The synthesis of closo- and nido-(aminoalkyl)dicarbaboranes: a re-examination of contradictory literature reports, crystal structure of [7-{H3N(CH2)3}-7,8-C2B9H11]·NH2NH2†
Batsanov, Andrei S.; Goeta, Andrés E.; Howard, Judith A. K.; Hughes, Andrew K.; Malget, John M.; Journal of the Chemical Society, Dalton Transactions  (2001) 1820–; doi:10.1039/b102009i

data_7010668
_publ_section_title
;
 The synthesis of closo- and nido-(aminoalkyl)dicarbaboranes: a
 re-examination of contradictory literature reports, crystal structure
 of [7-{H3N(CH2)3}-7,8-C2B9H11]&#x00B7;NH2NH2&#x2020;
;
_journal_issue                   12
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              1820
_journal_paper_doi               10.1039/b102009i
_journal_year                    2001
_chemical_formula_sum            'C28 H54 B9 N2 O2'
_chemical_formula_weight         548.02
_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   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 95.638(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.267(3)
_cell_length_b                   17.101(4)
_cell_length_c                   17.462(4)
_cell_measurement_reflns_used    497
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      19.11
_cell_measurement_theta_min      10.14
_cell_volume                     3348.2(14)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.932
_diffrn_measured_fraction_theta_max 0.932
_diffrn_measurement_device_type  'Bruker SMART-CCD'
_diffrn_measurement_method       \w
_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  0.0462
_diffrn_reflns_av_sigmaI/netI    0.0426
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            39997
_diffrn_reflns_theta_full        30.50
_diffrn_reflns_theta_max         30.50
_diffrn_reflns_theta_min         1.67
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    0.062
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_diffrn    1.087
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    .
_exptl_crystal_description       'irregular shape'
_exptl_crystal_F_000             1188
_exptl_crystal_size_max          0.54
_exptl_crystal_size_mid          0.36
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.485
_refine_diff_density_min         -0.215
_refine_diff_density_rms         0.046
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.014
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     590
_refine_ls_number_reflns         9520
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.014
_refine_ls_R_factor_all          0.1186
_refine_ls_R_factor_gt           0.0653
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0920P)^2^+1.2413P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1634
_refine_ls_wR_factor_ref         0.2012
_reflns_number_gt                5619
_reflns_number_total             9520
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b102009i.txt
_cod_data_source_block           8b
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               7010668