#------------------------------------------------------------------------------ #$Date: 2016-02-19 22:18:51 +0000 (Fri, 19 Feb 2016) $ #$Revision: 176760 $ #$URL: svn://www.crystallography.net/cod/cif/2/01/19/2011924.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/. The original data for this entry # were provided by IUCr Journals, http://journals.iucr.org/. # # The file may be used within the scientific community so long as # proper attribution is given to the journal article from which the # data were obtained. # data_2011924 loop_ _publ_author_name 'Vasiliev, Alexander D.' 'Astachov, Alexander M.' 'Nefedov, Andrey A.' 'Kruglyakova, Ludmila A.' 'Stepanov, Rudolf S.' _publ_section_title ; Nitroguanyl azide ; _journal_issue 5 _journal_name_full 'Acta Crystallographica Section C' _journal_page_first 625 _journal_page_last 626 _journal_paper_doi 10.1107/S0108270101002827 _journal_volume 57 _journal_year 2001 _chemical_formula_moiety 'C H2 N6 O2' _chemical_formula_sum 'C H2 N6 O2' _chemical_formula_weight 130.09 _chemical_name_systematic ; nitrocarbamimidoyl azide ; _space_group_IT_number 2 _symmetry_cell_setting triclinic _symmetry_space_group_name_Hall '-P 1' _symmetry_space_group_name_H-M 'P -1' _cell_angle_alpha 98.310(10) _cell_angle_beta 110.580(10) _cell_angle_gamma 75.108(9) _cell_formula_units_Z 4 _cell_length_a 9.9302(8) _cell_length_b 7.9433(9) _cell_length_c 7.1288(8) _cell_measurement_reflns_used 24 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 34 _cell_measurement_theta_min 26 _cell_volume 507.83(10) _computing_cell_refinement 'KM-4 Software' _computing_data_collection 'KM-4 Software (Kuma, 1991)' _computing_data_reduction 'DATARED in KM-4 Software' _computing_molecular_graphics 'SHELXTL (Sheldrick, 1995)' _computing_publication_material SHELXL97 _computing_structure_refinement 'SHELXL97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS97 (Sheldrick, 1990)' _diffrn_ambient_temperature 293(2) _diffrn_measured_fraction_theta_full .955 _diffrn_measured_fraction_theta_max .955 _diffrn_measurement_device_type 'Kuma KM-4 four-circle' _diffrn_measurement_method 'profile measured \q/2\q' _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.5418 _diffrn_reflns_av_R_equivalents .0147 _diffrn_reflns_av_sigmaI/netI .0103 _diffrn_reflns_limit_h_max 0 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_l_max 8 _diffrn_reflns_limit_l_min -8 _diffrn_reflns_number 1971 _diffrn_reflns_theta_full 69.99 _diffrn_reflns_theta_max 69.99 _diffrn_reflns_theta_min 4.88 _diffrn_standards_decay_% none _diffrn_standards_interval_count 50 _diffrn_standards_number 2 _exptl_absorpt_coefficient_mu 1.368 _exptl_absorpt_correction_type none _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.701 _exptl_crystal_density_method 'not measured' _exptl_crystal_description lump _exptl_crystal_F_000 264 _exptl_crystal_size_max .32 _exptl_crystal_size_mid .30 _exptl_crystal_size_min .29 _refine_diff_density_max .205 _refine_diff_density_min -.198 _refine_ls_extinction_coef .0089(14) _refine_ls_extinction_method 'SHELXL97 (Sheldrick, 1997)' _refine_ls_goodness_of_fit_ref 1.087 _refine_ls_hydrogen_treatment refall _refine_ls_matrix_type full _refine_ls_number_parameters 180 _refine_ls_number_reflns 1851 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.087 _refine_ls_R_factor_all .0360 _refine_ls_R_factor_gt .0339 _refine_ls_shift/su_max .009 _refine_ls_shift/su_mean .001 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w = 1/[\s^2^(Fo^2^)+(0.0537P)^2^+0.1095P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_ref .0951 _reflns_number_gt 1713 _reflns_number_total 1851 _reflns_threshold_expression I>2\s(I) _cod_data_source_file av1067.cif _cod_data_source_block 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 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_values 1715 2011-07-08 13:25:40Z adriana ; _cod_original_cell_volume 507.83(9) _cod_database_code 2011924 _cod_database_fobs_code 2011924 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_refinement_flags _atom_site_occupancy _atom_site_disorder_assembly _atom_site_disorder_group _atom_site_type_symbol C1A .74742(16) .00130(17) .6997(2) .0376(3) Uani d . 1 . . C N1A .66238(13) .10530(15) .55232(17) .0378(3) Uani d . 1 . . N N2A .87682(17) -.10340(18) .7291(2) .0512(4) Uani d . 