#------------------------------------------------------------------------------ #$Date: 2011-09-10 04:16:28 +0100 (Sat, 10 Sep 2011) $ #$Revision: 25271 $ #$URL: svn://www.crystallography.net/cod/cif/2/2202630.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_2202630 loop_ _publ_author_name 'Zhang, Rong Lan' 'Zhao, Jian She' 'Shi, Qi Zhen' 'Ng, Seik Weng' _publ_section_title ; Diaquabis(4,5-diazafluoren-9-one-\k^2^N,N')zinc(II) dinitrate ; _journal_issue 7 _journal_name_full 'Acta Crystallographica Section E' _journal_page_first m476 _journal_page_last m477 _journal_volume 59 _journal_year 2003 _chemical_formula_iupac '[Zn (C11 H6 N2 O)2 (H2 O)2] (N O3)2' _chemical_formula_moiety 'C22 H16 N4 O4 Zn 2+, 2N1 O3 1-' _chemical_formula_sum 'C22 H16 N6 O10 Zn' _chemical_formula_weight 589.78 _chemical_name_systematic ; Diaquabis(4,5-diazafluoren-9-one-\k^2^N,N')zinc(II) dinitrate ; _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 SHELXL-97 _cell_angle_alpha 94.909(4) _cell_angle_beta 91.394(4) _cell_angle_gamma 99.860(4) _cell_formula_units_Z 1 _cell_length_a 6.989(2) _cell_length_b 8.283(3) _cell_length_c 10.222(3) _cell_measurement_reflns_used 583 _cell_measurement_temperature 298(2) _cell_measurement_theta_max 23.3 _cell_measurement_theta_min 3.0 _cell_volume 580.4(3) _computing_cell_refinement 'SAINT (Bruker, 1997)' _computing_data_collection 'SMART (Bruker, 1997)' _computing_data_reduction SAINT _computing_molecular_graphics 'ORTEPII (Johnson, 1976)' _computing_publication_material SHELXL97 _computing_structure_refinement 'SHELXL97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS97 (Sheldrick, 1997)' _diffrn_ambient_temperature 298(2) _diffrn_measured_fraction_theta_full 0.91 _diffrn_measured_fraction_theta_max 0.91 _diffrn_measurement_device_type 'Bruker AXS 1K CCD' _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 0.034 _diffrn_reflns_av_sigmaI/netI 0.101 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_k_min -5 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_number 3777 _diffrn_reflns_theta_full 28.3 _diffrn_reflns_theta_max 28.3 _diffrn_reflns_theta_min 2.5 _diffrn_standards_decay_% 0 _exptl_absorpt_coefficient_mu 1.13 _exptl_absorpt_correction_T_max 0.844 _exptl_absorpt_correction_T_min 0.724 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details '(SADABS; Sheldrick, 1996)' _exptl_crystal_colour Yellow _exptl_crystal_density_diffrn 1.69 _exptl_crystal_density_method 'not measured' _exptl_crystal_description Block _exptl_crystal_F_000 300 _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.15 _refine_diff_density_max 0.69 _refine_diff_density_min -0.68 