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_7716452
_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 O2 P Sb'
_chemical_formula_sum            'C19 H20 Cl4 F10 O2 P Sb'
_chemical_formula_weight         764.87
_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             2021-05-02
_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                77.029(2)
_cell_angle_beta                 70.351(2)
_cell_angle_gamma                69.951(2)
_cell_formula_units_Z            4
_cell_length_a                   11.9408(3)
_cell_length_b                   14.7066(4)
_cell_length_c                   17.0446(4)
_cell_measurement_reflns_used    34091
_cell_measurement_temperature    100.01(12)
_cell_measurement_theta_max      31.9060
_cell_measurement_theta_min      2.0340
_cell_volume                     2627.82(12)
_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      100.01(12)
_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 0.936
_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    -18.00  99.00   1.00   33.00    --   26.03  19.00 -60.00  117
  2  \w     -4.00  42.00   1.00   33.00    --   26.03  77.00  30.00   46
  3  \w      6.00  95.00   1.00   33.00    --   26.03  57.00 120.00   89
  4  \w      6.00  83.00   1.00   33.00    --   26.03-125.00 148.00   77
  5  \w      1.00  98.00   1.00   33.00    --   26.03  38.00  30.00   97
  6  \w    -43.00  47.00   1.00   33.00    --   26.03 -57.00 -30.00   90
  7  \w     39.00 102.00   1.00   33.00    --   26.03 178.00 -90.00   63
  8  \w     -4.00  42.00   1.00   33.00    --   26.03  77.00 -60.00   46
  9  \w    -46.00  52.00   1.00   33.00    --   26.03 -38.00  60.00   98
 10  \w      6.00  95.00   1.00   33.00    --   26.03  57.00-150.00   89
 11  \w    -46.00  52.00   1.00   33.00    --   26.03 -38.00-150.00   98
 12  \w     -4.00  42.00   1.00   33.00    --   26.03  77.00-180.00   46
 13  \w     16.00  97.00   1.00   33.00    --   26.03-147.00 -17.00   81
 14  \w    -92.00  -2.00   1.00   33.00    --  -23.50 -57.00-180.00   90
 15  \w    -42.00   7.00   1.00   33.00    --  -23.50 -77.00-120.00   49
 16  \w    -92.00  -2.00   1.00   33.00    --  -23.50 -57.00   0.00   90
 17  \w      6.00  95.00   1.00   33.00    --   26.03  57.00 -60.00   89
 18  \w     39.00 102.00   1.00   33.00    --   26.03 178.00-180.00   63
 19  \w     -4.00  42.00   1.00   33.00    --   26.03  77.00  60.00   46
;
_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      0.0459536000
_diffrn_orient_matrix_UB_12      -0.0149819000
_diffrn_orient_matrix_UB_13      0.0216796000
_diffrn_orient_matrix_UB_21      0.0244946000
_diffrn_orient_matrix_UB_22      -0.0453399000
_diffrn_orient_matrix_UB_23      -0.0163855000
_diffrn_orient_matrix_UB_31      0.0404426000
_diffrn_orient_matrix_UB_32      0.0199129000
_diffrn_orient_matrix_UB_33      -0.0352736000
_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  0.0326
_diffrn_reflns_av_unetI/netI     0.0527
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.936
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            94844
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.936
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         32.228
_diffrn_reflns_theta_min         1.485
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.606
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.810
_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    1.933
_exptl_crystal_description       irregular
_exptl_crystal_F_000             1496
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.099
_exptl_crystal_size_min          0.056
_refine_diff_density_max         0.916
_refine_diff_density_min         -0.474
_refine_diff_density_rms         0.084
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.897
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     680
_refine_ls_number_reflns         20292
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.897
_refine_ls_R_factor_all          0.0291
_refine_ls_R_factor_gt           0.0220
_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^)+(0.0272P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0469
_refine_ls_wR_factor_ref         0.0479
_reflns_Friedel_coverage         0.000
_reflns_number_gt                17011
_reflns_number_total             20292
_reflns_threshold_expression     'I > 2\s(I)'
_twin_special_details
;
Component 2 rotated by 179.9996\% 
around [-0.32 -0.01 0.95] (reciprocal) or [-0.71 0.00 0.71] (direct)
;
_cod_data_source_file            d4dt01591f2.cif
_cod_data_source_block           10
_cod_depositor_comments
'Adding full bibliography for 7716449--7716457.cif.'
_cod_original_cell_volume        2627.82(13)
_cod_database_code               7716452
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C19 H20 Cl4 F10 O P Sb'
_shelx_estimated_absorpt_t_max   0.915
_shelx_estimated_absorpt_t_min   0.806
_diffrn_oxdiff_digest_frames
;
01724e926cbe5c5a2a8cf36cf100e61f4a014708da0
;
_diffrn_oxdiff_digest_hkl
;
0106f345445101743d893a5ab448002e1accdc
;
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.6013(4)
 0.3987(4)
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), C24(H24A,H24B)
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), C26(H26A,H26B,H26C), C27(H27A,H27B,
 H27C), C28(H28A,H28B,H28C), C30(H30A,H30B,H30C), C31(H31A,H31B,H31C), C32(H32A,
 H32B,H32C)
;
_shelx_res_checksum              53210
_shelx_hkl_checksum              55220
_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 1.103
_oxdiff_exptl_absorpt_empirical_full_min 0.921
_oxdiff_twin_integration_method  simultaneous
_oxdiff_twin_items               2