#------------------------------------------------------------------------------
#$Date: 2016-02-04 23:44:16 +0200 (Thu, 04 Feb 2016) $
#$Revision: 175905 $
#$URL: svn://www.crystallography.net/cod/cif/1/54/04/1540429.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_1540429
loop_
_publ_author_name
'Sarma, Debajit'
'Malliakas, Christos D.'
'Subrahmanyam, K. S.'
'Islam, Saiful M.'
'Kanatzidis, Mercouri G.'
_publ_section_title
;
 K2xSn4−xS8−x(x = 0.65--1): a new metal sulfide for rapid
 and selective removal of Cs+, Sr2+and UO22+ions
;
_journal_issue                   2
_journal_name_full               'Chem. Sci.'
_journal_page_first              1121
_journal_paper_doi               10.1039/C5SC03040D
_journal_volume                  7
_journal_year                    2016
_chemical_formula_sum            'K2 S7 Sn3'
_chemical_formula_weight         658.69
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           63
_space_group_name_Hall           '-C 2c 2'
_space_group_name_H-M_alt        'C m c m'
_symmetry_space_group_name_Hall  '-C 2c 2'
_symmetry_space_group_name_H-M   'C m c m'
_audit_creation_method           SHELXL
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   3.6831(2)
_cell_length_b                   25.8877(19)
_cell_length_c                   16.8155(11)
_cell_measurement_temperature    293(2)
_cell_volume                     1603.31(18)
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'image plate (34 cm diameter)'
_diffrn_detector_area_resol_mean 6.67
_diffrn_detector_type            STOE
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device       '2-circle goniometer'
_diffrn_measurement_device_type  'STOE IPDS 2'
_diffrn_measurement_method       'rotation method'
_diffrn_radiation_collimation    '0.5 mm diameter, monocapillary'
_diffrn_radiation_monochromator  'plane graphite'
_diffrn_radiation_polarisn_norm  0
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0590
_diffrn_reflns_av_unetI/netI     0.0219
_diffrn_reflns_laue_measured_fraction_full 0.997
_diffrn_reflns_laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       4
_diffrn_reflns_limit_h_min       -4
_diffrn_reflns_limit_k_max       34
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            13142
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.991
_diffrn_reflns_theta_min         2.422
_diffrn_source
'sealed X-ray tube, 12 x 0.4 mm long-fine focus'
_diffrn_source_current           40
_diffrn_source_power             2.00
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    6.026
_exptl_absorpt_correction_T_max  0.753
_exptl_absorpt_correction_T_min  0.249
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   X-Area
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.729
_exptl_crystal_description       block
_exptl_crystal_F_000             1200
_exptl_crystal_size_max          0.320
_exptl_crystal_size_mid          0.160
_exptl_crystal_size_min          0.050
_refine_diff_density_max         3.868
_refine_diff_density_min         -1.905
_refine_diff_density_rms         0.335
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.140
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     45
_refine_ls_number_reflns         1145
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.140
_refine_ls_R_factor_all          0.0796
_refine_ls_R_factor_gt           0.0749
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.1110P)²+74.4974P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2183
_refine_ls_wR_factor_ref         0.2237
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1072
_reflns_number_total             1145
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c5sc03040d2.cif
_cod_data_source_block           K2Sn3S7_Subcell
_cod_depositor_comments
'Adding full bibliography for 1540429--1540430.cif.'
