Synthesis of Alkali Metal Indium Thiophosphates Containing the Discrete Anions [In(PS4)(PS5)2]6- and [In(PS4)2(PS5)]6-
Alexander Rothenberger; Collin Morris; Mercouri G. Kanatzidis; Inorganic Chemistry 49 (2010) 5598–5602; doi:10.1021/ic100495b

data_4315782
_publ_contact_author
;
      Prof. M. G. Kanatzidis
      Department of Chemistry
      2145 Sheridan Road
      Northwestern University
      Evanston, IL 60208-3113
      USA
;
_publ_contact_author_email       m-kanatzidis@northwestern.edu
_publ_contact_author_fax         'Int + 847-491-5937'
_publ_contact_author_phone       'Int + 847-467-1541'
_publ_section_title
;
 Synthesis of Alkali Metal Indium Thiophosphates Containing the Discrete
 Anions [In(PS4)(PS5)2]6- and [In(PS4)2(PS5)]6-
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5598
_journal_page_last               5602
_journal_paper_doi               10.1021/ic100495b
_journal_volume                  49
_journal_year                    2010
_chemical_formula_sum            'Cs6 In P3 S13.5'
_chemical_formula_weight         1438.00
_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   undef
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                78.192(5)
_cell_angle_beta                 77.332(5)
_cell_angle_gamma                81.150(5)
_cell_formula_units_Z            2
_cell_length_a                   8.5474(5)
_cell_length_b                   10.8068(6)
_cell_length_c                   16.6108(9)
_cell_measurement_reflns_used    13426
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      29.55
_cell_measurement_theta_min      2.50
_cell_volume                     1455.74(15)
_computing_cell_refinement       'stoe x-area'
_computing_data_collection       'stoe x-area'
_computing_data_reduction        'stoe x-area'
_computing_molecular_graphics    'SHELXTL-97 (Sheldrick, 1997)'
_computing_publication_material  'SHELXTL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 6.67
_diffrn_measured_fraction_theta_full 0.938
_diffrn_measured_fraction_theta_max 0.918
_diffrn_measurement_device_type  'stoe ipds 2t'
_diffrn_measurement_method       rotation
_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  0.0518
_diffrn_reflns_av_sigmaI/netI    0.0480
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            13817
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         29.15
_diffrn_reflns_theta_min         2.46
_exptl_absorpt_coefficient_mu    9.332
_exptl_absorpt_correction_T_max  0.1662
_exptl_absorpt_correction_T_min  0.0895
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'stoe x-red 32'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    3.281
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1280
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.30
_refine_diff_density_max         3.319
_refine_diff_density_min         -3.371
_refine_diff_density_rms         0.249
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     262
_refine_ls_number_reflns         7216
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.054
_refine_ls_R_factor_all          0.0551
_refine_ls_R_factor_gt           0.0486
_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 w=1/[\s^2^(Fo^2^)+(0.0474P)^2^+15.3466P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1194
_refine_ls_wR_factor_ref         0.1234
_reflns_number_gt                6452
_reflns_number_total             7216
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic100495b_si_001_1.cif
_cod_data_source_block           3
_cod_original_cell_volume        1455.74(14)
_cod_original_formula_sum        'Cs6 In P3 S13.50'
_cod_database_code               4315782