# 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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#  fide research purposes only. It may contain copyright material 
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data_1
_database_code_depnum_ccdc_archive 'CCDC 917476'
_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C10 H14 Co3 N8 O8'
_chemical_formula_weight         551.08
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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'
Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_symmetry_cell_setting           Tetragonal
_symmetry_space_group_name_H-M   I4(1)/a
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-y+3/4, x+1/4, z+1/4'
'y+3/4, -x+3/4, z+3/4'
'x+1/2, y+1/2, z+1/2'
'-x+1, -y+1/2, z+1'
'-y+5/4, x+3/4, z+3/4'
'y+5/4, -x+5/4, z+5/4'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'y-3/4, -x-1/4, -z-1/4'
'-y-3/4, x-3/4, -z-3/4'
'-x+1/2, -y+1/2, -z+1/2'
'x, y+1/2, -z'
'y-1/4, -x+1/4, -z+1/4'
'-y-1/4, x-1/4, -z-1/4'
_cell_length_a                   20.7387(5)
_cell_length_b                   20.7387(5)
_cell_length_c                   8.4495(4)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     3634.1(2)
_cell_formula_units_Z            8
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    16302
_cell_measurement_theta_min      2.60
_cell_measurement_theta_max      28.25
_exptl_crystal_description       block
_exptl_crystal_colour            red
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.10
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.014
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2200
_exptl_absorpt_coefficient_mu    2.767
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.7324
_exptl_absorpt_correction_T_max  0.7693
_exptl_absorpt_process_details   'SADABS(Sheldrick, 1996)'
_exptl_special_details           
;
?
;
_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            16302
_diffrn_reflns_av_R_equivalents  0.0266
_diffrn_reflns_av_sigmaI/netI    0.0153
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_theta_min         2.60
_diffrn_reflns_theta_max         28.25
_reflns_number_total             2237
_reflns_number_gt                1995
_reflns_threshold_expression     >2sigma(I)
_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXS-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_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^)+(0.1400P)^2^+0.0000P] 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         2237
_refine_ls_number_parameters     133
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0427
_refine_ls_R_factor_gt           0.0371
_refine_ls_wR_factor_ref         0.1592
_refine_ls_wR_factor_gt          0.1510
_refine_ls_goodness_of_fit_ref   1.011
_refine_ls_restrained_S_all      1.011
_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 0.5000 0.5000 1.0000 0.0150(2) Uani 1 2 d S . .
Co2 Co 0.505259(18) 0.544916(19) 0.64087(5) 0.0159(2) Uani 1 1 d . . .
O1W O 0.55654(9) 0.54918(9) 0.8499(2) 0.0107(4) Uani 1 1 d . . .
O1 O 0.45851(11) 0.46796(11) 0.7873(3) 0.0220(5) Uani 1 1 d . . .
O2W O 0.55541(9) 0.47118(9) 0.5459(2) 0.0136(4) Uani 1 1 d . . .
O3W O 0.6890(2) 0.4760(3) 0.5719(7) 0.0971(18) Uani 1 1 d . . .
H3WA H 0.6876 0.4992 0.4890 0.146 Uiso 1 1 d R . .
H3WB H 0.7224 0.4868 0.6241 0.146 Uiso 1 1 d R . .
N1 N 0.56491(14) 0.61045(13) 0.5224(3) 0.0231(6) Uani 1 1 d . . .
N2 N 0.64006(13) 0.69014(14) 0.5175(3) 0.0232(6) Uani 1 1 d . . .
N3 N 0.56822(14) 0.42255(13) 0.9929(3) 0.0244(6) Uani 1 1 d . . .
N4 N 0.64879(16) 0.36512(16) 0.8571(3) 0.0319(7) Uani 1 1 d . . .
H4A H 0.6664 0.3586 0.7664 0.038 Uiso 1 1 calc R . .
C1 C 0.42092(15) 0.42151(15) 0.7651(4) 0.0215(6) Uani 1 1 d . . .
C2 C 0.59072(15) 0.61396(16) 0.3737(4) 0.0223(7) Uani 1 1 d . . .
C3 C 0.59581(17) 0.65652(17) 0.6017(4) 0.0272(7) Uani 1 1 d . . .
H3A H 0.5876 0.6651 0.7078 0.033 Uiso 1 1 calc R . .
C4 C 0.63697(15) 0.66375(15) 0.3727(4) 0.0213(6) Uani 1 1 d . . .
