#------------------------------------------------------------------------------ #$Date: 2010-05-06 08:38:22 +0300 (Thu, 06 May 2010) $ #$Revision: 1153 $ #$URL: file:///home/coder/svn-repositories/cod/cif/2/2101847.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_2101847 _journal_name_full 'Acta Crystallographica, Section B' _journal_volume 53 _space_group_IT_number 15 _symmetry_space_group_name_Hall '-C 2yc' _symmetry_space_group_name_H-M 'C 1 2/c 1' _[local]_cod_cif_authors_sg_H-M 'C 2/c' loop_ _publ_author_name 'Pinkerton, A. Alan' _publ_section_title ' ?' _journal_issue 3 _journal_page_first 504 _journal_page_last 512 _journal_year 1997 _chemical_formula_sum 'C2 H9 N11 O8' _chemical_formula_weight 315.20 _chemical_name_common 'Biguanidinium bis-dinitramide' _chemical_name_systematic ; ? ; _symmetry_cell_setting Monoclinic _audit_creation_method SHELXL _cell_angle_alpha 90.00 _cell_angle_beta 115.790(10) _cell_angle_gamma 90.00 _cell_formula_units_Z 4 _cell_length_a 11.892(2) _cell_length_b 8.1310(10) _cell_length_c 13.038(2) _cell_measurement_reflns_used 25 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 50 _cell_measurement_theta_min 39 _cell_volume 1135.1(3) _computing_cell_refinement 'P3/PC (Siemens, 1989a)' _computing_data_collection 'P3/PC (Siemens, 1989a)' _computing_data_reduction 'XDISK (Siemens, 1989b)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 1985)' _computing_publication_material 'SHELXTL (Sheldrick, 1985)' _computing_structure_refinement 'SHELXL-92 (Sheldrick, 1992)' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _diffrn_ambient_temperature 293(2) _diffrn_measurement_device 'Siemens R3m/V' _diffrn_measurement_method \q/2\q _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.54178 _diffrn_reflns_av_R_equivalents 0.0211 _diffrn_reflns_av_sigmaI/netI 0.0151 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_k_max 0 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_number 927 _diffrn_reflns_theta_max 60.05 _diffrn_reflns_theta_min 6.84 _diffrn_standards_decay_% 0.50 _diffrn_standards_interval_count 100 _diffrn_standards_number 3 _exptl_absorpt_coefficient_mu 1.59 _exptl_absorpt_correction_type none _exptl_crystal_colour colorless _exptl_crystal_density_diffrn 1.844 _exptl_crystal_description 'Clear chunky bipyramids' _exptl_crystal_F_000 648 _exptl_crystal_size_max 0.38 _exptl_crystal_size_mid 0.36 _exptl_crystal_size_min 0.22 _refine_diff_density_max 0.314 _refine_diff_density_min -0.403 _refine_ls_extinction_coef 0.034(3) _refine_ls_extinction_method 'SHELXL (SHeldrick, 1985)' _refine_ls_goodness_of_fit_all 1.128 _refine_ls_goodness_of_fit_obs 1.137 _refine_ls_hydrogen_treatment refall _refine_ls_matrix_type full _refine_ls_number_parameters 115 _refine_ls_number_reflns 845 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.128 _refine_ls_restrained_S_obs 1.137 _refine_ls_R_factor_all 0.0542 _refine_ls_R_factor_obs 0.0533 _refine_ls_shift/esd_max 0.000 _refine_ls_shift/esd_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_scheme 'w = 1/[\s^2^(Fo^2^)+(0.0962P)^2^+0.9237P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_wR_factor_all 0.1379 _refine_ls_wR_factor_obs 0.1360 _reflns_number_observed 812 _reflns_number_total 845 _reflns_observed_criterion >2sigma(I) _[local]_cod_data_source_file bk0035.cif 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_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 N1 0.1469(2) -0.4843(2) 0.9129(2) 0.0316(6) Uani d . 1 N N2 0.1446(2) -0.4146(2) 1.00920(15) 0.0302(6) Uani d . 1 N O1 0.1625(2) -0.4891(2) 1.09534(15) 0.0580(7) Uani d . 1 O O2 0.1298(2) -0.2645(2) 0.99970(15) 0.0407(6) Uani d . 1 O N3 0.1257(2) -0.6478(2) 0.90013(15) 0.0287(6) Uani d . 1 N O3 0.0901(2) -0.7336(2) 0.9577(2) 0.0456(6) Uani d . 1 O O4 0.1413(2) -0.7042(2) 0.8189(2) 0.0502(7) Uani d . 1 O N4 0.0000 -0.0261(3) 0.7500 0.0339(8) Uani d S 1 N H4 0.0000 0.074(5) 0.7500 0.043(10) Uiso d S 1 H C1 0.0750(2) -0.0959(2) 0.7074(2) 0.0223(6) Uani d . 1 C N5 0.1071(2) -0.0021(2) 0.6427(2) 0.0298(6) Uani d . 1 N H5A 0.073(3) 0.095(4) 0.619(2) 0.042(7) Uiso d . 1 H H5B 0.165(3) -0.036(3) 0.622(2) 0.045(7) Uiso d . 1 H N6 0.1139(2) -0.2471(2) 0.7307(2) 0.0317(6) Uani d . 1 N H6A 0.109(3) -0.300(4) 0.783(3) 0.045(8) Uiso d . 1 H H6B 0.153(3) -0.285(4) 0.691(3) 0.056(9) Uiso d . 1 H 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 N1 0.0432(12) 0.0238(11) 0.0319(11) -0.0064(8) 0.0202(9) -0.0009(7) N2 0.0289(10) 0.0329(12) 0.0286(11) -0.0082(7) 0.0123(8) -0.0020(8) O1 0.091(2) 0.0521(13) 0.0302(11) -0.0122(10) 0.0261(10) 0.0018(8) O2 0.0422(11) 0.0293(10) 0.0539(12) -0.0025(7) 0.0241(9) -0.0062(7) N3 0.0247(10) 0.0277(11) 0.0335(11) -0.0043(7) 0.0123(8) 0.0000(7) O3 0.0570(12) 0.0339(11) 0.0517(12) -0.0173(8) 0.0291(10) 0.0023(8) O4 0.0633(12) 0.0423(12) 0.0583(13) -0.0093(9) 0.0389(10) -0.0174(9) N4 0.051(2) 0.0163(13) 0.053(2) 0.000 0.0404(15) 0.000 C1 0.0224(10) 0.0226(11) 0.0220(11) -0.0027(8) 0.0098(9) -0.0026(8) N5 0.0369(11) 0.0266(12) 0.0352(12) 0.0046(8) 0.0243(10) 0.0056(8) N6 0.0340(12) 0.0288(12) 0.0393(12) 0.0085(8) 0.0222(10) 0.0101(9) 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 N1 N3 . 1.350(3) yes N1 N2 . 1.388(3) yes N2 O1 . 1.211(2) yes N2 O2 . 1.231(2) yes N3 O3 . 1.227(2) yes N3 O4 . 1.240(2) yes N4 C1 2_556 1.363(2) yes N4 C1 . 1.363(2) yes C1 N6 . 1.302(3) yes C1 N5 . 1.312(3) yes 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 _geom_angle_publ_flag N3 N1 N2 . 116.0(2) yes O1 N2 O2 . 123.3(2) yes O1 N2 N1 . 124.7(2) yes O2 N2 N1 . 111.8(2) yes O3 N3 O4 . 122.2(2) yes O3 N3 N1 . 125.4(2) yes O4 N3 N1 . 112.3(2) yes C1 N4 C1 2_556 130.8(3) yes N6 C1 N5 . 121.8(2) yes N6 C1 N4 . 121.8(2) yes N5 C1 N4 . 116.4(2) yes _cod_database_code 2101847