#------------------------------------------------------------------------------
#$Date: 2017-03-04 03:50:55 +0200 (Sat, 04 Mar 2017) $
#$Revision: 192941 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/34/53/4345376.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_4345376
loop_
_publ_author_name
'Shan, Yu-Liang'
'Leong, Bi-Xiang'
'Li, Yongxin'
'Ganguly, Rakesh'
'So, Cheuk-Wai'
_publ_section_title
;
 Donor-Acceptor Stabilized Tetra(silanimine).
;
_journal_issue                   3
_journal_name_full               'Inorganic chemistry'
_journal_page_first              1609
_journal_page_last               1615
_journal_paper_doi               10.1021/acs.inorgchem.6b02727
_journal_volume                  56
_journal_year                    2017
_chemical_formula_sum            'C18 H32 Cl3 Ge N3 Si2'
_chemical_formula_weight         525.58
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_cell_angle_alpha                90
_cell_angle_beta                 106.236(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.9206(8)
_cell_length_b                   8.2680(4)
_cell_length_c                   18.3628(9)
_cell_measurement_reflns_used    3602
_cell_measurement_temperature    103.(2)
_cell_measurement_theta_max      27.5037
_cell_measurement_theta_min      2.7210
_cell_volume                     2466.5(2)
_computing_cell_refinement       'SAINT V8.34A (Bruker AXS Inc., 2013)'
_computing_data_collection       'APEX2 (Bruker AXS Inc., 2014)'
_computing_data_reduction        'SAINT V8.34A (Bruker AXS Inc., 2013)'
_computing_molecular_graphics    'XP (Bruker AXS Inc., 2014)'
_computing_publication_material  'APEX2 (Bruker AXS Inc., 2014)'
_computing_structure_refinement  'SHELXL-2014/6 (Sheldrick, 2014)'
_diffrn_ambient_temperature      103.(2)
_diffrn_detector_area_resol_mean 8.3333
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0935
_diffrn_reflns_av_unetI/netI     0.0930
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            39499
_diffrn_reflns_theta_full        32.77
_diffrn_reflns_theta_max         32.77
_diffrn_reflns_theta_min         2.76
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    1.674
_exptl_absorpt_correction_T_max  0.78
_exptl_absorpt_correction_T_min  0.57
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2014/4 (Bruker AXS Inc.)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.415
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1088
_exptl_crystal_size_max          0.420
_exptl_crystal_size_mid          0.220
_exptl_crystal_size_min          0.160
_refine_diff_density_max         0.855
_refine_diff_density_min         -0.688
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.016
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     253
_refine_ls_number_reflns         9056
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.016
