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_1572020
_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 P S Sb'
_chemical_formula_sum            'C20 H25 F10 N P S Sb'
_chemical_formula_weight         654.19
_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             2022-10-17
_audit_creation_method
;
Olex2 1.5-alpha
(compiled 2022.06.10 svn.r3fa896fb for OlexSys, GUI svn.r6535)
;
_audit_update_record
;
2024-04-23 deposited with the CCDC.	2024-07-01 downloaded from the CCDC.
;
_cell_angle_alpha                64.175(2)
_cell_angle_beta                 85.3920(10)
_cell_angle_gamma                85.3580(10)
_cell_formula_units_Z            4
_cell_length_a                   9.9191(2)
_cell_length_b                   16.6017(3)
_cell_length_c                   17.2503(3)
_cell_measurement_reflns_used    55579
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      32.4320
_cell_measurement_theta_min      2.8440
_cell_volume                     2545.37(9)
_computing_cell_refinement       'CrysAlisPro 1.171.42.70a (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.70a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.70a (Rigaku OD, 2022)'
_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  (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 0.941
_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     15.00  83.00   1.00   64.00    --   16.99-144.00 104.14   68
  2  \w    -54.00  38.00   1.00   64.00    --   16.99 -38.00 -60.00   92
  3  \w     21.00  91.00   1.00   64.00    --   16.99-154.00   6.81   70
  4  \w     -8.00  85.00   1.00   64.00    --   16.99  57.00  30.00   93
  5  \w     21.00  91.00   1.00   64.00    --   16.99-154.00 -63.73   70
  6  \w     -4.00  88.00   1.00   64.00    --   16.99  38.00 120.00   92
  7  \w     -8.00  85.00   1.00   64.00    --   16.99  57.00 -90.00   93
  8  \w    -51.00  42.00   1.00   64.00    --   16.99 -57.00 120.00   93
  9  \w    -42.00  13.00   1.00   64.00    --  -17.14 -77.00  90.00   55
 10  \w    -88.00   4.00   1.00   64.00    --  -17.14 -38.00 120.00   92
 11  \w     20.00  89.00   1.00   64.00    --   16.99-152.00  51.34   69
 12  \w     -4.00  88.00   1.00   64.00    --   16.99  38.00 -60.00   92
 13  \w    -91.00 -43.00   1.00   64.00    --  -17.14 154.00  -1.06   48
 14  \w    -91.00 -43.00   1.00   64.00    --  -17.14 154.00-178.98   48
 15  \w    -92.00 -44.00   1.00   64.00    --  -17.14 156.00  95.75   48
 16  \w    -42.00  13.00   1.00   64.00    --  -17.14 -77.00  30.00   55
 17  \w    -59.00 -14.00   1.00   64.00    --  -17.14 109.00-124.89   45
 18  \w    -91.00 -43.00   1.00   64.00    --  -17.14 154.00  52.99   48
 19  \w    -42.00  47.00   1.00   64.00    --   16.99 -77.00-150.00   89
 20  \w    -15.00  10.00   1.00   64.00    --   16.99 -99.00   0.00   25
 21  \w    -15.00  55.00   1.00   64.00    --   16.99 -99.00  90.00   70
 22  \w     39.00 101.00   1.00   64.00    --   16.99 178.00 -90.00   62
 23  \w     -8.00  85.00   1.00   64.00    --   16.99  57.00 -60.00   93
 24  \w    -47.00  21.00   1.00   64.00    --  -17.14  77.00-180.00   68
 25  \w    -91.00 -43.00   1.00   64.00    --  -17.14 154.00 -55.33   48
;
_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      -0.0528748000
_diffrn_orient_matrix_UB_12      0.0276334000
_diffrn_orient_matrix_UB_13      0.0073957000
_diffrn_orient_matrix_UB_21      -0.0433676000
_diffrn_orient_matrix_UB_22      -0.0363496000
_diffrn_orient_matrix_UB_23      0.0161625000
_diffrn_orient_matrix_UB_31      0.0219929000
_diffrn_orient_matrix_UB_32      -0.0131882000
_diffrn_orient_matrix_UB_33      0.0421430000
_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  0.0545
_diffrn_reflns_av_unetI/netI     0.0340
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.941
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            142479
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.941
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         32.888
_diffrn_reflns_theta_min         2.531
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.311
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.789
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.70a (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    1.707
_exptl_crystal_description       irregular
_exptl_crystal_F_000             1296
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.987
_refine_diff_density_min         -0.509
_refine_diff_density_rms         0.089
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     656
_refine_ls_number_reflns         17900
_refine_ls_number_restraints     60
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.0454
_refine_ls_R_factor_gt           0.0300
_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^)+(0.0263P)^2^+1.4110P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0622
_refine_ls_wR_factor_ref         0.0680
_reflns_Friedel_coverage         0.000
_reflns_number_gt                14475
_reflns_number_total             17900
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4sc02785j2.cif
_cod_data_source_block           5a
_cod_depositor_comments
'Adding full bibliography for 1572016--1572022.cif.'
_cod_database_code               1572020
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C20H25F10NPSSb
_shelx_estimated_absorpt_t_max   0.962
_shelx_estimated_absorpt_t_min   0.848
_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. Uiso/Uaniso restraints and constraints
F16 \\sim F17 \\sim F18A \\sim F19A \\sim F20A \\sim C14A \\sim C23: within 2A
with sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A
F16 \\sim F17 \\sim F18B \\sim F19B \\sim F20B \\sim C14B \\sim C23: within 2A
with sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A
Uanis(C14A) = Uanis(C14B)
3. Others
 Sof(F18B)=Sof(F19B)=Sof(F20B)=Sof(C14B)=1-FVAR(1)
 Sof(F18A)=Sof(F19A)=Sof(F20A)=Sof(C14A)=FVAR(1)
4.a Secondary CH2 refined with riding coordinates:
 C5(H5A,H5B), C25(H25A,H25B)
4.b Aromatic/amide H refined with riding coordinates:
 C16(H16), C17(H17), C18(H18), C19(H19), C20(H20), C36(H36), C37(H37),
 C38(H38), C39(H39), C40(H40)
4.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), C27(H27A,H27B,H27C), C28(H28A,H28B,
 H28C), C29(H29A,H29B,H29C), C31(H31A,H31B,H31C), C32(H32A,H32B,H32C), C33(H33A,
 H33B,H33C)
;
_shelx_res_checksum              95572
_shelx_hkl_checksum              38155
_olex2_date_sample_data_collection 2022-10-14
_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 0.838