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_1572019
_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         'C20 H25 F10 N O P Sb'
_chemical_formula_sum            'C20 H25 F10 N O P Sb'
_chemical_formula_weight         638.13
_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             2022-10-27
_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                90
_cell_angle_beta                 106.7040(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.3875(2)
_cell_length_b                   11.51690(10)
_cell_length_c                   14.6407(2)
_cell_measurement_reflns_used    63902
_cell_measurement_temperature    100.01(13)
_cell_measurement_theta_max      34.0540
_cell_measurement_theta_min      2.2650
_cell_volume                     2485.09(5)
_computing_cell_refinement       'CrysAlisPro 1.171.42.72a (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.72a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.72a (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 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.01(13)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0951
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.972
_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    -42.00  -1.00   1.00   29.00    --  -30.87 -76.00-167.55   41
  2  \w   -100.00  -9.00   1.00   29.00    --  -30.87 -57.00 -90.00   91
  3  \w   -103.00  -5.00   1.00   29.00    --  -30.87 -38.00 -60.00   98
  4  \w   -100.00  -9.00   1.00   29.00    --  -30.87 -57.00  60.00   91
  5  \w   -107.00 -37.00   1.00   29.00    --  -30.87 178.00   0.00   70
  6  \w    -15.00  11.00   1.00   29.00    --  -30.87-101.00 118.95   26
  7  \w    -16.00  10.00   1.00   29.00    --  -30.87 -98.00-117.61   26
  8  \w    -18.00   9.00   1.00   29.00    --  -30.87 -97.00   0.25   27
  9  \w   -103.00  -5.00   1.00   29.00    --  -30.87 -38.00 120.00   98
 10  \w    -15.00  72.00   1.00   29.00    --   31.03 -99.00  30.00   87
 11  \w    -38.00  52.00   1.00   29.00    --   31.03 -57.00 -90.00   90
 12  \w    -15.00  72.00   1.00   29.00    --   31.03 -99.00-150.00   87
 13  \w    -42.00 104.00   1.00   29.00    --   31.03   0.00 -60.00  146
 14  \w    -41.00  57.00   1.00   29.00    --   31.03 -38.00 150.00   98
 15  \w    -15.00  11.00   1.00   29.00    --  -30.87-100.00  91.51   26
 16  \w   -100.00  -9.00   1.00   29.00    --  -30.87 -57.00  30.00   91
 17  \w   -103.00  -5.00   1.00   29.00    --  -30.87 -38.00-120.00   98
 18  \w   -107.00 -37.00   1.00   29.00    --  -30.87 178.00  30.00   70
 19  \w   -107.00 -37.00   1.00   29.00    --  -30.87 178.00-180.00   70
 20  \w    -12.00  14.00   1.00   29.00    --   31.03 104.00 -15.19   26
 21  \w    -41.00  57.00   1.00   29.00    --   31.03 -38.00 -30.00   98
 22  \w    -15.00  72.00   1.00   29.00    --   31.03 -99.00  60.00   87
 23  \w     11.00 100.00   1.00   29.00    --   31.03  57.00  90.00   89
 24  \w     -9.00  20.00   1.00   29.00    --   31.03  95.00 171.02   29
 25  \w    -12.00  14.00   1.00   29.00    --   31.03 103.00 -63.15   26
 26  \w    -15.00  72.00   1.00   29.00    --   31.03 -99.00 -60.00   87
 27  \w     -8.00  22.00   1.00   29.00    --   31.03  93.00  45.35   30
 28  \w    -42.00  68.00   1.00   29.00    --   31.03   0.00-150.00  110
 29  \w    -42.00 104.00   1.00   29.00    --   31.03   0.00-180.00  146
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Single source at offset/far, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0449333000
_diffrn_orient_matrix_UB_12      0.0211150000
_diffrn_orient_matrix_UB_13      0.0084270000
_diffrn_orient_matrix_UB_21      0.0033886000
_diffrn_orient_matrix_UB_22      0.0069825000
_diffrn_orient_matrix_UB_23      0.0490254000
_diffrn_orient_matrix_UB_31      0.0169374000
_diffrn_orient_matrix_UB_32      -0.0574261000
_diffrn_orient_matrix_UB_33      0.0090703000
_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  0.0667
_diffrn_reflns_av_unetI/netI     0.0253
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.972
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            147790
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.972
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         34.392
_diffrn_reflns_theta_min         2.244
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.262
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.742
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.72a (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    1.706
_exptl_crystal_description       plate
_exptl_crystal_F_000             1264
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.642
_refine_diff_density_min         -0.906
_refine_diff_density_rms         0.108
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.108
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     313
_refine_ls_number_reflns         10161
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.108
_refine_ls_R_factor_all          0.0337
_refine_ls_R_factor_gt           0.0287
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0352P)^2^+1.1370P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0709
_refine_ls_wR_factor_ref         0.0739
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9052
_reflns_number_total             10161
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4sc02785j2.cif
_cod_data_source_block           4
_cod_depositor_comments
'Adding full bibliography for 1572016--1572022.cif.'
_cod_database_code               1572019
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C20H25F10NOPSb
_shelx_estimated_absorpt_t_max   0.963
_shelx_estimated_absorpt_t_min   0.833
_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.a Secondary CH2 refined with riding coordinates:
 C5(H5A,H5B)
2.b Aromatic/amide H refined with riding coordinates:
 C16(H16), C17(H17), C18(H18), C19(H19), C20(H20)
2.c 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)
;
_shelx_res_checksum              83653
_shelx_hkl_checksum              64012
_olex2_date_sample_data_collection 2022-10-25
_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 1.576
_oxdiff_exptl_absorpt_empirical_full_min 0.682