#------------------------------------------------------------------------------
#$Date: 2021-01-27 00:15:22 +0200 (Wed, 27 Jan 2021) $
#$Revision: 261234 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/51/84/4518419.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_4518419
loop_
_publ_author_name
'Liao, Yi-Yu'
'Li, Jian-Rong'
'Zhang, Bo'
'Sun, Hai-Yan'
'Ma, Wen'
'Jin, Jian-Ce'
'Feng, Mei-Ling'
'Huang, Xiao-Ying'
_publ_section_title
;
 Robust and Flexible Thioantimonate Materials for Cs+ Remediation with
 Distinctive Structural Transformation: A Clear Insight into the
 Ion-Exchange Mechanism
;
_journal_name_full               'ACS Applied Materials & Interfaces'
_journal_paper_doi               10.1021/acsami.0c21756
_journal_year                    2021
_chemical_formula_moiety         'H O S14 Sb9, (K2), 3(H2 O)'
_chemical_formula_sum            'H7 K2 O4 S14 Sb9'
_chemical_formula_weight         1693.85
_space_group_crystal_system      orthorhombic
_space_group_IT_number           36
_space_group_name_Hall           'C 2c -2'
_space_group_name_H-M_alt        'C m c 21'
_atom_sites_solution_hydrogens   difmap
_audit_creation_method           SHELXL-2018/3
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   28.582(2)
_cell_length_b                   9.9030(7)
_cell_length_c                   11.2422(6)
_cell_measurement_reflns_used    4812
_cell_measurement_temperature    291(2)
_cell_measurement_theta_max      29.3850
_cell_measurement_theta_min      2.7810
_cell_volume                     3182.1(4)
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_diffrn_ambient_temperature      291(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.943
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0362
_diffrn_reflns_av_unetI/netI     0.0424
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.943
_diffrn_reflns_limit_h_max       36
_diffrn_reflns_limit_h_min       -39
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            10287
_diffrn_reflns_point_group_measured_fraction_full 0.979
_diffrn_reflns_point_group_measured_fraction_max 0.876
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.695
_diffrn_reflns_theta_min         2.176
_exptl_absorpt_coefficient_mu    8.707
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.29956
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            dark-brown
_exptl_crystal_density_diffrn    3.536
_exptl_crystal_description       flake-like
_exptl_crystal_F_000             3040
_exptl_crystal_size_max          0.500
_exptl_crystal_size_mid          0.190
_exptl_crystal_size_min          0.050
_refine_diff_density_max         2.182
_refine_diff_density_min         -1.457
_refine_diff_density_rms         0.216
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   -0.04(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.087
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     159
_refine_ls_number_reflns         4024
_refine_ls_number_restraints     25
_refine_ls_restrained_S_all      1.096
_refine_ls_R_factor_all          0.0482
_refine_ls_R_factor_gt           0.0395
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0500P)²+4.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0943
_refine_ls_wR_factor_ref         0.1012
_reflns_Friedel_coverage         0.770
_reflns_Friedel_fraction_full    0.955
_reflns_Friedel_fraction_max     0.801
_reflns_number_gt                3499
_reflns_number_total             4024
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            am0c21756_si_004.cif
_cod_data_source_block           x
_cod_original_cell_volume        3182.0(4)
_cod_database_code               4518419
_shelx_shelxl_version_number     2018/3
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_estimated_absorpt_t_min   0.098
_shelx_estimated_absorpt_t_max   0.670
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z+1/2'
'x, -y, z+1/2'
'-x, y, 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'
'-x+1/2, y+1/2, z'
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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Sb2 Sb 0.62924(3) 0.20348(8) 0.56377(8) 0.0355(2) Uani 1 1 d . . . . .
Sb3 Sb 0.68024(3) 0.51535(9) 0.70494(8) 0.0377(2) Uani 1 1 d . . . . .
Sb4 Sb 0.74489(3) 0.71582(8) 0.47823(7) 0.0344(2) Uani 1 1 d . . . . .
Sb5 Sb 0.68482(3) 0.90781(8) 0.71889(7) 0.0318(2) Uani 1 1 d . . . . .
S1 S 0.55583(14) 0.1658(7) 0.4595(4) 0.0718(14) Uani 1 1 d . . . . .
S2 S 0.61012(13) 0.0397(4) 0.7163(4) 0.0453(8) Uani 1 1 d . . . . .
S3 S 0.60339(16) 0.3946(4) 0.6829(5) 0.0643(14) Uani 1 1 d . . . . .
S4 S 0.68408(14) 0.5370(4) 0.4857(3) 0.0428(8) Uani 1 1 d . . . . .
S5 S 0.63175(14) 0.7127(3) 0.7447(3) 0.0377(8) Uani 1 1 d . . . . .
S6 S 0.68903(12) 0.9064(3) 0.5000(3) 0.0352(7) Uani 1 1 d . . . . .
