Bis(<i>tert</i>-butylthiolato-<i>S</i>)germanium–Imide Trimer
George, C.; Purdy, A. P.; Acta Crystallographica Section C 52 (1996) 2489–2491; doi:10.1107/S0108270196007822

data_2005511
_publ_section_title
;
 Bis(<i>tert</i>-butylthiolato-<i>S</i>)germanium--Imide Trimer
;
_journal_issue                   10
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              2489
_journal_page_last               2491
_journal_paper_doi               10.1107/S0108270196007822
_journal_volume                  52
_journal_year                    1996
_chemical_formula_iupac          '[Ge3 (C4 H9 S)6 (N H3)]'
_chemical_formula_structural     (((CH3)3CS)2GeNH)3
_chemical_formula_sum            'C24 H57 Ge3 N3 S6'
_chemical_formula_weight         797.86
_chemical_melting_point          494.1(10)
_chemical_name_systematic
;
Bis(tert-butylthio)germanium-Imide trimer
;
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 103.08(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   12.013(2)
_cell_length_b                   10.610(2)
_cell_length_c                   15.634(3)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    243(2)
_cell_measurement_theta_max      27.40
_cell_measurement_theta_min      5.25
_cell_volume                     1941.0(7)
_computing_cell_refinement       XSCANS
_computing_data_collection       'XSCANS (Siemens, 1994)'
_computing_data_reduction        XSCANS
_computing_molecular_graphics    SHELXTL
_computing_publication_material  SHELXTL
_computing_structure_refinement  SHELXTL
_computing_structure_solution    'SHELXTL (Sheldrick, 1994)'
_diffrn_ambient_temperature      243
_diffrn_measurement_device       'Siemens P4'
_diffrn_measurement_method       \q/2\q
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0211
_diffrn_reflns_av_sigmaI/netI    0.0533
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       2
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            3160
_diffrn_reflns_theta_max         58.21
_diffrn_reflns_theta_min         2.90
_diffrn_standards_decay_%        3.1
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    5.884
_exptl_absorpt_correction_T_max  0.92
_exptl_absorpt_correction_T_min  0.20
_exptl_absorpt_correction_type
'semi-empirical, \y scans (XPREP; Sheldrick, 1994)'
_exptl_crystal_colour            translucent
_exptl_crystal_density_diffrn    1.365
_exptl_crystal_density_meas      ?
_exptl_crystal_description       irregular
_exptl_crystal_F_000             828
_exptl_crystal_size_max          0.48
_exptl_crystal_size_mid          0.42
_exptl_crystal_size_min          0.31
_refine_diff_density_max         1.118
_refine_diff_density_min         -1.128
_refine_ls_abs_structure_details 'Flack (1983)'
_refine_ls_abs_structure_Flack   0.11(9)
_refine_ls_extinction_coef       0.0024(4)
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_all   1.038
_refine_ls_goodness_of_fit_obs   1.043
_refine_ls_hydrogen_treatment    'H atoms riding'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     354
_refine_ls_number_reflns         2904
_refine_ls_number_restraints     27
_refine_ls_restrained_S_all      1.459
_refine_ls_restrained_S_obs      1.525
_refine_ls_R_factor_all          0.0582
_refine_ls_R_factor_obs          0.0512
_refine_ls_shift/esd_max         0.149
_refine_ls_shift/esd_mean        0.008
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0772P)^2^+5.4341P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1320
_refine_ls_wR_factor_obs         0.1258
_reflns_number_observed          2643
_reflns_number_total             2904
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            fg1205.cif
_cod_data_source_block           pur42
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 

The following automatic conversions were performed:

'_chemical_melting_point' value '220-222 \%C' was changed to
'494.1(10)' - it was converted from degrees Celsius(C) to Kelvins(K),
the average value was taken and precision was
estimated.

'_symmetry_cell_setting' value 'Monoclinic' changed to
'monoclinic' according to
/home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 

The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc w =
1/[\s^2^(Fo^2^)+(0.0772P)^2^+5.4341P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to 'w =
1/[\s^2^(Fo^2^)+(0.0772P)^2^+5.4341P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        1940.9(7)
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               2005511