#------------------------------------------------------------------------------ #$Date: 2012-02-03 19:16:24 +0200 (Fri, 03 Feb 2012) $ #$Revision: 32112 $ #$URL: file:///home/coder/svn-repositories/cod/cif/2/01/26/2012641.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_2012641 loop_ _publ_author_name 'Tong, Ming-Liang' 'Li, Wei' 'Chen, Xiao-Ming' 'Zheng, Shao-Liang' 'Ng, Seik Weng' _publ_section_title Tetra-\m-acetato-\k^2^O:O'-bis[(4-phenylpyridine-\kN)copper(II)] _journal_issue 4 _journal_name_full 'Acta Crystallographica Section C' _journal_page_first m232 _journal_page_last m234 _journal_volume 58 _journal_year 2002 _chemical_formula_iupac '[Cu2 (C2 H3 O2)4 (C11 H9 N)2]' _chemical_formula_moiety 'C30 H30 Cu2 N2 O8' _chemical_formula_sum 'C30 H30 Cu2 N2 O8' _chemical_formula_weight 673.64 _chemical_name_systematic ; Tetra-\m-acetato-\k^2^O:O'-bis[(4-phenylpyridine-\kN)copper(II)] ; _space_group_IT_number 88 _symmetry_cell_setting tetragonal _symmetry_space_group_name_Hall '-I 4ad' _symmetry_space_group_name_H-M 'I 41/a :2' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_method SHELXL97 _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_formula_units_Z 8 _cell_length_a 20.598(4) _cell_length_b 20.598(4) _cell_length_c 14.070(8) _cell_measurement_reflns_used 25 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 15 _cell_measurement_theta_min 7 _cell_volume 5970(4) _computing_cell_refinement 'R3m Software' _computing_data_collection 'R3m Software (Siemens, 1990)' _computing_data_reduction 'R3m Software' _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 293(2) _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.999 _diffrn_measurement_device_type 'Siemens R3m four-circle' _diffrn_measurement_method '\w scan' _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 0.065 _diffrn_reflns_limit_h_max 27 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_limit_l_min -1 _diffrn_reflns_number 4097 _diffrn_reflns_theta_full 27.99 _diffrn_reflns_theta_max 27.99 _diffrn_reflns_theta_min 2.64 _diffrn_standards_decay_% 0 _diffrn_standards_interval_count 150 _diffrn_standards_number 2 _exptl_absorpt_coefficient_mu 1.477 _exptl_absorpt_correction_T_max 0.642 _exptl_absorpt_correction_T_min 0.543 _exptl_absorpt_correction_type empirical _exptl_absorpt_process_details '\y scan (North et al., 1968)' _exptl_crystal_colour green _exptl_crystal_density_diffrn 1.499 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_method 'not measured' _exptl_crystal_description block _exptl_crystal_F_000 2768 _exptl_crystal_size_max 0.42 _exptl_crystal_size_mid 0.36 _exptl_crystal_size_min 0.30 _refine_diff_density_max 0.37 _refine_diff_density_min -0.35 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.028 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 192 _refine_ls_number_reflns 3598 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.028 _refine_ls_R_factor_all 0.100 _refine_ls_R_factor_gt 0.053 _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^)+(0.0698P)^2^+0.2836P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.121 _refine_ls_wR_factor_ref 0.140 _reflns_number_gt 2304 _reflns_number_total 3598 _reflns_threshold_expression I>2\s(I) _[local]_cod_data_source_file jz1496.cif _[local]_cod_data_source_block I _[local]_cod_cif_authors_sg_H-M 'I 41/a' _cod_database_code 2012641 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-y+3/4, x+1/4, z+1/4' 'y+3/4, -x+3/4, z+3/4' 'x+1/2, y+1/2, z+1/2' '-x+1, -y+1/2, z+1' '-y+5/4, x+3/4, z+3/4' 'y+5/4, -x+5/4, z+5/4' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'y-3/4, -x-1/4, -z-1/4' '-y-3/4, x-3/4, -z-3/4' '-x+1/2, -y+1/2, -z+1/2' 'x, y+1/2, -z' 'y-1/4, -x+1/4, -z+1/4' '-y-1/4, x-1/4, -z-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_refinement_flags _atom_site_occupancy _atom_site_disorder_assembly _atom_site_disorder_group _atom_site_type_symbol Cu1 0.56251(2) 0.49404(2) 0.52102(3) 0.03223(16) Uani d . 1 . . Cu O1 0.54499(14) 0.55901(15) 0.6210(2) 0.0507(8) Uani d . 1 . . O O2 0.43997(14) 0.56960(16) 0.5851(2) 0.0515(8) Uani d . 1 . . O O3 0.53251(15) 0.42441(15) 0.6080(2) 0.0520(8) Uani d . 1 . . O O4 0.42748(14) 0.43425(15) 0.5714(2) 0.0514(8) Uani d . 1 . . O N1 0.66473(14) 0.48118(15) 0.5457(2) 0.0309(7) Uani d . 1 . . N C1 0.69170(19) 0.42261(19) 0.5335(3) 0.0358(9) Uani d . 1 . . C H1 0.6645 0.3878 0.5200 0.043 Uiso calc R 1 . . H C2 0.75699(19) 0.41091(19) 0.5398(3) 0.0366(9) Uani d . 1 . . C H2 0.7729 0.3692 0.5303 0.044 Uiso calc R 1 . . H C3 0.79982(18) 0.46170(18) 0.5605(3) 0.0305(8) Uani d . 1 . . C C4 0.77158(18) 0.52318(18) 0.5725(3) 0.0320(8) Uani d . 1 . . C H4 0.7976 0.5590 0.5851 0.038 Uiso calc R 1 . . H C5 0.70495(18) 0.53045(18) 0.5656(3) 0.0320(8) Uani d . 1 . . C H5 0.6873 0.5715 0.5752 0.038 Uiso calc R 1 . . H C6 0.87103(18) 0.4506(2) 0.5678(3) 0.0378(9) Uani d . 1 . . C C7 0.9007(2) 0.4006(2) 0.5169(3) 0.0469(11) Uani d . 1 . . C H7 0.8759 0.3745 0.4770 0.056 Uiso calc R 1 . . H C8 0.9665(2) 0.3896(3) 0.5250(4) 0.0694(17) Uani d . 1 . . C H8 0.9857 0.3561 0.4907 0.083 Uiso calc R 1 . . H C9 1.0041(2) 0.4281(3) 0.5837(4) 0.0691(17) Uani d . 1 . . C H9 1.0486 0.4210 0.5879 0.083 Uiso calc R 1 . . H C10 0.9756(2) 0.4767(3) 0.6359(5) 0.0705(17) Uani d . 1 . . C H10 1.0007 0.5018 0.6767 0.085 Uiso calc R 1 . . H C11 0.9099(2) 0.4885(2) 0.6280(4) 0.0513(12) Uani d . 1 . . C H11 0.8912 0.5219 0.6629 0.062 Uiso calc R 1 . . H C12 0.4898(2) 0.5837(2) 0.6326(3) 0.0372(9) Uani d . 1 . . C C13 0.4824(3) 0.6341(2) 0.7087(4) 0.0595(14) Uani d . 1 . . C H13A 0.4379 0.6359 0.7287 0.071 Uiso calc R 1 . . H H13B 0.4952 0.6756 0.6842 0.071 Uiso calc R 1 . . H H13C 0.5094 0.6230 0.7619 0.071 Uiso calc R 1 . . H C14 0.4736(2) 0.4087(2) 0.6153(3) 0.0419(10) Uani d . 