S7 S 0.76531(14) 0.7066(3) 0.6851(3) 0.0382(8) Uani 1 1 d . . . . .
K1 K 0.5848(3) 0.7638(9) 0.4615(6) 0.120(2) Uani 1 1 d . . . . .
Sb1 Sb 0.500000 0.0974(2) 0.60752(17) 0.0465(6) Uani 0.769(4) 2 d S TU P A 1
O1 O 0.500000 -0.122(2) 0.578(3) 0.078(8) Uani 0.769(4) 2 d S T P A 1
H1A H 0.500000 -0.154583 0.648057 0.093 Uiso 0.769(4) 2 d R U P A 1
Sb1B Sb 0.500000 0.2945(11) 0.6029(11) 0.092(3) Uani 0.231(4) 2 d S TU P A 2
O1B O 0.500000 0.149(8) 0.783(6) 0.055(17) Uani 0.231(4) 2 d S TU P A 2
H1B H 0.482390 0.183284 0.836151 0.083 Uiso 0.115(2) 1 d R U P A 2
O3 O 0.500000 0.360(4) 0.256(3) 0.168(13) Uani 1 2 d S TU P . .
H3A H 0.476230 0.309822 0.251818 0.252 Uiso 0.5 1 d R U P . .
H3B H 0.500000 0.417481 0.199908 0.252 Uiso 1 2 d R U P . .
O2 O 0.4424(16) 0.556(9) 0.455(7) 0.33(6) Uani 0.5 1 d . . P B 1
O2B O 0.482(2) 0.556(6) 0.488(6) 0.23(3) Uani 0.5 1 d . U P C 2
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
K K 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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
_geom_angle_publ_flag
S2 Sb2 S1 92.51(15) . . ?
S2 Sb2 S3 93.59(17) . . ?
S1 Sb2 S3 97.04(19) . . ?
S5 Sb3 S4 97.96(13) . . ?
S5 Sb3 S3 84.42(13) . . ?
S4 Sb3 S3 88.96(16) . . ?
S7 Sb4 S4 96.33(12) . . ?
S7 Sb4 S6 95.14(11) . . ?
S4 Sb4 S6 95.10(13) . . ?
S6 Sb5 S5 98.21(12) . . ?
S6 Sb5 S2 91.89(13) . 1_565 ?
S5 Sb5 S2 83.44(12) . 1_565 ?
Sb1 S1 Sb2 106.41(18) . . ?
Sb2 S1 Sb1B 98.9(3) . . ?
Sb2 S2 Sb5 99.50(13) . 1_545 ?
Sb2 S2 K1 103.59(18) . 3_565 ?
Sb5 S2 K1 117.6(2) 1_545 3_565 ?
Sb2 S3 Sb3 99.15(15) . . ?
Sb2 S3 K1 100.82(19) . 3_565 ?
Sb3 S3 K1 104.7(2) . 3_565 ?
Sb3 S4 Sb4 97.27(13) . . ?
Sb3 S4 K1 95.37(16) . . ?
Sb4 S4 K1 95.91(17) . . ?
Sb3 S5 Sb5 104.85(14) . . ?
Sb3 S5 K1 99.62(18) . . ?
Sb5 S5 K1 90.88(16) . . ?
Sb5 S6 Sb4 97.72(11) . . ?
Sb5 S6 K1 95.10(16) . . ?
Sb4 S6 K1 103.88(19) . . ?
O2 K1 O2B 23.5(19) 4_655 4_655 ?
O2 K1 O1 94.7(16) 4_655 1_565 ?
O2 K1 O1B 88.0(18) 4_655 2_664 ?
O1 K1 O1B 64.1(13) 1_565 2_664 ?
O2 K1 S6 135.9(12) 4_655 . ?
O2B K1 S6 154.3(14) 4_655 . ?
O1 K1 S6 120.7(5) 1_565 . ?
O1B K1 S6 129.3(11) 2_664 . ?
O2 K1 S2 125(2) 4_655 3_564 ?
O1 K1 S2 107.9(6) 1_565 3_564 ?
S6 K1 S2 71.16(17) . 3_564 ?
O2 K1 S5 91.8(18) 4_655 . ?
O2B K1 S5 93.3(13) 4_655 . ?
O1 K1 S5 88.1(6) 1_565 . ?
O1B K1 S5 152.1(11) 2_664 . ?
S6 K1 S5 66.33(16) . . ?
S2 K1 S5 136.9(2) 3_564 . ?
O2 K1 S3 67(2) 4_655 3_564 ?
O1 K1 S3 132.7(6) 1_565 3_564 ?
S6 K1 S3 99.7(2) . 3_564 ?
S2 K1 S3 60.81(15) 3_564 3_564 ?
S5 K1 S3 133.2(3) . 3_564 ?
O2 K1 S4 72.5(11) 4_655 . ?
O2B K1 S4 93.9(13) 4_655 . ?
