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_7244585
_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 N6 Zn), C2 H6 O2'
_chemical_formula_sum            'C18 H58 N12 O2 S14 Sn6 Zn2'
_chemical_formula_weight         1766.48
_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                 102.264(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   21.4593(5)
_cell_length_b                   12.9922(4)
_cell_length_c                   18.7194(6)
_cell_measurement_reflns_used    24882
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      60.5970
_cell_measurement_theta_min      3.4690
_cell_volume                     5099.9(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 0.992
_diffrn_measured_fraction_theta_max 0.963
_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     50.00 106.00   0.50    0.40    --   73.66  77.00 120.00  112
  2  \w    111.00 147.00   0.50    0.40    --   73.66  77.00 120.00   72
  3  \w     88.00 113.00   0.50    0.40    --   73.66 127.00 141.00   50
  4  \w     83.00 108.00   0.50    0.40    --   73.66 143.00 -48.00   50
  5  \w    -70.00 -21.00   0.50    0.40    --  -74.91  38.00 120.00   98
  6  \w    -90.00 -42.00   0.50    0.40    --  -74.91  57.00 150.00   96
  7  \w    -23.00   2.00   0.50    0.10    --   -0.62  77.00  60.00   50
  8  \w   -122.00 -42.00   0.50    0.40    --  -74.91 143.00 -48.00  160
  9  \w      2.00  35.00   0.50    0.10    --   -0.62  38.00-120.00   66
 10  \w     35.00  71.00   0.50    0.40    --   73.66 -38.00  30.00   72
 11  \w     63.00 120.00   0.50    0.40    --   73.66-143.00-103.00  114
 12  \w     43.00  68.00   0.50    0.40    --   73.66-127.00  66.00   50
 13  \w   -131.00-106.00   0.50    0.40    --  -74.91-143.00-103.00   50
 14  \w   -143.00-118.00   0.50    0.40    --  -74.91-125.00 -60.00   50
 15  \w   -140.00 -52.00   0.50    0.40    --  -74.91 -77.00-120.00  176
 16  \w   -110.00 -80.00   0.50    0.40    --  -74.91-125.00 -60.00   60
 17  \w   -130.00-103.00   0.50    0.40    --  -74.91-127.00  66.00   54
 18  \w   -147.00 -88.00   0.50    0.40    --  -74.91 -99.00 120.00  118
 19  \w    -70.00  15.00   0.50    0.10    --   -0.62 -57.00 120.00  170
;
_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      0.0478591000
_diffrn_orient_matrix_UB_12      0.0244596000
_diffrn_orient_matrix_UB_13      0.0558472000
_diffrn_orient_matrix_UB_21      0.0141242000
_diffrn_orient_matrix_UB_22      -0.0999490000
_diffrn_orient_matrix_UB_23      0.0110028000
_diffrn_orient_matrix_UB_31      0.0398458000
_diffrn_orient_matrix_UB_32      0.0058951000
_diffrn_orient_matrix_UB_33      -0.0460695000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0389
_diffrn_reflns_av_unetI/netI     0.0375
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.963
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            42421
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.963
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.559
_diffrn_reflns_theta_min         1.844
_diffrn_source                   'micro-focus metaljet'
_exptl_absorpt_coefficient_mu    4.421
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.56918
_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 light yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    2.301
_exptl_crystal_description       block
_exptl_crystal_F_000             3400
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.294
_refine_diff_density_min         -2.166
_refine_diff_density_rms         0.209
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.135
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     489
_refine_ls_number_reflns         11347
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.135
_refine_ls_R_factor_all          0.0491
_refine_ls_R_factor_gt           0.0428
_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^)+87.2251P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0927
_refine_ls_wR_factor_ref         0.0953
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10204
_reflns_number_total             11347
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2ce00043a2.cif
_cod_data_source_block           SnS-Zn
_cod_database_code               7244585
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.666
_shelx_estimated_absorpt_t_min   0.472
_reflns_odcompleteness_completeness 99.91
_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:
 N11(H11), N8(H8), N5(H5), N2(H2)
2.b Secondary CH2 refined with riding coordinates:
 N9(H9A,H9B), N12(H12A,H12B), N10(H10A,H10B), N4(H4A,H4B), N3(H3A,H3B),
 C14(H14A,H14B), N7(H7A,H7B), C16(H16A,H16B), N1(H1A,H1B), C15(H15A,H15B),
 N6(H6A,H6B), C13(H13A,H13B), C11(H11A,H11B), C5(H5A,H5B), C7(H7C,H7D), C9(H9C,
 H9D), C1(H1C,H1D), C2(H2A,H2B), C3(H3C,H3D), C17(H17A,H17B), C6(H6C,H6D),
 C8(H8A,H8B), C10(H10C,H10D), C4(H4C,H4D), C12(H12C,H12D), C18(H18A,H18B)
2.c Idealised tetrahedral OH refined as rotating group:
 O2(H2C), O1(H1)
;
_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 2.277
_oxdiff_exptl_absorpt_empirical_full_min 0.583