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_1566714
_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         'C43 H35 F P2 Pt S, 2(C2 F6 N O4 S2)'
_chemical_formula_sum            'C47 H35 F13 N2 O8 P2 Pt S5'
_chemical_formula_weight         1420.10
_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             2021-09-01
_audit_creation_method
;
Olex2 1.5-alpha
(compiled 2021.08.20 svn.r13c46975 for OlexSys, GUI svn.r6392)
;
_audit_update_record
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2021-11-02 deposited with the CCDC.	2022-03-14 downloaded from the CCDC.
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_cell_angle_alpha                90
_cell_angle_beta                 98.2970(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   23.6369(3)
_cell_length_b                   12.7303(2)
_cell_length_c                   18.9449(2)
_cell_measurement_reflns_used    92765
_cell_measurement_temperature    150.15
_cell_measurement_theta_max      25.00
_cell_measurement_theta_min      1.934
_cell_volume                     5640.95(13)
_computing_molecular_graphics    'Olex2 1.5-alpha (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-alpha (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      150.15
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type
'xtalab synergy, single source at offset/far, hypix'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0500
_diffrn_reflns_av_unetI/netI     0.0274
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            92765
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        24.998
_diffrn_reflns_theta_max         24.998
_diffrn_reflns_theta_min         1.934
_exptl_absorpt_coefficient_mu    2.823
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.85
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.672
_exptl_crystal_description       prism
_exptl_crystal_F_000             2800
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.09
_refine_diff_density_max         1.168
_refine_diff_density_min         -0.684
_refine_diff_density_rms         0.095
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     793
_refine_ls_number_reflns         9935
_refine_ls_number_restraints     9
_refine_ls_restrained_S_all      1.044
_refine_ls_R_factor_all          0.0385
_refine_ls_R_factor_gt           0.0346
_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^)+(0.0481P)^2^+12.6663P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0897
_refine_ls_wR_factor_ref         0.0923
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9052
_reflns_number_total             9935
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2sc00588c2.cif
_cod_data_source_block           7b_NTf2_2
_cod_database_code               1566714
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.785
_shelx_estimated_absorpt_t_min   0.728
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 S4-O7A \\sim S4-O7
 with sigma of 0.02
 S5-O5A \\sim S5-O5
 with sigma of 0.02
 S5-O6A \\sim S5-O6
 with sigma of 0.02
 O6A-N03J \\sim O6-N03J
 with sigma of 0.02
 O5A-O6 \\sim O5-O6
 with sigma of 0.02
 F8-C47 \\sim F10A-C47
 with sigma of 0.02
 F9-C47 \\sim F9A-C47
 with sigma of 0.02
 F10-C47 \\sim F8A-C47
 with sigma of 0.02
 F11A-C46 \\sim F11-C46
 with sigma of 0.02
 F12A-C46 \\sim F13-C46
 with sigma of 0.02
 F13A-C46 \\sim F12-C46
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(F10A) = Uanis(F8) = Uanis(F8A)
4. Rigid body (RIGU) restrains
 F8, F8A, F10, F9A, F9, F10A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(F10A)=Sof(F8A)=Sof(F9A)=1-FVAR(1)
 Sof(F10)=Sof(F8)=Sof(F9)=FVAR(1)
 Sof(F13)=Sof(F11)=Sof(F12)=1-FVAR(2)
 Sof(F13A)=Sof(F11A)=Sof(F12A)=FVAR(2)
 Fixed Sof: O6A(0.5) O5A(0.5) N03J(0.5) O7A(0.5) N2(0.5) O8A(0.5) O8(0.5)
 O7(0.5) O6(0.5) O5(0.5)
6.a Aromatic/amide H refined with riding coordinates:
 C16(H16), C33(H33), C2(H2), C35(H35), C3(H3), C29(H29), C11(H11), C32(H32),
 C42(H42), C17(H17), C27(H27), C6(H6), C28(H28), C22(H22), C24(H24), C36(H36),
 C41(H41), C34(H34), C9(H9), C10(H10), C4(H4), C5(H5), C40(H40), C39(H39),
 C23(H23), C15(H15), C14(H14), C8(H8), C12(H12), C26(H26), C38(H38), C21(H21)
6.b Idealised Me refined as rotating group:
 C43(H43A,H43B,H43C)
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_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              10905
_shelx_hkl_checksum              1622
_shelx_fab_checksum              95053
_olex2_submission_special_instructions 'No special instructions were received'