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_7128184
_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         'Cl, C54 H71 Cl2 N6 P, 2(C6 H5 F)'
_chemical_formula_sum            'C66 H81 Cl3 F2 N6 P'
_chemical_formula_weight         1133.68
_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   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2021-01-29
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6226)
;
_audit_update_record
;
2021-02-02 deposited with the CCDC.	2021-04-16 downloaded from the CCDC.
;
_cell_angle_alpha                70.944(2)
_cell_angle_beta                 82.683(2)
_cell_angle_gamma                75.308(2)
_cell_formula_units_Z            2
_cell_length_a                   12.4753(4)
_cell_length_b                   15.7403(5)
_cell_length_c                   17.5125(6)
_cell_measurement_reflns_used    9887
_cell_measurement_temperature    100
_cell_measurement_theta_max      29.77
_cell_measurement_theta_min      2.43
_cell_volume                     3140.38(18)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2013/4 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.983
_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  0.0552
_diffrn_reflns_av_unetI/netI     0.0595
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.983
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            53673
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.983
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.825
_diffrn_reflns_theta_min         1.690
_diffrn_source_current           0.59
_diffrn_source_power             0.0295
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.221
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.7156
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1175 before and 0.0595 after correction.
The Ratio of minimum to maximum transmission is 0.7156.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.199
_exptl_crystal_description       needle
_exptl_crystal_F_000             1206
_exptl_crystal_recrystallization_method
'crystallized out of a concentrated THF/fluorobenzene solution at room temperature'
_exptl_crystal_size_max          0.377
_exptl_crystal_size_mid          0.303
_exptl_crystal_size_min          0.302
_refine_diff_density_max         1.313
_refine_diff_density_min         -0.558
_refine_diff_density_rms         0.078
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     734
_refine_ls_number_reflns         17721
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.0743
_refine_ls_R_factor_gt           0.0565
_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^)+(0.0713P)^2^+2.3868P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1485
_refine_ls_wR_factor_ref         0.1615
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13451
_reflns_number_total             17721
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1cc01273h2.cif
_cod_data_source_block           p-1_a
_cod_depositor_comments
'Adding full bibliography for 7128183--7128185.cif.'
_cod_database_code               7128184
_shelxl_version_number           2013-4
_shelx_estimated_absorpt_t_max   0.936
_shelx_estimated_absorpt_t_min   0.921
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H) groups, All C(H,H,H) groups
2. Others
 Sof(H61)=Sof(F2B)=1-FVAR(1)
 Sof(H62)=Sof(F2A)=FVAR(1)
3.a Ternary CH refined with riding coordinates:
 C40(H40), C13(H13), C25(H25), C52(H52), C37(H37), C49(H49), C22(H22), C10(H10)
3.b Aromatic/amide H refined with riding coordinates:
 C29(H29), C35(H35), C30(H30), C3(H3), C34(H34), C2(H2), C33(H33), C8(H8),
 C7(H7), C6(H6), C47(H47), C20(H20), C45(H45), C18(H18), C46(H46), C19(H19),
 C59(H59), C60(H60), C62(H62), C66(H66), C61(H61), C63(H63), C56(H56), C65(H65),
  C57(H57), C64(H64), C58(H58)
3.c Idealised Me refined as rotating group:
 C42(H42A,H42B,H42C), C14(H14A,H14B,H14C), C41(H41A,H41B,H41C), C26(H26A,H26B,
 H26C), C23(H23A,H23B,H23C), C15(H15A,H15B,H15C), C54(H54A,H54B,H54C), C38(H38A,
 H38B,H38C), C39(H39A,H39B,H39C), C27(H27A,H27B,H27C), C24(H24A,H24B,H24C),
 C11(H11A,H11B,H11C), C12(H12A,H12B,H12C), C51(H51A,H51B,H51C), C50(H50A,H50B,
 H50C)
;
_shelx_res_checksum              51384
_shelx_hkl_checksum              75185
_olex2_date_sample_data_collection 2020-12-30
_olex2_date_sample_submission    2020-10-01
_olex2_exptl_crystal_mounting_method 'mounted on a glass capillary'
_olex2_submission_original_sample_id PL067
_olex2_submission_special_instructions 'No special instructions were received'