#------------------------------------------------------------------------------ #$Date: 2011-01-03 14:48:23 +0200 (Mon, 03 Jan 2011) $ #$Revision: 5312 $ #$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 loop_ _publ_author_name 'David Ihle/D. Williams' _chemical_formula_moiety ? _chemical_formula_sum 'C8 H12 N4' _chemical_formula_weight 164.22 _chemical_melting_point ? _chemical_name_common 2,2''-azo-bis-isobutyrylnitrile _chemical_name_systematic ; ? ; _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P-1 ' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _cell_angle_alpha 78.7260(10) _cell_angle_beta 81.593(2) _cell_angle_gamma 72.2190(10) _cell_formula_units_Z 1 _cell_length_a 5.4218(3) _cell_length_b 6.1566(4) _cell_length_c 7.6275(5) _cell_measurement_reflns_used 1813 _cell_measurement_temperature 183(2) _cell_measurement_theta_max 29.95 _cell_measurement_theta_min 2.73 _cell_volume 236.74(3) _diffrn_ambient_temperature 183(2) _diffrn_detector 'CCD area detector' _diffrn_detector_type 'Bruker SMART 6000' _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.999 _diffrn_measurement_device 'three-circle goniometer with fixed chi' _diffrn_measurement_device_type 'Bruker Platform goniometer' _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.1029 _diffrn_reflns_av_sigmaI/netI 0.0902 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_number 3295 _diffrn_reflns_theta_full 30.04 _diffrn_reflns_theta_max 30.04 _diffrn_reflns_theta_min 2.73 _diffrn_standards_decay_% 0.021 _exptl_absorpt_coefficient_mu 0.075 _exptl_absorpt_correction_T_max 0.9963 _exptl_absorpt_correction_T_min 0.9742 _exptl_absorpt_correction_type none _exptl_absorpt_process_details ? _exptl_crystal_colour colorless _exptl_crystal_density_diffrn 1.152 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_description 'diamond plate' _exptl_crystal_F_000 88 _exptl_crystal_id MSC02106 _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.05 _refine_diff_density_max 0.387 _refine_diff_density_min -0.229 _refine_diff_density_rms 0.055 _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_extinction_method SHELXL _refine_ls_goodness_of_fit_ref 0.989 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 80 _refine_ls_number_reflns 1383 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 0.989 _refine_ls_R_factor_all 0.0678 _refine_ls_R_factor_gt 0.0484 _refine_ls_shift/su_max 4.071 _refine_ls_shift/su_mean 0.051 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0587P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1194 _refine_ls_wR_factor_ref 0.1339 _reflns_number_gt 1002 _reflns_number_total 1383 _reflns_threshold_expression >2sigma(I) _cod_depositor_comments ; The following automatic conversions were performed: '_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic' according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29. Automatic conversion script Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius ; _cod_database_code 5000306 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' 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) 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' 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) . . ? 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) . ?