Arsenic-Containing Chalcophosphate Molecular Anions
Collin D. Morris; Mercouri G. Kanatzidis; Inorganic Chemistry 49 (2010) 9049–9054; doi:10.1021/ic101461w

data_4316679
_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
;
 Arsenic-Containing Chalcophosphate Molecular Anions
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              9049
_journal_page_last               9054
_journal_paper_doi               10.1021/ic101461w
_journal_volume                  49
_journal_year                    2010
_chemical_formula_moiety         'As P4 Se12, 5(Cs)'
_chemical_formula_sum            'As Cs5 P4 Se12'
_chemical_formula_weight         1810.87
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           84
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  '-P 4c'
_symmetry_space_group_name_H-M   'P 42/m'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   13.8260(8)
_cell_length_b                   13.8260(8)
_cell_length_c                   7.5173(4)
_cell_measurement_reflns_used    24100
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29.56
_cell_measurement_theta_min      2.71
_cell_volume                     1436.99(14)
_computing_cell_refinement       'STOE X-AREA'
_computing_data_collection       'STOE X-AREA'
_computing_data_reduction        'STOE X-RED'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 6.67
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_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  0.0731
_diffrn_reflns_av_sigmaI/netI    0.0411
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            10986
_diffrn_reflns_theta_full        29.15
_diffrn_reflns_theta_max         29.15
_diffrn_reflns_theta_min         4.00
_exptl_absorpt_coefficient_mu    22.837
_exptl_absorpt_correction_T_max  0.010
_exptl_absorpt_correction_T_min  0.006
_exptl_absorpt_correction_type   numerical
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    4.185
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rod
_exptl_crystal_F_000             1552
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.974
_refine_diff_density_min         -2.634
_refine_diff_density_rms         0.371
_refine_ls_extinction_coef       0.00061(7)
_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   1.429
_refine_ls_matrix_type           full
_refine_ls_number_parameters     65
_refine_ls_number_reflns         2060
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.429
_refine_ls_R_factor_all          0.0662
_refine_ls_R_factor_gt           0.0643
_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 w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+81.3465P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1417
_refine_ls_wR_factor_ref         0.1423
_reflns_number_gt                1997
_reflns_number_total             2060
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic101461w_si_001_4.cif
_cod_data_source_block           Cs5AsP4Se12
_cod_database_code               4316679