#------------------------------------------------------------------------------
#$Date: 2016-03-22 14:10:13 +0200 (Tue, 22 Mar 2016) $
#$Revision: 178986 $
#$URL: svn://www.crystallography.net/cod/cif/4/12/09/4120947.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_4120947
loop_
_publ_author_name
'Michael I. Lipschutz'
'Xinzheng Yang'
'Ruchira Chatterjee'
'T. Don Tilley'
_publ_section_title
;
 A Structurally Rigid Bis(amido) Ligand Framework in Low-Coordinate Ni(I),
 Ni(II), and Ni(III) Analogues Provides Access to a Ni(III) Methyl Complex
 via Oxidative Addition
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              15298
_journal_page_last               15301
_journal_paper_doi               10.1021/ja408151h
_journal_volume                  135
_journal_year                    2013
_chemical_formula_sum            'C30 H52 Co N2 Si2'
_chemical_formula_weight         555.85
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                102.530(4)
_cell_angle_beta                 92.358(4)
_cell_angle_gamma                113.879(3)
_cell_formula_units_Z            1
_cell_length_a                   8.8146(8)
_cell_length_b                   9.1675(8)
_cell_length_c                   11.1307(10)
_cell_measurement_reflns_used    9934
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.37
_cell_measurement_theta_min      2.55
_cell_volume                     794.44(13)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    ORTEP32
_computing_publication_material  WinGX
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    SIR97
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.366
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  'QUAZAR multilayer mirrors'
_diffrn_radiation_source         'microfocus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0230
_diffrn_reflns_av_sigmaI/netI    0.0131
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            21145
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.39
_diffrn_reflns_theta_min         1.89
_exptl_absorpt_coefficient_mu    0.635
_exptl_absorpt_correction_T_max  0.9750
_exptl_absorpt_correction_T_min  0.9277
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.162
_exptl_crystal_description       block
_exptl_crystal_F_000             301
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.318
_refine_diff_density_min         -0.192
_refine_diff_density_rms         0.039
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.076
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     167
_refine_ls_number_reflns         2919
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.076
_refine_ls_R_factor_all          0.0240
_refine_ls_R_factor_gt           0.0226
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0290P)²+0.3594P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0605
_refine_ls_wR_factor_ref         0.0614
_reflns_number_gt                2773
_reflns_number_total             2919
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja408151h_si_006.cif
_cod_data_source_block           shelxl
_cod_original_cell_volume        794.44(12)
_cod_database_code               4120947
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
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
C1 C 0.91108(15) 0.42269(15) 0.25403(11) 0.0133(2) Uani 1 1 d .
C2 C 0.76477(16) 0.27171(15) 0.21848(11) 0.0147(3) Uani 1 1 d .
C3 C 0.63138(16) 0.25963(16) 0.13866(12) 0.0184(3) Uani 1 1 d .
H3 H 0.5329 0.1589 0.1150 0.022 Uiso 1 1 calc R
C4 C 0.63971(17) 0.39132(18) 0.09335(13) 0.0209(3) Uani 1 1 d .
H4 H 0.5479 0.3810 0.0391 0.025 Uiso 1 1 calc R
C5 C 0.78329(17) 0.53862(17) 0.12784(13) 0.0197(3) Uani 1 1 d .
H5 H 0.7887 0.6289 0.0965 0.024 Uiso 1 1 calc R
C6 C 0.92014(16) 0.55725(15) 0.20755(12) 0.0155(3) Uani 1 1 d .
C7 C 1.07371(17) 0.72204(16) 0.24661(13) 0.0193(3) Uani 1 1 d .
H7 H 1.1667 0.7018 0.2830 0.023 Uiso 1 1 calc R
C8 C 1.0430(2) 0.84483(19) 0.34799(15) 0.0320(4) Uani 1 1 d .
H8A H 0.9499 0.8649 0.3161 0.048 Uiso 1 1 calc R
H8B H 1.1444 0.9489 0.3726 0.048 Uiso 1 1 calc R
H8C H 1.0150 0.7994 0.4203 0.048 Uiso 1 1 calc R
C9 C 1.1325(2) 0.79553(18) 0.13704(14) 0.0296(3) Uani 1 1 d .
