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_7247665
_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         'C48 H100 S4 Sn'
_chemical_formula_sum            'C48 H100 S4 Sn'
_chemical_formula_weight         924.20
_chemical_melting_point          310
_chemical_name_systematic        'Tin(IV) dodecanethiolate'
_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             2023-03-13
_audit_creation_method
;
Olex2 1.5
(compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748)
;
_audit_update_record
;
2023-05-01 deposited with the CCDC.	2023-10-04 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 91.38(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   71.41(10)
_cell_length_b                   8.120(11)
_cell_length_c                   9.297(14)
_cell_measurement_reflns_used    5256
_cell_measurement_temperature    160.15
_cell_measurement_theta_max      26.4090
_cell_measurement_theta_min      2.4350
_cell_volume                     5389(13)
_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    'olex2.solve 1.5 (Bourhis et al., 2015)'
_diffrn_ambient_temperature      160.15
_diffrn_measured_fraction_theta_full 0.705
_diffrn_measured_fraction_theta_max 0.705
_diffrn_measurement_device_type  'XtaLAB Mini (ROW)'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0615
_diffrn_reflns_av_unetI/netI     0.0963
_diffrn_reflns_Laue_measured_fraction_full 0.705
_diffrn_reflns_Laue_measured_fraction_max 0.705
_diffrn_reflns_limit_h_max       82
_diffrn_reflns_limit_h_min       -84
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -4
_diffrn_reflns_number            8786
_diffrn_reflns_point_group_measured_fraction_full 0.705
_diffrn_reflns_point_group_measured_fraction_max 0.705
_diffrn_reflns_theta_full        66.576
_diffrn_reflns_theta_max         66.576
_diffrn_reflns_theta_min         1.856
_exptl_absorpt_coefficient_mu    5.408
_exptl_absorpt_correction_T_max  0.7531
_exptl_absorpt_correction_T_min  0.3484
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1170 before and 0.0703 after correction.
The Ratio of minimum to maximum transmission is 0.4626.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colorless
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.139
_exptl_crystal_description       plate
_exptl_crystal_F_000             2008
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: CHCl3/EtOH'
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.09
_refine_diff_density_max         2.178
_refine_diff_density_min         -5.342
_refine_diff_density_rms         0.324
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.156
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     482
_refine_ls_number_reflns         6720
_refine_ls_number_restraints     368
_refine_ls_restrained_S_all      1.126
_refine_ls_R_factor_all          0.2569
_refine_ls_R_factor_gt           0.2477
_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^)+(0.0002P)^2^+1200.1409P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.5687
_refine_ls_wR_factor_ref         0.5722
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5966
_reflns_number_total             6720
