Supplementary Material (ESI) for Chemical Communications This journal is © The Royal Society of Chemistry 2001 data_k99254 _database_code_CSD 160965 _journal_coden_Cambridge 182 _publ_requested_journal 'Chemical Communications' loop_ _publ_author_name 'Jaska, Cory A.' 'Lough, Alan' 'Manners, I.' 'Temple, Karen' _publ_contact_author_name 'Prof I Manners' _publ_contact_author_address ; Prof I Manners Department of Chemistry University of Toronto 80 St. George Street Toronto M5S 1A1 CANADA ; _publ_contact_author_email 'IMANNERS@ALCHEMY.CHEM.UTORONTO.CA' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C4 H16 B2 N2' _chemical_formula_weight 113.81 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'B' 'B' 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 5.8330(7) _cell_length_b 6.0290(10) _cell_length_c 6.2400(10) _cell_angle_alpha 80.372(8) _cell_angle_beta 81.533(10) _cell_angle_gamma 65.942(8) _cell_volume 196.80(5) _cell_formula_units_Z 1 _cell_measurement_temperature 103(1) _cell_measurement_reflns_used 895 _cell_measurement_theta_min 3.32 _cell_measurement_theta_max 27.51 _exptl_crystal_description 'cut needle' _exptl_crystal_colour 'colourless' _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 0.960 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 64 _exptl_absorpt_coefficient_mu 0.055 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9837 _exptl_absorpt_correction_T_max 0.9864 _exptl_absorpt_process_details 'Denzo-SMN (Otwinowski & Minor, 1997)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 103(1) _diffrn_radiation_wavelength 0.71070 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Kappa-CCD' _diffrn_measurement_method '\w scans and \f scans with \k offsets' _diffrn_detector_area_resol_mean 9 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% none _diffrn_reflns_number 3782 _diffrn_reflns_av_R_equivalents 0.069 _diffrn_reflns_av_sigmaI/netI 0.0886 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -6 _diffrn_reflns_limit_k_max 7 _diffrn_reflns_limit_l_min -7 _diffrn_reflns_limit_l_max 8 _diffrn_reflns_theta_min 3.32 _diffrn_reflns_theta_max 27.51 _reflns_number_total 895 _reflns_number_gt 653 _reflns_threshold_expression >2sigma(I) computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'Denzo-SMN (Otwinowski & Minor, 1997)' _computing_data_reduction 'Denzo-SMN (Otwinowski & Minor, 1997)' _computing_structure_solution 'Bruker SHELXTL V5.1' _computing_structure_refinement 'Bruker SHELXTL V5.1' _computing_molecular_graphics 'Bruker SHELXTL V5.1' _computing_publication_material 'Bruker SHELXTL V5.1' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0986P)^2^+0.3873P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.05(12) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 895 _refine_ls_number_parameters 40 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1209 _refine_ls_R_factor_gt 0.0963 _refine_ls_wR_factor_ref 0.3002 _refine_ls_wR_factor_gt 0.2866 _refine_ls_goodness_of_fit_ref 1.162 _refine_ls_restrained_S_all 1.162 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group N1 N 0.4762(5) 0.1407(5) 0.8438(4) 0.0246(8) Uani 1 1 d . . . C2 C 0.6831(7) 0.1655(7) 0.6884(6) 0.0344(10) Uani 1 1 d . . . H2A H 0.6610 0.1411 0.5426 0.052 Uiso 1 1 calc R . . H2B H 0.8446 0.0425 0.7349 0.052 Uiso 1 1 calc R . . H2C H 0.6813 0.3294 0.6843 0.052 Uiso 1 1 calc R . . C1 C 0.2338(6) 0.3263(6) 0.7714(6) 0.0323(10) Uani 1 1 d . . . H1A H 0.2331 0.4900 0.7656 0.048 Uiso 1 1 calc R . . H1B H 0.0953 0.3118 0.8746 0.048 Uiso 1 1 calc R . . H1C H 0.2124 0.3001 0.6261 0.048 Uiso 1 1 calc R . . B1 B 0.4865(8) -0.1309(7) 0.9062(6) 0.0291(10) Uani 1 1 d . . . H1D H 0.3276 -0.1441 0.8859 0.035 Uiso 1 1 calc R . . H1E H 0.6315 -0.2532 0.8292 0.035 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 N1 0.0267(14) 0.0252(15) 0.0226(15) -0.0024(10) -0.0037(10) -0.0106(11) C2 0.037(2) 0.041(2) 0.0306(19) -0.0067(15) 0.0014(15) -0.0207(16) C1 0.0333(19) 0.0287(18) 0.0338(19) -0.0040(14) -0.0095(14) -0.0088(14) B1 0.039(2) 0.0257(19) 0.0254(19) -0.0044(14) -0.0055(15) -0.0141(16) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag N1 C2 1.474(4) . ? N1 C1 1.478(4) . ? N1 B1 1.595(4) 2_657 ? N1 B1 1.596(4) . ? B1 N1 1.595(4) 2_657 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 N1 C1 109.0(3) . . ? C2 N1 B1 114.6(3) . 2_657 ? C1 N1 B1 114.8(3) . 2_657 ? C2 N1 B1 115.6(3) . . ? C1 N1 B1 115.4(3) . . ? B1 N1 B1 86.3(2) 2_657 . ? N1 B1 N1 93.7(2) 2_657 . ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 27.51 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 0.499 _refine_diff_density_min -0.261 _refine_diff_density_rms 0.092