#------------------------------------------------------------------------------
#$Date: 2025-08-20 21:19:29 +0200 (Wed 20 de Aug de 2025) $
#$Revision: 301836 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/01/4300160.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_4300160
loop_
_publ_author_name
'Stephen R. Foley'
'Yuanlin Zhou'
'Glenn P. A. Yap'
'Darrin S. Richeson'
_publ_section_title
;
Synthesis of MII[N(SiMe3)2][Me3SiNC(tBu)NSiMe3] (M = Sn, Ge) from Amidinate
Precursors: Active Catalysts for Phenyl Isocyanate Cyclization
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              924
_journal_page_last               929
_journal_paper_doi               10.1021/ic991004b
_journal_volume                  39
_journal_year                    2000
_chemical_formula_sum            'C17 H45 Ge N3 Si4'
_chemical_formula_weight         476.51
_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                 111.806(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.791(1)
_cell_length_b                   10.176(1)
_cell_length_c                   19.542(2)
_cell_measurement_reflns_used    'reflections from 60 data frames'
_cell_measurement_temperature    203(2)
_cell_measurement_theta_max      28.29
_cell_measurement_theta_min      1.47
_cell_volume                     2730.9(4)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      203(2)
_diffrn_measured_fraction_theta_full 0.914
_diffrn_measured_fraction_theta_max 0.914
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_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  0.0591
_diffrn_reflns_av_sigmaI/netI    0.0736
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            16894
_diffrn_reflns_theta_full        28.52
_diffrn_reflns_theta_max         28.52
_diffrn_reflns_theta_min         2.17
_diffrn_standards_decay_%        <1
_diffrn_standards_number         '50 standard frames at start and end'
_exptl_absorpt_coefficient_mu    1.304
_exptl_absorpt_correction_T_max  0.928073
_exptl_absorpt_correction_T_min  0.522369
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Blessing, Acta Cryst. (1995) A51 33-38.'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.159
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1024
_exptl_crystal_size_max          .4
_exptl_crystal_size_mid          .4
_exptl_crystal_size_min          .4
_refine_diff_density_max         0.621
_refine_diff_density_min         -0.659
_refine_diff_density_rms         0.087
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     226
_refine_ls_number_reflns         6339
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.057
_refine_ls_R_factor_all          0.0603
_refine_ls_R_factor_gt           0.0442
_refine_ls_shift/su_max          0.014
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0300P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0886
_refine_ls_wR_factor_ref         0.0912
_reflns_number_gt                4547
_reflns_number_total             6339
_reflns_threshold_expression     >2sigma(I)
_cod_database_code               4300160
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_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
Ge Ge 0.415592(19) 0.06255(3) 0.231038(14) 0.02848(8) Uani 1 1 d . . .
Si1 Si 0.22445(5) -0.12194(8) 0.13773(4) 0.03813(19) Uani 1 1 d . . .
Si2 Si 0.45558(6) 0.32915(8) 0.14962(5) 0.03878(19) Uani 1 1 d . . .
Si3 Si 0.56063(5) -0.09244(7) 0.16619(4) 0.03436(18) Uani 1 1 d . . .
Si4 Si 0.58479(5) -0.10618(8) 0.32625(4) 0.03503(18) Uani 1 1 d . . .
N1 N 0.30323(14) 0.0059(2) 0.13812(11) 0.0285(5) Uani 1 1 d . . .
N2 N 0.39564(14) 0.1783(2) 0.14126(11) 0.0305(5) Uani 1 1 d . . .
N3 N 0.52052(14) -0.0520(2) 0.23685(11) 0.0275(4) Uani 1 1 d . . .
C1 C 0.2851(2) -0.2036(3) 0.22801(17) 0.0530(8) Uani 1 1 d . . .
H1A H 0.3487 -0.2350 0.2318 0.080 Uiso 1 1 calc R . .
H1B H 0.2458 -0.2773 0.2322 0.080 Uiso 1 1 calc R . .
H1C H 0.2924 -0.1414 0.2673 0.080 Uiso 1 1 calc R . .
C2 C 0.2098(3) -0.2483(3) 0.06538(19) 0.0688(10) Uani 1 1 d . . .
H2A H 0.2735 -0.2761 0.0673 0.103 Uiso 1 1 calc R . .
H2B H 0.1734 -0.2113 0.0172 0.103 Uiso 1 1 calc R . .
H2C H 0.1750 -0.3235 0.0739 0.103 Uiso 1 1 calc R . .
C3 C 0.1016(2) -0.0668(4) 0.1321(2) 0.0673(11) Uani 1 1 d . . .
H3A H 0.0685 -0.0229 0.0854 0.101 Uiso 1 1 calc R . .
