#------------------------------------------------------------------------------ #$Date: 2016-02-20 00:18:51 +0200 (Sat, 20 Feb 2016) $ #$Revision: 176760 $ #$URL: file:///home/coder/svn-repositories/cod/cif/2/01/39/2013949.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_2013949 loop_ _publ_author_name 'O\N-salicylidene-\b-alaninato-\k^3^O,N,O')copper(II)] urea disolvate ; _journal_issue 6 _journal_name_full 'Acta Crystallographica Section C' _journal_page_first m275 _journal_page_last m277 _journal_paper_doi 10.1107/S0108270104008030 _journal_volume 60 _journal_year 2004 _chemical_formula_iupac '[Cu2 (C10 H9 N O3)2 (H2 O)2], 2C H4 N2 O' _chemical_formula_moiety 'C20 H22 Cu2 N2 O8, 2C H4 N2 O' _chemical_formula_sum 'C22 H30 Cu2 N6 O10' _chemical_formula_weight 665.62 _chemical_name_systematic ; Di-\m-aqua-bis[(N-salicylidene-\b-alaninato-\k^3^O,N,O')copper(II)] urea disolvate ; _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 105.638(13) _cell_angle_beta 108.079(12) _cell_angle_gamma 98.697(12) _cell_formula_units_Z 1 _cell_length_a 7.3218(10) _cell_length_b 9.0547(14) _cell_length_c 10.7935(15) _cell_measurement_reflns_used 1272 _cell_measurement_temperature 120(2) _cell_measurement_theta_max 26.434 _cell_measurement_theta_min 3.036 _cell_volume 633.14(18) _computing_cell_refinement 'CrysAlis RED (Oxford Diffraction, 2002)' _computing_data_collection 'CrysAlis CCD (Oxford Diffraction, 2002)' _computing_data_reduction 'CrysAlis RED' _computing_molecular_graphics 'ORTEPIII (Johnson & Burnett, 1996)' _computing_publication_material ; SHELXL97 (Sheldrick, 1997) and PARST (Nardelli, 1995) ; _computing_structure_refinement 'SHELXL97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS97 (Sheldrick, 1990)' _diffrn_ambient_temperature 120(2) _diffrn_detector_area_resol_mean 16.3 _diffrn_measured_fraction_theta_full 0.991 _diffrn_measured_fraction_theta_max 0.991 _diffrn_measurement_device_type 'Kuma KM-4-Plus CCD' _diffrn_measurement_method '\w scan' _diffrn_radiation_monochromator 'Enhance (Oxford Diffraction)' _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0358 _diffrn_reflns_av_sigmaI/netI 0.0385 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_number 4325 _diffrn_reflns_theta_full 25.00 _diffrn_reflns_theta_max 25.00 _diffrn_reflns_theta_min 3.88 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 1.749 _exptl_absorpt_correction_T_max 0.88176 _exptl_absorpt_correction_T_min 0.45768 _exptl_absorpt_correction_type analytical _exptl_absorpt_process_details 'CrysAlis RED (Oxford Diffraction, 2002)' _exptl_crystal_colour 'dark blue' _exptl_crystal_density_diffrn 1.746 _exptl_crystal_density_method 'not measured' _exptl_crystal_description needle _exptl_crystal_F_000 342 _exptl_crystal_size_max 0.60 