Long-chain tin(iv) alkanethiolates (Sn(SCnH2n+1)4, n ≥ 12) with the coexistence of trans and gauche S–C bonds: a class of lamellar van der Waals molecular crystals
Wang, Tingting; Wan, Yixin; Yu, Nan; Gu, Kewei; Lu, Zhiwei; Wang, Junli; CrystEngComm 25 (2023) 5782–5786; doi:10.1039/D3CE00818E

data_7247667
_publ_section_title
;
 Long-chain tin(iv) alkanethiolates (Sn(SCnH2n+1)4, n &#x2265; 12) with
 the coexistence of trans and gauche S--C bonds: a class of lamellar van
 der Waals molecular crystals
;
_journal_issue                   41
_journal_name_full               CrystEngComm
_journal_page_first              5782
_journal_page_last               5786
_journal_paper_doi               10.1039/D3CE00818E
_journal_volume                  25
_journal_year                    2023
_chemical_formula_moiety         'C64 H132 S4 Sn'
_chemical_formula_sum            'C64 H132 S4 Sn'
_chemical_formula_weight         1148.62
_chemical_melting_point          330
_chemical_name_systematic        'Tin(IV) hexadecanethiolate'
_space_group_crystal_system      monoclinic
_space_group_IT_number           7
_space_group_name_Hall           'P -2yc'
_space_group_name_H-M_alt        'P 1 c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2023-01-06
_audit_creation_method
;
Olex2 1.5
(compiled 2021.11.18 svn.ra9532c28 for OlexSys, GUI svn.r6429)
;
_audit_update_record
;
2023-05-01 deposited with the CCDC.	2023-10-04 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 92.133(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   45.6447(14)
_cell_length_b                   8.1335(3)
_cell_length_c                   9.3171(3)
_cell_measurement_reflns_used    12783
_cell_measurement_temperature    100
_cell_measurement_theta_max      28.8330
_cell_measurement_theta_min      2.5760
_cell_volume                     3456.6(2)
_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 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'XM  (Sheldrick, 2008)'
_diffrn_ambient_temperature      298
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.891
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \f     -9.39 350.61   1.00   10.00  97.37 -39.07  28.85    --   360
  2  \w    -99.76  20.24   1.00   10.00    --  -39.07  86.77  22.72  120
  3  \w    -99.76  20.24   1.00   10.00    --  -39.07  86.77-121.28  120
  4  \w   -113.84 110.16   1.00   10.00    --  -17.84 -59.25  20.08  224
  5  \w    -99.76  20.24   1.00   10.00    --  -39.07  86.77 103.72  120
  6  \w   -113.07  88.93   1.00   10.00    --  -39.07 -59.25-177.92  202
  7  \f     -9.39 350.61   1.00   10.00 118.60 -17.84  28.85    --   360
  8  \w   -113.07  88.93   1.00   10.00    --  -39.07 -59.25  74.08  202
  9  \w    -99.76  20.24   1.00   10.00    --  -39.07  86.77 -31.28  120
 10  \w   -114.07 103.93   1.00   10.00    --  -24.07 -59.25  20.08  218
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type
'Saxi-CrysAlisPro-abstract goniometer imported SAXI images'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0013041000
_diffrn_orient_matrix_UB_12      0.0866802000
_diffrn_orient_matrix_UB_13      0.0056646000
_diffrn_orient_matrix_UB_21      0.0006998000
_diffrn_orient_matrix_UB_22      -0.0065630000
_diffrn_orient_matrix_UB_23      0.0759632000
_diffrn_orient_matrix_UB_31      0.0154772000
_diffrn_orient_matrix_UB_32      -0.0070359000
_diffrn_orient_matrix_UB_33      -0.0011020000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0798
_diffrn_reflns_av_unetI/netI     0.0669
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.891
_diffrn_reflns_limit_h_max       63
_diffrn_reflns_limit_h_min       -57
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            60728
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.891
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.753
_diffrn_reflns_theta_min         2.187
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.524
_exptl_absorpt_correction_T_max  0.09959
_exptl_absorpt_correction_T_min  0.07179
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.93a (Rigaku Oxford Diffraction, 2020)
Spherical absorption correction
using equivalent radius and absorption coefficient.
