#------------------------------------------------------------------------------
#$Date: 2016-03-21 17:03:29 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178766 $
#$URL: svn://www.crystallography.net/cod/cif/4/10/20/4102025.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_4102025
loop_
_publ_author_name
'Antje Meltzer'
'Shigeyoshi Inoue'
'Carsten Präsang'
'Matthias Driess'
_publ_section_title
;
 Steering S-H and N-H Bond Activation by a Stable N-Heterocyclic Silylene:
 Different Addition of H2S, NH3, and Organoamines on a Silicon(II) Ligand
 versus Its Si(II)\\rightarrowNi(CO)3Complex
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              3038
_journal_page_last               3046
_journal_paper_doi               10.1021/ja910305p
_journal_volume                  132
_journal_year                    2010
_chemical_formula_moiety         'C32 H43 N3 Ni O3 Si'
_chemical_formula_sum            'C32 H43 N3 Ni O3 Si'
_chemical_formula_weight         604.49
_chemical_name_common            HLSi(NH2)-Ni(CO)3
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           11
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yb'
_symmetry_space_group_name_H-M   'P 1 21/m 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                 111.974(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   8.8220(3)
_cell_length_b                   20.0098(4)
_cell_length_c                   9.7785(3)
_cell_measurement_reflns_used    5789
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      32.3341
_cell_measurement_theta_min      3.0238
_cell_volume                     1600.76(9)
_computing_cell_refinement
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.24 (release 21-04-2008 CrysAlis171 .NET)
(compiled Apr 21 2008,18:23:10)
;
_computing_data_collection
;
CrysAlis CCD, Oxford Diffraction Ltd.,
Version 1.171.32.24 (release 21-04-2008 CrysAlis171 .NET)
(compiled Apr 21 2008,18:23:10)
;
_computing_data_reduction
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.24 (release 21-04-2008 CrysAlis171 .NET)
(compiled Apr 21 2008,18:23:10)
;
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1986)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 16.3031
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Oxford Diffraction Xcalibur S Sapphire'
_diffrn_measurement_method       ω
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0399
_diffrn_reflns_av_sigmaI/netI    0.0432
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            12242
_diffrn_reflns_theta_full        24.99
_diffrn_reflns_theta_max         24.99
_diffrn_reflns_theta_min         3.03
_exptl_absorpt_coefficient_mu    0.679
_exptl_absorpt_correction_T_max  0.9604
_exptl_absorpt_correction_T_min  0.8819
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.24 (release 21-04-2008 CrysAlis171 .NET)
(compiled Apr 21 2008,18:23:10)
empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.254
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             644
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.393
_refine_diff_density_min         -0.341
_refine_diff_density_rms         0.058
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.103
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     199
_refine_ls_number_reflns         2907
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.146
_refine_ls_R_factor_all          0.0684
_refine_ls_R_factor_gt           0.0466
_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)+(0.0516P)²+0.2466P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0932
_refine_ls_wR_factor_ref         0.0998
_reflns_number_gt                2374
_reflns_number_total             2907
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja910305p_si_006.cif
_cod_data_source_block           m30
_cod_original_cell_volume        1600.76(8)
_cod_database_code               4102025
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z'
'-x, -y, -z'
'x, -y-1/2, 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
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni1 Ni 0.43167(6) 0.2500 0.96122(6) 0.02229(17) Uani 1 2 d S . .
Si1 Si 0.53244(12) 0.2500 0.78058(11) 0.0146(2) Uani 1 2 d S . .
N1 N 0.4809(2) 0.31772(10) 0.6415(2) 0.0145(5) Uani 1 1 d . . .
C1 C 0.5159(4) 0.37268(13) 0.4287(3) 0.0271(7) Uani 1 1 d . . .
H1A H 0.4178 0.3996 0.4122 0.041 Uiso 1 1 calc R . .
H1B H 0.5184 0.3587 0.3335 0.041 Uiso 1 1 calc R . .
H1C H 0.6133 0.3994 0.4820 0.041 Uiso 1 1 calc R . .
C2 C 0.5130(3) 0.31174(13) 0.5185(3) 0.0183(6) Uani 1 1 d . . .
C3 C 0.5423(4) 0.2500 0.4686(4) 0.0199(8) Uani 1 2 d S . .
H3 H 0.5864 0.2500 0.3936 0.024 Uiso 1 2 calc SR . .
C6 C 0.4277(3) 0.38234(12) 0.6754(3) 0.0199(6) Uani 1 1 d . . .
C7 C 0.2596(4) 0.39539(14) 0.6249(4) 0.0332(8) Uani 1 1 d . . .
C8 C 0.2105(4) 0.45755(15) 0.6568(5) 0.0499(10) Uani 1 1 d . . .
H8 H 0.0973 0.4681 0.6209 0.060 Uiso 1 1 calc R . .
C9 C 0.3227(5) 0.50437(15) 0.7398(4) 0.0498(10) Uani 1 1 d . . .
H9 H 0.2864 0.5462 0.7622 0.060 Uiso 1 1 calc R . .
C10 C 0.4859(4) 0.49023(14) 0.7893(4) 0.0371(8) Uani 1 1 d . . .
H10 H 0.5618 0.5225 0.8471 0.045 Uiso 1 1 calc R . .
C11 C 0.5446(3) 0.42989(13) 0.7575(3) 0.0234(6) Uani 1 1 d . . .
C12 C 0.1329(4) 0.34501(15) 0.5350(5) 0.0483(10) Uani 1 1 d . . .
H12 H 0.1845 0.2997 0.5556 0.058 Uiso 1 1 calc R . .
C13 C 0.0780(6) 0.3572(2) 0.3724(5) 0.0771(14) Uani 1 1 d U . .
