Crystal Structures, Electronic Structures, and Physical Properties of Tl4MQ4 (M = Zr or Hf; Q = S or Se)
Cheriyedath Raj Sankar; Savitree Bangarigadu-Sanasy; Abdeljalil Assoud; Holger Kleinke; Inorganic Chemistry 50 (2011) 245–249; doi:10.1021/ic101925a

data_4324132
_publ_section_title
;
 Crystal Structures, Electronic Structures, and Physical Properties of
 Tl4MQ4 (M = Zr or Hf; Q = S or Se)
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              245
_journal_page_last               249
_journal_paper_doi               10.1021/ic101925a
_journal_volume                  50
_journal_year                    2011
_chemical_formula_sum            'Se4 Tl4 Zr'
_chemical_formula_weight         1224.54
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   none
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                104.146(3)
_cell_angle_beta                 105.326(3)
_cell_angle_gamma                90.219(3)
_cell_formula_units_Z            5
_cell_length_a                   9.2744(19)
_cell_length_b                   9.2639(19)
_cell_length_c                   16.007(3)
_cell_measurement_temperature    296(2)
_cell_volume                     1282.7(4)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.977
_diffrn_measured_fraction_theta_max 0.977
_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  0.0445
_diffrn_reflns_av_sigmaI/netI    0.0902
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            12888
_diffrn_reflns_theta_full        30.00
_diffrn_reflns_theta_max         30.00
_diffrn_reflns_theta_min         2.96
_exptl_absorpt_coefficient_mu    77.689
_exptl_absorpt_correction_T_max  0.1471
_exptl_absorpt_correction_T_min  0.0626
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'APEX II'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    7.926
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2500
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.04
_refine_diff_density_max         7.418
_refine_diff_density_min         -5.236
_refine_diff_density_rms         0.870
_refine_ls_extinction_coef       0.000367(12)
_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   1.569
_refine_ls_hydrogen_treatment    none
_refine_ls_matrix_type           full
_refine_ls_number_parameters     206
_refine_ls_number_reflns         7296
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.569
_refine_ls_R_factor_all          0.1207
_refine_ls_R_factor_gt           0.0679
_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^)+(0.0002P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1108
_refine_ls_wR_factor_ref         0.1213
_reflns_number_gt                4460
_reflns_number_total             7296
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic101925a_si_002.cif
_cod_data_source_block           Tl4ZrSe4
_cod_original_cell_volume        1282.7(5)
_cod_database_code               4324132