Synthesis, Crystal Structures, and Optical Properties of Two New Layered Quaternary Tantalum Thiophosphates and the Thermal Conversion of Cs4Ta4P4S24 into Cs2Ta2P2S12
Andreas Gutzmann; Christian Näther; Wolfgang Bensch; Inorganic Chemistry 43 (2004) 2998–3004; doi:10.1021/ic035273k

data_4310923
_publ_section_title
;
 Synthesis, Crystal Structures, and Optical Properties of Two New Layered
 Quaternary Tantalum Thiophosphates and the Thermal Conversion of
 Cs4Ta4P4S24 into Cs2Ta2P2S12
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2998
_journal_page_last               3004
_journal_paper_doi               10.1021/ic035273k
_journal_volume                  43
_journal_year                    2004
_chemical_formula_sum            'Cs4 P4 S24 Ta4'
_chemical_formula_weight         2148.76
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 106.19(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.298(3)
_cell_length_b                   17.730(4)
_cell_length_c                   16.058(3)
_cell_measurement_temperature    293(2)
_cell_volume                     3909.3(15)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.930
_diffrn_measured_fraction_theta_max 0.930
_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  0.0582
_diffrn_reflns_av_sigmaI/netI    0.0400
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            35147
_diffrn_reflns_theta_full        28.04
_diffrn_reflns_theta_max         28.04
_diffrn_reflns_theta_min         2.24
_exptl_absorpt_coefficient_mu    16.283
_exptl_crystal_density_diffrn    3.651
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             3824
_refine_diff_density_max         1.705
_refine_diff_density_min         -1.686
_refine_diff_density_rms         0.278
_refine_ls_extinction_coef       0.00034(3)
_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   1.014
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     326
_refine_ls_number_reflns         8812
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.014
_refine_ls_R_factor_all          0.0481
_refine_ls_R_factor_gt           0.0352
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0550P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0831
_refine_ls_wR_factor_ref         0.0891
_reflns_number_gt                7163
_reflns_number_total             8812
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic035273ksi20031105_083449_2.cif
_cod_data_source_block           slagu662
_cod_original_cell_volume        3909.2(14)
_cod_database_code               4310923