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.05 _refine_diff_density_max 0.596 _refine_diff_density_min -0.459 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.013 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 181 _refine_ls_number_reflns 2210 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.013 _refine_ls_R_factor_all 0.0364 _refine_ls_R_factor_gt 0.0323 _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^)+(0.0577P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0830 _refine_ls_wR_factor_ref 0.0851 _reflns_number_gt 1941 _reflns_number_total 2210 _reflns_threshold_expression I>2\s(I) _cod_data_source_file fa1055.cif _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. Automatic conversion script Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 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_values 1715 2011-07-08 13:25:40Z adriana ; _cod_database_code 2013949 _cod_database_fobs_code 2013949 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_disorder_assembly _atom_site_disorder_group _atom_site_type_symbol Cu 0.53149(4) 0.69727(3) 0.07211(3) 0.01315(14) Uani d . 1 . . Cu O1 0.2898(2) 0.5182(2) 0.00128(17) 0.0131(4) Uani d . 1 . . O H1V 0.1761 0.5220 -0.0631 0.016 Uiso d R 1 . . H H1W 0.2531 0.5040 0.0719 0.016 Uiso d R 1 . . H O2 0.5760(3) 0.6614(2) 0.24738(18) 0.0158(4) Uani d . 1 . . O O3 0.7636(3) 0.6449(3) 0.4452(2) 0.0271(5) Uani d . 1 . . O O4 0.4524(3) 0.7080(2) -0.11013(18) 0.0155(4) Uani d . 1 . . O N1 0.7516(3) 0.8858(2) 0.1500(2) 0.0142(5) Uani d . 1 . . N C1 0.7449(4) 0.6912(3) 0.3453(3) 0.0156(6) Uani d . 1 . . C C2 0.9230(4) 0.7899(3) 0.3364(3) 0.0162(6) Uani d . 1 . . C H2A 0.9650 0.7234 0.2665 0.019 Uiso calc R 1 . . H H2B 1.0346 0.8264 0.4269 0.019 Uiso calc R 1 . . H C3 0.8776(4) 0.9338(3) 0.2969(3) 0.0161(6) Uani d . 1 . . C H3A 0.8091 0.9881 0.3543 0.019 Uiso calc R 1 . . H H3B 1.0035 1.0096 0.3156 0.019 Uiso calc R 1 . . H C4 0.7886(4) 0.9779(3) 0.0833(3) 0.0164(6) Uani d . 1 . . C H4 0.8936 1.0716 0.1346 0.020 Uiso calc R 1 . . H C5 0.6868(4) 0.9529(3) -0.0605(3) 0.0150(6) Uani d . 1 . . C C6 0.5321(4) 0.8162(3) -0.1517(3) 0.0145(5) Uani d . 1 . . C C7 0.4622(4) 0.7972(3) -0.2935(3) 0.0179(6) Uani d . 1 . . C H7 0.3666 0.7024 -0.3575 0.021 Uiso calc R 1 . . H C8 0.5288(4) 0.9126(4) -0.3423(3) 0.0217(6) Uani d . 1 . . C H8 0.4788 0.8961 -0.4387 0.026 Uiso calc R 1 . . H C9 0.6694(4) 1.0538(4) -0.2506(3) 0.0231(6) Uani d . 1 . . C H9 0.7086 1.1361 -0.2833 0.028 Uiso calc R 1 . . H C10 0.7499(4) 1.0716(3) -0.1128(3) 0.0196(6) Uani d . 1 . . C H10 0.8499 1.1651 -0.0510 0.024 Uiso calc R 1 . . H O12 0.0692(3) 0.4762(2) 0.15298(19) 0.0192(4) Uani d . 1 . . O N13 -0.0243(3) 0.3743(3) 0.2996(2) 0.0192(5) Uani d . 