Sulfonium cations as versatile strongly π-acidic ligands
Li, Ruiping; Barel, Nitsan; Subramaniyan, Vasudevan; Cohen, Orit; Tibika, Françoise; Tulchinsky, Yuri; Chemical Science  (2022) –; doi:10.1039/D2SC00588C

data_1566707
_publ_section_title
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 Sulfonium cations as versatile strongly \p-acidic ligands
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_journal_name_full               'Chemical Science'
_journal_paper_doi               10.1039/D2SC00588C
_journal_year                    2022
_chemical_formula_moiety         'C30 H33 P2 S, C24 H19 B, 0.5(C H2 Cl2)'
_chemical_formula_sum            'C54.5 H53 B Cl P2 S'
_chemical_formula_weight         848.23
_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
_audit_creation_date             2021-08-10
_audit_creation_method
;
Olex2 1.3-alpha
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_audit_update_record
;
2021-11-02 deposited with the CCDC.	2022-03-14 downloaded from the CCDC.
;
_cell_angle_alpha                81.957(4)
_cell_angle_beta                 80.897(4)
_cell_angle_gamma                69.046(5)
_cell_formula_units_Z            2
_cell_length_a                   8.8424(5)
_cell_length_b                   11.4067(6)
_cell_length_c                   24.8662(10)
_cell_measurement_reflns_used    8711
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.9080
_cell_measurement_theta_min      1.6930
_cell_volume                     2303.2(2)
_computing_cell_refinement       'CrysAlisPro 1.171.40.66a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.66a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.66a (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 1.3-alpha (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3-alpha (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2017/1 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w      2.24 182.19   0.30   29.99    --   28.00  73.79 -25.76  600
  2  \w      2.24 182.19   0.30   29.99    --   28.00  73.79  64.24  600
  3  \w      2.24 182.19   0.30   29.99    --   28.00  73.79 154.24  600
  4  \w      2.24 182.19   0.30   29.99    --   28.00  73.79-115.76  600
  5  \w      2.24  17.24   0.30   29.99    --   28.00  73.79 -25.76   50
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type
'Saxi-CrysAlisPro-abstract goniometer imported SAXI images'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0986
_diffrn_reflns_av_unetI/netI     0.0956
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            20848
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_min         1.666
_exptl_absorpt_coefficient_mu    0.234
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.38237
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.66a (Rigaku Oxford Diffraction, 2019)
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    1.223
_exptl_crystal_description       irregular
_exptl_crystal_F_000             896
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.726
_refine_diff_density_min         -0.484
_refine_diff_density_rms         0.114
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     467
_refine_ls_number_reflns         8109
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.062
_refine_ls_R_factor_all          0.1790
_refine_ls_R_factor_gt           0.1202
_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^)+(0.1432P)^2^+8.7072P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2962
_refine_ls_wR_factor_ref         0.3438
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4913
_reflns_number_total             8109
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2sc00588c2.cif
_cod_data_source_block           4a_BPh4
_cod_original_formula_sum        'C54.50 H53 B Cl P2 S'
_cod_database_code               1566707
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_max   0.968
_shelx_estimated_absorpt_t_min   0.961
_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. Others
 Fixed Sof: Cl2(0.5) Cl1(0.5) C55(0.5) H55A(0.5) H55B(0.5)
3.a Secondary CH2 refined with riding coordinates:
 C18(H18A,H18B), C17(H17A,H17B), C15(H15A,H15B), C14(H14A,H14B), C13(H13A,
 H13B), C55(H55A,H55B)
3.b Aromatic/amide H refined with riding coordinates:
 C36(H36), C24(H24), C23(H23), C22(H22), C21(H21), C20(H20), C2(H2), C3(H3),
 C4(H4), C5(H5), C6(H6), C50(H50), C51(H51), C52(H52), C53(H53), C54(H54),
 C48(H48), C47(H47), C46(H46), C45(H45), C44(H44), C38(H38), C39(H39), C40(H40),
  C41(H41), C42(H42), C30(H30), C29(H29), C28(H28), C27(H27), C26(H26),
 C32(H32), C8(H8), C9(H9), C10(H10), C11(H11), C12(H12), C33(H33), C34(H34)
3.c Fitted hexagon refined as free rotating group:
 C19(C24,C23,C22,C21,C20), C1(C2,C3,C4,C5,C6), C49(C50,C51,C52,C53,C54),
 C43(C48,C47,C46,C45,C44), C37(C38,C39,C40,C41,C42), C25(C30,C29,C28,C27,C26),
 C7(C8,C9,C10,C11,C12)
3.d Idealised Me refined as rotating group:
 C16(H16A,H16B,H16C)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              55549
_shelx_hkl_checksum              25686
_shelx_fab_checksum              72419
_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
;