#------------------------------------------------------------------------------
#$Date: 2019-11-17 12:25:34 +0200 (Sun, 17 Nov 2019) $
#$Revision: 229861 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/04/58/7045860.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_7045860
loop_
_publ_author_name
'Zaitsev, Kirill V.'
'Lam, Kevin'
'Poleshchuk, Oleg Kh'
'Kuz'mina, Lyudmila G.'
'Churakov, Andrei V.'
_publ_section_title
;
 Oligothienyl catenated germanes and silanes: synthesis, structure, and
 properties.
;
_journal_issue                   15
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              5431
_journal_page_last               5444
_journal_paper_doi               10.1039/c8dt00256h
_journal_volume                  47
_journal_year                    2018
_chemical_formula_moiety         'C18 H34 Ge4 S2'
_chemical_formula_sum            'C18 H34 Ge4 S2'
_chemical_formula_weight         604.93
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2016-01-19
_audit_creation_method
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_audit_update_record
;
2017-12-13 deposited with the CCDC.
2018-03-14 downloaded from the CCDC.
;
_cell_angle_alpha                90.805(2)
_cell_angle_beta                 94.883(2)
_cell_angle_gamma                112.136(2)
_cell_formula_units_Z            1
_cell_length_a                   6.7760(10)
_cell_length_b                   8.4190(13)
_cell_length_c                   12.5300(19)
_cell_measurement_reflns_used    3385
_cell_measurement_temperature    170
_cell_measurement_theta_max      30.248
_cell_measurement_theta_min      2.615
_cell_volume                     658.89(17)
_computing_cell_refinement       'SAINT v7.60A (Bruker, 2009)'
_computing_data_reduction        'SAINT v7.60A (Bruker, 2009)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XH (Sheldrick, 2008)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_temperature      170
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.987
_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  0.0173
_diffrn_reflns_av_unetI/netI     0.0256
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            7182
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         29.00
_diffrn_reflns_theta_min         2.62
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    4.676
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.5588
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.0994 before and 0.0260 after correction.
The Ratio of minimum to maximum transmission is 0.7490.
The λ/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.525
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             302
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.26
_refine_diff_density_max         1.204
_refine_diff_density_min         -0.466
_refine_diff_density_rms         0.100
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.099
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     114
_refine_ls_number_reflns         3464
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.099
_refine_ls_R_factor_all          0.0408
_refine_ls_R_factor_gt           0.0302
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0486P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0782
_refine_ls_wR_factor_ref         0.0814
_reflns_number_gt                2883
_reflns_number_total             3464
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c8dt00256h2.cif
_cod_data_source_block           p-1
_cod_depositor_comments
'Adding full bibliography for 7045857--7045860.cif.'
_cod_database_code               7045860
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3)
2.b Idealised Me refined as rotating group:
 C5(H5A,H5B,H5C), C6(H6A,H6B,H6C), C7(H7A,H7B,H7C), C8(H8A,H8B,H8C), C9(H9A,
 H9B,H9C)
;
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 'x, y, z'
2 '-x, -y, -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_calc_flag
_atom_site_refinement_flags_posn
Ge1 Ge 0.26349(4) 0.74446(3) 0.323418(19) 0.02551(8) Uani 1 d .
Ge2 Ge 0.21787(4) 0.46703(3) 0.24623(2) 0.03040(9) Uani 1 d .
S1 S -0.03203(9) 0.84566(8) 0.14204(5) 0.03083(14) Uani 1 d .
C1 C 0.2178(4) 0.8742(3) 0.20259(19) 0.0264(5) Uani 1 d .
C2 C 0.3712(4) 0.9850(3) 0.1462(2) 0.0331(5) Uani 1 d .
H2 H 0.5200 1.0177 0.1663 0.040 Uiso 1 calc R
C3 C 0.2900(4) 1.0471(3) 0.0551(2) 0.0328(5) Uani 1 d .
H3 H 0.3783 1.1251 0.0086 0.039 Uiso 1 calc R
C4 C 0.0705(4) 0.9828(3) 0.04108(19) 0.0256(5) Uani 1 d .
