#------------------------------------------------------------------------------
#$Date: 2016-03-23 16:00:54 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179358 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/55/4325537.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_4325537
loop_
_publ_author_name
'Yan-Qin Wang'
'Xiu-Mei Zhang'
'Xiu-Bing Li'
'Bing-Wu Wang'
'En-Qing Gao'
_publ_section_title
;
 Magnetic Systems with Mixed Carboxylate and Azide Bridges: Slow
 Relaxation in Co(II) Metamagnet and Spin Frustration in Mn(II) Compound
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              6314
_journal_page_last               6322
_journal_paper_doi               10.1021/ic200732f
_journal_volume                  50
_journal_year                    2011
_chemical_formula_sum            'C13 H15 Co N8 O3'
_chemical_formula_weight         390.26
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                112.285(2)
_cell_angle_beta                 90.944(2)
_cell_angle_gamma                105.8300(10)
_cell_formula_units_Z            2
_cell_length_a                   6.4671(3)
_cell_length_b                   11.7923(6)
_cell_length_c                   12.1807(9)
_cell_measurement_reflns_used    8033
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.29
_cell_measurement_theta_min      3.16
_cell_volume                     819.41(8)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'Bruker SHELXTL'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.972
_diffrn_measured_fraction_theta_max 0.972
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0187
_diffrn_reflns_av_sigmaI/netI    0.0183
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            10328
_diffrn_reflns_theta_full        26.51
_diffrn_reflns_theta_max         26.51
_diffrn_reflns_theta_min         1.82
_diffrn_standards_decay_%        2.5
_exptl_absorpt_coefficient_mu    1.080
_exptl_absorpt_correction_T_max  0.7801
_exptl_absorpt_correction_T_min  0.5902
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker, 1999)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.582
_exptl_crystal_description       plate
_exptl_crystal_F_000             400
_exptl_crystal_size_max          0.55
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.24
_refine_diff_density_max         0.477
_refine_diff_density_min         -0.263
_refine_diff_density_rms         0.054
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.096
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     241
_refine_ls_number_reflns         3308
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.096
_refine_ls_R_factor_all          0.0302
_refine_ls_R_factor_gt           0.0280
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0422P)²+0.4713P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0818
_refine_ls_wR_factor_ref         0.0837
_reflns_number_gt                3038
_reflns_number_total             3308
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic200732f_si_002_1.cif
_cod_data_source_block           1
_cod_original_sg_symbol_H-M      'P -1 '
_cod_database_code               4325537
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
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
Co1 Co 1.0000 0.0000 0.5000 0.02465(11) Uani 1 2 d S
Co2 Co 0.5000 0.0000 0.5000 0.02553(11) Uani 1 2 d S
N1 n 1.0029(3) 0.48279(15) 0.30154(14) 0.0305(3) Uani 1 1 d .
N2 n 1.3117(3) 0.11846(15) 0.60972(15) 0.0313(3) Uani 1 1 d .
N3 n 1.3573(3) 0.23062(16) 0.63501(17) 0.0370(4) Uani 1 1 d .
N4 n 1.3987(4) 0.34034(19) 0.6620(3) 0.0662(7) Uani 1 1 d .
N5 n 0.7897(3) 0.06812(16) 0.62637(15) 0.0325(4) Uani 1 1 d .
N6 n 0.8047(3) 0.0559(2) 0.71842(18) 0.0517(5) Uani 1 1 d .
N7 n 0.8228(6) 0.0467(5) 0.8075(3) 0.1124(14) Uani 1 1 d .
N8 n 0.3630(4) 0.1408(2) -0.0281(2) 0.0632(6) Uani 1 1 d .
O1 O 0.6443(2) 0.14258(13) 0.43920(13) 0.0343(3) Uani 1 1 d .
O2 O 0.9923(2) 0.14226(13) 0.44166(13) 0.0343(3) Uani 1 1 d .
O3 O 0.3404(4) 0.2874(2) 0.15153(18) 0.0706(6) Uani 1 1 d .
C1 C 0.8370(3) 0.18037(16) 0.42503(16) 0.0261(4) Uani 1 1 d .
C2 C 0.8950(3) 0.28841(17) 0.38082(16) 0.0263(4) Uani 1 1 d .
C3 C 0.7356(3) 0.31667(19) 0.32736(18) 0.0336(4) Uani 1 1 d .
H3A H 0.5904 0.2703 0.3190 0.040 Uiso 1 1 calc R
C4 C 0.7936(3) 0.4135(2) 0.28693(19) 0.0363(4) Uani 1 1 d .
