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_7247666
_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         'C56 H116 S4 Sn'
_chemical_formula_sum            'C56 H116 S4 Sn'
_chemical_formula_weight         1036.41
_chemical_melting_point          321
_chemical_name_systematic        'Tin(IV) tetradecanethiolate'
_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     dual
_audit_creation_date             2022-12-28
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2023-05-01 deposited with the CCDC.	2023-10-04 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 91.1170(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   81.184(4)
_cell_length_b                   7.8878(4)
_cell_length_c                   9.2530(5)
_cell_measurement_reflns_used    9907
_cell_measurement_temperature    150.00
_cell_measurement_theta_max      74.63
_cell_measurement_theta_min      4.36
_cell_volume                     5924.2(5)
_computing_cell_refinement       'SAINT V8.40A (Bruker, 2019)'
_computing_data_reduction        'SAINT V8.40A (Bruker, 2019)'
_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    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      150.00
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0320
_diffrn_reflns_av_unetI/netI     0.0338
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       101
_diffrn_reflns_limit_h_min       -99
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            46808
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         74.675
_diffrn_reflns_theta_min         1.633
_diffrn_source_current           1.0
_diffrn_source_power             0.05
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.969
_exptl_absorpt_correction_T_max  0.0872
_exptl_absorpt_correction_T_min  0.0088
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1173 before and 0.0550 after correction.
The Ratio of minimum to maximum transmission is 0.1009.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.162
_exptl_crystal_description       plate
_exptl_crystal_F_000             2264
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: CHCl3/EtOH'
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.466
_refine_diff_density_min         -0.852
_refine_diff_density_rms         0.162
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.186
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     554
_refine_ls_number_reflns         12081
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.186
_refine_ls_R_factor_all          0.0639
_refine_ls_R_factor_gt           0.0620
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0907P)^2^+4.1002P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1648
_refine_ls_wR_factor_ref         0.1673
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11454
_reflns_number_total             12081
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3ce00818e2.cif
_cod_data_source_block           cu_1228_9_0ma
_cod_database_code               7247666
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.636
_shelx_estimated_absorpt_t_min   0.436
_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.a Secondary CH2 refined with riding coordinates:
 C006(H00A,H00B), C007(H00C,H00D), C008(H00E,H00F), C009(H00G,H00H), C00A(H00I,
 H00J), C00B(H00K,H00L), C00C(H00M,H00N), C00D(H00O,H00P), C00E(H00Q,H00R),
 C00F(H00S,H00T), C00G(H00U,H00V), C00H(H00W,H00X), C00I(H00Y,H), C00J(H00Z,HA),
  C00K(H00,HB), C00L(H1,HC), C00M(H2,HD), C00N(H3,HE), C00O(H4,HF), C00P(H5,HG),
  C00Q(H6,HH), C00R(H7,HI), C00S(H8,HJ), C00T(H9,HK), C00U(H10,HL), C00V(H11,
 HM), C00W(H12,HN), C00X(H13,HO), C00Y(H14,HP), C00Z(H15,HQ), C010(H01A,H01B),
 C011(H01C,H01D), C012(H01E,H01F), C013(H01G,H01H), C014(H01I,H01J), C015(H01K,
 H01L), C016(H01M,H01N), C017(H01O,H01P), C018(H01Q,H01R), C019(H01S,H01T),
 C01A(H01U,H01V), C01B(H01W,H01X), C01C(H01Y,HR), C01D(H01Z,HS), C01E(H01,HT),
 C01F(H16,HU), C01G(H17,HV), C01H(H18,HW), C01I(H19,HX), C01J(H20,HY), C01K(H21,
 HZ), C01L(H22,H27)
2.b Idealised Me refined as rotating group:
 C01M(H23,H28,H29), C01N(H24,H30,H31), C01O(H25,H32,H33), C01P(H26,H34,H35)
;
_shelx_res_checksum              28149
_olex2_submission_special_instructions 'No special instructions were received'