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_1566708
_publ_section_title
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 Sulfonium cations as versatile strongly \p-acidic ligands
;
_journal_name_full               'Chemical Science'
_journal_paper_doi               10.1039/D2SC00588C
_journal_year                    2022
_chemical_formula_moiety
'C29 H31 P2 Pt S, 0.125(C2 H4 Cl4), 2(B0.5 F2)'
_chemical_formula_sum            'C29.25 H31.5 B Cl0.5 F4 P2 Pt S'
_chemical_formula_weight         776.67
_space_group_crystal_system      orthorhombic
_space_group_IT_number           55
_space_group_name_Hall           '-P 2 2ab'
_space_group_name_H-M_alt        'P b a m'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2020-07-20
_audit_creation_method
;
Olex2 1.3
(compiled 2019.09.11 svn.r3662 for OlexSys, GUI svn.r5938)
;
_audit_update_record
;
2021-11-02 deposited with the CCDC.	2022-03-14 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   20.9374(6)
_cell_length_b                   10.9959(3)
_cell_length_c                   14.9555(5)
_cell_measurement_reflns_used    6956
_cell_measurement_temperature    297.05(16)
_cell_measurement_theta_max      28.1890
_cell_measurement_theta_min      2.3690
_cell_volume                     3443.14(18)
_computing_cell_refinement       'CrysAlisPro 1.171.40.81a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.81a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.81a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      297.05(16)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.970
_diffrn_measured_fraction_theta_max 0.752
_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    -22.00  26.00   0.50   25.00    --    9.19 -62.00 103.00   96
  2  \w    -18.00  23.00   0.50   25.00    --  -10.29 -99.00 120.00   82
  3  \w    -24.00  21.00   0.50   25.00    --  -10.29 -99.00  90.00   90
  4  \w    -63.00 -47.50   0.50   25.00    --    9.19 -62.00 103.00   31
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type
'XtaLAB Synergy, Single source at offset/far, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0233471000
_diffrn_orient_matrix_UB_12      -0.0465201000
_diffrn_orient_matrix_UB_13      0.0035778000
_diffrn_orient_matrix_UB_21      -0.0004151000
_diffrn_orient_matrix_UB_22      0.0059718000
_diffrn_orient_matrix_UB_23      0.0472049000
_diffrn_orient_matrix_UB_31      -0.0245448000
_diffrn_orient_matrix_UB_32      -0.0443125000
_diffrn_orient_matrix_UB_33      0.0026262000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0391
_diffrn_reflns_av_unetI/netI     0.0368
_diffrn_reflns_Laue_measured_fraction_full 0.970
_diffrn_reflns_Laue_measured_fraction_max 0.752
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            17185
_diffrn_reflns_point_group_measured_fraction_full 0.970
_diffrn_reflns_point_group_measured_fraction_max 0.752
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         32.107
_diffrn_reflns_theta_min         2.496
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    4.305
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.609
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.81a (Rigaku Oxford Diffraction, 2020)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.498
_exptl_crystal_description       irregular
_exptl_crystal_F_000             1522
_exptl_crystal_size_max          0.194
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.093
_refine_diff_density_max         1.523
_refine_diff_density_min         -0.965
_refine_diff_density_rms         0.130
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.083
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     225
_refine_ls_number_reflns         4698
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.084
_refine_ls_R_factor_all          0.0652
_refine_ls_R_factor_gt           0.0454
_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^)+(0.0527P)^2^+4.7301P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1063
_refine_ls_wR_factor_ref         0.1137
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3577
_reflns_number_total             4698
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2sc00588c2.cif
_cod_data_source_block           9_BF4
_cod_original_formula_sum        'C29.25 H31.50 B Cl0.50 F4 P2 Pt S'
_cod_database_code               1566708
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C30 H28 P2 S Pt B F4'
_shelx_estimated_absorpt_t_max   0.690
_shelx_estimated_absorpt_t_min   0.489
_reflns_odcompleteness_completeness 92.27
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     28.22
_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. Restrained distances
 C1C-Cl1
 1.7 with sigma of 0.02
 C1C-Cl2
 1.7 with sigma of 0.02
3. Others
 Fixed Sof: H1A(0.5) H1B(0.5) H1C(0.5) Cl1(0.125) Cl2(0.125) C1C(0.125)
 H1CA(0.125) H1CB(0.125) F1(0.25) F2(0.5) F3(0.25) B1(0.25) F4(0.5) F5(0.25)
 F6(0.25)
4.a Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C3(H3A,H3B), C1C(H1CA,H1CB)
4.b Aromatic/amide H refined with riding coordinates:
 C5(H5), C6(H6), C7(H7), C8(H8), C9(H9), C11(H11), C12(H12), C13(H13),
 C14(H14), C15(H15)
4.c Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C)
;
_shelx_res_checksum              53189
_shelx_hkl_checksum              1690
_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
;
_oxdiff_exptl_absorpt_empirical_full_max 1.094
_oxdiff_exptl_absorpt_empirical_full_min 0.896