# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2014

#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  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.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_20101121

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C23 H17 Mn N3 O6'
_chemical_formula_weight         486.34

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'
Mn Mn 0.3368 0.7283 '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                   7.6099(3)
_cell_length_b                   10.4281(5)
_cell_length_c                   13.6427(7)
_cell_angle_alpha                84.281(4)
_cell_angle_beta                 89.806(4)
_cell_angle_gamma                70.891(4)
_cell_volume                     1017.40(8)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    4291
_cell_measurement_theta_min      2.4286
_cell_measurement_theta_max      26.7909

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.22
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.588
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             498
_exptl_absorpt_coefficient_mu    0.698
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.91967
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1996)'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      293(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  'Oxford XCalibur Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            8095
_diffrn_reflns_av_R_equivalents  0.0272
_diffrn_reflns_av_unetI/netI     0.0486
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         2.43
_diffrn_reflns_theta_max         25.02
_reflns_number_total             3449
_reflns_number_gt                2604
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'CrysAlisPro, Oxford Diffraction Ltd.'
_computing_cell_refinement       'CrysAlisPro, Oxford Diffraction Ltd.'
_computing_data_reduction        'CrysAlisPro, Oxford Diffraction Ltd.'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 1997)'
_computing_publication_material  'SHELXTL (Sheldrick, 1997)'

