#------------------------------------------------------------------------------ #$Date: 2011-09-28 15:24:46 +0100 (Wed, 28 Sep 2011) $ #$Revision: 26848 $ #$URL: svn://www.crystallography.net/cod/cif/2/20/50/2205035.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_2205035 loop_ _publ_author_name 'Cai-Feng Ding' 'Shu-Sheng Zhang' 'Bing-Qing Tian' 'Xue-Mei Li' 'Hong Xu' 'Ping-Kai Ouyang' _publ_section_title ; Diaquabis(6-nitro-3H-benzimidazol)copper(II) dinitrate ; _journal_issue 2 _journal_name_full 'Acta Crystallographica, Section E' _journal_page_first m235 _journal_page_last m236 _journal_volume 61 _journal_year 2005 _chemical_formula_iupac '[Cu (C7 H5 N3 O2 )2 (H2 O)2 ]2(N O3)' _chemical_formula_moiety '[Cu (C7 H5 N3 O2 )2 (H2 O)2 ]2+, 2 N O3 1-' _chemical_formula_sum 'C14 H14 Cu N8 O12' _chemical_formula_weight 549.87 _chemical_name_systematic ; Diaqua bis(6-nitro-3H-benzimidazol) copper(II) dinitrate ; _symmetry_cell_setting triclinic _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 69.491(2) _cell_angle_beta 78.012(2) _cell_angle_gamma 84.999(2) _cell_formula_units_Z 1 _cell_length_a 7.2372(8) _cell_length_b 8.1279(9) _cell_length_c 9.1779(10) _cell_measurement_reflns_used 2166 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 27.47 _cell_measurement_theta_min 2.41 _cell_volume 494.57(9) _computing_cell_refinement 'SAINT (Siemens, 1996)' _computing_data_collection 'SMART (Siemens, 1996)' _computing_data_reduction SAINT _computing_molecular_graphics SHELXTL _computing_publication_material ; SHELXTL, PARST (Nardelli, 1995) and PLATON (Spek, 2003) ; _computing_structure_refinement SHELXTL _computing_structure_solution 'SHELXTL (Sheldrick, 1997)' _diffrn_ambient_temperature 293(2) _diffrn_detector_area_resol_mean 8.33 _diffrn_measured_fraction_theta_full 0.945 _diffrn_measured_fraction_theta_max 0.945 _diffrn_measurement_device_type 'Bruker SMART 1000 CCD area-detector diffractometer' _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 0.0109 _diffrn_reflns_av_sigmaI/netI 0.0182 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_number 3050 _diffrn_reflns_theta_full 27.50 _diffrn_reflns_theta_max 27.50 _diffrn_reflns_theta_min 2.41 _diffrn_standards_decay_% negligible _diffrn_standards_interval_count none _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 1.192 _exptl_absorpt_correction_T_max 0.9319 _exptl_absorpt_correction_T_min 0.6803 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details '(SADABS; Sheldrick, 1996)' _exptl_crystal_colour blue _exptl_crystal_density_diffrn 1.846 _exptl_crystal_density_method 'not measured' _exptl_crystal_description plate _exptl_crystal_F_000 279 _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.32 _exptl_crystal_size_min 0.06 _refine_diff_density_max 0.363 _refine_diff_density_min -0.255 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.035 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 168 _refine_ls_number_reflns 2155 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.035 _refine_ls_R_factor_all 0.0317 _refine_ls_R_factor_gt 