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_7713647
_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 O Sb, C6 H4 N O3, C6 H5 N O3'
_chemical_formula_sum            'C48 H61 N2 O7 Sb'
_chemical_formula_weight         899.788
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_Int_Tables_number      14
_atom_sites_solution_primary     dual
_audit_creation_date             2022-07-16
_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                90
_cell_angle_beta                 101.383(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.7304(3)
_cell_length_b                   18.4840(3)
_cell_length_c                   15.7610(3)
_cell_measurement_reflns_used    36643
_cell_measurement_temperature    100.00(13)
_cell_measurement_theta_max      38.2580
_cell_measurement_theta_min      2.5370
_cell_volume                     4492.54(14)
_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)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(13)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.9779
_diffrn_measured_fraction_theta_max 0.9764
_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    -49.00  -9.00   0.50   27.30    --  -25.02 -61.00 -69.00   80
  2  \w     26.00  94.00   0.50   27.30    --   25.02  61.00  69.00  136
  3  \w    -47.00  21.00   0.50   27.30    --   25.02 -61.00 -69.00  136
  4  \w    -59.00 -14.00   0.50   27.30    --  -25.02 -57.00  90.00   90
  5  \w    -34.00   5.00   0.50   27.30    --   25.02 -19.00 120.00   78
  6  \w    -32.00  -6.00   0.50   27.30    --   25.02 -19.00 150.00   52
  7  \w    -47.00  -5.00   0.50   27.30    --   25.02 -19.00   0.00   84
  8  \w     19.00  60.00   0.50   27.30    --   25.02  57.00-150.00   82
;
_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      0.0133499000
_diffrn_orient_matrix_UB_12      0.0258761000
_diffrn_orient_matrix_UB_13      -0.0279217000
_diffrn_orient_matrix_UB_21      -0.0340604000
_diffrn_orient_matrix_UB_22      -0.0112002000
_diffrn_orient_matrix_UB_23      -0.0340100000
_diffrn_orient_matrix_UB_31      -0.0279149000
_diffrn_orient_matrix_UB_32      0.0259984000
_diffrn_orient_matrix_UB_33      0.0131569000
_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  0.0412
_diffrn_reflns_av_unetI/netI     0.0473
_diffrn_reflns_Laue_measured_fraction_full 0.9779
_diffrn_reflns_Laue_measured_fraction_max 0.9764
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            69536
_diffrn_reflns_point_group_measured_fraction_full 0.9779
_diffrn_reflns_point_group_measured_fraction_max 0.9764
_diffrn_reflns_theta_full        25.2417
_diffrn_reflns_theta_max         33.73
_diffrn_reflns_theta_min         2.32
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.666
_exptl_absorpt_correction_T_max  0.99616
_exptl_absorpt_correction_T_min  0.99616
_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    1.330
_exptl_crystal_description       sphere
_exptl_crystal_F_000             1878.698
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.1
_exptl_crystal_size_rad          0.068
_refine_diff_density_max         1.6238
_refine_diff_density_min         -0.5310
_refine_diff_density_rms         0.1009
_refine_ls_d_res_high            0.6400
_refine_ls_d_res_low             8.7782
_refine_ls_goodness_of_fit_ref   1.0040
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    61
_refine_ls_number_parameters     706
_refine_ls_number_reflns         17515
_refine_ls_number_restraints     69
_refine_ls_restrained_S_all      1.0020
_refine_ls_R_factor_all          0.0362
_refine_ls_R_factor_gt           0.0255
_refine_ls_shift/su_max          0.0008
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0129P)^2^+0.7501P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0471
_refine_ls_wR_factor_ref         0.0496
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              15
_reflns_limit_h_min              -24
_reflns_limit_k_max              28
_reflns_limit_k_min              0
_reflns_limit_l_max              24
_reflns_limit_l_min              -15
_reflns_number_gt                14446
_reflns_number_total             17515
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            d3dt02113k2.cif
_cod_data_source_block           6_p-nitrophenol
_cod_original_sg_symbol_Hall     '-P 2ybc (x-z,y,z)'
_cod_database_code               7713647
_chemical_oxdiff_formula         'C48 H61 N2 O7'
_chemical_oxdiff_usercomment     'Dipp3SbOH PNP2'
_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, All O(H) groups
2. Restrained distances
 C172-H17D
 1.08 with sigma of 0.02
 C181-H18B
 1.08 with sigma of 0.02
 C281-H28A
 1.08 with sigma of 0.02
 C281-H28B
 1.08 with sigma of 0.02
 C281-H28C
 1.08 with sigma of 0.02
 C282-H28D
 1.08 with sigma of 0.02
 C282-H28E
 1.08 with sigma of 0.01
 C282-H28F
 1.08 with sigma of 0.02
 C372-H37F
 1.08 with sigma of 0.02
 C28-H28
 1.08 with sigma of 0.02
 C42-H42 \\sim C43-H43 \\sim C45-H45 \\sim C45-H45
 with sigma of 0.02
 C52-H52 \\sim C53-H53 \\sim C55-H55 \\sim C55-H55
 with sigma of 0.02
 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 0.02
 C17-H17 \\sim C27-H27 \\sim C37-H37 \\sim C18-H18 \\sim C28-H28 \\sim C38-H38
 with sigma of 0.02
 C171-H17A \\sim C171-H17B \\sim C171-H17C \\sim C172-H17D \\sim C172-H17E
\\sim C172-H17F
 with sigma of 0.02
 C181-H18A \\sim C181-H18B \\sim C181-H18C \\sim C182-H18D \\sim C182-H18E
\\sim C182-H18F
 with sigma of 0.02
 C271-H27A \\sim C271-H27B \\sim C271-H27C \\sim C272-H27D \\sim C272-H27E
\\sim C272-H27F
 with sigma of 0.02
 C281-H28A \\sim C281-H28B \\sim C281-H28C \\sim C282-H28D \\sim C282-H28E
\\sim C282-H28F
 with sigma of 0.02
 C371-H37A \\sim C371-H37B \\sim C371-H37C \\sim C372-H37D \\sim C372-H37E
\\sim C372-H37F
 with sigma of 0.02
 C381-H38A \\sim C381-H38B \\sim C381-H38C \\sim C382-H38D \\sim C382-H38E
\\sim C382-H38F
 with sigma of 0.02
;
_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 1.522
_oxdiff_exptl_absorpt_empirical_full_min 0.625