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3ce00818e2.cif
_cod_data_source_block           30220_gkw_w_2_0m1_a_pl
_cod_database_code               7247665
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.642
_shelx_estimated_absorpt_t_min   0.563
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C14-C13 = C14-C15 = C16-C15 = C16-C17 = C18-C17 = C18-C19 = C20-C19 = C20-C21
 = C21-C22 = C23-C22 = C24-C23 = C37-C38 = C38-C39 = C39-C40 = C41-C40 = C42-
 C41 = C42-C43 = C44-C43 = C44-C45 = C46-C45 = C47-C46 = C48-C47 = C36-C35 =
 C34-C35 = C34-C33 = C33-C32 = C31-C32 = C30-C31 = C29-C30 = C28-C29 = C27-C28 =
  C26-C27 = C25-C26 = C1-C2 = C2-C3 = C3-C4 = C4-C5 = C5-C6 = C6-C7 = C7-C8 =
 C8-C9 = C9-C10 = C11-C10 = C12-C11
 1.53 with sigma of 0.01
 Sn1-S2 \\sim Sn1-S1 \\sim Sn1-S3 \\sim Sn1-S4
 with sigma of 0.02
 S3-C36 \\sim S4-C37 \\sim S2-C13 \\sim S1-C12
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C48) \\sim Ueq, Uanis(C47) \\sim Ueq, Uanis(C46) \\sim Ueq, Uanis(C45)
\\sim Ueq, Uanis(C44) \\sim Ueq, Uanis(C43) \\sim Ueq, Uanis(C42) \\sim Ueq,
Uanis(C41) \\sim Ueq, Uanis(C40) \\sim Ueq, Uanis(C39) \\sim Ueq, Uanis(C38)
\\sim Ueq, Uanis(C37) \\sim Ueq, Uanis(C24) \\sim Ueq, Uanis(C23) \\sim Ueq,
Uanis(C22) \\sim Ueq, Uanis(C21) \\sim Ueq, Uanis(C20) \\sim Ueq, Uanis(C19)
\\sim Ueq, Uanis(C18) \\sim Ueq, Uanis(C17) \\sim Ueq, Uanis(C16) \\sim Ueq,
Uanis(C15) \\sim Ueq, Uanis(C14) \\sim Ueq, Uanis(C13) \\sim Ueq, Uanis(C36)
\\sim Ueq, Uanis(C35) \\sim Ueq, Uanis(C34) \\sim Ueq, Uanis(C33) \\sim Ueq,
Uanis(C32) \\sim Ueq, Uanis(C31) \\sim Ueq, Uanis(C30) \\sim Ueq, Uanis(C29)
\\sim Ueq, Uanis(C28) \\sim Ueq, Uanis(C27) \\sim Ueq, Uanis(C26) \\sim Ueq,
Uanis(C25) \\sim Ueq, Uanis(C1) \\sim Ueq, Uanis(C2) \\sim Ueq, Uanis(C3) \\sim
Ueq, Uanis(C4) \\sim Ueq, Uanis(C5) \\sim Ueq, Uanis(C6) \\sim Ueq, Uanis(C7)
\\sim Ueq, Uanis(C8) \\sim Ueq, Uanis(C9) \\sim Ueq, Uanis(C10) \\sim Ueq,
Uanis(C11) \\sim Ueq, Uanis(C12) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(S2) \\sim Ueq, Uanis(S4) \\sim Ueq, Uanis(S3) \\sim Ueq, Uanis(S1) \\sim
Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C36) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
4.a Secondary CH2 refined with riding coordinates:
 C10(H10A,H10B), C11(H11A,H11B), C35(H35A,H35B), C32(H32A,H32B), C31(H31A,
 H31B), C12(H12A,H12B), C33(H33A,H33B), C34(H34A,H34B), C9(H9A,H9B), C8(H8A,
 H8B), C40(H40A,H40B), C39(H39A,H39B), C30(H30A,H30B), C38(H38A,H38B), C17(H17A,
 H17B), C41(H41A,H41B), C7(H7A,H7B), C43(H43A,H43B), C37(H37A,H37B), C19(H19A,
 H19B), C18(H18A,H18B), C15(H15A,H15B), C45(H45A,H45B), C42(H42A,H42B), C6(H6A,
 H6B), C16(H16A,H16B), C5(H5A,H5B), C36(H36A,H36B), C29(H29A,H29B), C28(H28A,
 H28B), C44(H44A,H44B), C22(H22A,H22B), C21(H21A,H21B), C23(H23A,H23B),
 C13(H13A,H13B), C20(H20A,H20B), C27(H27A,H27B), C26(H26A,H26B), C4(H4A,H4B),
 C14(H14A,H14B), C3(H3A,H3B), C46(H46A,H46B), C47(H47A,H47B), C2(H2A,H2B)
4.b Idealised Me refined as rotating group:
 C24(H24A,H24B,H24C), C25(H25A,H25B,H25C), C1(H1A,H1B,H1C), C48(H48A,H48B,H48C)
;
_shelx_res_checksum              66261
_olex2_submission_special_instructions 'No special instructions were received'