C5 C 0.0595(5) 0.7346(4) 0.4263(2) 0.0414(6) Uani 1 d .
H5A H -0.0860 0.6665 0.3944 0.062 Uiso 1 calc GR
H5B H 0.0705 0.8512 0.4452 0.062 Uiso 1 calc GR
H5C H 0.0914 0.6812 0.4910 0.062 Uiso 1 calc GR
C6 C 0.5575(4) 0.8765(4) 0.3840(2) 0.0380(6) Uani 1 d .
H6A H 0.5859 0.8292 0.4520 0.057 Uiso 1 calc GR
H6B H 0.5763 0.9967 0.3968 0.057 Uiso 1 calc GR
H6C H 0.6574 0.8699 0.3337 0.057 Uiso 1 calc GR
C7 C -0.0836(5) 0.3268(4) 0.2137(3) 0.0623(10) Uani 1 d .
H7A H -0.1519 0.2996 0.2806 0.094 Uiso 1 calc GR
H7B H -0.0992 0.2201 0.1751 0.094 Uiso 1 calc GR
H7C H -0.1523 0.3897 0.1690 0.094 Uiso 1 calc GR
C8 C 0.3522(6) 0.5078(4) 0.1128(3) 0.0531(8) Uani 1 d .
H8A H 0.2742 0.5560 0.0621 0.080 Uiso 1 calc GR
H8B H 0.3493 0.3991 0.0821 0.080 Uiso 1 calc GR
H8C H 0.5010 0.5887 0.1270 0.080 Uiso 1 calc GR
C9 C 0.3507(7) 0.3476(5) 0.3424(3) 0.0645(10) Uani 1 d .
H9A H 0.5011 0.4212 0.3621 0.097 Uiso 1 calc GR
H9B H 0.3424 0.2411 0.3061 0.097 Uiso 1 calc GR
H9C H 0.2753 0.3205 0.4072 0.097 Uiso 1 calc GR
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Ge1 0.02795(14) 0.02442(13) 0.02481(14) 0.00058(9) 0.00115(10) 0.01098(10)
Ge2 0.03386(15) 0.02301(14) 0.03394(16) 0.00226(10) 0.01039(11) 0.00882(11)
S1 0.0242(3) 0.0323(3) 0.0337(3) 0.0102(2) 0.0025(2) 0.0078(2)
C1 0.0263(11) 0.0227(11) 0.0285(12) -0.0005(9) -0.0008(9) 0.0081(9)
C2 0.0262(11) 0.0316(12) 0.0394(14) 0.0068(10) -0.0001(10) 0.0090(10)
C3 0.0242(11) 0.0318(12) 0.0410(15) 0.0116(11) 0.0040(10) 0.0084(10)
C4 0.0277(11) 0.0208(10) 0.0280(12) 0.0030(8) 0.0041(9) 0.0085(9)
C5 0.0450(15) 0.0484(16) 0.0361(15) 0.0019(12) 0.0113(12) 0.0223(13)
C6 0.0343(13) 0.0396(14) 0.0375(15) 0.0000(11) -0.0048(11) 0.0129(11)
C7 0.0408(17) 0.0447(18) 0.086(3) -0.0178(18) 0.0154(17) -0.0023(14)
C8 0.067(2) 0.0386(16) 0.0465(18) -0.0027(13) 0.0275(16) 0.0075(15)
C9 0.099(3) 0.059(2) 0.058(2) 0.0094(17) 0.013(2) 0.055(2)
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'
S S 0.1246 0.1234 '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
C1 Ge1 Ge2 105.24(7) . .
C1 Ge1 C6 104.46(11) . .
C5 Ge1 Ge2 113.70(9) . .
C5 Ge1 C1 108.73(11) . .
C5 Ge1 C6 111.09(13) . .
C6 Ge1 Ge2 112.93(9) . .
C7 Ge2 Ge1 110.50(11) . .
C7 Ge2 C8 108.55(16) . .
C7 Ge2 C9 109.48(17) . .
C8 Ge2 Ge1 106.80(9) . .
C8 Ge2 C9 110.13(16) . .
C9 Ge2 Ge1 111.32(11) . .
