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###        Electronic paper (Acta Crystallographica Section E)             ###
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#                                                                            #
# This CIF contains the data in a paper accepted for publication in Acta     #
# Crystallographica Section E. It conforms to the requirements of Notes      #
# for Authors for Section E, and has been peer reviewed under the auspices   #
# of the IUCr Commission on Journals.                                        #
#                                                                            #
# Full details of the Crystallographic Information File format               #
# are given in the paper "The Crystallographic Information File (CIF):       #
# a New Standard Archive File for Crystallography" by S. R. Hall, F. H.      #
# Allen and I. D. Brown [Acta Cryst. (1991), A47, 655-685].                  #
#                                                                            #
# The current version of the core CIF dictionary is obtainable from          #
# ftp://ftp.iucr.org/pub/cif_core.dic. The current version number is 2.1.    #
#                                                                            #
# Software is freely available for graphical display of the structure(s) in  #
# this CIF.  For information consult the CIF home page http://www.iucr.org/  #
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#            Copyright International Union of Crystallography                #
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##############################################################################
                                             
data_I
_audit_creation_method     SHELXL-97
_chemical_name_systematic
;
Hexacaesium nonaselenidotetraantimonate(III) hemihydrate
;
_chemical_name_common     ?
_chemical_formula_moiety     'Sb4 Se9, 0.5H2 O, 6Cs'
_chemical_formula_sum     'Cs6 H1 O0.5 Sb4 Se9'
_chemical_formula_iupac     'Cs6 Sb4 Se9, 0.5H2 O'
_chemical_formula_weight     2004.11
_chemical_melting_point     ?
_symmetry_cell_setting     monoclinic
_symmetry_space_group_name_H-M     'C 2/c'
_symmetry_space_group_name_Hall     '-C 2yc'
loop_
    _symmetry_equiv_pos_as_xyz
    'x, y, z'
    '-x, y, -z+1/2'
    'x+1/2, y+1/2, z'
    '-x+1/2, y+1/2, -z+1/2'
    '-x, -y, -z'
    'x, -y, z-1/2'
    '-x+1/2, -y+1/2, -z'
    'x+1/2, -y+1/2, z-1/2'
_cell_length_a     10.409(2)
_cell_length_b     19.064(4)
_cell_length_c     14.895(3)
_cell_angle_alpha     90.00
_cell_angle_beta     94.39(3)
_cell_angle_gamma     90.00
_cell_volume     2947.1(10)
_cell_formula_units_Z     4
_cell_measurement_reflns_used     17
_cell_measurement_theta_min     4.97
_cell_measurement_theta_max     13.12
_cell_measurement_temperature     293(2)
_exptl_crystal_description     block
_exptl_crystal_colour     red
_exptl_crystal_size_max     0.14
_exptl_crystal_size_mid     0.11
_exptl_crystal_size_min     0.10
_exptl_crystal_density_diffrn     4.537
_exptl_crystal_density_meas     ?
_exptl_crystal_density_method     'not measured'
_exptl_crystal_F_000     3380
_exptl_absorpt_coefficient_mu     22.038
_exptl_absorpt_correction_type     psi-scan
_exptl_absorpt_process_details     '(XPREP in SHELXTL-Plus; Sheldrick, 1995)'
_exptl_absorpt_correction_T_min     0.065
_exptl_absorpt_correction_T_max     0.108
_exptl_special_details
;
;
_diffrn_ambient_temperature     293(2)
_diffrn_radiation_type     MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_source     'fine-focus sealed tube'
_diffrn_radiation_monochromator     graphite
_diffrn_measurement_device_type     'Siemens P4 four-circle'
_diffrn_measurement_method     ω
_diffrn_detector_area_resol_mean     ?
_diffrn_reflns_number     2733
_diffrn_reflns_av_R_equivalents     0.0718
_diffrn_reflns_av_sigmaI/netI     0.0916
_diffrn_reflns_theta_min     2.23
_diffrn_reflns_theta_max     24.99
_diffrn_reflns_theta_full     25.00
_diffrn_measured_fraction_theta_max     0.987
_diffrn_measured_fraction_theta_full     0.987
_diffrn_reflns_limit_h_min     0
_diffrn_reflns_limit_h_max     12
_diffrn_reflns_limit_k_min     0
_diffrn_reflns_limit_k_max     22
_diffrn_reflns_limit_l_min     -17
_diffrn_reflns_limit_l_max     17
_diffrn_standards_number     3
_diffrn_standards_interval_count     97
_diffrn_standards_interval_time     ?
