A geminal antimony(iii)/phosphorus(iii) frustrated Lewis pair.
Krieft, Jonas; Trapp, Pia C.; Vishnevskiy, Yury V.; Neumann, Beate; Stammler, Hans-Georg; Lamm, Jan-Hendrik; Mitzel, Norbert W.; Chemical science 15 (2024) 12118–12125; doi:10.1039/d4sc02785j

data_1572021
_publ_section_title
;
 A geminal antimony(iii)/phosphorus(iii) frustrated Lewis pair.
;
_journal_issue                   30
_journal_name_full               'Chemical science'
_journal_page_first              12118
_journal_page_last               12125
_journal_paper_doi               10.1039/d4sc02785j
_journal_volume                  15
_journal_year                    2024
_chemical_formula_moiety         'C26 H40 Au F20 P2 Sb2, Cl'
_chemical_formula_sum            'C26 H40 Au Cl F20 P2 Sb2'
_chemical_formula_weight         1270.43
_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
_atom_sites_solution_primary     dual
_audit_creation_date             2022-11-29
_audit_creation_method
;
Olex2 1.5-ac5-024
(compiled 2022.04.12 svn.rca3783a0 for Rigaku Oxford Diffraction, GUI svn.r6498)
;
_audit_update_record
;
2024-04-23 deposited with the CCDC.	2024-07-01 downloaded from the CCDC.
;
_cell_angle_alpha                77.654(2)
_cell_angle_beta                 85.9190(10)
_cell_angle_gamma                80.909(2)
_cell_formula_units_Z            2
_cell_length_a                   8.8715(2)
_cell_length_b                   10.8958(2)
_cell_length_c                   21.7596(4)
_cell_measurement_reflns_used    62056
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      35.0240
_cell_measurement_theta_min      2.8060
_cell_volume                     2027.35(7)
_computing_cell_refinement       'CrysAlisPro 1.171.42.73a (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.73a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.73a (Rigaku OD, 2022)'
_computing_molecular_graphics    'Olex2 1.5-ac5-024 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-ac5-024 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.3114
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.954
_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     12.00  84.00   1.00   55.00    --   23.14-137.00-145.96   72
  2  \w     39.00 107.00   1.00   55.00    --   23.14 178.00 120.00   68
  3  \w      2.00  94.00   1.00   55.00    --   23.14  38.00  30.00   92
  4  \w    -48.00  44.00   1.00   55.00    --   23.14 -38.00  90.00   92
  5  \w     -2.00  92.00   1.00   55.00    --   23.14  57.00 150.00   94
  6  \w    -31.00  57.00   1.00   55.00    --   23.14 -87.00 -12.08   88
  7  \w      2.00  94.00   1.00   55.00    --   23.14  38.00 -90.00   92
  8  \w    -48.00  44.00   1.00   55.00    --   23.14 -38.00-150.00   92
  9  \w    -97.00 -43.00   1.00   55.00    --  -23.30 154.00 164.68   54
 10  \w    -42.00   7.00   1.00   55.00    --  -23.30 -77.00-120.00   49
 11  \w    -42.00   7.00   1.00   55.00    --  -23.30 -77.00   0.00   49
 12  \w    -97.00 -43.00   1.00   55.00    --  -23.30 154.00  -6.86   54
 13  \w     13.00  85.00   1.00   55.00    --   23.14-139.00 -27.00   72
 14  \w    -97.00 -43.00   1.00   55.00    --  -23.30 154.00 -84.68   54
 15  \w    -93.00 -39.00   1.00   55.00    --  -23.30 149.00 -52.48   54
 16  \w    -93.00 -39.00   1.00   55.00    --  -23.30 149.00  55.45   54
 17  \w    -42.00   7.00   1.00   55.00    --  -23.30 -77.00 150.00   49
 18  \w    -88.00 -36.00   1.00   55.00    --  -23.30 143.00 153.53   52
 19  \w    -92.00   2.00   1.00   55.00    --  -23.30 -57.00  90.00   94
 20  \w    -94.00  -3.00   1.00   55.00    --  -23.30 -38.00   0.00   91
 21  \w    -57.00  54.00   1.00   55.00    --  -23.30  19.00   0.00  111
 22  \w    -42.00   7.00   1.00   55.00    --  -23.30 -77.00 120.00   49
 23  \w    -15.00  61.00   1.00   55.00    --   23.14 -99.00-180.00   76
 24  \w    -62.00  45.00   1.00   55.00    --   23.14   0.00-120.00  107
 25  \w    -62.00 109.00   1.00   55.00    --   23.14   0.00-180.00  171
 26  \w    -62.00 109.00   1.00   55.00    --   23.14   0.00-150.00  171
 27  \w    -94.00  -3.00   1.00   55.00    --  -23.30 -38.00-150.00   91
 28  \w   -108.00 -58.00   1.00   55.00    --  -23.30 178.00  60.00   50
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0063359000
_diffrn_orient_matrix_UB_12      -0.0130045000
_diffrn_orient_matrix_UB_13      0.0333671000
_diffrn_orient_matrix_UB_21      0.0565708000
_diffrn_orient_matrix_UB_22      -0.0541864000
_diffrn_orient_matrix_UB_23      0.0010805000
_diffrn_orient_matrix_UB_31      0.0576679000
_diffrn_orient_matrix_UB_32      0.0378551000
_diffrn_orient_matrix_UB_33      0.0007873000
_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  0.0393
_diffrn_reflns_av_unetI/netI     0.0222
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.954
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            160871
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.954
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         35.310
_diffrn_reflns_theta_min         2.329
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    5.188
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.330
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.73a (Rigaku Oxford Diffraction, 2022)
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            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.081
_exptl_crystal_description       plate
_exptl_crystal_F_000             1208
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.03
_refine_diff_density_max         2.697
_refine_diff_density_min         -2.260
_refine_diff_density_rms         0.133
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.086
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     545
_refine_ls_number_reflns         17433
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.086
_refine_ls_R_factor_all          0.0357
_refine_ls_R_factor_gt           0.0303
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0155P)^2^+5.4687P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0595
_refine_ls_wR_factor_ref         0.0614
_reflns_Friedel_coverage         0.000
_reflns_number_gt                15922
_reflns_number_total             17433
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4sc02785j2.cif
_cod_data_source_block           6
_cod_depositor_comments
'Adding full bibliography for 1572016--1572022.cif.'
_cod_database_code               1572021
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C26H40AuClF20P2Sb2
_shelx_estimated_absorpt_t_max   0.860
_shelx_estimated_absorpt_t_min   0.382
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Others
 Sof(F11B)=Sof(F12B)=Sof(F13B)=Sof(F14B)=Sof(F15B)=Sof(C14B)=Sof(C15B)=1-FVAR(1)
 Sof(F11A)=Sof(F12A)=Sof(F13A)=Sof(F14A)=Sof(F15A)=Sof(C14A)=Sof(C15A)=FVAR(1)
3.a Secondary CH2 refined with riding coordinates:
 C5(H5A,H5B), C18(H18A,H18B)
3.b Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C), C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C11(H11A,H11B,H11C),
 C12(H12A,H12B,H12C), C13(H13A,H13B,H13C), C20(H20A,H20B,H20C), C21(H21A,H21B,
 H21C), C22(H22A,H22B,H22C), C24(H24A,H24B,H24C), C25(H25A,H25B,H25C), C26(H26A,
 H26B,H26C)
;
_shelx_res_checksum              10969
_shelx_hkl_checksum              24449
_olex2_date_sample_data_collection 2022-11-25
_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
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.233
_oxdiff_exptl_absorpt_empirical_full_min 0.850