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_7706229
_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         'C30 H30 B10'
_chemical_formula_sum            'C30 H30 B10'
_chemical_formula_weight         498.64
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2016-05-06
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_audit_update_record
;
2020-12-04 deposited with the CCDC.	2020-12-24 downloaded from the CCDC.
;
_cell_angle_alpha                85.718(2)
_cell_angle_beta                 75.442(2)
_cell_angle_gamma                76.838(2)
_cell_formula_units_Z            4
_cell_length_a                   11.3473(10)
_cell_length_b                   15.2698(14)
_cell_length_c                   17.5705(16)
_cell_measurement_reflns_used    4536
_cell_measurement_temperature    130
_cell_measurement_theta_max      28.61
_cell_measurement_theta_min      2.40
_cell_volume                     2868.8(5)
_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 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      130
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0352
_diffrn_reflns_av_unetI/netI     0.0783
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.985
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            29776
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.985
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.856
_diffrn_reflns_theta_min         1.803
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.060
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.6877
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.0451 before and 0.0387 after correction.
The Ratio of minimum to maximum transmission is 0.9217.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.154
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1040
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.330
_refine_diff_density_min         -0.307
_refine_diff_density_rms         0.051
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.998
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     721
_refine_ls_number_reflns         17777
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.998
_refine_ls_R_factor_all          0.1101
_refine_ls_R_factor_gt           0.0599
_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^)+(0.0661P)^2^+0.2661P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1313
_refine_ls_wR_factor_ref         0.1555
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10748
_reflns_number_total             17777
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt03740k2.cif
_cod_data_source_block           5a
_cod_depositor_comments
'Adding full bibliography for 7706227--7706229.cif.'
_cod_database_code               7706229
_shelx_estimated_absorpt_t_max   0.990
_shelx_estimated_absorpt_t_min   0.985
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All B(H) groups, All C(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C8(H8), C9(H9), C10(H10), C11(H11), C12(H12), C14(H14), C15(H15), C16(H16),
 C17(H17), C18(H18), C20(H20), C21(H21), C22(H22), C23(H23), C24(H24), C26(H26),
  C27(H27), C28(H28), C29(H29), C30(H30), C8A(H8AA), C9A(H9AA), C10A(H10B),
 C11A(H11B), C12A(H12B), C14A(H14A), C15A(H15A), C16A(H16A), C17A(H17A),
 C18A(H18A), C20A(H20A), C21A(H21A), C22A(H22A), C23A(H23A), C24A(H24A),
 C26A(H26A), C27A(H27A), C28A(H28A), C29A(H29A), C30A(H30A)
2.b Boron cage BH refined with riding coordinates:
 C1(H1), C2(H2), B5(H5), B6(H6), B7(H7), B8(H8A), B9(H9A), B10(H10A),
 B11(H11A), B12(H12A), C1A(H1A), C2A(H2A), B5A(H5A), B6A(H6A), B7A(H7A),
 B8A(H8AB), B9A(H9AB), B10A(H10C), B11A(H11C), B12A(H12C)
;
_shelx_res_checksum              71031
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'