H3B H 0.1085 -0.0065 0.1722 0.101 Uiso 1 1 calc R . .
H3C H 0.0637 -0.1425 0.1358 0.101 Uiso 1 1 calc R . .
C4 C 0.5581(2) 0.3210(3) 0.24030(17) 0.0501(8) Uani 1 1 d . . .
H4A H 0.6003 0.2478 0.2404 0.075 Uiso 1 1 calc R . .
H4B H 0.5327 0.3086 0.2790 0.075 Uiso 1 1 calc R . .
H4C H 0.5950 0.4022 0.2488 0.075 Uiso 1 1 calc R . .
C5 C 0.5080(2) 0.3593(3) 0.07757(18) 0.0540(8) Uani 1 1 d . . .
H5A H 0.4557 0.3643 0.0296 0.081 Uiso 1 1 calc R . .
H5B H 0.5515 0.2879 0.0778 0.081 Uiso 1 1 calc R . .
H5C H 0.5438 0.4414 0.0879 0.081 Uiso 1 1 calc R . .
C6 C 0.3779(2) 0.4706(3) 0.1531(2) 0.0613(9) Uani 1 1 d . . .
H6A H 0.3240 0.4787 0.1062 0.092 Uiso 1 1 calc R . .
H6B H 0.4164 0.5506 0.1630 0.092 Uiso 1 1 calc R . .
H6C H 0.3530 0.4564 0.1920 0.092 Uiso 1 1 calc R . .
C7 C 0.31212(18) 0.1160(3) 0.10403(13) 0.0291(5) Uani 1 1 d . . .
C8 C 0.23321(19) 0.1681(3) 0.03345(14) 0.0351(6) Uani 1 1 d . . .
C9 C 0.2758(2) 0.2569(3) -0.01035(16) 0.0523(8) Uani 1 1 d . . .
H9A H 0.3098 0.3299 0.0203 0.079 Uiso 1 1 calc R . .
H9B H 0.2236 0.2901 -0.0536 0.079 Uiso 1 1 calc R . .
H9C H 0.3210 0.2068 -0.0255 0.079 Uiso 1 1 calc R . .
C10 C 0.1594(2) 0.2465(3) 0.05569(17) 0.0497(8) Uani 1 1 d . . .
H10A H 0.1925 0.3184 0.0878 0.075 Uiso 1 1 calc R . .
H10B H 0.1302 0.1891 0.0814 0.075 Uiso 1 1 calc R . .
H10C H 0.1090 0.2813 0.0119 0.075 Uiso 1 1 calc R . .
C11 C 0.1810(2) 0.0536(3) -0.01710(15) 0.0477(8) Uani 1 1 d . . .
H11A H 0.1525 -0.0040 0.0089 0.072 Uiso 1 1 calc R . .
H11B H 0.2275 0.0046 -0.0313 0.072 Uiso 1 1 calc R . .
H11C H 0.1302 0.0879 -0.0608 0.072 Uiso 1 1 calc R . .
C12 C 0.6161(3) -0.2600(3) 0.17884(19) 0.0558(9) Uani 1 1 d . . .
H12A H 0.5688 -0.3243 0.1808 0.084 Uiso 1 1 calc R . .
H12B H 0.6727 -0.2626 0.2244 0.084 Uiso 1 1 calc R . .
H12C H 0.6357 -0.2800 0.1378 0.084 Uiso 1 1 calc R . .
C13 C 0.6558(2) 0.0241(3) 0.16142(19) 0.0569(9) Uani 1 1 d . . .
H13A H 0.7087 0.0283 0.2091 0.085 Uiso 1 1 calc R . .
H13B H 0.6275 0.1108 0.1479 0.085 Uiso 1 1 calc R . .
H13C H 0.6807 -0.0063 0.1247 0.085 Uiso 1 1 calc R . .
C14 C 0.4630(2) -0.0968(4) 0.07308(16) 0.0617(10) Uani 1 1 d . . .
H14A H 0.4122 -0.1569 0.0732 0.093 Uiso 1 1 calc R . .
H14B H 0.4900 -0.1262 0.0374 0.093 Uiso 1 1 calc R . .
H14C H 0.4358 -0.0094 0.0599 0.093 Uiso 1 1 calc R . .
C15 C 0.7188(2) -0.0751(4) 0.35560(18) 0.0594(9) Uani 1 1 d . . .
H15A H 0.7299 0.0176 0.3500 0.089 Uiso 1 1 calc R . .
H15B H 0.7446 -0.1265 0.3252 0.089 Uiso 1 1 calc R . .
H15C H 0.7513 -0.1002 0.4068 0.089 Uiso 1 1 calc R . .
C16 C 0.5674(3) -0.2854(3) 0.33847(18) 0.0572(9) Uani 1 1 d . . .