C5 C 0.60084(19) 0.40985(19) 0.8647(4) 0.0311(8) Uani 1 1 d . . .
H5A H 0.5908 0.4327 0.7733 0.037 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 0.0166(3) 0.0165(3) 0.0119(3) -0.00006(19) 0.00066(19) 0.00032(18)
Co2 0.0176(3) 0.0189(3) 0.0111(3) -0.00095(14) 0.00083(14) -0.00045(12)
O1W 0.0130(8) 0.0163(9) 0.0029(8) 0.0013(6) 0.0000(7) -0.0054(7)
O1 0.0278(11) 0.0217(10) 0.0165(11) -0.0011(9) -0.0019(9) -0.0075(8)
O2W 0.0159(9) 0.0184(9) 0.0064(9) -0.0043(7) -0.0034(7) 0.0046(7)
O3W 0.047(2) 0.157(5) 0.087(4) -0.035(4) 0.000(2) -0.003(3)
N1 0.0277(13) 0.0276(14) 0.0140(13) 0.0002(10) 0.0052(10) -0.0063(10)
N2 0.0243(13) 0.0271(13) 0.0181(13) -0.0003(10) 0.0019(10) -0.0065(10)
N3 0.0299(14) 0.0266(14) 0.0167(13) 0.0039(10) 0.0052(11) 0.0117(10)
N4 0.0402(17) 0.0424(17) 0.0132(13) 0.0033(12) 0.0051(12) 0.0179(13)
C1 0.0219(14) 0.0234(14) 0.0191(15) 0.0019(11) 0.0007(11) -0.0041(11)
C2 0.0236(15) 0.0255(15) 0.0178(16) -0.0003(11) 0.0018(11) -0.0072(12)
C3 0.0317(16) 0.0337(17) 0.0162(14) 0.0001(13) 0.0034(12) -0.0082(13)
C4 0.0220(14) 0.0232(14) 0.0187(16) -0.0018(11) -0.0006(11) -0.0059(11)
C5 0.0370(19) 0.0376(19) 0.0186(17) 0.0042(14) 0.0058(14) 0.0175(15)
_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 O1W 2.0062(18) 9_667 ?
Co1 O1W 2.0062(18) . ?
Co1 O1 2.101(2) . ?
Co1 O1 2.101(2) 9_667 ?
Co1 N3 2.141(3) . ?
Co1 N3 2.141(3) 9_667 ?
Co2 O2W 2.0158(19) . ?
Co2 O2W 2.0460(19) 9_666 ?
Co2 N2 2.059(3) 15_566 ?
Co2 O1W 2.0632(19) . ?
Co2 N1 2.093(3) . ?
Co2 O1 2.240(2) . ?
O1 C1 1.253(4) . ?
O2W Co2 2.0460(19) 9_666 ?
O3W H3WA 0.8500 . ?
O3W H3WB 0.8500 . ?
N1 C3 1.331(4) . ?
N1 C2 1.367(4) . ?
N2 C4 1.342(4) . ?
N2 C3 1.354(4) . ?
N2 Co2 2.059(3) 12_767 ?
N3 C5 1.304(4) . ?
N3 C4 1.374(4) 7_545 ?
N4 C5 1.361(4) . ?
N4 C1 1.395(4) 11_667 ?
N4 H4A 0.8600 . ?
C1 N4 1.395(4) 16_657 ?
C1 C2 1.406(5) 9_666 ?
C2 C1 1.406(5) 9_666 ?
C2 C4 1.409(4) . ?
C3 H3A 0.9300 . ?
C4 N3 1.374(4) 8_453 ?
C5 H5A 0.9300 . ?
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
O1W Co1 O1W 180.00(9) 9_667 . ?
O1W Co1 O1 98.10(8) 9_667 . ?
O1W Co1 O1 81.90(8) . . ?
O1W Co1 O1 81.90(8) 9_667 9_667 ?
O1W Co1 O1 98.10(8) . 9_667 ?
O1 Co1 O1 180.000(1) . 9_667 ?
O1W Co1 N3 91.29(9) 9_667 . ?
O1W Co1 N3 88.71(9) . . ?
O1 Co1 N3 90.53(11) . . ?
O1 Co1 N3 89.47(11) 9_667 . ?
O1W Co1 N3 88.71(9) 9_667 9_667 ?
O1W Co1 N3 91.29(9) . 9_667 ?
O1 Co1 N3 89.47(11) . 9_667 ?
