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_7244584
_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, C8 H25.73 Fe N6, C8 H25 Fe N6, C2 H6 O2'
_chemical_formula_sum            'C18 H56.73 Fe2 N12 O2 S14 Sn6'
_chemical_formula_weight         1746.17
_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   mixed
_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                 102.540(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   21.6663(5)
_cell_length_b                   13.0707(2)
_cell_length_c                   18.7948(4)
_cell_measurement_reflns_used    22536
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      33.1830
_cell_measurement_theta_min      1.8320
_cell_volume                     5195.60(19)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46c (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46c (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46c (Rigaku OD, 2018)'
_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_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.998
_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   -118.00  62.00   0.50    8.00    --  -28.00  45.00 180.00  360
  2  \w   -118.00  22.00   0.50    8.00    --  -28.00  45.00  90.00  280
  3  \w   -118.00 -38.00   0.50    8.00    --  -28.00  45.00   0.00  160
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type
'dtrek-CrysAlisPro-abstract goniometer imported rigaku-d*trek images'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0038022000
_diffrn_orient_matrix_UB_12      -0.0231994000
_diffrn_orient_matrix_UB_13      -0.0328722000
_diffrn_orient_matrix_UB_21      -0.0260755000
_diffrn_orient_matrix_UB_22      0.0284436000
_diffrn_orient_matrix_UB_23      -0.0196449000
_diffrn_orient_matrix_UB_31      0.0207257000
_diffrn_orient_matrix_UB_32      0.0400268000
_diffrn_orient_matrix_UB_33      -0.0051550000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0497
_diffrn_reflns_av_unetI/netI     0.0488
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            38430
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.101
_diffrn_reflns_theta_min         1.832
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    3.975
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.29133
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46c (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    2.232
_exptl_crystal_description       plank
_exptl_crystal_F_000             3363
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.063
_refine_diff_density_min         -0.801
_refine_diff_density_rms         0.136
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.986
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     492
_refine_ls_number_reflns         11456
_refine_ls_number_restraints     39
_refine_ls_restrained_S_all      0.986
_refine_ls_R_factor_all          0.0538
_refine_ls_R_factor_gt           0.0340
_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^)+(0.0334P)^2^+0.7053P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0670
_refine_ls_wR_factor_ref         0.0721
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8938
_reflns_number_total             11456
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2ce00043a2.cif
_cod_data_source_block           SnS-Fe
_cod_database_code               7244584
_shelxl_version_number           2013-2
_chemical_oxdiff_formula         'C11 H10 N O'
_shelx_estimated_absorpt_t_max   0.692
_shelx_estimated_absorpt_t_min   0.299
_reflns_odcompleteness_completeness 99.97
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     27.04
_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. Restrained distances
 H1-S12_$1
 2.5 with sigma of 0.02
 H1-N3
 3.74 with sigma of 0.02
 H1-C17
 1.78 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(Sn4) \\sim Ueq, Uanis(Sn6) \\sim Ueq, Uanis(Sn3) \\sim Ueq, Uanis(Sn5)
\\sim Ueq, Uanis(Sn1) \\sim Ueq, Uanis(Sn2) \\sim Ueq: with sigma of 0.1 and
sigma for terminal atoms of 0.2
4. Rigid body (RIGU) restrains
 Sn4
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.001
5. Others
 Fixed Sof: H4B(0.7347)
6.a Ternary CH refined with riding coordinates:
 N2(H2), N5(H5), N8(H8), N11(H11)
6.b Secondary CH2 refined with riding coordinates:
 N4(H4A,H4B), N6(H6A,H6B), N3(H3A,H3B), N1(H1A,H1B), C4(H4C,H4D), C2(H2A,H2B),
 C1(H1C,H1D), C3(H3C,H3D), N9(H9A,H9B), N12(H12A,H12B), C7(H7A,H7B), N7(H7C,
 H7D), C11(H11A,H11B), C10(H10A,H10B), C15(H15A,H15B), C16(H16A,H16B), C12(H12C,
 H12D), C14(H14A,H14B), C13(H13A,H13B), C8(H8A,H8B), C5(H5A,H5B), C9(H9C,H9D),
 C6(H6C,H6D), C17(H17A,H17B), C18(H18A,H18B)
6.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
_shelx_res_checksum              70657
_shelx_hkl_checksum              40733
_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
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 3.284
_oxdiff_exptl_absorpt_empirical_full_min 0.386