C1 S1 C4 93.37(11) . .
S1 C1 Ge1 123.34(13) . .
C2 C1 Ge1 126.81(18) . .
C2 C1 S1 109.51(18) . .
C1 C2 H2 122.8 . .
C1 C2 C3 114.4(2) . .
C3 C2 H2 122.8 . .
C2 C3 H3 123.5 . .
C4 C3 C2 112.9(2) . .
C4 C3 H3 123.5 . .
C3 C4 S1 109.78(18) . .
C3 C4 C4 129.3(3) . 2_575
C4 C4 S1 120.9(2) 2_575 .
Ge1 C5 H5A 109.5 . .
Ge1 C5 H5B 109.5 . .
Ge1 C5 H5C 109.5 . .
H5A C5 H5B 109.5 . .
H5A C5 H5C 109.5 . .
H5B C5 H5C 109.5 . .
Ge1 C6 H6A 109.5 . .
Ge1 C6 H6B 109.5 . .
Ge1 C6 H6C 109.5 . .
H6A C6 H6B 109.5 . .
H6A C6 H6C 109.5 . .
H6B C6 H6C 109.5 . .
Ge2 C7 H7A 109.5 . .
Ge2 C7 H7B 109.5 . .
Ge2 C7 H7C 109.5 . .
H7A C7 H7B 109.5 . .
H7A C7 H7C 109.5 . .
H7B C7 H7C 109.5 . .
Ge2 C8 H8A 109.5 . .
Ge2 C8 H8B 109.5 . .
Ge2 C8 H8C 109.5 . .
H8A C8 H8B 109.5 . .
H8A C8 H8C 109.5 . .
H8B C8 H8C 109.5 . .
Ge2 C9 H9A 109.5 . .
Ge2 C9 H9B 109.5 . .
Ge2 C9 H9C 109.5 . .
H9A C9 H9B 109.5 . .
H9A C9 H9C 109.5 . .
H9B C9 H9C 109.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ge1 Ge2 2.4141(5) .
Ge1 C1 1.950(2) .
Ge1 C5 1.949(3) .
Ge1 C6 1.957(3) .
Ge2 C7 1.939(3) .
Ge2 C8 1.944(3) .
Ge2 C9 1.950(3) .
S1 C1 1.723(2) .
S1 C4 1.733(2) .
C1 C2 1.365(3) .
C2 H2 0.9500 .
C2 C3 1.416(4) .
C3 H3 0.9500 .
C3 C4 1.372(3) .
C4 C4 1.452(5) 2_575
C5 H5A 0.9800 .
C5 H5B 0.9800 .
C5 H5C 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 .
C9 H9A 0.9800 .
C9 H9B 0.9800 .
C9 H9C 0.9800 .
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_4
Ge1 C1 C2 C3 173.51(18) .
Ge2 Ge1 C1 S1 77.69(14) .
Ge2 Ge1 C1 C2 -94.9(2) .
S1 C1 C2 C3 0.1(3) .
C1 Ge1 Ge2 C7 -77.88(15) .
C1 Ge1 Ge2 C8 40.00(14) .
C1 Ge1 Ge2 C9 160.25(15) .
C1 S1 C4 C3 0.0(2) .
C1 S1 C4 C4 -179.1(3) 2_575
C1 C2 C3 C4 -0.1(3) .
C2 C3 C4 S1 0.1(3) .
C2 C3 C4 C4 179.1(3) 2_575
C4 S1 C1 Ge1 -173.73(14) .
C4 S1 C1 C2 0.0(2) .
C5 Ge1 Ge2 C7 41.00(17) .
C5 Ge1 Ge2 C8 158.89(15) .
C5 Ge1 Ge2 C9 -80.87(16) .
C5 Ge1 C1 S1 -44.46(18) .
C5 Ge1 C1 C2 143.0(2) .
C6 Ge1 Ge2 C7 168.77(16) .
C6 Ge1 Ge2 C8 -73.35(15) .
C6 Ge1 Ge2 C9 46.90(16) .
C6 Ge1 C1 S1 -163.14(15) .
C6 Ge1 C1 C2 24.3(2) .
