#------------------------------------------------------------------------------ #$Date: 2012-02-26 21:34:47 +0000 (Sun, 26 Feb 2012) $ #$Revision: 35909 $ #$URL: svn://www.crystallography.net/cod/cif/7/05/13/7051319.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_7051319 loop_ _publ_author_name 'Castillo, Oscar' 'Luque, Antonio' 'Iglesias, Sonia' 'Vitoria, Pablo' 'Rom\'an, Pascual' _publ_contact_author ; 'Antonio Luque. Departamento de Quimica Inorganica. Facultad de Ciencias Universidad del Pais Vasco, Apdo. 644, E-48080 Bilbao, Spain ; _publ_section_title ; Synthesis, crystal structure, thermal behaviour and magnetic properties of a novel one-dimensional copper(II) complex containing neutral and deprotonated 3-hydroxypyridine ligands ; _journal_issue 10 _journal_name_full 'New Journal of Chemistry' _journal_page_first 771 _journal_volume 24 _journal_year 2000 _chemical_compound_source 'aqueous synthesis' _chemical_formula_sum 'C15 H19 Cu N3 O6' _chemical_formula_weight 400.87 _chemical_name_systematic ; catena-[(mu!2$-pyridin-3-onato-N,0)-{aqua-(pyridin-3-onato) (3-hydroxypyridine)-copper(II)}-water(1/2)] ; _space_group_IT_number 14 _symmetry_cell_setting monoclinic _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_space_group_name_H-M 'P 1 21/c 1' _atom_sites_solution_hydrogens difmap _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_method SHELXL _cell_angle_alpha 90.00 _cell_angle_beta 103.87(2) _cell_angle_gamma 90.00 _cell_formula_units_Z 4 _cell_length_a 8.992(2) _cell_length_b 13.718(1) _cell_length_c 14.130(3) _cell_measurement_reflns_used 25 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 12.02 _cell_measurement_theta_min 7.68 _cell_volume 1692.1(6) _computing_cell_refinement 'local programs' _computing_data_collection 'CAD4 programs' _computing_data_reduction 'XCAD (Harms and Wocadlo,1995)' _computing_molecular_graphics 'PLATON (Spek, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_structure_solution 'SIR-92 (Altomare, 1993)' _diffrn_ambient_temperature 293(2) _diffrn_measurement_device_type 'Enraf Nonius CAD4 diffractometer' _diffrn_measurement_method '\w/2\q mode' _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71069 _diffrn_reflns_av_R_equivalents 0.0285 _diffrn_reflns_av_sigmaI/netI 0.0540 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_number 5116 _diffrn_reflns_theta_max 30.00 _diffrn_reflns_theta_min 2.10 _diffrn_standards_interval_count 98 _diffrn_standards_interval_time 3600 _diffrn_standards_number 2 _exptl_absorpt_coefficient_mu 1.328 _exptl_absorpt_correction_type none _exptl_crystal_colour dark-green _exptl_crystal_density_diffrn 1.574 _exptl_crystal_density_meas 