Syntheses and Properties of Triborane(5) Possessing Bulky Diamino Substituents on Terminal Boron Atoms
Yumi Hayashi; Yasutomo Segawa; Makoto Yamashita; Kyoko Nozaki; Chem.Commun. 47 (2011) 5888–; doi:10.1039/c1cc11334h

data_7106408
_publ_section_title
;
 Syntheses and Properties of Triborane(5) Possessing Bulky Diamino
 Substituents on Terminal Boron Atoms
;
_journal_name_full               Chem.Commun.
_journal_page_first              5888
_journal_paper_doi               10.1039/c1cc11334h
_journal_volume                  47
_journal_year                    2011
_chemical_formula_sum            'C56 H80 B3 Cl N4 O'
_chemical_formula_weight         893.12
_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                103.183(5)
_cell_angle_beta                 98.129(5)
_cell_angle_gamma                103.201(5)
_cell_formula_units_Z            2
_cell_length_a                   11.478(5)
_cell_length_b                   12.946(6)
_cell_length_c                   19.381(8)
_cell_measurement_reflns_used    7686
_cell_measurement_temperature    103.1500
_cell_measurement_theta_max      27.4835
_cell_measurement_theta_min      3.0222
_cell_volume                     2672(2)
_computing_cell_refinement       'RIGAKU CrystalClear'
_computing_data_collection       'RIGAKU CrystalClear'
_computing_data_reduction        'RIGAKU CrystalClear'
_computing_molecular_graphics    ORTEP-III
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    SIR-97
_diffrn_ambient_temperature      103(2)
_diffrn_detector_area_resol_mean 7.31
_diffrn_measured_fraction_theta_full 0.975
_diffrn_measured_fraction_theta_max 0.975
_diffrn_measurement_device_type  'RIGAKU/MSC Meacury CCD'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71070
_diffrn_reflns_av_R_equivalents  0.0360
_diffrn_reflns_av_sigmaI/netI    0.0623
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            17544
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         3.02
_exptl_absorpt_coefficient_mu    0.112
_exptl_absorpt_correction_T_max  0.9670
_exptl_absorpt_correction_T_min  0.9356
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Jacobson, R. (1998) Private communication'
_exptl_crystal_colour            Yellow
_exptl_crystal_density_diffrn    1.110
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Prism
_exptl_crystal_F_000             968
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.30
_refine_diff_density_max         0.549
_refine_diff_density_min         -0.673
_refine_diff_density_rms         0.064
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.105
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     653
_refine_ls_number_reflns         9187
_refine_ls_number_restraints     298
_refine_ls_restrained_S_all      1.121
_refine_ls_R_factor_all          0.1163
_refine_ls_R_factor_gt           0.0904
_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^)+(0.1194P)^2^+2.7235P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2316
_refine_ls_wR_factor_ref         0.2529
_reflns_number_gt                7053
_reflns_number_total             9187
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c1cc11334h.txt
_cod_data_source_block           3
_cod_original_cell_volume        2672.6(19)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7106408