
C29 N5 N6 106.5(4) . . ?
C29 N5 Ni1 137.6(3) . . ?
N6 N5 Ni1 114.5(2) . . ?
C27 N6 B1 130.7(4) . . ?
C27 N6 N5 110.2(4) . . ?
N5 N6 B1 119.1(4) . . ?
C2AA Si0A C1AA 106.0(2) . . ?
C2AA Si0A C3AA 109.3(3) . . ?
C2AA Si0A C4AA 110.8(3) . . ?
C3AA Si0A C1AA 110.1(2) . . ?
C4AA Si0A C1AA 108.7(3) . . ?
C4AA Si0A C3AA 111.7(2) . . ?
C0AA S1 Ni1 86.23(16) . . ?
C0AA S2 Ni1 82.99(16) . . ?
N1 Ni1 N4 87.23(13) . . ?
N1 Ni1 N5 94.07(14) . . ?
N1 Ni1 S1 148.40(11) . . ?
N1 Ni1 S2 98.39(10) . . ?
N4 Ni1 S1 98.65(10) . . ?
N4 Ni1 S2 171.41(10) . . ?
N5 Ni1 N4 89.73(14) . . ?
N5 Ni1 S1 116.85(10) . . ?
N5 Ni1 S2 96.31(10) . . ?
S1 Ni1 S2 73.18(4) . . ?
H36A C36 H36B 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?
Si3 C36 H36A 109.5 . . ?
Si3 C36 H36B 109.5 . . ?
Si3 C36 H36C 109.5 . . ?
H37A C37 H37B 109.5 . . ?
H37A C37 H37C 109.5 . . ?
H37B C37 H37C 109.5 . . ?
Si3 C37 H37A 109.5 . . ?
Si3 C37 H37B 109.5 . . ?
Si3 C37 H37C 109.5 . . ?
H41A C41 H41B 109.5 . . ?
H41A C41 H41C 109.5 . . ?
H41B C41 H41C 109.5 . . ?
Si1A C41 H41A 109.5 . . ?
Si1A C41 H41B 109.5 . . ?
Si1A C41 H41C 109.5 . . ?
H42A C42 H42B 109.5 . . ?
H42A C42 H42C 109.5 . . ?
H42B C42 H42C 109.5 . . ?
Si1A C42 H42A 109.5 . . ?
Si1A C42 H42B 109.5 . . ?
Si1A C42 H42C 109.5 . . ?
C41 Si1A C40 109.8(5) . . ?
C42 Si1A C41 106.9(7) . . ?
C42 Si1A C40 110.6(5) . . ?
O0AA Si1A C41 112.6(5) . . ?
O0AA Si1A C42 107.3(5) . . ?
O0AA Si1A C40 109.7(4) . . ?
Si3 O0AA Si1A 147.9(6) . . ?
C36 Si3 C38 108.7(6) . . ?
C37 Si3 C36 114.5(7) . . ?
C37 Si3 C38 110.4(5) . . ?
O0AA Si3 C36 107.7(7) . . ?
O0AA Si3 C37 107.9(4) . . ?
O0AA Si3 C38 107.4(4) . . ?
Si3 C38 H38A 109.5 . . ?
Si3 C38 H38B 109.5 . . ?
Si3 C38 H38C 109.5 . . ?
H38A C38 H38B 109.5 . . ?
H38A C38 H38C 109.5 . . ?
H38B C38 H38C 109.5 . . ?
Si1A C40 H40A 109.5 . . ?
Si1A C40 H40B 109.5 . . ?
Si1A C40 H40C 109.5 . . ?
H40A C40 H40B 109.5 . . ?
H40A C40 H40C 109.5 . . ?
H40B C40 H40C 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
C1AA C0AA S1 Ni1 180.0(4) . . . . ?
C1AA C0AA S2 Ni1 -179.8(4) . . . . ?
C5AA C0BA C6AA C7AA 176.8(4) . . . . ?
C5AA C0BA N2 B1 5.9(7) . . . . ?
C5AA C0BA N2 N1 -178.3(4) . . . . ?
C0BA C6AA C7AA C9AA -176.6(4) . . . . ?
C0BA C6AA C7AA N1 1.5(5) . . . . ?
C6AA C0BA N2 B1 -176.7(4) . . . . ?
C6AA C0BA N2 N1 -0.9(4) . . . . ?
C6AA C7AA C9AA C8AA -35.4(6) . . . . ?
C6AA C7AA C9AA C15 138.5(4) . . . . ?
C6AA C7AA N1 N2 -2.0(4) . . . . ?
C6AA C7AA N1 Ni1 175.6(3) . . . . ?
C7AA C9AA C8AA C12 174.0(4) . . . . ?
C7AA C9AA C15 C14 -174.7(4) . . . . ?
C7AA N1 N2 C0BA 1.8(4) . . . . ?
C7AA N1 N2 B1 178.2(3) . . . . ?
C9AA C7AA N1 N2 176.1(3) . . . . ?
C9AA C7AA N1 Ni1 -6.2(6) . . . . ?
C9AA C8AA C12 C13 -0.5(7) . . . . ?
C8AA C9AA C15 C14 -0.7(6) . . . . ?
C8AA C12 C13 C14 2.1(7) . . . . ?
C12 C13 C14 C15 -3.0(8) . . . . ?
C13 C14 C15 C9AA 2.3(7) . . . . ?
C15 C9AA C8AA C12 -0.1(6) . . . . ?
C16 C17 C18 C19 -177.5(4) . . . . ?
C16 C17 N3 B1 -4.5(7) . . . . ?
C16 C17 N3 N4 177.9(4) . . . . ?
C17 C18 C19 C20 179.6(4) . . . . ?
C17 C18 C19 N4 0.0(5) . . . . ?
C17 N3 N4 C19 -0.4(4) . . . . ?
