#------------------------------------------------------------------------------
#$Date: 2019-11-24 11:50:55 +0200 (Sun, 24 Nov 2019) $
#$Revision: 237850 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/08/88/4088833.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_4088833
loop_
_publ_author_name
'Walewska, Małgorzata'
'Hlina, Johann'
'Baumgartner, Judith'
'Müller, Thomas'
'Marschner, Christoph'
_publ_section_title
;
 Basic Reactivity Pattern of a Cyclic Disilylated Germylene.
;
_journal_issue                   16
_journal_name_full               Organometallics
_journal_page_first              2728
_journal_page_last               2737
_journal_paper_doi               10.1021/acs.organomet.6b00482
_journal_volume                  35
_journal_year                    2016
_chemical_formula_sum            'C16 H50 Ge O Si8'
_chemical_formula_weight         555.87
_space_group_IT_number           13
_space_group_name_Hall           '-P 2yc'
_space_group_name_H-M_alt        'P 1 2/c 1'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 1 2/c 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                 119.13(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   12.715(3)
_cell_length_b                   8.6713(17)
_cell_length_c                   16.752(6)
_cell_measurement_reflns_used    8209
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      52.497
_cell_measurement_theta_min      4.705
_cell_volume                     1613.4(8)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_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      100(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'SMART APEX'
_diffrn_measurement_method       'ω 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  0.0329
_diffrn_reflns_av_sigmaI/netI    0.0235
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            12278
_diffrn_reflns_theta_full        26.23
_diffrn_reflns_theta_max         26.23
_diffrn_reflns_theta_min         1.83
_exptl_absorpt_coefficient_mu    1.253
_exptl_absorpt_correction_T_max  0.7701
_exptl_absorpt_correction_T_min  0.6025
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.144
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       blocks
_exptl_crystal_F_000             596
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.22
_refine_diff_density_max         0.595
_refine_diff_density_min         -0.186
_refine_diff_density_rms         0.064
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.094
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     139
_refine_ls_number_reflns         3250
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.094
_refine_ls_R_factor_all          0.0251
_refine_ls_R_factor_gt           0.0238
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0399P)²+0.1410P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0639
_refine_ls_wR_factor_ref         0.0645
_reflns_number_gt                3052
_reflns_number_total             3250
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om6b00482_si_002.cif
_cod_data_source_block           8_1096j
_cod_original_sg_symbol_H-M      P2/c
_cod_database_code               4088833
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'-x, -y, -z'
'x, -y, 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
Ge1 Ge 0.0000 0.59164(2) 0.2500 0.01848(8) Uani 1 2 d S
Si3 Si 0.25498(4) 0.66551(4) 0.49387(3) 0.02202(10) Uani 1 1 d .
Si4 Si 0.30428(3) 0.72342(4) 0.28308(3) 0.02082(10) Uani 1 1 d .
Si1 Si 0.17171(3) 0.74883(4) 0.34212(2) 0.01673(10) Uani 1 1 d .
Si2 Si 0.09293(3) 1.00094(4) 0.31827(2) 0.01828(10) Uani 1 1 d .
C2 C 0.19812(14) 1.14470(17) 0.30963(11) 0.0292(3) Uani 1 1 d .
H2A H 0.1618 1.2476 0.2981 0.044 Uiso 1 1 calc R
H2B H 0.2126 1.1155 0.2593 0.044 Uiso 1 1 calc R
H2C H 0.2747 1.1457 0.3670 0.044 Uiso 1 1 calc R
C1 C 0.06810(15) 1.06515(18) 0.41510(11) 0.0295(3) Uani 1 1 d .
H1A H 0.1450 1.0644 0.4722 0.044 Uiso 1 1 calc R
H1B H 0.0116 0.9947 0.4205 0.044 Uiso 1 1 calc R
H1C H 0.0348 1.1698 0.4030 0.044 Uiso 1 1 calc R
C6 C 0.35111(14) 0.51771(17) 0.28554(11) 0.0282(3) Uani 1 1 d .
H6A H 0.2793 0.4525 0.2546 0.042 Uiso 1 1 calc R
H6B H 0.3995 0.4839 0.3491 0.042 Uiso 1 1 calc R
H6C H 0.3989 0.5092 0.2542 0.042 Uiso 1 1 calc R
C7 C 0.22743(15) 0.7915(2) 0.16166(11) 0.0325(4) Uani 1 1 d .
H7A H 0.2827 0.7822 0.1368 0.049 Uiso 1 1 calc R
H7B H 0.2035 0.8996 0.1593 0.049 Uiso 1 1 calc R
H7C H 0.1558 0.7283 0.1254 0.049 Uiso 1 1 calc R
C8 C 0.44167(14) 0.84378(19) 0.35099(12) 0.0335(4) Uani 1 1 d .
