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#$Date: 2016-02-16 22:30:59 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176467 $
#$URL: svn://www.crystallography.net/cod/cif/4/33/01/4330116.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_4330116
loop_
_publ_author_name
'Honghan Fei'
'Cari S. Han'
'Scott R. J. Oliver'
_publ_section_title
;
 A Cationic Antimonite Chain Templated by Sulfate: [Sb6O74+][(SO42-)2]
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              8655
_journal_page_last               8657
_journal_paper_doi               10.1021/ic3013409
_journal_volume                  51
_journal_year                    2012
_chemical_formula_sum            'O7.5 S Sb3'
_chemical_formula_weight         517.31
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           37
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'C 2 -2c'
_symmetry_space_group_name_H-M   'C c c 2'
_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            8
_cell_length_a                   12.0329(6)
_cell_length_b                   18.9371(10)
_cell_length_c                   5.8595(3)
_cell_measurement_reflns_used    6001
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      59.006
_cell_measurement_theta_min      6.772
_cell_volume                     1335.19(12)
_computing_cell_refinement       'Bruker SAINT v7.34'
_computing_data_collection       'Bruker APEX-II v2.1-4'
_computing_data_reduction        'Bruker SAINT v7.34'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      296(2)
_diffrn_detector_area_resol_mean 83.33
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEX-II'
_diffrn_measurement_method       ω/2θ-scans
_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  0.0263
_diffrn_reflns_av_sigmaI/netI    0.0211
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       7
_diffrn_reflns_limit_l_min       -7
_diffrn_reflns_number            6647
_diffrn_reflns_theta_full        27.08
_diffrn_reflns_theta_max         27.08
_diffrn_reflns_theta_min         2.01
_exptl_absorpt_coefficient_mu    12.364
_exptl_absorpt_correction_T_max  0.7459
_exptl_absorpt_correction_T_min  0.4816
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    5.147
_exptl_crystal_description       needle
_exptl_crystal_F_000             1832
_exptl_crystal_size_max          0.245
_exptl_crystal_size_mid          0.035
_exptl_crystal_size_min          0.030
_refine_diff_density_max         0.682
_refine_diff_density_min         -0.463
_refine_diff_density_rms         0.170
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.04(2)
_refine_ls_extinction_coef       0.00164(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.097
_refine_ls_matrix_type           full
_refine_ls_number_parameters     107
_refine_ls_number_reflns         1479
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.096
_refine_ls_R_factor_all          0.0116
_refine_ls_R_factor_gt           0.0115
_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/[σ²(Fo²)+(0.0110P)²+0.3169P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0278
_refine_ls_wR_factor_ref         0.0278
_reflns_number_gt                1471
_reflns_number_total             1479
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic3013409_si_002.cif
_cod_data_source_block           xsc1206
_cod_original_formula_sum        'O7.50 S Sb3'
_cod_database_code               4330116
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z'
'x, -y, z+1/2'
'-x, y, z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, -y+1/2, z'
'x+1/2, -y+1/2, z+1/2'
'-x+1/2, y+1/2, z+1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
Sb1 Sb 0.187491(17) 0.434789(10) 0.49978(5) 0.01081(6) Uani 1 1 d .
Sb2 Sb 0.391731(17) 0.433840(10) 0.88813(4) 0.00985(6) Uani 1 1 d .
Sb3 Sb 0.407170(16) 0.292860(11) 0.51806(5) 0.01166(6) Uani 1 1 d .
O6 O 0.5562(2) 0.21432(14) 0.5972(6) 0.0382(8) Uani 1 1 d .
S1 S 0.63322(7) 0.15528(4) 0.55026(14) 0.01501(19) Uani 1 1 d .
O2 O 0.25834(15) 0.50085(13) 0.2762(5) 0.0111(4) Uani 1 1 d .
O3 O 0.4934(2) 0.33468(9) 0.7846(4) 0.0120(5) Uani 1 1 d .
O5 O 0.5000 0.5000 0.7432(8) 0.0113(6) Uani 1 2 d S
O4 O 0.34643(17) 0.39861(11) 0.5647(4) 0.0105(5) Uani 1 1 d .
O7 O 0.6927(2) 0.16760(15) 0.3374(6) 0.0301(7) Uani 1 1 d .
O9 O 0.5762(2) 0.08710(14) 0.5507(6) 0.0281(7) Uani 1 1 d .
O8 O 0.7154(2) 0.15505(12) 0.7446(5) 0.0195(6) Uani 1 1 d .
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'
S S 0.1246 0.1234 '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'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
O2 Sb1 O4 86.18(9) . .
O2 Sb1 O2 88.31(4) . 3_565
O4 Sb1 O2 71.91(8) . 3_565
O2 Sb1 O8 88.54(10) . 7_454
O4 Sb1 O8 74.81(9) . 7_454
O2 Sb1 O8 146.71(8) 3_565 7_454
O5 Sb2 O4 89.12(14) . .
O5 Sb2 O2 89.79(8) . 3_565
O4 Sb2 O2 73.05(10) . 3_565
O5 Sb2 O3 93.01(7) . .
O4 Sb2 O3 68.96(8) . .
O2 Sb2 O3 141.84(11) 3_565 .
O3 Sb3 O3 93.81(4) 4_654 .
O3 Sb3 O4 85.45(8) 4_654 .
O3 Sb3 O4 73.34(8) . .
