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_1572016
_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         'C13 H20 F10 P Sb'
_chemical_formula_sum            'C13 H20 F10 P Sb'
_chemical_formula_weight         519.01
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     dual
_audit_creation_date             2021-05-25
_audit_creation_method
;
Olex2 1.3-ac4
(compiled 2019.04.23 svn.r3594 for Rigaku Oxford Diffraction, GUI svn.r5739)
;
_audit_update_record
;
2024-04-23 deposited with the CCDC.	2024-07-01 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   16.0957(2)
_cell_length_b                   11.68730(10)
_cell_length_c                   20.2429(2)
_cell_measurement_reflns_used    69051
_cell_measurement_temperature    100.0(1)
_cell_measurement_theta_max      36.4540
_cell_measurement_theta_min      2.4950
_cell_volume                     3808.00(7)
_computing_cell_refinement       'CrysAlisPro 1.171.41.105a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.105a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.105a (Rigaku OD, 2021)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.0(1)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0951
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.980
_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    -28.00  32.00   1.00   16.00    --   36.00 -38.00 -60.00   60
  2  \w      0.00  29.00   1.00   16.00    --   36.00  90.00 177.91   29
  3  \w     10.00  35.00   1.00   16.00    --   36.00  72.00 -94.22   25
  4  \w     14.00 104.00   1.00   16.00    --   36.00  38.00 120.00   90
  5  \w     27.00  94.00   1.00   16.00    --   36.00-133.00 153.00   67
  6  \w      7.00  42.00   1.00   16.00    --   36.00  77.00  27.65   35
  7  \w     15.00 103.00   1.00   16.00    --   36.00  38.00-120.00   88
  8  \w     14.00 104.00   1.00   16.00    --   36.00  38.00  30.00   90
  9  \w     42.00 104.00   1.00   16.00    --   36.00 178.00 -90.00   62
 10  \w     42.00 110.00   1.00   16.00    --   36.00 178.00 120.00   68
 11  \w     17.00  43.00   1.00   16.00    --   36.00  57.00 150.00   26
 12  \w     52.00  86.00   1.00   16.00    --   36.00  57.00 150.00   34
 13  \w    -29.00  27.00   1.00   16.00    --   36.00 -77.00-120.00   56
 14  \w      3.00  28.00   1.00   16.00    --   36.00  86.00 112.61   25
 15  \w     12.00  93.00   1.00   16.00    --   36.00-136.00 -24.00   81
 16  \w      8.00  42.00   1.00   16.00    --   36.00  76.00 -46.21   34
 17  \w      6.00  31.00   1.00   16.00    --   36.00  86.00 -79.59   25
 18  \w    -31.00  76.00   1.00   16.00    --   36.00   0.00  30.00  107
 19  \w     14.00 103.00   1.00   16.00    --   35.84  65.00  -5.20   89
 20  \w     17.00 104.00   1.00   16.00    --   35.84  57.00-120.00   87
 21  \w     -2.00 108.00   1.00   16.00    --   35.84  19.00-180.00  110
 22  \w     39.00 110.00   1.00   16.00    --   35.84 178.00-180.00   71
 23  \w      3.00  33.00   1.00   16.00    --   35.84  84.00 165.68   30
 24  \w    -15.00  76.00   1.00   16.00    --   35.84 -99.00-180.00   91
 25  \w     16.00  68.00   1.00   16.00    --   35.84  48.00  35.64   52
;
_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      0.0061075000
_diffrn_orient_matrix_UB_12      -0.0007610000
_diffrn_orient_matrix_UB_13      0.0346917000
_diffrn_orient_matrix_UB_21      -0.0431677000
_diffrn_orient_matrix_UB_22      0.0088715000
_diffrn_orient_matrix_UB_23      0.0048688000
_diffrn_orient_matrix_UB_31      -0.0064608000
_diffrn_orient_matrix_UB_32      -0.0600381000
_diffrn_orient_matrix_UB_33      0.0002839000
_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  0.0462
_diffrn_reflns_av_unetI/netI     0.0156
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.980
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            186026
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.980
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         36.905
_diffrn_reflns_theta_min         2.948
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.619
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.227
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.105a (Rigaku Oxford Diffraction, 2021)
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    1.811
_exptl_crystal_description       cylindrically
_exptl_crystal_F_000             2032
_exptl_crystal_size_max          0.62
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.24
_refine_diff_density_max         0.849
_refine_diff_density_min         -1.206
_refine_diff_density_rms         0.073
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     358
_refine_ls_number_reflns         9432
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.031
_refine_ls_R_factor_all          0.0337
_refine_ls_R_factor_gt           0.0272
_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^)+(0.0208P)^2^+2.8579P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0589
_refine_ls_wR_factor_ref         0.0616
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8176
_reflns_number_total             9432
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4sc02785j2.cif
_cod_data_source_block           1
_cod_depositor_comments
'Adding full bibliography for 1572016--1572022.cif.'
_cod_database_code               1572016
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C13H20F10PSb
_shelx_estimated_absorpt_t_max   0.697
_shelx_estimated_absorpt_t_min   0.433
_diffrn_oxdiff_digest_frames
;
016f5f24993ed5b04500cba3dd31fc55e5015328946
;
_diffrn_oxdiff_digest_hkl
;
01a70d54875a810817963b991fa443adcd578c
;
_reflns_odcompleteness_completeness 99.84
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Uiso/Uaniso restraints and constraints
Uanis(F8B) = Uanis(F8)
Uanis(F10) = Uanis(F10B)
2. Others
 Sof(F6B)=Sof(F7B)=Sof(F8B)=Sof(F9B)=Sof(F10B)=Sof(C4B)=Sof(C5B)=1-FVAR(1)
 Sof(F6)=Sof(F7)=Sof(F8)=Sof(F9)=Sof(F10)=Sof(C4)=Sof(C5)=FVAR(1)
;
_shelx_res_checksum              58298
_shelx_hkl_checksum              87188
_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 2.381
_oxdiff_exptl_absorpt_empirical_full_min 0.620