#------------------------------------------------------------------------------ #$Date: 2012-02-26 23:34:47 +0200 (Sun, 26 Feb 2012) $ #$Revision: 35909 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/20/58/7205859.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_7205859 loop_ _publ_author_name 'Fang, Zhen-Lan' 'Yu, Rong-Min' 'Zhang, Jie' 'Lu, Can-Zhong' _publ_section_title ; Novel ligands and complexes in situ generated from the copper-mediated conversions of 2,5-bis(2-hydroxyphenyl)-1,3,4-oxadiazole: structures and magnetic properties ; _journal_issue 12 _journal_name_full CrystEngComm _journal_page_first 4032 _journal_volume 13 _journal_year 2011 _chemical_formula_moiety 'C14 H14 Cu2 N4 O5' _chemical_formula_sum 'C14 H14 Cu2 N4 O5' _chemical_formula_weight 445.39 _chemical_name_systematic ; ? ; _space_group_IT_number 15 _symmetry_cell_setting monoclinic _symmetry_space_group_name_Hall '-C 2yc' _symmetry_space_group_name_H-M 'C 1 2/c 1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_method SHELXL-97 _cell_angle_alpha 90.00 _cell_angle_beta 105.577(5) _cell_angle_gamma 90.00 _cell_formula_units_Z 4 _cell_length_a 20.435(3) _cell_length_b 4.9321(4) _cell_length_c 15.875(2) _cell_measurement_temperature 293(2) _cell_volume 1541.2(3) _computing_cell_refinement 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_data_collection 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_data_reduction 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_molecular_graphics 'SHELXL-97 (Sheldrick, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _diffrn_ambient_temperature 293(2) _diffrn_detector_area_resol_mean 14.6306 _diffrn_measured_fraction_theta_full 0.998 _diffrn_measured_fraction_theta_max 0.998 _diffrn_measurement_device_type Mercury70 _diffrn_measurement_method CCD_Profile_fitting _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 0.0359 _diffrn_reflns_av_sigmaI/netI 0.0359 _diffrn_reflns_limit_h_max 26 _diffrn_reflns_limit_h_min -26 _diffrn_reflns_limit_k_max 6 _diffrn_reflns_limit_k_min -4 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_number 5683 _diffrn_reflns_theta_full 27.46 _diffrn_reflns_theta_max 27.46 _diffrn_reflns_theta_min 2.66 _exptl_absorpt_coefficient_mu 2.795 _exptl_absorpt_correction_T_max 0.869 _exptl_absorpt_correction_T_min 0.764 _exptl_absorpt_correction_type multi-scan _exptl_crystal_colour green _exptl_crystal_density_diffrn 1.919 _exptl_crystal_density_method 'not measured' _exptl_crystal_description needle _exptl_crystal_F_000 896 _exptl_crystal_size_max 0.1600 _exptl_crystal_size_mid 0.0800 _exptl_crystal_size_min 0.0500 _refine_diff_density_max 0.967 _refine_diff_density_min -0.508 _refine_diff_density_rms 0.126 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.073 _refine_ls_hydrogen_treatment conster _refine_ls_matrix_type full _refine_ls_number_parameters 124 _refine_ls_number_reflns 1780 _refine_ls_number_restraints 5 _refine_ls_restrained_S_all 1.072 _refine_ls_R_factor_all 0.0672 _refine_ls_R_factor_gt 0.0534 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1007P)^2^+2.4442P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1552 _refine_ls_wR_factor_ref 0.1672 _reflns_number_gt 1419 _reflns_number_total 1777 _reflns_threshold_expression >2sigma(I) _[local]_cod_data_source_file c0ce00907e.txt _[local]_cod_data_source_block 3 _[local]_cod_cif_authors_sg_H-M 'C 2/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_enum 1555 2011-01-17 13:19:09Z saulius ; _cod_original_cell_volume 1541.3(3) _cod_database_code 7205859 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_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu1 