H8A H 0.4983 0.8287 0.3277 0.050 Uiso 1 1 calc R
H8B H 0.4800 0.8129 0.4154 0.050 Uiso 1 1 calc R
H8C H 0.4187 0.9528 0.3454 0.050 Uiso 1 1 calc R
C5 C 0.31587(15) 0.46576(18) 0.50537(11) 0.0335(4) Uani 1 1 d .
H5A H 0.3782 0.4648 0.4870 0.050 Uiso 1 1 calc R
H5B H 0.2506 0.3956 0.4660 0.050 Uiso 1 1 calc R
H5C H 0.3507 0.4321 0.5691 0.050 Uiso 1 1 calc R
C3 C 0.37988(17) 0.7960(2) 0.57182(12) 0.0430(4) Uani 1 1 d .
H3A H 0.4115 0.7615 0.6351 0.065 Uiso 1 1 calc R
H3B H 0.3494 0.9016 0.5656 0.065 Uiso 1 1 calc R
H3C H 0.4443 0.7933 0.5557 0.065 Uiso 1 1 calc R
C4 C 0.13629(17) 0.6632(2) 0.52940(12) 0.0407(4) Uani 1 1 d .
H4A H 0.1715 0.6272 0.5927 0.061 Uiso 1 1 calc R
H4B H 0.0710 0.5937 0.4893 0.061 Uiso 1 1 calc R
H4C H 0.1043 0.7676 0.5248 0.061 Uiso 1 1 calc R
O1 O 0.0263(3) 0.4529(4) 0.1827(3) 0.0397(9) Uani 0.50 1 d P
H90 H -0.018(4) 0.490(5) 0.306(3) 0.000(12) Uiso 0.50 1 d P
H91 H 0.017(7) 0.492(9) 0.147(4) 0.11(3) Uiso 0.50 1 d P
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'
Ge Ge 0.1547 1.8001 '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'
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
O1 Ge1 O1 95.5(3) 2 .
O1 Ge1 Si1 111.61(12) 2 .
O1 Ge1 Si1 113.46(12) . .
O1 Ge1 Si1 113.46(12) 2 2
O1 Ge1 Si1 111.61(12) . 2
Si1 Ge1 Si1 110.55(3) . 2
O1 Ge1 H90 3.1(18) 2 .
O1 Ge1 H90 98.1(16) . .
Si1 Ge1 H90 109.0(18) . .
Si1 Ge1 H90 113.6(17) 2 .
O1 Ge1 H91 112(2) 2 .
O1 Ge1 H91 18(2) . .
Si1 Ge1 H91 110(2) . .
Si1 Ge1 H91 98(2) 2 .
H90 Ge1 H91 115(3) . .
C3 Si3 C5 108.71(8) . .
C3 Si3 C4 109.07(9) . .
C5 Si3 C4 108.36(8) . .
C3 Si3 Si1 110.69(6) . .
C5 Si3 Si1 110.09(5) . .
C4 Si3 Si1 109.86(6) . .
C8 Si4 C7 108.89(8) . .
C8 Si4 C6 108.96(8) . .
C7 Si4 C6 108.42(7) . .
C8 Si4 Si1 109.97(6) . .
C7 Si4 Si1 109.07(6) . .
C6 Si4 Si1 111.48(5) . .
Si3 Si1 Si4 113.02(3) . .
Si3 Si1 Si2 113.61(2) . .
Si4 Si1 Si2 110.45(2) . .
Si3 Si1 Ge1 108.23(3) . .
Si4 Si1 Ge1 106.99(3) . .
Si2 Si1 Ge1 103.89(2) . .
C1 Si2 C2 107.08(8) . .
C1 Si2 Si1 111.36(5) . .
C2 Si2 Si1 111.57(5) . .
C1 Si2 Si2 109.08(6) . 2
C2 Si2 Si2 109.83(6) . 2
Si1 Si2 Si2 107.892(15) . 2
Si2 C2 H2A 109.5 . .
Si2 C2 H2B 109.5 . .
H2A C2 H2B 109.5 . .
Si2 C2 H2C 109.5 . .
H2A C2 H2C 109.5 . .
H2B C2 H2C 109.5 . .
Si2 C1 H1A 109.5 . .
Si2 C1 H1B 109.5 . .
H1A C1 H1B 109.5 . .
Si2 C1 H1C 109.5 . .
H1A C1 H1C 109.5 . .
H1B C1 H1C 109.5 . .
Si4 C6 H6A 109.5 . .
Si4 C6 H6B 109.5 . .
H6A C6 H6B 109.5 . .
Si4 C6 H6C 109.5 . .
H6A C6 H6C 109.5 . .
H6B C6 H6C 109.5 . .
Si4 C7 H7A 109.5 . .
Si4 C7 H7B 109.5 . .
H7A C7 H7B 109.5 . .
Si4 C7 H7C 109.5 . .
H7A C7 H7C 109.5 . .
H7B C7 H7C 109.5 . .
Si4 C8 H8A 109.5 . .
Si4 C8 H8B 109.5 . .
H8A C8 H8B 109.5 . .