_diffrn_standards_decay_%     15
_refine_special_details
;
  Refinement of F² against ALL reflections.  The weighted R-factor wR and
  goodness of fit S are based on F², conventional R-factors R are based
  on F, with F set to zero for negative F². The threshold expression of
  F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
  not relevant to the choice of reflections for refinement.  R-factors based
  on F² are statistically about twice as large as those based on F, and R-
  factors based on ALL data will be even larger.
;
_reflns_number_total     2563
_reflns_number_gt     1796
_reflns_threshold_expression     I>2σ(I)
_refine_ls_structure_factor_coef     Fsqd
_refine_ls_matrix_type     full
_refine_ls_R_factor_all     0.1108
_refine_ls_R_factor_gt     0.0667
_refine_ls_wR_factor_gt     0.1258
_refine_ls_wR_factor_ref     0.1348
_refine_ls_goodness_of_fit_ref     1.184
_refine_ls_restrained_S_all     1.184
_refine_ls_number_reflns     2563
_refine_ls_number_parameters     89
_refine_ls_number_restraints     0
_refine_ls_hydrogen_treatment     noref
_refine_ls_weighting_scheme     calc
_refine_ls_weighting_details
                  'w = 1/[σ²(Fo²)+(0.0473P)²] where P = (Fo²+2Fc²)/3'
_atom_sites_solution_hydrogens     ?
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary     difmap
_refine_ls_shift/su_max     0.000
_refine_ls_shift/su_mean     0.000
_refine_diff_density_max     1.541
_refine_diff_density_min     -1.716
_refine_ls_extinction_method     none
_refine_ls_extinction_coef     ?
loop_
    _atom_type_symbol
    _atom_type_description
    _atom_type_scat_dispersion_real
    _atom_type_scat_dispersion_imag
    _atom_type_scat_source
    'O' 'O' 0.0106 0.0060
                         'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
    'H' 'H' 0.0000 0.0000
                         'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
    'Se' 'Se' -0.0929 2.2259
                         'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
    'Sb' 'Sb' -0.5866 1.5461
                         'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
    'Cs' 'Cs' -0.3680 2.1192
                         'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_computing_data_collection     'R3m/V User's Guide (Siemens, 1989)'
_computing_cell_refinement     'R3m/V User's Guide'
_computing_data_reduction     'XDISK (Siemens, 1989)'
_computing_structure_solution     'SHELXS97 (Sheldrick, 1997)'
_computing_structure_refinement     'SHELXL97 (Sheldrick, 1997)'
_computing_molecular_graphics     'SHELXTL-Plus (Sheldrick, 1995)'
_computing_publication_material     SHELXL97
loop_
    _atom_site_label
    _atom_site_fract_x
    _atom_site_fract_y
    _atom_site_fract_z
    _atom_site_U_iso_or_equiv
    _atom_site_adp_type
    _atom_site_calc_flag
    _atom_site_refinement_flags
    _atom_site_occupancy
    _atom_site_disorder_assembly
    _atom_site_disorder_group
    _atom_site_type_symbol
    Cs1 0.31807(14) 0.20508(7) 0.89048(9) 0.0337(4) Uani d . 1 . . Cs
    Cs2 0.5000 0.02479(12) 0.7500 0.0469(6) Uani d S 1 . . Cs
    Cs3 0.15045(15) 0.34458(8) 0.59383(11) 0.0417(4) Uani d . 1 . . Cs
    Cs4 0.0000 -0.09570(15) 0.7500 0.0522(7) Uani d S 1 . . Cs
