# Electronic Supplementary Material (ESI) for Dalton Transactions
# This journal is © The Royal Society of Chemistry 2013


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#                                CCDC 
# 
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# 
#  This CIF contains data from an original supplementary publication 
#  deposited with the CCDC, and may include chemical, crystal,   
#  experimental, refinement, atomic coordinates, 
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted. 
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data_compound1
_database_code_depnum_ccdc_archive 'CCDC 905823'
#TrackingRef 'CCDC 905823-905825.cif'
_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C26 H40 Co4 N10 O18'
_chemical_formula_weight         1016.40
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'
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   P-1
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
_cell_length_a                   8.56250(10)
_cell_length_b                   10.60640(10)
_cell_length_c                   11.8189(2)
_cell_angle_alpha                112.8270(10)
_cell_angle_beta                 91.3910(10)
_cell_angle_gamma                105.3220(10)
_cell_volume                     944.38(2)
_cell_formula_units_Z            1
_cell_measurement_temperature    160(2)
_cell_measurement_reflns_used    8993
_cell_measurement_theta_min      6.62
_cell_measurement_theta_max      71.67
_exptl_crystal_description       parallelepiped
_exptl_crystal_colour            red
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.06
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.787
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             518
_exptl_absorpt_coefficient_mu    14.313
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.503
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_process_details   'CrystalClear, Rigaku MSC, 2005'
_exptl_special_details           
;
?
;
_diffrn_ambient_temperature      160(2)
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_type           CuK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Rigaku R-AXIS SPIDER IPDS'
_diffrn_measurement_method       '\q scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            12294
_diffrn_reflns_av_R_equivalents  0.1016
_diffrn_reflns_av_unetI/netI     0.1155
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_theta_min         7.25
_diffrn_reflns_theta_max         65.00
_reflns_number_total             2962
_reflns_number_gt                2247
_reflns_threshold_expression     >2sigma(I)
_computing_data_collection       'CrystalClear, Rigaku MSC, 2005'
_computing_cell_refinement       'CrystalClear, Rigaku MSC, 2005'
_computing_data_reduction        'CrystalClear, Rigaku MSC, 2005'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'DIAMOND (Brandenburg, 2012)'
_computing_publication_material  'WinGX (Farrugia, 1999)'
_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^)+(0.0876P)^2^+1.6931P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    refall
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         2962
_refine_ls_number_parameters     263
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1004
_refine_ls_R_factor_gt           0.0777
_refine_ls_wR_factor_ref         0.1945
_refine_ls_wR_factor_gt          0.1792
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_restrained_S_all      1.055
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
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 0.43614(11) 0.85840(10) 0.89973(10) 0.0218(3) Uani 1 1 d . . .
Co2 Co 0.40980(13) 1.12618(12) 0.83008(11) 0.0324(4) Uani 1 1 d . . .
N1 N 0.2133(6) 0.7409(6) 0.8454(5) 0.0253(14) Uani 1 1 d . . .
O1 O 0.4022(5) 0.9237(5) 0.7731(5) 0.0306(13) Uani 1 1 d . . .
O2 O 0.3594(5) 1.0072(5) 1.0060(5) 0.0303(12) Uani 1 1 d . . .
O3 O 0.4355(5) 0.7794(5) 1.0183(4) 0.0274(12) Uani 1 1 d . . .
N2 N 0.5475(6) 0.7248(5) 0.7890(5) 0.0231(13) Uani 1 1 d . . .
N3 N 0.4533(9) 1.1521(7) 0.6220(8) 0.0438(19) Uani 1 1 d . . .
O4 O 0.5605(7) 1.1938(6) 0.7172(6) 0.0406(14) Uani 1 1 d . . .
O5 O 0.3108(7) 1.0901(6) 0.6335(5) 0.0493(16) Uani 1 1 d . . .
O6 O 0.4854(7) 1.1645(7) 0.5283(6) 0.0567(17) Uani 1 1 d . . .
N4 N 0.2055(7) 1.2768(6) 0.8948(6) 0.0328(16) Uani 1 1 d . . .
O7 O 0.3434(6) 1.3437(5) 0.8828(5) 0.0390(14) Uani 1 1 d . . .
O8 O 0.1822(6) 1.1466(5) 0.8753(5) 0.0406(14) Uani 1 1 d . . .
O9 O 0.0975(6) 1.3352(6) 0.9254(6) 0.0496(16) Uani 1 1 d . . .
C1 C 0.2580(8) 0.8276(8) 0.6832(7) 0.0334(19) Uani 1 1 d . . .
H1A H 0.2884 0.7978 0.5985 0.047 Uiso 1 1 calc R . .
H1B H 0.1752 0.8786 0.6875 0.047 Uiso 1 1 calc R . .
C2 C 0.1868(9) 0.6979(8) 0.7087(7) 0.0331(19) Uani 1 1 d . . .
H2A H 0.0683 0.6578 0.6772 0.046 Uiso 1 1 calc R . .
H2B H 0.2405 0.6236 0.6663 0.046 Uiso 1 1 calc R . .
C3 C 0.2045(8) 0.9528(7) 1.0314(7) 0.036(2) Uani 1 1 d . . .
H3A H 0.1501 1.0288 1.0625 0.050 Uiso 1 1 calc R . .
H3B H 0.2125 0.9150 1.0952 0.050 Uiso 1 1 calc R . .
C4 C 0.1083(8) 0.8336(7) 0.9110(7) 0.0252(17) Uani 1 1 d . . .
H4A H 0.0097 0.7744 0.9287 0.035 Uiso 1 1 calc R . .
H4B H 0.0722 0.8753 0.8570 0.035 Uiso 1 1 calc R . .
C5 C 0.2854(8) 0.6704(8) 1.0069(7) 0.0308(18) Uani 1 1 d . . .
H5A H 0.2178 0.7111 1.0699 0.043 Uiso 1 1 calc R . .
H5B H 0.3103 0.5906 1.0200 0.043 Uiso 1 1 calc R . .
C6 C 0.1947(8) 0.6167(7) 0.8789(7) 0.0305(19) Uani 1 1 d . . .
H6A H 0.2398 0.5452 0.8187 0.043 Uiso 1 1 calc R . .
H6B H 0.0775 0.5703 0.8771 0.043 Uiso 1 1 calc R . .
C11 C 0.6052(8) 0.7460(8) 0.6914(7) 0.0318(18) Uani 1 1 d . . .
H11 H 0.5874 0.8221 0.6746 0.041 Uiso 1 1 calc R . .
C12 C 0.6899(9) 0.6607(9) 0.6143(8) 0.041(2) Uani 1 1 d . . .
H12 H 0.7297 0.6789 0.5461 0.053 Uiso 1 1 calc R . .
C13 C 0.7163(9) 0.5503(8) 0.6363(8) 0.042(2) Uani 1 1 d . . .
H13 H 0.7716 0.4891 0.5830 0.055 Uiso 1 1 calc R . .
C14 C 0.6606(8) 0.5304(7) 0.7375(8) 0.0347(19) Uani 1 1 d . . .
H14 H 0.6809 0.4571 0.7575 0.045 Uiso 1 1 calc R . .
C15 C 0.5755(8) 0.6167(7) 0.8098(7) 0.0321(18) Uani 1 1 d . . .
H15 H 0.5344 0.5991 0.8779 0.042 Uiso 1 1 calc R . .
N5 N -0.0084(11) 0.6719(10) 0.4156(9) 0.073(3) Uani 1 1 d . . .
C21 C 0.0361(11) 0.7652(12) 0.3889(8) 0.052(3) Uani 1 1 d . . .
C22 C 0.0986(11) 0.8917(10) 0.3606(9) 0.060(3) Uani 1 1 d . . .
H22A H 0.1470 0.9764 0.4378 0.090 Uiso 1 1 calc R . .
H22B H 0.0082 0.9064 0.3197 0.090 Uiso 1 1 calc R . .
H22C H 0.1819 0.8763 0.3056 0.090 Uiso 1 1 calc R . .
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 0.0150(6) 0.0204(6) 0.0331(8) 0.0116(5) 0.0075(5) 0.0089(4)
Co2 0.0250(6) 0.0316(7) 0.0454(9) 0.0184(7) 0.0087(6) 0.0116(5)
N1 0.023(3) 0.031(3) 0.030(4) 0.016(3) 0.004(3) 0.014(3)
O1 0.028(3) 0.037(3) 0.041(4) 0.025(3) 0.015(3) 0.018(2)
O2 0.014(2) 0.029(3) 0.040(3) 0.004(2) 0.008(2) 0.008(2)
O3 0.020(2) 0.040(3) 0.034(3) 0.024(3) 0.009(2) 0.013(2)
N2 0.017(3) 0.021(3) 0.031(4) 0.011(3) 0.002(3) 0.005(2)
N3 0.049(4) 0.037(4) 0.054(6) 0.025(4) 0.025(4) 0.014(3)
O4 0.036(3) 0.039(3) 0.044(4) 0.016(3) 0.005(3) 0.009(3)
O5 0.041(3) 0.050(4) 0.055(4) 0.022(3) 0.006(3) 0.010(3)
O6 0.068(4) 0.067(4) 0.041(4) 0.033(4) 0.018(3) 0.013(3)
N4 0.025(3) 0.033(3) 0.052(5) 0.024(3) 0.013(3) 0.017(3)
O7 0.026(3) 0.033(3) 0.060(4) 0.020(3) 0.016(3) 0.009(2)
O8 0.034(3) 0.029(3) 0.062(4) 0.022(3) 0.010(3) 0.011(2)
O9 0.039(3) 0.043(3) 0.083(5) 0.033(3) 0.030(3) 0.026(3)
C1 0.024(4) 0.051(5) 0.035(5) 0.026(4) 0.001(4) 0.013(4)
C2 0.030(4) 0.034(4) 0.035(5) 0.012(4) 0.000(4) 0.015(3)
C3 0.016(3) 0.029(4) 0.054(6) 0.009(4) 0.012(4) 0.006(3)
C4 0.018(3) 0.024(4) 0.034(5) 0.009(4) 0.005(3) 0.011(3)
C5 0.022(4) 0.031(4) 0.045(6) 0.022(4) 0.007(4) 0.005(3)
C6 0.020(4) 0.023(4) 0.048(6) 0.013(4) 0.009(4) 0.005(3)
C11 0.026(4) 0.031(4) 0.043(5) 0.017(4) 0.010(4) 0.011(3)
C12 0.036(4) 0.051(5) 0.044(6) 0.019(4) 0.025(4) 0.026(4)
C13 0.027(4) 0.038(4) 0.049(6) -0.001(4) 0.011(4) 0.019(4)
C14 0.030(4) 0.025(4) 0.046(6) 0.008(4) 0.003(4) 0.014(3)
C15 0.025(4) 0.032(4) 0.044(5) 0.018(4) 0.003(4) 0.013(3)
N5 0.074(6) 0.068(6) 0.068(7) 0.022(5) 0.011(5) 0.017(5)
C21 0.039(5) 0.069(7) 0.031(6) 0.002(5) -0.009(4) 0.018(5)
C22 0.044(5) 0.068(7) 0.060(7) 0.018(6) 0.006(5) 0.018(5)
_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
Co1 O2 1.884(4) . ?
