#------------------------------------------------------------------------------
#$Date: 2016-02-20 22:30:07 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176789 $
#$URL: svn://www.crystallography.net/cod/cif/2/22/97/2229733.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_2229733
loop_
_publ_author_name
'Hao, Junsheng'
'Liu, Haimei'
'Yuan, Hai-Yan'
_publ_section_title
;
 Bis(η³-2-tert-butyl-1-trimethylsilyl-3-phenyl-1-azaallyl)nickel(II)
;
_journal_coeditor_code           JJ2080
_journal_issue                   4
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m469
_journal_paper_doi               10.1107/S1600536811009469
_journal_volume                  67
_journal_year                    2011
_chemical_formula_iupac          '[Ni (C15 H24 N Si)2]'
_chemical_formula_moiety         'C30 H48 N2 Ni Si2'
_chemical_formula_sum            'C30 H48 N2 Ni Si2'
_chemical_formula_weight         551.59
_chemical_name_systematic
;
Bis(η³-2-tert-butyl-1-trimethylsilyl-3-phenyl-1-azaallyl)nickel(II)
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 94.84(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   10.309(6)
_cell_length_b                   9.289(6)
_cell_length_c                   16.521(9)
_cell_measurement_reflns_used    1405
_cell_measurement_temperature    213(2)
_cell_measurement_theta_max      26.72
_cell_measurement_theta_min      2.43
_cell_volume                     1576.4(16)
_computing_cell_refinement       'SAINT (Bruker, 2009)'
_computing_data_collection       'SMART (Bruker, 2009)'
_computing_data_reduction        'SAINT (Bruker, 2009)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      213(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Siemens SMART CCD area-detector'
_diffrn_measurement_method       'φ and ω'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0614
_diffrn_reflns_av_sigmaI/netI    0.0790
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            7488
_diffrn_reflns_theta_full        25.01
_diffrn_reflns_theta_max         25.01
_diffrn_reflns_theta_min         2.25
_exptl_absorpt_coefficient_mu    0.711
_exptl_absorpt_correction_T_max  0.8709
_exptl_absorpt_correction_T_min  0.8150
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2009)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.162
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             596
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.632
_refine_diff_density_min         -1.220
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.357
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     166
_refine_ls_number_reflns         2776
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.357
_refine_ls_R_factor_all          0.1083
_refine_ls_R_factor_gt           0.0956
_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)+(0.0426P)²+3.0952P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1811
_refine_ls_wR_factor_ref         0.1861
_reflns_number_gt                2446
_reflns_number_total             2776
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            jj2080.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               2229733
_cod_database_fobs_code          2229733
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'
loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni Ni 0.5000 0.5000 0.0000 0.0230(3) Uani d S 1 . .
N N 0.5562(5) 0.5466(5) 0.1104(3) 0.0258(11) Uani d . 1 . .
Si Si 0.60753(18) 0.6959(2) 0.16563(10) 0.0343(5) Uani d . 1 . .
C C1 0.6907(6) 0.2919(7) 0.0403(4) 0.0319(15) Uani d . 1 . .
C C2 0.7162(8) 0.1682(7) -0.0031(4) 0.0461(18) Uani d . 1 . .
H H2 0.6477 0.1078 -0.0208 0.055 Uiso calc R 1 . .
C C3 0.8420(9) 0.1330(10) -0.0205(5) 0.067(3) Uani d . 1 . .
H H3 0.8575 0.0502 -0.0498 0.080 Uiso calc R 1 . .
C C4 0.9421(9) 0.2215(11) 0.0060(6) 0.071(3) Uani d . 1 . .
H H4 1.0265 0.1984 -0.0052 0.086 Uiso calc R 1 . .
C C5 0.9199(7) 0.3447(9) 0.0491(5) 0.057(2) Uani d . 1 . .
H H5 0.9887 0.4047 0.0670 0.068 Uiso calc R 1 . .
C C6 0.7934(7) 0.3781(7) 0.0655(4) 0.0404(17) Uani d . 1 . .
H H6 0.7783 0.4615 0.0944 0.048 Uiso calc R 1 . .
C C7 0.5535(6) 0.3120(6) 0.0600(3) 0.0288(14) Uani d . 1 . .
H H7 0.4961 0.2299 0.0465 0.035 Uiso calc R 1 . .
C C8 0.5045(6) 0.4128(6) 0.1139(3) 0.0264(13) Uani d . 1 . .
C C9 0.3895(6) 0.3787(7) 0.1648(4) 0.0354(15) Uani d . 1 . .