    Sb1 0.11996(13) 0.11799(7) 0.65874(9) 0.0227(3) Uani d . 1 . . Sb
    Sb2 -0.14247(14) 0.04704(7) 0.47316(9) 0.0244(4) Uani d . 1 . . Sb
    Se1 0.0151(2) 0.15548(11) 0.50002(14) 0.0253(5) Uani d . 1 . . Se
    Se2 0.0000 0.21143(15) 0.7500 0.0252(7) Uani d S 1 . . Se
    Se3 -0.3104(2) 0.11586(13) 0.37927(16) 0.0381(6) Uani d . 1 . . Se
    Se4 0.3290(2) 0.18187(14) 0.64910(16) 0.0358(6) Uani d . 1 . . Se
    Se5 0.2113(3) 0.02934(12) 0.87011(17) 0.0427(7) Uani d . 1 . . Se
    O 0.5000 0.0000 0.0000 0.09(2) Uiso d SP 0.50 . . O
loop_
    _atom_site_aniso_label
    _atom_site_aniso_U_11
    _atom_site_aniso_U_22
    _atom_site_aniso_U_33
    _atom_site_aniso_U_12
    _atom_site_aniso_U_13
    _atom_site_aniso_U_23
    Cs1 0.0425(9) 0.0276(8) 0.0304(8) -0.0088(7) -0.0008(7) -0.0029(6)
    Cs2 0.0330(12) 0.0309(12) 0.0786(18) 0.000 0.0149(12) 0.000
    Cs3 0.0362(9) 0.0449(9) 0.0447(9) -0.0018(8) 0.0078(7) 0.0000(8)
    Cs4 0.0432(14) 0.0845(19) 0.0292(12) 0.000 0.0056(11) 0.000
    Sb1 0.0257(8) 0.0238(7) 0.0185(7) 0.0037(7) 0.0010(6) 0.0006(6)
    Sb2 0.0276(8) 0.0202(7) 0.0256(8) 0.0034(7) 0.0043(6) -0.0029(6)
    Se1 0.0269(12) 0.0273(11) 0.0211(10) -0.0015(10) -0.0026(9) 0.0051(9)
    Se2 0.0296(17) 0.0210(15) 0.0260(16) 0.000 0.0094(14) 0.000
    Se3 0.0317(13) 0.0391(14) 0.0410(14) 0.0078(12) -0.0128(11) -0.0056(11)
    Se4 0.0213(12) 0.0562(16) 0.0302(12) 0.0001(11) 0.0033(10) 0.0071(11)
    Se5 0.0624(18) 0.0257(12) 0.0439(15) -0.0046(13) 0.0302(14) -0.0074(11)
_geom_special_details
;
  All esds (except the esd in the dihedral angle between two l.s. planes)
  are estimated using the full covariance matrix.  The cell esds are taken
  into account individually in the estimation of esds in distances, angles
  and torsion angles; correlations between esds in cell parameters are only
  used when they are defined by crystal symmetry.  An approximate
(isotropic)
  treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
    _geom_bond_atom_site_label_1
    _geom_bond_atom_site_label_2
    _geom_bond_site_symmetry_2
    _geom_bond_distance
    _geom_bond_publ_flag
    Cs1 Se5 . 3.535(3) yes
    Cs1 Se4 . 3.633(3) yes
    Cs1 Se1 8_556 3.664(3) yes
    Cs1 Se3 8_556 3.665(3) yes
    Cs1 Se2 . 3.7807(19) yes
    Cs1 Se4 2_656 3.791(3) yes
    Cs1 Se3 2_556 3.834(3) yes
    Cs1 Se1 2_556 4.055(3) yes
    Cs2 Se5 2_656 3.614(3) yes
    Cs2 Se5 . 3.614(3) yes
    Cs2 Se4 2_656 3.740(3) yes
    Cs2 Se4 . 3.740(3) yes
    Cs2 O 2_655 3.7536(8) yes
    Cs2 O 1_556 3.7536(8) yes
    Cs2 Se3 5_556 3.769(3) yes
    Cs2 Se3 6_656 3.769(3) yes
    Cs3 O 4 3.5846(17) yes
    Cs3 Se3 7_456 3.670(3) yes
    Cs3 Se4 7_556 3.676(3) yes
    Cs3 Se4 . 3.677(3) yes
    Cs3 Se5 4_556 3.827(3) yes
    Cs3 Se1 7_556 3.850(3) yes
    Cs3 Se2 . 3.855(3) yes
    Cs3 Se1 . 4.078(3) yes
    Cs3 Se3 8_556 4.307(3) yes
    Cs4 Se5 . 3.622(3) yes
    Cs4 Se5 2_556 3.622(3) yes
    Cs4 Se1 5_556 3.886(2) yes
    Cs4 Se1 6_556 3.886(2) yes
    Cs4 Se3 5_556 3.905(3) yes
    Cs4 Se3 6_556 3.905(3) yes
    Sb1 Se4 . 2.507(3) yes
    Sb1 Se2 . 2.615(2) yes
    Sb1 Se1 . 2.626(3) yes
    Sb2 Se5 2_556 2.517(3) yes
    Sb2 Se3 . 2.522(3) yes
    Sb2 Se1 . 2.650(3) yes
    Se1 Cs1 8_455 3.664(3) ?