Si4 C8 H8C 109.5 . .
H8A C8 H8C 109.5 . .
H8B C8 H8C 109.5 . .
Si3 C5 H5A 109.5 . .
Si3 C5 H5B 109.5 . .
H5A C5 H5B 109.5 . .
Si3 C5 H5C 109.5 . .
H5A C5 H5C 109.5 . .
H5B C5 H5C 109.5 . .
Si3 C3 H3A 109.5 . .
Si3 C3 H3B 109.5 . .
H3A C3 H3B 109.5 . .
Si3 C3 H3C 109.5 . .
H3A C3 H3C 109.5 . .
H3B C3 H3C 109.5 . .
Si3 C4 H4A 109.5 . .
Si3 C4 H4B 109.5 . .
H4A C4 H4B 109.5 . .
Si3 C4 H4C 109.5 . .
H4A C4 H4C 109.5 . .
H4B C4 H4C 109.5 . .
Ge1 O1 H91 103(7) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ge1 O1 1.788(4) 2
Ge1 O1 1.788(4) .
Ge1 Si1 2.3929(7) .
Ge1 Si1 2.3929(7) 2
Ge1 H90 1.38(4) .
Ge1 H91 2.03(7) .
Si3 C3 1.8676(18) .
Si3 C5 1.8685(16) .
Si3 C4 1.8726(18) .
Si3 Si1 2.3420(10) .
Si4 C8 1.8710(16) .
Si4 C7 1.8723(17) .
Si4 C6 1.8746(16) .
Si4 Si1 2.3434(7) .
Si1 Si2 2.3563(6) .
Si2 C1 1.8814(16) .
Si2 C2 1.8848(15) .
Si2 Si2 2.3568(11) 2
C2 H2A 0.9800 .
C2 H2B 0.9800 .
C2 H2C 0.9800 .
C1 H1A 0.9800 .
C1 H1B 0.9800 .
C1 H1C 0.9800 .
C6 H6A 0.9800 .
C6 H6B 0.9800 .
C6 H6C 0.9800 .
C7 H7A 0.9800 .
C7 H7B 0.9800 .
C7 H7C 0.9800 .
C8 H8A 0.9800 .
C8 H8B 0.9800 .
C8 H8C 0.9800 .
C5 H5A 0.9800 .
C5 H5B 0.9800 .
C5 H5C 0.9800 .
C3 H3A 0.9800 .
C3 H3B 0.9800 .
C3 H3C 0.9800 .
C4 H4A 0.9800 .
C4 H4B 0.9800 .
C4 H4C 0.9800 .
O1 H91 0.64(6) .
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_4
C3 Si3 Si1 Si4 67.63(7) . .
C5 Si3 Si1 Si4 -52.59(6) . .
C4 Si3 Si1 Si4 -171.85(7) . .
C3 Si3 Si1 Si2 -59.25(7) . .
C5 Si3 Si1 Si2 -179.47(6) . .
C4 Si3 Si1 Si2 61.27(7) . .
C3 Si3 Si1 Ge1 -174.07(7) . .
C5 Si3 Si1 Ge1 65.72(6) . .
C4 Si3 Si1 Ge1 -53.55(7) . .
C8 Si4 Si1 Si3 -61.22(7) . .
C7 Si4 Si1 Si3 179.43(6) . .
C6 Si4 Si1 Si3 59.74(6) . .
C8 Si4 Si1 Si2 67.31(6) . .
C7 Si4 Si1 Si2 -52.03(6) . .
C6 Si4 Si1 Si2 -171.73(6) . .
C8 Si4 Si1 Ge1 179.75(6) . .
C7 Si4 Si1 Ge1 60.41(7) . .
C6 Si4 Si1 Ge1 -59.29(6) . .
O1 Ge1 Si1 Si3 1.29(14) 2 .
O1 Ge1 Si1 Si3 -105.18(15) . .
Si1 Ge1 Si1 Si3 128.57(2) 2 .
O1 Ge1 Si1 Si4 123.37(14) 2 .
O1 Ge1 Si1 Si4 16.90(15) . .
Si1 Ge1 Si1 Si4 -109.35(2) 2 .
O1 Ge1 Si1 Si2 -119.76(14) 2 .
O1 Ge1 Si1 Si2 133.76(15) . .
Si1 Ge1 Si1 Si2 7.515(11) 2 .
Si3 Si1 Si2 C1 -17.57(6) . .
Si4 Si1 Si2 C1 -145.78(6) . .
Ge1 Si1 Si2 C1 99.80(6) . .
Si3 Si1 Si2 C2 102.02(6) . .
Si4 Si1 Si2 C2 -26.19(6) . .
Ge1 Si1 Si2 C2 -140.61(6) . .
Si3 Si1 Si2 Si2 -137.26(3) . 2
Si4 Si1 Si2 Si2 94.53(4) . 2
Ge1 Si1 Si2 Si2 -19.89(3) . 2