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 0.78 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 186 _refine_ls_number_reflns 2623 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 0.78 _refine_ls_R_factor_all 0.080 _refine_ls_R_factor_gt 0.047 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean <0.001 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w = 1/[\s^2^(Fo^2^)+(0.0431P)^2^] where P = (Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.097 _refine_ls_wR_factor_ref 0.106 _reflns_number_gt 1462 _reflns_number_total 2623 _reflns_threshold_expression I>2\s(I) _[local]_cod_data_source_file fl6042.cif _[local]_cod_data_source_block I _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. '_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 2202630 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' 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_type_symbol Zn1 0.5000 0.5000 0.5000 0.0457(2) Uani d S 1 Zn O1 0.3247(4) 0.7199(3) -0.0513(2) 0.0630(10) Uani d . 1 O O2 0.0408(4) 0.3804(3) 0.7268(3) 0.0660(10) Uani d . 1 O O3 -0.0632(4) 0.1360(4) 0.7704(3) 0.0880(10) Uani d . 1 O O4 -0.0975(4) 0.2023(4) 0.5738(3) 0.0840(10) Uani d . 1 O O1w 0.2504(4) 0.5767(4) 0.5646(3) 0.0540(10) Uani d . 1 O N1 0.3430(4) 0.3900(3) 0.3051(2) 0.0420(10) Uani d . 1 N N2 0.5607(4) 0.7182(3) 0.3891(2) 0.0380(10) Uani d . 1 N N3 -0.0409(4) 0.2381(4) 0.6893(3) 0.0500(10) Uani d . 1 N C1 0.2327(5) 0.2530(5) 0.2529(4) 0.0590(10) Uani d . 1 C C2 0.1519(5) 0.2336(5) 0.1239(4) 0.0590(10) Uani d . 1 C C3 0.1838(5) 0.3646(5) 0.0461(3) 0.0510(10) Uani d . 1 C C4 0.2976(5) 0.5080(4) 0.1002(3) 0.0390(10) Uani d . 1 C C5 0.3703(4) 0.5115(4) 0.2281(3) 0.0370(10) Uani d . 1 C C6 0.3604(5) 0.6745(4) 0.0542(3) 0.0440(10) Uani d . 1 C C7 0.4790(4) 0.6760(4) 0.2698(3) 0.0360(10) Uani d . 1 C C8 0.4755(5) 0.7760(4) 0.1684(3) 0.0400(10) Uani d . 1 C C9 0.5667(5) 0.9356(5) 0.1903(3) 0.0540(10) Uani d . 1 C C10 0.6543(5) 0.9853(5) 0.3144(4) 0.0540(10) Uani d . 1 C C11 0.6497(5) 0.8769(4) 0.4093(3) 0.0460(10) Uani d . 1 C H1w1 0.187(6) 0.516(5) 0.613(4) 0.07(2) Uiso d . 1 H H1w2 0.194(5) 0.628(4) 0.520(3) 0.050(10) Uiso d . 1 H H1 0.2071 0.1647 0.3041 0.070 Uiso calc R 1 H H2 0.0775 0.1337 0.0909 0.071 Uiso calc R 1 H H3 0.1303 0.3556 -0.0390 0.061 Uiso calc R 1 H H9 0.5703 1.0079 0.1253 0.065 Uiso calc R 1 H H10 0.7169 1.0936 0.3334 0.065 Uiso calc R 1 H H11 0.7105 0.9143 0.4909 0.056 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 Zn1 0.0509(4) 0.0449(4) 0.0414(4) 0.0049(3) -0.0058(3) 0.0127(3) O1 0.083(2) 0.063(2) 0.0420(10) 0.006(2) -0.0110(10) 0.0190(10) O2 0.081(2) 0.053(2) 0.059(2) -0.002(2) 0.0100(10) 0.002(2) O3 