#------------------------------------------------------------------------------ #$Date: 2011-09-10 04:16:28 +0100 (Sat, 10 Sep 2011) $ #$Revision: 25271 $ #$URL: svn://www.crystallography.net/cod/cif/2/2006229.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_2006229 loop_ _publ_author_name 'Warda, S. A.' _publ_section_title ; A (4-Ethylpyridine)(N-salicylideneglycinato)copper(II) Tetramer ; _journal_issue 6 _journal_name_full 'Acta Crystallographica Section C' _journal_page_first 697 _journal_page_last 699 _journal_volume 53 _journal_year 1997 _chemical_formula_iupac '[Cu(C9 H7 N1 O3)(C7 H9 N)]4' _chemical_formula_structural '(C9H7CuNO3 C7H9N)~4~' _chemical_formula_sum 'C64 H64 Cu4 N8 O12' _chemical_formula_weight 5962.2 _chemical_name_systematic ; (4-Ethylpyridine)(N-salicylideneglycinato)copper(II) Tetramer ; _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' _audit_creation_method 'SHELXL96 (Sheldrick, 1996)' _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_formula_units_Z 4 _cell_length_a 28.6630(7) _cell_length_b 28.6630(7) _cell_length_c 7.25719(10) _cell_measurement_reflns_used 25 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 46.27 _cell_measurement_theta_min 28.74 _cell_volume 5962.3(2) _computing_cell_refinement 'CAD4 EXPRESS' _computing_data_collection 'CAD4 EXPRESS (Enraf-Nonius, 1994)' _computing_data_reduction 'XCAD4 (Harms, 1993)' _computing_molecular_graphics 'XP (Siemens, 1994), SHELXTL (Sheldrick, 1994)' _computing_publication_material SHELXL-96 _computing_structure_refinement 'SHELXL-96 (Sheldrick,1996)' _computing_structure_solution 'SHELXS86 (Sheldrick, 1985)' _diffrn_ambient_temperature 293(2) _diffrn_measurement_device 'Enraf Nonius CAD4' _diffrn_measurement_method '\w-2\q scans' _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.54178 _diffrn_reflns_av_R_equivalents 0.0336 _diffrn_reflns_av_sigmaI/netI 0.0158 _diffrn_reflns_limit_h_max 0 _diffrn_reflns_limit_h_min -32 _diffrn_reflns_limit_k_max 32 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_l_max 0 _diffrn_reflns_limit_l_min -8 _diffrn_reflns_number 2315 _diffrn_reflns_theta_max 59.88 _diffrn_reflns_theta_min 3.08 _diffrn_standards_decay_% 0 _diffrn_standards_interval_time 120 _diffrn_standards_number 2 _exptl_absorpt_coefficient_mu 2.194 _exptl_absorpt_correction_T_max 0.769 _exptl_absorpt_correction_T_min 0.364 _exptl_absorpt_correction_type 'empirically with \y scans' _exptl_crystal_colour 'Dark green' _exptl_crystal_density_diffrn 1.550 _exptl_crystal_description Prism _exptl_crystal_F_000 2864 _exptl_crystal_size_max 0.205 _exptl_crystal_size_mid 0.125 _exptl_crystal_size_min 0.120 _refine_diff_density_max 0.613 _refine_diff_density_min -0.465 _refine_ls_extinction_coef 