_refine_ls_R_factor_all          0.0958
_refine_ls_R_factor_gt           0.0508
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0452P)²+0.0148P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1041
_refine_ls_wR_factor_ref         0.1198
_reflns_number_gt                5869
_reflns_number_total             9056
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            ic6b02727_si_001.cif
_cod_data_source_block           I
_cod_database_code               4345376
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -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_adp
_atom_site_refinement_flags_posn
_atom_site_occupancy
C C1 0.12501(14) 0.2411(3) 0.32501(15) 0.0137(5) Uani d . . 1
C C2 0.11737(17) 0.3365(3) 0.39383(17) 0.0222(6) Uani d . . 1
H H2A 0.1056 0.2621 0.431 0.033 Uiso calc U R 1
H H2B 0.0725 0.4151 0.3779 0.033 Uiso calc U R 1
H H2C 0.1691 0.3936 0.4168 0.033 Uiso calc U R 1
C C3 0.04665(15) 0.1452(3) 0.28821(18) 0.0233(6) Uani d . . 1
H H3A 0.0549 0.0805 0.2462 0.035 Uiso calc U R 1
H H3B 0.0008 0.2203 0.2688 0.035 Uiso calc U R 1
H H3C 0.0341 0.0735 0.326 0.035 Uiso calc U R 1
C C4 0.14411(17) 0.3567(3) 0.26711(17) 0.0212(6) Uani d . . 1
H H4A 0.1969 0.4105 0.2897 0.032 Uiso calc U R 1
H H4B 0.1004 0.4381 0.2522 0.032 Uiso calc U R 1
H H4C 0.1472 0.2957 0.2223 0.032 Uiso calc U R 1
C C5 0.21382(14) 0.0043(3) 0.39593(14) 0.0098(5) Uani d . . 1
C C6 0.16180(14) -0.0581(3) 0.44246(14) 0.0116(5) Uani d . . 1
C C7 0.10529(15) -0.1805(3) 0.41404(16) 0.0182(5) Uani d . . 1
H H7 0.0988 -0.2215 0.3644 0.022 Uiso calc U R 1
C C8 0.05829(16) -0.2427(3) 0.45870(18) 0.0230(6) Uani d . . 1
H H8 0.0191 -0.3256 0.4396 0.028 Uiso calc U R 1
C C9 0.06906(17) -0.1828(3) 0.53148(17) 0.0230(6) Uani d . . 1
H H9 0.0379 -0.2265 0.5625 0.028 Uiso calc U R 1
C C10 0.12468(17) -0.0602(3) 0.55911(17) 0.0224(6) Uani d . . 1
H H10 0.1311 -0.0188 0.6087 0.027 Uiso calc U R 1
C C11 0.17106(16) 0.0025(3) 0.51455(15) 0.0173(5) Uani d . . 1
H H11 0.2093 0.0871 0.5335 0.021 Uiso calc U R 1
C C12 0.34259(15) -0.1773(3) 0.44036(15) 0.0143(5) Uani d . . 1
C C13 0.29500(17) -0.3316(3) 0.44568(18) 0.0231(6) Uani d . . 1
H H13A 0.2581 -0.3117 0.4774 0.035 Uiso calc U R 1
H H13B 0.3338 -0.4179 0.4683 0.035 Uiso calc U R 1
H H13C 0.2626 -0.3641 0.3948 0.035 Uiso calc U R 1
C C14 0.38435(18) -0.1114(4) 0.51896(16) 0.0267(7) Uani d . . 1
H H14A 0.4128 -0.0103 0.5144 0.04 Uiso calc U R 1
H H14B 0.4243 -0.1907 0.5473 0.04 Uiso calc U R 1
H H14C 0.3429 -0.0907 0.5459 0.04 Uiso calc U R 1
C C15 0.40590(17) -0.2129(3) 0.39760(17) 0.0252(6) Uani d . . 1
H H15A 0.3781 -0.2577 0.3476 0.038 Uiso calc U R 1
H H15B 0.4461 -0.2914 0.4263 0.038 Uiso calc U R 1
H H15C 0.4343 -0.1127 0.3914 0.038 Uiso calc U R 1
C C16 0.33167(16) 0.4240(3) 0.20430(16) 0.0191(6) Uani d . . 1
H H16A 0.273 0.4232 0.1769 0.029 Uiso calc U R 1
