Bis[4-(2-azaniumylethyl)piperazin-1-ium] di-μ-sulfido-bis[disulfidogermanate(II)]
Zhang, Bei-Bei; Xu, Chao; Duan, Taike; Chen, Qun; Zhang, Qian-Feng; Acta Crystallographica Section E 68 (2012) m822–; doi:10.1107/S1600536812022040

data_2235162
_publ_section_title
;
 Bis[4-(2-azaniumylethyl)piperazin-1-ium]
 di-\m-sulfido-bis[disulfidogermanate(II)]
;
_journal_coeditor_code           MW2068
_journal_issue                   6
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m822
_journal_paper_doi               10.1107/S1600536812022040
_journal_volume                  68
_journal_year                    2012
_chemical_formula_iupac          '(C6 H17 N3)2 [Ge2 S6]'
_chemical_formula_moiety         '2(C6 H17 N3 2+), Ge2 S6 4-'
_chemical_formula_sum            'C12 H34 Ge2 N6 S6'
_chemical_formula_weight         600.10
_chemical_name_systematic
;
Bis[4-(2-azaniumylethyl)piperazin-1-ium]
di-\m-sulfido-bis[disulfidogermanate(II)]
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_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_method           SHELXL-97
_cell_angle_alpha                72.1560(10)
_cell_angle_beta                 78.3230(10)
_cell_angle_gamma                89.7920(10)
_cell_formula_units_Z            1
_cell_length_a                   7.49850(10)
_cell_length_b                   8.27090(10)
_cell_length_c                   10.41770(10)
_cell_measurement_reflns_used    6350
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      26.43
_cell_measurement_theta_min      2.52
_cell_volume                     601.107(13)
_computing_cell_refinement       'SAINT (Bruker, 2005)'
_computing_data_collection       'APEX2 (Bruker, 2005)'
_computing_data_reduction        'SAINT (Bruker, 2005)'
_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 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker APEXII CCD area-detector'
_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  0.0178
_diffrn_reflns_av_sigmaI/netI    0.0158
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            11264
_diffrn_reflns_theta_full        27.54
_diffrn_reflns_theta_max         27.54
_diffrn_reflns_theta_min         2.10
_exptl_absorpt_coefficient_mu    3.033
_exptl_absorpt_correction_T_max  0.6939
_exptl_absorpt_correction_T_min  0.5684
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1997)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.657
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       slab
_exptl_crystal_F_000             308
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.13
_refine_diff_density_max         0.335
_refine_diff_density_min         -0.197
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     118
_refine_ls_number_reflns         2756
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.0192
_refine_ls_R_factor_gt           0.0172
_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^)+(0.0255P)^2^+0.0568P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0429
_refine_ls_wR_factor_ref         0.0437
_reflns_number_gt                2558
_reflns_number_total             2756
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            mw2068.cif
_cod_data_source_block           I
_cod_original_cell_volume        601.107(12)
_cod_database_code               2235162
_cod_database_fobs_code          2235162