#------------------------------------------------------------------------------
#$Date: 2016-02-16 03:10:39 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176453 $
#$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'
'Román, 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_paper_doi               10.1039/b004072j
_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       'ω/2θ 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/[σ²(Fo²)+(0.0527P)²+0.0000P] where P=(Fo²+2Fc²)/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)
_cod_data_source_file            b004072j.txt
_cod_data_source_block           compound1
_cod_original_cell_volume        1692.1(5)
_cod_original_sg_symbol_H-M      P21/c
_cod_original_formula_sum        'C15 H19 Cu1 N3 O6'
_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_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 ?
