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_7716457
_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         'C25 H20 Cl8 F10 O4 P Sb'
_chemical_formula_sum            'C25 H20 Cl8 F10 O4 P Sb'
_chemical_formula_weight         1010.73
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2024-04-18
_audit_creation_method
;
Olex2 1.5-alpha
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2024-04-23 deposited with the CCDC.	2024-06-24 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 99.9478(7)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   11.25738(7)
_cell_length_b                   38.60501(18)
_cell_length_c                   16.16983(12)
_cell_measurement_reflns_used    141772
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      32.2160
_cell_measurement_theta_min      2.0260
_cell_volume                     6921.62(8)
_computing_cell_refinement       'CrysAlisPro 1.171.40.82a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.82a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.82a (Rigaku OD, 2020)'
_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 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      6.00  95.00   1.00   58.50    --   26.03  57.00-120.00   89
  2  \w      6.00  95.00   1.00   58.50    --   26.03  57.00  30.00   89
  3  \w     -4.00  42.00   1.00   58.50    --   26.03  77.00 150.00   46
  4  \w    -46.00  52.00   1.00   58.50    --   26.03 -38.00 -60.00   98
  5  \w     -4.00  42.00   1.00   58.50    --   26.03  77.00 -30.00   46
  6  \w      6.00  95.00   1.00   58.50    --   26.03  57.00 120.00   89
  7  \w    -15.00  68.00   1.00   58.50    --   26.03 -99.00  90.00   83
  8  \w    -43.00  47.00   1.00   58.50    --   26.03 -57.00-120.00   90
  9  \w      1.00  98.00   1.00   58.50    --   26.03  38.00 -30.00   97
 10  \w      6.00  95.00   1.00   58.50    --   26.03  57.00-150.00   89
 11  \w    -43.00  47.00   1.00   58.50    --   26.03 -57.00 150.00   90
 12  \w     -4.00  42.00   1.00   58.50    --   26.03  77.00-120.00   46
 13  \w    -15.00  68.00   1.00   58.50    --   26.03 -99.00 -90.00   83
 14  \w    -15.00  68.00   1.00   58.50    --   26.03 -99.00 120.00   83
 15  \w     -4.00  42.00   1.00   58.50    --   26.03  77.00  30.00   46
 16  \w    -15.00  68.00   1.00   58.50    --   26.03 -99.00  60.00   83
 17  \w    -47.00  99.00   1.00   58.50    --   26.03   0.00-180.00  146
 18  \w    -47.00  99.00   1.00   58.50    --   26.03   0.00-150.00  146
 19  \w    -47.00  57.00   1.00   58.50    --   26.03   0.00-120.00  104
 20  \w     37.00 103.00   1.00   58.50    --   26.03-178.00  90.00   66
;
_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      0.0380962000
_diffrn_orient_matrix_UB_12      0.0009473000
_diffrn_orient_matrix_UB_13      0.0397611000
_diffrn_orient_matrix_UB_21      0.0025818000
_diffrn_orient_matrix_UB_22      0.0182733000
_diffrn_orient_matrix_UB_23      -0.0038085000
_diffrn_orient_matrix_UB_31      -0.0513338000
_diffrn_orient_matrix_UB_32      0.0016224000
_diffrn_orient_matrix_UB_33      0.0197085000
_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  0.0455
_diffrn_reflns_av_unetI/netI     0.0197
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       54
_diffrn_reflns_limit_k_min       -54
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            279858
_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         30.033
_diffrn_reflns_theta_min         1.658
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.549
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.778
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.82a (Rigaku Oxford Diffraction, 2020)
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    1.940
_exptl_crystal_description       irregular
_exptl_crystal_F_000             3952
_exptl_crystal_size_max          0.186
_exptl_crystal_size_mid          0.098
_exptl_crystal_size_min          0.054
_refine_diff_density_max         1.739
_refine_diff_density_min         -0.912
_refine_diff_density_rms         0.121
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.217
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     977
_refine_ls_number_reflns         20241
_refine_ls_number_restraints     10
_refine_ls_restrained_S_all      1.221
_refine_ls_R_factor_all          0.0571
_refine_ls_R_factor_gt           0.0526
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0336P)^2^+26.0742P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1179
_refine_ls_wR_factor_ref         0.1199
_reflns_Friedel_coverage         0.000
_reflns_number_gt                18660
_reflns_number_total             20241
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt01591f2.cif
_cod_data_source_block           9
_cod_depositor_comments
'Adding full bibliography for 7716449--7716457.cif.'
_cod_database_code               7716457
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C25H20Cl8F10O4PSb
_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. Restrained distances
 C32A-C31 \\sim C32B-C31 \\sim C33-C31 \\sim C34A-C31 \\sim C34B-C31
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C34B) = Uanis(C34A)
Uanis(C30B) = Uanis(C30A)
4. Others
 Sof(F16B)=Sof(F17B)=Sof(F18B)=Sof(F19B)=Sof(F20B)=Sof(C29B)=Sof(C30B)=
 Sof(H30C)=Sof(H30D)=Sof(C32B)=Sof(H32D)=Sof(H32E)=Sof(H32F)=Sof(C34B)=
 Sof(H34D)=Sof(H34E)=Sof(H34F)=Sof(C36B)=Sof(H36D)=Sof(H36E)=Sof(H36F)=1-FVAR(1)
 Sof(F16A)=Sof(F17A)=Sof(F18A)=Sof(F19A)=Sof(F20A)=Sof(C29A)=Sof(C30A)=
 Sof(H30A)=Sof(H30B)=Sof(C32A)=Sof(H32A)=Sof(H32B)=Sof(H32C)=Sof(C34A)=
 Sof(H34A)=Sof(H34B)=Sof(H34C)=Sof(C36A)=Sof(H36A)=Sof(H36B)=Sof(H36C)=FVAR(1)
5.a Secondary CH2 refined with riding coordinates:
 C5(H5A,H5B), C30A(H30A,H30B), C30B(H30C,H30D)
5.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), C32A(H32A,H32B,H32C), C32B(H32D,H32E,
 H32F), C33(H33A,H33B,H33C), C34A(H34A,H34B,H34C), C34B(H34D,H34E,H34F),
 C36A(H36A,H36B,H36C), C36B(H36D,H36E,H36F), C37(H37A,H37B,H37C), C38(H38A,H38B,
 H38C)
;
_shelx_res_checksum              71297
_shelx_hkl_checksum              1857
_olex2_date_sample_data_collection 2021-03-19
_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 1.184
_oxdiff_exptl_absorpt_empirical_full_min 0.880