_cod_database_code               1540429
_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   0.249
_shelx_estimated_absorpt_t_max   0.753
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'
'-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
Sn1 Sn 0.0000 0.18670(3) 0.48613(7) 0.0257(4) Uani 1 2 d S T P
Sn2 Sn -0.5000 0.06612(8) 0.51825(15) 0.0346(6) Uani 0.5 2 d S T P
S1 S 0.0000 0.27693(12) 0.4206(2) 0.0244(7) Uani 1 2 d S T P
S2 S -0.5000 0.15494(15) 0.3979(3) 0.0343(9) Uani 1 2 d S T P
S3 S 0.0000 0.10403(15) 0.5675(3) 0.0401(10) Uani 1 2 d S T P
S4 S -0.5000 0.0163(3) 0.4038(8) 0.053(3) Uani 0.5 2 d S T P
K1 K -0.5000 0.2438(7) 0.2500 0.213(11) Uani 1 4 d S T P
K2 K 0.0000 0.1628(14) 0.7500 0.44(3) Uani 1 4 d S T P
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
S S 0.1246 0.1234 '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'
Sn Sn -0.6537 1.4246 '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
S2 Sn1 S2 94.69(14) . 1_655
S2 Sn1 S3 92.44(12) . .
S2 Sn1 S3 92.44(12) 1_655 .
S2 Sn1 S1 92.52(11) . .
S2 Sn1 S1 92.52(11) 1_655 .
S3 Sn1 S1 172.67(14) . .
S2 Sn1 S1 177.44(9) . 13_556
S2 Sn1 S1 87.45(9) 1_655 13_556
S3 Sn1 S1 88.87(10) . 13_556
S1 Sn1 S1 85.97(10) . 13_556
S2 Sn1 S1 87.45(9) . 13_456
S2 Sn1 S1 177.44(9) 1_655 13_456
S3 Sn1 S1 88.87(10) . 13_456
S1 Sn1 S1 85.97(10) . 13_456
S1 Sn1 S1 90.39(11) 13_556 13_456
S3 Sn2 S3 110.2(2) 1_455 .
S3 Sn2 S4 123.35(12) 1_455 .
S3 Sn2 S4 123.35(12) . .
S3 Sn2 S4 100.3(2) 1_455 9_456
S3 Sn2 S4 100.3(2) . 9_456
S4 Sn2 S4 87.7(4) . 9_456
Sn1 S1 Sn1 94.03(10) . 13_556
Sn1 S1 Sn1 94.03(10) . 13_456
Sn1 S1 Sn1 90.39(11) 13_556 13_456
Sn1 S1 K1 97.3(3) . 1_655
Sn1 S1 K1 102.12(10) 13_556 1_655
Sn1 S1 K1 162.42(17) 13_456 1_655
Sn1 S1 K1 97.3(3) . .
Sn1 S1 K1 162.42(17) 13_556 .
Sn1 S1 K1 102.12(10) 13_456 .
K1 S1 K1 63.18(11) 1_655 .
Sn1 S1 K2 134.7(5) . 13_456
Sn1 S1 K2 131.3(5) 13_556 13_456
Sn1 S1 K2 87.9(2) 13_456 13_456
K1 S1 K2 74.6(2) 1_655 13_456
K1 S1 K2 38.7(5) . 13_456
Sn1 S1 K2 134.7(5) . 13_556
Sn1 S1 K2 87.9(2) 13_556 13_556
Sn1 S1 K2 131.3(5) 13_456 13_556
K1 S1 K2 38.7(6) 1_655 13_556
K1 S1 K2 74.6(2) . 13_556
K2 S1 K2 58.8(3) 13_456 13_556
Sn1 S2 Sn1 94.69(14) . 1_455
Sn1 S2 K1 102.26(19) . .
Sn1 S2 K1 102.26(19) 1_455 .
Sn2 S3 Sn2 110.2(2) . 1_655
Sn2 S3 Sn1 99.78(14) . .
Sn2 S3 Sn1 99.78(14) 1_655 .
Sn2 S3 K2 121.63(19) . .
Sn2 S3 K2 121.63(19) 1_655 .
Sn1 S3 K2 96.2(6) . .
Sn2 S4 Sn2 92.3(4) . 9_456
K2 K1 S2 132.8(2) 13_456 10_556
K2 K1 S2 132.8(2) 13_456 .
S2 K1 S2 94.5(5) 10_556 .
