The elusive three-coordinate dicationic hydrido boron complex.
Chen, Wen-Ching; Lee, Ching-Yu; Lin, Bo-Chao; Hsu, Yu-Chen; Shen, Jiun-Shian; Hsu, Chao-Ping; Yap, Glenn P. A.; Ong, Tiow-Gan; Journal of the American Chemical Society 136 (2014) 914–917; doi:10.1021/ja4120852

data_4120529
_publ_section_title
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 The elusive three-coordinate dicationic hydrido boron complex.
;
_journal_issue                   3
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              914
_journal_page_last               917
_journal_paper_doi               10.1021/ja4120852
_journal_volume                  136
_journal_year                    2014
_chemical_formula_sum            'C30 H36 Al Cl3 N4'
_chemical_formula_weight         585.96
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 99.887(2)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   34.7075(9)
_cell_length_b                   11.0418(3)
_cell_length_c                   15.8058(4)
_cell_measurement_reflns_used    7575
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.15
_cell_measurement_theta_min      2.28
_cell_volume                     5967.3(3)
_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      100(2)
_diffrn_detector_area_resol_mean 8.33
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.982
_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  0.0423
_diffrn_reflns_av_unetI/netI     0.0623
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.982
_diffrn_reflns_limit_h_max       44
_diffrn_reflns_limit_h_min       -44
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            22267
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.982
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         27.098
_diffrn_reflns_theta_min         1.938
_exptl_absorpt_coefficient_mu    0.363
_exptl_absorpt_correction_T_max  0.9703
_exptl_absorpt_correction_T_min  0.8454
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'APEX2 (Bruker, 2007)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.304
_exptl_crystal_description       plate
_exptl_crystal_F_000             2464
_exptl_crystal_size_max          0.320
_exptl_crystal_size_mid          0.180
_exptl_crystal_size_min          0.080
_refine_diff_density_max         0.459
_refine_diff_density_min         -0.447
_refine_diff_density_rms         0.070
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     388
_refine_ls_number_reflns         6472
_refine_ls_number_restraints     124
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.0917
_refine_ls_R_factor_gt           0.0548
_refine_ls_shift/su_max          0.007
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
; 
 w=1/[\s^2^(Fo^2^)+(0.0810P)^2^+0.4316P] 
 where P=(Fo^2^+2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1379
_refine_ls_wR_factor_ref         0.1558
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4262
_reflns_number_total             6472
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja4120852_si_003.cif
_cod_data_source_block           i14390
_cod_database_code               4120529
_shelx_estimated_absorpt_t_min   0.893
_shelx_estimated_absorpt_t_max   0.972
_shelxl_version_number           2013-2
_shelx_res_checksum              61131
_shelx_hkl_checksum              95026