Cationic complex directed thiostannate layers with excellent proton conduction and photocatalysis properties
Liu, Kai-Li; Luo, Ming-Bu; Zhou, Xuechou; Lin, Qipu; CrystEngComm  (2022) –; doi:10.1039/D2CE00043A

data_7244586
_publ_section_title
;
 Cationic complex directed thiostannate layers with excellent proton
 conduction and photocatalysis properties
;
_journal_name_full               CrystEngComm
_journal_paper_doi               10.1039/D2CE00043A
_journal_year                    2022
_chemical_formula_moiety         'S14 Sn6, 2(C8 H26 Mn N6), C2 H6 O2'
_chemical_formula_sum            'C18 H58 Mn2 N12 O2 S14 Sn6'
_chemical_formula_weight         1745.62
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2022-03-01
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2022-03-03 deposited with the CCDC.	2022-03-10 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 103.740(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   21.7391(6)
_cell_length_b                   13.0228(3)
_cell_length_c                   18.5826(6)
_cell_measurement_reflns_used    40932
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      60.5970
_cell_measurement_theta_min      3.4590
_cell_volume                     5110.3(3)
_computing_cell_refinement       'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.957
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w     63.00  88.00   0.50    0.28    --   72.41  38.00  30.00   50
  2  \w    108.00 134.00   0.50    0.28    --   72.41  38.00  30.00   52
  3  \w     89.00 118.00   0.50    0.28    --   72.41 101.00  45.00   58
  4  \w    112.00 138.00   0.50    0.28    --   72.41  19.00-180.00   52
  5  \w     57.00  82.00   0.50    0.28    --   72.41  19.00-180.00   50
  6  \w     53.00 105.00   0.50    0.28    --   72.41 -99.00-180.00  104
  7  \w     20.00 111.00   0.50    0.28    --   72.41-125.00-180.00  182
  8  \w      0.00  64.00   0.50    0.28    --   72.41-101.00 -58.00  128
  9  \w     71.00 102.00   0.50    0.28    --   72.41-101.00 -58.00   62
 10  \w      2.00  95.00   0.50    0.28    --   72.41 -77.00 -60.00  186
 11  \w      0.00  32.00   0.50    0.28    --   72.41 -77.00-120.00   64
 12  \w     58.00  94.00   0.50    0.28    --   72.41 -77.00-120.00   72
 13  \w     28.00  88.00   0.50    0.28    --   72.41 -57.00   0.00  120
 14  \w      0.00  71.00   0.50    0.28    --   72.41 -38.00   0.00  142
 15  \w      0.00  45.00   0.50    0.28    --   72.41 -38.00 -30.00   90
 16  \w     -1.00  48.00   0.50    0.07    --   -1.25  77.00  60.00   98
 17  \w    -85.00 -59.00   0.50    0.28    --  -74.91 101.00  45.00   52
 18  \w   -110.00 -26.00   0.50    0.28    --  -74.91 125.00  60.00  168
 19  \w    -17.00  72.00   0.50    0.07    --   -1.25  57.00 -60.00  178
 20  \w     15.00  41.00   0.50    0.07    --   -1.25  77.00-180.00   52
 21  \w    -91.00 -26.00   0.50    0.28    --  -74.91 125.00-180.00  130
 22  \w    -70.00  -1.00   0.50    0.28    --  -74.91  38.00-120.00  138
 23  \w    -68.00  -7.00   0.50    0.28    --  -74.91  38.00-150.00  122
 24  \w    -40.00  -1.00   0.50    0.28    --  -74.91  38.00   0.00   78
 25  \w   -129.00 -89.00   0.50    0.28    --  -74.91 -99.00-180.00   80
 26  \w   -130.00 -90.00   0.50    0.28    --  -74.91-101.00 -58.00   80
 27  \w   -116.00 -81.00   0.50    0.28    --  -74.91-125.00 -60.00   70
 28  \w   -147.00 -86.00   0.50    0.28    --  -74.91-125.00 120.00  122
 29  \w    -74.00  13.00   0.50    0.07    --   -1.25 -38.00 150.00  174
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'ROD, Synergy Custom system, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0600921000
_diffrn_orient_matrix_UB_12      0.0177360000
_diffrn_orient_matrix_UB_13      0.0026538000
_diffrn_orient_matrix_UB_21      0.0071012000
_diffrn_orient_matrix_UB_22      -0.0620735000
_diffrn_orient_matrix_UB_23      0.0588805000
_diffrn_orient_matrix_UB_31      0.0188640000
_diffrn_orient_matrix_UB_32      0.0800300000
_diffrn_orient_matrix_UB_33      0.0450888000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           GaK\a
_diffrn_radiation_wavelength     1.3405
_diffrn_reflns_av_R_equivalents  0.0912
_diffrn_reflns_av_unetI/netI     0.0491
_diffrn_reflns_Laue_measured_fraction_full 0.988
_diffrn_reflns_Laue_measured_fraction_max 0.957
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            73178
_diffrn_reflns_point_group_measured_fraction_full 0.988
_diffrn_reflns_point_group_measured_fraction_max 0.957
_diffrn_reflns_theta_full        53.543
_diffrn_reflns_theta_max         60.871
_diffrn_reflns_theta_min         3.467
_diffrn_source                   'micro-focus metaljet'
_exptl_absorpt_coefficient_mu    21.638
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.57300
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.93a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear whiteish yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   whiteish
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    2.269
_exptl_crystal_description       plank
_exptl_crystal_F_000             3360
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.484
_refine_diff_density_min         -2.133
_refine_diff_density_rms         0.254
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     489
_refine_ls_number_reflns         11334
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.061
_refine_ls_R_factor_all          0.0470
_refine_ls_R_factor_gt           0.0402
_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/[\s^2^(Fo^2^)+(0.0541P)^2^+24.2264P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1014
_refine_ls_wR_factor_ref         0.1068
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9951
_reflns_number_total             11334
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2ce00043a2.cif
_cod_data_source_block           SnS-Mn
_cod_database_code               7244586
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.221
_shelx_estimated_absorpt_t_min   0.098
_reflns_odcompleteness_completeness 100.00
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     56.82
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All N(H) groups, All N(H,H) groups
 At 1.5 times of:
  All O(H) groups
2.a Ternary CH refined with riding coordinates:
 N8(H8), N2(H2), N11(H11), N5(H5)
2.b Secondary CH2 refined with riding coordinates:
 N10(H10A,H10B), N7(H7A,H7B), N9(H9A,H9B), N12(H12A,H12B), C12(H12C,H12D),
 C11(H11A,H11B), C9(H9C,H9D), N3(H3A,H3B), C10(H10C,H10D), C13(H13A,H13B),
 N4(H4A,H4B), C14(H14A,H14B), N1(H1A,H1B), N6(H6A,H6B), C3(H3C,H3D), C15(H15A,
 H15B), C16(H16A,H16B), C5(H5A,H5B), C6(H6C,H6D), C2(H2A,H2B), C18(H18A,H18B),
 C4(H4C,H4D), C1(H1C,H1D), C7(H7C,H7D), C17(H17A,H17B), C8(H8A,H8B)
2.c Idealised tetrahedral OH refined as rotating group:
 O1(H1), O2(H2C)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 4.632
_oxdiff_exptl_absorpt_empirical_full_min 0.342