Co1 O3 1.891(4) . ?
Co1 N1 1.915(6) . ?
Co1 O1 1.921(5) . ?
Co1 O2 1.922(5) 2_677 ?
Co1 N2 1.991(5) . ?
Co1 Co1 2.907(2) 2_677 ?
Co2 O3 1.939(5) 2_677 ?
Co2 O1 1.968(5) . ?
Co2 O4 2.073(5) . ?
Co2 O8 2.077(5) . ?
Co2 O5 2.303(6) . ?
Co2 O7 2.373(5) . ?
N1 C6 1.488(8) . ?
N1 C2 1.491(9) . ?
N1 C4 1.513(7) . ?
O1 C1 1.458(9) . ?
O2 C3 1.390(7) . ?
O2 Co1 1.922(5) 2_677 ?
O3 C5 1.446(7) . ?
O3 Co2 1.939(5) 2_677 ?
N2 C15 1.339(8) . ?
N2 C11 1.341(8) . ?
N3 O6 1.195(8) . ?
N3 O5 1.262(8) . ?
N3 O4 1.286(9) . ?
N4 O9 1.232(7) . ?
N4 O7 1.250(7) . ?
N4 O8 1.266(7) . ?
C1 C2 1.498(10) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C3 C4 1.516(10) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C5 C6 1.503(10) . ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
C6 H6A 0.9900 . ?
C6 H6B 0.9900 . ?
C11 C12 1.383(9) . ?
C11 H11 0.9500 . ?
C12 C13 1.365(10) . ?
C12 H12 0.9500 . ?
C13 C14 1.368(10) . ?
C13 H13 0.9500 . ?
C14 C15 1.369(9) . ?
C14 H14 0.9500 . ?
C15 H15 0.9500 . ?
N5 C21 1.128(12) . ?
C21 C22 1.475(13) . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
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 O3 92.1(2) . . ?
O2 Co1 N1 88.3(2) . . ?
O3 Co1 N1 85.8(2) . . ?
O2 Co1 O1 86.7(2) . . ?
O3 Co1 O1 171.4(2) . . ?
N1 Co1 O1 85.6(2) . . ?
O2 Co1 O2 80.40(18) . 2_677 ?
O3 Co1 O2 85.6(2) . 2_677 ?
N1 Co1 O2 165.6(2) . 2_677 ?
O1 Co1 O2 102.5(2) . 2_677 ?
O2 Co1 N2 171.2(2) . . ?
O3 Co1 N2 92.0(2) . . ?
N1 Co1 N2 99.7(2) . . ?
O1 Co1 N2 90.4(2) . . ?
O2 Co1 N2 92.2(2) 2_677 . ?
O2 Co1 Co1 40.67(14) . 2_677 ?
O3 Co1 Co1 88.47(16) . 2_677 ?
N1 Co1 Co1 128.38(17) . 2_677 ?
O1 Co1 Co1 96.07(16) . 2_677 ?
O2 Co1 Co1 39.73(12) 2_677 2_677 ?
N2 Co1 Co1 131.75(16) . 2_677 ?
O3 Co2 O1 103.6(2) 2_677 . ?
O3 Co2 O4 97.8(2) 2_677 . ?
O1 Co2 O4 102.57(19) . . ?
O3 Co2 O8 108.2(2) 2_677 . ?
O1 Co2 O8 108.99(19) . . ?
O4 Co2 O8 132.2(2) . . ?
O3 Co2 O5 154.5(2) 2_677 . ?
O1 Co2 O5 91.3(2) . . ?
O4 Co2 O5 58.2(2) . . ?
O8 Co2 O5 85.7(2) . . ?
O3 Co2 O7 87.81(19) 2_677 . ?
O1 Co2 O7 164.88(19) . . ?
O4 Co2 O7 85.41(18) . . ?
O8 Co2 O7 57.22(17) . . ?
O5 Co2 O7 81.98(19) . . ?
C6 N1 C2 112.8(5) . . ?
C6 N1 C4 112.4(5) . . ?
C2 N1 C4 111.4(5) . . ?
C6 N1 Co1 107.4(4) . . ?
C2 N1 Co1 105.5(4) . . ?
C4 N1 Co1 106.7(4) . . ?
C1 O1 Co1 111.7(4) . . ?
C1 O1 Co2 112.3(4) . . ?
Co1 O1 Co2 116.5(3) . . ?
C3 O2 Co1 110.8(4) . . ?
C3 O2 Co1 136.5(5) . 2_677 ?
Co1 O2 Co1 99.60(18) . 2_677 ?
C5 O3 Co1 114.4(4) . . ?
C5 O3 Co2 120.9(4) . 2_677 ?
Co1 O3 Co2 122.2(2) . 2_677 ?
C15 N2 C11 117.1(6) . . ?
C15 N2 Co1 123.4(5) . . ?
C11 N2 Co1 119.5(4) . . ?
O6 N3 O5 122.3(8) . . ?
O6 N3 O4 123.6(7) . . ?
O5 N3 O4 114.1(7) . . ?
N3 O4 Co2 98.9(4) . . ?
N3 O5 Co2 88.8(5) . . ?
O9 N4 O7 121.4(6) . . ?
O9 N4 O8 121.5(6) . . ?
O7 N4 O8 117.1(5) . . ?
N4 O7 Co2 86.1(3) . . ?
N4 O8 Co2 99.5(4) . . ?
O1 C1 C2 110.5(6) . . ?
O1 C1 H1A 109.5 . . ?
C2 C1 H1A 109.5 . . ?
O1 C1 H1B 109.5 . . ?
C2 C1 H1B 109.5 . . ?
H1A C1 H1B 108.1 . . ?
N1 C2 C1 108.5(6) . . ?
N1 C2 H2A 110.0 . . ?
C1 C2 H2A 110.0 . . ?
N1 C2 H2B 110.0 . . ?
C1 C2 H2B 110.0 . . ?
H2A C2 H2B 108.4 . . ?
O2 C3 C4 107.0(6) . . ?
O2 C3 H3A 110.3 . . ?
C4 C3 H3A 110.3 . . ?
O2 C3 H3B 110.3 . . ?
C4 C3 H3B 110.3 . . ?
H3A C3 H3B 108.6 . . ?
N1 C4 C3 110.0(5) . . ?
N1 C4 H4A 109.7 . . ?
C3 C4 H4A 109.7 . . ?
N1 C4 H4B 109.7 . . ?
C3 C4 H4B 109.7 . . ?
H4A C4 H4B 108.2 . . ?
O3 C5 C6 108.0(5) . . ?
O3 C5 H5A 110.1 . . ?
C6 C5 H5A 110.1 . . ?
O3 C5 H5B 110.1 . . ?
C6 C5 H5B 110.1 . . ?
H5A C5 H5B 108.4 . . ?
N1 C6 C5 108.3(5) . . ?
N1 C6 H6A 110.0 . . ?
C5 C6 H6A 110.0 . . ?
N1 C6 H6B 110.0 . . ?
C5 C6 H6B 110.0 . . ?
H6A C6 H6B 108.4 . . ?
N2 C11 C12 122.2(7) . . ?
N2 C11 H11 118.9 . . ?
C12 C11 H11 118.9 . . ?
C13 C12 C11 119.9(7) . . ?
C13 C12 H12 120.1 . . ?
C11 C12 H12 120.1 . . ?
C12 C13 C14 118.0(6) . . ?
C12 C13 H13 121.0 . . ?
C14 C13 H13 121.0 . . ?
C13 C14 C15 119.7(7) . . ?
C13 C14 H14 120.2 . . ?
C15 C14 H14 120.2 . . ?
N2 C15 C14 123.1(7) . . ?
N2 C15 H15 118.4 . . ?
C14 C15 H15 118.4 . . ?
N5 C21 C22 177.0(11) . . ?
C21 C22 H22A 109.5 . . ?
C21 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
C21 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
_diffrn_measured_fraction_theta_max 0.922
_diffrn_reflns_theta_full        65.00
_diffrn_measured_fraction_theta_full 0.922
_refine_diff_density_max         0.745
_refine_diff_density_min         -0.858
_refine_diff_density_rms         0.121
# start Validation Reply Form
_vrf_PLAT029_compound1           
;
PROBLEM: _diffrn_measured_fraction_theta_full Low ....... 0.922
RESPONSE: We have collected data to 2theta=143 deg trying to cover all
possibly accessible reciprocal space, but only those to 2theta=130 deg
were used for the refinement. This alert is due to instrument limitations
for triclinic crystals with small unit cell axis (~10 A) measured with
Cu radiation.