H4A H 0.6877 0.4313 0.2493 0.044 Uiso 1 1 calc R
C5 C 1.1593(3) 0.4570(2) 0.35272(19) 0.0363(4) Uani 1 1 d .
H5A H 1.3031 0.5056 0.3613 0.044 Uiso 1 1 calc R
C6 C 1.1089(3) 0.3592(2) 0.39275(19) 0.0347(4) Uani 1 1 d .
H6A H 1.2182 0.3412 0.4275 0.042 Uiso 1 1 calc R
C7 C 1.0599(4) 0.5899(2) 0.2593(2) 0.0393(5) Uani 1 1 d .
H7A H 1.2104 0.6403 0.2889 0.047 Uiso 1 1 calc R
H7B H 0.9709 0.6459 0.2921 0.047 Uiso 1 1 calc R
C8 C 1.0266(4) 0.5411(2) 0.1245(2) 0.0381(5) Uani 1 1 d .
C9 C 1.1351(5) 0.4608(3) 0.0554(2) 0.0648(8) Uani 1 1 d .
C10 C 0.8919(5) 0.5804(3) 0.0686(2) 0.0628(8) Uani 1 1 d .
C11 C 0.5043(8) 0.2336(4) -0.0642(4) 0.1014(13) Uani 1 1 d .
H11A H 0.5344 0.3177 -0.0013 0.152 Uiso 1 1 calc R
H11B H 0.4356 0.2321 -0.1354 0.152 Uiso 1 1 calc R
H11C H 0.6376 0.2132 -0.0799 0.152 Uiso 1 1 calc R
C12 C 0.2988(7) 0.0066(4) -0.1112(4) 0.1048(15) Uani 1 1 d .
H12B H 0.2045 -0.0448 -0.0763 0.157 Uiso 1 1 calc R
H12C H 0.4254 -0.0213 -0.1278 0.157 Uiso 1 1 calc R
H12A H 0.2239 -0.0028 -0.1843 0.157 Uiso 1 1 calc R
C13 C 0.2946(5) 0.1780(3) 0.0768(3) 0.0617(7) Uani 1 1 d .
H9 H 1.226(6) 0.425(3) 0.091(3) 0.084(10) Uiso 1 1 d .
H10 H 0.815(6) 0.638(3) 0.116(3) 0.076(9) Uiso 1 1 d .
H13 H 0.187(6) 0.112(4) 0.095(3) 0.091(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 0.0033 0.0016 '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'
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'
H H 0.0000 0.0000 '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
O2 Co1 O2 180.0 2_756 .
O2 Co1 N5 87.70(6) 2_756 2_756
O2 Co1 N5 92.30(6) . 2_756
O2 Co1 N5 92.30(6) 2_756 .
O2 Co1 N5 87.70(6) . .
N5 Co1 N5 180.00(8) 2_756 .
O2 Co1 N2 89.24(6) 2_756 .
O2 Co1 N2 90.76(6) . .
N5 Co1 N2 81.02(6) 2_756 .
N5 Co1 N2 98.98(6) . .
O2 Co1 N2 90.76(6) 2_756 2_756
O2 Co1 N2 89.24(6) . 2_756
N5 Co1 N2 98.98(6) 2_756 2_756
N5 Co1 N2 81.02(6) . 2_756
N2 Co1 N2 180.0 . 2_756
O1 Co2 O1 180.0 2_656 .
O1 Co2 N5 91.76(6) 2_656 .
O1 Co2 N5 88.24(6) . .
O1 Co2 N5 88.24(6) 2_656 2_656
O1 Co2 N5 91.76(6) . 2_656
N5 Co2 N5 180.00(6) . 2_656
O1 Co2 N2 90.87(6) 2_656 2_756
O1 Co2 N2 89.13(6) . 2_756
N5 Co2 N2 80.48(6) . 2_756
N5 Co2 N2 99.52(6) 2_656 2_756
O1 Co2 N2 89.13(6) 2_656 1_455
O1 Co2 N2 90.87(6) . 1_455
N5 Co2 N2 99.52(6) . 1_455
N5 Co2 N2 80.48(6) 2_656 1_455
N2 Co2 N2 180.00(9) 2_756 1_455
C4 N1 C5 121.04(15) . .
C4 N1 C7 118.94(16) . .
C5 N1 C7 120.02(17) . .
N3 N2 Co1 116.71(13) . .