0.00044(5) _refine_ls_extinction_method 'SHELXL96 (Sheldrick, 1996)' _refine_ls_goodness_of_fit_all 1.124 _refine_ls_goodness_of_fit_obs 1.153 _refine_ls_hydrogen_treatment 'H atoms riding' _refine_ls_matrix_type full _refine_ls_number_parameters 200 _refine_ls_number_reflns 2205 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.124 _refine_ls_restrained_S_obs 1.153 _refine_ls_R_factor_all 0.0475 _refine_ls_R_factor_obs 0.0435 _refine_ls_shift/esd_max 0.001 _refine_ls_shift/esd_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_scheme 'calc w = 1/[\s^2^(Fo^2^)+(0.0768P)^2^+10.6290P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_wR_factor_all 0.1254 _refine_ls_wR_factor_obs 0.1225 _reflns_number_observed 2015 _reflns_number_total 2205 _reflns_observed_criterion >2sigma(I) _[local]_cod_data_source_file jz1191.cif _[local]_cod_data_source_block tet_1 _[local]_cod_cif_authors_sg_H-M 'I 41/a' _cod_depositor_comments ; The following automatic conversions were performed: '_symmetry_cell_setting' value 'Tetragonal' changed to 'tetragonal' 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 2006229 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_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 Cu 0.0470(4) 0.0393(3) 0.0209(3) -0.00323(19) -0.01006(19) 0.00121(18) N1 0.0404(14) 0.0422(15) 0.0206(13) -0.0017(11) -0.0023(11) -0.0014(11) O1 0.0718(17) 0.0472(14) 0.0315(13) -0.0148(12) -0.0198(12) 0.0071(11) C1 0.0487(19) 0.0382(18) 0.0336(18) 0.0048(14) -0.0032(15) 0.0046(14) N2 0.0416(15) 0.0407(14) 0.0221(13) 0.0006(11) -0.0037(11) 0.0018(11) C2 0.055(2) 0.046(2) 0.055(2) -0.0059(16) -0.0094(18) 0.0008(18) O2 0.0593(15) 0.0436(13) 0.0327(13) -0.0027(11) -0.0137(11) -0.0008(10) C3 0.061(2) 0.044(2) 0.063(3) -0.0033(17) 0.010(2) 0.0109(19) O3 0.0803(18) 0.0446(14) 0.0280(12) -0.0136(12) -0.0048(12) -0.0030(10) C4 0.070(3) 0.051(2) 0.042(2) 0.0071(18) 0.0141(19) 0.0135(17) C5 0.053(2) 0.049(2) 0.0297(18) 0.0093(16) 0.0022(15) 0.0042(15) C6 0.0425(17) 0.0401(17) 0.0222(16) 0.0074(13) 0.0023(13) 0.0023(13) C7 0.0428(17) 0.0463(18) 0.0183(15) 0.0057(13) -0.0046(13) -0.0014(14) C8 0.050(2) 0.049(2) 0.0281(17) -0.0089(15) -0.0091(14) -0.0013(14) C9 0.0501(19) 0.0437(19) 0.0172(14) -0.0057(15) 0.0042(14) -0.0039(13) C10 0.049(2) 0.051(2) 0.0320(18) -0.0107(15) -0.0086(15) 0.0071(15) C11 0.052(2) 0.049(2) 0.0301(18) -0.0027(16) -0.0069(15) 0.0123(15) C12 0.0453(19) 0.0499(19) 0.0238(16) 0.0079(15) -0.0063(14) 0.0013(14) C13 0.0472(19) 0.0492(19) 0.0321(18) -0.0092(15) -0.0123(15) 0.0060(15) C14 0.0459(19) 0.0466(19) 0.0261(16) -0.0059(15) -0.0069(14) 0.0075(14) C15 0.061(2) 0.068(2) 0.0319(19) 0.0008(19) -0.0166(17) 0.0092(17) C16 0.113(4) 0.081(3) 0.053(3) -0.014(3) -0.050(3) 0.009(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_thermal_displace_type _atom_site_calc_flag _atom_site_refinement_flags _atom_site_occupancy _atom_site_type_symbol Cu 0.37617(2) 0.68736(2) -0.34303(6) 0.0357(3) Uani d . 