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_4315783
_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            'In K6 P3 S13.5'
_chemical_formula_weight         875.14
_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_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                65.878(5)
_cell_angle_beta                 86.249(6)
_cell_angle_gamma                64.173(5)
_cell_formula_units_Z            2
_cell_length_a                   10.8546(7)
_cell_length_b                   11.0628(7)
_cell_length_c                   12.8098(9)
_cell_measurement_reflns_used    20984
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      29.7
_cell_measurement_theta_min      2.1
_cell_volume                     1251.74(17)
_computing_cell_refinement       'stoe x-area'
_computing_data_collection       'stoe x-area'
_computing_data_reduction        'stoe x-area'
_computing_molecular_graphics    Diamond
_computing_publication_material  Diamond
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      200(2)
_diffrn_detector_area_resol_mean 6.67
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.950
_diffrn_measurement_device_type  'stoe ipds 2'
_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  0.0720
_diffrn_reflns_av_sigmaI/netI    0.0658
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            19947
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         29.53
_diffrn_reflns_theta_min         2.10
_exptl_absorpt_coefficient_mu    3.250
_exptl_absorpt_correction_T_max  0.4422
_exptl_absorpt_correction_T_min  0.2933
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'stoe x-red'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.322
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             848
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.30
_refine_diff_density_max         1.132
_refine_diff_density_min         -1.383
_refine_diff_density_rms         0.195
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.315
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     244
_refine_ls_number_reflns         6650
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.315
_refine_ls_R_factor_all          0.0984
_refine_ls_R_factor_gt           0.0717
_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^)+(0.0098P)^2^+6.0333P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0900
_refine_ls_wR_factor_ref         0.0965
_reflns_number_gt                5364
_reflns_number_total             6650
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic100495b_si_001_2.cif
_cod_data_source_block           1
_cod_original_cell_volume        1251.75(14)
_cod_original_formula_sum        'In K6 P3 S13.50'
_cod_database_code               4315783