Alkali-metal fluoroarsenates(iii) revisited; the As4F13‒ anion, the crystal structure of CsAs4F13 and Raman spectra of MAs4F13 (M = Cs, Rb)
Klampfer, Peter; Benkič, Primož; Volavšek, Bogdan; Jesih, Adolf; Dalton Transactions  (2003) 163–; doi:10.1039/b210507a

data_7012392
_publ_section_title
;
 Alkali-metal fluoroarsenates(iii) revisited; the As4F13-- anion, the
 crystal structure of CsAs4F13 and Raman spectra of MAs4F13 (M = Cs,
 Rb)
;
_journal_issue                   2
_journal_name_full               'Dalton Transactions'
_journal_page_first              163
_journal_paper_doi               10.1039/b210507a
_journal_year                    2003
_chemical_formula_sum            'As4 Cs F13'
_chemical_formula_weight         679.59
_space_group_IT_number           82
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  'I -4'
_symmetry_space_group_name_H-M   'I -4'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   9.568(4)
_cell_length_b                   9.568(4)
_cell_length_c                   6.726(3)
_cell_measurement_reflns_used    1778
_cell_measurement_temperature    200(1)
_cell_measurement_theta_max      30.0326
_cell_measurement_theta_min      3.0088
_cell_volume                     615.7(5)
_computing_cell_refinement       'Rigaku Corporation (1999). CrystalClear.'
_computing_data_collection       'Rigaku Corporation (1999). CrystalClear.'
_computing_data_reduction        'Rigaku Corporation (1999). CrystalClear.'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      200(1)
_diffrn_detector_area_resol_mean 14.6306
_diffrn_measured_fraction_theta_full 88.5000
_diffrn_measured_fraction_theta_max 30.0326
_diffrn_measurement_details
;
scan:
    Number of images: 100
               Slice: -20.0000 - 30.0000
         Image width: 0.5000
            Exp time: 10.0000
       Rotation axis: Omega
               Omega: 0.0000
                 Chi: -90.0000
                 Phi: 0.0000
                 XTD: 34.8676
              2theta: -9.9231
scan:
    Number of images: 360
               Slice: -90.0000 - 90.0000
         Image width: 0.5000
            Exp time: 10.0000
       Rotation axis: Phi
               Omega: 0.0000
                 Chi: 0.0000
                 Phi: 0.0000
                 XTD: 34.8676
              2theta: -9.9231

;
_diffrn_measurement_device_details
;
AFC7: Eulerian 3-circle
;
_diffrn_measurement_device_type
;
Mercury CCD (2x2 bin mode)
;
_diffrn_measurement_method       dtprofit.ref
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.1027
_diffrn_reflns_av_sigmaI/netI    0.0868
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -5
_diffrn_reflns_number            2336
_diffrn_reflns_theta_full        30.26
_diffrn_reflns_theta_max         30.0326
_diffrn_reflns_theta_min         3.0088
_exptl_absorpt_coefficient_mu    13.814
_exptl_absorpt_correction_T_max  0.252
_exptl_absorpt_correction_T_min  0.0518
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    3.665
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Prism
_exptl_crystal_F_000             608
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.297
_refine_diff_density_min         -1.333
_refine_diff_density_rms         0.309
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.00(3)
_refine_ls_extinction_coef       0.124(4)
_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   0.992
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     42
_refine_ls_number_reflns         760
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.992
_refine_ls_R_factor_all          0.0378
_refine_ls_R_factor_gt           0.0363
_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^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0683
_refine_ls_wR_factor_ref         0.0686
_reflns_number_gt                695
_reflns_number_total             760
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b210507a.txt
_cod_data_source_block           CsAs4F13
_cod_original_cell_volume        615.8(4)
_cod_original_sg_symbol_H-M      I-4
_cod_database_code               7012392