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_4309370
_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         'C26 H11 B F15 N, C H2 Cl2'
_chemical_formula_structural     (C6F5)3BNH2CH(Me)Ph.CH2Cl2
_chemical_formula_sum            'C27 H13 B Cl2 F15 N'
_chemical_formula_weight         718.09
_chemical_name_common            'Compound 1d'
_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                 96.60(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.736(2)
_cell_length_b                   8.7560(18)
_cell_length_c                   29.330(6)
_cell_measurement_temperature    140(1)
_cell_volume                     2738.9(10)
_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 0.855
_diffrn_measured_fraction_theta_max 0.855
_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  0.0791
_diffrn_reflns_av_sigmaI/netI    0.0685
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            12120
_diffrn_reflns_theta_full        25.35
_diffrn_reflns_theta_max         25.35
_diffrn_reflns_theta_min         1.40
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    0.361
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            'clear, colourless'
_exptl_crystal_density_diffrn    1.741
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1424
_exptl_crystal_size_max          0.8
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.674
_refine_diff_density_min         -0.887
_refine_diff_density_rms         0.101
_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     415
_refine_ls_number_reflns         4288
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0921
_refine_ls_R_factor_gt           0.0751
_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^)+(0.1232P)^2^+6.8222P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2273
_refine_ls_wR_factor_ref         0.2361
_reflns_number_gt                3213
_reflns_number_total             4288
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            ic050663nsi20050429_025944_05.cif
_cod_data_source_block           simonl11
_cod_original_sg_symbol_H-M      'P 21/n '
_cod_database_code               4309370