;


data_compound2
_database_code_depnum_ccdc_archive 'CCDC 905824'
#TrackingRef 'CCDC 905823-905825.cif'
_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C52 H60 Co4 N14 O20'
_chemical_formula_weight         1436.86
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'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   P2(1)/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                   12.0397(2)
_cell_length_b                   17.0443(3)
_cell_length_c                   13.8828(2)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.6000(10)
_cell_angle_gamma                90.00
_cell_volume                     2848.71(8)
_cell_formula_units_Z            2
_cell_measurement_temperature    160(2)
_cell_measurement_reflns_used    16098
_cell_measurement_theta_min      6.89
_cell_measurement_theta_max      71.93
_exptl_crystal_description       parallelepiped
_exptl_crystal_colour            red
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.03
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.675
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1476
_exptl_absorpt_coefficient_mu    9.746
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_correction_T_min  0.188
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_process_details   'CrystalClear, Rigaku MSC, 2005'
_exptl_special_details           
;
?
;
_diffrn_ambient_temperature      160(2)
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_type           CuK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Rigaku R-AXIS SPIDER IPDS'
_diffrn_measurement_method       '\q scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            20852
_diffrn_reflns_av_R_equivalents  0.0753
_diffrn_reflns_av_unetI/netI     0.0801
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         6.89
_diffrn_reflns_theta_max         60.98
_reflns_number_total             4114
_reflns_number_gt                2566
_reflns_threshold_expression     >2sigma(I)
_computing_data_collection       'CrystalClear, Rigaku MSC, 2005'
_computing_cell_refinement       'CrystalClear, Rigaku MSC, 2005'
_computing_data_reduction        'CrystalClear, Rigaku MSC, 2005'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'DIAMOND (Brandenburg, 2012)'
_computing_publication_material  'WinGX (Farrugia, 1999)'
_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^)+(0.1120P)^2^+1.8587P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         4114
_refine_ls_number_parameters     411
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1105
_refine_ls_R_factor_gt           0.0736
_refine_ls_wR_factor_ref         0.2201
_refine_ls_wR_factor_gt          0.1857
_refine_ls_goodness_of_fit_ref   1.081
_refine_ls_restrained_S_all      1.081
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
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 0.13832(9) 0.07137(6) 0.12215(7) 0.0469(4) Uani 1 1 d . . .
Co2 Co -0.10040(9) 0.04116(6) 0.05022(7) 0.0438(4) Uani 1 1 d . . .
O61 O 0.0454(4) -0.0179(3) 0.0942(4) 0.0444(13) Uani 1 1 d . . .
N1 N -0.2176(5) 0.1322(3) 0.0328(4) 0.0527(15) Uani 1 1 d . . .
N2 N -0.1867(5) 0.0371(3) 0.1819(4) 0.0499(15) Uani 1 1 d . . .
C1 C -0.2279(7) 0.1796(4) -0.0415(6) 0.070(2) Uani 1 1 d . . .
H1 H -0.1823 0.1700 -0.0957 0.091 Uiso 1 1 calc R . .
C2 C -0.2995(9) 0.2419(5) -0.0465(9) 0.088(3) Uani 1 1 d . . .
H2 H -0.3041 0.2740 -0.1023 0.114 Uiso 1 1 calc R . .
C3 C -0.3646(9) 0.2562(5) 0.0323(10) 0.102(4) Uani 1 1 d . . .
H3 H -0.4134 0.3000 0.0323 0.133 Uiso 1 1 calc R . .
C4 C -0.3595(7) 0.2078(5) 0.1106(8) 0.081(3) Uani 1 1 d . . .
H4 H -0.4052 0.2171 0.1648 0.105 Uiso 1 1 calc R . .
C5 C -0.2851(6) 0.1435(4) 0.1097(6) 0.059(2) Uani 1 1 d . . .
C6 C -0.2742(6) 0.0877(4) 0.1895(5) 0.0514(18) Uani 1 1 d . . .
C7 C -0.3441(6) 0.0866(5) 0.2671(6) 0.068(2) Uani 1 1 d . . .
H7 H -0.4023 0.1241 0.2715 0.088 Uiso 1 1 calc R . .
C8 C -0.3295(7) 0.0311(6) 0.3387(6) 0.072(2) Uani 1 1 d . . .
H8 H -0.3779 0.0291 0.3922 0.093 Uiso 1 1 calc R . .
C9 C -0.2424(8) -0.0215(5) 0.3303(5) 0.066(2) Uani 1 1 d . . .
H9 H -0.2298 -0.0604 0.3783 0.086 Uiso 1 1 calc R . .
C10 C -0.1742(7) -0.0165(4) 0.2510(5) 0.061(2) Uani 1 1 d . . .
H10 H -0.1153 -0.0533 0.2456 0.080 Uiso 1 1 calc R . .
N11 N 0.0896(5) 0.0848(3) 0.2542(4) 0.0505(15) Uani 1 1 d . . .
N12 N 0.2542(6) 0.0100(3) 0.1844(5) 0.0574(17) Uani 1 1 d . . .
C11 C 0.0044(7) 0.1295(4) 0.2827(5) 0.060(2) Uani 1 1 d . . .
H11 H -0.0381 0.1580 0.2365 0.078 Uiso 1 1 calc R . .
C12 C -0.0218(9) 0.1341(4) 0.3791(6) 0.076(3) Uani 1 1 d . . .
H12 H -0.0799 0.1682 0.3985 0.099 Uiso 1 1 calc R . .
C13 C 0.0320(11) 0.0920(5) 0.4459(6) 0.097(4) Uani 1 1 d . . .
H13 H 0.0116 0.0948 0.5117 0.126 Uiso 1 1 calc R . .
C14 C 0.1168(10) 0.0451(5) 0.4175(6) 0.091(4) Uani 1 1 d . . .
H14 H 0.1559 0.0139 0.4633 0.118 Uiso 1 1 calc R . .
C15 C 0.1457(8) 0.0432(4) 0.3211(6) 0.064(2) Uani 1 1 d . . .
C16 C 0.2435(8) 0.0020(4) 0.2826(6) 0.069(3) Uani 1 1 d . . .
C17 C 0.3204(12) -0.0387(5) 0.3378(9) 0.103(4) Uani 1 1 d . . .
H17 H 0.3128 -0.0431 0.4056 0.134 Uiso 1 1 calc R . .
C18 C 0.4065(12) -0.0721(6) 0.2920(12) 0.114(5) Uani 1 1 d . . .
H18 H 0.4612 -0.0993 0.3288 0.149 Uiso 1 1 calc R . .
C19 C 0.4181(9) -0.0679(5) 0.1918(11) 0.104(4) Uani 1 1 d . . .
H19 H 0.4768 -0.0938 0.1595 0.135 Uiso 1 1 calc R . .
C20 C 0.3391(8) -0.0237(5) 0.1424(8) 0.076(3) Uani 1 1 d . . .
H20 H 0.3468 -0.0175 0.0748 0.099 Uiso 1 1 calc R . .
N31 N 0.2219(5) 0.1712(3) 0.1150(4) 0.0588(17) Uani 1 1 d . . .
O31 O 0.0166(4) 0.1272(2) 0.0761(3) 0.0478(12) Uani 1 1 d . . .
O32 O 0.1934(4) 0.0496(3) -0.0013(3) 0.0543(13) Uani 1 1 d . . .
O33 O 0.3986(11) 0.2874(5) 0.2869(8) 0.220(7) Uani 1 1 d . . .
H33O H 0.4568 0.2606 0.2930 0.286 Uiso 1 1 calc R . .
C31 C 0.0450(7) 0.1997(4) 0.0343(5) 0.064(2) Uani 1 1 d . . .
H31A H -0.0197 0.2356 0.0347 0.083 Uiso 1 1 calc R . .
H31B H 0.0681 0.1919 -0.0333 0.083 Uiso 1 1 calc R . .
C32 C 0.1386(7) 0.2337(4) 0.0924(6) 0.062(2) Uani 1 1 d . . .
H32A H 0.1744 0.2765 0.0557 0.081 Uiso 1 1 calc R . .
H32B H 0.1097 0.2561 0.1530 0.081 Uiso 1 1 calc R . .
C33 C 0.2523(8) 0.1115(4) -0.0446(6) 0.088(3) Uani 1 1 d . . .
H33A H 0.2015 0.1436 -0.0850 0.114 Uiso 1 1 calc R . .
H33B H 0.3116 0.0903 -0.0861 0.114 Uiso 1 1 calc R . .
C34 C 0.3013(8) 0.1600(5) 0.0337(8) 0.097(3) Uani 1 1 d . . .
H34A H 0.3223 0.2119 0.0074 0.126 Uiso 1 1 calc R . .
H34B H 0.3697 0.1344 0.0584 0.126 Uiso 1 1 calc R . .
C35 C 0.2809(9) 0.1957(4) 0.2068(7) 0.089(3) Uani 1 1 d . . .
H35A H 0.3309 0.1525 0.2270 0.116 Uiso 1 1 calc R . .
H35B H 0.2247 0.2022 0.2577 0.116 Uiso 1 1 calc R . .
C36 C 0.3485(8) 0.2704(4) 0.2011(8) 0.089(3) Uani 1 1 d . . .
H36A H 0.4058 0.2645 0.1510 0.116 Uiso 1 1 calc R . .
H36B H 0.2993 0.3144 0.1821 0.116 Uiso 1 1 calc R . .
N41 N -0.0881(7) 0.1702(5) -0.2841(6) 0.073(2) Uani 1 1 d . . .
O41 O -0.1538(7) 0.2238(4) -0.2727(5) 0.116(3) Uani 1 1 d . . .
O42 O -0.0304(6) 0.1508(4) -0.2109(6) 0.114(3) Uani 1 1 d . . .
O43 O -0.0803(10) 0.1354(5) -0.3568(6) 0.193(5) Uani 1 1 d . . .
N51 N 0.4052(9) 0.1342(6) 0.4455(7) 0.087(3) Uani 1 1 d . . .
