#------------------------------------------------------------------------------ #$Date: 2011-09-10 04:16:28 +0100 (Sat, 10 Sep 2011) $ #$Revision: 25271 $ #$URL: svn://www.crystallography.net/cod/cif/2/2300018.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_2300018 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 H9 N11 O8' _chemical_formula_weight 315.20 _chemical_name_common 'biguanidinium bis-dinitramide' _chemical_name_systematic ; ? ; _space_group_IT_number 15 _symmetry_cell_setting monoclinic _symmetry_space_group_name_Hall '-C 2yc' _symmetry_space_group_name_H-M 'C 1 2/c 1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_method SHELXTL _cell_angle_alpha 90.00 _cell_angle_beta 116.2250(10) _cell_angle_gamma 90.00 _cell_formula_units_Z 4 _cell_length_a 11.8391(9) _cell_length_b 8.1392(6) _cell_length_c 13.0265(10) _cell_measurement_reflns_used 2518 _cell_measurement_temperature 250.0(10) _cell_measurement_theta_max 23.30 _cell_measurement_theta_min 3.99 _cell_volume 1126.04(15) _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 250.0(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 0.0327 _diffrn_reflns_av_sigmaI/netI 0.0370 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_number 3810 _diffrn_reflns_theta_max 28.31 _diffrn_reflns_theta_min 3.15 _exptl_absorpt_coefficient_mu 0.179 _exptl_absorpt_correction_T_max 0.990313 _exptl_absorpt_correction_T_min 0.624536 _exptl_absorpt_correction_type 'Empirical :Multipole Expansion' _exptl_crystal_colour colorless _exptl_crystal_density_diffrn 1.859 _exptl_crystal_density_method '? ' _exptl_crystal_description block _exptl_crystal_F_000 648 _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.20 _refine_diff_density_max 0.317 _refine_diff_density_min -0.318 _refine_ls_extinction_coef 0.0052(19) _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 1.067 _refine_ls_goodness_of_fit_obs 1.117 _refine_ls_matrix_type full _refine_ls_number_parameters 115 _refine_ls_number_reflns 1402 _refine_ls_number_restraints 5 _refine_ls_restrained_S_all 1.071 _refine_ls_restrained_S_obs 1.122 _refine_ls_R_factor_all 0.0582 _refine_ls_R_factor_obs 0.0456 _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^)+(0.0853P)^2^+0.3144P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_wR_factor_all 0.1384 _refine_ls_wR_factor_obs 0.1287 _reflns_number_observed 1128 _reflns_number_total 1402 _reflns_observed_criterion >2sigma(I) _[local]_cod_data_source_file do0021.cif _[local]_cod_data_source_block II250K _[local]_cod_cif_authors_sg_H-M 'C2/c ' _cod_depositor_comments ; The following automatic conversions were performed: '_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic' 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_database_code 2300018 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' 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 C1 0.0244(7) 0.0213(7) 0.0189(7) 0.0027(6) 0.0110(6) 0.0022(5) N1 0.0500(13) 0.0156(9) 0.0454(12) 0.000 0.0378(11) 0.000 N2 0.0353(7) 0.0236(7) 0.0301(7) -0.0023(6) 0.0221(6) -0.0051(5) N3 0.0320(8) 0.0236(8) 0.0329(8) -0.0070(5) 0.0198(7) -0.0077(5) N4 0.0259(7) 0.0226(7) 0.0295(7) -0.0040(5) 0.0128(6) -0.0003(5) N5 0.0402(8) 0.0213(7) 0.0270(7) -0.0062(6) 0.0185(6) -0.0013(5) N6 0.0294(7) 0.0282(8) 0.0241(7) -0.0064(6) 0.0127(6) -0.0017(5) O1 0.0785(11) 0.0436(9) 0.0242(7) -0.0098(7) 0.0223(7) 0.0015(5) O2 0.0398(7) 0.0248(7) 0.0435(8) -0.0021(5) 0.0212(6) -0.0051(5) O3 0.0515(8) 0.0288(7) 0.0426(8) -0.0140(6) 0.0261(7) 0.0026(5) O4 0.0534(8) 0.0360(8) 0.0457(8) -0.0069(6) 0.0315(7) -0.0138(6) 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 C1 0.42459(14) 0.4041(2) 0.29229(12) 0.0210(3) Uani d . 1 C N1 0.5000 0.4751(2) 0.2500 0.0309(5) Uani d SD 1 N N2 0.39198(14) 0.4987(2) 0.35683(12) 0.0269(4) Uani d D 1 N N3 0.38501(13) 0.2526(2) 0.26843(12) 0.0275(4) Uani d D 1 N N4 0.37436(12) 0.1478(2) 0.59969(12) 0.0258(4) Uani d . 1 N N5 0.35366(14) -0.0160(2) 0.58704(12) 0.0281(4) Uani d . 1 N N6 0.35626(12) -0.0866(2) 0.49072(11) 0.0269(4) Uani d . 1 N O1 0.3393(2) -0.0110(2) 0.40435(11) 0.0489(5) Uani d . 1 O O2 0.37022(12) -0.23616(15) 0.50034(11) 0.0350(4) Uani d . 1 O O3 0.40998(14) 0.23416(15) 0.54227(12) 0.0391(4) Uani d . 1 O O4 0.35841(14) 0.2039(2) 0.68119(12) 0.0415(4) Uani d . 1 O H1 0.5000 0.5981(13) 0.2500 0.070(11) Uiso d SD 1 H H2A 0.4291(19) 0.6095(15) 0.3813(18) 0.044(6) Uiso d D 1 H H2B 0.3261(15) 0.465(2) 0.3796(17) 0.041(6) Uiso d D 1 H H3A 0.344(2) 0.201(3) 0.3127(17) 0.049(6) Uiso d D 1 H H3B 0.395(2) 0.186(3) 0.2099(16) 0.060(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_site_symmetry_1 _geom_angle N3 C1 N2 . 121.85(14) N3 C1 N1 . 122.15(14) N2 C1 N1 . 115.98(14) C1 N1 C1 2_655 130.0(2) O3 N4 O4 . 122.12(15) O3 N4 N5 . 125.61(14) O4 N4 N5 . 112.21(13) N4 N5 N6 . 116.20(12) O1 N6 O2 . 123.69(15) O1 N6 N5 . 124.29(15) O2 N6 N5 . 111.89(13) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance C1 N3 . 1.307(2) C1 N2 . 1.317(2) C1 N1 . 1.367(2) N1 C1 2_655 1.367(2) N4 O3 . 1.229(2) N4 O4 . 1.244(2) N4 N5 . 1.352(2) N5 N6 . 1.393(2) N6 O1 . 1.218(2) N6 O2 . 1.228(2)