Quaternary rare-earth sulfides RE 3 M 0.5 GeS 7 (RE=La‒Nd, Sm; M=Co, Ni) and Y 3 Pd 0.5 SiS 7
Iyer, Abishek K.; Yin, Wenlong; Lee, Emma J.; Lin, Xinsong; Mar, Arthur; Journal of Solid State Chemistry 250 (2017) 14–23; doi:10.1016/j.jssc.2017.03.009

data_1560470
_publ_section_title
;
 Quaternary rare-earth sulfides RE 3 M 0.5 GeS 7 (RE=La--Nd, Sm; M=Co, Ni)
 and Y 3 Pd 0.5 SiS 7
;
_journal_name_full               'Journal of Solid State Chemistry'
_journal_page_first              14
_journal_page_last               23
_journal_paper_doi               10.1016/j.jssc.2017.03.009
_journal_volume                  250
_journal_year                    2017
_chemical_absolute_configuration ad
_chemical_formula_structural     'Nd3 Ni0.50 Ge S7'
_chemical_formula_sum            'Ge Nd3 Ni0.5 S7'
_chemical_formula_weight         759.09
_chemical_name_common
'neodymium nickel germanium sulfide (3/0.5/1/7)'
_chemical_name_systematic
'neodymium nickel germanium sulfide (3/0.5/1/7)'
_space_group_crystal_system      hexagonal
_space_group_IT_number           173
_space_group_name_Hall           'P 6c'
_space_group_name_H-M_alt        'P 63'
_atom_sites_solution_hydrogens   .
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            2
_cell_length_a                   10.0760(3)
_cell_length_b                   10.0760(3)
_cell_length_c                   5.7605(2)
_cell_measurement_reflns_used    7588
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      33.06
_cell_measurement_theta_min      2.33
_cell_volume                     506.49(3)
_computing_cell_refinement       'Bruker SAINT 8.34A (Bruker, 2013)'
_computing_data_collection       'Bruker APEX 2 (Bruker, 2008)'
_computing_data_reduction        'Bruker SAINT 8.34A'
_computing_molecular_graphics    'ATOMS 5.1 (Dowty, 1999)'
_computing_publication_material  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker PLATFORM/SMART APEX II CCD'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0254
_diffrn_reflns_av_unetI/netI     0.0179
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            7287
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         33.137
_diffrn_reflns_theta_min         2.334
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    20.332
_exptl_absorpt_correction_T_max  0.461
_exptl_absorpt_correction_T_min  0.361
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'SHELXL-2014/7 (Sheldrick, 2014)'
_exptl_crystal_colour            grey
_exptl_crystal_density_diffrn    4.977
_exptl_crystal_description       irregular
_exptl_crystal_F_000             676
_exptl_crystal_size_max          0.075
_exptl_crystal_size_mid          0.061
_exptl_crystal_size_min          0.061
_refine_diff_density_max         1.169
_refine_diff_density_min         -0.705
_refine_diff_density_rms         0.148
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.009(17)
_refine_ls_extinction_coef       0.0122(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014)'
_refine_ls_goodness_of_fit_ref   1.104
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     41
_refine_ls_number_reflns         1286
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.104
_refine_ls_R_factor_all          0.0131
_refine_ls_R_factor_gt           0.0129
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0116P)^2^+0.3902P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0298
_refine_ls_wR_factor_ref         0.0299
_reflns_Friedel_coverage         0.846
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.998
_reflns_number_gt                1270
_reflns_number_total             1286
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            mmc20.cif
_cod_data_source_block           9
_cod_original_formula_sum        'Ge Nd3 Ni0.50 S7'
_cod_database_code               1560470
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.311
_shelx_estimated_absorpt_t_max   0.370
_shelx_res_checksum              49196
_shelx_hkl_checksum              72970