#------------------------------------------------------------------------------ #$Date: 2012-02-03 19:16:24 +0200 (Fri, 03 Feb 2012) $ #$Revision: 32112 $ #$URL: file:///home/coder/svn-repositories/cod/cif/2/01/38/2013804.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_2013804 loop_ _publ_author_name 'Glidewell, Christopher' 'Low, John N.' 'Skakle, Janet M. S.' 'Wardell, James L.' _publ_section_title ; Hydrogen bonding in nitroaniline analogues: 4-nitrobenzaldehyde hydrazone forms hydrogen-bonded sheets of R_4^4(26) rings ; _journal_issue 1 _journal_name_full 'Acta Crystallographica Section C' _journal_page_first o33 _journal_page_last o34 _journal_volume 60 _journal_year 2004 _chemical_formula_iupac 'C7 H7 N3 O2' _chemical_formula_moiety 'C7 H7 N3 O2' _chemical_formula_sum 'C7 H7 N3 O2' _chemical_formula_weight 165.16 _chemical_name_systematic ; 4-Nitrobenzaldehyde hydrazone ; _space_group_IT_number 7 _symmetry_cell_setting monoclinic _symmetry_space_group_name_Hall 'P -2yc' _symmetry_space_group_name_H-M 'P 1 c 1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _cell_angle_alpha 90.00 _cell_angle_beta 95.064(2) _cell_angle_gamma 90.00 _cell_formula_units_Z 2 _cell_length_a 3.7070(2) _cell_length_b 6.3963(3) _cell_length_c 15.4047(10) _cell_measurement_reflns_used 829 _cell_measurement_temperature 120(2) _cell_measurement_theta_max 27.36 _cell_measurement_theta_min 3.18 _cell_volume 363.84(4) _computing_cell_refinement 'DENZO--SMN (Otwinowski & Minor, 1997)' _computing_data_collection 'KappaCCD Server Software (Nonius, 1997)' _computing_data_reduction DENZO--SMN _computing_molecular_graphics ' PLATON (Spek, 2003)' _computing_publication_material 'SHELXL97 and PRPKAPPA (Ferguson, 1999)' _computing_structure_refinement 'OSCAIL andSHELXL97 (Sheldrick, 1997)' _computing_structure_solution 'OSCAIL (McArdle, 2003) and SHELXS97 (Sheldrick, 1997)' _diffrn_ambient_temperature 120(2) _diffrn_measured_fraction_theta_full 0.996 _diffrn_measured_fraction_theta_max 0.996 _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_method '\f scans, and \w scans with \k offsets' _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'fine-focus sealed X-ray tube' _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0711 _diffrn_reflns_av_sigmaI/netI 0.0399 _diffrn_reflns_limit_h_max 4 _diffrn_reflns_limit_h_min -4 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_number 4784 _diffrn_reflns_theta_full 27.36 _diffrn_reflns_theta_max 27.36 _diffrn_reflns_theta_min 3.18 _diffrn_standards_decay_% negligible _exptl_absorpt_coefficient_mu 0.115 _exptl_absorpt_correction_T_max 0.994 _exptl_absorpt_correction_T_min 0.967 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details '(SORTAV; Blessing, 1995, 1997)' _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.508 _exptl_crystal_density_method 'not measured' _exptl_crystal_description plate _exptl_crystal_F_000 172 _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.05 _refine_diff_density_max 0.248 _refine_diff_density_min -0.236 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.165 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 109 _refine_ls_number_reflns 829 _refine_ls_number_restraints 2 _refine_ls_restrained_S_all 1.164 _refine_ls_R_factor_all 0.0473 _refine_ls_R_factor_gt 0.0402 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0357P)^2^+0.1524P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0964 _refine_ls_wR_factor_ref 0.1018 _reflns_number_gt 765 _reflns_number_total 829 _reflns_threshold_expression I>2\s(I) _[local]_cod_data_source_file gg1201.cif _[local]_cod_data_source_block I _[local]_cod_cif_authors_sg_H-M 'P c' _cod_depositor_comments ; The following automatic conversions were performed: '_exptl_absorpt_correction_type' value 'Multi-scan' changed to 'multi-scan' 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 2013804 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x, -y, z+1/2' 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 C1 0.4362(7) 0.2888(5) 0.32040(19) 0.0193(6) Uani d . 