O51 O 0.4641(5) 0.1570(5) 0.3871(5) 0.113(3) Uani 1 1 d . . .
O52 O 0.3147(8) 0.1422(5) 0.4639(7) 0.142(4) Uani 1 1 d . . .
O53 O 0.4565(8) 0.0867(5) 0.5069(6) 0.144(3) Uani 1 1 d . . .
H61O H 0.051(6) -0.048(4) 0.124(5) 0.05(3) 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
Co1 0.0735(9) 0.0260(6) 0.0409(7) 0.0012(5) -0.0053(6) -0.0043(5)
Co2 0.0699(8) 0.0275(6) 0.0340(7) 0.0011(4) 0.0045(6) 0.0057(5)
O61 0.073(4) 0.027(3) 0.033(3) 0.004(2) -0.002(2) -0.003(2)
N1 0.069(4) 0.038(3) 0.051(4) -0.004(3) -0.013(3) 0.001(3)
N2 0.070(4) 0.039(3) 0.041(3) -0.001(3) 0.006(3) 0.005(3)
C1 0.090(6) 0.039(4) 0.080(6) 0.015(4) -0.013(5) 0.004(4)
C2 0.104(8) 0.039(5) 0.119(9) 0.001(5) -0.048(7) 0.011(5)
C3 0.097(8) 0.038(5) 0.171(12) -0.013(7) -0.056(8) 0.022(5)
C4 0.076(6) 0.053(6) 0.113(8) -0.031(5) -0.023(6) 0.021(5)
C5 0.063(5) 0.048(5) 0.065(5) -0.025(4) -0.016(4) 0.006(4)
C6 0.057(5) 0.042(4) 0.056(5) -0.017(4) 0.006(4) 0.003(4)
C7 0.056(5) 0.073(6) 0.075(6) -0.029(5) 0.012(5) -0.012(4)
C8 0.073(6) 0.076(6) 0.065(6) -0.021(5) 0.012(5) -0.019(5)
C9 0.098(7) 0.059(5) 0.041(5) -0.010(4) 0.012(4) -0.027(5)
C10 0.096(6) 0.045(4) 0.044(5) -0.001(4) 0.017(4) 0.002(4)
N11 0.085(5) 0.030(3) 0.036(3) 0.004(3) -0.008(3) -0.011(3)
N12 0.074(5) 0.028(3) 0.070(5) 0.004(3) -0.022(4) -0.006(3)
C11 0.099(6) 0.028(4) 0.052(5) -0.009(3) 0.009(4) -0.009(4)
C12 0.148(9) 0.035(4) 0.044(5) -0.010(4) 0.013(5) -0.018(5)
C13 0.211(13) 0.038(5) 0.043(5) -0.016(4) 0.015(7) -0.031(7)
C14 0.193(12) 0.045(5) 0.034(5) 0.010(4) -0.020(6) -0.022(6)
C15 0.113(7) 0.025(4) 0.052(5) 0.000(4) -0.019(5) -0.010(4)
C16 0.099(7) 0.040(5) 0.066(6) 0.009(4) -0.043(5) -0.016(5)
C17 0.154(11) 0.038(6) 0.115(9) 0.009(6) -0.070(9) -0.016(6)
C18 0.132(11) 0.054(7) 0.155(13) 0.015(8) -0.087(10) -0.020(7)
C19 0.075(7) 0.055(6) 0.180(13) -0.002(7) -0.036(8) -0.012(5)
C20 0.067(6) 0.042(5) 0.120(8) 0.004(5) -0.018(6) -0.015(5)
N31 0.083(5) 0.030(3) 0.063(4) 0.003(3) -0.003(4) -0.001(3)
O31 0.071(3) 0.028(2) 0.045(3) 0.004(2) 0.000(2) 0.004(2)
O32 0.077(3) 0.035(3) 0.051(3) 0.002(2) 0.015(3) -0.006(2)
O33 0.310(14) 0.098(6) 0.249(11) 0.068(7) -0.198(11) -0.127(8)
C31 0.101(7) 0.034(4) 0.057(5) 0.014(4) -0.003(5) -0.004(4)
C32 0.087(6) 0.031(4) 0.069(5) -0.001(4) 0.006(5) -0.009(4)
C33 0.135(8) 0.031(4) 0.100(7) -0.012(5) 0.071(6) -0.022(5)
C34 0.098(7) 0.052(6) 0.142(9) -0.023(6) 0.049(7) -0.022(5)
C35 0.127(8) 0.040(5) 0.099(7) 0.004(5) -0.041(6) -0.031(5)
C36 0.105(7) 0.033(4) 0.128(8) 0.000(5) -0.038(6) -0.015(5)
N41 0.103(6) 0.053(5) 0.062(5) 0.008(4) 0.005(5) -0.019(4)
O41 0.157(7) 0.064(4) 0.127(6) -0.009(4) -0.050(5) 0.037(5)
O42 0.127(6) 0.097(5) 0.119(6) 0.064(5) 0.012(5) 0.025(4)
O43 0.311(13) 0.143(8) 0.126(7) -0.097(6) 0.096(8) -0.112(8)
N51 0.099(8) 0.104(7) 0.059(6) -0.029(5) 0.003(6) -0.024(6)
O51 0.070(4) 0.185(8) 0.082(5) -0.001(5) 0.014(4) 0.014(5)
O52 0.121(7) 0.098(6) 0.210(10) -0.059(6) 0.081(7) -0.011(5)
O53 0.170(9) 0.146(8) 0.114(7) 0.007(6) -0.042(6) -0.065(7)
_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
Co1 O31 1.856(4) . ?
Co1 O32 1.881(5) . ?
Co1 O61 1.926(5) . ?
Co1 N12 1.940(6) . ?
Co1 N11 1.944(6) . ?
Co1 N31 1.980(6) . ?
Co2 O32 2.023(5) 3 ?
Co2 O31 2.063(4) . ?
Co2 O61 2.108(6) . ?
Co2 N1 2.109(6) . ?
Co2 N2 2.113(6) . ?
Co2 O61 2.155(5) 3 ?
O61 Co2 2.155(5) 3 ?
O61 H61O 0.65(7) . ?
N1 C1 1.315(9) . ?
N1 C5 1.363(9) . ?
N2 C10 1.333(8) . ?
N2 C6 1.367(8) . ?
C1 C2 1.369(11) . ?
C1 H1 0.9500 . ?
C2 C3 1.374(14) . ?
C2 H2 0.9500 . ?
C3 C4 1.365(13) . ?
C3 H3 0.9500 . ?
C4 C5 1.416(10) . ?
C4 H4 0.9500 . ?
C5 C6 1.466(10) . ?
C6 C7 1.373(10) . ?
C7 C8 1.382(12) . ?
C7 H7 0.9500 . ?
C8 C9 1.386(11) . ?
C8 H8 0.9500 . ?
C9 C10 1.383(10) . ?
C9 H9 0.9500 . ?
C10 H10 0.9500 . ?
N11 C11 1.341(9) . ?
N11 C15 1.344(9) . ?
N12 C20 1.314(10) . ?
N12 C16 1.376(10) . ?
C11 C12 1.381(10) . ?
C11 H11 0.9500 . ?
C12 C13 1.335(12) . ?
C12 H12 0.9500 . ?
C13 C14 1.358(14) . ?
C13 H13 0.9500 . ?
C14 C15 1.387(11) . ?
C14 H14 0.9500 . ?
C15 C16 1.476(12) . ?
C16 C17 1.383(12) . ?
C17 C18 1.348(16) . ?
C17 H17 0.9500 . ?
C18 C19 1.400(16) . ?
C18 H18 0.9500 . ?
C19 C20 1.389(13) . ?
C19 H19 0.9500 . ?
C20 H20 0.9500 . ?
N31 C32 1.494(9) . ?
N31 C34 1.499(10) . ?
N31 C35 1.511(10) . ?
O31 C31 1.408(7) . ?
O32 C33 1.409(8) . ?
O32 Co2 2.023(5) 3 ?
O33 C36 1.362(10) . ?
O33 H33O 0.8400 . ?
C31 C32 1.497(10) . ?
C31 H31A 0.9900 . ?
C31 H31B 0.9900 . ?
C32 H32A 0.9900 . ?
C32 H32B 0.9900 . ?
C33 C34 1.484(12) . ?
C33 H33A 0.9900 . ?
C33 H33B 0.9900 . ?
C34 H34A 0.9900 . ?
C34 H34B 0.9900 . ?
C35 C36 1.514(10) . ?
C35 H35A 0.9900 . ?
C35 H35B 0.9900 . ?
C36 H36A 0.9900 . ?
C36 H36B 0.9900 . ?
N41 O43 1.175(8) . ?
N41 O41 1.219(9) . ?
N41 O42 1.269(9) . ?
N51 O52 1.129(10) . ?
N51 O51 1.150(9) . ?
N51 O53 1.324(11) . ?
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
O31 Co1 O32 94.1(2) . . ?
O31 Co1 O61 83.2(2) . . ?
O32 Co1 O61 82.5(2) . . ?
O31 Co1 N12 172.8(3) . . ?
O32 Co1 N12 92.3(3) . . ?
O61 Co1 N12 94.5(2) . . ?
O31 Co1 N11 91.1(2) . . ?
O32 Co1 N11 174.3(2) . . ?
O61 Co1 N11 95.9(2) . . ?
N12 Co1 N11 82.3(3) . . ?
O31 Co1 N31 86.7(2) . . ?
O32 Co1 N31 86.6(2) . . ?
O61 Co1 N31 164.5(2) . . ?
N12 Co1 N31 97.0(2) . . ?
N11 Co1 N31 96.0(2) . . ?
O32 Co2 O31 167.66(18) 3 . ?
O32 Co2 O61 100.86(19) 3 . ?
O31 Co2 O61 74.01(18) . . ?
O32 Co2 N1 99.0(2) 3 . ?
O31 Co2 N1 87.2(2) . . ?
O61 Co2 N1 159.8(2) . . ?
