Oxidation-dependent Lewis acidity in chalcogen adducts of Sb/P frustrated Lewis pairs.
Krieft, Jonas; Neumann, Beate; Stammler, Hans-Georg; Mitzel, Norbert W.; Dalton transactions (Cambridge, England : 2003) 53 (2024) 11762–11768; doi:10.1039/d4dt01591f

data_7716449
_publ_section_title
;
 Oxidation-dependent Lewis acidity in chalcogen adducts of Sb/P frustrated
 Lewis pairs.
;
_journal_issue                   28
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              11762
_journal_page_last               11768
_journal_paper_doi               10.1039/d4dt01591f
_journal_volume                  53
_journal_year                    2024
_chemical_formula_moiety         'C13 H20 F10 O P Sb'
_chemical_formula_sum            'C13 H20 F10 O P Sb'
_chemical_formula_weight         535.01
_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             2021-09-07
_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.	2024-06-24 downloaded from the CCDC.
;
_cell_angle_alpha                87.221(2)
_cell_angle_beta                 89.312(2)
_cell_angle_gamma                77.017(2)
_cell_formula_units_Z            4
_cell_length_a                   10.6777(2)
_cell_length_b                   11.9730(3)
_cell_length_c                   15.3503(3)
_cell_measurement_reflns_used    44092
_cell_measurement_temperature    100.00(11)
_cell_measurement_theta_max      31.8200
_cell_measurement_theta_min      1.9270
_cell_volume                     1910.03(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      100.00(11)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0951
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.945
_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    -66.00  42.00   1.00   13.50    --  -30.27  77.00 120.00  108
  2  \w   -114.00 -39.00   1.00   13.50    --  -30.27-178.00 -90.00   75
  3  \w    -42.00  57.00   1.00   13.50    --   30.43 -57.00-120.00   99
  4  \w     -5.00  42.00   1.00   13.50    --   30.43  77.00  60.00   47
  5  \w     -5.00  42.00   1.00   13.50    --   30.43  77.00 -90.00   47
  6  \w      4.00 103.00   1.00   13.50    --   30.43  57.00 120.00   99
  7  \w     37.00 115.00   1.00   13.50    --   30.43-178.00 -60.00   78
  8  \w     -5.00  42.00   1.00   13.50    --   30.43  77.00 -30.00   47
  9  \w     -5.00  42.00   1.00   13.50    --   30.43  77.00-180.00   47
 10  \w    -47.00 108.00   1.00   13.50    --   30.43   0.00 -60.00  155
 11  \w     -5.00  42.00   1.00   13.50    --   30.43  77.00-150.00   47
 12  \w    -15.00  79.00   1.00   13.50    --   30.43 -99.00 -30.00   94
 13  \w     -6.00 106.00   1.00   13.50    --   30.43  38.00  30.00  112
 14  \w   -106.00   6.00   1.00   13.50    --  -30.27 -38.00-150.00  112
 15  \w    -42.00   5.00   1.00   13.50    --  -30.27 -77.00   0.00   47
 16  \w   -104.00  48.00   1.00   13.50    --  -30.27  19.00-120.00  152
 17  \w   -103.00  -3.00   1.00   13.50    --  -30.27 -57.00  90.00  100
 18  \w    -47.00 108.00   1.00   13.50    --   30.43   0.00-180.00  155
 19  \w    -15.00  79.00   1.00   13.50    --   30.43 -99.00  60.00   94
 20  \w    -47.00 108.00   1.00   13.50    --   30.43   0.00-120.00  155
 21  \w    -47.00 108.00   1.00   13.50    --   30.43   0.00-150.00  155
 22  \w    -47.00 108.00   1.00   13.50    --   30.43   0.00 -90.00  155
 23  \w    -34.00  -8.00   1.00   13.50    --   30.43 128.00 -24.27   26
 24  \w    -47.00 -10.00   1.00   13.50    --   30.43   0.00 -60.00   37
;
_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      0.0083805000
_diffrn_orient_matrix_UB_12      -0.0501840000
_diffrn_orient_matrix_UB_13      -0.0241501000
_diffrn_orient_matrix_UB_21      0.0621928000
_diffrn_orient_matrix_UB_22      -0.0201595000
_diffrn_orient_matrix_UB_23      0.0181889000
_diffrn_orient_matrix_UB_31      -0.0266285000
_diffrn_orient_matrix_UB_32      -0.0279186000
_diffrn_orient_matrix_UB_33      0.0350160000
_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  0.0270
_diffrn_reflns_av_unetI/netI     0.0409
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.945
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            116799
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.945
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         32.046
_diffrn_reflns_theta_min         1.747
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.621
_exptl_absorpt_correction_T_max  -0.010
_exptl_absorpt_correction_T_min  10000000.000
_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    1.861
_exptl_crystal_description       block
_exptl_crystal_F_000             1048
_exptl_crystal_size_max          0.245
_exptl_crystal_size_mid          0.086
_exptl_crystal_size_min          0.084
_refine_diff_density_max         2.147
_refine_diff_density_min         -1.080
_refine_diff_density_rms         0.125
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     482
_refine_ls_number_reflns         20644
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.053
_refine_ls_R_factor_all          0.0452
_refine_ls_R_factor_gt           0.0376
_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^)+(0.0335P)^2^+5.1517P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0926
_refine_ls_wR_factor_ref         0.0947
_reflns_Friedel_coverage         0.000
_reflns_number_gt                17695
_reflns_number_total             20644
_reflns_threshold_expression     'I > 2\s(I)'
_twin_special_details
;
Component 2 rotated by -179.9258\% 
around [0.01 0.03 1.00] (reciprocal) or [-0.00 -0.01 1.00] (direct)
;
_cod_data_source_file            d4dt01591f2.cif
_cod_data_source_block           2
_cod_depositor_comments
'Adding full bibliography for 7716449--7716457.cif.'
_cod_database_code               7716449
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C26H40F20O2P2Sb2
_diffrn_oxdiff_digest_frames
;
0177ca74b16c70c760a3068557eb359cbc02247b893
;
_diffrn_oxdiff_digest_hkl
;
018d3d5ab2e7234c62efd415f27c304bf3a96c
;
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.7495(5)
 0.2505(5)
2. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
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              98713
_shelx_hkl_checksum              60055
_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 1.617
_oxdiff_exptl_absorpt_empirical_full_min 0.668
_oxdiff_twin_integration_method  simultaneous
_oxdiff_twin_items               2