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_7713649
_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         'C42 H56 N O4 Sb'
_chemical_formula_sum            'C42 H56 N O4 Sb'
_chemical_formula_weight         760.677
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_Int_Tables_number      2
_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                87.478(2)
_cell_angle_beta                 77.760(2)
_cell_angle_gamma                83.096(2)
_cell_formula_units_Z            2
_cell_length_a                   9.8747(2)
_cell_length_b                   12.6935(3)
_cell_length_c                   15.4719(3)
_cell_measurement_reflns_used    34167
_cell_measurement_temperature    99.95(17)
_cell_measurement_theta_max      38.1740
_cell_measurement_theta_min      2.1520
_cell_volume                     1881.15(7)
_computing_cell_refinement       'CrysAlisPro 1.171.41.122a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.122a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.122a (Rigaku OD, 2021)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine 1.5 (Bourhis et al., 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      99.95(17)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.9996
_diffrn_measured_fraction_theta_max 0.9993
_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     23.00  80.00   0.50   10.84    --   25.02-142.00-177.00  114
  2  \w     24.00  75.00   0.50   10.84    --   25.02-129.00  -6.00  102
  3  \w    -68.00 -42.00   0.50   10.84    --  -25.02 118.00 -47.29   52
  4  \w    -30.00  -4.00   0.50   10.84    --  -25.02  38.00  60.00   52
  5  \w    -13.00  48.00   0.50   10.84    --  -25.02  38.00 -60.00  122
  6  \w    -33.00  -8.00   0.50   10.84    --  -25.02 -69.00 -99.70   50
  7  \w    -59.00 -11.00   0.50   10.84    --  -25.02 -57.00 150.00   96
  8  \w    -30.00  -5.00   0.50   10.84    --  -25.02 -73.00 -59.90   50
  9  \w     53.00  92.00   0.50   10.84    --   25.02 178.00 120.00   78
 10  \w      4.00  29.00   0.50   10.84    --   25.02  73.00 124.46   50
 11  \w    -48.00  22.00   0.50   10.84    --   25.02 -38.00  90.00  140
 12  \w      5.00  30.00   0.50   10.84    --   25.02  70.00 -46.55   50
 13  \w    -25.00   2.00   0.50   10.84    --   25.02 -19.00 -60.00   54
 14  \w      4.00  29.00   0.50   10.84    --   25.02  73.00 167.85   50
 15  \w    -31.00   5.00   0.50   10.84    --   25.02 -19.00 -30.00   72
 16  \w     30.00  58.00   0.50   10.84    --   25.02  57.00  30.00   56
 17  \w      4.00  29.00   0.50   10.84    --   25.02  73.00 -98.81   50
 18  \w      6.00  36.00   0.50   10.84    --   25.02  68.00 -72.95   60
 19  \w      8.00  33.00   0.50   10.84    --   25.02  70.00-137.89   50
 20  \w    -48.00  23.00   0.50   10.84    --   25.02 -38.00-150.00  142
 21  \w      8.00  33.00   0.50   10.84    --   25.02  70.00  73.21   50
 22  \w      5.00  32.00   0.50   10.84    --   25.02  71.00 -99.05   54
;
_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      0.0215189000
_diffrn_orient_matrix_UB_12      0.0280334000
_diffrn_orient_matrix_UB_13      -0.0403049000
_diffrn_orient_matrix_UB_21      -0.0125665000
_diffrn_orient_matrix_UB_22      -0.0429569000
_diffrn_orient_matrix_UB_23      -0.0239137000
_diffrn_orient_matrix_UB_31      -0.0696558000
_diffrn_orient_matrix_UB_32      0.0232003000
_diffrn_orient_matrix_UB_33      0.0022489000
_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  0.0515
_diffrn_reflns_av_unetI/netI     0.0603
_diffrn_reflns_Laue_measured_fraction_full 0.9996
_diffrn_reflns_Laue_measured_fraction_max 0.9993
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            62483
_diffrn_reflns_point_group_measured_fraction_full 0.9996
_diffrn_reflns_point_group_measured_fraction_max 0.9993
_diffrn_reflns_theta_full        25.2417
_diffrn_reflns_theta_max         33.73
_diffrn_reflns_theta_min         2.08
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.775
_exptl_absorpt_correction_T_max  0.99699
_exptl_absorpt_correction_T_min  0.99699
_exptl_absorpt_correction_type   sphere
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.122a (Rigaku Oxford Diffraction, 2021)
Spherical absorption correction
using equivalent radius and absorption coefficient.
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.343
_exptl_crystal_description       sphere
_exptl_crystal_F_000             795.225
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.06
_exptl_crystal_size_rad          0.053
_refine_diff_density_max         1.0393
_refine_diff_density_min         -0.5747
_refine_diff_density_rms         0.1179
_refine_ls_d_res_high            0.6400
_refine_ls_d_res_low             9.7707
_refine_ls_goodness_of_fit_ref   0.9511
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    56
_refine_ls_number_parameters     601
_refine_ls_number_reflns         15034
_refine_ls_number_restraints     55
_refine_ls_restrained_S_all      0.9493
_refine_ls_R_factor_all          0.0341
_refine_ls_R_factor_gt           0.0276
_refine_ls_shift/su_max          -0.0020
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+1.0209P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0488
_refine_ls_wR_factor_ref         0.0535
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              15
_reflns_limit_h_min              -14
_reflns_limit_k_max              19
_reflns_limit_k_min              -19
_reflns_limit_l_max              24
_reflns_limit_l_min              0
_reflns_number_gt                13292
_reflns_number_total             15034
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            d3dt02113k2.cif
_cod_data_source_block           6
_cod_database_code               7713649
_chemical_oxdiff_formula         'C42 H56 N1 O4'
_chemical_oxdiff_usercomment     'Dipp3SbOH PNP'
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All O(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C17-H17 \\sim C27-H27 \\sim C37-H37
 with sigma of 0.005
 C18-H18 \\sim C28-H28 \\sim C38-H38
 with sigma of 0.005
 C13-H13 \\sim C14-H14 \\sim C15-H15 \\sim C23-H23 \\sim C24-H24 \\sim C25-H25
\\sim C33-H33 \\sim C34-H34
 \\sim C35-H35
 with sigma of 0.01
 C42-H42 \\sim C43-H43 \\sim C45-H45 \\sim C46-H46
 with sigma of 0.01
 C171-H17d \\sim C171-H17e \\sim C171-H17f \\sim C172-H17a \\sim C172-H17b
\\sim C172-H17c \\sim C181-
 H18a \\sim C181-H18b \\sim C181-H18c \\sim C182-H18d \\sim C182-H18e \\sim
C182-H18f \\sim C271-H27a ~
 C271-H27b \\sim C271-H27c \\sim C272-H27d \\sim C272-H27e \\sim C272-H27f
\\sim C281-H28d \\sim C281-
 H28e \\sim C281-H28f \\sim C282-H28a \\sim C282-H28b \\sim C282-H28c \\sim
C371-H37d \\sim C371-H37e ~
 C371-H37f \\sim C372-H37a \\sim C372-H37b \\sim C372-H37c \\sim C381-H38d
\\sim C381-H38e \\sim C381-
 H38f \\sim C382-H38a \\sim C382-H38b \\sim C382-H38c
 with sigma of 0.01
;
_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 1.640
_oxdiff_exptl_absorpt_empirical_full_min 0.631