#------------------------------------------------------------------------------ #$Date: 2011-09-10 06:16:28 +0300 (Sat, 10 Sep 2011) $ #$Revision: 25271 $ #$URL: file:///home/coder/svn-repositories/cod/cif/2/2300009.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_2300009 loop_ _publ_author_name 'Bolotina, Nadezhda B.' 'Hardie, Michaele J.' 'Pinkerton, A. Alan' _publ_section_title ; Energetic materials: variable-temperature crystal structures of two biguanidinium dinitramides ; _journal_issue 6 _journal_name_full 'Journal of Applied Crystallography' _journal_page_first 1334 _journal_page_last 1341 _journal_volume 36 _journal_year 2003 _chemical_formula_sum 'C2 H8 N8 O4' _chemical_formula_weight 208.16 _chemical_name_common 'biguanidinium mono-dinitramide' _chemical_name_systematic ; ? ; _space_group_IT_number 2 _symmetry_cell_setting triclinic _symmetry_space_group_name_Hall '-P 1' _symmetry_space_group_name_H-M 'P -1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_method SHELXTL _cell_angle_alpha 85.236(2) _cell_angle_beta 82.032(2) _cell_angle_gamma 81.190(2) _cell_formula_units_Z 2 _cell_length_a 4.29280(10) _cell_length_b 9.3043(2) _cell_length_c 10.5438(3) _cell_measurement_reflns_used 2330 _cell_measurement_temperature 100.0(10) _cell_measurement_theta_max 22.24 _cell_measurement_theta_min 5.79 _cell_volume 411.326(18) _computing_cell_refinement 'Siemens SAINT, 1996b' _computing_data_collection 'Siemens SMART, 1996a' _computing_data_reduction 'Siemens SAINT, 1996b' _computing_molecular_graphics SHELXTL _computing_publication_material 'SHELXTL and the Toledo cifomatic' _computing_structure_refinement SHELXTL _computing_structure_solution 'SHELXTL (Sheldrick, 1997)' _diffrn_ambient_temperature 100.0(10) _diffrn_measurement_device Platform _diffrn_measurement_method '\w scans' _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 0.0532 _diffrn_reflns_av_sigmaI/netI 0.0651 _diffrn_reflns_limit_h_max 5 _diffrn_reflns_limit_h_min -5 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_number 5628 _diffrn_reflns_theta_max 28.29 _diffrn_reflns_theta_min 1.95 _exptl_absorpt_coefficient_mu 0.153 _exptl_absorpt_correction_T_max 0.990303 _exptl_absorpt_correction_T_min 0.701332 _exptl_absorpt_correction_type 'Empirical :Multipole Expansion' _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.681 _exptl_crystal_density_method 'not measured' _exptl_crystal_description block _exptl_crystal_F_000 216 _exptl_crystal_size_max 0.23 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.06 _refine_diff_density_max 0.362 _refine_diff_density_min -0.406 _refine_ls_extinction_coef 0.030(11) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_method SHELXTL _refine_ls_goodness_of_fit_all 1.068 _refine_ls_goodness_of_fit_obs 1.131 _refine_ls_matrix_type full _refine_ls_number_parameters 160 _refine_ls_number_reflns 2046 _refine_ls_number_restraints 8 _refine_ls_restrained_S_all 1.068 _refine_ls_restrained_S_obs 1.131 _refine_ls_R_factor_all 0.0903 _refine_ls_R_factor_obs 0.0560 _refine_ls_shift/esd_max 0.000 _refine_ls_shift/esd_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0730P)^2^+0.1341P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_wR_factor_all 0.1497 _refine_ls_wR_factor_obs 0.1303 _reflns_number_observed 1425 _reflns_number_total 2046 _reflns_observed_criterion >2sigma(I) _[local]_cod_data_source_file do0021.cif _[local]_cod_data_source_block I100K _[local]_cod_cif_authors_sg_H-M P-1 _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_values 1715 2011-07-08 13:25:40Z adriana ; _cod_original_cell_volume 411.33(2) _cod_database_code 2300009 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' 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 O4 0.0201(9) 0.0070(8) 0.0257(9) 0.0059(6) 0.0012(7) -0.0016(6) N1 0.0150(10) 0.0090(9) 0.0179(10) 0.0036(7) 0.0024(8) -0.0004(7) O3 0.0214(9) 0.0127(8) 0.0207(9) -0.0004(7) 0.0047(7) -0.0011(7) N3 0.0159(10) 0.0097(9) 0.0149(9) 0.0023(7) 0.0001(7) -0.0023(7) O1 0.0175(9) 0.0146(8) 0.0220(9) 0.0053(7) 0.0048(7) -0.0016(7) O2 0.0291(10) 0.0122(9) 0.0262(9) 0.0083(7) 0.0056(8) 0.0068(7) N2 0.0173(10) 0.0111(9) 0.0138(9) 0.0014(8) -0.0005(7) -0.0013(7) N6 0.0253(11) 0.0095(9) 0.0168(10) 0.0014(8) 0.0037(8) -0.0008(8) N8 0.0192(11) 0.0130(10) 0.0188(10) 0.0063(8) 0.0004(8) 0.0010(8) N4 0.0189(10) 0.0086(9) 0.0163(10) 0.0026(8) 0.0015(8) 0.0002(7) C1 0.0161(11) 0.0080(10) 0.0171(11) 0.0022(8) -0.0012(9) -0.0006(8) C2 0.0156(11) 0.0084(10) 0.0176(11) -0.0009(8) -0.0010(8) -0.0026(8) N7 0.0197(11) 0.0129(10) 0.0163(10) 0.0049(8) 0.0023(8) -0.0021(8) N5 0.0319(12) 0.0095(9) 0.0184(10) 0.0029(8) 0.0046(9) -0.0004(8) loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_calc_flag _atom_site_refinement_flags _atom_site_occupancy _atom_site_type_symbol O4 -1.5645(4) 0.7799(2) 0.7444(2) 0.0188(4) Uani d . 1 O N1 -1.1560(5) 0.5867(2) 0.7079(2) 0.0150(4) Uani d . 1 N O3 -1.5460(4) 0.5754(2) 0.8597(2) 0.0192(4) Uani d . 1 O N3 -1.4326(5) 0.6549(2) 0.7695(2) 0.0141(4) Uani d . 1 N O1 -0.7652(4) 0.5940(2) 0.5549(2) 0.0195(4) Uani d . 1 O O2 -1.1286(4) 0.7833(2) 0.5562(2) 0.0250(5) Uani d . 1 O N2 -1.0196(5) 0.6627(2) 0.6019(2) 0.0146(4) Uani d . 1 N N6 -0.5253(5) 1.3140(2) 0.7020(2) 0.0182(5) Uani d D 1 N N8 -1.0239(5) 1.3129(2) 0.9107(2) 0.0183(5) Uani d D 1 N N4 -0.6120(5) 1.1165(2) 0.8550(2) 0.0155(4) Uani d . 1 N C1 -0.5118(5) 1.1720(2) 0.7385(2) 0.0142(5) Uani d . 1 C C2 -0.8257(6) 1.1917(2) 0.9398(2) 0.0139(5) Uani d . 1 C N7 -0.8490(5) 1.1378(2) 1.0607(2) 0.0174(5) Uani d D 1 N N5 -0.3742(5) 1.0770(2) 0.6518(2) 0.0214(5) Uani d D 1 N H7B -1.040(5) 1.171(3) 1.122(2) 0.029(8) Uiso d D 1 H H6A -0.579(8) 1.387(3) 0.769(2) 0.043(9) Uiso d D 1 H H7A -0.695(7) 1.052(3) 1.086(3) 0.050(10) Uiso d D 1 H H5A -0.252(6) 1.108(3) 0.5696(17) 0.025(7) Uiso d D 1 H H8B -1.180(6) 1.352(3) 0.984(2) 0.032(8) Uiso d D 1 H H8A -1.038(8) 1.359(3) 0.8224(15) 0.037(9) Uiso d D 1 H H5B -0.397(8) 0.9720(15) 0.673(3) 0.046(10) Uiso d D 1 H H6B -0.448(7) 1.339(3) 0.6100(13) 0.026(7) Uiso d D 1 H 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' O O 0.0106 0.0060 '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 N3 N1 N2 116.1(2) O4 N3 O3 121.6(2) O4 N3 N1 127.0(2) O3 N3 N1 111.5(2) O2 N2 O1 122.4(2) O2 N2 N1 126.3(2) O1 N2 N1 111.3(2) C1 N4 C2 123.2(2) N4 C1 N5 116.8(2) N4 C1 N6 126.0(2) N5 C1 N6 117.2(2) N7 C2 N8 117.9(2) N7 C2 N4 116.7(2) N8 C2 N4 125.3(2) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance O4 N3 1.238(2) N1 N3 1.363(2) N1 N2 1.381(3) O3 N3 1.247(2) O1 N2 1.239(2) O2 N2 1.233(3) N6 C1 1.340(3) N8 C2 1.345(3) N4 C1 1.333(3) N4 C2 1.346(3) C1 N5 1.338(3) C2 N7 1.326(3)