The structure-directing amine changes everything: structures and optical properties of two-dimensional thiostannates.
Filsø, Mette Ø; Chaaban, Iman; Al Shehabi, Amer; Skibsted, Jørgen; Lock, Nina; Acta crystallographica Section B, Structural science, crystal engineering and materials 73 (2017) 931–940; doi:10.1107/S2052520617010630

data_2311790
_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         'S7 Sn3, 2(C7 H13 N2)'
_chemical_formula_sum            'C14 H26 N4 S7 Sn3'
_chemical_formula_weight         830.94
_chemical_name_common            1AEP-SnS-1
_space_group_crystal_system      orthorhombic
_space_group_IT_number           18
_space_group_name_Hall           'P 2 2ab'
_space_group_name_H-M_alt        'P 21 21 2'
_atom_sites_solution_hydrogens   geom
_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                90
_cell_formula_units_Z            4
_cell_length_a                   13.2299(2)
_cell_length_b                   22.2673(3)
_cell_length_c                   9.0772(2)
_cell_measurement_reflns_used    9207
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      26.454
_cell_measurement_theta_min      2.243
_cell_volume                     2674.09(8)
_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 1.000
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_device_type  'Bruker X8 APEX-II diffractometer'
_diffrn_measurement_method
; 
Narrow slices collected using \f- and \w-scans 
;
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0587
_diffrn_reflns_av_unetI/netI     0.0776
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.985
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            34528
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.956
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         32.425
_diffrn_reflns_theta_min         1.829
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    3.337
_exptl_absorpt_correction_T_max  0.8330
_exptl_absorpt_correction_T_min  0.7094
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
SADABS (Sheldrick, 2004) 
;
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_diffrn    2.064
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1600
_exptl_crystal_recrystallization_method solvothermal
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.647
_refine_diff_density_min         -0.594
_refine_diff_density_rms         0.136
_refine_ls_abs_structure_details
;
 Flack x determined using 2184 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.015(14)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.958
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     264
_refine_ls_number_reflns         9206
_refine_ls_number_restraints     281
_refine_ls_restrained_S_all      0.956
_refine_ls_R_factor_all          0.0826
_refine_ls_R_factor_gt           0.0383
_refine_ls_shift/su_max          0.010
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0195P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0499
_refine_ls_wR_factor_ref         0.0574
_reflns_Friedel_coverage         0.748
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.921
_reflns_number_gt                6297
_reflns_number_total             9206
_reflns_threshold_expression     'I > 4\s(I)'
_cod_data_source_file            ao5023sup1.cif
_cod_data_source_block           SnS_1AEP_300K
_cod_database_code               2311790
_shelx_shelxl_version_number     2014/7
_shelx_res_checksum              4317
_shelx_hkl_checksum              50831
_ccdc_publ_extra_info
'In the chemical diagram it appears that the position of the double bond is different in the two cations. The double bond is expected to be delocalized over the two positions in both cations.'