K2 K1 S1 75.9(3) 13_456 10_456
S2 K1 S1 64.32(10) 10_556 10_456
S2 K1 S1 139.9(4) . 10_456
K2 K1 S1 75.9(3) 13_456 1_455
S2 K1 S1 139.9(4) 10_556 1_455
S2 K1 S1 64.32(10) . 1_455
S1 K1 S1 109.4(2) 10_456 1_455
K2 K1 S1 75.9(3) 13_456 10_556
S2 K1 S1 64.32(10) 10_556 10_556
S2 K1 S1 139.9(4) . 10_556
S1 K1 S1 63.18(11) 10_456 10_556
S1 K1 S1 151.7(6) 1_455 10_556
K2 K1 S1 75.9(3) 13_456 .
S2 K1 S1 139.9(4) 10_556 .
S2 K1 S1 64.32(10) . .
S1 K1 S1 151.7(6) 10_456 .
S1 K1 S1 63.18(11) 1_455 .
S1 K1 S1 109.4(2) 10_556 .
K2 K1 K1 89.999(1) 13_456 1_455
S2 K1 K1 90.0 10_556 1_455
S2 K1 K1 90.0 . 1_455
S1 K1 K1 58.41(5) 10_456 1_455
S1 K1 K1 58.41(5) 1_455 1_455
S1 K1 K1 121.59(5) 10_556 1_455
S1 K1 K1 121.59(5) . 1_455
K2 K1 K1 89.999(1) 13_456 1_655
S2 K1 K1 90.0 10_556 1_655
S2 K1 K1 90.0 . 1_655
S1 K1 K1 121.59(5) 10_456 1_655
S1 K1 K1 121.59(5) 1_455 1_655
S1 K1 K1 58.41(5) 10_556 1_655
S1 K1 K1 58.41(5) . 1_655
K1 K1 K1 180.0 1_455 1_655
K2 K1 K2 56.7(4) 13_456 13_556
S2 K1 K2 111.9(2) 10_556 13_556
S2 K1 K2 111.9(2) . 13_556
S1 K1 K2 107.7(3) 10_456 13_556
S1 K1 K2 107.7(3) 1_455 13_556
S1 K1 K2 55.12(15) 10_556 13_556
S1 K1 K2 55.12(15) . 13_556
K1 K1 K2 146.7(4) 1_455 13_556
K1 K1 K2 33.3(4) 1_655 13_556
K2 K1 K2 56.7(4) 13_456 13_356
S2 K1 K2 111.9(2) 10_556 13_356
S2 K1 K2 111.9(2) . 13_356
S1 K1 K2 55.12(15) 10_456 13_356
S1 K1 K2 55.12(15) 1_455 13_356
S1 K1 K2 107.7(3) 10_556 13_356
S1 K1 K2 107.7(3) . 13_356
K1 K1 K2 33.3(4) 1_455 13_356
K1 K1 K2 146.7(4) 1_655 13_356
K2 K1 K2 113.4(8) 13_556 13_356
K1 K2 S3 116.4(6) 13_456 10_557
K1 K2 S3 116.4(6) 13_456 .
S3 K2 S3 127.3(11) 10_557 .