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² 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/[σ²(Fo²)+(0.1254P)²+0.0000P] where P=(Fo²+2Fc²)/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         3449
_refine_ls_number_parameters     305
_refine_ls_number_restraints     6
_refine_ls_R_factor_all          0.0746
_refine_ls_R_factor_gt           0.0554
_refine_ls_wR_factor_ref         0.1756
_refine_ls_wR_factor_gt          0.1614
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_restrained_S_all      1.032
_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
Mn1 Mn 0.59474(8) 0.75521(6) 0.76149(4) 0.0274(3) Uani 1 1 d . . .
N2 N 0.6675(5) 0.8917(4) 0.8613(3) 0.0350(9) Uani 1 1 d . . .
O3 O 0.3021(4) 0.8374(3) 0.7868(2) 0.0452(8) Uani 1 1 d . . .
O1 O -0.1273(4) 0.6687(3) 0.7166(2) 0.0370(7) Uani 1 1 d . . .
O5 O 0.5489(5) 0.9106(5) 0.6371(3) 0.0839(11) Uani 1 1 d D . .
N3 N 0.4555(4) 0.6137(3) 0.6951(2) 0.0283(8) Uani 1 1 d . . .
N1 N 0.6840(5) 0.6303(4) 0.9118(3) 0.0326(8) Uani 1 1 d . . .
C13 C 0.5335(5) 0.4895(4) 0.6601(3) 0.0295(9) Uani 1 1 d . . .
O2 O -0.1394(4) 0.7326(4) 0.5562(2) 0.0578(10) Uani 1 1 d . . .
O4 O 0.0449(4) 0.8898(4) 0.6908(3) 0.0642(11) Uani 1 1 d . . .
C6 C 0.7200(5) 0.8378(4) 0.9549(3) 0.0307(10) Uani 1 1 d . . .
C5 C 0.7306(5) 0.6988(4) 0.9817(3) 0.0307(10) Uani 1 1 d . . .
C14 C 0.7261(5) 0.4199(5) 0.6746(3) 0.0370(10) Uani 1 1 d . . .
H14 H 0.8000 0.4597 0.7063 0.044 Uiso 1 1 calc R . .
C11 C 0.7083(7) 1.0981(5) 0.9009(4) 0.0534(13) Uani 1 1 d . . .
H11 H 0.7051 1.1864 0.8797 0.064 Uiso 1 1 calc R . .
C18 C 0.4241(6) 0.4283(5) 0.6108(3) 0.0344(10) Uani 1 1 d . . .
C7 C 0.7658(6) 0.9113(5) 1.0260(3) 0.0413(11) Uani 1 1 d . . .
C23 C -0.0541(5) 0.6820(5) 0.6348(3) 0.0349(10) Uani 1 1 d . . .
C21 C 0.2733(5) 0.6755(4) 0.6846(3) 0.0288(9) Uani 1 1 d . . .
C20 C 0.1554(5) 0.6180(5) 0.6361(3) 0.0303(10) Uani 1 1 d . . .
C1 C 0.6999(6) 0.5004(5) 0.9367(4) 0.0415(11) Uani 1 1 d . . .
H1 H 0.6651 0.4537 0.8899 0.050 Uiso 1 1 calc R . .
C19 C 0.2316(6) 0.4977(5) 0.5991(3) 0.0355(10) Uani 1 1 d . . .
H19 H 0.1568 0.4604 0.5658 0.043 Uiso 1 1 calc R . .
C9 C 0.8350(7) 0.7171(6) 1.1480(4) 0.0538(14) Uani 1 1 d . . .
H9 H 0.8733 0.6775 1.2118 0.065 Uiso 1 1 calc R . .
C12 C 0.6653(7) 1.0189(5) 0.8356(4) 0.0469(12) Uani 1 1 d . . .
H12 H 0.6333 1.0561 0.7707 0.056 Uiso 1 1 calc R . .
C17 C 0.5111(7) 0.2987(5) 0.5766(4) 0.0471(12) Uani 1 1 d . . .
H17 H 0.4407 0.2580 0.5431 0.057 Uiso 1 1 calc R . .
C22 C 0.1980(6) 0.8124(5) 0.7240(4) 0.0388(11) Uani 1 1 d . . .
C15 C 0.8033(6) 0.2962(5) 0.6429(4) 0.0476(12) Uani 1 1 d . . .
H15 H 0.9299 0.2508 0.6543 0.057 Uiso 1 1 calc R . .
C4 C 0.7928(5) 0.6358(5) 1.0771(3) 0.0369(11) Uani 1 1 d . . .
C8 C 0.8202(7) 0.8474(6) 1.1237(4) 0.0496(13) Uani 1 1 d . . .
H8 H 0.8459 0.8975 1.1712 0.059 Uiso 1 1 calc R . .
C3 C 0.8117(6) 0.4990(5) 1.0980(4) 0.0474(13) Uani 1 1 d . . .
H3 H 0.8562 0.4539 1.1597 0.057 Uiso 1 1 calc R . .
C10 C 0.7553(7) 1.0466(5) 0.9961(4) 0.0511(13) Uani 1 1 d . . .
H10 H 0.7803 1.1003 1.0410 0.061 Uiso 1 1 calc R . .
C2 C 0.7648(7) 0.4307(5) 1.0275(4) 0.0482(12) Uani 1 1 d . . .
H2 H 0.7765 0.3390 1.0406 0.058 Uiso 1 1 calc R . .
C16 C 0.6966(7) 0.2340(6) 0.5927(4) 0.0528(13) Uani 1 1 d . . .
H16 H 0.7530 0.1489 0.5706 0.063 Uiso 1 1 calc R . .
O6 O 0.8024(5) 0.9581(5) 0.4351(3) 0.0839(11) Uani 1 1 d D . .
H6A H 0.786(5) 0.899(4) 0.381(3) 0.040(6) Uiso 1 1 d D . .
H6B H 0.667(3) 1.017(3) 0.435(3) 0.040(6) Uiso 1 1 d D . .
H5B H 0.466(4) 0.988(3) 0.622(3) 0.040(6) Uiso 1 1 d D . .
H5A H 0.656(3) 0.889(4) 0.603(3) 0.040(6) Uiso 1 1 d D . .