C C10 0.3392(9) 0.2272(9) 0.1507(6) 0.079(3) Uani d . 1 . .
H H10A 0.2748 0.2066 0.1878 0.119 Uiso calc R 1 . .
H H10B 0.4100 0.1603 0.1594 0.119 Uiso calc R 1 . .
H H10C 0.3009 0.2184 0.0959 0.119 Uiso calc R 1 . .
C C11 0.4382(8) 0.3936(10) 0.2540(4) 0.064(2) Uani d . 1 . .
H H11A 0.3679 0.3754 0.2872 0.096 Uiso calc R 1 . .
H H11B 0.4706 0.4894 0.2641 0.096 Uiso calc R 1 . .
H H11C 0.5069 0.3255 0.2671 0.096 Uiso calc R 1 . .
C C12 0.2786(7) 0.4838(9) 0.1442(5) 0.063(2) Uani d . 1 . .
H H12A 0.2472 0.4728 0.0881 0.095 Uiso calc R 1 . .
H H12B 0.3093 0.5805 0.1534 0.095 Uiso calc R 1 . .
H H12C 0.2092 0.4646 0.1779 0.095 Uiso calc R 1 . .
C C13 0.7233(8) 0.6372(9) 0.2517(4) 0.059(2) Uani d . 1 . .
H H13A 0.6765 0.5887 0.2914 0.088 Uiso calc R 1 . .
H H13B 0.7669 0.7198 0.2760 0.088 Uiso calc R 1 . .
H H13C 0.7864 0.5728 0.2320 0.088 Uiso calc R 1 . .
C C14 0.4802(8) 0.8102(8) 0.2082(5) 0.063(2) Uani d . 1 . .
H H14A 0.4187 0.8418 0.1650 0.094 Uiso calc R 1 . .
H H14B 0.5206 0.8925 0.2350 0.094 Uiso calc R 1 . .
H H14C 0.4358 0.7551 0.2465 0.094 Uiso calc R 1 . .
C C15 0.6989(9) 0.8097(9) 0.0976(5) 0.066(3) Uani d . 1 . .
H H15A 0.7616 0.7517 0.0727 0.099 Uiso calc R 1 . .
H H15B 0.7430 0.8852 0.1286 0.099 Uiso calc R 1 . .
H H15C 0.6394 0.8512 0.0562 0.099 Uiso calc R 1 . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
N Ni N . 3_665 180.0 ?
N Ni C8 . . 39.8(2) ?
N Ni C8 3_665 . 140.2(2) ?
N Ni C8 . 3_665 140.2(2) ?
N Ni C8 3_665 3_665 39.8(2) ?
C8 Ni C8 . 3_665 180.0 ?
N Ni C7 . 3_665 108.3(2) ?
N Ni C7 3_665 3_665 71.7(2) ?
C8 Ni C7 . 3_665 139.7(2) ?
C8 Ni C7 3_665 3_665 40.3(2) ?
N Ni C7 . . 71.7(2) ?
N Ni C7 3_665 . 108.3(2) ?
C8 Ni C7 . . 40.3(2) ?
C8 Ni C7 3_665 . 139.7(2) ?
C7 Ni C7 3_665 . 180.0 ?
C8 N Si . . 145.2(4) ?
C8 N Ni . . 75.2(3) ?
Si N Ni . . 137.9(3) ?
N Si C15 . . 106.7(3) ?
N Si C13 . . 108.5(3) ?
C15 Si C13 . . 107.7(4) ?
N Si C14 . . 117.6(3) ?
C15 Si C14 . . 108.2(4) ?
C13 Si C14 . . 107.7(4) ?
C6 C1 C2 . . 117.8(6) ?
C6 C1 C7 . . 125.8(6) ?
C2 C1 C7 . . 116.2(6) ?
C1 C2 C3 . . 121.4(8) ?
C1 C2 H2 . . 119.3 ?
C3 C2 H2 . . 119.3 ?
C4 C3 C2 . . 119.1(8) ?
C4 C3 H3 . . 120.5 ?
C2 C3 H3 . . 120.5 ?
C3 C4 C5 . . 120.9(8) ?
C3 C4 H4 . . 119.6 ?
C5 C4 H4 . . 119.6 ?
C4 C5 C6 . . 119.1(8) ?
C4 C5 H5 . . 120.5 ?
C6 C5 H5 . . 120.5 ?
C1 C6 C5 . . 121.8(7) ?
C1 C6 H6 . . 119.1 ?
C5 C6 H6 . . 119.1 ?
