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_4319611
_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 Hf3 Se14'
_chemical_formula_weight         2172.55
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 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                 111.88(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   22.758(5)
_cell_length_b                   8.8442(18)
_cell_length_c                   14.276(3)
_cell_measurement_temperature    153(2)
_cell_volume                     2666.4(11)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      153(2)
_diffrn_measured_fraction_theta_full 0.963
_diffrn_measured_fraction_theta_max 0.963
_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  0.0765
_diffrn_reflns_av_sigmaI/netI    0.0516
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            11786
_diffrn_reflns_theta_full        28.28
_diffrn_reflns_theta_max         28.28
_diffrn_reflns_theta_min         1.93
_exptl_absorpt_coefficient_mu    36.131
_exptl_crystal_density_diffrn    5.412
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             3648
_refine_diff_density_max         5.197
_refine_diff_density_min         -3.580
_refine_diff_density_rms         0.571
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.422
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     96
_refine_ls_number_reflns         3189
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.422
_refine_ls_R_factor_all          0.0541
_refine_ls_R_factor_gt           0.0468
_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 
 [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          0.1114
_refine_ls_wR_factor_ref         0.1134
_reflns_number_gt                2705
_reflns_number_total             3189
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0011260_7.cif
_cod_data_source_block           cshfse
_cod_original_cell_volume        2666.5(9)
_cod_database_code               4319611