The Molecular Structure of (PSH^+^)(nido-7,8-C~2~B~9~H~12~^-^) Determined by Neutron Diffraction (PS = Proton Sponge, 1,8-Bis(dimethylamino)naphthalene)
Mark A. Fox; Andrés E. Goeta; Judith A. K. Howard; Andrew K. Hughes; Andrew L. Johnson; Dave A. Keen; Ken Wade; Chick C. Wilson; Inorganic Chemistry 40 (2001) 173–175; doi:10.1021/ic000961e

data_4319136
_publ_contact_author_address
;
    Chemistry Department
    Durham University
    Science Site, South Road.
    DURHAM, DH1 3LE
    UK
;
_publ_contact_author_email       A.K.Hughes@durham.ac.uk
_publ_contact_author_fax         '(44) 191 386 1127'
_publ_contact_author_name
;
Dr. Andrew K Hughes
;
_publ_contact_author_phone       '(44) 191 374 3111'
_publ_section_title
;
 The Molecular Structure of (PSH^+^)(nido-7,8-C~2~B~9~H~12~^-^) Determined
 by Neutron Diffraction (PS = Proton Sponge,
 1,8-Bis(dimethylamino)naphthalene)
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              173
_journal_page_last               175
_journal_paper_doi               10.1021/ic000961e
_journal_volume                  40
_journal_year                    2001
_chemical_formula_sum            'C16 H31 B9 N2'
_chemical_formula_weight         348.72
_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   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                68.524(5)
_cell_angle_beta                 86.359(7)
_cell_angle_gamma                79.712(8)
_cell_formula_units_Z            2
_cell_length_a                   8.129(1)
_cell_length_b                   11.251(2)
_cell_length_c                   12.392(2)
_cell_measurement_reflns_used    279
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      20.62
_cell_measurement_theta_min      2.55
_cell_volume                     1037.7(3)
_computing_cell_refinement       'SMART-NT V5.0 (Bruker, 1999a)'
_computing_data_collection       'SMART-NT V5.0 (Bruker, 1999a)'
_computing_data_reduction        'SAINT-NT V5.0 (Bruker, 1999b)'
_computing_molecular_graphics    'SHELXTL-NT V5.1 (Bruker, 1999c)'
_computing_publication_material  'SHELXTL-NT V5.1 (Bruker, 1999c)'
_computing_structure_refinement  'SHELXTL-NT V5.1 (Bruker, 1999c)'
_computing_structure_solution    'SHELXTL-NT V5.1 (Bruker, 1999c)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.0458
_diffrn_reflns_av_sigmaI/netI    0.0444
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            6319
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.77
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    0.058
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.116
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'irregular shape'
_exptl_crystal_F_000             372
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.28
_refine_diff_density_max         0.213
_refine_diff_density_min         -0.221
_refine_diff_density_rms         0.042
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.092
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     368
_refine_ls_number_reflns         3652
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.092
_refine_ls_R_factor_all          0.0811
_refine_ls_R_factor_gt           0.0561
_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^)+(0.0302P)^2^+0.7920P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1178
_refine_ls_wR_factor_ref         0.1284
_reflns_number_gt                2823
_reflns_number_total             3652
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic000961e_2.cif
_cod_data_source_block           98srv012
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
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_cod_database_code               4319136