Variation in pnictogen-oxygen bonding unlocks greatly enhanced Brønsted basicity for the monomeric stibine oxide.
Wenger, John S.; Getahun, Addis; Johnstone, Timothy C.; Dalton transactions (Cambridge, England : 2003)  (2023) –; doi:10.1039/d3dt02113k

data_7713648
_publ_section_title
;
 Variation in pnictogen-oxygen bonding unlocks greatly enhanced
 Br&#xf8;nsted basicity for the monomeric stibine oxide.
;
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_paper_doi               10.1039/d3dt02113k
_journal_year                    2023
_chemical_formula_moiety         'C36 H52 As O, C F3 O3 S, C H Cl3'
_chemical_formula_sum            'C38 H53 As Cl3 F3 O4 S'
_chemical_formula_weight         844.13
_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   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2022-07-15
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2023-03-21 deposited with the CCDC.	2023-07-28 downloaded from the CCDC.
;
_cell_angle_alpha                92.4510(10)
_cell_angle_beta                 101.6540(10)
_cell_angle_gamma                100.5970(10)
_cell_formula_units_Z            2
_cell_length_a                   10.1956(2)
_cell_length_b                   14.2779(2)
_cell_length_c                   14.7095(2)
_cell_measurement_reflns_used    18782
_cell_measurement_temperature    101(1)
_cell_measurement_theta_max      77.0620
_cell_measurement_theta_min      3.0690
_cell_volume                     2054.26(6)
_computing_cell_refinement       'CrysAlisPro 1.171.42.53a (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.53a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.53a (Rigaku OD, 2022)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      101(1)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_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    -38.00 -13.00   0.50    0.12    --  -84.25  57.00  90.00   50
  2  \w    -59.00 -33.00   0.50    0.12    --  -84.25  57.00 -30.00   52
  3  \w    -69.00 -12.00   0.50    0.12    --  -84.25  77.00-120.00  114
  4  \w    -62.00 -15.00   0.50    0.12    --  -84.25  57.00-120.00   94
  5  \w    -38.00 -13.00   0.50    0.12    --  -84.25  38.00-150.00   50
  6  \w    -42.00 -13.00   0.50    0.12    --  -84.25  38.00-180.00   58
  7  \w    -39.00 -13.00   0.50    0.12    --  -84.25  38.00  60.00   52
  8  \w    -60.00  23.00   0.50    0.05    --  -49.41  57.00  90.00  166
  9  \w    -28.00  -3.00   0.50    0.05    --  -49.41  27.00  88.00   50
 10  \w    -24.00  24.00   0.50    0.05    --  -49.41  19.00-150.00   96
 11  \w     59.00  85.00   0.50    0.05    --   49.41  27.00  88.00   52
 12  \w    103.00 173.00   0.50    0.12    --  105.75  27.00  88.00  140
 13  \w    104.00 173.00   0.50    0.12    --  105.75  19.00  30.00  138
 14  \w    125.00 177.00   0.50    0.12    --  105.75  19.00 -30.00  104
 15  \w    112.00 177.00   0.50    0.12    --  105.75  38.00 -60.00  130
 16  \w    152.00 177.00   0.50    0.12    --  105.75  38.00-150.00   50
 17  \w    102.00 142.00   0.50    0.12    --  105.75  38.00-150.00   80
 18  \w    -21.00  23.00   0.50    0.05    --   49.41 -19.00-150.00   88
 19  \w     34.00  59.00   0.50    0.12    --  105.75 -77.00-150.00   50
 20  \w     35.00  66.00   0.50    0.12    --  105.75 -57.00-120.00   62
 21  \w     80.00 106.00   0.50    0.12    --  105.75 -77.00-150.00   52
 22  \w     38.00  63.00   0.50    0.12    --  105.75 -57.00-150.00   50
 23  \w    -23.00  34.00   0.50    0.05    --   49.41 -27.00 -74.00  114
 24  \w     34.00  60.00   0.50    0.12    --  105.75 -57.00  90.00   52
 25  \w     47.00 100.00   0.50    0.12    --  105.75 -77.00  30.00  106
 26  \w     41.00  89.00   0.50    0.12    --  105.75 -99.00  30.00   96
 27  \w     34.00 106.00   0.50    0.12    --  105.75 -99.00   0.00  144
 28  \w     34.00 104.00   0.50    0.12    --  105.75 -99.00 120.00  140
