#------------------------------------------------------------------------------
#$Date: 2016-02-16 22:30:59 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176467 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/03/4320383.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_4320383
loop_
_publ_author_name
'Oscar Castillo'
'Antonio Luque'
'Pascual Román'
'Francesc Lloret'
'Miguel Julve'
_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       '+34-946 012 701'
_publ_section_title
;
 Syntheses, Crystal Structures, and Magnetic Properties of One-Dimensional
 Oxalato-Bridged Co(II), Ni(II), and Cu(II) Complexes withn-Aminopyridine
 (n= 2-4) as Terminal Ligand
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5526
_journal_page_last               5535
_journal_paper_doi               10.1021/ic0103401
_journal_volume                  40
_journal_year                    2001
_chemical_compound_source        'aqueous synthesis'
_chemical_formula_structural     '[Co(C2O4)(C5H6N2)2]'
_chemical_formula_sum            'C12 H12 Co N4 O4'
_chemical_formula_weight         335.19
_chemical_name_systematic
;
catena-(mu-oxalato)-bis(2-aminopyridine)-cobalt(II)
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             12-mar-01
_audit_creation_method           SHELXL
_cell_angle_alpha                90
_cell_angle_beta                 94.21(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.885(2)
_cell_length_b                   11.010(2)
_cell_length_c                   8.755(1)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      13.94
_cell_measurement_theta_min      6.15
_cell_volume                     1334.8(3)
_computing_cell_refinement       'local programs'
_computing_data_collection       ' CAD4 Express (Enraf Nonius, 1994)'
_computing_data_reduction        'XCAD4 (Harms & Wocadlo, 1995)'
_computing_molecular_graphics    'PLATON (Spek, 1990)'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'DIRDIF-92 (Beurskens, 1992)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'Enraf Nonius CAD4 diffractometer'
_diffrn_measurement_method       'ω/2θ mode'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'x-ray tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.065
_diffrn_reflns_av_sigmaI/netI    0.111
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            2162
_diffrn_reflns_theta_max         30.03
_diffrn_reflns_theta_min         2.36
_diffrn_standards_decay_%        1
_diffrn_standards_interval_count 100
_diffrn_standards_interval_time  60
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    1.31
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.668
_exptl_crystal_density_meas      1.66(1)
_exptl_crystal_density_method    flotation
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             684
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.655
_refine_diff_density_min         -0.534
_refine_diff_density_rms         0.105
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_all   0.951
_refine_ls_goodness_of_fit_gt    1.103
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     120
_refine_ls_number_reflns         1947
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.951
_refine_ls_restrained_S_gt       1.103
_refine_ls_R_factor_all          0.1340
_refine_ls_R_factor_gt           0.0581
_refine_ls_shift/esd_mean        0.001
_refine_ls_shift/su_max          -0.012
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0659P)²+0.00P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1392
_refine_ls_wR_factor_gt          0.1187
_reflns_number_gt                1100
_reflns_number_total             1947
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            ic0103401_1.cif
_cod_data_source_block           compound1
_cod_original_formula_sum        'C12 H12 Co1 N4 O4'
_cod_database_code               4320383
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'
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
Co1 0.0179(3) 0.0404(5) 0.0270(4) 0 0.0027(2) 0
O1 0.0235(12) 0.052(2) 0.0286(14) -0.0071(12) -0.0019(11) 0.0085(12)
O2 0.0222(12) 0.049(2) 0.0322(14) -0.0039(12) 0.0019(10) 0.0044(11)
C1 0.019(2) 0.041(2) 0.027(2) 0.007(2) 0.0053(14) -0.002(2)
N11 0.025(2) 0.044(2) 0.040(2) 0.005(2) 0.0038(14) -0.0012(14)
C12 0.024(2) 0.049(3) 0.035(2) -0.008(2) 0.0038(15) -0.006(2)
C13 0.033(2) 0.060(3) 0.041(2) 0.000(2) 0.006(2) -0.013(2)
C14 0.045(2) 0.055(3) 0.058(3) 0.015(3) 0.008(2) -0.014(2)
C15 0.044(3) 0.086(4) 0.077(4) 0.041(4) -0.013(3) -0.017(3)
C16 0.034(2) 0.073(4) 0.079(4) 0.032(3) -0.013(2) -0.018(3)
N17 0.032(2) 0.100(4) 0.048(2) 0.028(3) -0.008(2) -0.026(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_thermal_displace_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_group
Co1 Co 0.0000 0.15128(8) 0.2500 0.0284(2) Uani 1 d S .