O1 Co1 N3 90.53(11) 9_667 9_667 ?
N3 Co1 N3 180.0 . 9_667 ?
O2W Co2 O2W 83.48(8) . 9_666 ?
O2W Co2 N2 169.93(10) . 15_566 ?
O2W Co2 N2 89.64(10) 9_666 15_566 ?
O2W Co2 O1W 96.15(8) . . ?
O2W Co2 O1W 169.82(8) 9_666 . ?
N2 Co2 O1W 89.32(10) 15_566 . ?
O2W Co2 N1 89.84(10) . . ?
O2W Co2 N1 95.77(10) 9_666 . ?
N2 Co2 N1 98.18(11) 15_566 . ?
O1W Co2 N1 94.40(9) . . ?
O2W Co2 O1 84.41(9) . . ?
O2W Co2 O1 92.50(8) 9_666 . ?
N2 Co2 O1 88.57(10) 15_566 . ?
O1W Co2 O1 77.35(8) . . ?
N1 Co2 O1 169.34(10) . . ?
Co1 O1W Co2 102.60(8) . . ?
C1 O1 Co1 128.7(2) . . ?
C1 O1 Co2 137.3(2) . . ?
Co1 O1 Co2 94.01(8) . . ?
Co2 O2W Co2 96.52(8) . 9_666 ?
H3WA O3W H3WB 107.9 . . ?
C3 N1 C2 103.6(3) . . ?
C3 N1 Co2 120.7(2) . . ?
C2 N1 Co2 134.9(2) . . ?
C4 N2 C3 103.7(3) . . ?
C4 N2 Co2 129.9(2) . 12_767 ?
C3 N2 Co2 125.7(2) . 12_767 ?
C5 N3 C4 114.4(3) . 7_545 ?
C5 N3 Co1 121.2(2) . . ?
C4 N3 Co1 124.1(2) 7_545 . ?
C5 N4 C1 125.1(3) . 11_667 ?
C5 N4 H4A 117.4 . . ?
C1 N4 H4A 117.4 11_667 . ?
O1 C1 N4 118.5(3) . 16_657 ?
O1 C1 C2 129.3(3) . 9_666 ?
N4 C1 C2 112.2(3) 16_657 9_666 ?
N1 C2 C1 132.2(3) . 9_666 ?
N1 C2 C4 108.1(3) . . ?
C1 C2 C4 119.7(3) 9_666 . ?
N1 C3 N2 115.5(3) . . ?
N1 C3 H3A 122.2 . . ?
N2 C3 H3A 122.2 . . ?
N2 C4 N3 126.2(3) . 8_453 ?
N2 C4 C2 109.0(3) . . ?
N3 C4 C2 124.7(3) 8_453 . ?
N3 C5 N4 123.8(3) . . ?
N3 C5 H5A 118.1 . . ?
N4 C5 H5A 118.1 . . ?
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_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O1W Co1 O1W Co2 -81(100) 9_667 . . . ?
O1 Co1 O1W Co2 16.52(9) . . . . ?
O1 Co1 O1W Co2 -163.48(9) 9_667 . . . ?
N3 Co1 O1W Co2 107.25(10) . . . . ?
N3 Co1 O1W Co2 -72.75(10) 9_667 . . . ?
O2W Co2 O1W Co1 -98.54(9) . . . . ?
O2W Co2 O1W Co1 -11.2(5) 9_666 . . . ?
N2 Co2 O1W Co1 72.99(10) 15_566 . . . ?
N1 Co2 O1W Co1 171.14(10) . . . . ?
O1 Co2 O1W Co1 -15.70(9) . . . . ?
O1W Co1 O1 C1 -14.4(3) 9_667 . . . ?
O1W Co1 O1 C1 165.6(3) . . . . ?
O1 Co1 O1 C1 -128(89) 9_667 . . . ?
N3 Co1 O1 C1 77.0(3) . . . . ?
N3 Co1 O1 C1 -103.0(3) 9_667 . . . ?
O1W Co1 O1 Co2 165.15(9) 9_667 . . . ?
O1W Co1 O1 Co2 -14.85(9) . . . . ?
O1 Co1 O1 Co2 51(71) 9_667 . . . ?
N3 Co1 O1 Co2 -103.47(11) . . . . ?
N3 Co1 O1 Co2 76.53(11) 9_667 . . . ?
O2W Co2 O1 C1 -68.3(3) . . . . ?
O2W Co2 O1 C1 14.9(3) 9_666 . . . ?
