Reinvestigation of Ge~4~Se~9~ based on single-crystal data
Jung-Eun Kwak; Hoseop Yun; Acta Crystallographica Section C 61 (2005) i81–i82; doi:10.1107/S0108270105021979

data_2014978
_publ_section_title
;
 Reinvestigation of Ge~4~Se~9~ based on single-crystal data
;
_journal_coeditor_code           FA1148
_journal_issue                   8
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              i81
_journal_page_last               i82
_journal_paper_doi               10.1107/S0108270105021979
_journal_volume                  61
_journal_year                    2005
_chemical_formula_iupac          'Ge4 Se9'
_chemical_formula_sum            'Ge4 Se9'
_chemical_formula_weight         1001.08
_chemical_name_systematic
;
Tetragermanium nonaselenide
;
_space_group_IT_number           29
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2c -2ac'
_symmetry_space_group_name_H-M   'P c a 21'
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.805(6)
_cell_length_b                   7.002(2)
_cell_length_c                   12.071(6)
_cell_measurement_reflns_used    11241
_cell_measurement_temperature    291(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      3.13
_cell_volume                     1504.9(10)
_computing_cell_refinement       RAPID-AUTO
_computing_data_collection       'RAPID-AUTO (Rigaku, 2005)'
_computing_data_reduction        RAPID-AUTO
_computing_molecular_graphics
'locally modified version of ORTEP (Johnson, 1965)'
_computing_publication_material  'WinGX (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      291(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPID-S'
_diffrn_measurement_method       \w
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0602
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            13705
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         3.13
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    29.642
_exptl_absorpt_correction_T_max  0.220
_exptl_absorpt_correction_T_min  0.042
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   '(NUMABS; Higashi, 2000)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    4.419
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1736
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.050
_refine_diff_density_max         1.319
_refine_diff_density_min         -0.934
_refine_ls_abs_structure_details 'Flack (1983), with 1615 Friedel pairs'
_refine_ls_abs_structure_Flack   0.11(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.06
_refine_ls_matrix_type           full
_refine_ls_number_parameters     118
_refine_ls_number_reflns         3410
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.06
_refine_ls_R_factor_gt           0.0371
_refine_ls_shift/su_max          0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[\s^2^(Fo^2^)+(0.0242P)^2^+4.9288P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.0742
_reflns_number_gt                2837
_reflns_number_total             3410
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            fa1148.cif
_cod_data_source_block           I
_cod_original_cell_volume        1504.8(10)
_cod_original_sg_symbol_Hall     'P 2C -2AC'
_cod_database_code               2014978
_cod_database_fobs_code          2014978