N3 N2 Co2 122.50(13) . 1_655
Co1 N2 Co2 95.47(6) . 1_655
N4 N3 N2 178.3(2) . .
N6 N5 Co1 117.33(14) . .
N6 N5 Co2 127.08(15) . .
Co1 N5 Co2 97.40(7) . .
N7 N6 N5 178.5(4) . .
C13 N8 C11 120.0(3) . .
C13 N8 C12 121.9(3) . .
C11 N8 C12 118.0(3) . .
C1 O1 Co2 128.30(11) . .
C1 O2 Co1 129.79(11) . .
O1 C1 O2 129.26(16) . .
O1 C1 C2 116.20(15) . .
O2 C1 C2 114.54(15) . .
C6 C2 C3 118.98(16) . .
C6 C2 C1 119.99(16) . .
C3 C2 C1 121.03(16) . .
C4 C3 C2 119.58(18) . .
C4 C3 H3A 120.2 . .
C2 C3 H3A 120.2 . .
N1 C4 C3 120.33(17) . .
N1 C4 H4A 119.8 . .
C3 C4 H4A 119.8 . .
N1 C5 C6 120.61(18) . .
N1 C5 H5A 119.7 . .
C6 C5 H5A 119.7 . .
C2 C6 C5 119.44(17) . .
C2 C6 H6A 120.3 . .
C5 C6 H6A 120.3 . .
N1 C7 C8 112.17(17) . .
N1 C7 H7A 109.2 . .
C8 C7 H7A 109.2 . .
N1 C7 H7B 109.2 . .
C8 C7 H7B 109.2 . .
H7A C7 H7B 107.9 . .
C9 C8 C10 118.4(2) . .
C9 C8 C7 121.3(2) . .
C10 C8 C7 120.3(2) . .
C8 C9 C10 120.7(2) . 2_765
C8 C9 H9 121(2) . .
C10 C9 H9 118(2) 2_765 .
C8 C10 C9 120.9(2) . 2_765
C8 C10 H10 119.4(19) . .
C9 C10 H10 119.8(19) 2_765 .
N8 C11 H11A 109.5 . .
N8 C11 H11B 109.5 . .
H11A C11 H11B 109.5 . .
N8 C11 H11C 109.5 . .
H11A C11 H11C 109.5 . .
H11B C11 H11C 109.5 . .
N8 C12 H12B 109.5 . .
N8 C12 H12C 109.5 . .
H12B C12 H12C 109.5 . .
N8 C12 H12A 109.5 . .
H12B C12 H12A 109.5 . .
H12C C12 H12A 109.5 . .
O3 C13 N8 126.3(3) . .
O3 C13 H13 116(2) . .
N8 C13 H13 117(2) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Co1 O2 2.0664(12) 2_756
Co1 O2 2.0664(12) .
Co1 N5 2.1426(16) 2_756
Co1 N5 2.1426(16) .
Co1 N2 2.1820(16) .
Co1 N2 2.1820(16) 2_756
Co2 O1 2.0874(12) 2_656
Co2 O1 2.0874(12) .
Co2 N5 2.1614(16) .
Co2 N5 2.1614(16) 2_656
Co2 N2 2.1875(16) 2_756
Co2 N2 2.1875(16) 1_455
N1 C4 1.345(3) .
N1 C5 1.339(3) .
N1 C7 1.498(2) .
N2 N3 1.186(2) .
N2 Co2 2.1875(16) 1_655
N3 N4 1.157(3) .
N5 N6 1.189(2) .
N6 N7 1.138(3) .
N8 C13 1.312(4) .
N8 C11 1.435(5) .
N8 C12 1.454(4) .
O1 C1 1.243(2) .
O2 C1 1.249(2) .
O3 C13 1.214(4) .
C1 C2 1.523(2) .
C2 C6 1.379(3) .
C2 C3 1.389(3) .
C3 C4 1.374(3) .
C3 H3A 0.9300 .
C4 H4A 0.9300 .
C5 C6 1.379(3) .
C5 H5A 0.9300 .
C6 H6A 0.9300 .
C7 C8 1.509(3) .
C7 H7A 0.9700 .
C7 H7B 0.9700 .
C8 C9 1.369(3) .
C8 C10 1.370(3) .
C9 C10 1.392(4) 2_765
C9 H9 0.99(4) .
C10 C9 1.392(4) 2_765
C10 H10 0.97(3) .
C11 H11A 0.9600 .
C11 H11B 0.9600 .
C11 H11C 0.9600 .
