Pd-Catalyzed sequential B(3)-I/B(4)-H bond activation for the synthesis of 3,4-benzo-<i>o</i>-carboranes.
Ge, Yixiu; Zhang, Jie; Qiu, Zaozao; Xie, Zuowei; Dalton transactions (Cambridge, England : 2003) 50 (2021) 1766–1773; doi:10.1039/d0dt03740k

data_7706227
_publ_section_title
;
 Pd-Catalyzed sequential B(3)-I/B(4)-H bond activation for the synthesis
 of 3,4-benzo-<i>o</i>-carboranes.
;
_journal_issue                   5
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              1766
_journal_page_last               1773
_journal_paper_doi               10.1039/d0dt03740k
_journal_volume                  50
_journal_year                    2021
_chemical_formula_moiety         'C16 H22 B10'
_chemical_formula_sum            'C16 H22 B10'
_chemical_formula_weight         322.43
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2020-11-30
_audit_creation_method
;
Olex2 1.3-dev
(compiled 2020.11.05 svn.r80d884aa for OlexSys, GUI svn.r5830)
;
_audit_update_record
;
2020-12-04 deposited with the CCDC.	2020-12-24 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 117.947(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.7334(19)
_cell_length_b                   21.183(4)
_cell_length_c                   10.197(2)
_cell_measurement_reflns_used    2790
_cell_measurement_temperature    130
_cell_measurement_theta_max      28.59
_cell_measurement_theta_min      2.37
_cell_volume                     1857.3(6)
_computing_cell_refinement       'SAINT v7.68A (Bruker, 2009)'
_computing_data_collection       'Bruker APEX DUO'
_computing_data_reduction        'SAINT v7.68A (Bruker, 2009)'
_computing_molecular_graphics    'Olex2 1.3-dev (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3-dev (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      130.0
_diffrn_measured_fraction_theta_full 1.000
_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           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0481
_diffrn_reflns_av_unetI/netI     0.0550
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            18620
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         30.636
_diffrn_reflns_theta_min         1.923
_exptl_absorpt_coefficient_mu    0.057
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.6667
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.1147 before and 0.0472 after correction.
The Ratio of minimum to maximum transmission is 0.8936.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.153
_exptl_crystal_description       prism
_exptl_crystal_F_000             672
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.288
_refine_diff_density_min         -0.196
_refine_diff_density_rms         0.042
_refine_ls_extinction_coef       0.0023(12)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.011
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     271
_refine_ls_number_reflns         5718
_refine_ls_number_restraints     28
_refine_ls_restrained_S_all      1.009
_refine_ls_R_factor_all          0.0890
_refine_ls_R_factor_gt           0.0490
_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^)+(0.0638P)^2^+0.1061P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1147
_refine_ls_wR_factor_ref         0.1332
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3715
_reflns_number_total             5718
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt03740k2.cif
_cod_data_source_block           4a
_cod_depositor_comments
'Adding full bibliography for 7706227--7706229.cif.'
_cod_original_cell_volume        1857.2(6)
_cod_database_code               7706227
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.999
_shelx_estimated_absorpt_t_min   0.993
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All B(H) groups, All C(H) groups
2. Restrained distances
 B9-H9A \\sim B10-H10A \\sim B12-H12A \\sim B11-H11 \\sim B7-H7A \\sim B5-H5
\\sim B4-H4A \\sim B6-H6A
 with sigma of 0.02
3.a Aromatic/amide H refined with riding coordinates:
 C4(H4), C6(H6), C7(H7), C8(H8), C9(H9), C10(H10), C12(H12), C13(H13),
 C14(H14), C15(H15), C16(H16)
;
_shelx_res_checksum              74706
_olex2_submission_special_instructions 'No special instructions were received'