1.56(1) _exptl_crystal_density_method flotation _exptl_crystal_description prismatic _exptl_crystal_F_000 828 _refine_diff_density_max 0.491 _refine_diff_density_min -0.484 _refine_diff_density_rms 0.086 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.007 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 286 _refine_ls_number_reflns 4932 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.007 _refine_ls_R_factor_all 0.0716 _refine_ls_R_factor_gt 0.0373 _refine_ls_shift/su_max 0.030 _refine_ls_shift/su_mean 0.001 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0527P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0909 _refine_ls_wR_factor_ref 0.0972 _reflns_number_gt 3395 _reflns_number_total 4932 _reflns_threshold_expression >2sigma(I) _[local]_cod_data_source_file b004072j.txt _[local]_cod_data_source_block compound1 _[local]_cod_cif_authors_sg_H-M P21/c _[local]_cod_chemical_formula_sum_orig 'C15 H19 Cu1 N3 O6' _cod_original_cell_volume 1692.1(5) _cod_database_code 7051319 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -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 0.08254(3) 0.224977(18) 0.743223(19) 0.02100(8) Uani 1 1 d . . . O1 O 0.1894(2) 0.17909(16) 0.89412(13) 0.0340(4) Uani 1 1 d . . . O27 O 0.4367(2) 0.23581(15) 0.49736(12) 0.0390(4) Uani 1 1 d . . . O17 O -0.3105(2) 0.23639(15) 0.96627(13) 0.0407(4) Uani 1 1 d . . . O37 O 0.1251(2) 0.36373(11) 0.72192(12) 0.0292(4) Uani 1 1 d . . . N31 N 0.0178(2) 0.59580(13) 0.80696(13) 0.0236(4) Uani 1 1 d . . . N21 N 0.2717(2) 0.18386(13) 0.70004(14) 0.0245(4) Uani 1 1 d . . . N11 N -0.1164(2) 0.26660(14) 0.77479(14) 0.0259(4) Uani 1 1 d . . . O2 O 0.1170(3) 0.43677(15) 0.53848(14) 0.0488(5) Uani 1 1 d . . . O3 O 0.3824(4) 0.5320(2) 0.5310(3) 0.1075(12) Uani 1 1 d . . . C12 C -0.1528(3) 0.24033(18) 0.85745(18) 0.0290(5) Uani 1 1 d . . . C13 C -0.2876(3) 0.26803(18) 0.88154(17) 0.0286(5) Uani 1 1 d . . . C14 C -0.3902(3) 0.32635(19) 0.81505(19) 0.0342(5) Uani 1 1 d . . . C15 C -0.3522(3) 0.3522(2) 0.7302(2) 0.0347(5) Uani 1 1 d . . . C16 C -0.2156(3) 0.32188(18) 0.71128(17) 0.0292(5) Uani 1 1 d . . . C22 C 0.2975(3) 0.22195(17) 0.61849(16) 0.0253(4) Uani 1 1 d . . . C23 C 0.4203(3) 0.19540(18) 0.57861(17) 0.0273(5) Uani 1 1 d . . . C24 C 0.5201(3) 0.1252(2) 0.6301(2) 0.0360(6) Uani 1 1 d . . . C25 C 0.4940(3) 0.0867(2) 0.7144(2) 0.0403(6) Uani 1 1 d . . . C26 C 0.3690(3) 0.11634(18) 0.74773(19) 0.0346(5) Uani 1 1 d . . . C32 C 0.0337(3) 0.52106(15) 0.74917(17) 0.0261(5) Uani 1 1 d . . . C33 C 0.1109(3) 0.43448(15) 0.78321(17) 0.0242(4) Uani 1 1 d . . . C34 C 0.1708(3) 0.42846(17) 0.88368(19) 0.0325(5) Uani 1 1 d . . . C35 