Bis{2,2'-[(2-aminoethyl)azanediyl]diethanaminium} di-μ-sulfido-bis(disulfidogermanate)
Xu, Chao; Zhang, Jing-Jing; Duan, Taike; Chen, Qun; Zhang, Qian-Feng; Acta Crystallographica Section E 68 (2012) m154–; doi:10.1107/S160053681200092X

data_2233503
_publ_section_title
;
 Bis{2,2'-[(2-aminoethyl)azanediyl]diethanaminium}
 di-\m-sulfido-bis(disulfidogermanate)
;
_journal_coeditor_code           HY2497
_journal_issue                   2
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m154
_journal_paper_doi               10.1107/S160053681200092X
_journal_volume                  68
_journal_year                    2012
_chemical_formula_iupac          '(C6 H20 N4)2 [Ge2 S6]'
_chemical_formula_moiety         '2(C6 H20 N4 2+), Ge2 S6 4-'
_chemical_formula_sum            'C12 H40 Ge2 N8 S6'
_chemical_formula_weight         634.06
_chemical_name_systematic
;
Bis{2,2'-[(2-aminoethyl)azanediyl]diethanaminium}
di-\m-sulfido-bis(disulfidogermanate)
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 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                 122.637(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   25.2845(17)
_cell_length_b                   7.3173(4)
_cell_length_c                   16.6001(9)
_cell_measurement_reflns_used    3750
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      26.83
_cell_measurement_theta_min      2.94
_cell_volume                     2586.3(3)
_computing_cell_refinement       'SAINT (Bruker, 2007)'
_computing_data_collection       'APEX2 (Bruker, 2007)'
_computing_data_reduction        'SAINT (Bruker, 2007)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'Bruker APEXII CCD'
_diffrn_measurement_method       '\f and \w 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  0.0505
_diffrn_reflns_av_sigmaI/netI    0.0464
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            11988
_diffrn_reflns_theta_full        27.53
_diffrn_reflns_theta_max         27.53
_diffrn_reflns_theta_min         1.91
_exptl_absorpt_coefficient_mu    2.826
_exptl_absorpt_correction_T_max  0.6765
_exptl_absorpt_correction_T_min  0.6158
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1996)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.628
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1312
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.052
_refine_diff_density_min         -1.075
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     159
_refine_ls_number_reflns         2952
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.0626
_refine_ls_R_factor_gt           0.0418
_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/[\s^2^(Fo^2^)+(0.0694P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0974
_refine_ls_wR_factor_ref         0.1111
_reflns_number_gt                2243
_reflns_number_total             2952
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            hy2497.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               2233503
_cod_database_fobs_code          2233503