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_1572018
_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 O2 P S Sb'
_chemical_formula_sum            'C13 H20 F10 O2 P S Sb'
_chemical_formula_weight         583.07
_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   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2021-08-25
_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                   17.0497(5)
_cell_length_b                   11.9276(3)
_cell_length_c                   20.3495(6)
_cell_measurement_reflns_used    22394
_cell_measurement_temperature    100.00(11)
_cell_measurement_theta_max      31.7580
_cell_measurement_theta_min      1.9860
_cell_volume                     4138.3(2)
_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      100.00(11)
_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 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    -46.00  52.00   1.00   38.50    --   26.03 -38.00  30.00   98
  2  \w     17.00  96.00   1.00   38.50    --   26.03-145.00-132.00   79
  3  \w    -13.00  68.00   1.00   38.50    --   26.03 -99.00   0.00   81
  4  \w      6.00  95.00   1.00   38.50    --   26.03  57.00 -60.00   89
  5  \w    -12.00  96.00   1.00   38.50    --   26.03  19.00-180.00  108
  6  \w     33.00  90.00   1.00   38.50    --   26.03  57.00-150.00   57
  7  \w     -4.00  42.00   1.00   38.50    --   26.03  77.00  90.00   46
  8  \w      6.00  85.00   1.00   38.50    --   26.03  57.00  30.00   79
  9  \w    -42.00  55.00   1.00   38.50    --   26.03 -77.00-120.00   97
 10  \w     -4.00  42.00   1.00   38.50    --   26.03  77.00-180.00   46
 11  \w    -47.00  17.00   1.00   38.50    --   26.03 -19.00 120.00   64
;
_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      0.0377671000
_diffrn_orient_matrix_UB_12      -0.0181888000
_diffrn_orient_matrix_UB_13      0.0099725000
_diffrn_orient_matrix_UB_21      -0.0123084000
_diffrn_orient_matrix_UB_22      0.0010451000
_diffrn_orient_matrix_UB_23      0.0332849000
_diffrn_orient_matrix_UB_31      -0.0123650000
_diffrn_orient_matrix_UB_32      -0.0566281000
_diffrn_orient_matrix_UB_33      -0.0025808000
_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  0.0476
_diffrn_reflns_av_unetI/netI     0.0209
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            77118
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.080
_diffrn_reflns_theta_min         2.002
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.605
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.551
_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    1.872
_exptl_crystal_description       needle
_exptl_crystal_F_000             2288
_exptl_crystal_size_max          0.29
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.258
_refine_diff_density_min         -0.597
_refine_diff_density_rms         0.086
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.076
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     305
_refine_ls_number_reflns         6082
_refine_ls_number_restraints     99
_refine_ls_restrained_S_all      1.085
_refine_ls_R_factor_all          0.0453
_refine_ls_R_factor_gt           0.0320
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0290P)^2^+5.3181P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0699
_refine_ls_wR_factor_ref         0.0751
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4917
_reflns_number_total             6082
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4sc02785j2.cif
_cod_data_source_block           3
_cod_depositor_comments
'Adding full bibliography for 1572016--1572022.cif.'
_cod_database_code               1572018
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C13H20F10O2PSSb
_shelx_estimated_absorpt_t_max   0.939
_shelx_estimated_absorpt_t_min   0.653
_diffrn_oxdiff_digest_frames
;
01747171b75cc2a57308bc6dd197df4d9300850df07
;
_diffrn_oxdiff_digest_hkl
;
015f85afb02ae973ff31560410a95185c7164b
;
_reflns_odcompleteness_completeness 99.97
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     30.01
_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. Rigid body (RIGU) restrains
 Sb1, F1A, F2, F3A, F4A, F5A, C1, C2A, F1B, F3B, F4B, F5B, C2B
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
3. Others
 Sof(F1A)=Sof(F3A)=Sof(F4A)=Sof(F5A)=Sof(C2A)=1-FVAR(1)
 Sof(F1B)=Sof(F3B)=Sof(F4B)=Sof(F5B)=Sof(C2B)=FVAR(1)
4.a Secondary CH2 refined with riding coordinates:
 C5(H5A,H5B)
4.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)
;
_shelx_res_checksum              94115
_shelx_hkl_checksum              87396
_olex2_date_sample_data_collection 2021-08-23
_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 1.267
_oxdiff_exptl_absorpt_empirical_full_min 0.805