N2 Co2 O1 C1 104.5(3) 15_566 . . . ?
O1W Co2 O1 C1 -165.9(3) . . . . ?
N1 Co2 O1 C1 -126.0(5) . . . . ?
O2W Co2 O1 Co1 112.25(9) . . . . ?
O2W Co2 O1 Co1 -164.55(9) 9_666 . . . ?
N2 Co2 O1 Co1 -74.98(11) 15_566 . . . ?
O1W Co2 O1 Co1 14.65(8) . . . . ?
N1 Co2 O1 Co1 54.6(5) . . . . ?
O2W Co2 O2W Co2 0.0 9_666 . . 9_666 ?
N2 Co2 O2W Co2 47.1(6) 15_566 . . 9_666 ?
O1W Co2 O2W Co2 169.76(8) . . . 9_666 ?
N1 Co2 O2W Co2 -95.82(10) . . . 9_666 ?
O1 Co2 O2W Co2 93.17(9) . . . 9_666 ?
O2W Co2 N1 C3 -125.4(3) . . . . ?
O2W Co2 N1 C3 151.2(3) 9_666 . . . ?
N2 Co2 N1 C3 60.7(3) 15_566 . . . ?
O1W Co2 N1 C3 -29.2(3) . . . . ?
O1 Co2 N1 C3 -68.1(6) . . . . ?
O2W Co2 N1 C2 42.2(3) . . . . ?
O2W Co2 N1 C2 -41.2(3) 9_666 . . . ?
N2 Co2 N1 C2 -131.7(3) 15_566 . . . ?
O1W Co2 N1 C2 138.4(3) . . . . ?
O1 Co2 N1 C2 99.4(5) . . . . ?
O1W Co1 N3 C5 146.6(3) 9_667 . . . ?
O1W Co1 N3 C5 -33.4(3) . . . . ?
O1 Co1 N3 C5 48.5(3) . . . . ?
O1 Co1 N3 C5 -131.5(3) 9_667 . . . ?
N3 Co1 N3 C5 84(100) 9_667 . . . ?
O1W Co1 N3 C4 -40.3(3) 9_667 . . 7_545 ?
O1W Co1 N3 C4 139.7(3) . . . 7_545 ?
O1 Co1 N3 C4 -138.4(3) . . . 7_545 ?
O1 Co1 N3 C4 41.6(3) 9_667 . . 7_545 ?
N3 Co1 N3 C4 -103(100) 9_667 . . 7_545 ?
Co1 O1 C1 N4 22.2(5) . . . 16_657 ?
Co2 O1 C1 N4 -157.1(3) . . . 16_657 ?
Co1 O1 C1 C2 -156.5(3) . . . 9_666 ?
Co2 O1 C1 C2 24.1(6) . . . 9_666 ?
C3 N1 C2 C1 179.7(4) . . . 9_666 ?
Co2 N1 C2 C1 10.7(6) . . . 9_666 ?
C3 N1 C2 C4 -0.2(4) . . . . ?
Co2 N1 C2 C4 -169.2(2) . . . . ?
C2 N1 C3 N2 -0.1(4) . . . . ?
Co2 N1 C3 N2 170.8(2) . . . . ?
C4 N2 C3 N1 0.4(4) . . . . ?
Co2 N2 C3 N1 -170.8(2) 12_767 . . . ?
C3 N2 C4 N3 179.4(3) . . . 8_453 ?
Co2 N2 C4 N3 -10.0(5) 12_767 . . 8_453 ?
C3 N2 C4 C2 -0.5(4) . . . . ?
Co2 N2 C4 C2 170.2(2) 12_767 . . . ?
N1 C2 C4 N2 0.4(4) . . . . ?
C1 C2 C4 N2 -179.5(3) 9_666 . . . ?
N1 C2 C4 N3 -179.4(3) . . . 8_453 ?
C1 C2 C4 N3 0.7(5) 9_666 . . 8_453 ?
C4 N3 C5 N4 0.2(6) 7_545 . . . ?
Co1 N3 C5 N4 174.0(3) . . . . ?
C1 N4 C5 N3 -3.0(7) 11_667 . . . ?
_diffrn_measured_fraction_theta_max 0.996
_diffrn_reflns_theta_full        28.25
_diffrn_measured_fraction_theta_full 0.996
_refine_diff_density_max         1.204
_refine_diff_density_min         -0.718
_refine_diff_density_rms         0.123