O1 K1 S4 147.0(6) 1_565 . ?
O1B K1 S4 142.3(13) 2_664 . ?
S6 K1 S4 63.44(17) . . ?
S2 K1 S4 104.2(2) 3_564 . ?
S5 K1 S4 62.71(17) . . ?
S3 K1 S4 71.05(18) 3_564 . ?
O2 K1 K1 69.3(12) 4_655 4_655 ?
O1 K1 K1 35.5(5) 1_565 4_655 ?
S6 K1 K1 153.61(16) . 4_655 ?
S2 K1 K1 102.09(15) 3_564 4_655 ?
S5 K1 K1 112.58(15) . 4_655 ?
S3 K1 K1 98.61(15) 3_564 4_655 ?
S4 K1 K1 141.42(14) . 4_655 ?
O2 K1 H1B 84(2) 4_655 2_664 ?
O1 K1 H1B 62.0(17) 1_565 2_664 ?
S6 K1 H1B 133.6(16) . 2_664 ?
S2 K1 H1B 65.3(14) 3_564 2_664 ?
S5 K1 H1B 149.3(14) . 2_664 ?
S3 K1 H1B 72.7(16) 3_564 2_664 ?
S4 K1 H1B 142.4(17) . 2_664 ?
K1 K1 H1B 38.0(14) 4_655 2_664 ?
O1 Sb1 S1 100.0(6) . 4_655 ?
O1 Sb1 S1 100.0(6) . . ?
S1 Sb1 S1 83.2(2) 4_655 . ?
Sb1 O1 K1 116.2(6) . 4_645 ?
Sb1 O1 K1 116.2(6) . 1_545 ?
K1 O1 K1 109.0(9) 4_645 1_545 ?
Sb1 O1 H1A 103.4 . . ?
K1 O1 H1A 105.4 4_645 . ?
K1 O1 H1A 105.4 1_545 . ?
O1B Sb1B S1 102.7(14) . . ?
S1 Sb1B S1 75.7(4) . 4_655 ?
K1 O1B K1 96.0(19) 3_565 2_665 ?
Sb1B O1B H1B 109.6 . . ?
K1 O1B H1B 84.5 3_565 . ?
K1 O1B H1B 12.7 2_665 . ?
K1 O1B H1B 12.7(10) 3_565 4_655 ?
K1 O1B H1B 84.5(10) 2_665 4_655 ?
H3A O3 H3B 110.6 . . ?
H3A O3 H3A 107.5 . 4_655 ?
H3B O3 H3A 110.6 . 4_655 ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Sb2 S2 2.423(4) . ?
Sb2 S1 2.432(4) . ?
Sb2 S3 2.433(4) . ?
Sb2 S7 3.308(4) 8_645 ?
Sb2 S6 3.477(3) 1_545 ?
Sb2 S5 3.682(4) 3_564 ?
Sb2 S4 3.759(4) . ?
Sb3 S5 2.437(3) . ?
Sb3 S4 2.476(4) . ?
Sb3 S3 2.513(5) . ?
Sb3 S7 3.090(4) . ?
Sb3 S4 3.201(4) 3_565 ?
Sb3 S7 3.438(4) 8_645 ?
Sb4 S7 2.400(3) . ?
Sb4 S4 2.483(4) . ?
Sb4 S6 2.484(3) . ?
Sb4 S7 3.396(3) 6_664 ?
Sb4 S6 3.608(4) 8_645 ?
Sb4 S4 3.774(4) 8_655 ?
Sb5 S6 2.463(3) . ?
Sb5 S5 2.473(3) . ?
Sb5 S2 2.503(4) 1_565 ?
Sb5 S7 3.067(4) . ?
Sb5 S7 3.306(3) 8_655 ?
Sb5 S6 3.659(3) 3_575 ?
S1 Sb1 2.403(5) . ?
S1 Sb1B 2.602(11) . ?
S2 Sb1 3.425(4) . ?
S2 K1 3.450(9) 3_565 ?
S3 Sb1B 3.244(6) . ?
S3 K1 3.542(9) 3_565 ?
S4 K1 3.629(10) . ?
S5 K1 3.492(8) . ?
S6 K1 3.325(9) . ?
K1 O2 2.20(9) 4_655 ?
K1 O2B 2.81(6) 4_655 ?
K1 O1 2.977(18) 1_565 ?
K1 O1B 3.26(5) 2_664 ?
K1 H1B 2.44(5) 2_664 ?
Sb1 O1 2.20(2) . ?
O1 H1A 0.8515 . ?
Sb1B O1B 2.49(7) . ?
Sb1B O2B 2.95(6) 4_655 ?
Sb1B O2B 2.95(6) . ?
O1B H1B 0.8500 . ?
O1B H1B 0.8499 4_655 ?
O3 H3A 0.8425 . ?
O3 H3B 0.8509 . ?
O3 H3A 0.8426 4_655 ?