1 . . N H13A -0.1500 0.3465 0.2443 0.023 Uiso d R 1 . . H H13B 0.0096 0.3544 0.3779 0.023 Uiso d R 1 . . H N14 0.3036(3) 0.4881(3) 0.3522(2) 0.0216(5) Uani d . 1 . . N H14A 0.3984 0.5368 0.3322 0.026 Uiso d R 1 . . H H14B 0.3331 0.4667 0.4298 0.026 Uiso d R 1 . . H C11 0.1149(4) 0.4467(3) 0.2647(3) 0.0143(5) Uani d . 1 . . C 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 0.0121(2) 0.0134(2) 0.0123(2) 0.00116(13) 0.00253(13) 0.00526(13) O1 0.0122(9) 0.0157(9) 0.0117(9) 0.0027(7) 0.0039(7) 0.0064(7) O2 0.0123(9) 0.0197(10) 0.0148(9) 0.0022(8) 0.0035(7) 0.0075(8) O3 0.0192(10) 0.0445(13) 0.0189(11) 0.0044(10) 0.0040(8) 0.0185(10) O4 0.0148(9) 0.0158(10) 0.0149(9) 0.0015(7) 0.0034(7) 0.0075(8) N1 0.0111(11) 0.0124(11) 0.0163(11) 0.0029(9) 0.0036(9) 0.0024(9) C1 0.0155(13) 0.0168(13) 0.0129(13) 0.0041(11) 0.0043(11) 0.0036(10) C2 0.0135(13) 0.0196(14) 0.0128(13) 0.0038(11) 0.0037(11) 0.0029(11) C3 0.0128(13) 0.0144(14) 0.0160(14) 0.0009(11) 0.0033(11) 0.0012(11) C4 0.0119(13) 0.0119(13) 0.0265(15) 0.0046(10) 0.0090(11) 0.0052(11) C5 0.0140(13) 0.0158(13) 0.0227(14) 0.0093(11) 0.0109(11) 0.0101(11) C6 0.0119(13) 0.0156(13) 0.0230(14) 0.0086(11) 0.0103(11) 0.0100(11) C7 0.0149(13) 0.0211(14) 0.0232(14) 0.0080(11) 0.0093(11) 0.0117(12) C8 0.0212(14) 0.0315(16) 0.0250(15) 0.0145(13) 0.0144(12) 0.0179(13) C9 0.0215(15) 0.0287(16) 0.0367(17) 0.0132(13) 0.0192(13) 0.0244(14) C10 0.0159(13) 0.0168(14) 0.0337(17) 0.0075(11) 0.0142(12) 0.0124(12) O12 0.0125(9) 0.0307(11) 0.0166(10) 0.0046(8) 0.0040(8) 0.0139(8) N13 0.0125(11) 0.0271(13) 0.0176(12) 0.0016(10) 0.0031(9) 0.0119(10) N14 0.0121(11) 0.0334(14) 0.0188(12) 0.0018(10) 0.0021(9) 0.0146(11) C11 0.0145(13) 0.0118(13) 0.0150(13) 0.0041(10) 0.0045(10) 0.0027(10) 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 O4 Cu O2 . . 171.49(7) O4 Cu N1 . . 94.28(8) O2 Cu N1 . . 94.14(8) O4 Cu O1 . . 87.02(7) O2 Cu O1 . . 84.48(7) N1 Cu O1 . . 173.92(8) O4 Cu O1 . 2_665 89.27(7) O2 Cu O1 . 2_665 90.47(7) N1 Cu O1 . 2_665 100.16(7) O1 Cu O1 . 2_665 85.79(7) O4 Cu Cu . 2_665 87.69(6) O2 Cu Cu . 2_665 87.11(6) N1 Cu Cu . 2_665 136.09(6) O1 Cu Cu . 2_665 49.85(5) O1 Cu Cu 2_665 2_665 35.94(4) Cu O1 Cu . 2_665 94.21(7) Cu O1 H1V . . 118.8 Cu O1 H1V 2_665 . 118.6 Cu O1 H1W . . 111.3 Cu O1 H1W 2_665 . 108.7 H1V O1 H1W . . 105.0 C1 O2 Cu . . 126.47(17) C6 O4 Cu . . 127.48(16) C4 N1 C3 . . 117.1(2) C4 N1 Cu . . 124.39(19) C3 N1 Cu . . 118.39(17) O3 C1 O2 . . 122.4(3) O3 C1 C2 . . 120.2(2) O2 C1 C2 . . 117.4(2) C1 C2 C3 . . 111.8(2) C1 C2 H2A . . 109.2 C3 C2 H2A . . 109.2 C1 C2 H2B . . 109.2 C3 C2 H2B . . 109.2 H2A C2 H2B . . 107.9 N1 C3 C2 . . 110.8(2) N1 C3 H3A . . 109.5 C2 C3 H3A . . 109.5 N1 C3 H3B . . 109.5 C2 C3 H3B . . 109.5 H3A C3 H3B . . 108.1 N1 C4 C5 . . 126.4(3) N1 C4 H4 . . 116.8 C5 C4 H4 . . 116.8 C6 C5 C10 . . 119.3(2) C6 C5 C4 . . 123.5(2) C10 C5 C4 . . 117.2(2) O4 C6 C7 . . 