C8 C7 C1 . . 128.1(5) ?
C8 C7 Ni . . 69.3(3) ?
C1 C7 Ni . . 102.8(4) ?
C8 C7 H7 . . 114.7 ?
C1 C7 H7 . . 114.7 ?
Ni C7 H7 . . 114.7 ?
N C8 C7 . . 114.7(5) ?
N C8 C9 . . 122.3(5) ?
C7 C8 C9 . . 122.6(5) ?
N C8 Ni . . 64.9(3) ?
C7 C8 Ni . . 70.4(3) ?
C9 C8 Ni . . 128.6(4) ?
C10 C9 C12 . . 108.8(7) ?
C10 C9 C11 . . 108.4(6) ?
C12 C9 C11 . . 109.8(6) ?
C10 C9 C8 . . 112.1(5) ?
C12 C9 C8 . . 110.1(5) ?
C11 C9 C8 . . 107.7(5) ?
C9 C10 H10A . . 109.5 ?
C9 C10 H10B . . 109.5 ?
H10A C10 H10B . . 109.5 ?
C9 C10 H10C . . 109.5 ?
H10A C10 H10C . . 109.5 ?
H10B C10 H10C . . 109.5 ?
C9 C11 H11A . . 109.5 ?
C9 C11 H11B . . 109.5 ?
H11A C11 H11B . . 109.5 ?
C9 C11 H11C . . 109.5 ?
H11A C11 H11C . . 109.5 ?
H11B C11 H11C . . 109.5 ?
C9 C12 H12A . . 109.5 ?
C9 C12 H12B . . 109.5 ?
H12A C12 H12B . . 109.5 ?
C9 C12 H12C . . 109.5 ?
H12A C12 H12C . . 109.5 ?
H12B C12 H12C . . 109.5 ?
Si C13 H13A . . 109.5 ?
Si C13 H13B . . 109.5 ?
H13A C13 H13B . . 109.5 ?
Si C13 H13C . . 109.5 ?
H13A C13 H13C . . 109.5 ?
H13B C13 H13C . . 109.5 ?
Si C14 H14A . . 109.5 ?
Si C14 H14B . . 109.5 ?
H14A C14 H14B . . 109.5 ?
Si C14 H14C . . 109.5 ?
H14A C14 H14C . . 109.5 ?
H14B C14 H14C . . 109.5 ?
Si C15 H15A . . 109.5 ?
Si C15 H15B . . 109.5 ?
H15A C15 H15B . . 109.5 ?
Si C15 H15C . . 109.5 ?
H15A C15 H15C . . 109.5 ?
H15B C15 H15C . . 109.5 ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Ni N . 1.916(5) ?
Ni N 3_665 1.916(5) ?
Ni C8 . 2.045(5) ?
Ni C8 3_665 2.045(5) ?
Ni C7 3_665 2.060(6) ?
Ni C7 . 2.060(6) ?
N C8 . 1.355(7) ?
N Si . 1.720(5) ?
Si C15 . 1.857(7) ?
Si C13 . 1.860(8) ?
Si C14 . 1.871(7) ?
C1 C6 . 1.365(9) ?
C1 C2 . 1.390(9) ?
C1 C7 . 1.490(8) ?
C2 C3 . 1.390(10) ?
C2 H2 . 0.9300 ?
C3 C4 . 1.362(12) ?
C3 H3 . 0.9300 ?
C4 C5 . 1.377(11) ?
C4 H4 . 0.9300 ?
C5 C6 . 1.389(9) ?
C5 H5 . 0.9300 ?
C6 H6 . 0.9300 ?
C7 C8 . 1.414(8) ?
C7 H7 . 0.9800 ?
C8 C9 . 1.544(8) ?
C9 C10 . 1.511(10) ?
C9 C12 . 1.521(10) ?
C9 C11 . 1.523(9) ?
C10 H10A . 0.9600 ?
C10 H10B . 0.9600 ?
C10 H10C . 0.9600 ?
C11 H11A . 0.9600 ?
C11 H11B . 0.9600 ?
C11 H11C . 0.9600 ?
C12 H12A . 0.9600 ?
C12 H12B . 0.9600 ?
C12 H12C . 0.9600 ?
C13 H13A . 0.9600 ?
C13 H13B . 0.9600 ?
C13 H13C . 0.9600 ?
C14 H14A . 0.9600 ?
C14 H14B . 0.9600 ?
C14 H14C . 0.9600 ?
C15 H15A . 0.9600 ?
C15 H15B . 0.9600 ?
C15 H15C . 0.9600 ?