C 0.1528(3) 0.50504(18) 0.94319(19) 0.0345(5) Uani 1 1 d . . . C36 C 0.0756(3) 0.58794(17) 0.90313(17) 0.0288(5) Uani 1 1 d . . . H321 H -0.012(3) 0.528(2) 0.679(2) 0.035(7) Uiso 1 1 d . . . H361 H 0.065(3) 0.644(2) 0.9377(19) 0.031(7) Uiso 1 1 d . . . H341 H 0.221(3) 0.3746(19) 0.9074(18) 0.024(6) Uiso 1 1 d . . . H351 H 0.192(3) 0.497(2) 1.007(2) 0.041(8) Uiso 1 1 d . . . H11 H 0.259(4) 0.202(2) 0.922(2) 0.039(9) Uiso 1 1 d . . . H12 H 0.166(4) 0.145(3) 0.934(3) 0.073(13) Uiso 1 1 d . . . H261 H 0.346(3) 0.088(2) 0.807(2) 0.040(8) Uiso 1 1 d . . . H221 H 0.232(4) 0.269(2) 0.593(2) 0.047(9) Uiso 1 1 d . . . H121 H -0.080(4) 0.198(2) 0.903(2) 0.047(9) Uiso 1 1 d . . . H151 H -0.421(4) 0.387(2) 0.683(2) 0.048(9) Uiso 1 1 d . . . H251 H 0.551(4) 0.042(2) 0.747(2) 0.048(9) Uiso 1 1 d . . . H161 H -0.192(3) 0.3399(19) 0.6532(19) 0.026(6) Uiso 1 1 d . . . H141 H -0.482(3) 0.342(2) 0.831(2) 0.045(8) Uiso 1 1 d . . . H241 H 0.603(4) 0.114(3) 0.607(2) 0.061(10) Uiso 1 1 d . . . H171 H -0.417(6) 0.251(4) 0.979(4) 0.074(23) Uiso 1 1 d . . . H21 H 0.1226 0.4000 0.5989 0.050 Uiso 1 1 d . . . H22 H 0.0249 0.4600 0.5250 0.050 Uiso 1 1 d . . . H31 H 0.2976 0.5033 0.5170 0.050 Uiso 1 1 d . . . H32 H 0.3467 0.6000 0.5249 0.050 Uiso 1 1 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 0.02521(13) 0.01738(12) 0.02555(13) 0.00090(11) 0.01615(10) 0.00060(11) O1 0.0319(10) 0.0448(11) 0.0246(9) 0.0059(8) 0.0055(8) -0.0052(9) O27 0.0272(8) 0.0643(12) 0.0309(9) 0.0092(9) 0.0178(7) 0.0059(9) O17 0.0337(9) 0.0595(12) 0.0363(9) 0.0050(9) 0.0229(8) 0.0087(9) O37 0.0420(9) 0.0171(7) 0.0364(9) 0.0015(6) 0.0248(8) 0.0009(7) N31 0.0267(9) 0.0176(8) 0.0298(9) -0.0007(7) 0.0134(7) 0.0003(7) N21 0.0252(9) 0.0222(8) 0.0304(10) 0.0010(7) 0.0153(8) 0.0015(7) N11 0.0261(9) 0.0258(9) 0.0301(9) -0.0019(8) 0.0154(7) 0.0011(8) O2 0.0637(14) 0.0497(12) 0.0379(10) 0.0059(9) 0.0216(10) 0.0219(10) O3 0.105(3) 0.0554(17) 0.173(4) -0.024(2) 0.055(3) -0.0205(17) C12 0.0271(11) 0.0326(11) 0.0319(12) 0.0009(10) 0.0162(9) 0.0036(9) C13 0.0256(10) 0.0339(12) 0.0307(11) -0.0042(10) 0.0153(9) 0.0002(10) C14 0.0242(11) 0.0370(13) 0.0440(14) -0.0033(11) 0.0135(10) 0.0055(10) C15 0.0289(12) 0.0366(13) 0.0387(14) 0.0024(11) 0.0086(11) 0.0043(10) C16 0.0308(12) 0.0309(11) 0.0278(11) -0.0007(9) 0.0106(9) -0.0016(10) C22 0.0227(10) 0.0294(10) 0.0272(10) -0.0004(10) 0.0125(8) 0.0023(9) C23 0.0218(10) 0.0346(11) 0.0292(11) -0.0048(9) 0.0130(9) -0.0043(9) C24 0.0273(12) 0.0414(14) 0.0452(15) -0.0021(11) 0.0203(11) 0.0069(10) C25 0.0380(14) 0.0364(13) 0.0519(16) 0.0118(12) 0.0215(13) 0.0153(11) C26 0.0411(14) 0.0281(11) 0.0419(14) 0.0106(10) 0.0242(12) 0.0094(10) C32 0.0319(12) 