O3 Sb3 O6 85.93(10) 4_654 .
O3 Sb3 O6 73.08(10) . .
O4 Sb3 O6 144.62(10) . .
S1 O6 Sb3 155.6(2) . .
O7 S1 O9 111.94(18) . .
O7 S1 O6 110.26(17) . .
O9 S1 O6 111.93(18) . .
O7 S1 O8 108.94(16) . .
O9 S1 O8 107.69(15) . .
O6 S1 O8 105.84(16) . .
Sb1 O2 Sb2 118.84(14) . 3_564
Sb1 O2 Sb1 131.54(9) . 3_564
Sb2 O2 Sb1 101.37(10) 3_564 3_564
Sb3 O3 Sb3 132.97(10) 4_655 .
Sb3 O3 Sb2 117.44(11) 4_655 .
Sb3 O3 Sb2 104.27(10) . .
Sb2 O5 Sb2 129.7(2) . 2_665
Sb1 O4 Sb2 107.67(10) . .
Sb1 O4 Sb3 126.89(10) . .
Sb2 O4 Sb3 108.98(9) . .
S1 O8 Sb1 113.52(13) . 7
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Sb1 O2 2.002(3) .
Sb1 O4 2.067(2) .
Sb1 O2 2.199(3) 3_565
Sb1 O8 2.290(3) 7_454
Sb2 O5 1.997(2) .
Sb2 O4 2.082(2) .
Sb2 O2 2.130(2) 3_565
Sb2 O3 2.322(2) .
Sb3 O3 1.982(2) 4_654
Sb3 O3 2.035(2) .
Sb3 O4 2.149(2) .
Sb3 O6 2.376(3) .
O6 S1 1.478(3) .
S1 O7 1.457(3) .
S1 O9 1.462(3) .
S1 O8 1.508(3) .
O2 Sb2 2.130(2) 3_564
O2 Sb1 2.199(3) 3_564
O3 Sb3 1.982(2) 4_655
O5 Sb2 1.997(2) 2_665
O8 Sb1 2.290(3) 7
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_4
O3 Sb3 O6 S1 -70.2(5) 4_654 .
O3 Sb3 O6 S1 -165.4(5) . .
O4 Sb3 O6 S1 -146.4(4) . .
Sb3 O6 S1 O7 56.9(5) . .
Sb3 O6 S1 O9 -68.4(5) . .
Sb3 O6 S1 O8 174.6(4) . .
O4 Sb1 O2 Sb2 -52.72(12) . 3_564
O2 Sb1 O2 Sb2 19.26(11) 3_565 3_564
O8 Sb1 O2 Sb2 -127.60(13) 7_454 3_564
O4 Sb1 O2 Sb1 165.22(18) . 3_564
O2 Sb1 O2 Sb1 -122.80(19) 3_565 3_564
O8 Sb1 O2 Sb1 90.35(17) 7_454 3_564
O3 Sb3 O3 Sb3 -108.1(2) 4_654 4_655
O4 Sb3 O3 Sb3 167.85(19) . 4_655
O6 Sb3 O3 Sb3 -23.48(17) . 4_655
O3 Sb3 O3 Sb2 99.45(5) 4_654 .
O4 Sb3 O3 Sb2 15.36(8) . .
O6 Sb3 O3 Sb2 -175.97(12) . .
O5 Sb2 O3 Sb3 98.19(15) . 4_655
O4 Sb2 O3 Sb3 -173.92(14) . 4_655
O2 Sb2 O3 Sb3 -168.31(11) 3_565 4_655
O5 Sb2 O3 Sb3 -104.20(15) . .
O4 Sb2 O3 Sb3 -16.30(9) . .
O2 Sb2 O3 Sb3 -10.70(19) 3_565 .
O4 Sb2 O5 Sb2 -177.16(6) . 2_665
O2 Sb2 O5 Sb2 109.78(8) 3_565 2_665
O3 Sb2 O5 Sb2 -108.29(6) . 2_665
O2 Sb1 O4 Sb2 108.66(12) . .
O2 Sb1 O4 Sb2 19.19(10) 3_565 .
O8 Sb1 O4 Sb2 -161.82(12) 7_454 .
O2 Sb1 O4 Sb3 -119.60(14) . .
O2 Sb1 O4 Sb3 150.93(15) 3_565 .
O8 Sb1 O4 Sb3 -30.08(13) 7_454 .
O5 Sb2 O4 Sb1 -109.76(8) . .
O2 Sb2 O4 Sb1 -19.71(9) 3_565 .
O3 Sb2 O4 Sb1 156.68(12) . .
O5 Sb2 O4 Sb3 109.37(8) . .
O2 Sb2 O4 Sb3 -160.58(11) 3_565 .
O3 Sb2 O4 Sb3 15.81(8) . .
O3 Sb3 O4 Sb1 115.78(15) 4_654 .
O3 Sb3 O4 Sb1 -148.87(16) . .
O6 Sb3 O4 Sb1 -167.82(15) . .
O3 Sb3 O4 Sb2 -112.98(11) 4_654 .
O3 Sb3 O4 Sb2 -17.62(9) . .
O6 Sb3 O4 Sb2 -36.6(2) . .
O7 S1 O8 Sb1 -135.68(16) . 7
O9 S1 O8 Sb1 -14.1(2) . 7
O6 S1 O8 Sb1 105.78(17) . 7
