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_7127875
_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_sum            'C8 H17 B10 N O S'
_chemical_formula_weight         283.38
_space_group_crystal_system      orthorhombic
_space_group_IT_number           33
_space_group_name_Hall           'P 2c -2n'
_space_group_name_H-M_alt        'P n a 21'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2016/6
_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                   13.0313(7)
_cell_length_b                   12.7774(7)
_cell_length_c                   9.0470(4)
_cell_measurement_reflns_used    1305
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      30.74
_cell_measurement_theta_min      4.22
_cell_volume                     1506.38(13)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.996
_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  0.0795
_diffrn_reflns_av_unetI/netI     0.0814
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            10291
_diffrn_reflns_point_group_measured_fraction_full 0.915
_diffrn_reflns_point_group_measured_fraction_max 0.889
_diffrn_reflns_theta_full        53.594
_diffrn_reflns_theta_max         57.051
_diffrn_reflns_theta_min         5.212
_exptl_absorpt_coefficient_mu    1.150
_exptl_absorpt_correction_T_max  0.751
_exptl_absorpt_correction_T_min  0.590
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.250
_exptl_crystal_description       block
_exptl_crystal_F_000             584
_exptl_crystal_size_max          0.370
_exptl_crystal_size_mid          0.140
_exptl_crystal_size_min          0.120
_refine_diff_density_max         0.252
_refine_diff_density_min         -0.295
_refine_diff_density_rms         0.055
_refine_ls_abs_structure_details
; 
 Flack x determined using 745 quotients [(I+)-(I-)]/[(I+)+(I-)] 
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). 
;
_refine_ls_abs_structure_Flack   0.00(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     195
_refine_ls_number_reflns         2745
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.0653
_refine_ls_R_factor_gt           0.0397
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0437P)^2^+0.0594P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0941
_refine_ls_wR_factor_ref         0.1042
_reflns_Friedel_coverage         0.674
_reflns_Friedel_fraction_full    0.821
_reflns_Friedel_fraction_max     0.766
_reflns_number_gt                2282
_reflns_number_total             2745
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0cc08290b2.cif
_cod_data_source_block           ga_90513da_a
_cod_depositor_comments
'Adding full bibliography for 7127874--7127881.cif.'
_cod_database_code               7127875
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_min   0.676
_shelx_estimated_absorpt_t_max   0.874
_shelx_res_checksum              6004