1 . . C C15 0.4580(3) 0.3528(3) 0.6807(4) 0.0701(17) Uani d . 1 . . C H15A 0.4779 0.3600 0.7415 0.084 Uiso calc R 1 . . H H15B 0.4743 0.3132 0.6539 0.084 Uiso calc R 1 . . H H15C 0.4118 0.3495 0.6885 0.084 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 Cu1 0.0231(2) 0.0362(3) 0.0374(3) 0.00184(19) -0.0010(2) 0.0014(2) O1 0.0379(17) 0.059(2) 0.0552(19) 0.0065(14) -0.0070(15) -0.0185(17) O2 0.0326(16) 0.063(2) 0.059(2) 0.0082(14) -0.0042(15) -0.0235(17) O3 0.0398(17) 0.0535(19) 0.063(2) -0.0018(14) -0.0060(16) 0.0232(17) O4 0.0384(17) 0.057(2) 0.059(2) -0.0037(14) 0.0009(16) 0.0221(17) N1 0.0264(15) 0.0353(17) 0.0310(18) 0.0019(13) -0.0010(13) -0.0005(14) C1 0.035(2) 0.033(2) 0.040(2) -0.0040(16) -0.0019(18) -0.0003(18) C2 0.034(2) 0.0287(19) 0.047(3) 0.0027(16) -0.0044(19) -0.0002(18) C3 0.0267(18) 0.038(2) 0.0268(19) 0.0013(16) 0.0001(16) -0.0003(17) C4 0.0290(19) 0.033(2) 0.034(2) -0.0025(15) -0.0007(17) -0.0033(17) C5 0.0304(19) 0.033(2) 0.032(2) 0.0042(16) 0.0014(17) -0.0029(17) C6 0.0272(19) 0.048(2) 0.038(2) 0.0065(17) 0.0011(18) 0.0022(19) C7 0.032(2) 0.057(3) 0.052(3) 0.010(2) -0.004(2) -0.010(2) C8 0.035(2) 0.091(4) 0.083(4) 0.023(3) -0.001(3) -0.022(4) C9 0.027(2) 0.105(5) 0.075(4) 0.013(3) -0.011(3) -0.010(3) C10 0.034(2) 0.092(4) 0.086(4) 0.001(3) -0.016(3) -0.028(4) C11 0.033(2) 0.062(3) 0.059(3) 0.001(2) -0.001(2) -0.015(3) C12 0.040(2) 0.036(2) 0.036(2) 0.0006(18) 0.0023(19) -0.0018(18) C13 0.066(3) 0.058(3) 0.055(3) 0.010(3) -0.002(3) -0.017(3) C14 0.049(3) 0.036(2) 0.040(2) -0.009(2) -0.001(2) 0.006(2) C15 0.080(4) 0.062(3) 0.068(4) -0.025(3) -0.016(3) 0.034(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 O1 . 1.975(3) yes Cu1 O4 9_666 1.979(3) yes Cu1 O3 . 1.984(3) yes Cu1 O2 9_666 1.987(3) yes Cu1 N1 . 2.150(3) yes Cu1 Cu1 9_666 2.6536(10) ? O1 C12 . 1.257(5) ? O2 C12 . 1.259(5) ? O2 Cu1 9_666 1.987(3) ? O3 C14 . 1.260(5) ? O4 C14 . 1.250(5) ? O4 Cu1 9_666 1.979(3) ? N1 C5 . 1.340(5) ? N1 C1 . 1.339(5) ? C1 C2 . 1.369(5) ? C1 H1 . 0.9300 ? C2 C3 . 1.399(5) ? C2 H2 . 0.9300 ? C3 C4 . 1.404(5) ? C3 C6 . 1.488(5) ? C4 C5 . 1.384(5) ? C4 H4 . 0.9300 ? C5 H5 . 0.9300 ? C6 C7 . 1.395(6) ? C6 C11 . 1.403(6) ? C7 C8 . 1.378(6) ? C7 H7 . 0.9300 ? C8 C9 . 1.383(7) ? C8 H8 . 0.9300 ? C9 C10 . 1.375(7) ? C9 H9 . 0.9300 ? C10 C11 . 1.379(6) ? C10 H10 . 0.9300 ? C11 H11 . 0.9300 ? C12 C13 . 1.498(6) ? C13 H13A . 0.9600 ? C13 H13B . 0.9600 ? C13 H13C . 0.9600 ? C14 C15 . 1.509(6) ? C15 H15A . 0.9600 ? C15 H15B . 0.9600 ? C15 H15C . 0.9600 ? 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 O1 Cu1 O4 . 9_666 88.94(15) yes O1 Cu1 O3 . . 89.63(15) yes O4 Cu1 O3 9_666 . 167.80(12) yes O1 Cu1 O2 . 9_666 167.79(12) yes O4 Cu1 O2 9_666 9_666 90.08(15) yes O3 Cu1 O2 . 9_666 88.76(15) yes O1 Cu1 N1 . . 98.49(12) yes O4 Cu1 N1 9_666 . 95.51(12) yes O3 Cu1 N1 . . 96.69(12) yes O2 Cu1 N1 9_666 . 93.73(12) yes O1 Cu1 Cu1 . 