0.086(2) 0.070(2) 0.111(2) 0.006(2) 0.009(2) 0.044(2) O4 0.097(2) 0.081(2) 0.072(2) 0.028(2) -0.039(2) -0.015(2) O1w 0.053(2) 0.056(2) 0.057(2) 0.011(2) 0.0050(10) 0.022(2) N1 0.048(2) 0.040(2) 0.038(2) 0.003(2) -0.0070(10) 0.0090(10) N2 0.036(2) 0.039(2) 0.039(2) 0.0050(10) -0.002(2) 0.0020(10) N3 0.043(2) 0.048(2) 0.061(2) 0.012(2) 0.002(2) 0.006(2) C1 0.063(3) 0.042(2) 0.066(3) -0.007(2) -0.006(2) 0.016(2) C2 0.061(2) 0.052(3) 0.058(2) -0.007(2) -0.015(2) 0.007(2) C3 0.049(2) 0.059(3) 0.042(2) 0.007(2) -0.008(2) 0.003(2) C4 0.038(2) 0.042(2) 0.035(2) 0.007(2) -0.0040(10) 0.004(2) C5 0.036(2) 0.036(2) 0.037(2) 0.006(2) -0.0030(10) 0.003(2) C6 0.049(2) 0.047(2) 0.038(2) 0.013(2) 0.001(2) 0.007(2) C7 0.034(2) 0.036(2) 0.040(2) 0.009(2) 0.0020(10) 0.006(2) C8 0.043(2) 0.037(2) 0.039(2) 0.007(2) 0.001(2) 0.008(2) C9 0.072(3) 0.041(2) 0.052(2) 0.008(2) 0.002(2) 0.018(2) C10 0.065(2) 0.036(2) 0.058(2) -0.001(2) -0.001(2) 0.005(2) C11 0.047(2) 0.042(2) 0.048(2) 0.004(2) -0.003(2) 0.000(2) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 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' Zn Zn 0.2839 1.4301 '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_site_symmetry_3 _geom_angle _geom_angle_publ_flag O1w Zn1 O1w . 2_666 180.00(10) yes O1w Zn1 N1 . . 90.50(10) yes O1w Zn1 N1 . 2_666 89.50(10) yes O1w Zn1 N2 . . 89.30(10) yes O1w Zn1 N2 . 2_666 90.80(10) yes O1w Zn1 N1 2_666 . 89.50(10) no O1w Zn1 N1 2_666 2_666 90.50(10) no O1w Zn1 N2 2_666 . 90.80(10) no O1w Zn1 N2 2_666 2_666 89.30(10) no N1 Zn1 N1 . 2_666 180.0 yes N1 Zn1 N2 . . 81.30(10) yes N1 Zn1 N2 . 2_666 98.70(10) yes N1 Zn1 N2 2_666 . 98.70(10) no N1 Zn1 N2 2_666 2_666 81.30(10) no N2 Zn1 N2 . 2_666 180.00(10) yes C1 N1 C5 . . 115.2(3) no C1 N1 Zn1 . . 140.2(2) no C5 N1 Zn1 . . 104.5(2) no C7 N2 C11 . . 114.2(3) no C7 N2 Zn1 . . 107.2(2) no C11 N2 Zn1 . . 138.5(2) no O3 N3 O4 . . 121.6(4) no O3 N3 O2 . . 118.2(3) no O4 N3 O2 . . 120.2(3) no N1 C1 C2 . . 123.4(3) no C3 C2 C1 . . 119.6(3) no C4 C3 C2 . . 117.2(3) no C3 C4 C5 . . 117.7(3) no C3 C4 C6 . . 134.3(3) no C5 C4 C6 . . 107.9(3) no N1 C5 C4 . . 126.8(3) no N1 C5 C7 . . 123.7(3) no C4 C5 C7 . . 109.4(3) no O1 C6 C4 . . 127.6(3) no O1 C6 C8 . . 126.9(3) no C4 C6 C8 . . 105.5(3) no N2 C7 C8 . . 127.2(3) no N2 C7 C5 . . 123.3(3) no C8 C7 C5 . . 109.5(3) no C9 C8 C7 . . 117.8(3) no C9 C8 C6 . . 134.5(3) no C7 C8 C6 . . 107.6(3) no C8 C9 C10 . . 117.0(3) no C11 C10 C9 . . 121.0(3) no N2 C11 C10 . . 122.8(3) no Zn1 O1w H1w1 . . 115(3) no Zn1 O1w H1w2 . . 120(3) no H1w1 O1w H1w2 . . 118(4) no N1 C1 H1 . . 118.3 no C2 C1 H1 . . 118.3 no C3 C2 H2 . . 120.2 no C1 C2 H2 . . 120.2 no C4 C3 H3 . . 