Transition metal-mediated B(4)-H hydroxylation/halogenation of o-carboranes bearing a 2-pyridylsulfenyl ligand.
Guo, Shu-Ting; Cui, Peng-Fei; Yuan, Run-Ze; Jin, Guo-Xin; Chemical communications (Cambridge, England) 57 (2021) 2412–2415; doi:10.1039/d0cc08290b

data_7127876
_publ_section_title
;
 Transition metal-mediated B(4)-H hydroxylation/halogenation of
 o-carboranes bearing a 2-pyridylsulfenyl ligand.
;
_journal_issue                   19
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              2412
_journal_page_last               2415
_journal_paper_doi               10.1039/d0cc08290b
_journal_volume                  57
_journal_year                    2021
_chemical_formula_moiety         'C8 H16 B10 Br N S'
_chemical_formula_sum            'C8 H16 B10 Br N S'
_chemical_formula_weight         346.29
_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
_audit_creation_date             2020-10-18
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_audit_update_record
;
2020-10-18 deposited with the CCDC.	2021-01-29 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.880(3)
_cell_length_b                   12.558(3)
_cell_length_c                   14.122(3)
_cell_measurement_reflns_used    4710
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      56.64
_cell_measurement_theta_min      4.10
_cell_volume                     1574.8(7)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      200.01
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           GaK\a
_diffrn_radiation_wavelength     1.34138
_diffrn_reflns_av_R_equivalents  0.0606
_diffrn_reflns_av_unetI/netI     0.0582
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            10415
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        53.594
_diffrn_reflns_theta_max         55.948
_diffrn_reflns_theta_min         5.119
_exptl_absorpt_coefficient_mu    3.121
_exptl_absorpt_correction_T_max  0.7512
_exptl_absorpt_correction_T_min  0.4961
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1441 before and 0.0725 after correction.
The Ratio of minimum to maximum transmission is 0.6604.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.461
_exptl_crystal_description       block
_exptl_crystal_F_000             688
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.054
_refine_diff_density_min         -0.362
_refine_diff_density_rms         0.090
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.51(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     192
_refine_ls_number_reflns         3089
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.022
_refine_ls_R_factor_all          0.0550
_refine_ls_R_factor_gt           0.0417
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0660P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1030
_refine_ls_wR_factor_ref         0.1088
_reflns_Friedel_coverage         0.738
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                2618
_reflns_number_total             3089
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0cc08290b2.cif
_cod_data_source_block           200927c_0m_a
_cod_depositor_comments
'Adding full bibliography for 7127874--7127881.cif.'
_cod_original_cell_volume        1574.7(7)
_cod_database_code               7127876
_shelx_estimated_absorpt_t_max   0.788
_shelx_estimated_absorpt_t_min   0.706
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.49(5) 0.51(5)
2. Fixed Uiso
 At 1.2 times of:
  All B(H) groups, All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3.a Aromatic/amide H refined with riding coordinates:
 C5(H5A), C6(H6A), C7(H7A), C8(H8A)
3.b Idealised Me refined as rotating group:
 C3(H3A,H3B,H3C)
3.c Boron cage BH refined with riding coordinates:
 B3(H3), B5(H5), B6(H6), B7(H7), B8(H8), B9(H9), B10(H10), B11(H11), B12(H12)
;
_shelx_res_checksum              90046
_shelx_shelxl_version_number     2016/6
_olex2_submission_special_instructions 'No special instructions were received'