H9A H 1.1472 0.7135 0.0717 0.044 Uiso 1 1 calc R
H9B H 1.2394 0.8934 0.1651 0.044 Uiso 1 1 calc R
H9C H 1.0485 0.8268 0.1041 0.044 Uiso 1 1 calc R
C10 C 0.74859(16) 0.12529(15) 0.26873(12) 0.0172(3) Uani 1 1 d .
H10 H 0.8633 0.1461 0.3052 0.021 Uiso 1 1 calc R
C11 C 0.63937(19) 0.11094(18) 0.37347(13) 0.0268(3) Uani 1 1 d .
H11A H 0.6893 0.2130 0.4403 0.040 Uiso 1 1 calc R
H11B H 0.6327 0.0179 0.4062 0.040 Uiso 1 1 calc R
H11C H 0.5265 0.0928 0.3407 0.040 Uiso 1 1 calc R
C12 C 0.67973(18) -0.03729(17) 0.16728(13) 0.0238(3) Uani 1 1 d .
H12A H 0.5634 -0.0659 0.1349 0.036 Uiso 1 1 calc R
H12B H 0.6838 -0.1251 0.2024 0.036 Uiso 1 1 calc R
H12C H 0.7479 -0.0249 0.0996 0.036 Uiso 1 1 calc R
C13 C 1.15858(18) 0.23326(18) 0.16100(14) 0.0256(3) Uani 1 1 d .
H13A H 1.0757 0.1309 0.1755 0.038 Uiso 1 1 calc R
H13B H 1.2586 0.2182 0.1385 0.038 Uiso 1 1 calc R
H13C H 1.1105 0.2611 0.0931 0.038 Uiso 1 1 calc R
C14 C 1.39740(17) 0.58690(17) 0.28041(13) 0.0215(3) Uani 1 1 d .
H14A H 1.3667 0.6134 0.2049 0.032 Uiso 1 1 calc R
H14B H 1.4951 0.5620 0.2712 0.032 Uiso 1 1 calc R
H14C H 1.4248 0.6815 0.3520 0.032 Uiso 1 1 calc R
C15 C 1.28702(18) 0.34430(19) 0.44062(14) 0.0266(3) Uani 1 1 d .
H15A H 1.3101 0.4320 0.5165 0.040 Uiso 1 1 calc R
H15B H 1.3891 0.3286 0.4268 0.040 Uiso 1 1 calc R
H15C H 1.1984 0.2414 0.4495 0.040 Uiso 1 1 calc R
N1 N 1.04494(13) 0.44044(12) 0.34202(9) 0.0136(2) Uani 1 1 d .
Si1 Si 1.21731(4) 0.40342(4) 0.30520(3) 0.01424(9) Uani 1 1 d .
Co1 Co 1.0000 0.5000 0.5000 0.01469(8) Uani 1 2 d S
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
C6 C1 C2 119.70(11) .
C6 C1 N1 120.47(11) .
C2 C1 N1 119.74(11) .
C3 C2 C1 119.07(12) .
C3 C2 C10 119.61(11) .
C1 C2 C10 121.29(11) .
C4 C3 C2 121.35(12) .
C4 C3 H3 119.3 .
C2 C3 H3 119.3 .
C3 C4 C5 119.45(12) .
C3 C4 H4 120.3 .
C5 C4 H4 120.3 .
C4 C5 C6 121.47(12) .
C4 C5 H5 119.3 .
C6 C5 H5 119.3 .
C5 C6 C1 118.95(12) .
C5 C6 C7 120.15(12) .
C1 C6 C7 120.86(11) .
C6 C7 C8 111.17(11) .
C6 C7 C9 112.71(11) .
C8 C7 C9 110.69(12) .
C6 C7 H7 107.3 .
C8 C7 H7 107.3 .
C9 C7 H7 107.3 .
C7 C8 H8A 109.5 .
