#------------------------------------------------------------------------------
#$Date: 2016-02-16 22:30:59 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176467 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/18/4301885.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_4301885
loop_
_publ_author_name
'Anastasia N. Georgopoulou'
'Catherine P. Raptopoulou'
'Vassilis Psycharis'
'Rafael Ballesteros'
'Belén Abarca'
'Athanassios K. Boudalis'
_publ_section_title
;
Ferromagnetic CuII4, CoII4, and NiII6 Azido Complexes Derived from
Metal-Assisted Methanolysis of Di-2,6-(2-pyridylcarbonyl)pyridine
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3167
_journal_page_last               3176
_journal_paper_doi               10.1021/ic900115c
_journal_volume                  48
_journal_year                    2009
_chemical_formula_sum            'C38.5 H36 Co4 N14 O14.5'
_chemical_formula_weight         1162.53
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           12
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-I 2y'
_symmetry_space_group_name_H-M   'I 1 2/m 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 100.2780(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   11.3290(2)
_cell_length_b                   13.9776(2)
_cell_length_c                   15.1100(3)
_cell_measurement_temperature    180(2)
_cell_volume                     2354.31(7)
_computing_cell_refinement       'CrystalClear, Rigaku, MSC, 2005'
_computing_data_collection       'CrystalClear, Rigaku, MSC, 2005'
_computing_data_reduction        'CrystalClear, Rigaku, MSC, 2005'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      180(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Rigaku, R-AXIS SPIDER IPDS'
_diffrn_measurement_method       'θ scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0752
_diffrn_reflns_av_sigmaI/netI    0.0544
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            12882
_diffrn_reflns_theta_full        65.00
_diffrn_reflns_theta_max         65.00
_diffrn_reflns_theta_min         7.27
_exptl_absorpt_coefficient_mu    11.546
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.630
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.640
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       parall
_exptl_crystal_F_000             1178
_exptl_crystal_size_max          0.37
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.23
_refine_diff_density_max         0.561
_refine_diff_density_min         -0.773
_refine_diff_density_rms         0.091
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     221
_refine_ls_number_reflns         2087
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.0477
_refine_ls_R_factor_gt           0.0462
_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/[σ²(Fo²)+(0.0651P)²+7.4255P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1216
_refine_ls_wR_factor_ref         0.1231
_reflns_number_gt                2006
_reflns_number_total             2087
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic900115c_si_001_2.cif
_cod_data_source_block           complex2
_cod_original_sg_symbol_H-M      'I 2/m'
_cod_original_formula_sum        'C38.50 H36 Co4 N14 O14.50'
_cod_database_code               4301885
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z'
'x+1/2, y+1/2, z+1/2'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z'
'-x+1/2, -y+1/2, -z+1/2'
'x+1/2, -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
Co1 Co 0.18806(6) 0.0000 0.11993(4) 0.0147(2) Uani 1 2 d S . .
Co2 Co 0.0000 0.12603(5) 0.0000 0.0143(2) Uani 1 2 d S . .
O1 O -0.17150(18) 0.13988(16) -0.07372(14) 0.0159(5) Uani 1 1 d . . .
O2 O -0.35753(19) 0.21447(17) -0.07676(15) 0.0230(5) Uani 1 1 d . . .
N1 N -0.0780(2) 0.2227(2) 0.07855(17) 0.0201(6) Uani 1 1 d . . .
N2 N -0.2753(3) 0.0000 -0.0124(2) 0.0162(8) Uani 1 2 d S . .
C1 C -0.0195(3) 0.2751(3) 0.1467(3) 0.0320(9) Uani 1 1 d . . .
C2 C -0.0767(4) 0.3409(4) 0.1920(3) 0.0475(13) Uani 1 1 d . . .
C3 C -0.1970(4) 0.3545(3) 0.1659(3) 0.0441(11) Uani 1 1 d . . .
C4 C -0.2592(3) 0.3023(3) 0.0937(3) 0.0322(9) Uani 1 1 d . . .
C5 C -0.1963(3) 0.2360(2) 0.0524(2) 0.0197(7) Uani 1 1 d . . .
C6 C -0.2561(3) 0.1695(2) -0.0238(2) 0.0167(7) Uani 1 1 d . . .
C7 C -0.3091(2) 0.0832(2) 0.0178(2) 0.0160(7) Uani 1 1 d . . .
C8 C -0.3854(3) 0.0859(3) 0.0807(2) 0.0192(7) Uani 1 1 d . . .
C9 C -0.4238(4) 0.0000 0.1106(3) 0.0219(10) Uani 1 2 d S . .
