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_4335589
_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 S12'
_chemical_formula_weight         1564.95
_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                   12.6726(15)
_cell_length_b                   12.6726(15)
_cell_length_c                   6.1281(14)
_cell_measurement_reflns_used    2262
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.4663
_cell_measurement_theta_min      2.2729
_cell_volume                     984.1(3)
_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 0.995
_diffrn_measured_fraction_theta_max 0.995
_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  0.1088
_diffrn_reflns_av_sigmaI/netI    0.0747
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       7
_diffrn_reflns_limit_l_min       -7
_diffrn_reflns_number            7490
_diffrn_reflns_theta_full        27.47
_diffrn_reflns_theta_max         27.47
_diffrn_reflns_theta_min         3.22
_exptl_absorpt_coefficient_mu    42.222
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.5617
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            lawnblue
_exptl_crystal_density_diffrn    5.281
_exptl_crystal_description       block
_exptl_crystal_F_000             1352
_exptl_crystal_size_max          0.089
_exptl_crystal_size_mid          0.056
_exptl_crystal_size_min          0.028
_refine_diff_density_max         2.016
_refine_diff_density_min         -1.682
_refine_diff_density_rms         0.335
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.05(2)
_refine_ls_extinction_coef       0.00069(9)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_matrix_type           full
_refine_ls_number_parameters     49
_refine_ls_number_reflns         1120
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.101
_refine_ls_R_factor_all          0.0631
_refine_ls_R_factor_gt           0.0560
_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^)+(0.0000P)^2^+32.5200P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0881
_refine_ls_wR_factor_ref         0.0914
_reflns_number_gt                1026
_reflns_number_total             1120
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic400995z_si_002.cif
_cod_data_source_block           a
_cod_database_code               4335589