119.1(2) O4 C6 C5 . . 123.4(2) C7 C6 C5 . . 117.5(2) C8 C7 C6 . . 121.8(3) C8 C7 H7 . . 119.1 C6 C7 H7 . . 119.1 C7 C8 C9 . . 120.5(3) C7 C8 H8 . . 119.8 C9 C8 H8 . . 119.8 C10 C9 C8 . . 119.1(3) C10 C9 H9 . . 120.5 C8 C9 H9 . . 120.5 C9 C10 C5 . . 121.4(3) C9 C10 H10 . . 119.3 C5 C10 H10 . . 119.3 C11 N13 H13A . . 120.0 C11 N13 H13B . . 120.0 H13A N13 H13B . . 120.0 C11 N14 H14A . . 120.0 C11 N14 H14B . . 120.0 H14A N14 H14B . . 120.0 O12 C11 N13 . . 120.9(2) O12 C11 N14 . . 121.1(2) N13 C11 N14 . . 118.0(2) 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 O4 . 1.9046(18) ? Cu O2 . 1.9417(18) ? Cu N1 . 1.942(2) ? Cu O1 . 1.9922(18) ? Cu O1 2_665 2.5941(18) ? Cu Cu 2_665 3.3847(9) ? O1 Cu 2_665 2.5941(18) ? O1 H1V . 0.9161 ? O1 H1W . 0.9165 ? O2 C1 . 1.286(3) ? O3 C1 . 1.236(3) ? O4 C6 . 1.314(3) ? N1 C4 . 1.289(3) ? N1 C3 . 1.468(3) ? C1 C2 . 1.510(4) ? C2 C3 . 1.527(4) ? C2 H2A . 0.9900 ? C2 H2B . 0.9900 ? C3 H3A . 0.9900 ? C3 H3B . 0.9900 ? C4 C5 . 1.435(4) ? C4 H4 . 0.9500 ? C5 C6 . 1.418(4) ? C5 C10 . 1.423(4) ? C6 C7 . 1.408(4) ? C7 C8 . 1.381(4) ? C7 H7 . 0.9500 ? C8 C9 . 1.401(4) ? C8 H8 . 0.9500 ? C9 C10 . 1.372(4) ? C9 H9 . 0.9500 ? C10 H10 . 0.9500 ? O12 C11 . 1.260(3) ? N13 C11 . 1.335(4) ? N13 H13A . 0.8801 ? N13 H13B . 0.8796 ? N14 C11 . 1.336(3) ? N14 H14A . 0.8801 ? N14 H14B . 0.8795 ? 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 O1 H1V O12 2_565 0.92 1.76 2.656(2) 165 y O1 H1W O12 . 0.92 1.84 2.688(3) 153 y N13 H13A O4 2_565 0.88 2.13 3.009(3) 177 y N13 H13B O3 2_666 0.88 2.10 2.891(3) 149 y N14 H14A O2 . 0.88 2.16 3.022(3) 167 y N14 H14B O3 2_666 0.88 2.11 2.895(3) 148 y 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_site_symmetry_4 _geom_torsion O4 Cu O1 Cu . 2_665 89.49(7) N1 Cu O2 C1 . . -33.7(2) O1 Cu O2 C1 . . 152.2(2) O1 Cu O2 C1 2_665 . 66.5(2) Cu Cu O2 C1 2_665 . 102.3(2) N1 Cu O4 C6 . . -1.4(2) O1 Cu O4 C6 . . 172.62(19) O1 Cu O4 C6 2_665 . -101.55(19) Cu Cu O4 C6 2_665 . -137.48(19) O4 Cu N1 C4 . . 6.3(2) O2 Cu N1 C4 . . -172.5(2) O1 Cu N1 C4 2_665 . 96.3(2) Cu Cu N1 C4 2_665 . 97.4(2) O4 Cu N1 C3 . . -177.99(17) O2 Cu N1 C3 . . 3.26(18) O1 Cu N1 C3 2_665 . -87.96(18) Cu Cu N1 C3 2_665 . -86.88(19) Cu O2 C1 O3 . . -169.6(2) Cu O2 C1 C2 . . 11.8(3) O3 C1 C2 C3 . . -133.6(3) O2 C1 C2 C3 . . 45.0(3) C4 N1 C3 C2 . . -141.5(2) Cu N1 C3 C2 . . 42.4(3) C1 C2 C3 N1 . . -73.8(3) C3 N1 C4 C5 . . 179.0(2) Cu N1 C4 C5 . . -5.2(4) N1 C4 C5 C6 . . -2.4(4) N1 C4 C5 C10 . . 179.0(2) Cu O4 C6 C7 . . 175.13(17) Cu O4 C6 C5 . . -4.8(3) C10 C5 C6 O4 . . -173.6(2) C4 C5 C6 O4 . . 7.8(4) C10 C5 C6 C7 . . 6.4(4) C4 C5 C6 C7 . . -172.1(2) O4 C6 C7 C8 . . 174.8(2) C5 C6 C7 C8 . . -5.2(4) C6 C7 C8 C9 . . -0.1(4) C7 C8 C9 C10 . . 4.2(4) C8 C9 C10 C5 . . -2.9(4) C6 C5 C10 C9 . . -2.5(4) C4 C5 C10 C9 . . 176.2(3)