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_7716454
_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         'C19 H20 Cl4 F10 O3 P Sb'
_chemical_formula_sum            'C19 H20 Cl4 F10 O3 P Sb'
_chemical_formula_weight         780.87
_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 1.3-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                87.019(2)
_cell_angle_beta                 72.235(2)
_cell_angle_gamma                68.647(2)
_cell_formula_units_Z            2
_cell_length_a                   10.4459(2)
_cell_length_b                   11.2266(2)
_cell_length_c                   12.8446(3)
_cell_measurement_reflns_used    48090
_cell_measurement_temperature    100.00(11)
_cell_measurement_theta_max      31.7720
_cell_measurement_theta_min      2.1620
_cell_volume                     1333.05(5)
_computing_cell_refinement       'CrysAlisPro 1.171.41.119a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.119a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.119a (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 0.933
_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    -43.00  47.00   1.00   16.50    --   26.03 -57.00 150.00   90
  2  \w    -15.00  68.00   1.00   16.50    --   26.03 -99.00   0.00   83
  3  \w     -4.00  42.00   1.00   16.50    --   26.03  77.00 -60.00   46
  4  \w     -4.00  42.00   1.00   16.50    --   26.03  77.00 120.00   46
  5  \w      1.00  98.00   1.00   16.50    --   26.03  38.00-120.00   97
  6  \w     37.00 103.00   1.00   16.50    --   26.03-178.00   0.00   66
  7  \w    -43.00  47.00   1.00   16.50    --   26.03 -57.00  60.00   90
  8  \w     -4.00  42.00   1.00   16.50    --   26.03  77.00-180.00   46
  9  \w    -15.00  68.00   1.00   16.50    --   26.03 -99.00-180.00   83
 10  \w      6.00  95.00   1.00   16.50    --   26.03  57.00  30.00   89
 11  \w      1.00  98.00   1.00   16.50    --   26.03  38.00 -30.00   97
 12  \w    -47.00  99.00   1.00   16.50    --   26.03   0.00-180.00  146
 13  \w    -92.00  -2.00   1.00   16.50    --  -23.50 -57.00-180.00   90
 14  \w     -4.00  42.00   1.00   16.50    --   26.03  77.00-120.00   46
 15  \w    -47.00  99.00   1.00   16.50    --   26.03   0.00-150.00  146
 16  \w    -47.00  99.00   1.00   16.50    --   26.03   0.00 -90.00  146
 17  \w     -3.00  76.00   1.00   16.50    --   26.03-114.00  81.00   79
 18  \w    -47.00  99.00   1.00   16.50    --   26.03   0.00-180.00  146
 19  \w    -15.00  68.00   1.00   16.50    --   26.03 -99.00-120.00   83
 20  \w    -47.00  99.00   1.00   16.50    --   26.03   0.00-120.00  146
 21  \w    -15.00  68.00   1.00   16.50    --   26.03 -99.00  30.00   83
 22  \w     -4.00  42.00   1.00   16.50    --   26.03  77.00  60.00   46
 23  \w    -47.00  99.00   1.00   16.50    --   26.03   0.00 -30.00  146
 24  \w    -47.00  99.00   1.00   16.50    --   26.03   0.00   0.00  146
 25  \w    -47.00  41.00   1.00   16.50    --   26.03   0.00  30.00   88
 26  \w    -47.00  99.00   1.00   16.50    --   26.03   0.00 -60.00  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      -0.0565086000
_diffrn_orient_matrix_UB_12      -0.0185076000
_diffrn_orient_matrix_UB_13      0.0337146000
_diffrn_orient_matrix_UB_21      -0.0002739000
_diffrn_orient_matrix_UB_22      -0.0316765000
_diffrn_orient_matrix_UB_23      -0.0462483000
_diffrn_orient_matrix_UB_31      0.0517499000
_diffrn_orient_matrix_UB_32      -0.0572401000
_diffrn_orient_matrix_UB_33      0.0100931000
_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  0.0466
_diffrn_reflns_av_unetI/netI     0.0232
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.933
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            83450
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.933
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         32.350
_diffrn_reflns_theta_min         1.668
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.588
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.505
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.119a (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    1.945
_exptl_crystal_description       irregular
_exptl_crystal_F_000             764
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.395
_refine_diff_density_min         -0.632
_refine_diff_density_rms         0.110
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.097
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     349
_refine_ls_number_reflns         8894
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.097
_refine_ls_R_factor_all          0.0309
_refine_ls_R_factor_gt           0.0271
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0367P)^2^+0.7291P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0673
_refine_ls_wR_factor_ref         0.0694
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8214
_reflns_number_total             8894
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt01591f2.cif
_cod_data_source_block           6
_cod_depositor_comments
'Adding full bibliography for 7716449--7716457.cif.'
_cod_database_code               7716454
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C19H20Cl4F10O3PSb
_shelx_estimated_absorpt_t_max   0.883
_shelx_estimated_absorpt_t_min   0.702
_diffrn_oxdiff_digest_frames
;
016ebd5780243f0e0a77040a2d90b0d201025202243
;
_diffrn_oxdiff_digest_hkl
;
01dab50df3b3bf8409381c21c0094efe70f699
;
_reflns_odcompleteness_completeness 100.00
_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.a Secondary CH2 refined with riding coordinates:
 C5(H5A,H5B)
2.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              96904
_shelx_hkl_checksum              90967
_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 1.577
_oxdiff_exptl_absorpt_empirical_full_min 0.717