Syntheses and structural characterization of non-centrosymmetric Na2M2M'S6 (M, M′=Ga, In, Si, Ge, Sn, Zn, Cd) sulfides
Yohannan, Jinu P.; Vidyasagar, Kanamaluru; Journal of Solid State Chemistry 238 (2016) 147–155; doi:10.1016/j.jssc.2016.03.026

data_1561500
_publ_section_title
;
 Syntheses and structural characterization of non-centrosymmetric
 Na2M2M'S6 (M, M&#x2032;=Ga, In, Si, Ge, Sn, Zn, Cd) sulfides
;
_journal_name_full               'Journal of Solid State Chemistry'
_journal_page_first              147
_journal_page_last               155
_journal_paper_doi               10.1016/j.jssc.2016.03.026
_journal_volume                  238
_journal_year                    2016
_chemical_formula_sum            'Ge2 Na2 S6 Zn'
_chemical_formula_weight         448.99
_space_group_IT_number           9
_space_group_name_Hall           'C -2yc'
_space_group_name_H-M_alt        'C 1 c 1'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'C -2yc'
_symmetry_space_group_name_H-M   'C 1 c 1'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 99.959(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   7.2630(2)
_cell_length_b                   12.3404(4)
_cell_length_c                   11.3057(5)
_cell_measurement_reflns_used    2209
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      23.808
_cell_measurement_theta_min      3.292
_cell_volume                     998.04(6)
_computing_cell_refinement       APEXII,Bruker,2004
_computing_data_collection       APEXII,Bruker,2004
_computing_data_reduction        SAINT,Bruker,2004
_computing_molecular_graphics    'ORTEP-3 (Farrugia, 1997)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker ApexII ccd area detector'
_diffrn_measurement_method       'phi and omega 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  0.0458
_diffrn_reflns_av_sigmaI/netI    0.0521
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            7532
_diffrn_reflns_theta_full        26.49
_diffrn_reflns_theta_max         26.49
_diffrn_reflns_theta_min         3.29
_exptl_absorpt_coefficient_mu    9.636
_exptl_absorpt_correction_T_max  0.749
_exptl_absorpt_correction_T_min  0.567
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS(Bruker,2004)
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.988
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             848
_exptl_crystal_size_max          0.06
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.719
_refine_diff_density_min         -0.664
_refine_diff_density_rms         0.146
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.003(15)
_refine_ls_extinction_coef       0.0001
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_matrix_type           full
_refine_ls_number_parameters     100
_refine_ls_number_reflns         1925
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.0382
_refine_ls_R_factor_gt           0.0319
_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^)+(0.0188P)^2^+3.1203P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0580
_refine_ls_wR_factor_ref         0.0604
_reflns_number_gt                1759
_reflns_number_total             1925
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            JSSC-2016-238-147.cif
_cod_data_source_block           Na2Ge2ZnS6
_cod_original_sg_symbol_Hall     C-2yc
_cod_original_sg_symbol_H-M      Cc
_cod_database_code               1561500