O1 O 0.0827(2) 0.0096(3) 0.1584(3) 0.0348(7) Uani 1 d . .
O2 O -0.0783(2) 0.1176(3) 0.0388(3) 0.0343(7) Uani 1 d . .
C1 C 0.0465(2) -0.0317(4) 0.0343(4) 0.0285(8) Uani 1 d . .
N11 N 0.0924(2) 0.2821(3) 0.1523(4) 0.0362(8) Uani 1 d . .
C12 C 0.1854(3) 0.3047(4) 0.1940(5) 0.0362(9) Uani 1 d . .
C13 C 0.2400(3) 0.3846(5) 0.1090(5) 0.0444(11) Uani 1 d . .
C14 C 0.1992(4) 0.4373(5) -0.0175(6) 0.0527(12) Uani 1 d . .
C15 C 0.1032(4) 0.4146(6) -0.0616(7) 0.070(2) Uani 1 d . .
C16 C 0.0543(3) 0.3378(6) 0.0258(7) 0.063(2) Uani 1 d . .
N17 N 0.2257(3) 0.2526(6) 0.3192(5) 0.0603(14) Uani 1 d . .
H131 H 0.306(4) 0.395(5) 0.153(6) 0.060(15) Uiso 1 d . .
H141 H 0.232(4) 0.495(5) -0.071(5) 0.053(14) Uiso 1 d . .
H151 H 0.074(4) 0.454(5) -0.154(6) 0.074(17) Uiso 1 d . .
H161 H -0.007(5) 0.338(6) 0.005(8) 0.10(2) Uiso 1 d . .
H171 H 0.204(3) 0.198(4) 0.357(5) 0.035(13) Uiso 1 d . .
H172 H 0.291(5) 0.262(6) 0.348(7) 0.081(19) Uiso 1 d . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
O O 0.0106 0.0060 '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'
Co Co 0.3494 0.9721 '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'
C C 0.0033 0.0016 '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
O2 Co1 O2 159.7(2) 2_555 . ?
O2 Co1 O1 78.4(1) 2_555 2_555 ?
O2 Co1 O1 86.8(1) . 2_555 ?
O2 Co1 O1 86.8(1) 2_555 . ?
O2 Co1 O1 78.4(1) . . ?
O1 Co1 O1 85.8(2) 2_555 . ?
O2 Co1 N11 93.1(1) 2_555 2_555 ?
O2 Co1 N11 100.5(1) . 2_555 ?
O1 Co1 N11 89.2(1) 2_555 2_555 ?
O1 Co1 N11 174.9(1) . 2_555 ?
O2 Co1 N11 100.5(1) 2_555 . ?
O2 Co1 N11 93.1(1) . . ?
O1 Co1 N11 174.9(1) 2_555 . ?
N11 Co1 N11 95.8(2) 2_555 . ?
O1 Co1 N11 89.2(1) . . ?
C1 O1 Co1 113.6(2) . . ?
C1 O2 Co1 113.9(2) 5_555 . ?
O2 C1 O1 126.2(3) 5_555 . ?
O2 C1 C1 117.5(4) 5_555 5_555 ?
O1 C1 C1 116.3(4) . 5_555 ?
C16 N11 C12 117.1(4) . . ?
C16 N11 Co1 115.1(3) . . ?
C12 N11 Co1 127.4(3) . . ?
N17 C12 N11 119.1(4) . . ?
N17 C12 C13 119.7(4) . . ?
N11 C12 C13 121.2(4) . . ?
C14 C13 C12 119.7(4) . . ?
C13 C14 C15 119.6(5) . . ?
C16 C15 C14 117.9(5) . . ?
N11 C16 C15 124.5(4) . . ?
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
Co1 O1 2.128(3) . ?
Co1 O1 2.128(3) 2_555 ?
Co1 O2 2.108(3) . ?
Co1 O2 2.108(3) 2_555 ?
Co1 N11 2.149(3) . ?
Co1 N11 2.149(3) 2_555 ?
O1 C1 1.249(4) . ?
O2 C1 1.241(5) 5_555 ?
C1 O2 1.241(5) 5_555 ?
C1 C1 1.550(7) 5_555 ?
N11 C16 1.340(6) . ?
N11 C12 1.339(5) . ?
C12 N17 1.324(6) . ?
C12 C13 1.409(6) . ?
C13 C14 1.338(7) . ?
C14 C15 1.383(7) . ?
C15 C16 1.356(7) . ?
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
N17 H171 O2 0.76(4) 2.21(4) 2.883(4) 148(4) 2_555 ?