_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
Mn1 O1 2.125(3) 1_655 ?
Mn1 O3 2.149(3) . ?
Mn1 O5 2.171(4) . ?
Mn1 N2 2.257(4) . ?
Mn1 N1 2.293(3) . ?
Mn1 N3 2.327(3) . ?
N2 C12 1.332(6) . ?
N2 C6 1.349(5) . ?
O3 C22 1.270(5) . ?
O1 C23 1.261(5) . ?
O1 Mn1 2.125(3) 1_455 ?
O5 H5B 0.851(18) . ?
O5 H5A 0.911(18) . ?
N3 C21 1.325(5) . ?
N3 C13 1.370(5) . ?
N1 C1 1.329(6) . ?
N1 C5 1.360(5) . ?
C13 C14 1.411(5) . ?
C13 C18 1.411(6) . ?
O2 C23 1.232(5) . ?
O4 C22 1.237(5) . ?
C6 C7 1.406(6) . ?
C6 C5 1.435(6) . ?
C5 C4 1.408(6) . ?
C14 C15 1.345(6) . ?
C14 H14 0.9300 . ?
C11 C10 1.357(7) . ?
C11 C12 1.381(7) . ?
C11 H11 0.9300 . ?
C18 C19 1.407(5) . ?
C18 C17 1.421(6) . ?
C7 C10 1.406(7) . ?
C7 C8 1.427(7) . ?
C23 C20 1.513(5) . ?
C21 C20 1.426(6) . ?
C21 C22 1.507(6) . ?
C20 C19 1.347(6) . ?
C1 C2 1.378(6) . ?
C1 H1 0.9300 . ?
C19 H19 0.9300 . ?
C9 C8 1.335(7) . ?
C9 C4 1.449(7) . ?
C9 H9 0.9300 . ?
C12 H12 0.9300 . ?
C17 C16 1.358(6) . ?
C17 H17 0.9300 . ?
C15 C16 1.410(7) . ?
C15 H15 0.9300 . ?
C4 C3 1.386(7) . ?
C8 H8 0.9300 . ?
C3 C2 1.365(7) . ?
C3 H3 0.9300 . ?
C10 H10 0.9300 . ?
C2 H2 0.9300 . ?
C16 H16 0.9300 . ?
O6 H6A 1.039(18) . ?
O6 H6B 1.009(18) . ?

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
O1 Mn1 O3 171.90(11) 1_655 . ?
O1 Mn1 O5 88.69(13) 1_655 . ?
O3 Mn1 O5 87.24(14) . . ?
O1 Mn1 N2 93.88(12) 1_655 . ?
O3 Mn1 N2 93.19(12) . . ?
O5 Mn1 N2 91.08(17) . . ?
O1 Mn1 N1 88.09(11) 1_655 . ?
O3 Mn1 N1 97.76(12) . . ?
O5 Mn1 N1 163.48(17) . . ?
N2 Mn1 N1 72.98(13) . . ?
O1 Mn1 N3 100.46(12) 1_655 . ?
O3 Mn1 N3 73.28(12) . . ?
O5 Mn1 N3 98.73(17) . . ?
N2 Mn1 N3 162.74(12) . . ?
N1 Mn1 N3 97.79(12) . . ?
C12 N2 C6 117.7(4) . . ?
C12 N2 Mn1 125.9(3) . . ?
C6 N2 Mn1 116.3(3) . . ?
C22 O3 Mn1 114.6(3) . . ?
C23 O1 Mn1 130.8(3) . 1_455 ?
Mn1 O5 H5B 134(3) . . ?
Mn1 O5 H5A 107(2) . . ?
H5B O5 H5A 118(3) . . ?
C21 N3 C13 119.2(3) . . ?
C21 N3 Mn1 110.2(3) . . ?
C13 N3 Mn1 130.3(2) . . ?
C1 N1 C5 117.4(4) . . ?
C1 N1 Mn1 127.9(3) . . ?
C5 N1 Mn1 114.7(3) . . ?
N3 C13 C14 119.8(4) . . ?
N3 C13 C18 121.2(3) . . ?
C14 C13 C18 119.0(4) . . ?
N2 C6 C7 122.8(4) . . ?
N2 C6 C5 117.9(4) . . ?
C7 C6 C5 119.2(4) . . ?
N1 C5 C4 121.8(4) . . ?
N1 C5 C6 118.1(4) . . ?
C4 C5 C6 120.1(4) . . ?
C15 C14 C13 120.3(4) . . ?
C15 C14 H14 119.9 . . ?
C13 C14 H14 119.9 . . ?
C10 C11 C12 119.8(5) . . ?
C10 C11 H11 120.1 . . ?
C12 C11 H11 120.1 . . ?
C19 C18 C13 118.2(4) . . ?
C19 C18 C17 122.7(4) . . ?
C13 C18 C17 119.1(4) . . ?
C10 C7 C6 117.2(4) . . ?
C10 C7 C8 123.1(4) . . ?
C6 C7 C8 119.7(4) . . ?
O2 C23 O1 125.5(4) . . ?
O2 C23 C20 119.7(4) . . ?
O1 C23 C20 114.6(3) . . ?
N3 C21 C20 122.1(4) . . ?
N3 C21 C22 116.1(4) . . ?
C20 C21 C22 121.7(3) . . ?
C19 C20 C21 119.1(4) . . ?
C19 C20 C23 119.4(4) . . ?
C21 C20 C23 121.3(4) . . ?
N1 C1 C2 124.2(5) . . ?
N1 C1 H1 117.9 . . ?
C2 C1 H1 117.9 . . ?
C20 C19 C18 120.2(4) . . ?
C20 C19 H19 119.9 . . ?
C18 C19 H19 119.9 . . ?
C8 C9 C4 121.5(5) . . ?
C8 C9 H9 119.3 . . ?
C4 C9 H9 119.3 . . ?
N2 C12 C11 123.0(5) . . ?
N2 C12 H12 118.5 . . ?
C11 C12 H12 118.5 . . ?
C16 C17 C18 120.3(4) . . ?
C16 C17 H17 119.9 . . ?
C18 C17 H17 119.9 . . ?
O4 C22 O3 126.7(4) . . ?
O4 C22 C21 117.4(4) . . ?
O3 C22 C21 115.9(4) . . ?
C14 C15 C16 121.5(4) . . ?
C14 C15 H15 119.3 . . ?
C16 C15 H15 119.3 . . ?
C3 C4 C5 118.1(4) . . ?
C3 C4 C9 123.6(4) . . ?
C5 C4 C9 118.3(4) . . ?
C9 C8 C7 121.1(5) . . ?
C9 C8 H8 119.4 . . ?
C7 C8 H8 119.4 . . ?
C2 C3 C4 119.8(4) . . ?
C2 C3 H3 120.1 . . ?
C4 C3 H3 120.1 . . ?
C11 C10 C7 119.3(5) . . ?
C11 C10 H10 120.4 . . ?
C7 C10 H10 120.4 . . ?
C3 C2 C1 118.6(5) . . ?
C3 C2 H2 120.7 . . ?
C1 C2 H2 120.7 . . ?
C17 C16 C15 119.8(5) . . ?
C17 C16 H16 120.1 . . ?
C15 C16 H16 120.1 . . ?
H6A O6 H6B 96(2) . . ?