    Se1 Cs3 7_556 3.850(3) ?
    Se1 Cs4 5_556 3.886(2) ?
    Se1 Cs1 2_556 4.055(3) ?
    Se2 Sb1 2_556 2.615(2) ?
    Se2 Cs1 2_556 3.7807(19) ?
    Se2 Cs3 2_556 3.855(3) ?
    Se3 Cs1 8_455 3.665(3) ?
    Se3 Cs3 7_456 3.670(3) ?
    Se3 Cs2 5_556 3.769(3) ?
    Se3 Cs1 2_556 3.834(3) ?
    Se3 Cs4 5_556 3.905(3) ?
    Se3 Cs3 8_455 4.307(3) ?
    Se4 Cs3 7_556 3.676(3) ?
    Se4 Cs1 2_656 3.791(3) ?
    Se5 Sb2 2_556 2.517(3) ?
    Se5 Cs3 4_546 3.827(3) ?
    O Cs3 8 3.5846(17) ?
    O Cs3 4_545 3.5846(17) ?
    O Cs2 1_554 3.7536(8) ?
    O Cs2 5_656 3.7536(8) ?
loop_
    _geom_angle_atom_site_label_1
    _geom_angle_atom_site_label_2
    _geom_angle_atom_site_label_3
    _geom_angle_site_symmetry_1
    _geom_angle_site_symmetry_3
    _geom_angle
    _geom_angle_publ_flag
    Se4 Sb1 Se2 . . 98.62(9) yes
    Se4 Sb1 Se1 . . 96.84(9) yes
    Se2 Sb1 Se1 . . 95.76(7) yes
    Se5 Sb2 Se3 2_556 . 110.46(10) yes
    Se5 Sb2 Se1 2_556 . 100.45(9) yes
    Se3 Sb2 Se1 . . 94.16(9) yes
    Sb1 Se1 Sb2 . . 97.67(8) yes
    Sb1 Se2 Sb1 . 2_556 94.14(11) yes
data_global
_journal_date_recd_electronic     2005-10-11
_journal_date_accepted     2005-10-19
_journal_name_full     'Acta Crystallographica, Section E'
_journal_year     2005
_journal_volume     61
_journal_issue     11
_journal_page_first     i240
_journal_page_last     i242
_journal_paper_category     EI
_journal_coeditor_code     WM6103
_publ_contact_author
;
       William S. Sheldrick
       Lehrstuhl für Analytische Chemie
       Ruhr-Universität Bochum
       Universitätsstrasse 150
       44780 Bochum
       Germany
;
_publ_contact_author_email     william.sheldrick@rub.de
_publ_contact_author_fax     '049 234 32-14420'
_publ_contact_author_phone     '049 234 32-24192'
_publ_section_title
;
Hexacaesium nonaselenidotetraantimonate(III) hemihydrate
;
loop_
    _publ_author_name
    _publ_author_address
    'Tobias van Almsick'
;
Lehrstuhl für Analytische Chemie
Ruhr-Universität Bochum
Universitätsstraße 150
44780 Bochum
Germany
;
    'William S. Sheldrick'
;
Lehrstuhl für Analytische Chemie
Ruhr-Universität Bochum
Universitätsstraße 150
44780 Bochum
Germany
;