1 . . N H1A .917(3) -.160(3) .842(4) .071(6) Uiso d . 1 . . H H2A .923(3) -.099(3) .645(3) .071(6) Uiso d . 1 . . H N3A .71542(13) .11576(15) .40460(17) .0373(3) Uani d . 1 . . N N4A .68901(17) .00020(18) .8506(2) .0516(4) Uani d . 1 . . N N5A .56250(16) .09674(17) .82266(18) .0453(3) Uani d . 1 . . N N6A .45205(19) .1744(2) .8220(2) .0592(4) Uani d . 1 . . N O1A .62908(12) .21175(15) .27048(16) .0494(3) Uani d . 1 . . O O2A .83855(13) .03785(16) .40061(18) .0558(3) Uani d . 1 . . O C1B .22185(15) .48405(17) -.05571(19) .0347(3) Uani d . 1 . . C N1B .14663(12) .37780(14) -.02858(16) .0342(3) Uani d . 1 . . N N2B .20705(17) .55960(19) -.2144(2) .0495(4) Uani d . 1 . . N H1B .262(3) .626(3) -.206(3) .074(7) Uiso d . 1 . . H H2B .144(2) .535(3) -.328(3) .063(6) Uiso d . 1 . . H N3B .03547(13) .33446(14) -.18819(16) .0372(3) Uani d . 1 . . N N4B .33450(14) .52520(18) .11267(18) .0448(3) Uani d . 1 . . N N5B .33850(13) .46870(17) .27080(18) .0433(3) Uani d . 1 . . N N6B .35467(17) .4289(2) .4216(2) .0621(4) Uani d . 1 . . N O1B -.03604(12) .24662(14) -.15028(16) .0481(3) Uani d . 1 . . O O2B .00660(14) .37831(17) -.35940(16) .0603(4) Uani d . 1 . . O loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 C1A .0448(8) .0351(6) .0353(7) -.0093(6) .0144(6) .0050(5) N1A .0404(7) .0422(6) .0348(6) -.0084(5) .0151(5) .0089(5) N2A .0534(9) .0501(7) .0495(8) .0026(6) .0198(7) .0194(6) N3A .0396(7) .0417(6) .0343(6) -.0124(5) .0126(5) .0066(5) N4A .0597(9) .0551(8) .0431(7) .0013(6) .0247(6) .0180(6) N5A .0582(10) .0483(7) .0374(6) -.0154(7) .0224(6) .0038(5) N6A .0574(10) .0678(9) .0597(9) -.0113(8) .0310(7) .0010(7) O1A .0499(7) .0594(6) .0415(6) -.0087(5) .0131(5) .0222(5) O2A .0456(7) .0729(8) .0532(7) -.0001(6) .0258(5) .0157(6) C1B .0339(7) .0376(7) .0337(6) -.0046(5) .0132(5) .0059(5) N1B .0353(7) .0382(6) .0294(5) -.0088(5) .0086(4) .0071(4) N2B .0559(9) .0619(8) .0384(7) -.0244(7) .0122(6) .0143(6) N3B .0397(7) .0368(6) .0335(6) -.0074(5) .0097(5) .0052(4) N4B .0396(7) .0592(8) .0394(7) -.0182(6) .0101(5) .0087(5) N5B .0329(7) .0589(7) .0361(7) -.0129(5) .0063(5) .0042(5) N6B .0520(9) .0948(11) .0374(7) -.0200(8) .0065(6) .0118(7) O1B .0505(7) .0478(6) .0517(6) -.0227(5) .0159(5) .0011(5) O2B .0718(8) .0753(8) .0321(5) -.0312(6) -.0006(5) .0157(5) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C .0181 .0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N .0311 .0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O .0492 .0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H .0000 .0000 '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 N2A C1A N1A 131.75(14) N2A C1A N4A 112.86(13) N1A C1A N4A 115.38(13) C1A N1A N3A 117.98(12) C1A N2A H1A 117.9(14) C1A N2A H2A 116.5(15) H1A N2A H2A 125(2) O2A N3A O1A 121.65(11) O2A N3A N1A 123.97(11) O1A N3A N1A 114.38(12) N5A N4A C1A 113.99(12) N6A N5A N4A 170.43(14) N2B C1B N1B 131.03(14) N2B C1B N4B 113.11(13) N1B C1B N4B 115.86(11) C1B N1B N3B 118.01(11) C1B N2B H1B 119.2(16) C1B N2B H2B 119.1(14) H1B N2B H2B 122(2) O1B N3B O2B 121.71(12) O1B N3B N1B 114.80(11) O2B N3B N1B 123.49(11) N5B N4B C1B 113.28(11) N6B N5B N4B 171.87(15) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag C1A N1A . 1.3296(18) ? C1A N2A . 1.303(2) ? C1A N4A . 1.3921(18) ? N1A N3A . 1.3532(15) ? N2A H1A . .89(2) ? N2A H2A . .89(2) ? N3A O2A . 1.2284(16) ? N3A O1A . 1.2366(16) ? N4A N5A . 1.257(2) ? N5A N6A . 1.1104(19) ? C1B N2B . 1.3024(18) ? C1B N1B . 1.3343(17) ? C1B N4B . 1.3891(18) ? N1B N3B . 1.3531(16) ? N2B H1B . .83(2) ? N2B H2B . .87(2) ? N3B O1B . 1.2280(15) ? N3B O2B . 1.2324(15) ? N4B N5B . 1.2566(17) ? N5B N6B . 1.1104(18) ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_publ_flag N2A H2A O2A 1_555 .88(3) 1.99(2) 2.608(2) 126(2) yes N2B H2B O2B 1_555 .86(2) 2.01(2) 2.589(2) 123(2) yes N2A H1A O1B 2_656 .89(3) 2.21(3) 3.088(2) 167(2) yes N2B H1B O1A 2_665 .83(3) 2.07(3) 2.880(2) 164(2) yes N2B H2B O2B 2_564 .86(2) 2.29(2) 3.056(2) 148(2) yes loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion N2A C1A N1A N3A -3.0(2) N4A C1A N1A N3A 178.00(12) C1A N1A N3A O2A -1.6(2) C1A N1A N3A O1A 178.43(12) N2A C1A N4A N5A -178.20(14) N1A C1A N4A N5A 1.02(19) N2B C1B N1B N3B .9(2) N4B C1B N1B N3B 179.78(11) C1B N1B N3B O1B -175.06(12) C1B N1B N3B O2B 5.01(19) N2B C1B N4B N5B 172.47(13) N1B C1B N4B N5B -6.64(19)