C10 C -0.3283(4) 0.2922(3) -0.1306(3) 0.0358(9) Uani 1 1 d . . .
N11 N 0.2924(4) 0.0000 0.2846(3) 0.0258(9) Uani 1 2 d S . .
O11 O 0.3514(3) 0.0000 0.2204(2) 0.0373(10) Uani 1 2 d S . .
O12 O 0.1790(3) 0.0000 0.2595(2) 0.0358(9) Uani 1 2 d S . .
O13 O 0.3404(4) 0.0000 0.3626(2) 0.0438(10) Uani 1 2 d S . .
N21 N -0.0080(3) 0.0000 0.0876(2) 0.0162(8) Uani 1 2 d S . .
N22 N -0.0609(3) 0.0000 0.1528(3) 0.0226(9) Uani 1 2 d S . .
N23 N -0.1114(4) 0.0000 0.2107(3) 0.0428(13) Uani 1 2 d S . .
OM O -0.476(2) 0.5000 -0.016(2) 0.074(7) Uani 0.25 2 d SP . .
CM C -0.533(2) 0.5000 -0.090(2) 0.076(11) Uani 0.25 2 d SP . .
H1 H 0.067(4) 0.269(3) 0.154(3) 0.053(14) Uiso 1 1 d . . .
H2 H -0.046(5) 0.376(4) 0.228(4) 0.08(2) Uiso 1 1 d . . .
H3 H -0.230(4) 0.399(3) 0.194(3) 0.046(13) Uiso 1 1 d . . .
H4 H -0.347(4) 0.306(4) 0.076(3) 0.054(14) Uiso 1 1 d . . .
H8 H -0.410(3) 0.143(2) 0.100(2) 0.006(7) Uiso 1 1 d . . .
H9 H -0.485(6) 0.0000 0.153(4) 0.046(18) Uiso 1 2 d S . .
H10A H -0.284(4) 0.266(3) -0.177(3) 0.038(12) Uiso 1 1 d . . .
H10B H -0.405(5) 0.319(4) -0.155(3) 0.058(15) Uiso 1 1 d . . .
H10C H -0.278(4) 0.335(3) -0.098(3) 0.029(11) 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 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Co Co -2.3653 3.6143 '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
N2 Co1 O1 76.12(6) 5 5 ?
N2 Co1 O1 76.12(6) 5 2 ?
O1 Co1 O1 141.12(12) 5 2 ?
N2 Co1 O12 154.35(14) 5 . ?
O1 Co1 O12 108.43(6) 5 . ?
O1 Co1 O12 108.43(6) 2 . ?
N2 Co1 O11 94.78(14) 5 . ?
O1 Co1 O11 104.47(6) 5 . ?
O1 Co1 O11 104.47(6) 2 . ?
O12 Co1 O11 59.57(13) . . ?
N2 Co1 N21 115.96(14) 5 . ?
O1 Co1 N21 84.12(6) 5 . ?
O1 Co1 N21 84.12(6) 2 . ?
O12 Co1 N21 89.69(13) . . ?
O11 Co1 N21 149.27(13) . . ?
O1 Co2 O1 169.26(13) . 2 ?
O1 Co2 N1 78.13(9) . . ?
O1 Co2 N1 94.88(9) 2 . ?
O1 Co2 N1 94.88(9) . 2 ?
O1 Co2 N1 78.13(9) 2 2 ?
N1 Co2 N1 99.66(15) . 2 ?
O1 Co2 N21 83.51(11) . 5 ?
O1 Co2 N21 105.17(11) 2 5 ?
N1 Co2 N21 156.61(11) . 5 ?
N1 Co2 N21 96.21(10) 2 5 ?
O1 Co2 N21 105.17(11) . . ?
O1 Co2 N21 83.51(11) 2 . ?
N1 Co2 N21 96.21(10) . . ?
N1 Co2 N21 156.61(11) 2 . ?
N21 Co2 N21 74.65(14) 5 . ?
C6 O1 Co2 114.19(18) . . ?
C6 O1 Co1 115.85(19) . 5 ?
Co2 O1 Co1 96.49(9) . 5 ?
C6 O2 C10 114.1(3) . . ?
C1 N1 C5 118.9(3) . . ?
C1 N1 Co2 126.0(2) . . ?
C5 N1 Co2 115.0(2) . . ?
C7 N2 C7 121.9(4) . 6 ?
C7 N2 Co1 118.82(19) . 5 ?
C7 N2 Co1 118.82(19) 6 5 ?
N1 C1 C2 122.4(4) . . ?
N1 C1 H1 113(3) . . ?
C2 C1 H1 124(3) . . ?