H16A H 0.4985 -0.3041 0.3240 0.086 Uiso 1 1 calc R . .
H16B H 0.6011 -0.3092 0.3898 0.086 Uiso 1 1 calc R . .
H16C H 0.5935 -0.3359 0.3079 0.086 Uiso 1 1 calc R . .
C17 C 0.5457(2) -0.0197(3) 0.39512(15) 0.0570(9) Uani 1 1 d . . .
H17A H 0.5528 0.0745 0.3910 0.085 Uiso 1 1 calc R . .
H17B H 0.5859 -0.0484 0.4444 0.085 Uiso 1 1 calc R . .
H17C H 0.4781 -0.0402 0.3856 0.085 Uiso 1 1 calc R . .
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'
Ge Ge 0.1547 1.8001 '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
N3 Ge N1 104.84(8) . . ?
N3 Ge N2 104.96(8) . . ?
N1 Ge N2 65.65(8) . . ?
N3 Ge C7 112.61(8) . . ?
N1 Ge C7 33.08(8) . . ?
N2 Ge C7 33.19(8) . . ?
N1 Si1 C1 104.13(12) . . ?
N1 Si1 C2 114.02(14) . . ?
C1 Si1 C2 106.96(16) . . ?
N1 Si1 C3 114.24(14) . . ?
C1 Si1 C3 107.89(15) . . ?
C2 Si1 C3 109.06(17) . . ?
N2 Si2 C4 104.81(12) . . ?
N2 Si2 C6 112.61(13) . . ?
C4 Si2 C6 107.25(15) . . ?
N2 Si2 C5 114.30(13) . . ?
C4 Si2 C5 107.82(14) . . ?
C6 Si2 C5 109.60(16) . . ?
N3 Si3 C14 114.35(12) . . ?
N3 Si3 C13 111.97(13) . . ?
C14 Si3 C13 107.00(17) . . ?
N3 Si3 C12 111.89(13) . . ?
C14 Si3 C12 104.57(16) . . ?
C13 Si3 C12 106.47(15) . . ?
N3 Si4 C17 111.94(12) . . ?
N3 Si4 C16 112.81(13) . . ?
C17 Si4 C16 105.86(16) . . ?
N3 Si4 C15 112.03(13) . . ?
C17 Si4 C15 105.94(16) . . ?
C16 Si4 C15 107.80(16) . . ?
C7 N1 Si1 144.41(18) . . ?
C7 N1 Ge 90.49(15) . . ?
Si1 N1 Ge 122.50(11) . . ?
C7 N2 Si2 143.17(18) . . ?
C7 N2 Ge 90.18(15) . . ?
Si2 N2 Ge 121.29(11) . . ?
Si4 N3 Si3 120.07(11) . . ?
Si4 N3 Ge 112.46(10) . . ?
Si3 N3 Ge 127.24(11) . . ?
N1 C7 N2 111.6(2) . . ?
N1 C7 C8 123.8(2) . . ?
N2 C7 C8 124.4(2) . . ?
N1 C7 Ge 56.43(12) . . ?
N2 C7 Ge 56.64(12) . . ?
C8 C7 Ge 166.10(17) . . ?
C9 C8 C7 111.9(2) . . ?
C9 C8 C11 107.5(2) . . ?
C7 C8 C11 110.4(2) . . ?
C9 C8 C10 109.5(2) . . ?
C7 C8 C10 107.9(2) . . ?
C11 C8 C10 109.6(2) . . ?
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
Ge N3 1.9101(19) . ?
Ge N1 2.037(2) . ?
Ge N2 2.042(2) . ?
Ge C7 2.445(2) . ?
Si1 N1 1.745(2) . ?
Si1 C1 1.853(3) . ?
Si1 C2 1.864(3) . ?
Si1 C3 1.866(3) . ?
Si2 N2 1.749(2) . ?
Si2 C4 1.858(3) . ?
Si2 C6 1.858(3) . ?
Si2 C5 1.867(3) . ?
Si3 N3 1.743(2) . ?
Si3 C14 1.857(3) . ?
Si3 C13 1.870(3) . ?
Si3 C12 1.868(3) . ?
Si4 N3 1.740(2) . ?
Si4 C17 1.871(3) . ?
Si4 C16 1.870(3) . ?
Si4 C15 1.874(3) . ?
N1 C7 1.334(3) . ?
N2 C7 1.338(3) . ?
C7 C8 1.533(3) . ?
C8 C9 1.532(4) . ?
C8 C11 1.537(4) . ?
C8 C10 1.540(4) . ?
loop_
_cod_related_entry_id
_cod_related_entry_database
_cod_related_entry_code
1 PubChem 139126113