Cu 0.46885(3) 0.26427(10) 0.59875(3) 0.0325(3) Uani 1 1 d . . . N2 N 0.40254(16) -0.0161(7) 0.5448(2) 0.0224(7) Uani 1 1 d . . . O2 O 0.45818(16) -0.5118(6) 0.35124(19) 0.0372(8) Uani 1 1 d . . . N1 N 0.48227(18) -0.1014(7) 0.4730(2) 0.0306(8) Uani 1 1 d . . . C7 C 0.4220(2) -0.1501(10) 0.4860(3) 0.0326(9) Uani 1 1 d . . . C6 C 0.3796(2) -0.3607(9) 0.4339(3) 0.0306(9) Uani 1 1 d . . . O3 O 0.4052(2) 0.4440(10) 0.6543(3) 0.0614(11) Uani 1 1 d D . . H3B H 0.417(4) 0.403(18) 0.7080(15) 0.092 Uiso 1 1 d D . . H3C H 0.3630(10) 0.412(18) 0.640(5) 0.092 Uiso 1 1 d D . . C5 C 0.3139(2) -0.3900(11) 0.4452(3) 0.0415(11) Uani 1 1 d . . . H5A H 0.3008 -0.2769 0.4847 0.050 Uiso 1 1 calc R . . C4 C 0.2687(3) -0.5784(12) 0.4005(3) 0.0510(13) Uani 1 1 d . . . H4A H 0.2258 -0.5931 0.4098 0.061 Uiso 1 1 calc R . . C3 C 0.2875(3) -0.7476(10) 0.3411(4) 0.0466(14) Uani 1 1 d . . . H3A H 0.2576 -0.8789 0.3109 0.056 Uiso 1 1 calc R . . C2 C 0.3515(3) -0.7186(10) 0.3271(3) 0.0403(12) Uani 1 1 d . . . H2A H 0.3633 -0.8312 0.2865 0.048 Uiso 1 1 calc R . . C1 C 0.3989(2) -0.5267(9) 0.3715(3) 0.0322(9) Uani 1 1 d . . . O4 O 0.5000 -0.0678(12) 0.7500 0.0607(16) Uani 1 2 d SD . . H1 H 0.509(3) -0.176(10) 0.714(3) 0.043(15) Uiso 1 1 d D . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.0348(4) 0.0335(4) 0.0317(4) -0.0080(2) 0.0133(3) -0.0046(2) N2 0.0208(16) 0.0282(17) 0.0208(15) -0.0078(13) 0.0103(12) -0.0045(12) O2 0.0408(19) 0.0389(19) 0.0350(17) -0.0090(14) 0.0156(14) -0.0107(14) N1 0.0294(19) 0.031(2) 0.0316(19) -0.0087(15) 0.0094(15) -0.0071(14) C7 0.032(2) 0.034(2) 0.031(2) 0.0022(19) 0.0081(18) 0.0002(18) C6 0.031(2) 0.033(2) 0.028(2) -0.0021(18) 0.0077(17) -0.0044(18) O3 0.054(3) 0.074(3) 0.059(2) -0.018(2) 0.021(2) -0.006(2) C5 0.037(3) 0.046(3) 0.042(3) -0.010(2) 0.012(2) -0.008(2) C4 0.039(3) 0.059(3) 0.054(3) -0.003(3) 0.012(2) -0.015(2) C3 0.048(3) 0.049(3) 0.038(3) -0.006(2) 0.003(2) -0.023(2) C2 0.051(3) 0.041(3) 0.028(2) -0.0047(19) 0.009(2) -0.008(2) C1 0.038(2) 0.031(2) 0.027(2) 0.0013(17) 0.0081(18) -0.0067(18) O4 0.077(4) 0.039(3) 0.058(4) 0.000 0.003(3) 0.000 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 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Cu1 O2 92.41(14) 5_656 5_656 ? N1 Cu1 N2 81.48(13) 5_656 . ? O2 Cu1 N2 173.29(12) 5_656 . ? N1 Cu1 O3 169.87(17) 5_656 . ? O2 Cu1 O3 93.52(16) 5_656 . ? N2 Cu1 O3 92.93(16) . . ? C7 N2 Cu1 111.5(3) . . ? C1 O2 Cu1 126.0(3) . 5_656 ? C7 N1 N1 112.8(4) . 5_656 ? C7 N1 Cu1 133.1(3) . 5_656 ? N1 N1 Cu1 114.0(3) 5_656 5_656 ? N2 C7 N1 120.0(4) . . ? N2 C7 C6 121.6(4) . . ? N1 C7 C6 118.4(4) . . ? C5 C6 C1 118.8(4) . . ? C5 C6 C7 116.2(4) . . ? C1 C6 C7 124.9(4) . . ? Cu1 O3 H3B 108(6) . . ? Cu1 O3 H3C 123(6) . . ? H3B O3 H3C 103(7) . . ? C4 C5 C6 122.5(5) . . ? C4 C5 H5A 118.7 . . ? C6 C5 H5A 118.7 . . ? C5 C4 C3 119.4(5) . . ? C5 C4 H4A 120.3 . . ? C3 C4 H4A 120.3 . . ? C4 C3 C2 119.3(5) . . ? C4 C3 H3A 120.4 . . ? C2 C3 H3A 120.4 . . ? C3 C2 C1 122.8(5) . . ? C3 C2 H2A 118.6 . . ? C1 C2 H2A 118.6 . . ? O2 C1 C2 117.7(4) . . ? O2 C1 C6 125.2(4) . . ? C2 C1 C6 117.2(4) . . ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 N1 1.885(3) 5_656 ? Cu1 O2 1.926(3) 5_656 ? Cu1 N2 1.965(3) . ? Cu1 O3 1.967(4) . ? N2 C7 1.290(5) . ? O2 C1 1.337(5) . ? O2 Cu1 1.926(3) 5_656 ? N1 C7 1.325(5) . ? N1 N1 1.388(7) 5_656 ? N1 Cu1 1.885(3) 5_656 ? C7 C6 1.459(7) . ? C6 C5 1.408(6) . ? C6 C1 1.420(6) . ? O3 H3B 0.846(7) . ? O3 H3C 0.845(7) . ? C5 C4 1.367(7) . ? C5 H5A 0.9300 . ? C4 C3 1.388(8) . ? C4 H4A 0.9300 . ? C3 C2 1.391(8) . ? C3 H3A 0.9300 . ? C2 C1 1.402(6) . ? C2 H2A 0.9300 . ? O4 H1 0.836(10) . ?