C7 C8 H8B 109.5 .
H8A C8 H8B 109.5 .
C7 C8 H8C 109.5 .
H8A C8 H8C 109.5 .
H8B C8 H8C 109.5 .
C7 C9 H9A 109.5 .
C7 C9 H9B 109.5 .
H9A C9 H9B 109.5 .
C7 C9 H9C 109.5 .
H9A C9 H9C 109.5 .
H9B C9 H9C 109.5 .
C2 C10 C12 112.71(11) .
C2 C10 C11 110.55(11) .
C12 C10 C11 110.40(11) .
C2 C10 H10 107.7 .
C12 C10 H10 107.7 .
C11 C10 H10 107.7 .
C10 C11 H11A 109.5 .
C10 C11 H11B 109.5 .
H11A C11 H11B 109.5 .
C10 C11 H11C 109.5 .
H11A C11 H11C 109.5 .
H11B C11 H11C 109.5 .
C10 C12 H12A 109.5 .
C10 C12 H12B 109.5 .
H12A C12 H12B 109.5 .
C10 C12 H12C 109.5 .
H12A C12 H12C 109.5 .
H12B C12 H12C 109.5 .
Si1 C13 H13A 109.5 .
Si1 C13 H13B 109.5 .
H13A C13 H13B 109.5 .
Si1 C13 H13C 109.5 .
H13A C13 H13C 109.5 .
H13B C13 H13C 109.5 .
Si1 C14 H14A 109.5 .
Si1 C14 H14B 109.5 .
H14A C14 H14B 109.5 .
Si1 C14 H14C 109.5 .
H14A C14 H14C 109.5 .
H14B C14 H14C 109.5 .
Si1 C15 H15A 109.5 .
Si1 C15 H15B 109.5 .
H15A C15 H15B 109.5 .
Si1 C15 H15C 109.5 .
H15A C15 H15C 109.5 .
H15B C15 H15C 109.5 .
C1 N1 Si1 125.51(8) .
C1 N1 Co1 109.11(8) .
Si1 N1 Co1 125.33(6) .
N1 Si1 C13 110.39(6) .
N1 Si1 C15 106.08(6) .
C13 Si1 C15 110.58(7) .
N1 Si1 C14 113.86(6) .
C13 Si1 C14 107.65(7) .
C15 Si1 C14 108.27(6) .
N1 Co1 N1 180.00(3) 2_766
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
C1 C6 1.4129(18) .
C1 C2 1.4180(17) .
C1 N1 1.4347(16) .
C2 C3 1.3964(18) .
C2 C10 1.5207(18) .
C3 C4 1.383(2) .
C3 H3 0.9500 .
C4 C5 1.387(2) .
C4 H4 0.9500 .
C5 C6 1.3968(19) .
C5 H5 0.9500 .
C6 C7 1.5214(18) .
C7 C8 1.528(2) .
C7 C9 1.5283(19) .
C7 H7 1.0000 .
C8 H8A 0.9800 .
C8 H8B 0.9800 .
C8 H8C 0.9800 .
C9 H9A 0.9800 .
C9 H9B 0.9800 .
C9 H9C 0.9800 .
C10 C12 1.5317(18) .
C10 C11 1.5361(19) .
C10 H10 1.0000 .
C11 H11A 0.9800 .
C11 H11B 0.9800 .
C11 H11C 0.9800 .
C12 H12A 0.9800 .
C12 H12B 0.9800 .
C12 H12C 0.9800 .
C13 Si1 1.8625(14) .
C13 H13A 0.9800 .
C13 H13B 0.9800 .
C13 H13C 0.9800 .
C14 Si1 1.8711(13) .
C14 H14A 0.9800 .
C14 H14B 0.9800 .
C14 H14C 0.9800 .
C15 Si1 1.8685(14) .
C15 H15A 0.9800 .
C15 H15B 0.9800 .
C15 H15C 0.9800 .
N1 Si1 1.7320(11) .
N1 Co1 1.8339(10) .
Co1 N1 1.8339(10) 2_766
