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#$Date: 2019-12-26 21:25:46 +0200 (Thu, 26 Dec 2019) $
#$Revision: 246106 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/31/17/2311789.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_2311789
loop_
_publ_author_name
'Filsø, Mette Ø'
'Chaaban, Iman'
'Al Shehabi, Amer'
'Skibsted, Jørgen'
'Lock, Nina'
_publ_section_title
;
 The structure-directing amine changes everything: structures and optical
 properties of two-dimensional thiostannates.
;
_journal_coeditor_code           AO5023SUP1
_journal_issue                   'Pt 5'
_journal_name_full
'Acta crystallographica Section B, Structural science, crystal engineering and materials'
_journal_page_first              931
_journal_page_last               940
_journal_paper_doi               10.1107/S2052520617010630
_journal_volume                  73
_journal_year                    2017
_chemical_formula_moiety         'S28 Sn12'
_chemical_formula_sum            'S28 Sn12'
_chemical_formula_weight         2322.20
_chemical_name_common            tren-SnS-1
_space_group_crystal_system      hexagonal
_space_group_IT_number           194
_space_group_name_Hall           '-P 6c 2c'
_space_group_name_H-M_alt        'P 63/m m c'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            1
_cell_length_a                   13.2748(4)
_cell_length_b                   13.2748(4)
_cell_length_c                   19.1521(7)
_cell_measurement_reflns_used    1297
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      26.546
_cell_measurement_theta_min      2.7665
_cell_volume                     2922.83(16)
_computing_cell_refinement       'APEX2 v2010.1-2 (Bruker AXS, 2005-2009)'
_computing_data_collection       'APEX2 v2010.1-2 (Bruker AXS, 2005-2009)'
_computing_data_reduction        'APEX2 v2010.1-2 (Bruker AXS, 2005-2009)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'ShelXle (Huebschle, 2011)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      298(2)
_diffrn_detector_area_resol_mean 12.00
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'APEX2 charged-coupled device'
_diffrn_measurement_method
; 
Narrow slices collected using φ- and ω-scans 
;
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0482
_diffrn_reflns_av_unetI/netI     0.0221
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            20714
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.428
_diffrn_reflns_theta_min         1.771
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    3.018
_exptl_absorpt_correction_T_max  0.7685
_exptl_absorpt_correction_T_min  0.6569
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
SADABS (Sheldrick, 2004) 
;
_exptl_crystal_colour            'pale green'
_exptl_crystal_density_diffrn    1.319
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1048
_exptl_crystal_recrystallization_method solvothermal
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.539
_refine_diff_density_min         -1.160
_refine_diff_density_rms         0.319
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.149
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     22
_refine_ls_number_reflns         1297
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.149
_refine_ls_R_factor_all          0.0802
_refine_ls_R_factor_gt           0.0584
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.1418P)²+5.8926P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2148
_refine_ls_wR_factor_ref         0.2266
_reflns_Friedel_coverage         0.000
_reflns_number_gt                959
_reflns_number_total             1297
_reflns_threshold_expression     'I > 4σ(I)'
_cod_data_source_file            ao5023sup1.cif
_cod_data_source_block           SnS_TAEA_300K
_cod_original_cell_volume        2922.8(2)
_cod_database_code               2311789
_shelx_shelxl_version_number     2014/7
_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.
;
_ccdc_publ_extra_info
'The molecular cations between the thiostannate layers are disordered, and only the structure of anionic polymeric layers have been determined.'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'-x, -y, z+1/2'
'y, -x+y, z+1/2'
'x-y, x, z+1/2'
'y, x, -z'
'x-y, -y, -z'
'-x, -x+y, -z'
'-y, -x, -z+1/2'
'-x+y, y, -z+1/2'
'x, x-y, -z+1/2'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'x, y, -z-1/2'
'-y, x-y, -z-1/2'
'-x+y, -x, -z-1/2'
'-y, -x, z'
'-x+y, y, z'
'x, x-y, z'
'y, x, z-1/2'
'x-y, -y, z-1/2'
'-x, -x+y, 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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
Sn1 Sn 0.84744(6) 0.42372(3) 0.49152(5) 0.0495(4) Uani 1 2 d S T P
S1 S 0.6667 0.3333 0.5743(3) 0.0445(10) Uani 1 6 d S T P
S2 S 0.76919(14) 0.23081(14) 0.4409(2) 0.0644(10) Uani 1 2 d S T P
S3 S 0.9780(3) 0.48899(13) 0.58937(18) 0.0653(9) Uani 1 2 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'
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
S3 Sn1 S2 122.85(10) . 2_655
S3 Sn1 S2 122.85(10) . .
S2 Sn1 S2 114.11(19) 2_655 .
S3 Sn1 S3 88.98(11) . 13_766
S2 Sn1 S3 92.81(8) 2_655 13_766
S2 Sn1 S3 92.81(8) . 13_766
S3 Sn1 S1 91.34(12) . .
S2 Sn1 S1 87.02(8) 2_655 .
S2 Sn1 S1 87.02(8) . .
S3 Sn1 S1 179.68(12) 13_766 .
Sn1 S1 Sn1 87.02(13) 3_665 2_655
Sn1 S1 Sn1 87.02(13) 3_665 .
Sn1 S1 Sn1 87.02(13) 2_655 .
Sn1 S2 Sn1 95.44(11) . 3_665
Sn1 S3 Sn1 91.02(11) . 13_766
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Sn1 S3 2.401(3) .
Sn1 S2 2.433(2) 2_655
Sn1 S2 2.433(2) .
Sn1 S3 2.535(3) 13_766
Sn1 S1 2.614(3) .
S1 Sn1 2.614(3) 3_665
S1 Sn1 2.614(3) 2_655
S2 Sn1 2.433(2) 3_665
S3 Sn1 2.535(3) 13_766