O32 Co2 N2 89.4(2) 3 . ?
O31 Co2 N2 102.4(2) . . ?
O61 Co2 N2 98.6(2) . . ?
N1 Co2 N2 77.8(2) . . ?
O32 Co2 O61 73.82(19) 3 3 ?
O31 Co2 O61 94.39(18) . 3 ?
O61 Co2 O61 85.3(2) . 3 ?
N1 Co2 O61 103.9(2) . 3 ?
N2 Co2 O61 163.2(2) . 3 ?
Co1 O61 Co2 99.3(2) . . ?
Co1 O61 Co2 98.6(2) . 3 ?
Co2 O61 Co2 94.7(2) . 3 ?
Co1 O61 H61O 115(7) . . ?
Co2 O61 H61O 129(7) . . ?
Co2 O61 H61O 114(7) 3 . ?
C1 N1 C5 118.3(7) . . ?
C1 N1 Co2 126.9(6) . . ?
C5 N1 Co2 114.7(5) . . ?
C10 N2 C6 117.2(6) . . ?
C10 N2 Co2 126.4(5) . . ?
C6 N2 Co2 115.6(5) . . ?
N1 C1 C2 124.8(9) . . ?
N1 C1 H1 117.6 . . ?
C2 C1 H1 117.6 . . ?
C1 C2 C3 117.5(10) . . ?
C1 C2 H2 121.2 . . ?
C3 C2 H2 121.2 . . ?
C4 C3 C2 120.3(9) . . ?
C4 C3 H3 119.8 . . ?
C2 C3 H3 119.8 . . ?
C3 C4 C5 118.9(10) . . ?
C3 C4 H4 120.5 . . ?
C5 C4 H4 120.5 . . ?
N1 C5 C4 120.0(8) . . ?
N1 C5 C6 116.8(6) . . ?
C4 C5 C6 123.2(8) . . ?
N2 C6 C7 122.1(8) . . ?
N2 C6 C5 114.5(6) . . ?
C7 C6 C5 123.4(8) . . ?
C6 C7 C8 119.9(8) . . ?
C6 C7 H7 120.1 . . ?
C8 C7 H7 120.1 . . ?
C7 C8 C9 118.3(8) . . ?
C7 C8 H8 120.9 . . ?
C9 C8 H8 120.9 . . ?
C10 C9 C8 118.9(8) . . ?
C10 C9 H9 120.6 . . ?
C8 C9 H9 120.6 . . ?
N2 C10 C9 123.5(8) . . ?
N2 C10 H10 118.2 . . ?
C9 C10 H10 118.2 . . ?
C11 N11 C15 118.4(7) . . ?
C11 N11 Co1 125.8(5) . . ?
C15 N11 Co1 115.8(6) . . ?
C20 N12 C16 118.5(8) . . ?
C20 N12 Co1 126.7(6) . . ?
C16 N12 Co1 114.8(6) . . ?
N11 C11 C12 120.1(8) . . ?
N11 C11 H11 119.9 . . ?
C12 C11 H11 119.9 . . ?
C13 C12 C11 121.9(9) . . ?
C13 C12 H12 119.0 . . ?
C11 C12 H12 119.0 . . ?
C12 C13 C14 118.4(9) . . ?
C12 C13 H13 120.8 . . ?
C14 C13 H13 120.8 . . ?
C13 C14 C15 119.4(9) . . ?
C13 C14 H14 120.3 . . ?
C15 C14 H14 120.3 . . ?
N11 C15 C14 121.7(9) . . ?
N11 C15 C16 113.4(7) . . ?
C14 C15 C16 124.7(8) . . ?
N12 C16 C17 122.0(11) . . ?
N12 C16 C15 113.3(7) . . ?
C17 C16 C15 124.7(10) . . ?
C18 C17 C16 117.6(12) . . ?
C18 C17 H17 121.2 . . ?
C16 C17 H17 121.2 . . ?
C17 C18 C19 122.2(12) . . ?
C17 C18 H18 118.9 . . ?
C19 C18 H18 118.9 . . ?
C20 C19 C18 116.3(12) . . ?
C20 C19 H19 121.9 . . ?
C18 C19 H19 121.9 . . ?
N12 C20 C19 123.4(11) . . ?
N12 C20 H20 118.3 . . ?
C19 C20 H20 118.3 . . ?
C32 N31 C34 111.4(6) . . ?
C32 N31 C35 106.8(6) . . ?
C34 N31 C35 111.8(7) . . ?
C32 N31 Co1 106.5(4) . . ?
C34 N31 Co1 104.9(4) . . ?
C35 N31 Co1 115.4(5) . . ?
C31 O31 Co1 113.4(5) . . ?
C31 O31 Co2 136.1(4) . . ?
Co1 O31 Co2 103.32(19) . . ?
C33 O32 Co1 115.1(4) . . ?
C33 O32 Co2 135.1(5) . 3 ?
Co1 O32 Co2 104.9(2) . 3 ?
C36 O33 H33O 109.5 . . ?
O31 C31 C32 107.6(6) . . ?
O31 C31 H31A 110.2 . . ?
C32 C31 H31A 110.2 . . ?
O31 C31 H31B 110.2 . . ?
C32 C31 H31B 110.2 . . ?
H31A C31 H31B 108.5 . . ?
N31 C32 C31 109.7(6) . . ?
N31 C32 H32A 109.7 . . ?
C31 C32 H32A 109.7 . . ?
N31 C32 H32B 109.7 . . ?
C31 C32 H32B 109.7 . . ?
H32A C32 H32B 108.2 . . ?
O32 C33 C34 107.6(7) . . ?
O32 C33 H33A 110.2 . . ?
C34 C33 H33A 110.2 . . ?
O32 C33 H33B 110.2 . . ?
C34 C33 H33B 110.2 . . ?
H33A C33 H33B 108.5 . . ?
C33 C34 N31 111.7(7) . . ?
C33 C34 H34A 109.3 . . ?
N31 C34 H34A 109.3 . . ?
C33 C34 H34B 109.3 . . ?
N31 C34 H34B 109.3 . . ?
H34A C34 H34B 107.9 . . ?
N31 C35 C36 115.9(7) . . ?
N31 C35 H35A 108.3 . . ?
C36 C35 H35A 108.3 . . ?
N31 C35 H35B 108.3 . . ?
C36 C35 H35B 108.3 . . ?
H35A C35 H35B 107.4 . . ?
O33 C36 C35 111.6(8) . . ?
O33 C36 H36A 109.3 . . ?
C35 C36 H36A 109.3 . . ?
O33 C36 H36B 109.3 . . ?
C35 C36 H36B 109.3 . . ?
H36A C36 H36B 108.0 . . ?
O43 N41 O41 123.2(11) . . ?
O43 N41 O42 120.5(11) . . ?
O41 N41 O42 116.2(8) . . ?
O52 N51 O51 136.2(13) . . ?
O52 N51 O53 111.9(11) . . ?
O51 N51 O53 111.9(11) . . ?
_diffrn_measured_fraction_theta_max 0.946
_diffrn_reflns_theta_full        60.98
_diffrn_measured_fraction_theta_full 0.946
_refine_diff_density_max         1.076
_refine_diff_density_min         -0.714
_refine_diff_density_rms         0.086


data_compound3
_database_code_depnum_ccdc_archive 'CCDC 905825'
#TrackingRef 'CCDC 905823-905825.cif'
_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C66 H74 Co4 N16 O22'
_chemical_formula_weight         1679.13
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'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   P2(1)/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                   11.3408(2)
_cell_length_b                   26.0914(4)
_cell_length_c                   13.6498(2)
_cell_angle_alpha                90.00
_cell_angle_beta                 116.3050(10)
_cell_angle_gamma                90.00
_cell_volume                     3620.70(10)
_cell_formula_units_Z            2
_cell_measurement_temperature    160(2)
_cell_measurement_reflns_used    39487
_cell_measurement_theta_min      6.58
_cell_measurement_theta_max      71.97
_exptl_crystal_description       parallelepiped
_exptl_crystal_colour            red
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.08
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.540
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1732
_exptl_absorpt_coefficient_mu    7.791
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.476
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_process_details   'CrystalClear, Rigaku MSC, 2005'
_exptl_special_details           
;
?
;
_diffrn_ambient_temperature      160(2)
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_type           CuK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Rigaku R-AXIS SPIDER IPDS'
_diffrn_measurement_method       '\q scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            42679
_diffrn_reflns_av_R_equivalents  0.0438
_diffrn_reflns_av_unetI/netI     0.0330
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         6.59
_diffrn_reflns_theta_max         65.00
_reflns_number_total             6020
_reflns_number_gt                5445
_reflns_threshold_expression     >2sigma(I)
_computing_data_collection       'CrystalClear, Rigaku MSC, 2005'
_computing_cell_refinement       'CrystalClear, Rigaku MSC, 2005'
_computing_data_reduction        'CrystalClear, Rigaku MSC, 2005'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'DIAMOND (Brandenburg, 2012)'
_computing_publication_material  'WinGX (Farrugia, 1999)'
_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^)+(0.0827P)^2^+2.7225P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         6020
_refine_ls_number_parameters     562
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0514
_refine_ls_R_factor_gt           0.0470
_refine_ls_wR_factor_ref         0.1332
_refine_ls_wR_factor_gt          0.1296
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_restrained_S_all      1.052
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
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 0.22972(5) 0.962473(16) 0.14584(3) 0.01761(15) Uani 1 1 d . . .
Co2 Co 0.00718(5) 1.043344(16) 0.08306(3) 0.01841(15) Uani 1 1 d . . .
O61 O 0.0400(2) 0.96058(7) 0.08585(16) 0.0208(5) Uani 1 1 d . . .
N1 N 0.2576(3) 0.95281(9) 0.2965(2) 0.0210(5) Uani 1 1 d . . .
N2 N 0.2553(2) 0.88850(9) 0.15090(18) 0.0218(5) Uani 1 1 d . . .