H13A H 0.0370 0.4031 0.3502 0.116 Uiso 1 1 calc R . .
H13B H -0.0093 0.3257 0.3194 0.116 Uiso 1 1 calc R . .
H13C H 0.1704 0.3509 0.3411 0.116 Uiso 1 1 calc R . .
C14 C -0.0163(5) 0.3437(2) 0.5774(5) 0.0755(13) Uani 1 1 d U . .
H14A H -0.0766 0.3858 0.5475 0.113 Uiso 1 1 calc R . .
H14B H 0.0188 0.3382 0.6844 0.113 Uiso 1 1 calc R . .
H14C H -0.0871 0.3063 0.5275 0.113 Uiso 1 1 calc R . .
C15 C 0.7267(4) 0.41891(13) 0.8094(3) 0.0283(7) Uani 1 1 d . . .
H15 H 0.7456 0.3766 0.7638 0.034 Uiso 1 1 calc R . .
C16 C 0.8046(5) 0.41106(17) 0.9770(3) 0.0497(9) Uani 1 1 d . . .
H16A H 0.7993 0.4537 1.0242 0.074 Uiso 1 1 calc R . .
H16B H 0.9190 0.3975 1.0053 0.074 Uiso 1 1 calc R . .
H16C H 0.7453 0.3769 1.0089 0.074 Uiso 1 1 calc R . .
C17 C 0.8129(4) 0.47596(15) 0.7611(4) 0.0391(8) Uani 1 1 d . . .
H17A H 0.7621 0.4817 0.6540 0.059 Uiso 1 1 calc R . .
H17B H 0.9288 0.4649 0.7887 0.059 Uiso 1 1 calc R . .
H17C H 0.8028 0.5175 0.8100 0.059 Uiso 1 1 calc R . .
C31 C 0.3187(4) 0.32454(18) 0.9603(4) 0.0398(8) Uani 1 1 d . . .
C32 C 0.6195(6) 0.2500 1.1149(5) 0.0357(11) Uani 1 2 d S . .
O1 O 0.2499(3) 0.37174(14) 0.9677(3) 0.0688(9) Uani 1 1 d . . .
O2 O 0.7449(4) 0.2500 1.2082(4) 0.0625(11) Uani 1 2 d S . .
N3 N 0.7412(4) 0.2500 0.8388(4) 0.0226(8) Uani 1 2 d S . .
H1 H 0.788(5) 0.2500 0.782(5) 0.027 Uiso 1 2 d S . .
H2 H 0.791(5) 0.2500 0.920(5) 0.027 Uiso 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'
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'
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
C32 Ni1 C31 110.25(13) . 4_565 ?
C32 Ni1 C31 110.25(13) . . ?
C31 Ni1 C31 112.7(2) 4_565 . ?
C32 Ni1 Si1 98.44(14) . . ?
C31 Ni1 Si1 112.18(10) 4_565 . ?
C31 Ni1 Si1 112.18(10) . . ?
N3 Si1 N1 100.51(11) . 4_565 ?
N3 Si1 N1 100.51(11) . . ?
N1 Si1 N1 94.04(13) 4_565 . ?
N3 Si1 Ni1 115.44(14) . . ?
N1 Si1 Ni1 120.99(7) 4_565 . ?
N1 Si1 Ni1 120.99(7) . . ?
C2 N1 C6 118.6(2) . . ?
C2 N1 Si1 121.17(17) . . ?
C6 N1 Si1 119.61(16) . . ?
N1 C2 C3 121.7(2) . . ?
N1 C2 C1 120.4(2) . . ?
C3 C2 C1 118.0(2) . . ?
C2 C3 C2 125.8(3) 4_565 . ?
C7 C6 C11 121.8(2) . . ?
C7 C6 N1 118.3(2) . . ?
C11 C6 N1 119.9(2) . . ?
C8 C7 C6 117.7(3) . . ?
C8 C7 C12 120.0(3) . . ?
C6 C7 C12 122.2(3) . . ?
C9 C8 C7 121.5(3) . . ?
C10 C9 C8 119.7(3) . . ?
C9 C10 C11 122.0(3) . . ?
C10 C11 C6 117.2(3) . . ?
C10 C11 C15 119.2(3) . . ?
C6 C11 C15 123.5(2) . . ?
C13 C12 C7 112.4(3) . . ?
C13 C12 C14 108.8(3) . . ?
C7 C12 C14 112.2(3) . . ?
C11 C15 C16 111.8(3) . . ?
C11 C15 C17 112.0(2) . . ?
C16 C15 C17 109.2(3) . . ?
O1 C31 Ni1 176.3(3) . . ?
O2 C32 Ni1 176.0(4) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ni1 C32 1.772(5) . ?
Ni1 C31 1.792(3) 4_565 ?
Ni1 C31 1.792(3) . ?
Ni1 Si1 2.2551(11) . ?
Si1 N3 1.712(4) . ?
Si1 N1 1.852(2) 4_565 ?
Si1 N1 1.852(2) . ?
N1 C2 1.340(3) . ?
N1 C6 1.456(3) . ?
C1 C2 1.509(3) . ?
C2 C3 1.388(3) . ?
C3 C2 1.388(3) 4_565 ?
C6 C7 1.401(4) . ?
C6 C11 1.412(4) . ?
C7 C8 1.391(4) . ?
C7 C12 1.517(5) . ?
C8 C9 1.384(5) . ?
C9 C10 1.366(5) . ?
C10 C11 1.394(4) . ?
C11 C15 1.509(4) . ?
C12 C13 1.499(6) . ?
C12 C14 1.521(5) . ?
C15 C16 1.529(4) . ?
C15 C17 1.541(4) . ?
C31 O1 1.140(4) . ?
C32 O2 1.141(5) . ?
