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_7010667
_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_moiety         'C19 H35 B10 N O2 Si,(C5 H12)1.5'
_chemical_formula_sum            'C26.5 H53 B10 N O2 Si'
_chemical_formula_weight         553.89
_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                101.58(1)
_cell_angle_beta                 90.07(1)
_cell_angle_gamma                96.13(1)
_cell_formula_units_Z            4
_cell_length_a                   14.448(1)
_cell_length_b                   14.680(1)
_cell_length_c                   16.137(1)
_cell_measurement_reflns_used    950
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      22.0
_cell_measurement_theta_min      12.0
_cell_volume                     3332.9(4)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_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      120(2)
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'SMART 1K CCD area detector'
_diffrn_measurement_method       '\w scans'
_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  0.0454
_diffrn_reflns_av_sigmaI/netI    0.0565
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            37934
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.5
_diffrn_reflns_theta_min         1.7
_diffrn_standards_decay_%        0.4
_diffrn_standards_interval_count 'not measured'
_diffrn_standards_number         'not measured'
_exptl_absorpt_coefficient_mu    0.096
_exptl_absorpt_correction_T_max  0.9627
_exptl_absorpt_correction_T_min  0.9447
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.104
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1196
_exptl_crystal_size_max          0.6
_exptl_crystal_size_mid          0.5
_exptl_crystal_size_min          0.4
_refine_diff_density_max         0.788
_refine_diff_density_min         -0.524
_refine_diff_density_rms         0.091
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     722
_refine_ls_number_reflns         15202
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.1319
_refine_ls_R_factor_gt           0.0835
_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^)+(0.1494P)^2^+2.6177P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2354
_refine_ls_wR_factor_ref         0.2750
_reflns_number_gt                9555
_reflns_number_total             15202
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b102009i.txt
_cod_data_source_block           7b
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_sg_symbol_H-M      P-1
_cod_original_formula_sum        'C26.50 H53 B10 N O2 Si'
_cod_database_code               7010667