Intra- and inter-molecular C‒H⋯F‒C and N‒H⋯F‒C hydrogen bonding in secondary amine adducts of B(C6F5)3: relevance to key interactions in alkene polymerisation catalysis
Mountford, Andrew J.; Hughes, David L.; Lancaster, Simon J.; Chemical Communications (Cambridge, United Kingdom)  (2003) 2148–2149; doi:10.1039/b305613a

data_7113865
_publ_section_title
;
 Intra- and inter-molecular C--H&#x22EF;F--C and N--H&#x22EF;F--C hydrogen
 bonding in secondary amine adducts of B(C6F5)3: relevance to key interactions
 in alkene polymerisation catalysis
;
_journal_coden_ASTM              CHCOFS
_journal_issue                   17
_journal_name_full
;
 Chemical Communications (Cambridge, United Kingdom)
;
_journal_page_first              2148
_journal_page_last               2149
_journal_paper_doi               10.1039/b305613a
_journal_year                    2003
_chemical_formula_moiety         'C22 H9 B F15 N'
_chemical_formula_structural     (C6F5)3B-cyclo-NHC4H8
_chemical_formula_sum            'C22 H9 B F15 N'
_chemical_formula_weight         583.11
_chemical_name_common            'complex 1'
_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                 117.22(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.232(1)
_cell_length_b                   11.510(1)
_cell_length_c                   14.543(1)
_cell_measurement_temperature    140(1)
_cell_volume                     2118.5(3)
_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 0.936
_diffrn_measured_fraction_theta_max 0.936
_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  0.0596
_diffrn_reflns_av_sigmaI/netI    0.0452
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            12139
_diffrn_reflns_theta_full        25.33
_diffrn_reflns_theta_max         25.33
_diffrn_reflns_theta_min         1.66
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    0.200
_exptl_absorpt_correction_type   'not applied'
_exptl_crystal_colour            'clear, colourless,'
_exptl_crystal_density_diffrn    1.828
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'square prisms'
_exptl_crystal_F_000             1152
_exptl_crystal_size_max          0.65
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.203
_refine_diff_density_min         -0.212
_refine_diff_density_rms         0.046
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.094
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     352
_refine_ls_number_reflns         3616
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.094
_refine_ls_R_factor_all          0.0382
_refine_ls_R_factor_gt           0.0332
_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^)+(0.0468P)^2^+0.365P] where P==(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0928
_refine_ls_wR_factor_ref         0.0954
_reflns_number_gt                3125
_reflns_number_total             3616
_reflns_threshold_expression     I>2sigma(I)
_cod_duplicate_entry             7103874
_cod_data_source_file            b305613a.txt
_cod_data_source_block           andym5
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               7113865