9_666 85.34(9) ? O4 Cu1 Cu1 9_666 9_666 83.43(9) ? O3 Cu1 Cu1 . 9_666 84.38(9) ? O2 Cu1 Cu1 9_666 9_666 82.45(8) ? N1 Cu1 Cu1 . 9_666 176.02(9) ? C12 O1 Cu1 . . 122.2(3) ? C12 O2 Cu1 . 9_666 124.9(3) ? C14 O3 Cu1 . . 122.4(3) ? C14 O4 Cu1 . 9_666 124.1(3) ? C5 N1 C1 . . 116.9(3) ? C5 N1 Cu1 . . 123.1(3) ? C1 N1 Cu1 . . 119.8(3) ? N1 C1 C2 . . 123.9(4) ? N1 C1 H1 . . 118.1 ? C2 C1 H1 . . 118.1 ? C1 C2 C3 . . 120.1(4) ? C1 C2 H2 . . 120.0 ? C3 C2 H2 . . 120.0 ? C2 C3 C4 . . 116.0(3) ? C2 C3 C6 . . 121.4(3) ? C4 C3 C6 . . 122.6(3) ? C5 C4 C3 . . 120.0(3) ? C5 C4 H4 . . 120.0 ? C3 C4 H4 . . 120.0 ? N1 C5 C4 . . 123.1(3) ? N1 C5 H5 . . 118.5 ? C4 C5 H5 . . 118.5 ? C7 C6 C11 . . 118.0(4) ? C7 C6 C3 . . 120.7(4) ? C11 C6 C3 . . 121.3(4) ? C8 C7 C6 . . 120.7(5) ? C8 C7 H7 . . 119.7 ? C6 C7 H7 . . 119.7 ? C7 C8 C9 . . 120.4(5) ? C7 C8 H8 . . 119.8 ? C9 C8 H8 . . 119.8 ? C10 C9 C8 . . 119.8(4) ? C10 C9 H9 . . 120.1 ? C8 C9 H9 . . 120.1 ? C9 C10 C11 . . 120.3(5) ? C9 C10 H10 . . 119.8 ? C11 C10 H10 . . 119.8 ? C10 C11 C6 . . 120.7(5) ? C10 C11 H11 . . 119.6 ? C6 C11 H11 . . 119.6 ? O1 C12 O2 . . 125.1(4) ? O1 C12 C13 . . 117.7(4) ? O2 C12 C13 . . 117.2(4) ? C12 C13 H13A . . 109.5 ? C12 C13 H13B . . 109.5 ? H13A C13 H13B . . 109.5 ? C12 C13 H13C . . 109.5 ? H13A C13 H13C . . 109.5 ? H13B C13 H13C . . 109.5 ? O4 C14 O3 . . 125.7(4) ? O4 C14 C15 . . 117.4(4) ? O3 C14 C15 . . 116.9(4) ? C14 C15 H15A . . 109.5 ? C14 C15 H15B . . 109.5 ? H15A C15 H15B . . 109.5 ? C14 C15 H15C . . 109.5 ? H15A C15 H15C . . 109.5 ? H15B C15 H15C . . 109.5 ? 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 O4 Cu1 O1 C12 9_666 82.3(4) O3 Cu1 O1 C12 . -85.6(3) O2 Cu1 O1 C12 9_666 -3.1(9) N1 Cu1 O1 C12 . 177.7(3) Cu1 Cu1 O1 C12 9_666 -1.2(3) O1 Cu1 O3 C14 . 86.1(4) O4 Cu1 O3 C14 9_666 2.9(9) O2 Cu1 O3 C14 9_666 -81.8(4) N1 Cu1 O3 C14 . -175.4(4) Cu1 Cu1 O3 C14 9_666 0.8(4) O1 Cu1 N1 C5 . -40.5(3) O4 Cu1 N1 C5 9_666 49.2(3) O3 Cu1 N1 C5 . -131.2(3) O2 Cu1 N1 C5 9_666 139.7(3) Cu1 Cu1 N1 C5 9_666 123.5(12) O1 Cu1 N1 C1 . 145.1(3) O4 Cu1 N1 C1 9_666 -125.2(3) O3 Cu1 N1 C1 . 54.4(3) O2 Cu1 N1 C1 9_666 -34.8(3) Cu1 Cu1 N1 C1 9_666 -50.9(15) C5 N1 C1 C2 . -0.4(6) Cu1 N1 C1 C2 . 174.4(3) N1 C1 C2 C3 . 0.3(7) C1 C2 C3 C4 . -0.8(6) C1 C2 C3 C6 . -180.0(4) C2 C3 C4 C5 . 1.3(6) C6 C3 C4 C5 . -179.5(4) C1 N1 C5 C4 . 0.9(6) Cu1 N1 C5 C4 . -173.6(3) C3 C4 C5 N1 . -1.4(6) C2 C3 C6 C7 . 28.1(6) C4 C3 C6 C7 . -151.0(4) C2 C3 C6 C11 . -149.9(4) C4 C3 C6 C11 . 31.0(6) C11 C6 C7 C8 . -0.7(7) C3 C6 C7 C8 . -178.8(5) C6 C7 C8 C9 . -0.1(9) C7 C8 C9 C10 . 1.3(10) C8 C9 C10 C11 . -1.7(10) C9 C10 C11 C6 . 0.9(9) C7 C6 C11 C10 . 0.3(8) C3 C6 C11 C10 . 178.4(5) Cu1 O1 C12 O2 . 1.7(6) Cu1 O1 C12 C13 . -178.1(3) Cu1 O2 C12 O1 9_666 -1.2(6) Cu1 O2 C12 C13 9_666 178.7(3) Cu1 O4 C14 O3 9_666 0.2(7) Cu1 O4 C14 C15 9_666 -177.8(3) Cu1 O3 C14 O4 . -0.8(7) Cu1 O3 C14 C15 . 177.2(3)