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_4319607
_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 S14 Ti3'
_chemical_formula_weight         1124.18
_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                 113.801(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   21.329(3)
_cell_length_b                   8.4146(10)
_cell_length_c                   13.6778(16)
_cell_measurement_temperature    153(2)
_cell_volume                     2246.0(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 0.939
_diffrn_measured_fraction_theta_max 0.939
_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  0.0318
_diffrn_reflns_av_sigmaI/netI    0.0212
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            13483
_diffrn_reflns_theta_full        28.99
_diffrn_reflns_theta_max         28.99
_diffrn_reflns_theta_min         2.09
_exptl_absorpt_coefficient_mu    8.717
_exptl_crystal_density_diffrn    3.324
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2040
_refine_diff_density_max         2.471
_refine_diff_density_min         -0.807
_refine_diff_density_rms         0.175
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.006
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     96
_refine_ls_number_reflns         2810
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.006
_refine_ls_R_factor_all          0.0252
_refine_ls_R_factor_gt           0.0219
_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          0.0543
_refine_ls_wR_factor_ref         0.0563
_reflns_number_gt                2583
_reflns_number_total             2810
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0011260_3.cif
_cod_data_source_block           cstis
_cod_original_cell_volume        2246.1(5)
_cod_database_code               4319607