# Supplementary Material (ESI) for New Journal of Chemistry # This journal is © The Royal Society of Chemistry and # The Centre National de la Recherche Scientifique, 2000 # CCDC Number: 440/200 # CIF-file generated for [Cu(µ-3-pyO-N,0)(3-pyOH)(3-pyO)(H2O)].2H2O # (ref. B004072J) data_compound1 _audit_creation_method SHELXL _publ_contact_author ; 'Antonio Luque. Departamento de Quimica Inorganica. Facultad de Ciencias Universidad del Pais Vasco, Apdo. 644, E-48080 Bilbao, Spain ; _publ_contact_author_email 'qipluara@lg.ehu.es' _publ_contact_author_fax '+34-94-464 85 00' _publ_contact_author_phone '+34-94-601 27 01' _publ_requested_journal 'New Journal of Chemistry' _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. New Journal of Chemistry. ; loop_ _publ_author_name _publ_author_address 'Oscar Castillo' ; Departamento de Quimica Inorganica. Facultad de Ciencias Universidad del Pais Vasco, Apartado. 644, E-48080 Bilbao, Spain ; 'Antonio Luque' ; Departamento de Quimica Inorganica. Facultad de Ciencias Universidad del Pais Vasco, Apartado. 644, E-48080 Bilbao, Spain ; 'Sonia Iglesias' ; Departamento de Quimica Inorganica. Facultad de Ciencias Universidad del Pais Vasco, Apartado. 644, E-48080 Bilbao, Spain ; 'Pablo Vitoria' ; Departamento de Quimica Inorganica. Facultad de Ciencias Universidad del Pais Vasco, Apartado. 644, E-48080 Bilbao, Spain ; 'Pascual Roman' ; Departamento de Quimica Inorganica. Facultad de Ciencias Universidad del Pais Vasco, Apartado. 644, E-48080 Bilbao, Spain ; _chemical_name_systematic ; catena-[(mu!2$-pyridin-3-onato-N,0)-{aqua-(pyridin-3-onato) (3-hydroxypyridine)-copper(II)}-water(1/2)] ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C15 H19 Cu1 N3 O6' _chemical_formula_weight 400.87 _chemical_compound_source 'aqueous synthesis' 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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P21/c' 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' _cell_length_a 8.992(2) _cell_length_b 13.718(1) _cell_length_c 14.130(3) _cell_angle_alpha 90.00 _cell_angle_beta 103.87(2) _cell_angle_gamma 90.00 _cell_volume 1692.1(5) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 7.68 _cell_measurement_theta_max 12.02 _exptl_crystal_description 'prismatic' _exptl_crystal_colour 'dark-green' _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas 1.56(1) _exptl_crystal_density_diffrn 1.574 _exptl_crystal_density_method 'flotation' _exptl_crystal_F_000 828 _exptl_absorpt_coefficient_mu 1.328 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Enraf Nonius CAD4 diffractometer' _diffrn_measurement_method '\w/2\q mode' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 2 _diffrn_standards_interval_count 98 _diffrn_standards_interval_time 3600 _diffrn_standards_decay_% ? _diffrn_reflns_number 5116 _diffrn_reflns_av_R_equivalents 0.0285 _diffrn_reflns_av_sigmaI/netI 0.0540 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.10 _diffrn_reflns_theta_max 30.00 _reflns_number_total 4932 _reflns_number_gt 3395 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CAD4 programs' _computing_cell_refinement 'local programs' _computing_data_reduction 'XCAD (Harms and Wocadlo,1995)' _computing_structure_solution 'SIR-92 (Altomare, 1993)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'PLATON (Spek, 1990)' _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0527P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4932 _refine_ls_number_parameters 286 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0716 _refine_ls_R_factor_gt 0.0373 _refine_ls_wR_factor_ref 0.0972 _refine_ls_wR_factor_gt 0.0909 _refine_ls_goodness_of_fit_ref 1.007 _refine_ls_restrained_S_all 1.007 _refine_ls_shift/su_max 0.030 _refine_ls_shift/su_mean 0.001 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) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; 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_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_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 # #D H A D - H H...A D...A D - H...A symm(A) # 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 ? _refine_diff_density_max 0.491 _refine_diff_density_min -0.484 _refine_diff_density_rms 0.086