0.0300 _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^)+(0.0487P)^2^+0.2519P] where P = (Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0812 _refine_ls_wR_factor_ref 0.0829 _reflns_number_gt 2051 _reflns_number_total 2155 _reflns_threshold_expression I>2\s(I) _[local]_cod_data_source_file cv6433.cif _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. Automatic conversion script Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius ; _cod_database_code 2205035 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 Cu1 0.5000 0.0000 0.0000 0.02959(12) Uani d S 1 Cu O1W 0.3149(2) 0.1463(2) -0.12950(18) 0.0344(3) Uani d . 1 O O1 0.2300(3) -0.4267(2) 0.84578(19) 0.0665(6) Uani d . 1 O O2 0.3499(3) -0.5052(2) 0.6454(2) 0.0540(4) Uani d . 1 O O3 0.6614(2) 0.2872(2) -0.12636(19) 0.0438(4) Uani d . 1 O O4 0.9286(2) 0.39691(19) -0.2664(2) 0.0518(4) Uani d . 1 O O5 0.9189(2) 0.1407(2) -0.0878(2) 0.0588(5) Uani d . 1 O N1 0.2610(2) 0.2827(2) 0.28790(19) 0.0348(4) Uani d . 1 N H1 0.2253 0.3837 0.2951 0.042 Uiso calc R 1 H N2 0.3813(2) 0.08288(19) 0.17878(17) 0.0316(3) Uani d . 1 N N3 0.2836(3) -0.3933(2) 0.7032(2) 0.0392(4) Uani d . 1 N N4 0.8365(2) 0.2760(2) -0.15957(19) 0.0339(3) Uani d . 1 N C1 0.2495(3) 0.1261(2) 0.4104(2) 0.0289(4) Uani d . 1 C C2 0.1797(3) 0.0858(3) 0.5721(2) 0.0341(4) Uani d . 1 C H2 0.1281 0.1720 0.6144 0.041 Uiso calc R 1 H C3 0.1906(3) -0.0864(3) 0.6657(2) 0.0355(4) Uani d . 1 C H3 0.1462 -0.1200 0.7745 0.043 Uiso calc R 1 H C4 0.2686(3) -0.2118(2) 0.5973(2) 0.0312(4) Uani d . 1 C C5 0.3374(3) -0.1763(2) 0.4369(2) 0.0294(4) Uani d . 1 C H5 0.3872 -0.2636 0.3955 0.035 Uiso calc R 1 H C6 0.3269(2) -0.0012(2) 0.3424(2) 0.0270(3) Uani d . 1 C C7 0.3379(3) 0.2503(2) 0.1549(2) 0.0359(4) Uani d . 1 C H7 0.3588 0.3371 0.0554 0.043 Uiso calc R 1 H H1W1 0.215(4) 0.127(4) -0.101(3) 0.046(8) Uiso d . 1 H H2W1 0.333(4) 0.240(4) -0.179(4) 0.051(8) 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 Cu1 0.0426(2) 0.02300(17) 0.01943(16) 0.00639(12) -0.00433(12) -0.00508(12) O1W 0.0360(8) 0.0308(7) 0.0311(7) -0.0004(6) -0.0071(6) -0.0037(6) O1 0.1113(17) 0.0462(10) 0.0282(8) -0.0007(10) -0.0110(9) 0.0032(7) O2 0.0622(10) 0.0320(8) 0.0473(9) 0.0125(7) 0.0038(8) 0.0005(7) O3 0.0315(7) 0.0478(8) 0.0496(9) 0.0040(6) -0.0039(6) -0.0165(7) O4 0.0462(9) 0.0286(7) 0.0603(10) 0.0001(6) 0.0097(8) -0.0016(7) O5 0.0456(9) 0.0377(8) 0.0687(12) 0.0071(7) -0.0075(8) 0.0081(8) N1 0.0477(9) 0.0234(7) 0.0320(8) 0.0075(6) -0.0064(7) -0.0105(6) N2 0.0459(9) 0.0228(7) 0.0210(7) 0.0051(6) -0.0041(6) -0.0038(6) N3 0.0424(9) 0.0345(9) 0.0313(8) 0.0000(7) -0.0086(7) 0.0009(7) N4 0.0357(8) 0.0282(7) 0.0342(8) 0.0022(6) -0.0028(7) -0.0087(7) C1 0.0322(9) 0.0276(8) 0.0269(8) 0.0032(7) -0.0067(7) -0.0097(7) C2 0.0376(10) 0.0369(10) 0.0294(9) 0.0033(8) -0.0038(7) -0.0157(8) C3 0.0385(10) 0.0415(10) 0.0241(8) -0.0017(8) -0.0034(7) -0.0093(8) C4 0.0321(9) 0.0283(9) 0.0277(9) -0.0001(7) -0.0082(7) -0.0015(7) C5 0.0318(9) 0.0247(8) 0.0281(8) 0.0034(7) -0.0056(7) -0.0057(7) C6 0.0302(8) 0.0264(8) 0.0223(8) 0.0029(6) -0.0053(6) -0.0063(7) C7 0.0524(12) 0.0243(8) 0.0253(9) 0.0057(8) -0.0056(8) -0.0041(7) 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' Cu Cu 0.3201 1.2651 '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 N2 Cu1 N2 . 