 29  \w     76.00 102.00   0.50    0.12    --  105.75 -99.00  60.00   52
 30  \w     55.00  94.00   0.50    0.12    --  105.75 -99.00 -60.00   78
 31  \w     72.00 106.00   0.50    0.12    --  105.75 -99.00 -90.00   68
 32  \w     76.00 106.00   0.50    0.12    --  105.75 -99.00-150.00   60
 33  \w     42.00 100.00   0.50    0.12    --  105.75 -99.00-180.00  116
 34  \w     37.00  87.00   0.50    0.12    --  105.75 -99.00 -30.00  100
 35  \w     41.00  89.00   0.50    0.12    --  105.75 -99.00 150.00   96
 36  \w   -122.00 -59.00   0.50    0.05    --  -49.41 -27.00 -74.00  126
 37  \w   -157.00-107.00   0.50    0.12    --  -84.25 -27.00 -74.00  100
 38  \w   -156.00-102.00   0.50    0.12    --  -84.25 -77.00-150.00  108
 39  \w   -121.00 -95.00   0.50    0.05    --  -49.41-125.00-120.00   52
 40  \w   -118.00 -87.00   0.50    0.05    --  -49.41-125.00  60.00   62
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0190803000
_diffrn_orient_matrix_UB_12      0.1051427000
_diffrn_orient_matrix_UB_13      0.0374362000
_diffrn_orient_matrix_UB_21      0.1546500000
_diffrn_orient_matrix_UB_22      0.0133362000
_diffrn_orient_matrix_UB_23      0.0044711000
_diffrn_orient_matrix_UB_31      -0.0219260000
_diffrn_orient_matrix_UB_32      0.0300051000
_diffrn_orient_matrix_UB_33      -0.1004663000
_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  0.0335
_diffrn_reflns_av_unetI/netI     0.0303
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            25894
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        67.078
_diffrn_reflns_theta_max         67.078
_diffrn_reflns_theta_min         3.078
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    3.811
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.447
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.53a (Rigaku Oxford Diffraction, 2022)
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            colorless
_exptl_crystal_density_diffrn    1.365
_exptl_crystal_description       block
_exptl_crystal_F_000             880
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.13
_refine_diff_density_max         1.269
_refine_diff_density_min         -0.961
_refine_diff_density_rms         0.067
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     467
_refine_ls_number_reflns         7326
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.0383
_refine_ls_R_factor_gt           0.0362
_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^)+(0.0453P)^2^+2.4368P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0942
_refine_ls_wR_factor_ref         0.0957
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6843
_reflns_number_total             7326
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt02113k2.cif
_cod_data_source_block           2b_triclinic
_cod_database_code               7713648
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C37 H52 S1 O4 F3 As1'
_chemical_oxdiff_usercomment     AG0006
_shelx_estimated_absorpt_t_max   0.637
_shelx_estimated_absorpt_t_min   0.474
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 O1-H1
 0.84 with sigma of 0.02
3.a Ternary CH refined with riding coordinates:
 C37(H37), C38(H38), C28(H28), C27(H27), C18(H18), C17(H17), C01D(H01D)
3.b Aromatic/amide H refined with riding coordinates:
 C23(H23), C15(H15), C24(H24), C25(H25), C13(H13), C33(H33), C14(H14),
 C34(H34), C35(H35)
3.c Idealised Me refined as rotating group:
 C382(H38A,H38B,H38C), C381(H38D,H38E,H38F), C371(H37A,H37B,H37C), C281(H28A,
 H28B,H28C), C181(H18A,H18B,H18C), C171(H17A,H17B,H17C), C271(H27A,H27B,H27C),
 C272(H27D,H27E,H27F), C282(H28D,H28E,H28F), C372(H37D,H37E,H37F), C172(H17D,
 H17E,H17F), C182(H18D,H18E,H18F)
;
_shelx_res_checksum              33503
_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 1.620
_oxdiff_exptl_absorpt_empirical_full_min 0.764