data_xpan425s _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C4 H10 B N3' _chemical_formula_sum 'C4 H10 B N3' _chemical_formula_weight 110.96 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' 'B' 'B' 0.0013 0.0007 '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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 11.4755(11) _cell_length_b 4.6745(5) _cell_length_c 12.6976(13) _cell_angle_alpha 90.00 _cell_angle_beta 100.463(2) _cell_angle_gamma 90.00 _cell_volume 669.80(12) _cell_formula_units_Z 4 _cell_measurement_temperature 203(2) _cell_measurement_reflns_used 1533 _cell_measurement_theta_min 3.26 _cell_measurement_theta_max 24.45 _exptl_crystal_description columnar _exptl_crystal_colour colorless _exptl_crystal_size_max 0.34 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.100 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 240 _exptl_absorpt_coefficient_mu 0.070 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9765 _exptl_absorpt_correction_T_max 0.9902 _exptl_absorpt_process_details 'Bruker Sadabs' _exptl_special_details ; ? ; _diffrn_ambient_temperature 203(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Smart Apex CCD' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7448 _diffrn_reflns_av_R_equivalents 0.0543 _diffrn_reflns_av_sigmaI/netI 0.0512 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -6 _diffrn_reflns_limit_k_max 6 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 3.26 _diffrn_reflns_theta_max 32.24 _reflns_number_total 2211 _reflns_number_gt 1286 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0780P)^2^+0.0000P] 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 refall _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2211 _refine_ls_number_parameters 113 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1035 _refine_ls_R_factor_gt 0.0571 _refine_ls_wR_factor_ref 0.1626 _refine_ls_wR_factor_gt 0.1412 _refine_ls_goodness_of_fit_ref 1.037 _refine_ls_restrained_S_all 1.037 _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 B B 0.28709(17) -0.1670(3) 0.61064(12) 0.0518(4) Uani 1 1 d . . . H1A H 0.2144(13) -0.147(3) 0.5376(13) 0.065(4) Uiso 1 1 d . . . H1B H 0.3081(13) -0.391(4) 0.6295(13) 0.072(5) Uiso 1 1 d . . . H1C H 0.3714(17) -0.062(4) 0.5949(14) 0.079(5) Uiso 1 1 d . . . N1 N 0.15490(10) 0.1608(2) 0.71312(9) 0.0494(3) Uani 1 1 d . . . C1 C 0.24707(11) -0.0122(2) 0.71015(9) 0.0422(3) Uani 1 1 d . . . N2 N 0.30388(10) -0.0223(2) 0.81368(8) 0.0477(3) Uani 1 1 d . . . C2 C 0.24332(15) 0.1450(4) 0.87295(12) 0.0601(4) Uani 1 1 d . . . H2 H 0.2720(14) 0.167(4) 0.9500(15) 0.074(5) Uiso 1 1 d . . . N3 N 0.15183(13) 0.2617(3) 0.81483(11) 0.0638(4) Uani 1 1 d . . . C3 C 0.06442(18) 0.2538(5) 0.62513(16) 0.0670(5) Uani 1 1 d . . . H3A H -0.003(2) 0.175(5) 0.6279(18) 0.113(8) Uiso 1 1 d . . . H3B H 0.0796(19) 0.198(5) 0.5559(19) 0.110(8) Uiso 1 1 d . . . H3C H 0.057(2) 0.458(6) 0.625(2) 0.132(9) Uiso 1 1 d . . . C4 C 0.41177(16) -0.1841(4) 0.85405(14) 0.0636(5) Uani 1 1 d . . . H4A H 0.4189(17) -0.236(4) 0.9296(18) 0.101(7) Uiso 1 1 d . . . H4B H 0.4069(18) -0.359(6) 0.816(2) 0.108(8) Uiso 1 1 d . . . H4C H 0.483(2) -0.067(5) 0.8557(17) 0.114(7) Uiso 1 1 d . . . 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 B 0.0645(11) 0.0500(9) 0.0437(8) -0.0044(7) 0.0173(7) -0.0050(8) N1 0.0515(7) 0.0513(6) 0.0480(6) -0.0003(5) 0.0161(5) -0.0020(5) C1 0.0493(7) 0.0401(6) 0.0387(6) 0.0021(5) 0.0122(5) -0.0078(5) N2 0.0542(7) 0.0541(6) 0.0366(5) 0.0012(5) 0.0134(5) -0.0045(5) C2 0.0698(10) 0.0705(9) 0.0435(8) -0.0091(7) 0.0198(7) -0.0050(8) N3 0.0724(9) 0.0676(8) 0.0577(8) -0.0109(6) 0.0285(7) 0.0030(7) C3 0.0546(10) 0.0758(12) 0.0703(12) 0.0110(9) 0.0105(8) 0.0050(9) C4 0.0609(10) 0.0793(12) 0.0498(9) 0.0134(8) 0.0077(7) 0.0040(8) _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 B C1 1.594(2) . ? B H1A 1.133(15) . ? B H1B 1.090(19) . ? B H1C 1.134(19) . ? N1 C1 1.3374(17) . ? N1 N3 1.3813(17) . ? N1 C3 1.447(2) . ? C1 N2 1.3580(15) . ? N2 C2 1.3605(19) . ? N2 C4 1.462(2) . ? C2 N3 1.289(2) . ? C2 H2 0.979(18) . ? C3 H3A 0.87(3) . ? C3 H3B 0.96(3) . ? C3 H3C 0.96(3) . ? C4 H4A 0.98(2) . ? C4 H4B 0.94(3) . ? C4 H4C 0.98(3) . ? 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 C1 B H1A 109.7(8) . . ? C1 B H1B 110.2(9) . . ? H1A B H1B 110.9(11) . . ? C1 B H1C 108.8(9) . . ? H1A B H1C 110.2(11) . . ? H1B B H1C 106.9(12) . . ? C1 N1 N3 112.78(12) . . ? C1 N1 C3 128.33(13) . . ? N3 N1 C3 118.87(14) . . ? N1 C1 N2 103.70(11) . . ? N1 C1 B 129.78(12) . . ? N2 C1 B 126.49(12) . . ? C1 N2 C2 108.17(12) . . ? C1 N2 C4 125.77(12) . . ? C2 N2 C4 126.06(13) . . ? N3 C2 N2 111.79(14) . . ? N3 C2 H2 128.2(10) . . ? N2 C2 H2 120.0(10) . . ? C2 N3 N1 103.56(13) . . ? N1 C3 H3A 111.4(15) . . ? N1 C3 H3B 113.6(12) . . ? H3A C3 H3B 104(2) . . ? N1 C3 H3C 110.8(15) . . ? H3A C3 H3C 110(2) . . ? H3B C3 H3C 107(2) . . ? N2 C4 H4A 112.7(12) . . ? N2 C4 H4B 107.5(13) . . ? H4A C4 H4B 105.8(18) . . ? N2 C4 H4C 111.8(13) . . ? H4A C4 H4C 101.3(16) . . ? H4B C4 H4C 118(2) . . ? _diffrn_measured_fraction_theta_max 0.936 _diffrn_reflns_theta_full 31.00 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.157 _refine_diff_density_min -0.145 _refine_diff_density_rms 0.038