2_655 180.00(11) yes N2 Cu1 O1W . 2_655 89.89(6) yes N2 Cu1 O1W 2_655 2_655 90.11(6) ? N2 Cu1 O1W . . 90.11(6) yes N2 Cu1 O1W 2_655 . 89.89(6) ? O1W Cu1 O1W 2_655 . 180.00(14) yes Cu1 O1W H1W1 . . 118(2) ? Cu1 O1W H2W1 . . 122(2) ? H1W1 O1W H2W1 . . 113(3) ? C7 N1 C1 . . 107.58(15) ? C7 N1 H1 . . 126.2 ? C1 N1 H1 . . 126.2 ? C7 N2 C6 . . 104.89(15) ? C7 N2 Cu1 . . 121.36(12) ? C6 N2 Cu1 . . 133.74(12) ? O2 N3 O1 . . 122.71(18) ? O2 N3 C4 . . 118.64(17) ? O1 N3 C4 . . 118.65(18) ? O4 N4 O5 . . 119.91(17) ? O4 N4 O3 . . 120.52(16) ? O5 N4 O3 . . 119.55(17) ? N1 C1 C2 . . 131.06(17) ? N1 C1 C6 . . 105.90(15) ? C2 C1 C6 . . 123.03(17) ? C3 C2 C1 . . 116.84(17) ? C3 C2 H2 . . 121.6 ? C1 C2 H2 . . 121.6 ? C2 C3 C4 . . 119.72(17) ? C2 C3 H3 . . 120.1 ? C4 C3 H3 . . 120.1 ? C5 C4 C3 . . 124.84(17) ? C5 C4 N3 . . 117.45(17) ? C3 C4 N3 . . 117.68(17) ? C4 C5 C6 . . 115.23(16) ? C4 C5 H5 . . 122.4 ? C6 C5 H5 . . 122.4 ? C5 C6 N2 . . 131.43(16) ? C5 C6 C1 . . 120.32(16) ? N2 C6 C1 . . 108.25(15) ? N2 C7 N1 . . 113.37(16) ? N2 C7 H7 . . 123.3 ? N1 C7 H7 . . 123.3 ? 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 Cu1 N2 . 1.9931(15) yes Cu1 N2 2_655 1.9931(15) ? Cu1 O1W 2_655 2.0036(14) ? Cu1 O1W . 2.0036(14) yes O1W H1W1 . 0.73(3) ? O1W H2W1 . 0.74(3) ? O1 N3 . 1.223(2) yes O2 N3 . 1.223(2) yes O3 N4 . 1.244(2) ? O4 N4 . 1.240(2) ? O5 N4 . 1.241(2) ? N1 C7 . 1.336(2) yes N1 C1 . 1.367(2) yes N1 H1 . 0.8600 ? N2 C7 . 1.320(2) yes N2 C6 . 1.400(2) yes N3 C4 . 1.464(2) ? C1 C2 . 1.394(3) ? C1 C6 . 1.407(2) ? C2 C3 . 1.368(3) ? C2 H2 . 0.9300 ? C3 C4 . 1.397(3) ? C3 H3 . 0.9300 ? C4 C5 . 1.387(3) ? C5 C6 . 1.388(2) ? C5 H5 . 0.9300 ? C7 H7 . 0.9300 ? 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 O4 2_665 0.86 1.98 2.799(2) 158 yes O1W H1W1 O5 1_455 0.73(3) 2.12(3) 2.814(2) 161(3) yes O1W H1W1 O5 2_655 0.73(3) 2.39(3) 2.882(2) 127(3) yes O1W H2W1 O2 1_564 0.74(3) 2.13(3) 2.857(2) 167(3) yes C7 H7 O1 1_564 0.93 2.47 3.301(2) 149 yes C7 H7 O3 1_555 0.93 2.56 3.050(2) 114 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_site_symmetry_1 _geom_torsion N2 Cu1 N2 C7 2_655 -15E1(10) O1W Cu1 N2 C7 2_655 134.74(17) O1W Cu1 N2 C7 . -45.26(17) N2 Cu1 N2 C6 2_655 3E1(10) O1W Cu1 N2 C6 2_655 -44.79(18) O1W Cu1 N2 C6 . 135.21(18) C7 N1 C1 C2 . -179.3(2) C7 N1 C1 C6 . 0.8(2) N1 C1 C2 C3 . -179.2(2) C6 C1 C2 C3 . 0.6(3) C1 C2 C3 C4 . -0.2(3) C2 C3 C4 C5 . -0.5(3) C2 C3 C4 N3 . 177.78(18) O2 N3 C4 C5 . -2.3(3) O1 N3 C4 C5 . 177.4(2) O2 N3 C4 C3 . 179.35(19) O1 N3 C4 C3 . -1.0(3) C3 C4 C5 C6 . 0.7(3) N3 C4 C5 C6 . -177.52(16) C4 C5 C6 N2 . 179.97(19) C4 C5 C6 C1 . -0.3(3) C7 N2 C6 C5 . -179.9(2) Cu1 N2 C6 C5 . -0.4(3) C7 N2 C6 C1 . 0.3(2) Cu1 N2 C6 C1 . 179.91(14) N1 C1 C6 C5 . 179.52(17) C2 C1 C6 C5 . -0.3(3) N1 C1 C6 N2 . -0.7(2) C2 C1 C6 N2 . 179.44(17) C6 N2 C7 N1 . 0.2(2) Cu1 N2 C7 N1 . -179.44(14) C1 N1 C7 N2 . -0.7(3)