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_4319135
_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                68.34(1)
_cell_angle_beta                 86.55(1)
_cell_angle_gamma                79.98(1)
_cell_formula_units_Z            2
_cell_length_a                   8.110(2)
_cell_length_b                   11.134(2)
_cell_length_c                   12.342(2)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    30(1)
_cell_volume                     1019.9(4)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      30(1)
_diffrn_measured_fraction_theta_full 0.292
_diffrn_measured_fraction_theta_max 0.292
_diffrn_measurement_device       SXD
_diffrn_measurement_method       'time-of-flight LAUE diffraction'
_diffrn_radiation_monochromator  none
_diffrn_radiation_probe          neutron
_diffrn_radiation_source         'ISIS spallation source'
_diffrn_radiation_type           neutron
_diffrn_radiation_wavelength     0.5-5.0
_diffrn_reflns_av_R_equivalents  0.0660
_diffrn_reflns_av_sigmaI/netI    0.0484
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            19586
_diffrn_reflns_theta_full        14.49
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.596
_exptl_absorpt_correction_T_max  0.56
_exptl_absorpt_correction_T_min  0.10
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;
The linear absorption coefficient is wavelength dependent
 and it is calculated as: 
          mu = 1.25 + 14.71 * lambda  [cm^-1]
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.110
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'thin plate'
_exptl_crystal_F_000             11.53
_exptl_crystal_size_max          3
_exptl_crystal_size_mid          2.5
_exptl_crystal_size_min          1
_refine_diff_density_max         2.805
_refine_diff_density_min         -2.373
_refine_diff_density_rms         0.543
_refine_ls_extinction_coef       0.690
_refine_ls_extinction_method     'Becker-Coppens Lorentzian model'
_refine_ls_goodness_of_fit_ref   1.100
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     523
_refine_ls_number_reflns         5005
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.100
_refine_ls_R_factor_all          0.0982
_refine_ls_R_factor_gt           0.0982
_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^)+(0.0897P)^2^+101.7556P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2372
_refine_ls_wR_factor_ref         0.2372
_reflns_number_gt                5005
_reflns_number_total             5005
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic000961e_1.cif
_cod_data_source_block           00aeg014
_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 
;
_cod_database_code               4319135