#------------------------------------------------------------------------------
#$Date: 2019-11-08 00:40:35 +0100 (vie 08 de nov de 2019) $
#$Revision: 224543 $
#$URL: svn://www.crystallography.net/cod/cif/7/04/91/7049111.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_7049111
loop_
_publ_author_name
'Dornsiepen, Eike'
'Dehnen, Stefanie'
_publ_section_title
;
 Dinuclear organogermanium chalcogenide complexes as intermediates towards
 functionalized clusters.
;
_journal_issue                   11
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              3671
_journal_page_last               3675
_journal_paper_doi               10.1039/c9dt00310j
_journal_volume                  48
_journal_year                    2019
_chemical_formula_sum            'C12 H22 Cl2 Ge2 O2 Te2'
_chemical_formula_weight         669.57
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2017/1
_audit_update_record
;
2019-01-18 deposited with the CCDC.    2019-02-18 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 104.500(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   8.2073(3)
_cell_length_b                   11.4851(4)
_cell_length_c                   10.9961(4)
_cell_measurement_reflns_used    24895
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      75.27
_cell_measurement_theta_min      3.85
_cell_volume                     1003.50(6)
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2017)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  'STOE STADIVARI'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_unetI/netI     0.0264
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            2037
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         74.860
_diffrn_reflns_theta_min         5.666
_exptl_absorpt_coefficient_mu    28.612
_exptl_absorpt_correction_T_max  0.2519
_exptl_absorpt_correction_T_min  0.0000
_exptl_absorpt_correction_type   sphere
_exptl_absorpt_process_details   'STOE LANA'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    2.216
_exptl_crystal_description       block
_exptl_crystal_F_000             624
_exptl_crystal_size_rad          0.094
_refine_diff_density_max         2.097
_refine_diff_density_min         -1.273
_refine_diff_density_rms         0.209
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.116
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     95
_refine_ls_number_reflns         2037
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.116
_refine_ls_R_factor_all          0.0563
_refine_ls_R_factor_gt           0.0515
_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)+(0.1091P)²+1.6360P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1492
_refine_ls_wR_factor_ref         0.1608
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1846
_reflns_number_total             2037
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c9dt00310j2.cif
_cod_data_source_block           platon_tw
_cod_depositor_comments
'Adding full bibliography for 7049110--7049112.cif.'
_cod_database_code               7049111
_shelx_shelxl_version_number     2017/1
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
loop_
_space_group_symop_operation_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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
Te1 Te 0.72515(6) 0.43465(4) 0.53993(4) 0.0451(2) Uani 1 1 d . .
C1 C 0.5882(9) 0.6891(7) 0.2915(8) 0.0464(16) Uani 1 1 d . .
O1 O 0.8259(7) 0.5108(5) 0.2882(5) 0.0514(13) Uani 1 1 d . .
Cl1 Cl 0.4330(3) 0.42397(18) 0.1938(2) 0.0527(5) Uani 1 1 d . .
Ge1 Ge 0.52441(10) 0.53833(8) 0.35784(8) 0.0431(3) Uani 1 1 d . .
C6 C 0.9370(11) 0.5960(9) 0.1299(9) 0.058(2) Uani 1 1 d . .
H6A H 0.878891 0.597425 0.042509 0.086 Uiso 1 1 calc R U
H6B H 1.013413 0.531264 0.145755 0.086 Uiso 1 1 calc R U
H6C H 0.998868 0.667144 0.151569 0.086 Uiso 1 1 calc R U
C5 C 0.8119(9) 0.5838(7) 0.2077(8) 0.0452(16) Uani 1 1 d . .
C4 C 0.6692(10) 0.6698(7) 0.1824(7) 0.0483(16) Uani 1 1 d . .
H4A H 0.583171 0.643174 0.110270 0.058 Uiso 1 1 calc R U
H4B H 0.710560 0.743965 0.160393 0.058 Uiso 1 1 calc R U
C3 C 0.7029(10) 0.7526(7) 0.4013(8) 0.0495(17) Uani 1 1 d . .
H3A H 0.738460 0.824999 0.372547 0.074 Uiso 1 1 calc R U
H3B H 0.799727 0.705333 0.436374 0.074 Uiso 1 1 calc R U
H3C H 0.643129 0.767749 0.464295 0.074 Uiso 1 1 calc R U
C2 C 0.4226(11) 0.7576(8) 0.2427(9) 0.0541(19) Uani 1 1 d . .
H2A H 0.447140 0.832609 0.213194 0.081 Uiso 1 1 calc R U
H2B H 0.367723 0.767224 0.309563 0.081 Uiso 1 1 calc R U
H2C H 0.349985 0.715369 0.174995 0.081 Uiso 1 1 calc R U
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ge Ge -1.0885 0.8855 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Te Te -0.1759 6.3531 '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_3
Ge1 Te1 Ge1 81.90(3) 3_666
C3 C1 C4 112.9(6) .
C3 C1 C2 110.3(7) .
C4 C1 C2 108.6(6) .
C3 C1 Ge1 107.0(5) .
C4 C1 Ge1 111.5(6) .
C2 C1 Ge1 106.2(5) .
C1 Ge1 Cl1 106.5(2) .
C1 Ge1 Te1 121.0(2) .
Cl1 Ge1 Te1 112.65(7) .
C1 Ge1 Te1 111.3(2) 3_666
Cl1 Ge1 Te1 106.40(7) 3_666
Te1 Ge1 Te1 98.10(3) 3_666
C5 C6 H6A 109.5 .
C5 C6 H6B 109.5 .
H6A C6 H6B 109.5 .
C5 C6 H6C 109.5 .
H6A C6 H6C 109.5 .
H6B C6 H6C 109.5 .
O1 C5 C6 122.2(8) .
O1 C5 C4 121.3(7) .
C6 C5 C4 116.5(7) .
C5 C4 C1 115.0(7) .
C5 C4 H4A 108.5 .
C1 C4 H4A 108.5 .
C5 C4 H4B 108.5 .
C1 C4 H4B 108.5 .
H4A C4 H4B 107.5 .
C1 C3 H3A 109.5 .
C1 C3 H3B 109.5 .
H3A C3 H3B 109.5 .
C1 C3 H3C 109.5 .
H3A C3 H3C 109.5 .
H3B C3 H3C 109.5 .
C1 C2 H2A 109.5 .
C1 C2 H2B 109.5 .
H2A C2 H2B 109.5 .
C1 C2 H2C 109.5 .
H2A C2 H2C 109.5 .
H2B C2 H2C 109.5 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Te1 Ge1 2.5475(10) .
Te1 Ge1 2.5901(10) 3_666
C1 C3 1.519(11) .
C1 C4 1.526(11) .
C1 C2 1.546(11) .
C1 Ge1 1.999(8) .
O1 C5 1.204(10) .
Cl1 Ge1 2.205(2) .
C6 C5 1.498(12) .
C6 H6A 0.9600 .
C6 H6B 0.9600 .
C6 H6C 0.9600 .
C5 C4 1.504(11) .
C4 H4A 0.9700 .
C4 H4B 0.9700 .
C3 H3A 0.9600 .
C3 H3B 0.9600 .
C3 H3C 0.9600 .
C2 H2A 0.9600 .
C2 H2B 0.9600 .
C2 H2C 0.9600 .