C1 C 0.2587(3) 0.98759(12) 0.3684(2) 0.0240(7) Uani 1 1 d . . .
H1 H 0.2475 1.0227 0.3481 0.031 Uiso 1 1 calc R . .
C2 C 0.2760(3) 0.97373(13) 0.4731(2) 0.0287(7) Uani 1 1 d . . .
H2 H 0.2760 0.9994 0.5224 0.037 Uiso 1 1 calc R . .
C3 C 0.2929(3) 0.92365(13) 0.5048(2) 0.0313(8) Uani 1 1 d . . .
H3 H 0.3059 0.9144 0.5762 0.041 Uiso 1 1 calc R . .
C4 C 0.2910(3) 0.88558(12) 0.4302(2) 0.0289(7) Uani 1 1 d . . .
C5 C 0.3073(4) 0.83167(13) 0.4521(3) 0.0379(9) Uani 1 1 d . . .
H5 H 0.3182 0.8192 0.5210 0.049 Uiso 1 1 calc R . .
C6 C 0.3073(4) 0.79819(13) 0.3765(3) 0.0375(8) Uani 1 1 d . . .
H6 H 0.3190 0.7627 0.3936 0.049 Uiso 1 1 calc R . .
C7 C 0.2902(3) 0.81514(12) 0.2709(2) 0.0294(7) Uani 1 1 d . . .
C8 C 0.2927(4) 0.78283(12) 0.1892(3) 0.0340(8) Uani 1 1 d . . .
H8 H 0.3047 0.7469 0.2005 0.044 Uiso 1 1 calc R . .
C9 C 0.2775(4) 0.80460(12) 0.0926(3) 0.0346(8) Uani 1 1 d . . .
H9 H 0.2787 0.7834 0.0365 0.045 Uiso 1 1 calc R . .
C10 C 0.2601(3) 0.85744(12) 0.0755(2) 0.0260(7) Uani 1 1 d . . .
H10 H 0.2516 0.8715 0.0084 0.034 Uiso 1 1 calc R . .
C11 C 0.2719(3) 0.86726(11) 0.2477(2) 0.0224(6) Uani 1 1 d . . .
C12 C 0.2733(3) 0.90268(11) 0.3275(2) 0.0223(6) Uani 1 1 d . . .
N21 N 0.0320(3) 1.12434(10) 0.09755(19) 0.0234(6) Uani 1 1 d . . .
N22 N -0.0187(3) 1.05927(10) 0.22582(19) 0.0239(6) Uani 1 1 d . . .
C21 C 0.0629(3) 1.15621(12) 0.0358(2) 0.0304(7) Uani 1 1 d . . .
H21 H 0.0763 1.1423 -0.0228 0.040 Uiso 1 1 calc R . .
C22 C 0.0762(4) 1.20887(13) 0.0535(3) 0.0380(8) Uani 1 1 d . . .
H22 H 0.1002 1.2300 0.0086 0.049 Uiso 1 1 calc R . .
C23 C 0.0547(4) 1.23008(13) 0.1359(3) 0.0402(9) Uani 1 1 d . . .
H23 H 0.0607 1.2661 0.1472 0.052 Uiso 1 1 calc R . .
C24 C 0.0236(4) 1.19765(12) 0.2042(3) 0.0333(8) Uani 1 1 d . . .
C25 C 0.0022(4) 1.21577(14) 0.2938(3) 0.0435(9) Uani 1 1 d . . .
H25 H 0.0051 1.2515 0.3079 0.057 Uiso 1 1 calc R . .
C26 C -0.0218(4) 1.18269(14) 0.3583(3) 0.0442(10) Uani 1 1 d . . .
H26 H -0.0350 1.1957 0.4176 0.057 Uiso 1 1 calc R . .
C27 C -0.0281(3) 1.12848(13) 0.3404(2) 0.0319(8) Uani 1 1 d . . .
C28 C -0.0530(3) 1.09279(14) 0.4056(2) 0.0346(8) Uani 1 1 d . . .
H28 H -0.0626 1.1038 0.4680 0.045 Uiso 1 1 calc R . .
C29 C -0.0633(4) 1.04222(13) 0.3786(3) 0.0316(8) Uani 1 1 d . . .
H29 H -0.0824 1.0177 0.4210 0.041 Uiso 1 1 calc R . .
C30 C -0.0455(3) 1.02660(13) 0.2877(2) 0.0271(7) Uani 1 1 d . . .
H30 H -0.0528 0.9912 0.2697 0.035 Uiso 1 1 calc R . .
C31 C -0.0117(3) 1.10974(11) 0.2503(2) 0.0234(7) Uani 1 1 d . . .
C32 C 0.0155(3) 1.14474(11) 0.1817(2) 0.0247(7) Uani 1 1 d . . .
N41 N 0.4137(2) 0.98147(9) 0.18133(18) 0.0227(5) Uani 1 1 d . . .
O41 O 0.7508(3) 0.93420(11) 0.36255(18) 0.0361(6) Uani 1 1 d . . .
O42 O 0.2013(2) 1.03307(7) 0.15055(16) 0.0231(5) Uani 1 1 d . . .
O43 O 0.1959(2) 0.96216(7) -0.00020(16) 0.0225(5) Uani 1 1 d . . .
C41 C 0.5211(3) 0.94625(13) 0.2553(2) 0.0252(7) Uani 1 1 d . . .
C42 C 0.6581(3) 0.95932(14) 0.2678(3) 0.0310(8) Uani 1 1 d . . .
C43 C 0.4336(3) 1.03336(12) 0.2361(3) 0.0257(7) Uani 1 1 d . . .
C44 C 0.3117(3) 1.06542(12) 0.1772(3) 0.0266(7) Uani 1 1 d . . .
C45 C 0.4187(3) 0.98493(14) 0.0734(2) 0.0270(7) Uani 1 1 d . . .
C46 C 0.2842(3) 0.99525(13) -0.0178(2) 0.0276(7) Uani 1 1 d . . .
N51 N 0.9413(3) 0.87183(10) 0.2511(2) 0.0325(6) Uani 1 1 d . . .
O51 O 0.9985(3) 0.83853(10) 0.2246(2) 0.0530(7) Uani 1 1 d . . .
O52 O 0.9188(3) 0.86536(10) 0.3317(2) 0.0519(7) Uani 1 1 d . . .
O53 O 0.9051(3) 0.91170(9) 0.1957(2) 0.0514(7) Uani 1 1 d . . .
N52 N -0.3492(3) 1.13722(12) 0.1875(2) 0.0428(8) Uani 1 1 d . . .
O54 O -0.3499(3) 1.14754(12) 0.2762(2) 0.0642(9) Uani 1 1 d . . .
O55 O -0.3528(3) 1.09264(11) 0.1591(3) 0.0696(9) Uani 1 1 d . . .
O56 O -0.3393(5) 1.17181(12) 0.1305(3) 0.0876(13) Uani 1 1 d . . .
N61 N 0.6472(7) 0.8946(2) 0.5552(5) 0.125(2) Uani 1 1 d . . .
C61 C 0.6538(6) 0.8614(2) 0.5113(5) 0.0786(15) Uani 1 1 d . . .
C62 C 0.6709(7) 0.8245(2) 0.4368(6) 0.110(2) Uani 1 1 d . . .
H62A H 0.5904 0.8234 0.3677 0.165 Uiso 1 1 calc R . .
H62B H 0.6887 0.7904 0.4704 0.165 Uiso 1 1 calc R . .
H62C H 0.7448 0.8353 0.4228 0.165 Uiso 1 1 calc R . .
C1M C -0.6398(10) 1.1763(6) -0.0872(12) 0.150(6) Uani 0.60 1 d P . .
O1M O -0.5529(7) 1.1442(3) -0.0835(5) 0.106(2) Uani 0.60 1 d P . .
C2M C -0.5998(15) 1.2185(8) 0.2829(12) 0.105(6) Uani 0.40 1 d P . .
O2M O -0.5812(12) 1.2128(6) 0.1938(13) 0.149(5) Uani 0.40 1 d P . .
H61O H 0.001(4) 0.9365(18) 0.123(4) 0.069(13) Uiso 1 1 d . . .
H41O H 0.791(4) 0.9170(16) 0.343(3) 0.044(13) Uiso 1 1 d . . .
H41A H 0.521(3) 0.9487(12) 0.329(3) 0.031(9) Uiso 1 1 d . . .
H41B H 0.503(3) 0.9122(13) 0.230(3) 0.024(8) Uiso 1 1 d . . .
H42A H 0.683(4) 0.9987(15) 0.281(3) 0.040(10) Uiso 1 1 d . . .
H42B H 0.675(3) 0.9487(12) 0.208(3) 0.024(8) Uiso 1 1 d . . .
H43A H 0.506(3) 1.0479(11) 0.231(3) 0.019(8) Uiso 1 1 d . . .
H43B H 0.446(3) 1.0274(13) 0.313(3) 0.035(9) Uiso 1 1 d . . .
H44A H 0.313(3) 1.0903(13) 0.222(3) 0.028(9) Uiso 1 1 d . . .
H44B H 0.310(3) 1.0820(12) 0.109(3) 0.022(8) Uiso 1 1 d . . .
H45A H 0.482(3) 1.0098(12) 0.073(2) 0.020(8) Uiso 1 1 d . . .
H45B H 0.447(3) 0.9500(12) 0.062(2) 0.015(7) Uiso 1 1 d . . .
H46A H 0.293(3) 0.9885(13) -0.081(3) 0.030(9) Uiso 1 1 d . . .
