Intra- and Intermolecular N-H...F-C Hydrogen-Bonding Interactions in Amine Adducts of Tris(pentafluorophenyl)borane and -alane
Andrew J. Mountford; Simon J. Lancaster; Simon J. Coles; Peter N. Horton; David L. Hughes; Michael B. Hursthouse; Mark E. Light; Inorganic Chemistry 44 (2005) 5921–5933; doi:10.1021/ic050663n

data_4309377
_publ_section_title
;
Intra- and Intermolecular N-H...F-C Hydrogen-Bonding Interactions in
Amine Adducts of Tris(pentafluorophenyl)borane and -alane
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5921
_journal_page_last               5933
_journal_paper_doi               10.1021/ic050663n
_journal_volume                  44
_journal_year                    2005
_chemical_formula_moiety         'C23 H11 Al F15 N'
_chemical_formula_structural     (C6F5)3Al-N(H)C5H10
_chemical_formula_sum            'C23 H11 Al F15 N'
_chemical_formula_weight         613.31
_chemical_name_common            'Compound 2f'
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 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                 108.95(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   21.346(4)
_cell_length_b                   10.968(2)
_cell_length_c                   22.090(4)
_cell_measurement_temperature    140(1)
_cell_volume                     4891.5(18)
_computing_cell_refinement       'DENZO/CELL (Otwinowski and Minor, 1985)'
_computing_data_collection       'MSC R-Axis-II control software'
_computing_data_reduction
'DENZO, SCALEPACK (Otwinowski and Minor, 1985)'
_computing_molecular_graphics    'ORTEP (Johnson, 1971)'
_computing_publication_material  'SHELXL (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS (Sheldrick, 1997)'
_diffrn_ambient_temperature      140(1)
_diffrn_measured_fraction_theta_full 0.969
_diffrn_measured_fraction_theta_max 0.969
_diffrn_measurement_device       'Rigaku R-Axis-IIc'
_diffrn_measurement_method       'image-plate oscillation photos'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           Mo-K\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0570
_diffrn_reflns_av_sigmaI/netI    0.0508
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            26026
_diffrn_reflns_theta_full        25.35
_diffrn_reflns_theta_max         25.35
_diffrn_reflns_theta_min         1.88
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    0.211
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            'clear, colourless'
_exptl_crystal_density_diffrn    1.666
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prisms
_exptl_crystal_F_000             2432
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.250
_refine_diff_density_min         -0.288
_refine_diff_density_rms         0.043
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     750
_refine_ls_number_reflns         8691
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0475
_refine_ls_R_factor_gt           0.0367
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0537P)^2^+0.4864P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0965
_refine_ls_wR_factor_ref         0.1009
_reflns_number_gt                7053
_reflns_number_total             8691
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            ic050663nsi20050429_025944_12.cif
_cod_data_source_block           simonl9
_cod_original_cell_volume        4891.6(17)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4309377