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.104
_exptl_crystal_description       plate
_exptl_crystal_F_000             1260
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: CHCl3/EtOH'
_exptl_crystal_size_rad          0.400
_refine_diff_density_max         1.216
_refine_diff_density_min         -0.908
_refine_diff_density_rms         0.174
_refine_ls_abs_structure_details
;
 Twinning involves inversion, so Flack parameter cannot be determined
;
_refine_ls_extinction_coef       0.028(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.112
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     630
_refine_ls_number_reflns         17139
_refine_ls_number_restraints     110
_refine_ls_restrained_S_all      1.112
_refine_ls_R_factor_all          0.0846
_refine_ls_R_factor_gt           0.0809
_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/[\s^2^(Fo^2^)+(0.1530P)^2^+1.2753P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2176
_refine_ls_wR_factor_ref         0.2241
_reflns_Friedel_coverage         0.999
_reflns_Friedel_fraction_full    0.998
_reflns_Friedel_fraction_max     0.891
_reflns_number_gt                16107
_reflns_number_total             17139
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3ce00818e2.cif
_cod_data_source_block           mo_221128_wjl_3_autored
_cod_database_code               7247667
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C11 H10 N O'
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.38(8)
 0.13(4) 0.34(5) 0.15(4)
2. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3. Restrained distances
 H64A_$1-H16C
 2.2 with sigma of 0.02
 C13-C14 = C15-C16 = C29-C30 = C31-C32 = C61-C62 = C63-C64 = C45-C46 = C47-C48
 1.5 with sigma of 0.02
 C62-C63 = C46-C47 = C31-C30 = C15-C14
 1.5 with sigma of 0.02
4. Rigid bond restraints
 C13, C14, C15, C16, C29, C30, C31, C32, C45, C46, C47, C48, C61, C62, C63, C64
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C17, C36, C26, C25, C18, C37
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
5. Uiso/Uaniso restraints and constraints
Uanis(C30) \\sim Ueq, Uanis(C31) \\sim Ueq, Uanis(C32) \\sim Ueq, Uanis(C14)
\\sim Ueq, Uanis(C15) \\sim Ueq, Uanis(C16) \\sim Ueq, Uanis(C48) \\sim Ueq,
Uanis(C47) \\sim Ueq, Uanis(C46) \\sim Ueq, Uanis(C62) \\sim Ueq, Uanis(C63)
\\sim Ueq, Uanis(C64) \\sim Ueq: with sigma of 0.01 and sigma for terminal
atoms of 0.02
6.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C2(H2A,H2B), C3(H3A,H3B), C4(H4A,H4B), C5(H5A,H5B), C6(H6A,H6B),
 C7(H7A,H7B), C8(H8A,H8B), C9(H9A,H9B), C10(H10A,H10B), C11(H11A,H11B),
 C12(H12A,H12B), C13(H13A,H13B), C14(H14A,H14B), C15(H15A,H15B), C17(H17A,H17B),
  C18(H18A,H18B), C19(H19A,H19B), C20(H20A,H20B), C21(H21A,H21B), C22(H22A,
 H22B), C23(H23A,H23B), C24(H24A,H24B), C25(H25A,H25B), C26(H26A,H26B),
 C27(H27A,H27B), C28(H28A,H28B), C29(H29A,H29B), C30(H30A,H30B), C31(H31A,H31B),
  C33(H33A,H33B), C34(H34A,H34B), C35(H35A,H35B), C36(H36A,H36B), C37(H37A,
 H37B), C38(H38A,H38B), C39(H39A,H39B), C40(H40A,H40B), C41(H41A,H41B),
 C42(H42A,H42B), C43(H43A,H43B), C44(H44A,H44B), C45(H45A,H45B), C46(H46A,H46B),
  C47(H47A,H47B), C49(H49A,H49B), C50(H50A,H50B), C51(H51A,H51B), C52(H52A,
 H52B), C53(H53A,H53B), C54(H54A,H54B), C55(H55A,H55B), C56(H56A,H56B),
 C57(H57A,H57B), C58(H58A,H58B), C59(H59A,H59B), C60(H60A,H60B), C61(H61A,H61B),
  C62(H62A,H62B), C63(H63A,H63B)
6.b Idealised Me refined as rotating group:
 C16(H16A,H16B,H16C), C32(H32A,H32B,H32C), C48(H48A,H48B,H48C), C64(H64A,H64B,
 H64C)
;
_shelx_res_checksum              99776
_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 1.874
_oxdiff_exptl_absorpt_empirical_full_min 0.754