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_7716455
_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_absolute_configuration ad
_chemical_formula_moiety         'C13 H20 F10 P Sb Se'
_chemical_formula_sum            'C13 H20 F10 P Sb Se'
_chemical_formula_weight         597.97
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2021-09-23
_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                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   6.71696(7)
_cell_length_b                   11.89385(13)
_cell_length_c                   24.6205(2)
_cell_measurement_reflns_used    56609
_cell_measurement_temperature    99.98(10)
_cell_measurement_theta_max      31.7900
_cell_measurement_theta_min      2.3770
_cell_volume                     1966.94(3)
_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    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      99.98(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 0.977
_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     36.00  88.00   1.00    2.50    --   26.03-132.00 100.87   52
  2  \w    -17.00  97.00   1.00    2.50    --   26.03  19.00 120.00  114
  3  \w      7.00  59.00   1.00    2.50    --   26.03  57.00-120.00   52
  4  \w    -43.00  42.00   1.00    2.50    --   26.03 -57.00 150.00   85
  5  \w      5.00  98.00   1.00    2.50    --   26.03  38.00-180.00   93
  6  \w      9.00  95.00   1.00    2.50    --   26.03  57.00 -60.00   86
  7  \w     39.00  87.00   1.00    2.50    --   26.03 178.00  60.00   48
  8  \w    -10.00  65.00   1.00    2.50    --   26.03 -99.00 -90.00   75
  9  \w    -47.00  69.00   1.00    2.50    --   26.03 -19.00   0.00  116
 10  \w     -4.00  37.00   1.00    2.50    --   26.03  77.00  30.00   41
 11  \w      6.00  38.00   1.00    2.50    --   26.03  77.00  90.00   32
 12  \w    -35.00  -9.00   1.00    2.50    --   26.03 132.00 170.69   26
 13  \w    -99.00 -39.00   1.00    2.50    --  -23.50-178.00-180.00   60
 14  \w     39.00 102.00   1.00    2.50    --   26.03 178.00  30.00   63
 15  \w    -47.00  99.00   1.00    2.50    --   26.03   0.00-180.00  146
 16  \w    -47.00  99.00   1.00    2.50    --   26.03   0.00-120.00  146
 17  \w    -15.00  68.00   1.00    2.50    --   26.03 -99.00-120.00   83
 18  \w      6.00  95.00   1.00    2.50    --   26.03  57.00-150.00   89
 19  \w     -4.00  42.00   1.00    2.50    --   26.03  77.00 150.00   46
 20  \w    -47.00  99.00   1.00    2.50    --   26.03   0.00-150.00  146
 21  \w      6.00  95.00   1.00    2.50    --   26.03  57.00  30.00   89
 22  \w     37.00 103.00   1.00    2.50    --   26.03-178.00-120.00   66
 23  \w    -47.00  99.00   1.00    2.50    --   26.03   0.00 -60.00  146
 24  \w    -47.00  99.00   1.00    2.50    --   26.03   0.00 -30.00  146
 25  \w    -47.00  99.00   1.00    2.50    --   26.03   0.00   0.00  146
 26  \w    -47.00  87.00   1.00    2.50    --   26.03   0.00  30.00  134
 27  \w    -47.00  99.00   1.00    2.50    --   26.03   0.00 -90.00  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      -0.0215203000
_diffrn_orient_matrix_UB_12      0.0379829000
_diffrn_orient_matrix_UB_13      -0.0214261000
_diffrn_orient_matrix_UB_21      -0.0792663000
_diffrn_orient_matrix_UB_22      -0.0351338000
_diffrn_orient_matrix_UB_23      -0.0086052000
_diffrn_orient_matrix_UB_31      -0.0663678000
_diffrn_orient_matrix_UB_32      0.0296690000
_diffrn_orient_matrix_UB_33      0.0172234000
_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  0.0363
_diffrn_reflns_av_unetI/netI     0.0150
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.977
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            120071
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.966
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         32.211
_diffrn_reflns_theta_min         1.902
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    3.420
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.526
_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    2.019
_exptl_crystal_description       block
_exptl_crystal_F_000             1152
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.537
_refine_diff_density_min         -0.311
_refine_diff_density_rms         0.067
_refine_ls_abs_structure_details
;
 Flack x determined using 2707 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.0308(19)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.072
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     241
_refine_ls_number_reflns         6704
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.072
_refine_ls_R_factor_all          0.0175
_refine_ls_R_factor_gt           0.0156
_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^)+(0.0118P)^2^+0.7530P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0304
_refine_ls_wR_factor_ref         0.0308
_reflns_Friedel_coverage         0.746
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.951
_reflns_number_gt                6490
_reflns_number_total             6704
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt01591f2.cif
_cod_data_source_block           4
_cod_depositor_comments
'Adding full bibliography for 7716449--7716457.cif.'
_cod_database_code               7716455
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C13H20F10PSbSe
_shelx_estimated_absorpt_t_max   0.772
_shelx_estimated_absorpt_t_min   0.427
_diffrn_oxdiff_digest_frames
;
01c30e2830c06273514cf4963f65fa5b9c025740137
;
_diffrn_oxdiff_digest_hkl
;
01c44f81d6df98078561e3ad206110405e0ad9
;
_reflns_odcompleteness_completeness 99.94
_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              4419
_shelx_hkl_checksum              4895
_olex2_date_sample_data_collection 2021-09-23
_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 1.606
_oxdiff_exptl_absorpt_empirical_full_min 0.821