Redetermination of the lanthanum iron sulfide La~52~Fe~12~S~90~
Mills, Allison M.; Bräunling, Daniel; Ruck, Michael; Acta Crystallographica, Section C 62 (2006) i56–i58; doi:10.1107/S0108270106014879

data_2015504
_publ_section_title
;
Redetermination of the lanthanum iron sulfide La~52~Fe~12~S~90~
;
_journal_coeditor_code           IZ1068
_journal_issue                   8
_journal_name_full               'Acta Crystallographica, Section C'
_journal_page_first              i56
_journal_page_last               i58
_journal_paper_doi               10.1107/S0108270106014879
_journal_volume                  62
_journal_year                    2006
_chemical_formula_iupac          'La52 Fe12 S90'
_chemical_formula_moiety         'Fe12 La52 S90'
_chemical_formula_sum            'Fe12 La52 S90'
_chemical_formula_weight         10778.92
_chemical_name_common            'lanthanum iron sulfide'
_chemical_name_systematic
;
lanthanum(III) iron(II) sulfide
;
_space_group_IT_number           166
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  '-R 3 2"'
_symmetry_space_group_name_H-M   'R -3 m :H'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            1
_cell_length_a                   14.0426(5)
_cell_length_b                   14.0426(5)
_cell_length_c                   21.7760(10)
_cell_measurement_reflns_used    22416
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.27
_cell_measurement_theta_min      1.92
_cell_volume                     3718.8(3)
_computing_cell_refinement       X-AREA
_computing_data_collection       'X-AREA (Stoe & Cie, 2004)'
_computing_data_reduction        'X-RED (Stoe & Cie, 2001)'
_computing_molecular_graphics    'DIAMOND (Brandenburg, 1999)'
_computing_publication_material  SHELXL97
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 6.67
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Stoe IPDS-II'
_diffrn_measurement_method       \w
_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  0.0409
_diffrn_reflns_av_sigmaI/netI    0.0126
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            19622
_diffrn_reflns_theta_full        27.00
_diffrn_reflns_theta_max         27.00
_diffrn_reflns_theta_min         1.92
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    16.956
_exptl_absorpt_correction_T_max  0.3628
_exptl_absorpt_correction_T_min  0.2101
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
;
[X-RED (Stoe & Cie, 2001); crystal description optimized based on
equivalent reflections using X-SHAPE (Stoe & Cie, 1999)]
;
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    4.813
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             4716
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.10
_refine_diff_density_max         3.267
_refine_diff_density_min         -4.120
_refine_ls_extinction_coef       0.00033(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL97
_refine_ls_goodness_of_fit_ref   1.195
_refine_ls_matrix_type           full
_refine_ls_number_parameters     65
_refine_ls_number_reflns         1018
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.194
_refine_ls_R_factor_all          0.0438
_refine_ls_R_factor_gt           0.0429
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.033P)^2^+405P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1037
_refine_ls_wR_factor_ref         0.1042
_reflns_number_gt                1000
_reflns_number_total             1018
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            iz1068.cif
_cod_original_sg_symbol_H-M      'R -3 m'
_cod_database_code               2015504