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_7716453
_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 Se'
_chemical_formula_sum            'C19 H20 Cl4 F10 O2 P Sb Se'
_chemical_formula_weight         843.83
_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
_atom_sites_solution_primary     dual
_audit_creation_date             2023-05-17
_audit_creation_method
;
Olex2 1.5-dev
(compiled 2023.04.26 svn.r751481ca for OlexSys, GUI svn.r6781)
;
_audit_update_record
;
2024-04-23 deposited with the CCDC.	2024-06-24 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 94.395(3)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   15.5087(4)
_cell_length_b                   17.1296(4)
_cell_length_c                   21.3832(7)
_cell_measurement_reflns_used    20407
_cell_measurement_temperature    100.0(1)
_cell_measurement_theta_max      75.9370
_cell_measurement_theta_min      3.2940
_cell_volume                     5663.9(3)
_computing_cell_refinement       'CrysAlisPro 1.171.42.90a (Rigaku OD, 2023)'
_computing_data_collection       'CrysAlisPro 1.171.42.90a (Rigaku OD, 2023)'
_computing_data_reduction        'CrysAlisPro 1.171.42.90a (Rigaku OD, 2023)'
_computing_molecular_graphics    'Olex2 1.5-dev (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-dev (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      100.0(1)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.3114
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_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    -86.00 -17.00   1.00   12.50    --  -38.50 125.00  90.00   69
  2  \w    -53.00  33.00   1.00   12.50    --  -38.50  38.00  90.00   86
  3  \w    -96.00 -42.00   1.00   12.50    --  -38.50 -38.00-120.00   54
  4  \w    -54.00  -7.00   1.00   12.50    --  -38.50 125.00-180.00   47
  5  \w   -115.00  -8.00   1.00   12.50    --  -38.50 -19.00 -90.00  107
  6  \w     41.00  93.00   1.00   12.50    --   42.70-125.00   0.00   52
  7  \w    128.00 155.00   1.00   44.00    --  111.00 125.00  90.00   27
  8  \w     91.00 171.00   1.00   44.00    --  111.00  30.00-180.00   80
  9  \w     46.00  73.00   1.00   44.00    --  111.00 -70.00 162.90   27
 10  \w     63.00  90.00   1.00   44.00    --  111.00-125.00 -30.00   27
 11  \w     80.00 107.00   1.00   44.00    --  111.00 -30.00 -90.00   27
 12  \w     40.00  65.00   1.00   44.00    --  111.00 -94.00-180.00   25
 13  \w    120.00 170.00   1.00   44.00    --  111.00  77.00  30.00   50
 14  \w     63.00  92.00   1.00   44.00    --  111.00 -94.00  60.00   29
 15  \w     96.00 133.00   1.00   44.00    --  111.00 -45.00-150.00   37
 16  \w     63.00 106.00   1.00   44.00    --  111.00 -94.00 150.00   43
 17  \w     32.00 106.00   1.00   44.00    --  111.00 -94.00-120.00   74
 18  \w    140.00 176.00   1.00   44.00    --  111.00  30.00 150.00   36
 19  \w     55.00 108.00   1.00   44.00    --  111.00-113.00-133.00   53
 20  \w     97.00 168.00   1.00   44.00    --  111.00  30.00-150.00   71
 21  \w     95.00 132.00   1.00   44.00    --  111.00 -45.00 150.00   37
 22  \w     85.00 113.00   1.00   44.00    --  111.00-125.00   0.00   28
 23  \w    106.00 131.00   1.00   44.00    --  111.00 -30.00-120.00   25
 24  \w     76.00 103.00   1.00   44.00    --  111.00  15.00 -60.00   27
 25  \w    129.00 162.00   1.00   44.00    --  111.00  15.00 -60.00   33
 26  \w     46.00  73.00   1.00   44.00    --  111.00 -61.00 -30.00   27
 27  \w    100.00 134.00   1.00   44.00    --  111.00 -61.00 -30.00   34
 28  \w     34.00 104.00   1.00   44.00    --  111.00 -15.00-150.00   70
 29  \w    106.00 131.00   1.00   44.00    --  111.00 -15.00-150.00   25
 30  \w     70.00 107.00   1.00   44.00    --  111.00 -94.00 120.00   37
 31  \w     83.00 110.00   1.00   44.00    --  111.00 -45.00  30.00   27
 32  \w     42.00  71.00   1.00   44.00    --  111.00 -77.00 150.00   29
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0201137000
_diffrn_orient_matrix_UB_12      0.0879484000
_diffrn_orient_matrix_UB_13      -0.0025319000
_diffrn_orient_matrix_UB_21      -0.0105687000
_diffrn_orient_matrix_UB_22      0.0066134000
_diffrn_orient_matrix_UB_23      0.0708653000
_diffrn_orient_matrix_UB_31      0.0970087000
_diffrn_orient_matrix_UB_32      -0.0175155000
_diffrn_orient_matrix_UB_33      0.0139350000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0790
_diffrn_reflns_av_unetI/netI     0.0548
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            46220
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         68.248
_diffrn_reflns_theta_min         2.858
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    14.004
_exptl_absorpt_correction_T_max  0.60775
_exptl_absorpt_correction_T_min  0.57540
_exptl_absorpt_correction_type   sphere
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.90a (Rigaku Oxford Diffraction, 2023)
Spherical absorption correction
using equivalent radius and absorption coefficient.
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.979
_exptl_crystal_description       plate
_exptl_crystal_F_000             3264
_exptl_crystal_size_max          0.09
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.01
_exptl_crystal_size_rad          0.026
_refine_diff_density_max         1.607
_refine_diff_density_min         -1.975
_refine_diff_density_rms         0.163
_refine_ls_extinction_coef       0.00017(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     698
_refine_ls_number_reflns         10305
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.058
_refine_ls_R_factor_all          0.0665
_refine_ls_R_factor_gt           0.0580
_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^)+(0.0872P)^2^+18.7781P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1514
_refine_ls_wR_factor_ref         0.1602
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8829
_reflns_number_total             10305
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt01591f2.cif
_cod_data_source_block           8
_cod_depositor_comments
'Adding full bibliography for 7716449--7716457.cif.'
_cod_database_code               7716453
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C19 H20 Cl4 F10 O2 P Sb Se'
_shelx_estimated_absorpt_t_max   0.873
_shelx_estimated_absorpt_t_min   0.365
_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), C24(H24A,H24B)
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), 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              61197
_shelx_hkl_checksum              24953
_olex2_date_sample_data_collection 2023-05-12
_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 2.565
_oxdiff_exptl_absorpt_empirical_full_min 0.424