Syntheses, Structures, and Nonlinear Optical Properties of Quaternary Chalcogenides: Pb4Ga4GeQ12 (Q = S, Se)
Yu-Kun Chen; Mei-Chun Chen; Liu-Jiang Zhou; Ling Chen; Li-Ming Wu; Inorganic Chemistry 52 (2013) 8334–8341; doi:10.1021/ic400995z

data_4335590
_publ_section_title
;
 Syntheses, Structures, and Nonlinear Optical Properties of Quaternary
 Chalcogenides: Pb4Ga4GeQ12 (Q = S, Se)
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              8334
_journal_page_last               8341
_journal_paper_doi               10.1021/ic400995z
_journal_volume                  52
_journal_year                    2013
_chemical_formula_sum            'Ga4 Ge Pb4 Se12'
_chemical_formula_weight         2127.75
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           114
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  'P -4 2n'
_symmetry_space_group_name_H-M   'P -4 21 c'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   13.064(7)
_cell_length_b                   13.064(7)
_cell_length_c                   6.310(5)
_cell_measurement_reflns_used    1049
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.4565
_cell_measurement_theta_min      2.2036
_cell_volume                     1076.9(12)
_computing_cell_refinement       'Bruker XSCANS'
_computing_data_collection       'Bruker XSCANS'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       '\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  0.0725
_diffrn_reflns_av_sigmaI/netI    0.0427
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       7
_diffrn_reflns_limit_l_min       -7
_diffrn_reflns_number            6694
_diffrn_reflns_theta_full        24.98
_diffrn_reflns_theta_max         24.98
_diffrn_reflns_theta_min         3.49
_exptl_absorpt_coefficient_mu    57.706
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.6761
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            darkred
_exptl_crystal_density_diffrn    6.562
_exptl_crystal_description       block
_exptl_crystal_F_000             1784
_exptl_crystal_size_max          0.089
_exptl_crystal_size_mid          0.068
_exptl_crystal_size_min          0.052
_refine_diff_density_max         3.670
_refine_diff_density_min         -3.166
_refine_diff_density_rms         0.517
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.07(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.069
_refine_ls_matrix_type           full
_refine_ls_number_parameters     48
_refine_ls_number_reflns         945
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.099
_refine_ls_R_factor_all          0.0602
_refine_ls_R_factor_gt           0.0534
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0873P)^2^+18.8669P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1342
_refine_ls_wR_factor_ref         0.1385
_reflns_number_gt                861
_reflns_number_total             945
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic400995z_si_003.cif
_cod_data_source_block           a
_cod_original_cell_volume        1076.8(11)
_cod_database_code               4335590