A Pd-catalyzed route to carborane-fused boron heterocycles.
Zhu, Mengjie; Wang, Puzhao; Wu, Zhengqiu; Zhong, Yangfa; Su, Laiman; Xin, Yuquan; Spokoyny, Alexander M.; Zou, Chao; Mu, Xin; Chemical science 15 (2024) 10392–10401; doi:10.1039/d4sc02214a

data_1571741
_publ_section_title
;
 A Pd-catalyzed route to carborane-fused boron heterocycles.
;
_journal_issue                   27
_journal_name_full               'Chemical science'
_journal_page_first              10392
_journal_page_last               10401
_journal_paper_doi               10.1039/d4sc02214a
_journal_volume                  15
_journal_year                    2024
_chemical_formula_sum            'C31 H46 B12 Cl2 N2 O4'
_chemical_formula_weight         711.32
_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_method           SHELXL-2013
_audit_update_record
;
2024-05-07 deposited with the CCDC.	2024-05-28 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 103.7720(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.2799(2)
_cell_length_b                   29.3893(6)
_cell_length_c                   13.7124(3)
_cell_measurement_reflns_used    9321
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      140.429
_cell_measurement_theta_min      6.015
_cell_volume                     4023.68(14)
_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-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.947
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0819
_diffrn_reflns_av_unetI/netI     0.0540
_diffrn_reflns_Laue_measured_fraction_full 0.947
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       34
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            37765
_diffrn_reflns_point_group_measured_fraction_full 0.947
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         65.499
_diffrn_reflns_theta_min         3.007
_exptl_absorpt_coefficient_mu    1.725
_exptl_absorpt_correction_T_max  0.7533
_exptl_absorpt_correction_T_min  0.4988
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.174
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             1488
_exptl_crystal_size_max          0.170
_exptl_crystal_size_mid          0.140
_exptl_crystal_size_min          0.110
_refine_diff_density_max         0.400
_refine_diff_density_min         -0.446
_refine_diff_density_rms         0.053
_refine_ls_extinction_coef       0.0085(15)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     561
_refine_ls_number_reflns         6894
_refine_ls_number_restraints     93
_refine_ls_restrained_S_all      1.119
_refine_ls_R_factor_all          0.1168
_refine_ls_R_factor_gt           0.0944
_refine_ls_shift/su_max          0.025
_refine_ls_shift/su_mean         0.004
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1734P)^2^+1.8010P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2632
_refine_ls_wR_factor_ref         0.2951
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5023
_reflns_number_total             6894
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4sc02214a2.cif
_cod_data_source_block           cu_d8v23466_0m
_cod_depositor_comments
'Adding full bibliography for 1571739--1571749.cif.'
_cod_original_cell_volume        4023.67(14)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               1571741
_shelx_estimated_absorpt_t_min   0.758
_shelx_estimated_absorpt_t_max   0.833
_shelxl_version_number           2013-4
_shelx_res_checksum              86336