Deboronation of ortho-carborane by an iminophosphorane: crystal structures of the novel carborane adduct nido-C2B10H12·HNP(NMe2)3 and the borenium salt [(Me2N)3PNHBNP(NMe2)3]2O2+(C2B9H12−)2
Davidson, Matthew G.; Fox, Mark A.; Hibbert, Thomas G.; Howard, Judith A. K.; Mackinnon, Angus; Neretin, Ivan S.; Wade, Kenneth; Chemical Communications  (1999) 1649–; doi:10.1039/a903030a

data_7110562
_publ_section_title
;
 Deboronation of ortho-carborane by an iminophosphorane: crystal
 structures of the novel carborane adduct nido-C2B10H12&#x00B7;HNP(NMe2)3
 and the borenium salt [(Me2N)3PNHBNP(NMe2)3]2O2+(C2B9H12&#x2212;)2
;
_journal_issue                   17
_journal_name_full               'Chemical Communications'
_journal_page_first              1649
_journal_paper_doi               10.1039/a903030a
_journal_year                    1999
_chemical_formula_moiety         'C2 H12 B10,C6 H19 N4 P'
_chemical_formula_sum            'C8 H31 B10 N4 P'
_chemical_formula_weight         322.44
_chemical_name_common
'1,2-dicarbadodecaborane-imino-tris(dimethylamino)phosphorane adduct'
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   10.799(2)
_cell_length_b                   17.252(4)
_cell_length_c                   20.326(4)
_cell_measurement_temperature    153(2)
_cell_volume                     3786.8(13)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    SHELXTL
_computing_publication_material  SHELXTL
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      153(2)
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.1712
_diffrn_reflns_av_sigmaI/netI    0.1165
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            25525
_diffrn_reflns_theta_full        27.49
_diffrn_reflns_theta_max         27.49
_diffrn_reflns_theta_min         2.00
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    0.141
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.131
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1376
_refine_diff_density_max         0.450
_refine_diff_density_min         -0.406
_refine_diff_density_rms         0.072
_refine_ls_extinction_coef       0.0006(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     267
_refine_ls_number_reflns         4337
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.053
_refine_ls_R_factor_all          0.1681
_refine_ls_R_factor_gt           0.0766
_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^)+(0.0561P)^2^+4.3755P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1457
_refine_ls_wR_factor_ref         0.1873
_reflns_number_gt                2221
_reflns_number_total             4337
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            903030asup1.cif
_cod_data_source_block           (3)
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Orthorhombic' changed to
'orthorhombic' according to
/home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named
'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 
;
_cod_original_cell_volume        3786.9(13)
_cod_original_sg_symbol_H-M      Pbca
_cod_database_code               7110562