H H16B 0.3614 0.4926 0.1772 0.029 Uiso calc U R 1
H H16C 0.3389 0.4668 0.2555 0.029 Uiso calc U R 1
C C17 0.37146(17) 0.1457(3) 0.11306(16) 0.0229(6) Uani d . . 1
H H17A 0.396 0.0377 0.1156 0.034 Uiso calc U R 1
H H17B 0.4031 0.2219 0.0914 0.034 Uiso calc U R 1
H H17C 0.3145 0.142 0.081 0.034 Uiso calc U R 1
C C18 0.48362(16) 0.2097(4) 0.26833(17) 0.0252(6) Uani d . . 1
H H18A 0.4885 0.2577 0.3182 0.038 Uiso calc U R 1
H H18B 0.5169 0.272 0.2423 0.038 Uiso calc U R 1
H H18C 0.5033 0.0977 0.2747 0.038 Uiso calc U R 1
Cl Cl1 0.37132(4) 0.27668(8) 0.39745(4) 0.01852(14) Uani d . . 1
Cl Cl2 0.17641(4) -0.20673(8) 0.23929(4) 0.02169(15) Uani d . . 1
Cl Cl3 0.15453(4) 0.08491(8) 0.10273(4) 0.02559(16) Uani d . . 1
Ge Ge1 0.25549(2) -0.08808(3) 0.17081(2) 0.01620(8) Uani d . . 1
N N1 0.19723(12) 0.1294(2) 0.34719(12) 0.0107(4) Uani d . . 1
N N2 0.28807(12) -0.0510(2) 0.39475(12) 0.0110(4) Uani d . . 1
N N3 0.31247(12) 0.0812(2) 0.24779(12) 0.0131(4) Uani d . . 1
Si Si1 0.29538(4) 0.10687(8) 0.33088(4) 0.01091(14) Uani d . . 1
Si Si2 0.37313(4) 0.21324(9) 0.21054(4) 0.01538(15) Uani d . . 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'
Cl Cl 0.1484 0.1585 '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
N1 C1 C2 110.2(2)
N1 C1 C3 110.0(2)
C2 C1 C3 111.7(2)
N1 C1 C4 105.1(2)
C2 C1 C4 109.6(2)
C3 C1 C4 110.0(2)
N2 C5 N1 105.9(2)
N2 C5 C6 126.9(2)
N1 C5 C6 127.2(2)
N2 C5 Si1 53.04(12)
N1 C5 Si1 52.88(12)
C6 C5 Si1 177.01(17)
C11 C6 C7 120.3(2)
C11 C6 C5 120.0(2)
C7 C6 C5 119.7(2)
C6 C7 C8 119.6(3)
C9 C8 C7 119.5(3)
C10 C9 C8 120.6(3)
C9 C10 C11 119.9(3)
C6 C11 C10 120.0(2)
N2 C12 C14 109.5(2)
N2 C12 C15 105.1(2)
C14 C12 C15 110.6(2)
N2 C12 C13 111.6(2)
C14 C12 C13 110.6(2)
C15 C12 C13 109.3(2)
N3 Ge1 Cl2 98.58(6)
N3 Ge1 Cl3 94.89(6)
Cl2 Ge1 Cl3 96.02(3)
C5 N1 C1 131.2(2)
C5 N1 Si1 90.03(15)
C1 N1 Si1 138.59(17)
C5 N2 C12 131.7(2)
C5 N2 Si1 89.93(15)
C12 N2 Si1 137.63(17)
Si1 N3 Si2 123.57(12)
Si1 N3 Ge1 124.22(12)
Si2 N3 Ge1 111.80(11)
N3 Si1 N1 125.79(11)
N3 Si1 N2 125.37(10)
N1 Si1 N2 74.08(9)
N3 Si1 Cl1 113.36(8)
N1 Si1 Cl1 106.61(8)
N2 Si1 Cl1 104.79(7)
N3 Si1 C5 138.06(10)
N1 Si1 C5 37.09(9)
N2 Si1 C5 37.03(9)
Cl1 Si1 C5 108.55(7)
N3 Si2 C17 109.41(11)
N3 Si2 C16 110.60(11)
C17 Si2 C16 108.36(13)
N3 Si2 C18 111.58(12)
C17 Si2 C18 106.46(14)
C16 Si2 C18 110.29(13)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
C1 N1 1.494(3)
C1 C2 1.526(4)
C1 C3 1.530(3)
C1 C4 1.530(4)
C5 N2 1.343(3)
C5 N1 1.345(3)
C5 C6 1.480(3)
C5 Si1 2.230(3)
C6 C11 1.383(4)
C6 C7 1.390(3)
C7 C8 1.391(4)
C8 C9 1.389(4)
C9 C10 1.380(4)
C10 C11 1.383(4)
C12 N2 1.487(3)
C12 C14 1.519(4)
C12 C15 1.524(4)
C12 C13 1.526(4)
C16 Si2 1.870(3)
C17 Si2 1.868(3)
C18 Si2 1.874(3)
Cl1 Si1 2.0586(9)
Cl2 Ge1 2.2968(7)
Cl3 Ge1 2.3093(7)
Ge1 N3 2.031(2)
N1 Si1 1.778(2)
N2 Si1 1.782(2)
N3 Si1 1.644(2)
N3 Si2 1.762(2)