_diffrn_measured_fraction_theta_max 0.958
_diffrn_reflns_theta_full        25.02
_diffrn_measured_fraction_theta_full 0.958
_refine_diff_density_max         1.773
_refine_diff_density_min         -1.736
_refine_diff_density_rms         0.126
_database_code_depnum_ccdc_archive 'CCDC 975535'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  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.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_1206

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C40 H34 Co N6 O14'
_chemical_formula_weight         881.66

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'

_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                   8.6479(4)
_cell_length_b                   9.4452(4)
_cell_length_c                   12.1753(6)
_cell_angle_alpha                96.438(4)
_cell_angle_beta                 96.446(4)
_cell_angle_gamma                104.773(4)
_cell_volume                     945.23(8)
_cell_formula_units_Z            1
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    4016
_cell_measurement_theta_min      2.4573
_cell_measurement_theta_max      25.1623

_exptl_crystal_description       block
_exptl_crystal_colour            red
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.18
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.549
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             455
_exptl_absorpt_coefficient_mu    0.536
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.85716
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1996)'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      293(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  'Oxford XCalibur Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            6518
_diffrn_reflns_av_R_equivalents  0.0213
_diffrn_reflns_av_unetI/netI     0.0362
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_theta_min         2.46
_diffrn_reflns_theta_max         25.00
_reflns_number_total             3021
_reflns_number_gt                2522
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'CrysAlisPro, Oxford Diffraction Ltd.'
_computing_cell_refinement       'CrysAlisPro, Oxford Diffraction Ltd.'
_computing_data_reduction        'CrysAlisPro, Oxford Diffraction Ltd.'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 1997)'
_computing_publication_material  'SHELXTL (Sheldrick, 1997)'