0.0209(10) 0.0280(11) 0.0010(8) 0.0121(10) 0.0037(9) C33 0.0275(11) 0.0176(9) 0.0329(11) 0.0009(8) 0.0179(9) -0.0010(8) C34 0.0346(13) 0.0236(11) 0.0388(13) 0.0056(10) 0.0079(11) 0.0058(10) C35 0.0396(14) 0.0336(12) 0.0281(12) 0.0018(10) 0.0041(11) 0.0009(10) C36 0.0339(12) 0.0234(10) 0.0307(12) -0.0047(9) 0.0110(10) -0.0005(9) 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' Cu Cu 0.3201 1.2651 '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' 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 O37 Cu1 N21 90.87(7) . . ? O37 Cu1 N11 88.60(7) . . ? N21 Cu1 N11 175.28(8) . . ? O37 Cu1 N31 150.40(7) . 2_546 ? N21 Cu1 N31 89.23(7) . 2_546 ? N11 Cu1 N31 88.93(7) . 2_546 ? O37 Cu1 O1 111.44(8) . . ? N21 Cu1 O1 90.52(8) . . ? N11 Cu1 O1 94.04(8) . . ? N31 Cu1 O1 98.16(8) 2_546 . ? C33 O37 Cu1 123.5(1) . . ? C36 N31 C32 119.0(2) . . ? C36 N31 Cu1 117.1(2) . 2_556 ? C32 N31 Cu1 123.8(2) . 2_556 ? C22 N21 C26 118.5(2) . . ? C22 N21 Cu1 119.0(2) . . ? C26 N21 Cu1 122.5(2) . . ? C12 N11 C16 118.4(2) . . ? C12 N11 Cu1 122.0(2) . . ? C16 N11 Cu1 119.6(2) . . ? N11 C12 C13 123.5(2) . . ? O17 C13 C12 117.5(2) . . ? O17 C13 C14 124.7(2) . . ? C12 C13 C14 117.8(2) . . ? C15 C14 C13 118.2(2) . . ? C14 C15 C16 120.8(2) . . ? N11 C16 C15 121.4(2) . . ? N21 C22 C23 124.1(2) . . ? O27 C23 C24 123.6(2) . . ? O27 C23 C22 120.4(2) . . ? C24 C23 C22 116.1(2) . . ? C25 C24 C23 119.7(2) . . ? C24 C25 C26 120.3(2) . . ? N21 C26 C25 121.3(2) . . ? N31 C32 C33 123.8(2) . . ? O37 C33 C34 123.1(2) . . ? O37 C33 C32 120.9(2) . . ? C34 C33 C32 116.0(2) . . ? C35 C34 C33 120.2(2) . . ? C34 C35 C36 119.9(2) . . ? N31 C36 C35 121.2(2) . . ? 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 O37 1.979(2) . ? Cu1 N21 2.021(2) . ? Cu1 N11 2.027(2) . ? Cu1 N31 2.037(2) 2_546 ? Cu1 O1 2.210(2) . ? O27 C23 1.315(3) . ? O17 C13 1.335(3) . ? O37 C33 1.327(3) . ? N31 C36 1.338(3) . ? N31 C32 1.340(3) . ? N21 C22 1.335(3) . ? N21 C26 1.340(3) . ? N11 C12 1.336(3) . ? N11 C16 1.339(3) . ? C12 C13 1.389(3) . ? C13 C14 1.399(3) . ? C14 C15 1.370(4) . ? C15 C16 1.381(3) . ? C22 C23 1.403(3) . ? C23 C24 1.396(4) . ? C24 C25 1.374(4) . ? C25 C26 1.380(3) . ? C32 C33 1.401(3) . ? C33 C34 1.395(3) . ? C34 C35 1.379(4) . ? C35 C36 1.381(3) . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A _geom_hbond_publ_flag O1 H11 O27 0.73(3) 1.90(3) 2.623(3) 178(4) 4_555 ? O1 H12 O2 0.80(4) 1.99(4) 2.783(3) 177(4) 4_555 ? O2 H21 O37 0.9825 1.8030 2.764(3) 164.94 . ? O2 H22 O2 0.8649 1.9721 2.743(3) 147.75 3_566 ? O3 H31 O2 0.8386 1.9490 2.745(4) 158.06 . ? O3 H32 O17 0.9836 1.9083 2.880(4) 168.92 2_556 ? O17 H171 O27 1.04(6) 1.41(6) 2.446(3) 176(5) 4_455 ?