C12 H12B 0.9600 .
C12 H12C 0.9600 .
C12 H12A 0.9600 .
C13 H13 0.98(4) .
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_4
O2 Co1 N2 N3 -159.26(15) 2_756 .
O2 Co1 N2 N3 20.74(15) . .
N5 Co1 N2 N3 112.94(15) 2_756 .
N5 Co1 N2 N3 -67.06(15) . .
N2 Co1 N2 N3 -49(100) 2_756 .
O2 Co1 N2 Co2 70.01(6) 2_756 1_655
O2 Co1 N2 Co2 -109.99(6) . 1_655
N5 Co1 N2 Co2 -17.78(6) 2_756 1_655
N5 Co1 N2 Co2 162.22(6) . 1_655
N2 Co1 N2 Co2 180(100) 2_756 1_655
Co1 N2 N3 N4 83(8) . .
Co2 N2 N3 N4 -161(8) 1_655 .
O2 Co1 N5 N6 30.25(18) 2_756 .
O2 Co1 N5 N6 -149.75(18) . .
N5 Co1 N5 N6 138.7(7) 2_756 .
N2 Co1 N5 N6 -59.35(18) . .
N2 Co1 N5 N6 120.65(18) 2_756 .
O2 Co1 N5 Co2 -108.48(6) 2_756 .
O2 Co1 N5 Co2 71.52(6) . .
N5 Co1 N5 Co2 0(100) 2_756 .
N2 Co1 N5 Co2 161.93(6) . .
N2 Co1 N5 Co2 -18.07(6) 2_756 .
O1 Co2 N5 N6 -24.08(19) 2_656 .
O1 Co2 N5 N6 155.92(19) . .
N5 Co2 N5 N6 47.3(7) 2_656 .
N2 Co2 N5 N6 -114.67(19) 2_756 .
N2 Co2 N5 N6 65.33(19) 1_455 .
O1 Co2 N5 Co1 108.64(6) 2_656 .
O1 Co2 N5 Co1 -71.36(6) . .
N5 Co2 N5 Co1 180.0(6) 2_656 .
N2 Co2 N5 Co1 18.06(6) 2_756 .
N2 Co2 N5 Co1 -161.94(6) 1_455 .
Co1 N5 N6 N7 81(11) . .
Co2 N5 N6 N7 -154(11) . .
O1 Co2 O1 C1 179(100) 2_656 .
N5 Co2 O1 C1 38.79(17) . .
N5 Co2 O1 C1 -141.21(17) 2_656 .
N2 Co2 O1 C1 -41.71(17) 2_756 .
N2 Co2 O1 C1 138.29(17) 1_455 .
O2 Co1 O2 C1 -11(100) 2_756 .
N5 Co1 O2 C1 139.10(17) 2_756 .
N5 Co1 O2 C1 -40.90(17) . .
N2 Co1 O2 C1 -139.85(17) . .
N2 Co1 O2 C1 40.15(17) 2_756 .
Co2 O1 C1 O2 1.1(3) . .
Co2 O1 C1 C2 -179.07(11) . .
Co1 O2 C1 O1 0.0(3) . .
Co1 O2 C1 C2 -179.88(12) . .
O1 C1 C2 C6 162.67(18) . .
O2 C1 C2 C6 -17.5(3) . .
O1 C1 C2 C3 -17.8(3) . .
O2 C1 C2 C3 162.02(18) . .
C6 C2 C3 C4 0.4(3) . .
C1 C2 C3 C4 -179.08(18) . .
C5 N1 C4 C3 1.7(3) . .
C7 N1 C4 C3 -178.41(19) . .
C2 C3 C4 N1 -1.6(3) . .
C4 N1 C5 C6 -0.6(3) . .
C7 N1 C5 C6 179.55(19) . .
C3 C2 C6 C5 0.7(3) . .
C1 C2 C6 C5 -179.80(18) . .
N1 C5 C6 C2 -0.6(3) . .
C4 N1 C7 C8 -69.4(2) . .
C5 N1 C7 C8 110.5(2) . .
N1 C7 C8 C9 -59.5(3) . .
N1 C7 C8 C10 122.9(3) . .
C10 C8 C9 C10 -0.4(5) . 2_765
C7 C8 C9 C10 -178.0(3) . 2_765
C9 C8 C10 C9 0.4(5) . 2_765
C7 C8 C10 C9 178.0(3) . 2_765
C11 N8 C13 O3 -0.7(5) . .
C12 N8 C13 O3 179.7(3) . .
