Ce53Fe12S90X3(X = Cl, Br, I): The First Rare-Earth Transition-Metal Sulfide Halides
Mills, Allison M.; Ruck, Michael; Inorganic Chemistry 45 (2006) 5172–5178; doi:10.1021/ic0521372

data_4332071
_publ_section_title
;
 Ce53Fe12S90X3(X = Cl, Br, I):&#x00A0; The First Rare-Earth
 Transition-Metal Sulfide Halides
;
_journal_issue                   13
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5172
_journal_page_last               5178
_journal_paper_doi               10.1021/ic0521372
_journal_volume                  45
_journal_year                    2006
_chemical_formula_moiety         'Br3 Ce53 Fe12 S90'
_chemical_formula_sum            'Br3 Ce53 Fe12 S90'
_chemical_formula_weight         11221.69
_chemical_name_common            'cerium iron sulfide bromide'
_chemical_name_systematic
; 
 cerium iron sulfide bromide 
;
_space_group_IT_number           166
_symmetry_cell_setting           rhombohedral
_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
_audit_creation_method           SHELXL97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            1
_cell_length_a                   13.916(1)
_cell_length_b                   13.916(1)
_cell_length_c                   21.824(2)
_cell_measurement_reflns_used    15994
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.18
_cell_measurement_theta_min      5.52
_cell_volume                     3660.1(5)
_computing_cell_refinement       'STOE X-AREA (Stoe & Cie, 1999)'
_computing_data_collection       'STOE X-AREA (Stoe & Cie, 1999)'
_computing_data_reduction        'STOE X-RED (Stoe & Cie, 2001)'
_computing_molecular_graphics    'DIAMOND (Brandenburg, 1999)'
_computing_publication_material  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_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 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  0.0703
_diffrn_reflns_av_sigmaI/netI    0.0222
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -7
_diffrn_reflns_number            14137
_diffrn_reflns_theta_full        26.68
_diffrn_reflns_theta_max         26.68
_diffrn_reflns_theta_min         1.93
_exptl_absorpt_coefficient_mu    19.346
_exptl_absorpt_correction_T_max  0.2296
_exptl_absorpt_correction_T_min  0.1476
_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    5.091
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             4931
_exptl_crystal_preparation       'grown in a CeBr3 flux'
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.15
_refine_diff_density_max         2.797
_refine_diff_density_min         -3.049
_refine_diff_density_rms         0.298
_refine_ls_extinction_coef       0.000283(17)
_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   1.247
_refine_ls_matrix_type           full
_refine_ls_number_parameters     75
_refine_ls_number_reflns         981
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.247
_refine_ls_R_factor_all          0.0352
_refine_ls_R_factor_gt           0.0324
_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^)+(0.0296P)^2^+173.2605P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0766
_refine_ls_wR_factor_ref         0.0779
_reflns_number_gt                935
_reflns_number_total             981
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ic0521372sup2.cif
_cod_data_source_block           am55h
_cod_original_cell_volume        3660.0(5)
_cod_original_sg_symbol_H-M      'R -3 m'
_cod_database_code               4332071