Syntheses and Structures of the Infinite Chain Compounds Cs4Ti3Se13, Rb4Ti3S14, Cs4Ti3S14, Rb4Hf3S14, Rb4Zr3Se14, Cs4Zr3Se14, and Cs4Hf3Se14
Fu Qiang Huang; James A. Ibers; Inorganic Chemistry 40 (2001) 2346–2351; doi:10.1021/ic0011260

data_4319605
_publ_section_title
;
 Syntheses and Structures of the Infinite Chain Compounds Cs4Ti3Se13,
 Rb4Ti3S14, Cs4Ti3S14, Rb4Hf3S14, Rb4Zr3Se14, Cs4Zr3Se14, and Cs4Hf3Se14
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2346
_journal_page_last               2351
_journal_paper_doi               10.1021/ic0011260
_journal_volume                  40
_journal_year                    2001
_chemical_formula_sum            'Cs4 Se13 Ti3'
_chemical_formula_weight         1701.81
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 100.0083(9)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   10.2524(6)
_cell_length_b                   32.4680(18)
_cell_length_c                   14.6747(8)
_cell_measurement_temperature    153(2)
_cell_volume                     4810.5(5)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      153(2)
_diffrn_measured_fraction_theta_full 0.919
_diffrn_measured_fraction_theta_max 0.919
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'standard-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0485
_diffrn_reflns_av_sigmaI/netI    0.0652
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       42
_diffrn_reflns_limit_k_min       -44
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            49054
_diffrn_reflns_theta_full        28.88
_diffrn_reflns_theta_max         28.88
_diffrn_reflns_theta_min         1.25
_exptl_absorpt_coefficient_mu    26.597
_exptl_crystal_density_diffrn    4.700
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             5824
_refine_diff_density_max         2.180
_refine_diff_density_min         -2.390
_refine_diff_density_rms         0.327
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.597(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.077
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     723
_refine_ls_number_reflns         22477
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.077
_refine_ls_R_factor_all          0.0543
_refine_ls_R_factor_gt           0.0431
_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 
 [1.00000+0.00000exp(0.00(sin\q/\l)^2^)]/ 
   [\s^2^(Fo^2^)+0.0000+0.0000*P+(0.0400P)^2^+0.0000sin\q/\l] 
 where P = 1.00000Fo^2^ + 0.00000Fc^2^ 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0913
_refine_ls_wR_factor_ref         0.0949
_reflns_number_gt                19149
_reflns_number_total             22477
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0011260_1.cif
_cod_data_source_block           cts
_cod_database_code               4319605