From Oxygen Atom Transfer by Stibine Oxide to Hydroxoantimony Formation via Lewis Acid Capture
NGUYEN, THIEN; González-Ortiz, Francisca; Camaret, Ethan; PARK, GYEONGJIN; Chemical Communications  (2026) –; doi:10.1039/D5CC06702B

data_7135317
_publ_section_title
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 From Oxygen Atom Transfer by Stibine Oxide to Hydroxoantimony Formation
 via Lewis Acid Capture
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_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/D5CC06702B
_journal_year                    2026
_chemical_formula_moiety         'C30 H11 B F15 O Sb, 0.5(C7 H8)'
_chemical_formula_sum            'C33.5 H15 B F15 O Sb'
_chemical_formula_weight         851.01
_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'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2025-12-05
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2025-12-05 deposited with the CCDC.	2025-12-08 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 99.943(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.1599(10)
_cell_length_b                   15.9561(15)
_cell_length_c                   19.0317(18)
_cell_measurement_reflns_used    9608
_cell_measurement_temperature    100.00
_cell_measurement_theta_max      30.489
_cell_measurement_theta_min      2.487
_cell_volume                     3038.9(5)
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_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_temperature      100.00
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'APEX II'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0193
_diffrn_reflns_av_unetI/netI     0.0098
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            82622
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.130
_diffrn_reflns_theta_min         2.775
_exptl_absorpt_coefficient_mu    1.030
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.6543
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0579 before and 0.0422 after correction.
The Ratio of minimum to maximum transmission is 0.8770.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.860
_exptl_crystal_description       block
_exptl_crystal_F_000             1660
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.286
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.473
_refine_diff_density_min         -0.680
_refine_diff_density_rms         0.067
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.112
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     500
_refine_ls_number_reflns         8139
_refine_ls_number_restraints     126
_refine_ls_restrained_S_all      1.114
_refine_ls_R_factor_all          0.0249
_refine_ls_R_factor_gt           0.0219
_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^)+(0.0173P)^2^+3.4164P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0513
_refine_ls_wR_factor_ref         0.0538
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7572
_reflns_number_total             8139
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5cc06702b2.cif
_cod_data_source_block           jp016_a
_cod_original_formula_sum        'C33.50 H15 B F15 O Sb'
_cod_database_code               7135317
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.861
_shelx_estimated_absorpt_t_min   0.747
_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
 O1-H1
 0.87 with sigma of 0.01
 C37-C36 = C37-C32
 2.52 with sigma of 0.04
 C31-C35
 2.42 with sigma of 0.04
 C31-C33
 2.41 with sigma of 0.04
 C36-C34
 2.39 with sigma of 0.04
 C35-C33 = C34-C32
 2.4 with sigma of 0.04
 C31-C36 \\sim C36-C35 \\sim C35-C34 \\sim C34-C33 \\sim C33-C32 \\sim C32-C31
 with sigma of 0.02
 C31-C33 \\sim C31-C35 \\sim C32-C34 \\sim C36-C32 \\sim C35-C33 \\sim C36-C34
 with sigma of 0.04
 C37-C32 \\sim C37-C36
 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
C31 \\sim C32 \\sim C33 \\sim C34 \\sim C35 \\sim C36 \\sim C37: within 2A with
sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A
4. Rigid body (RIGU) restrains
 C31, C32, C33, C34, C35, C36, C37
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Fixed Sof: C31(0.5) C32(0.5) H32(0.5) C33(0.5) H33(0.5) C34(0.5) H34(0.5)
 C35(0.5) H35(0.5) C36(0.5) H36(0.5) C37(0.5) H37A(0.5) H37B(0.5) H37C(0.5)
6.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C6(H6), C8(H8), C9(H9), C10(H10), C11(H11),
 C12(H12), C32(H32), C33(H33), C34(H34), C35(H35), C36(H36)
6.b Idealised Me refined as rotating group:
 C37(H37A,H37B,H37C)
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_shelx_res_checksum              57258
_olex2_submission_special_instructions 'No special instructions were received'