1 . . C C2 0.4310(7) 0.1965(5) 0.40249(19) 0.0220(6) Uani d . 1 . . C C3 0.3088(8) 0.3066(5) 0.4712(2) 0.0216(6) Uani d . 1 . . C C4 0.1947(7) 0.5132(5) 0.4569(2) 0.0195(6) Uani d . 1 . . C C5 0.2066(7) 0.6112(5) 0.37713(19) 0.0221(6) Uani d . 1 . . C C6 0.3267(8) 0.4974(5) 0.30925(19) 0.0230(7) Uani d . 1 . . C C11 0.5515(7) 0.1757(5) 0.24483(19) 0.0220(6) Uani d . 1 . . C N4 0.0612(7) 0.6280(4) 0.52911(17) 0.0235(6) Uani d . 1 . . N N11 0.6376(7) -0.0166(4) 0.24894(16) 0.0245(6) Uani d . 1 . . N N12 0.7161(8) -0.1091(4) 0.17187(19) 0.0293(6) Uani d . 1 . . N O1 -0.0046(8) 0.8169(3) 0.51917(18) 0.0382(6) Uani d . 1 . . O O2 0.0131(6) 0.5344(4) 0.59654(15) 0.0310(6) Uani d . 1 . . O H2 0.5106 0.0595 0.4109 0.026 Uiso calc R 1 . . H H3 0.3024 0.2449 0.5257 0.026 Uiso calc R 1 . . H H5 0.1357 0.7499 0.3695 0.027 Uiso calc R 1 . . H H6 0.3351 0.5604 0.2551 0.028 Uiso calc R 1 . . H H11 0.5620 0.2466 0.1924 0.026 Uiso calc R 1 . . H H12A 0.7053 -0.0369 0.1246 0.035 Uiso calc R 1 . . H H12B 0.7759 -0.2390 0.1711 0.035 Uiso calc R 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 C1 0.0157(14) 0.0191(15) 0.0229(14) -0.0021(11) -0.0005(11) -0.0015(12) C2 0.0211(16) 0.0191(14) 0.0256(15) -0.0005(12) 0.0010(13) 0.0015(12) C3 0.0237(15) 0.0209(15) 0.0198(13) -0.0030(12) 0.0003(11) 0.0019(12) C4 0.0178(14) 0.0190(13) 0.0216(13) -0.0019(11) 0.0011(11) -0.0034(12) C5 0.0236(16) 0.0190(13) 0.0234(16) -0.0009(13) -0.0003(12) -0.0008(12) C6 0.0276(16) 0.0206(14) 0.0203(14) -0.0017(12) -0.0007(12) 0.0023(12) C11 0.0232(16) 0.0234(14) 0.0194(14) -0.0030(13) 0.0016(12) 0.0016(12) N4 0.0233(14) 0.0237(13) 0.0234(13) -0.0014(10) 0.0012(11) -0.0021(12) N11 0.0262(13) 0.0226(13) 0.0250(14) 0.0009(11) 0.0043(11) -0.0025(11) N12 0.0377(16) 0.0235(14) 0.0270(13) 0.0025(11) 0.0049(11) -0.0036(11) O1 0.0588(17) 0.0232(11) 0.0337(12) 0.0065(12) 0.0109(12) -0.0036(10) O2 0.0422(14) 0.0289(11) 0.0228(11) 0.0001(10) 0.0076(10) -0.0001(10) 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 C1 C2 . 1.397(4) y C2 C3 . 1.381(4) y C3 C4 . 1.399(4) y C4 C5 . 1.383(4) y C5 C6 . 1.380(4) y C6 C1 . 1.401(4) y C1 C11 . 1.466(4) y C11 N11 . 1.271(4) y N11 N12 . 1.380(4) y C4 N4 . 1.456(4) y N4 O1 . 1.239(3) y N4 O2 . 1.226(3) y C2 H2 . 0.93 no C3 H3 . 0.93 no C5 H5 . 0.93 no C6 H6 . 0.93 no C11 H11 . 0.93 no N12 H12A . 0.86 no N12 H12B . 0.86 no 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 0.0000 '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 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0000 '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 _geom_angle_publ_flag C2 C1 C6 119.1(3) no C2 C1 C11 122.6(3) no C6 C1 C11 118.3(3) no C3 C2 C1 120.7(3) no C3 C2 H2 119.7 no C1 C2 H2 119.7 no C2 C3 C4 118.4(3) no C2 C3 H3 120.8 no C4 C3 H3 120.8 no C5 C4 C3 122.4(3) no C5 C4 N4 119.3(3) no C3 C4 N4 118.3(3) no C6 C5 C4 118.2(3) no C6 C5 H5 120.9 no C4 C5 H5 120.9 no C5 C6 C1 121.3(3) no C5 C6 H6 119.4 no C1 C6 H6 119.4 no N11 C11 C1 121.8(3) no N11 C11 H11 119.1 no C1 C11 H11 119.1 no C11 N11 N12 116.3(3) no N11 N12 H12A 120.0 no N11 N12 H12B 120.0 no H12A N12 H12B 120.0 no O2 N4 O1 122.6(3) no O2 N4 C4 119.1(3) no O1 N4 C4 118.3(3) no 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 N12 H12A O1 2_664 0.86 2.47 3.245(4) 151 y N12 H12B O2 2_654 0.86 2.42 3.191(4) 150 y 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 _geom_torsion_publ_flag C6 C1 C2 C3 2.1(4) no C11 C1 C2 C3 -177.8(3) no C1 C2 C3 C4 -0.8(4) no C2 C3 C4 C5 -1.2(4) no C2 C3 C4 N4 179.2(3) no C3 C4 C5 C6 1.8(4) no N4 C4 C5 C6 -178.6(3) no C4 C5 C6 C1 -0.4(4) no C2 C1 C6 C5 -1.5(4) no C11 C1 C6 C5 178.4(3) no C2 C1 C11 N11 3.3(4) no C6 C1 C11 N11 -176.5(3) no C1 C11 N11 N12 175.5(3) no C5 C4 N4 O2 172.0(3) no C3 C4 N4 O2 -8.4(4) no C5 C4 N4 O1 -6.9(4) no C3 C4 N4 O1 172.7(3) no