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_1566713
_publ_section_title
;
 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         'C32 H39 P2 Pt S, C24 H20 B'
_chemical_formula_sum            'C56 H59 B P2 Pt S'
_chemical_formula_weight         1031.93
_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             2020-01-22
_audit_creation_method
;
Olex2 1.3-alpha
(compiled Nov 21 2019 18:26:39 for OlexSys, GUI svn.r6003)
;
_audit_update_record
;
2021-11-02 deposited with the CCDC.	2022-03-14 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 102.4960(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.6775(2)
_cell_length_b                   15.3273(2)
_cell_length_c                   19.3126(3)
_cell_measurement_reflns_used    44361
_cell_measurement_temperature    293.2(4)
_cell_measurement_theta_max      32.1620
_cell_measurement_theta_min      1.9730
_cell_volume                     4819.76(12)
_computing_cell_refinement       'CrysAlisPro 1.171.40.68a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.68a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.68a (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 2014/4 (Sheldrick, 2014)'
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      293.2(4)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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     -7.00  29.00   0.50    3.50    --   11.54 -57.00   0.00   72
  2  \w     21.00  46.00   0.50    3.50    --   11.54 -99.00 -60.00   50
  3  \w     18.00  43.00   0.50    3.50    --   11.54-132.00   7.00   50
  4  \w     39.00  79.00   0.50    3.50    --   11.54-178.00 -30.00   80
  5  \w     21.00  46.00   0.50    3.50    --   11.54-137.00-170.00   50
  6  \w    -23.00  16.00   0.50    3.50    --   11.54 -99.00 -60.00   78
  7  \w    -23.00   2.00   0.50    3.50    --  -12.64 -99.00   0.00   50
  8  \w    -55.00 -14.00   0.50    3.50    --   11.54 -57.00   0.00   82
  9  \w    -19.00  21.00   0.50    3.50    --  -12.64 -99.00 -90.00   80
 10  \w    -84.00  -2.00   0.50    3.50    --  -12.64 -57.00  60.00  164
 11  \w    -21.00  24.00   0.50    3.50    --  -12.64 -99.00 120.00   90
 12  \w    -87.00 -45.00   0.50    3.50    --  -12.64-178.00  90.00   84
 13  \w    -88.00 -63.00   0.50    3.50    --  -12.64-178.00 -90.00   50
 14  \w    -86.00 -41.00   0.50    3.50    --  -12.64-178.00-120.00   90
 15  \w    -14.00  83.00   0.50    3.50    --   11.54  77.00-180.00  194
 16  \w     42.00  87.00   0.50    3.50    --   11.54 178.00   0.00   90
 17  \w    -67.00 -42.00   0.50    3.50    --  -12.64 132.00  76.00   50
 18  \w    -69.00 -44.00   0.50    3.50    --  -12.64 137.00-106.00   50
;
_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      -0.0226482000
_diffrn_orient_matrix_UB_12      0.0345880000
_diffrn_orient_matrix_UB_13      0.0109537000
_diffrn_orient_matrix_UB_21      0.0249406000
_diffrn_orient_matrix_UB_22      0.0307414000
_diffrn_orient_matrix_UB_23      -0.0129820000
_diffrn_orient_matrix_UB_31      -0.0276102000
_diffrn_orient_matrix_UB_32      -0.0005988000
_diffrn_orient_matrix_UB_33      -0.0335701000
_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  0.0328
_diffrn_reflns_av_unetI/netI     0.0178
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            83399
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_min         1.825
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    3.057
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.615
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.68a (Rigaku Oxford Diffraction, 2019)
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            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.422
_exptl_crystal_description       irregular
_exptl_crystal_F_000             2096
_exptl_crystal_size_max          0.354
_exptl_crystal_size_mid          0.149
_exptl_crystal_size_min          0.149
_refine_diff_density_max         0.650
_refine_diff_density_min         -0.387
_refine_diff_density_rms         0.050
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     552
_refine_ls_number_reflns         8484
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.0216
_refine_ls_R_factor_gt           0.0177
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0166P)^2^+2.6772P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0401
_refine_ls_wR_factor_ref         0.0412
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7645
_reflns_number_total             8484
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2sc00588c2.cif
_cod_data_source_block           6a_BPh4
_cod_database_code               1566713
_shelx_shelxl_version_number     2017/1
_chemical_oxdiff_formula         'C56 H59 P2 S Pt B'
_reflns_odcompleteness_completeness 99.94
_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, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C15-C16A \\sim C15-C16
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C16) = Uanis(C16A)
Uanis(C16) = Uanis(C16A) = Uanis(C15)
4. Others
 Sof(H15C)=Sof(H15D)=Sof(C16)=Sof(H16D)=Sof(H16E)=Sof(H16F)=1-FVAR(1)
 Sof(H15A)=Sof(H15B)=Sof(C16A)=Sof(H16A)=Sof(H16B)=Sof(H16C)=FVAR(1)
5.a Secondary CH2 refined with riding coordinates:
 C18(H18A,H18B), C13(H13A,H13B), C14(H14A,H14B), C17(H17A,H17B), C15(H15C,
 H15D), C15(H15A,H15B)
5.b Aromatic/amide H refined with riding coordinates:
 C30(H30), C6(H6), C12(H12), C20(H20), C44(H44), C24(H24), C50(H50), C46(H46),
 C48(H48), C40(H40), C34(H34), C2(H2), C26(H26), C29(H29), C10(H10), C52(H52),
 C49(H49), C28(H28), C47(H47), C11(H11), C27(H27), C5(H5), C9(H9), C56(H56),
 C41(H41), C55(H55), C42(H42), C8(H8), C36(H36), C53(H53), C43(H43), C23(H23),
 C35(H35), C37(H37), C3(H3), C54(H54), C4(H4), C21(H21), C22(H22), C38(H38)
5.c Idealised Me refined as rotating group:
 C32(H32A,H32B,H32C), C31(H31A,H31B,H31C), C16A(H16A,H16B,H16C), C16(H16D,H16E,
 H16F)
;
_shelx_res_checksum              75516
_shelx_hkl_checksum              555
_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 1.284
_oxdiff_exptl_absorpt_empirical_full_min 0.840