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_7110563
_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 B9 1-,C6 H20 N4 P 1+'
_chemical_formula_sum            'C8 H32 B9 N4 P'
_chemical_formula_weight         312.64
_chemical_name_systematic
; 
 tris(dimethylamino)phosphiniminium 7,8-dicarba-nido-undecaborane 
;
_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   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 91.88(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.580(2)
_cell_length_b                   13.182(3)
_cell_length_c                   12.385(2)
_cell_measurement_reflns_used    474
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      23
_cell_measurement_theta_min      12
_cell_volume                     1889.5(6)
_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      150(2)
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.984
_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  0.0296
_diffrn_reflns_av_sigmaI/netI    0.0264
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            14804
_diffrn_reflns_theta_full        29.13
_diffrn_reflns_theta_max         29.13
_diffrn_reflns_theta_min         2.26
_diffrn_standards_decay_%        0.2
_diffrn_standards_interval_time  '8 hours'
_diffrn_standards_number         340
_exptl_absorpt_coefficient_mu    0.140
_exptl_absorpt_correction_T_max  0.9726
_exptl_absorpt_correction_T_min  0.9462
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.099
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             672
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.392
_refine_diff_density_min         -0.338
_refine_diff_density_rms         0.043
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.091
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     296
_refine_ls_number_reflns         4992
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.091
_refine_ls_R_factor_all          0.0534
_refine_ls_R_factor_gt           0.0435
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0502P)^2^+0.7894P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1093
_refine_ls_wR_factor_ref         0.1178
_reflns_number_gt                4283
_reflns_number_total             4992
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            903030asup1.cif
_cod_data_source_block           (4)
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               7110563