C3 C2 C1 119.0(4) . . ?
C3 C2 H2 114(5) . . ?
C1 C2 H2 126(5) . . ?
C2 C3 C4 119.6(4) . . ?
C2 C3 H3 117(3) . . ?
C4 C3 H3 123(3) . . ?
C5 C4 C3 118.3(4) . . ?
C5 C4 H4 119(3) . . ?
C3 C4 H4 122(3) . . ?
N1 C5 C4 121.9(3) . . ?
N1 C5 C6 114.8(3) . . ?
C4 C5 C6 123.3(3) . . ?
O1 C6 O2 113.2(2) . . ?
O1 C6 C7 110.4(3) . . ?
O2 C6 C7 104.0(2) . . ?
O1 C6 C5 109.5(2) . . ?
O2 C6 C5 110.9(3) . . ?
C7 C6 C5 108.7(2) . . ?
N2 C7 C8 120.6(3) . . ?
N2 C7 C6 112.9(3) . . ?
C8 C7 C6 126.5(3) . . ?
C9 C8 C7 118.0(3) . . ?
C9 C8 H8 121.5(19) . . ?
C7 C8 H8 120.5(19) . . ?
C8 C9 C8 120.9(4) . 6 ?
C8 C9 H9 119.5(2) . . ?
C8 C9 H9 119.5(2) 6 . ?
O2 C10 H10A 109(2) . . ?
O2 C10 H10B 103(3) . . ?
H10A C10 H10B 114(4) . . ?
O2 C10 H10C 112(3) . . ?
H10A C10 H10C 106(3) . . ?
H10B C10 H10C 113(4) . . ?
O13 N11 O11 122.6(4) . . ?
O13 N11 O12 123.1(4) . . ?
O11 N11 O12 114.3(4) . . ?
N11 O11 Co1 92.0(3) . . ?
N11 O12 Co1 94.0(3) . . ?
N22 N21 Co1 116.0(3) . . ?
N22 N21 Co2 123.46(11) . 5 ?
Co1 N21 Co2 89.16(10) . 5 ?
N22 N21 Co2 123.46(11) . . ?
Co1 N21 Co2 89.16(10) . . ?
Co2 N21 Co2 105.35(14) 5 . ?
N23 N22 N21 178.4(5) . . ?
OM OM CM 105(6) 5_465 . ?
OM OM CM 47(4) 5_465 5_465 ?
CM OM CM 151.5(18) . 5_465 ?
OM CM OM 28.5(18) . 5_465 ?
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 N2 2.046(4) 5 ?
Co1 O1 2.073(2) 5 ?
Co1 O1 2.073(2) 2 ?
Co1 O12 2.130(3) . ?
Co1 O11 2.174(4) . ?
Co1 N21 2.187(4) . ?
Co2 O1 2.069(2) . ?
Co2 O1 2.069(2) 2 ?
Co2 N1 2.095(3) . ?
Co2 N1 2.095(3) 2 ?
Co2 N21 2.215(2) 5 ?
Co2 N21 2.215(2) . ?
O1 C6 1.384(3) . ?
O1 Co1 2.073(2) 5 ?
O2 C6 1.424(4) . ?
O2 C10 1.431(5) . ?
N1 C1 1.339(5) . ?
N1 C5 1.341(4) . ?
N2 C7 1.331(4) . ?
N2 C7 1.331(4) 6 ?
N2 Co1 2.046(4) 5 ?
C1 C2 1.376(6) . ?
C1 H1 0.97(5) . ?
C2 C3 1.363(6) . ?
C2 H2 0.76(6) . ?
C3 C4 1.394(6) . ?
C3 H3 0.87(5) . ?
C4 C5 1.384(5) . ?
C4 H4 0.99(5) . ?
C5 C6 1.540(5) . ?
C6 C7 1.532(4) . ?
C7 C8 1.394(4) . ?
C8 C9 1.381(4) . ?
C8 H8 0.92(3) . ?
C9 C8 1.381(4) 6 ?
C9 H9 1.03(6) . ?
C10 H10A 1.01(4) . ?
C10 H10B 0.96(5) . ?
C10 H10C 0.91(4) . ?
N11 O13 1.207(5) . ?
N11 O11 1.272(5) . ?
N11 O12 1.273(5) . ?
N21 N22 1.242(5) . ?
N21 Co2 2.215(2) 5 ?
N22 N23 1.127(6) . ?
OM OM 0.78(4) 5_465 ?
OM CM 1.19(4) . ?
OM CM 1.59(4) 5_465 ?
CM OM 1.59(4) 5_465 ?