1 Cu N1 0.41124(9) 0.68678(9) -0.1164(3) 0.0344(6) Uani d . 1 N O1 0.34926(9) 0.62762(8) -0.2935(3) 0.0502(7) Uani d . 1 O C1 0.34876(12) 0.60566(11) -0.1356(5) 0.0401(8) Uani d . 1 C N2 0.33638(9) 0.69614(9) -0.5653(3) 0.0348(6) Uani d . 1 N C2 0.31934(13) 0.56658(13) -0.1139(6) 0.0517(9) Uani d . 1 C H2 0.3012 0.5569 -0.2129 0.062 Uiso calc R 1 H O2 0.38921(9) 0.75579(8) -0.3301(3) 0.0452(6) Uani d . 1 O C3 0.31672(14) 0.54250(13) 0.0487(6) 0.0559(10) Uani d . 1 C H3 0.2970 0.5168 0.0573 0.067 Uiso calc R 1 H O3 0.43752(10) 0.80643(8) -0.1976(3) 0.0510(7) Uani d . 1 O C4 0.34297(14) 0.55560(13) 0.2012(6) 0.0545(10) Uani d . 1 C H4 0.3406 0.5393 0.3116 0.065 Uiso calc R 1 H C5 0.37238(12) 0.59314(12) 0.1850(5) 0.0440(8) Uani d . 1 C H5 0.3904 0.6019 0.2856 0.053 Uiso calc R 1 H C6 0.37595(11) 0.61865(11) 0.0202(4) 0.0349(7) Uani d . 1 C C7 0.40544(11) 0.65867(11) 0.0196(4) 0.0358(7) Uani d . 1 C H7 0.4219 0.6650 0.1271 0.043 Uiso calc R 1 H C8 0.44079(12) 0.72756(12) -0.0994(5) 0.0423(8) Uani d . 1 C H8A 0.4722 0.7201 -0.1395 0.051 Uiso calc R 1 H H8B 0.4422 0.7374 0.0284 0.051 Uiso calc R 1 H C9 0.42096(12) 0.76701(11) -0.2181(4) 0.0370(7) Uani d . 1 C C10 0.34546(12) 0.73137(13) -0.6815(5) 0.0440(8) Uani d . 1 C H10 0.3691 0.7523 -0.6520 0.053 Uiso calc R 1 H C11 0.32102(12) 0.73780(12) -0.8430(5) 0.0438(8) Uani d . 1 C H11 0.3286 0.7625 -0.9207 0.053 Uiso calc R 1 H C12 0.28528(12) 0.70761(12) -0.8897(4) 0.0397(8) Uani d . 1 C C13 0.27560(12) 0.67217(12) -0.7679(5) 0.0428(8) Uani d . 1 C H13 0.2517 0.6512 -0.7932 0.051 Uiso calc R 1 H C14 0.30136(12) 0.66762(12) -0.6082(4) 0.0395(8) Uani d . 1 C H14 0.2939 0.6436 -0.5271 0.047 Uiso calc R 1 H C15 0.25948(14) 0.71450(15) -1.0685(5) 0.0538(10) Uani d . 1 C H15A 0.2424 0.7436 -1.0603 0.065 Uiso calc R 1 H H15B 0.2824 0.7180 -1.1658 0.065 Uiso calc R 1 H C16 0.2263(2) 0.67758(17) -1.1251(7) 0.0823(16) Uani d . 1 C H16A 0.2122 0.6859 -1.2405 0.124 Uiso calc R 1 H H16B 0.2025 0.6743 -1.0330 0.124 Uiso calc R 1 H H16C 0.2427 0.6485 -1.1384 0.124 Uiso calc R 1 H loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu -1.9646 0.5888 '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_3 _geom_angle _geom_angle_publ_flag O1 Cu N1 . 92.42(10) y O1 Cu N2 . 91.98(10) y N1 Cu N2 . 172.24(11) y O1 Cu O2 . 160.98(11) y N1 Cu O2 . 82.59(10) y N2 Cu O2 . 91.21(10) y O1 Cu O3 12_765 115.78(11) y N1 Cu O3 12_765 96.75(10) y N2 Cu O3 12_765 87.08(9) y O2 Cu O3 12_765 83.11(10) y C7 N1 C8 . 