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² 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/[σ²(Fo²)+(0.0544P)²+0.0000P] where P=(Fo²+2Fc²)/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         3021
_refine_ls_number_parameters     293
_refine_ls_number_restraints     6
_refine_ls_R_factor_all          0.0395
_refine_ls_R_factor_gt           0.0305
_refine_ls_wR_factor_ref         0.0899
_refine_ls_wR_factor_gt          0.0784
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_restrained_S_all      1.045
_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 0.5000 1.0000 0.5000 0.02354(15) Uani 1 2 d S . .
O1 O 0.4652(3) 0.4004(2) 0.19282(17) 0.0612(6) Uani 1 1 d . . .
O2 O 0.3155(2) 0.5461(2) 0.13792(15) 0.0469(5) Uani 1 1 d . . .
H2A H 0.3278 0.5125 0.0755 0.070 Uiso 1 1 calc R . .
O5 O -0.0613(2) 1.1632(2) 0.06973(16) 0.0475(5) Uani 1 1 d . . .
O3 O 0.6208(2) 0.75282(18) 0.24746(14) 0.0368(4) Uani 1 1 d . . .
O4 O 0.60457(18) 0.94052(17) 0.36839(13) 0.0304(4) Uani 1 1 d . . .
N1 N 0.4030(2) 0.7546(2) 0.47355(15) 0.0234(4) Uani 1 1 d . . .
N2 N 0.2934(2) 1.0081(2) 0.38595(16) 0.0274(5) Uani 1 1 d . . .
N3 N -0.1340(2) 0.9814(2) 0.17581(16) 0.0296(5) Uani 1 1 d . . .
H17 H -0.2140 0.9112 0.1863 0.035 Uiso 1 1 calc R . .
C9 C 0.4386(3) 0.6999(2) 0.37812(19) 0.0250(5) Uani 1 1 d . . .
C8 C 0.3773(3) 0.5496(3) 0.3292(2) 0.0286(6) Uani 1 1 d . . .
C7 C 0.2866(3) 0.4546(3) 0.3895(2) 0.0347(6) Uani 1 1 d . . .
H7 H 0.2487 0.3544 0.3613 0.042 Uiso 1 1 calc R . .
C6 C 0.2505(3) 0.5062(3) 0.4927(2) 0.0295(6) Uani 1 1 d . . .
C1 C 0.3046(3) 0.6600(3) 0.53168(19) 0.0260(5) Uani 1 1 d . . .
C2 C 0.2578(3) 0.7156(3) 0.6307(2) 0.0315(6) Uani 1 1 d . . .
H2 H 0.2918 0.8166 0.6569 0.038 Uiso 1 1 calc R . .
C3 C 0.1622(3) 0.6214(3) 0.6888(2) 0.0376(6) Uani 1 1 d . . .
H3 H 0.1307 0.6593 0.7539 0.045 Uiso 1 1 calc R . .
C4 C 0.1109(3) 0.4687(3) 0.6516(2) 0.0409(7) Uani 1 1 d . . .
H4 H 0.0473 0.4059 0.6926 0.049 Uiso 1 1 calc R . .
C5 C 0.1538(3) 0.4127(3) 0.5563(2) 0.0393(7) Uani 1 1 d . . .
H5 H 0.1193 0.3112 0.5322 0.047 Uiso 1 1 calc R . .
C11 C 0.5633(3) 0.8056(3) 0.3248(2) 0.0255(5) Uani 1 1 d . . .
C10 C 0.3957(3) 0.4922(3) 0.2140(2) 0.0339(6) Uani 1 1 d . . .
C12 C 0.1461(3) 0.9455(3) 0.4085(2) 0.0360(6) Uani 1 1 d . . .
H12 H 0.1385 0.9046 0.4744 0.043 Uiso 1 1 calc R . .
C13 C 0.0062(3) 0.9374(3) 0.3414(2) 0.0353(6) Uani 1 1 d . . .
H13 H -0.0929 0.8916 0.3616 0.042 Uiso 1 1 calc R . .
C14 C 0.0124(3) 0.9977(3) 0.24268(19) 0.0260(5) Uani 1 1 d . . .
C16 C 0.2983(3) 1.0673(3) 0.2907(2) 0.0320(6) Uani 1 1 d . . .
H16 H 0.3992 1.1120 0.2727 0.038 Uiso 1 1 calc R . .
C17 C -0.1655(3) 1.0639(3) 0.0957(2) 0.0291(6) Uani 1 1 d . . .
C15 C 0.1641(3) 1.0661(3) 0.2180(2) 0.0313(6) Uani 1 1 d . . .
H15 H 0.1748 1.1102 0.1537 0.038 Uiso 1 1 calc R . .
C18 C -0.3389(3) 1.0281(3) 0.04554(19) 0.0270(5) Uani 1 1 d . . .
C20 C -0.4043(3) 1.1442(3) 0.0262(2) 0.0330(6) Uani 1 1 d . . .
H20 H -0.3398 1.2412 0.0436 0.040 Uiso 1 1 calc R . .
C19 C -0.4352(3) 0.8838(3) 0.0188(2) 0.0329(6) Uani 1 1 d . . .
H19 H -0.3916 0.8056 0.0311 0.039 Uiso 1 1 calc R . .
O6 O 0.0494(3) 0.6853(3) 0.1175(2) 0.0631(6) Uani 1 1 d D . .
O7 O 0.2732(3) 0.4409(3) 0.93207(17) 0.0656(7) Uani 1 1 d D . .
H6B H 0.061(4) 0.731(4) 0.054(2) 0.105(14) Uiso 1 1 d D . .
H7A H 0.160(2) 0.402(4) 0.912(3) 0.101(14) Uiso 1 1 d D . .
H6A H 0.132(3) 0.643(4) 0.131(3) 0.095(14) Uiso 1 1 d D . .
H7B H 0.324(3) 0.436(4) 0.874(2) 0.089(13) Uiso 1 1 d D . .


