Unprecedented formation of polycyclic diazadiborepine derivatives through cage deboronation of m-carborane
Nicole Harmgarth; Cristian G. Hrib; Volker Lorenz; Liane Hilfert; Frank T. Edelmann; Chem.Commun. 50 (2014) 13239–; doi:10.1039/C4cc06261B

data_7115853
_publ_section_title
;
 Unprecedented formation of polycyclic diazadiborepine derivatives through
 cage deboronation of m-carborane
;
_journal_name_full               Chem.Commun.
_journal_page_first              13239
_journal_paper_doi               10.1039/C4cc06261B
_journal_volume                  50
_journal_year                    2014
_chemical_formula_sum            'C24 H59 B10 Li N4 O2'
_chemical_formula_weight         550.79
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 96.55(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.379(3)
_cell_length_b                   18.730(4)
_cell_length_c                   14.184(3)
_cell_measurement_reflns_used    52723
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      29.58
_cell_measurement_theta_min      2.18
_cell_volume                     3531.1(13)
_computing_cell_refinement       'STOE X-AREA'
_computing_data_collection       'STOE X-AREA'
_computing_data_reduction        'STOE X-RED'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      153(2)
_diffrn_detector_area_resol_mean 6.67
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'STOE IPDS 2T'
_diffrn_measurement_method       'rotation method'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0935
_diffrn_reflns_av_sigmaI/netI    0.0595
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            41812
_diffrn_reflns_theta_full        28.28
_diffrn_reflns_theta_max         28.28
_diffrn_reflns_theta_min         2.22
_exptl_absorpt_coefficient_mu    0.059
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.036
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1200
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.54
_exptl_crystal_size_min          0.36
_refine_diff_density_max         0.625
_refine_diff_density_min         -0.342
_refine_diff_density_rms         0.050
_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     426
_refine_ls_number_reflns         8744
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.118
_refine_ls_R_factor_all          0.0936
_refine_ls_R_factor_gt           0.0661
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1678
_refine_ls_wR_factor_ref         0.1805
_reflns_number_gt                6410
_reflns_number_total             8744
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c4cc06261b2.cif
_cod_data_source_block           ip366
_cod_original_cell_volume        3531.0(12)
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               7115853