121.1(3) ? C7 N1 Cu . 126.4(2) ? C8 N1 Cu . 111.8(2) ? C1 O1 Cu . 126.9(2) ? O1 C1 C2 . 119.1(3) ? O1 C1 C6 . 124.4(3) ? C2 C1 C6 . 116.5(3) ? C14 N2 C10 . 117.5(3) ? C14 N2 Cu . 122.9(2) ? C10 N2 Cu . 119.5(2) ? C3 C2 C1 . 122.0(4) ? C9 O2 Cu . 114.5(2) ? C2 C3 C4 . 121.3(3) ? C5 C4 C3 . 118.4(3) ? C4 C5 C6 . 121.7(3) ? C5 C6 C1 . 120.0(3) ? C5 C6 C7 . 117.7(3) ? C1 C6 C7 . 122.2(3) ? N1 C7 C6 . 125.7(3) ? N1 C8 C9 . 109.3(3) ? O3 C9 O2 . 126.0(3) ? O3 C9 C8 . 117.8(3) ? O2 C9 C8 . 116.2(3) ? N2 C10 C11 . 122.5(3) ? C10 C11 C12 . 120.1(3) ? C13 C12 C11 . 117.0(3) ? C13 C12 C15 . 123.5(3) ? C11 C12 C15 . 119.5(3) ? C12 C13 C14 . 120.1(3) ? N2 C14 C13 . 122.8(3) ? C16 C15 C12 . 117.4(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 Cu O1 . 1.912(2) y Cu N1 . 1.927(3) y Cu N2 . 1.992(2) y Cu O2 . 1.999(2) y Cu O3 12_765 2.458(2) y N1 C7 . 1.285(4) ? N1 C8 . 1.449(4) ? O1 C1 . 1.308(4) ? C1 C2 . 1.411(5) ? C1 C6 . 1.422(5) ? N2 C14 . 1.331(4) ? N2 C10 . 1.341(4) ? C2 C3 . 1.369(6) ? O2 C9 . 1.262(4) ? C3 C4 . 1.390(6) ? O3 C9 . 1.235(4) ? C4 C5 . 1.372(5) ? C5 C6 . 1.405(5) ? C6 C7 . 1.425(5) ? C8 C9 . 1.531(5) ? C10 C11 . 1.378(5) ? C11 C12 . 1.383(5) ? C12 C13 . 1.374(5) ? C12 C15 . 1.506(5) ? C13 C14 . 1.381(5) ? C15 C16 . 1.481(6) ? 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 O1 Cu N1 C7 . -13.1(3) N2 Cu N1 C7 . 111.3(8) O2 Cu N1 C7 . 148.4(3) O3 Cu N1 C7 12_765 -129.5(3) O1 Cu N1 C8 . 177.0(2) N2 Cu N1 C8 . -58.6(9) O2 Cu N1 C8 . -21.4(2) O3 Cu N1 C8 12_765 60.7(2) N1 Cu O1 C1 . 15.1(3) N2 Cu O1 C1 . -158.5(3) O2 Cu O1 C1 . -59.0(5) O3 Cu O1 C1 12_765 113.8(3) Cu O1 C1 C2 . 167.0(3) Cu O1 C1 C6 . -12.4(5) O1 Cu N2 C14 . 9.0(3) N1 Cu N2 C14 . -115.5(8) O2 Cu N2 C14 . -152.3(3) O3 Cu N2 C14 12_765 124.7(3) O1 Cu N2 C10 . -169.2(3) N1 Cu N2 C10 . 66.4(9) O2 Cu N2 C10 . 29.6(3) O3 Cu N2 C10 12_765 -53.4(3) O1 C1 C2 C3 . -179.1(3) C6 C1 C2 C3 . 0.4(5) O1 Cu O2 C9 . 91.0(4) N1 Cu O2 C9 . 15.3(2) N2 Cu O2 C9 . -169.3(2) O3 Cu O2 C9 12_765 -82.4(2) C1 C2 C3 C4 . 0.3(6) C2 C3 C4 C5 . -0.9(6) C3 C4 C5 C6 . 0.9(5) C4 C5 C6 C1 . -0.2(5) C4 C5 C6 C7 . 176.5(3) O1 C1 C6 C5 . 179.0(3) C2 C1 C6 C5 . -0.5(5) O1 C1 C6 C7 . 2.5(5) C2 C1 C6 C7 . -177.0(3) C8 N1 C7 C6 . 177.6(3) Cu N1 C7 C6 . 8.6(5) C5 C6 C7 N1 . -177.1(3) C1 C6 C7 N1 . -0.5(5) C7 N1 C8 C9 . -146.8(3) Cu N1 C8 C9 . 23.7(3) Cu O2 C9 O3 . 173.8(3) Cu O2 C9 C8 . -5.4(4) N1 C8 C9 O3 . 168.9(3) N1 C8 C9 O2 . -11.9(4) C14 N2 C10 C11 . -2.0(5) Cu N2 C10 C11 . 176.2(3) N2 C10 C11 C12 . 0.7(6) C10 C11 C12 C13 . 0.6(5) C10 C11 C12 C15 . -178.8(3) C11 C12 C13 C14 . -0.6(5) C15 C12 C13 C14 . 178.8(3) C10 N2 C14 C13 . 2.1(5) Cu N2 C14 C13 . -176.1(3) C12 C13 C14 N2 . -0.8(6) C13 C12 C15 C16 . -8.0(6) C11 C12 C15 C16 . 171.4(4)