H46B H 0.251(4) 1.0332(14) -0.023(3) 0.038(10) 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
Co1 0.0250(3) 0.0183(3) 0.0123(2) 0.00058(16) 0.0108(2) 0.00052(18)
Co2 0.0270(3) 0.0177(3) 0.0132(2) -0.00107(16) 0.0112(2) 0.00030(18)
O61 0.0296(13) 0.0182(11) 0.0183(10) 0.0009(7) 0.0141(9) -0.0001(8)
N1 0.0230(15) 0.0212(13) 0.0218(12) -0.0017(9) 0.0125(11) -0.0001(10)
N2 0.0284(15) 0.0234(13) 0.0175(11) -0.0001(9) 0.0136(11) 0.0016(10)
C1 0.0270(18) 0.0254(16) 0.0205(14) -0.0042(12) 0.0115(13) 0.0002(12)
C2 0.038(2) 0.0360(18) 0.0160(14) -0.0063(12) 0.0158(14) -0.0042(15)
C3 0.036(2) 0.043(2) 0.0181(14) 0.0022(13) 0.0151(14) -0.0003(15)
C4 0.039(2) 0.0335(18) 0.0189(14) 0.0034(12) 0.0173(14) -0.0019(14)
C5 0.056(2) 0.0347(19) 0.0284(16) 0.0124(14) 0.0238(16) 0.0039(17)
C6 0.058(2) 0.0249(17) 0.0332(17) 0.0103(14) 0.0234(17) 0.0038(16)
C7 0.036(2) 0.0257(17) 0.0274(16) 0.0036(12) 0.0151(14) 0.0044(14)
C8 0.049(2) 0.0197(16) 0.0361(17) 0.0019(13) 0.0214(16) 0.0051(15)
C9 0.046(2) 0.0269(17) 0.0335(17) -0.0091(14) 0.0203(16) 0.0032(15)
C10 0.0319(19) 0.0276(16) 0.0200(14) -0.0033(12) 0.0130(13) 0.0036(13)
C11 0.0300(18) 0.0235(15) 0.0184(13) 0.0017(11) 0.0151(13) 0.0012(12)
C12 0.0283(18) 0.0243(16) 0.0176(13) 0.0005(11) 0.0130(12) -0.0008(12)
N21 0.0277(15) 0.0242(13) 0.0196(12) -0.0011(10) 0.0117(11) 0.0007(11)
N22 0.0293(15) 0.0246(13) 0.0189(12) -0.0019(10) 0.0116(11) 0.0012(11)
C21 0.040(2) 0.0295(17) 0.0239(15) 0.0034(12) 0.0158(14) -0.0008(14)
C22 0.055(2) 0.0273(18) 0.0332(17) 0.0062(14) 0.0213(17) -0.0019(16)
C23 0.059(3) 0.0195(17) 0.0410(19) -0.0026(14) 0.0211(18) -0.0047(16)
C24 0.042(2) 0.0257(17) 0.0304(16) -0.0060(13) 0.0149(15) -0.0011(15)
C25 0.063(3) 0.0294(19) 0.043(2) -0.0149(15) 0.0279(19) -0.0016(17)
C26 0.061(3) 0.041(2) 0.039(2) -0.0212(16) 0.0308(19) -0.0076(18)
C27 0.035(2) 0.0384(19) 0.0252(15) -0.0095(13) 0.0163(15) -0.0028(15)
C28 0.037(2) 0.051(2) 0.0209(15) -0.0058(14) 0.0173(14) -0.0031(16)
C29 0.033(2) 0.045(2) 0.0194(15) 0.0048(13) 0.0142(15) -0.0001(15)
C30 0.0306(19) 0.0314(17) 0.0206(15) 0.0035(12) 0.0125(14) 0.0004(14)
C31 0.0238(17) 0.0277(16) 0.0186(14) -0.0043(11) 0.0092(12) -0.0001(13)
C32 0.0292(18) 0.0242(16) 0.0192(14) -0.0028(11) 0.0092(13) 0.0014(13)
N41 0.0274(15) 0.0260(13) 0.0175(11) 0.0002(10) 0.0123(11) -0.0006(11)
O41 0.0345(15) 0.0494(16) 0.0234(11) 0.0016(10) 0.0118(11) 0.0119(12)
O42 0.0295(13) 0.0202(11) 0.0226(11) -0.0007(8) 0.0143(10) -0.0014(9)
O43 0.0289(13) 0.0255(11) 0.0160(10) 0.0019(7) 0.0127(9) -0.0005(8)
C41 0.0247(18) 0.0301(18) 0.0192(15) 0.0015(12) 0.0084(13) 0.0013(14)
C42 0.026(2) 0.042(2) 0.0240(17) 0.0011(13) 0.0103(15) 0.0030(14)
C43 0.0248(19) 0.0254(16) 0.0276(17) -0.0034(12) 0.0122(14) -0.0036(13)
C44 0.0309(19) 0.0205(16) 0.0291(16) -0.0036(13) 0.0140(14) -0.0038(13)
C45 0.0304(19) 0.040(2) 0.0168(14) -0.0002(13) 0.0162(14) -0.0052(15)
C46 0.035(2) 0.0358(19) 0.0165(15) 0.0039(12) 0.0158(14) -0.0017(15)
N51 0.0438(18) 0.0289(15) 0.0310(14) 0.0006(11) 0.0222(13) 0.0028(13)
O51 0.077(2) 0.0426(15) 0.0555(16) 0.0051(12) 0.0436(16) 0.0202(14)
O52 0.080(2) 0.0550(17) 0.0400(14) 0.0128(12) 0.0441(15) 0.0187(15)
O53 0.080(2) 0.0320(14) 0.0588(16) 0.0133(12) 0.0457(16) 0.0102(13)
N52 0.060(2) 0.0339(17) 0.0413(17) 0.0010(13) 0.0284(16) -0.0041(15)
O54 0.096(3) 0.066(2) 0.0486(17) 0.0107(14) 0.0487(17) 0.0144(17)
O55 0.090(3) 0.0411(18) 0.091(2) -0.0134(16) 0.052(2) -0.0134(16)
O56 0.174(4) 0.0449(18) 0.0524(18) 0.0047(14) 0.058(2) -0.026(2)
N61 0.170(6) 0.094(4) 0.088(4) -0.050(3) 0.036(4) -0.020(4)
C61 0.078(4) 0.073(4) 0.074(3) -0.013(3) 0.024(3) -0.018(3)
C62 0.114(6) 0.075(4) 0.132(6) -0.002(4) 0.046(5) 0.005(4)
C1M 0.042(6) 0.183(13) 0.154(11) -0.100(10) -0.021(6) 0.008(7)
O1M 0.086(5) 0.152(7) 0.068(4) -0.043(4) 0.024(4) 0.015(5)
C2M 0.060(9) 0.193(19) 0.065(9) -0.018(10) 0.031(8) 0.005(10)
O2M 0.090(9) 0.148(12) 0.181(14) -0.009(11) 0.034(9) 0.030(8)
_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
Co1 O43 1.855(2) . ?
Co1 O42 1.876(2) . ?
Co1 O61 1.935(2) . ?
Co1 N2 1.948(2) . ?
Co1 N1 1.954(2) . ?
Co1 N41 1.985(3) . ?
Co2 O42 1.992(2) . ?
Co2 O43 2.072(2) 3_575 ?
Co2 O61 2.126(2) 3_575 ?
Co2 N21 2.130(3) . ?
Co2 N22 2.136(2) . ?
Co2 O61 2.1886(19) . ?
O61 Co2 2.126(2) 3_575 ?
O61 H61O 1.02(5) . ?
N1 C1 1.333(4) . ?
N1 C12 1.362(4) . ?
N2 C10 1.330(4) . ?
N2 C11 1.367(3) . ?
C1 C2 1.401(4) . ?
C1 H1 0.9500 . ?
C2 C3 1.363(5) . ?
C2 H2 0.9500 . ?
C3 C4 1.416(4) . ?
C3 H3 0.9500 . ?
C4 C12 1.398(4) . ?
C4 C5 1.433(4) . ?
C5 C6 1.352(5) . ?
C5 H5 0.9500 . ?
C6 C7 1.436(4) . ?
C6 H6 0.9500 . ?
C7 C11 1.391(4) . ?
C7 C8 1.409(4) . ?
C8 C9 1.374(5) . ?
C8 H8 0.9500 . ?
C9 C10 1.398(4) . ?
C9 H9 0.9500 . ?
C10 H10 0.9500 . ?
C11 C12 1.423(4) . ?
N21 C21 1.337(4) . ?
N21 C32 1.352(4) . ?
N22 C30 1.326(4) . ?
N22 C31 1.352(4) . ?
C21 C22 1.392(5) . ?
C21 H21 0.9500 . ?
C22 C23 1.369(5) . ?
C22 H22 0.9500 . ?
C23 C24 1.414(5) . ?
C23 H23 0.9500 . ?
C24 C32 1.408(4) . ?
C24 C25 1.428(5) . ?
C25 C26 1.344(5) . ?
C25 H25 0.9500 . ?
C26 C27 1.432(5) . ?
C26 H26 0.9500 . ?
C27 C28 1.401(5) . ?
C27 C31 1.410(4) . ?
C28 C29 1.361(5) . ?
C28 H28 0.9500 . ?
C29 C30 1.403(4) . ?
C29 H29 0.9500 . ?
C30 H30 0.9500 . ?
C31 C32 1.436(4) . ?
N41 C45 1.502(3) . ?
N41 C41 1.502(4) . ?
N41 C43 1.515(4) . ?
O41 C42 1.415(4) . ?
O41 H41O 0.76(4) . ?
O42 C44 1.417(4) . ?
O43 C46 1.421(4) . ?
O43 Co2 2.072(2) 3_575 ?
C41 C42 1.525(5) . ?
C41 H41A 1.01(4) . ?
C41 H41B 0.94(3) . ?
C42 H42A 1.06(4) . ?
C42 H42B 0.96(3) . ?
C43 C44 1.507(5) . ?
C43 H43A 0.93(3) . ?
C43 H43B 1.01(4) . ?
C44 H44A 0.89(3) . ?
C44 H44B 1.02(3) . ?
C45 C46 1.505(5) . ?
C45 H45A 0.96(3) . ?
C45 H45B 1.00(3) . ?
C46 H46A 0.94(3) . ?
