Lewis base-free thiophosphonium ion: a cationic sulfur atom transfer reagent.
Löwe, Pawel; Witteler, Tim; Dielmann, Fabian; Chemical communications (Cambridge, England) 57 (2021) 5043–5046; doi:10.1039/d1cc01273h

data_7128183
_publ_section_title
;
 Lewis base-free thiophosphonium ion: a cationic sulfur atom transfer
 reagent.
;
_journal_issue                   41
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              5043
_journal_page_last               5046
_journal_paper_doi               10.1039/d1cc01273h
_journal_volume                  57
_journal_year                    2021
_chemical_formula_moiety         'C54 H72 N6 P S, C32 H12 B F24, 2(C H2 Cl2)'
_chemical_formula_sum            'C88 H88 B Cl4 F24 N6 P S'
_chemical_formula_weight         1901.28
_chemical_name_systematic        'Thiophosphonium salt'
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2018-05-14
_audit_creation_method
;
Olex2 1.2
(compiled 2018.04.26 svn.r3504 for OlexSys, GUI svn.r5492)
;
_audit_update_record
;
2021-01-20 deposited with the CCDC.	2021-04-16 downloaded from the CCDC.
;
_cell_angle_alpha                83.0761(13)
_cell_angle_beta                 77.4361(13)
_cell_angle_gamma                79.3360(12)
_cell_formula_units_Z            2
_cell_length_a                   12.5476(3)
_cell_length_b                   18.3022(4)
_cell_length_c                   20.6150(5)
_cell_measurement_reflns_used    9654
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29.595
_cell_measurement_theta_min      2.243
_cell_volume                     4525.10(19)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_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    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0254
_diffrn_reflns_av_unetI/netI     0.0264
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            77013
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.619
_diffrn_reflns_theta_min         1.459
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.269
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.8346
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1433 before and 0.0318 after correction. The Ratio of minimum to maximum transmission is 0.8346. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.395
_exptl_crystal_description       block
_exptl_crystal_F_000             1956
_exptl_crystal_size_max          0.59
_exptl_crystal_size_mid          0.58
_exptl_crystal_size_min          0.24
_refine_diff_density_max         1.542
_refine_diff_density_min         -1.127
_refine_diff_density_rms         0.063
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.005
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1142
_refine_ls_number_reflns         25293
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.005
_refine_ls_R_factor_all          0.0528
_refine_ls_R_factor_gt           0.0450
_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^)+(0.0621P)^2^+3.1515P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1178
_refine_ls_wR_factor_ref         0.1239
_reflns_Friedel_coverage         0.000
_reflns_number_gt                21668
_reflns_number_total             25293
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1cc01273h2.cif
_cod_data_source_block           compound4
_cod_depositor_comments
'Adding full bibliography for 7128183--7128185.cif.'
_cod_database_code               7128183
_shelxl_version_number           2013-4
_shelx_estimated_absorpt_t_max   0.938
_shelx_estimated_absorpt_t_min   0.858
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C10(H10), C13(H13), C22(H22), C25(H25), C37(H37), C40(H40), C49(H49), C52(H52)
2.b Secondary CH2 refined with riding coordinates:
 C87(H87A,H87B), C88(H88A,H88B)
2.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C6(H6), C7(H7), C8(H8), C18(H18), C19(H19), C20(H20),
 C29(H29), C30(H30), C33(H33), C34(H34), C35(H35), C45(H45), C46(H46), C47(H47),
  C56(H56), C58(H58), C60(H60), C64(H64), C66(H66), C68(H68), C72(H72),
 C74(H74), C76(H76), C80(H80), C82(H82), C84(H84)
2.d Idealised Me refined as rotating group:
 C11(H11A,H11B,H11C), C12(H12A,H12B,H12C), C14(H14A,H14B,H14C), C15(H15A,H15B,
 H15C), C23(H23A,H23B,H23C), C24(H24A,H24B,H24C), C26(H26A,H26B,H26C), C27(H27A,
 H27B,H27C), C38(H38A,H38B,H38C), C39(H39A,H39B,H39C), C41(H41A,H41B,H41C),
 C42(H42A,H42B,H42C), C50(H50A,H50B,H50C), C51(H51A,H51B,H51C), C53(H53A,H53B,
 H53C), C54(H54A,H54B,H54C)
;
_shelx_res_checksum              8850
_shelx_hkl_checksum              98172
_olex2_submission_special_instructions 'No special instructions were received'