Synthesis and Structural Characterization of 9-Azido-9-Borafluorene: Monomer and Cyclotrimer of a Borole Azide
Sunanda Biswas; Iris M. Oppel; Holger F. Bettinger; Inorganic Chemistry 49 (2010) 4499–4506; doi:10.1021/ic902436s

data_4315565
_publ_contact_author
;
        H. F. Bettinger
        Institut f\"ur Organische Chemie 
        Universit\"at T\"ubingen
        Auf der Morgenstelle 18
        72076 T\"ubingen
        Bundesrepublik Deutschland
;
_publ_contact_author_email       holger.bettinger@uni-tuebingen.de
_publ_contact_author_fax         '049 7071 295244'
_publ_contact_author_phone       '049 7071 2972072'
_publ_section_title
;
 Synthesis and Structural Characterization of 9-Azido-9-Borafluorene:
 Monomer and Cyclotrimer of a Borole Azide
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4499
_journal_page_last               4506
_journal_paper_doi               10.1021/ic902436s
_journal_volume                  49
_journal_year                    2010
_chemical_formula_sum            'C36 H27 B3 O3'
_chemical_formula_weight         540.01
_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                70.466(4)
_cell_angle_beta                 74.187(3)
_cell_angle_gamma                61.449(4)
_cell_formula_units_Z            4
_cell_length_a                   13.0852(5)
_cell_length_b                   13.3035(6)
_cell_length_c                   19.6082(7)
_cell_measurement_reflns_used    10279
_cell_measurement_temperature    108(2)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      3.02
_cell_volume                     2799.4(2)
_computing_cell_refinement       'CrysAlis RED Oxford diffraction'
_computing_data_collection       'CrysAlis CCD Oxford diffraction'
_computing_data_reduction        'CrysAlis RED Oxford diffraction'
_computing_molecular_graphics    SHELXL-97
_computing_publication_material  SHELXL-97
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      108(2)
_diffrn_detector_area_resol_mean 8.4171
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device_type  'Xcalibur^TM^2, Oxford Diffraction'
_diffrn_measurement_method       '560 frames in \w and 15 sec'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0199
_diffrn_reflns_av_sigmaI/netI    0.0498
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            25207
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         3.06
_exptl_absorpt_coefficient_mu    0.078
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.281
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1128
_exptl_crystal_size_max          0.58
_exptl_crystal_size_mid          0.55
_exptl_crystal_size_min          0.23
_refine_diff_density_max         0.305
_refine_diff_density_min         -0.220
_refine_diff_density_rms         0.043
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.882
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     757
_refine_ls_number_reflns         12695
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.882
_refine_ls_R_factor_all          0.0591
_refine_ls_R_factor_gt           0.0360
_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^)+(0.0449P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0789
_refine_ls_wR_factor_ref         0.0821
_reflns_number_gt                8414
_reflns_number_total             12695
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic902436s_si_001_5.cif
_cod_data_source_block           compound-5
_cod_original_cell_volume        2799.41(22)
_cod_database_code               4315565