C17 N3 N4 Ni1 167.5(3) . . . . ?
C18 C17 N3 B1 178.0(4) . . . . ?
C18 C17 N3 N4 0.4(5) . . . . ?
C18 C19 C20 C21 56.1(6) . . . . ?
C18 C19 C20 C25 -124.4(5) . . . . ?
C18 C19 N4 N3 0.3(4) . . . . ?
C18 C19 N4 Ni1 -163.4(3) . . . . ?
C19 C20 C21 C22 177.4(4) . . . . ?
C19 C20 C25 C24 -178.8(4) . . . . ?
C20 C19 N4 N3 -179.4(4) . . . . ?
C20 C19 N4 Ni1 16.9(6) . . . . ?
C20 C21 C22 C23 1.6(7) . . . . ?
C21 C20 C25 C24 0.7(6) . . . . ?
C21 C22 C23 C24 0.5(7) . . . . ?
C22 C23 C24 C25 -1.9(7) . . . . ?
C23 C24 C25 C20 1.2(6) . . . . ?
C25 C20 C21 C22 -2.2(6) . . . . ?
C26 C27 C28 C29 179.7(5) . . . . ?
C26 C27 N6 B1 0.0(7) . . . . ?
C26 C27 N6 N5 -179.2(4) . . . . ?
C27 C28 C29 C30 178.9(4) . . . . ?
C27 C28 C29 N5 -0.9(5) . . . . ?
C28 C27 N6 B1 179.4(4) . . . . ?
C28 C27 N6 N5 0.2(5) . . . . ?
C28 C29 C30 C31 -135.9(5) . . . . ?
C28 C29 C30 C35 41.6(7) . . . . ?
C28 C29 N5 N6 1.0(5) . . . . ?
C28 C29 N5 Ni1 -163.5(3) . . . . ?
C29 C30 C31 C32 -178.2(5) . . . . ?
C29 C30 C35 C34 179.1(5) . . . . ?
C29 N5 N6 C27 -0.8(4) . . . . ?
C29 N5 N6 B1 180.0(4) . . . . ?
C30 C29 N5 N6 -178.8(4) . . . . ?
C30 C29 N5 Ni1 16.7(7) . . . . ?
C30 C31 C32 C33 -2.2(8) . . . . ?
C31 C30 C35 C34 -3.4(7) . . . . ?
C31 C32 C33 C34 -0.9(9) . . . . ?
C32 C33 C34 C35 1.8(9) . . . . ?
C33 C34 C35 C30 0.4(8) . . . . ?
C35 C30 C31 C32 4.4(8) . . . . ?
B1 N3 N4 C19 -178.3(3) . . . . ?
B1 N3 N4 Ni1 -10.4(4) . . . . ?
N1 C7AA C9AA C8AA 146.8(4) . . . . ?
N1 C7AA C9AA C15 -39.3(6) . . . . ?
N2 C0BA C6AA C7AA -0.4(5) . . . . ?
N2 B1 N3 C17 129.5(4) . . . . ?
N2 B1 N3 N4 -53.1(5) . . . . ?
N2 B1 N6 C27 -112.5(5) . . . . ?
N2 B1 N6 N5 66.6(5) . . . . ?
N3 C17 C18 C19 -0.2(5) . . . . ?
N3 B1 N2 C0BA -124.3(4) . . . . ?
N3 B1 N2 N1 60.2(5) . . . . ?
N3 B1 N6 C27 128.0(5) . . . . ?
N3 B1 N6 N5 -53.0(5) . . . . ?
N4 C19 C20 C21 -124.3(4) . . . . ?
N4 C19 C20 C25 55.2(6) . . . . ?
N5 C29 C30 C31 43.9(7) . . . . ?
N5 C29 C30 C35 -138.7(5) . . . . ?
N6 C27 C28 C29 0.4(5) . . . . ?
N6 B1 N2 C0BA 116.4(5) . . . . ?
N6 B1 N2 N1 -59.1(5) . . . . ?
N6 B1 N3 C17 -110.6(5) . . . . ?
N6 B1 N3 N4 66.9(5) . . . . ?
S1 C0AA C1AA Si0A -90.3(4) . . . . ?
S1 C0AA S2 Ni1 -2.4(3) . . . . ?
S2 C0AA C1AA Si0A 87.0(4) . . . . ?
S2 C0AA S1 Ni1 2.5(3) . . . . ?
Ni1 N1 N2 C0BA -176.5(3) . . . . ?
Ni1 N1 N2 B1 -0.1(4) . . . . ?
Ni1 N5 N6 C27 167.8(3) . . . . ?
Ni1 N5 N6 B1 -11.5(4) . . . . ?
C41 Si1A O0AA Si3 153.8(9) . . . . ?
C42 Si1A O0AA Si3 -88.9(10) . . . . ?
Si1A O0AA Si3 C36 29.1(11) . . . . ?
Si1A O0AA Si3 C37 -94.9(10) . . . . ?
Si1A O0AA Si3 C38 146.1(9) . . . . ?
C40 Si1A O0AA Si3 31.3(12) . . . . ?

_smtbx_masks_special_details     ?
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 -0.462 0.500 0.000 390.1 77.5 ?
2 0.296 0.253 0.122 7.2 0.0 ?
3 0.704 0.747 0.878 7.2 0.0 ?

_olex2_submission_special_instructions 'No special instructions were received'

_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent'
_solvent_exptl_crystal_recrystallization_method 'Hexamethyl disiloxane'
_chemical_properties_physical    ', Air-sensitive,Moisture-sensitive'