121.4 no C2 C3 H3 . . 121.4 no C8 C9 H9 . . 121.5 no C10 C9 H9 . . 121.5 no C11 C10 H10 . . 119.5 no C9 C10 H10 . . 119.5 no N2 C11 H11 . . 118.6 no C10 C11 H11 . . 118.6 no 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 Zn1 O1w . 2.061(3) yes Zn1 O1w 2_666 2.061(3) no Zn1 N1 . 2.290(3) yes Zn1 N1 2_666 2.290(3) no Zn1 N2 . 2.201(3) yes Zn1 N2 2_666 2.201(3) no O1 C6 . 1.206(3) no O2 N3 . 1.242(4) no O3 N3 . 1.228(4) no O4 N3 . 1.231(4) no N1 C1 . 1.320(4) no N1 C5 . 1.321(4) no N2 C7 . 1.327(4) no N2 C11 . 1.351(4) no C1 C2 . 1.407(5) no C2 C3 . 1.390(5) no C3 C4 . 1.376(4) no C4 C5 . 1.387(4) no C4 C6 . 1.493(5) no C5 C7 . 1.465(4) no C6 C8 . 1.508(5) no C7 C8 . 1.383(4) no C8 C9 . 1.363(4) no C9 C10 . 1.393(5) no C10 C11 . 1.375(4) no O1w H1w1 . 0.82(4) no O1w H1w2 . 0.79(3) no C1 H1 . 0.93 no C2 H2 . 0.93 no C3 H3 . 0.93 no C9 H9 . 0.93 no C10 H10 . 0.93 no C11 H11 . 0.93 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 O1w H1w1 O2 . 0.82(4) 1.89(4) 2.702(4) 179(4) no O1w H1w2 O4 2_566 0.79(3) 1.97(4) 2.744(4) 167(3) no 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_site_symmetry_1 _geom_torsion _geom_torsion_publ_flag O1w Zn1 N1 C1 . -86.2(4) no O1w Zn1 N1 C1 2_666 93.8(4) no N2 Zn1 N1 C1 . -175.3(4) no N2 Zn1 N1 C1 2_666 4.7(4) no O1w Zn1 N1 C5 . 89.5(2) no O1w Zn1 N1 C5 2_666 -90.5(2) no N2 Zn1 N1 C5 . 0.3(2) no N2 Zn1 N1 C5 2_666 -179.7(2) no O1w Zn1 N2 C7 . -90.9(2) no O1w Zn1 N2 C7 2_666 89.1(2) no N1 Zn1 N2 C7 2_666 179.7(2) no N1 Zn1 N2 C7 . -0.3(2) no O1w Zn1 N2 C11 . 87.0(3) no O1w Zn1 N2 C11 2_666 -93.0(3) no N1 Zn1 N2 C11 2_666 -2.4(3) no N1 Zn1 N2 C11 . 177.6(3) no C5 N1 C1 C2 . 1.3(5) no Zn1 N1 C1 C2 . 176.7(3) no N1 C1 C2 C3 . -1.5(6) no C1 C2 C3 C4 . 1.0(6) no C2 C3 C4 C5 . -0.5(5) no C2 C3 C4 C6 . -177.4(4) no C1 N1 C5 C4 . -0.8(5) no Zn1 N1 C5 C4 . -177.8(3) no C1 N1 C5 C7 . 176.6(3) no Zn1 N1 C5 C7 . -0.4(4) no C3 C4 C5 N1 . 0.5(5) no C6 C4 C5 N1 . 178.1(3) no C3 C4 C5 C7 . -177.2(3) no C6 C4 C5 C7 . 0.4(4) no C3 C4 C6 O1 . -2.4(6) no C5 C4 C6 O1 . -179.5(3) no C3 C4 C6 C8 . 176.6(4) no C5 C4 C6 C8 . -0.5(3) no C11 N2 C7 C8 . -0.5(5) no Zn1 N2 C7 C8 . 178.0(3) no C11 N2 C7 C5 . -178.3(3) no Zn1 N2 C7 C5 . 0.2(4) no N1 C5 C7 N2 . 0.2(5) no C4 C5 C7 N2 . 177.9(3) no N1 C5 C7 C8 . -178.0(3) no C4 C5 C7 C8 . -0.2(4) no N2 C7 C8 C9 . 0.7(5) no C5 C7 C8 C9 . 178.8(3) no N2 C7 C8 C6 . -178.2(3) no C5 C7 C8 C6 . -0.1(4) no O1 C6 C8 C9 . 0.7(6) no C4 C6 C8 C9 . -178.3(4) no O1 C6 C8 C7 . 179.4(3) no C4 C6 C8 C7 . 0.4(3) no C7 C8 C9 C10 . -0.8(5) no C6 C8 C9 C10 . 177.8(4) no C8 C9 C10 C11 . 0.6(5) no C7 N2 C11 C10 . 0.3(5) no Zn1 N2 C11 C10 . -177.5(3) no C9 C10 C11 N2 . -0.4(6) no