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_7115854
_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            'C32 H65 B10 Li N4 O2'
_chemical_formula_weight         652.92
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                91.5720(10)
_cell_angle_beta                 90.3580(10)
_cell_angle_gamma                109.925(2)
_cell_formula_units_Z            4
_cell_length_a                   10.7877(2)
_cell_length_b                   12.0470(2)
_cell_length_c                   36.7599(3)
_cell_measurement_reflns_used    122680
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      75.6770
_cell_measurement_theta_min      3.8920
_cell_volume                     4489.02(13)
_computing_cell_refinement
; 
CrysAlisPro, Agilent Technologies, 
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET) 
(compiled Feb  1 2013,16:14:44) 
;
_computing_data_collection
; 
CrysAlisPro, Agilent Technologies, 
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET) 
(compiled Feb  1 2013,16:14:44) 
;
_computing_data_reduction
; 
CrysAlisPro, Agilent Technologies, 
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET) 
(compiled Feb  1 2013,16:14:44) 
;
_computing_molecular_graphics    'Bruker XP'
_computing_publication_material  SHELXL-97
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 10.3543
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Xcalibur, Atlas, Nova'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0517
_diffrn_reflns_av_sigmaI/netI    0.0166
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       46
_diffrn_reflns_limit_l_min       -46
_diffrn_reflns_number            324886
_diffrn_reflns_theta_full        75.87
_diffrn_reflns_theta_max         75.87
_diffrn_reflns_theta_min         3.61
_exptl_absorpt_coefficient_mu    0.413
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.77413
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
CrysAlisPro, Agilent Technologies, 
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET) 
(compiled Feb  1 2013,16:14:44) 
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    0.966
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1416
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.545
_refine_diff_density_min         -0.546
_refine_diff_density_rms         0.043
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     995
_refine_ls_number_reflns         18627
_refine_ls_number_restraints     83
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.0518
_refine_ls_R_factor_gt           0.0477
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0579P)^2^+2.1882P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1220
_refine_ls_wR_factor_ref         0.1256
_reflns_number_gt                17223
_reflns_number_total             18627
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c4cc06261b2.cif
_cod_data_source_block           magd90
_cod_original_cell_volume        4489.01(12)
_cod_database_code               7115854