#------------------------------------------------------------------------------ #$Date: 2013-08-29 16:37:19 +0100 (Thu, 29 Aug 2013) $ #$Revision: 88064 $ #$URL: svn://www.crystallography.net/cod/cif/2/20/68/2206859.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_2206859 loop_ _publ_author_name 'Grigoriev, Mikhail S.' 'Moisy, Philippe' 'Den Auwer, Christophe' 'Charushnikova, Iraida A.' _publ_section_title ; Hydrazinium nitrate ; _journal_coeditor_code BR6216 _journal_issue 10 _journal_name_full 'Acta Crystallographica Section E' _journal_page_first i216 _journal_page_last i217 _journal_volume 61 _journal_year 2005 _chemical_formula_iupac 'N2 H5 +, N1 O3 -' _chemical_formula_moiety 'N2 H5 +, N1 O3 -' _chemical_formula_sum 'H5 N3 O3' _chemical_formula_weight 95.07 _chemical_name_systematic ; Hydrazinium nitrate ; _space_group_IT_number 14 _symmetry_cell_setting monoclinic _symmetry_space_group_name_Hall '-P 2yn' _symmetry_space_group_name_H-M 'P 1 21/n 1' _atom_sites_solution_hydrogens difmap _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_method SHELXL-97 _cell_angle_alpha 90.00 _cell_angle_beta 91.340(3) _cell_angle_gamma 90.00 _cell_formula_units_Z 4 _cell_length_a 7.9649(4) _cell_length_b 5.6569(3) _cell_length_c 8.1221(3) _cell_measurement_reflns_used 2616 _cell_measurement_temperature 120(2) _cell_measurement_theta_max 27.44 _cell_measurement_theta_min 3.54 _cell_volume 365.85(3) _computing_cell_refinement 'HKL (Otwinowski & Minor, 1997)' _computing_data_collection 'COLLECT (Nonius, 1998)' _computing_data_reduction HKL _computing_molecular_graphics 'SHELXTL (Sheldrick, 1997b)' _computing_publication_material SHELXTL _computing_structure_refinement 'SHELXL97 (Sheldrick, 1997a)' _computing_structure_solution 'SHELXS97 (Sheldrick, 1997a)' _diffrn_ambient_temperature 120(2) _diffrn_measured_fraction_theta_full 0.982 _diffrn_measured_fraction_theta_max 0.982 _diffrn_measurement_device_type ; Nonius KappaCCD area-detector ; _diffrn_measurement_method '\f and \w' _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 0.0425 _diffrn_reflns_av_sigmaI/netI 0.0341 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_k_max 6 _diffrn_reflns_limit_k_min -7 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_number 2616 _diffrn_reflns_theta_full 27.44 _diffrn_reflns_theta_max 27.44 _diffrn_reflns_theta_min 3.54 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 0.174 _exptl_absorpt_correction_type none _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.726 _exptl_crystal_density_method 'not measured' _exptl_crystal_description fragment _exptl_crystal_F_000 200 _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.15 _refine_diff_density_max 0.185 _refine_diff_density_min -0.263 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.097 _refine_ls_hydrogen_treatment refall _refine_ls_matrix_type full _refine_ls_number_parameters 75 _refine_ls_number_reflns 824 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.097 _refine_ls_R_factor_all 0.0305 _refine_ls_R_factor_gt 0.0281 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w = 1/[\s^2^(Fo^2^)+(0.0338P)^2^+0.0639P] where P = (Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0700 _refine_ls_wR_factor_ref 0.0720 _reflns_number_gt 772 _reflns_number_total 824 _reflns_threshold_expression I>2\s(I) _[local]_cod_data_source_file br6216.cif _[local]_cod_data_source_block I _[local]_cod_cif_authors_sg_H-M 'P 21/n' _cod_database_code 2206859 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -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 N N 0.0061 0.0033 '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' O O 0.0106 0.0060 '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_adp_type _atom_site_calc_flag _atom_site_occupancy _atom_site_type_symbol O1 0.96785(8) 0.23386(12) 0.58479(8) 0.0186(2) Uani d 1 O O2 0.81207(8) 0.10354(12) 0.78062(8) 0.0189(2) Uani d 1 O O3 0.70853(8) 0.13309(12) 0.53166(8) 0.0178(2) Uani d 1 O N1 0.35432(10) 0.34749(14) 0.65521(10) 0.0154(2) Uani d 1 N H1 0.3322(16) 0.295(2) 0.5512(18) 0.022(3) Uiso d 1 H H2 0.4440(16) 0.444(3) 0.6482(16) 0.024(3) Uiso d 1 H N2 0.41983(10) 0.14757(14) 0.74737(10) 0.0149(2) Uani d 1 N H3 0.4431(15) 0.190(2) 0.8492(17) 0.019(3) Uiso d 1 H H4 0.5070(16) 0.091(2) 0.7017(15) 0.019(3) Uiso d 1 H H5 0.3395(17) 0.038(3) 0.7542(16) 0.024(3) Uiso d 1 H N3 0.82928(9) 0.15701(13) 0.63245(9) 0.0137(2) Uani d 1 N 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 O1 0.0148(3) 0.0208(4) 0.0201(4) -0.0039(3) -0.0003(3) -0.0009(3) O2 0.0241(4) 0.0189(4) 0.0136(3) 0.0001(3) -0.0008(3) 0.0023(2) O3 0.0152(3) 0.0219(4) 0.0162(4) -0.0008(2) -0.0044(3) -0.0031(2) N1 0.0163(4) 0.0153(4) 0.0145(4) -0.0007(3) -0.0027(3) 0.0015(3) N2 0.0144(4) 0.0151(4) 0.0151(4) 0.0008(3) -0.0011(3) 0.0007(3) N3 0.0151(4) 0.0114(4) 0.0145(4) 0.0010(3) -0.0018(3) -0.0017(3) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_publ_flag O1 N3 1.2558(10) yes O2 N3 1.2516(10) yes O3 N3 1.2556(10) yes N1 N2 1.4468(11) yes N1 H1 0.909(15) ? N1 H2 0.903(14) ? N2 H3 0.878(14) ? N2 H4 0.856(13) ? N2 H5 0.893(15) ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_publ_flag N2 N1 H1 106.5(8) ? N2 N1 H2 103.3(9) ? H1 N1 H2 106.1(11) ? N1 N2 H3 109.7(9) ? N1 N2 H4 110.6(9) ? H3 N2 H4 110.8(12) ? N1 N2 H5 108.9(9) ? H3 N2 H5 105.6(12) ? H4 N2 H5 111.1(12) ? O2 N3 O3 120.10(7) yes O2 N3 O1 119.79(7) yes O3 N3 O1 120.11(7) 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 H1 N1 N2 H3 180.0(12) H1 N1 N2 H4 57.5(12) H1 N1 N2 H5 -64.8(12) H2 N1 N2 H3 68.5(12) H2 N1 N2 H4 -54.1(13) H2 N1 N2 H5 -176.4(12) 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 N1 H1 O2 4_565 0.909(15) 2.274(14) 3.0657(10) 145.4(11) yes N1 H2 O2 2_656 0.903(14) 2.206(14) 3.0603(11) 157.5(12) yes N2 H3 O1 4_566 0.878(14) 1.966(14) 2.8386(11) 172.6(12) yes N2 H4 O3 . 0.856(13) 2.155(13) 2.9245(10) 149.5(12) yes N2 H5 N1 2_546 0.893(15) 2.035(15) 2.8908(11) 160.1(12) yes _cod_database_fobs_code 2206859