C46 H46B 1.05(4) . ?
N51 O51 1.230(3) . ?
N51 O53 1.244(3) . ?
N51 O52 1.246(3) . ?
N52 O55 1.221(4) . ?
N52 O56 1.229(4) . ?
N52 O54 1.244(4) . ?
N61 C61 1.075(7) . ?
C61 C62 1.473(8) . ?
C62 H62A 0.9800 . ?
C62 H62B 0.9800 . ?
C62 H62C 0.9800 . ?
C1M O1M 1.276(13) . ?
C2M O2M 1.332(19) . ?
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
O43 Co1 O42 94.83(8) . . ?
O43 Co1 O61 83.30(9) . . ?
O42 Co1 O61 82.16(9) . . ?
O43 Co1 N2 89.45(9) . . ?
O42 Co1 N2 175.24(9) . . ?
O61 Co1 N2 96.31(9) . . ?
O43 Co1 N1 172.00(9) . . ?
O42 Co1 N1 92.34(9) . . ?
O61 Co1 N1 94.19(10) . . ?
N2 Co1 N1 83.27(9) . . ?
O43 Co1 N41 87.59(9) . . ?
O42 Co1 N41 85.67(10) . . ?
O61 Co1 N41 164.11(9) . . ?
N2 Co1 N41 96.60(11) . . ?
N1 Co1 N41 96.50(10) . . ?
O42 Co2 O43 167.41(8) . 3_575 ?
O42 Co2 O61 100.97(9) . 3_575 ?
O43 Co2 O61 73.75(8) 3_575 3_575 ?
O42 Co2 N21 90.98(9) . . ?
O43 Co2 N21 100.87(9) 3_575 . ?
O61 Co2 N21 96.20(8) 3_575 . ?
O42 Co2 N22 100.07(9) . . ?
O43 Co2 N22 86.71(9) 3_575 . ?
O61 Co2 N22 158.21(10) 3_575 . ?
N21 Co2 N22 77.78(9) . . ?
O42 Co2 O61 73.43(9) . . ?
O43 Co2 O61 94.60(8) 3_575 . ?
O61 Co2 O61 86.01(8) 3_575 . ?
N21 Co2 O61 164.38(10) . . ?
N22 Co2 O61 105.48(9) . . ?
Co1 O61 Co2 99.10(9) . 3_575 ?
Co1 O61 Co2 97.51(9) . . ?
Co2 O61 Co2 93.99(8) 3_575 . ?
Co1 O61 H61O 117(3) . . ?
Co2 O61 H61O 124(3) 3_575 . ?
Co2 O61 H61O 121(3) . . ?
C1 N1 C12 117.9(2) . . ?
C1 N1 Co1 129.2(2) . . ?
C12 N1 Co1 112.91(18) . . ?
C10 N2 C11 117.8(3) . . ?
C10 N2 Co1 129.2(2) . . ?
C11 N2 Co1 112.98(18) . . ?
N1 C1 C2 121.8(3) . . ?
N1 C1 H1 119.1 . . ?
C2 C1 H1 119.1 . . ?
C3 C2 C1 120.5(3) . . ?
C3 C2 H2 119.7 . . ?
C1 C2 H2 119.7 . . ?
C2 C3 C4 119.3(3) . . ?
C2 C3 H3 120.4 . . ?
C4 C3 H3 120.4 . . ?
C12 C4 C3 116.5(3) . . ?
C12 C4 C5 118.1(3) . . ?
C3 C4 C5 125.4(3) . . ?
C6 C5 C4 121.2(3) . . ?
C6 C5 H5 119.4 . . ?
C4 C5 H5 119.4 . . ?
C5 C6 C7 121.4(3) . . ?
C5 C6 H6 119.3 . . ?
C7 C6 H6 119.3 . . ?
C11 C7 C8 117.3(3) . . ?
C11 C7 C6 118.0(3) . . ?
C8 C7 C6 124.7(3) . . ?
C9 C8 C7 118.3(3) . . ?
C9 C8 H8 120.8 . . ?
C7 C8 H8 120.8 . . ?
C8 C9 C10 121.1(3) . . ?
C8 C9 H9 119.5 . . ?
C10 C9 H9 119.5 . . ?
N2 C10 C9 121.5(3) . . ?
N2 C10 H10 119.2 . . ?
C9 C10 H10 119.2 . . ?
N2 C11 C7 124.0(3) . . ?
N2 C11 C12 115.3(3) . . ?
C7 C11 C12 120.7(3) . . ?
N1 C12 C4 124.0(3) . . ?
N1 C12 C11 115.4(2) . . ?
C4 C12 C11 120.5(3) . . ?
C21 N21 C32 117.7(3) . . ?
C21 N21 Co2 128.3(2) . . ?
C32 N21 Co2 114.03(19) . . ?
C30 N22 C31 118.3(3) . . ?
C30 N22 Co2 128.2(2) . . ?
C31 N22 Co2 113.45(19) . . ?
N21 C21 C22 122.9(3) . . ?
N21 C21 H21 118.6 . . ?
C22 C21 H21 118.6 . . ?
C23 C22 C21 119.8(3) . . ?
C23 C22 H22 120.1 . . ?
C21 C22 H22 120.1 . . ?
C22 C23 C24 119.1(3) . . ?
C22 C23 H23 120.4 . . ?
C24 C23 H23 120.4 . . ?
C32 C24 C23 117.0(3) . . ?
C32 C24 C25 119.5(3) . . ?
C23 C24 C25 123.5(3) . . ?
C26 C25 C24 120.6(3) . . ?
C26 C25 H25 119.7 . . ?
C24 C25 H25 119.7 . . ?
C25 C26 C27 122.2(3) . . ?
C25 C26 H26 118.9 . . ?
C27 C26 H26 118.9 . . ?
C28 C27 C31 117.7(3) . . ?
C28 C27 C26 123.9(3) . . ?
C31 C27 C26 118.4(3) . . ?
C29 C28 C27 119.3(3) . . ?
C29 C28 H28 120.3 . . ?
C27 C28 H28 120.3 . . ?
C28 C29 C30 119.5(3) . . ?
C28 C29 H29 120.2 . . ?
C30 C29 H29 120.2 . . ?
N22 C30 C29 122.6(3) . . ?
N22 C30 H30 118.7 . . ?
C29 C30 H30 118.7 . . ?
N22 C31 C27 122.5(3) . . ?
N22 C31 C32 117.7(3) . . ?
C27 C31 C32 119.8(3) . . ?
N21 C32 C24 123.5(3) . . ?
N21 C32 C31 117.0(3) . . ?
C24 C32 C31 119.5(3) . . ?
C45 N41 C41 108.9(2) . . ?
C45 N41 C43 111.6(2) . . ?
C41 N41 C43 108.4(2) . . ?
C45 N41 Co1 105.57(18) . . ?
C41 N41 Co1 117.56(19) . . ?
C43 N41 Co1 104.70(19) . . ?
C42 O41 H41O 106(3) . . ?
C44 O42 Co1 116.61(19) . . ?
C44 O42 Co2 135.07(19) . . ?
Co1 O42 Co2 106.73(10) . . ?
C46 O43 Co1 110.67(17) . . ?
C46 O43 Co2 130.23(18) . 3_575 ?
Co1 O43 Co2 103.75(10) . 3_575 ?
N41 C41 C42 114.9(3) . . ?
N41 C41 H41A 105.7(19) . . ?
C42 C41 H41A 109(2) . . ?
N41 C41 H41B 110.3(19) . . ?
C42 C41 H41B 108(2) . . ?
H41A C41 H41B 109(3) . . ?
O41 C42 C41 107.8(3) . . ?
O41 C42 H42A 105(2) . . ?
C41 C42 H42A 115(2) . . ?
O41 C42 H42B 107.3(19) . . ?
C41 C42 H42B 115(2) . . ?
H42A C42 H42B 106(3) . . ?
C44 C43 N41 109.4(3) . . ?
C44 C43 H43A 111.4(19) . . ?
N41 C43 H43A 105.8(19) . . ?
C44 C43 H43B 108(2) . . ?
N41 C43 H43B 107(2) . . ?
H43A C43 H43B 115(3) . . ?
O42 C44 C43 107.7(3) . . ?
O42 C44 H44A 111(2) . . ?
C43 C44 H44A 108(2) . . ?
O42 C44 H44B 111.0(17) . . ?
C43 C44 H44B 111.5(18) . . ?
H44A C44 H44B 108(3) . . ?
N41 C45 C46 110.9(3) . . ?
N41 C45 H45A 112.9(18) . . ?
C46 C45 H45A 111.0(18) . . ?
N41 C45 H45B 104.4(17) . . ?
C46 C45 H45B 108.4(17) . . ?
H45A C45 H45B 109(3) . . ?
O43 C46 C45 106.5(2) . . ?
O43 C46 H46A 115(2) . . ?
C45 C46 H46A 104(2) . . ?
O43 C46 H46B 109(2) . . ?
C45 C46 H46B 115(2) . . ?
H46A C46 H46B 108(3) . . ?
O51 N51 O53 119.2(3) . . ?
O51 N51 O52 120.3(3) . . ?
O53 N51 O52 120.5(3) . . ?
O55 N52 O56 119.9(3) . . ?
O55 N52 O54 120.1(3) . . ?
O56 N52 O54 119.9(3) . . ?
N61 C61 C62 166.8(8) . . ?
C61 C62 H62A 109.5 . . ?
C61 C62 H62B 109.5 . . ?
H62A C62 H62B 109.5 . . ?
C61 C62 H62C 109.5 . . ?
H62A C62 H62C 109.5 . . ?
H62B C62 H62C 109.5 . . ?
_diffrn_measured_fraction_theta_max 0.976
_diffrn_reflns_theta_full        65.00
_diffrn_measured_fraction_theta_full 0.976
_refine_diff_density_max         0.662
_refine_diff_density_min         -0.594
_refine_diff_density_rms         0.079
#===END