#------------------------------------------------------------------------------ #$Date: 2008-01-14 00:15:36 +0200 (Mon, 14 Jan 2008) $ #$Revision: 14 $ #$URL: file:///home/coder/svn-repositories/cod/cif/5/5000306.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_5000306 _chemical_name_systematic ; ? ; _chemical_name_common '2,2''-azo-bis-isobutyrylnitrile' _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C8 H12 N4' _chemical_formula_weight 164.22 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' _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 5.4218(3) _cell_length_b 6.1566(4) _cell_length_c 7.6275(5) _cell_angle_alpha 78.7260(10) _cell_angle_beta 81.593(2) _cell_angle_gamma 72.2190(10) _cell_volume 236.74(3) _cell_formula_units_Z 1 _cell_measurement_temperature 183(2) _cell_measurement_reflns_used 1813 _cell_measurement_theta_min 2.73 _cell_measurement_theta_max 29.95 _exptl_crystal_description diamond plate _exptl_crystal_colour colorless _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.152 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 88 _exptl_absorpt_coefficient_mu 0.075 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min 0.9742 _exptl_absorpt_correction_T_max 0.9963 _exptl_absorpt_process_details ? _diffrn_ambient_temperature 183(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 'three-circle goniometer with fixed chi' _diffrn_measurement_device_type 'Bruker Platform goniometer' _diffrn_detector 'CCD area detector' _diffrn_detector_type 'Bruker SMART 6000' _diffrn_standards_decay_% 0.021 _diffrn_reflns_number 3295 _diffrn_reflns_av_R_equivalents 0.1029 _diffrn_reflns_av_sigmaI/netI 0.0902 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 2.73 _diffrn_reflns_theta_max 30.04 _reflns_number_total 1383 _reflns_number_gt 1002 _reflns_threshold_expression >2sigma(I) _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^)+(0.0587P)^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 mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00(4) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 1383 _refine_ls_number_parameters 80 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0678 _refine_ls_R_factor_gt 0.0484 _refine_ls_wR_factor_ref 0.1339 _refine_ls_wR_factor_gt 0.1194 _refine_ls_goodness_of_fit_ref 0.989 _refine_ls_restrained_S_all 0.989 _refine_ls_shift/su_max 4.071 _refine_ls_shift/su_mean 0.051 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 0.03480(18) 0.39902(17) 0.53750(14) 0.0231(3) Uani 1 1 d . . . C2 C -0.1223(2) 0.34801(18) 0.70947(15) 0.0209(3) Uani 1 1 d . . . C3 C -0.3432(2) 0.5506(2) 0.74731(16) 0.0250(3) Uani 1 1 d . . . N4 N -0.5185(2) 0.69990(19) 0.78319(16) 0.0364(4) Uani 1 1 d . . . C5 C -0.2253(3) 0.1483(2) 0.69330(18) 0.0267(3) Uani 1 1 d . . . C6 C 0.0617(2) 0.2779(2) 0.85702(17) 0.0259(3) Uani 1 1 d . . . H7 H -0.334(3) 0.193(3) 0.597(2) 0.039(4) Uiso 1 1 d . . . H8 H -0.319(3) 0.103(3) 0.808(2) 0.028(4) Uiso 1 1 d . . . H9 H -0.072(3) 0.016(3) 0.672(2) 0.034(4) Uiso 1 1 d . . . H10 H -0.031(3) 0.244(2) 0.971(2) 0.027(4) Uiso 1 1 d . . . H11 H 0.192(3) 0.141(3) 0.837(2) 0.037(4) Uiso 1 1 d . . . H12 H 0.140(3) 0.402(3) 0.861(2) 0.033(4) 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 N1 0.0213(5) 0.0194(5) 0.0249(5) 0.0001(4) 0.0044(4) -0.0057(4) C2 0.0187(5) 0.0175(5) 0.0239(5) -0.0005(4) 0.0040(4) -0.0056(4) C3 0.0232(6) 0.0208(6) 0.0269(6) 0.0025(4) 0.0041(4) -0.0072(5) N4 0.0284(6) 0.0255(6) 0.0444(7) 0.0005(5) 0.0109(5) -0.0021(5) C5 0.0276(6) 0.0219(6) 0.0312(6) -0.0016(5) 0.0003(5) -0.0110(5) C6 0.0226(6) 0.0245(6) 0.0287(6) -0.0019(5) 0.0007(5) -0.0071(5) _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 N1 1.2305(19) 2_566 ? N1 C2 1.4901(14) . ? C2 C3 1.4837(15) . ? C2 C6 1.5244(18) . ? C2 C5 1.5288(17) . ? C3 N4 1.1451(16) . ? 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 N1 N1 C2 114.27(11) 2_566 . ? C3 C2 N1 112.16(8) . . ? C3 C2 C6 110.06(10) . . ? N1 C2 C6 106.62(9) . . ? C3 C2 C5 109.71(9) . . ? N1 C2 C5 107.21(10) . . ? C6 C2 C5 111.02(10) . . ? N4 C3 C2 176.60(11) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 30.04 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.387 _refine_diff_density_min -0.229 _refine_diff_density_rms 0.055 _exptl_crystal_id MSC02106 _publ_author_name 'David Ihle/D. Williams' _chemical_name_common ? _chemical-formula_structural ? _chemical_formula_sum ? _chemical_formula_weight ? _symmetry_cell_setting ? _symmetry_space_group_name_H-M ? _cell_length_a ? _cell_length_b ? _cell_length_c ? _cell_angle_alpha ? _cell_angle_beta ? _cell_angle_gamma ? _cell_volume ? _cell_formula_units_Z ? _cell_measurement_temperature ? _exptl_crystal_colour ? _exptl_crystal_density_diffrn ? _refine_ls_wR_factor_ref ? _refine_ls_R_factor_gt ? _diffrn_ambient_temperature ? _cell_measurement_reflns_used ? _exptl_absorpt_coefficient_mu ?