Catalytic Regioselective Cage B(8)-H Arylation of o-Carboranes via "Cage-Walking" Strategy.
Lyu, Hairong; Zhang, Jie; Yang, Jingting; Quan, Yangjian; Xie, Zuowei; Journal of the American Chemical Society 141 (2019) 4219–4224; doi:10.1021/jacs.9b00302

data_4127480
_publ_section_title
;
 Catalytic Regioselective Cage B(8)-H Arylation of o-Carboranes via
 &quot;Cage-Walking&quot; Strategy.
;
_journal_issue                   10
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              4219
_journal_page_last               4224
_journal_paper_doi               10.1021/jacs.9b00302
_journal_volume                  141
_journal_year                    2019
_chemical_formula_sum            'C21 H29 B10 F3 N4 O4 Pd S'
_chemical_formula_weight         705.04
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/6
_cell_angle_alpha                81.928(8)
_cell_angle_beta                 80.420(9)
_cell_angle_gamma                83.744(9)
_cell_formula_units_Z            2
_cell_length_a                   7.259(2)
_cell_length_b                   13.814(4)
_cell_length_c                   15.014(5)
_cell_measurement_reflns_used    1780
_cell_measurement_temperature    172(2)
_cell_measurement_theta_max      15
_cell_measurement_theta_min      15
_cell_volume                     1464.2(8)
_computing_cell_refinement       'BRUKER D8VENTURE DIFFRACTOMETER'
_computing_data_collection       'BRUKER D8VENTURE DIFFRACTOMETER'
_computing_data_reduction        'BRUKER D8VENTURE DIFFRACTOMETER'
_computing_molecular_graphics    'BRUKER SHELXTL'
_computing_publication_material  'BRUKER SHELXTL'
_computing_structure_refinement  'SHELXL-2014/6 (Sheldrick, 2014)'
_diffrn_ambient_temperature      172(2)
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  'BRUKER D8VENTURE DIFFRACTOMETER'
_diffrn_measurement_method       'PHI & OMEGA SCAN'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0579
_diffrn_reflns_av_unetI/netI     0.0468
_diffrn_reflns_Laue_measured_fraction_full 0.988
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            29002
_diffrn_reflns_point_group_measured_fraction_full 0.988
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.244
_diffrn_reflns_theta_min         2.773
_exptl_absorpt_coefficient_mu    0.762
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.5720
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.599
_exptl_crystal_description       block
_exptl_crystal_F_000             708
_exptl_crystal_size_max          0.500
_exptl_crystal_size_mid          0.400
_exptl_crystal_size_min          0.200
_refine_diff_density_max         2.141
_refine_diff_density_min         -1.991
_refine_diff_density_rms         0.159
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.108
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     397
_refine_ls_number_reflns         5240
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.108
_refine_ls_R_factor_all          0.0873
_refine_ls_R_factor_gt           0.0702
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0337P)^2^+18.8685P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1625
_refine_ls_wR_factor_ref         0.1781
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4461
_reflns_number_total             5240
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja9b00302_si_006.cif
_cod_data_source_block           B&#x0092;
_cod_original_cell_volume        1464.1(8)
_cod_database_code               4127480
_shelx_estimated_absorpt_t_min   0.702
_shelx_estimated_absorpt_t_max   0.862
_shelxl_version_number           2014/6
_shelx_res_checksum              97091
_shelx_hkl_checksum              4807