K1 K2 K2 89.999(3) 13_456 1_655
S3 K2 K2 90.0 10_557 1_655
S3 K2 K2 90.0 . 1_655
K1 K2 K2 89.999(1) 13_456 1_455
S3 K2 K2 90.000(1) 10_557 1_455
S3 K2 K2 90.000(1) . 1_455
K2 K2 K2 180.0 1_655 1_455
K1 K2 S1 65.4(5) 13_456 6
S3 K2 S1 59.95(8) 10_557 6
S3 K2 S1 150.51(6) . 6
K2 K2 S1 60.59(13) 1_655 6
K2 K2 S1 119.41(14) 1_455 6
K1 K2 S1 65.4(5) 13_456 13_456
S3 K2 S1 150.51(6) 10_557 13_456
S3 K2 S1 59.95(7) . 13_456
K2 K2 S1 119.41(14) 1_655 13_456
K2 K2 S1 60.59(13) 1_455 13_456
S1 K2 S1 130.8(10) 6 13_456
K1 K2 S1 65.4(5) 13_456 6_455
S3 K2 S1 59.95(7) 10_557 6_455
S3 K2 S1 150.51(6) . 6_455
K2 K2 S1 119.41(14) 1_655 6_455
K2 K2 S1 60.59(13) 1_455 6_455
S1 K2 S1 58.8(3) 6 6_455
S1 K2 S1 99.8(6) 13_456 6_455
K1 K2 S1 65.4(5) 13_456 13_556
S3 K2 S1 150.51(6) 10_557 13_556
S3 K2 S1 59.95(7) . 13_556
K2 K2 S1 60.59(13) 1_655 13_556
K2 K2 S1 119.41(14) 1_455 13_556
S1 K2 S1 99.8(6) 6 13_556
S1 K2 S1 58.8(3) 13_456 13_556
S1 K2 S1 130.8(10) 6_455 13_556
K1 K2 K1 56.7(4) 13_456 13_556
S3 K2 K1 104.11(16) 10_557 13_556
S3 K2 K1 104.11(16) . 13_556
K2 K2 K1 33.3(4) 1_655 13_556
K2 K2 K1 146.7(4) 1_455 13_556
S1 K2 K1 50.3(2) 6 13_556
S1 K2 K1 100.5(6) 13_456 13_556
S1 K2 K1 100.5(6) 6_455 13_556
S1 K2 K1 50.3(2) 13_556 13_556
K1 K2 K1 56.7(4) 13_456 13_356
S3 K2 K1 104.11(16) 10_557 13_356
S3 K2 K1 104.11(16) . 13_356
K2 K2 K1 146.7(4) 1_655 13_356
K2 K2 K1 33.3(4) 1_455 13_356
S1 K2 K1 100.5(6) 6 13_356
S1 K2 K1 50.3(2) 13_456 13_356
S1 K2 K1 50.3(2) 6_455 13_356
S1 K2 K1 100.5(6) 13_556 13_356
K1 K2 K1 113.4(8) 13_556 13_356
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Sn1 S2 2.504(3) .
Sn1 S2 2.504(3) 1_655
Sn1 S3 2.540(4) .
Sn1 S1 2.583(3) .
Sn1 S1 2.596(3) 13_556
Sn1 S1 2.596(3) 13_456
Sn2 S3 2.245(3) 1_455
Sn2 S3 2.245(3) .
Sn2 S4 2.316(13) .
Sn2 S4 2.504(9) 9_456
S1 Sn1 2.596(3) 13_556
S1 Sn1 2.596(3) 13_456
S1 K1 3.515(5) 1_655
S1 K1 3.516(5) .
S1 K2 3.750(16) 13_456
S1 K2 3.750(16) 13_556
S2 Sn1 2.504(3) 1_455
S2 K1 3.387(13) .
S3 Sn2 2.245(3) 1_655
S3 K2 3.425(17) .
S4 Sn2 2.504(9) 9_456
K1 K2 2.42(4) 13_456
K1 S2 3.386(13) 10_556
K1 S1 3.515(5) 10_456
K1 S1 3.515(5) 1_455
K1 S1 3.515(5) 10_556
K1 K1 3.6831(2) 1_455
K1 K1 3.6831(2) 1_655
K1 K2 4.41(2) 13_556
K1 K2 4.41(2) 13_356
K2 K1 2.42(4) 13_456
K2 S3 3.425(17) 10_557
K2 K2 3.6831(2) 1_655
K2 K2 3.6831(2) 1_455
K2 S1 3.750(16) 6
K2 S1 3.750(16) 13_456
K2 S1 3.750(16) 6_455
K2 S1 3.750(16) 13_556
K2 K1 4.41(2) 13_556
K2 K1 4.41(2) 13_356