_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 O4 2.0208(16) . ?
Co1 O4 2.0208(16) 2_676 ?
Co1 N2 2.1594(18) . ?
Co1 N2 2.1594(18) 2_676 ?
Co1 N1 2.2274(18) . ?
Co1 N1 2.2274(18) 2_676 ?
O1 C10 1.195(3) . ?
O2 C10 1.320(3) . ?
O2 H2A 0.8200 . ?
O5 C17 1.221(3) . ?
O3 C11 1.229(3) . ?
O4 C11 1.267(3) . ?
N1 C9 1.318(3) . ?
N1 C1 1.383(3) . ?
N2 C12 1.333(3) . ?
N2 C16 1.343(3) . ?
N3 C17 1.360(3) . ?
N3 C14 1.389(3) . ?
N3 H17 0.8600 . ?
C9 C8 1.416(3) . ?
C9 C11 1.528(3) . ?
C8 C7 1.370(3) . ?
C8 C10 1.487(3) . ?
C7 C6 1.394(3) . ?
C7 H7 0.9300 . ?
C6 C1 1.415(3) . ?
C6 C5 1.415(3) . ?
C1 C2 1.404(3) . ?
C2 C3 1.369(3) . ?
C2 H2 0.9300 . ?
C3 C4 1.402(4) . ?
C3 H3 0.9300 . ?
C4 C5 1.350(4) . ?
C4 H4 0.9300 . ?
C5 H5 0.9300 . ?
C12 C13 1.362(3) . ?
C12 H12 0.9300 . ?
C13 C14 1.387(3) . ?
C13 H13 0.9300 . ?
C14 C15 1.389(3) . ?
C16 C15 1.375(3) . ?
C16 H16 0.9300 . ?
C17 C18 1.492(3) . ?
C15 H15 0.9300 . ?
C18 C19 1.384(3) . ?
C18 C20 1.386(3) . ?
C20 C19 1.381(3) 2_475 ?
C20 H20 0.9300 . ?
C19 C20 1.381(3) 2_475 ?
C19 H19 0.9300 . ?
O6 H6B 0.932(17) . ?
O6 H6A 0.913(17) . ?
O7 H7A 0.943(18) . ?
O7 H7B 0.880(17) . ?

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
O4 Co1 O4 180.0 . 2_676 ?
O4 Co1 N2 89.50(7) . . ?
O4 Co1 N2 90.50(7) 2_676 . ?
O4 Co1 N2 90.50(7) . 2_676 ?
O4 Co1 N2 89.50(7) 2_676 2_676 ?
N2 Co1 N2 180.0 . 2_676 ?
O4 Co1 N1 78.21(6) . . ?
O4 Co1 N1 101.79(6) 2_676 . ?
N2 Co1 N1 87.91(7) . . ?
N2 Co1 N1 92.09(7) 2_676 . ?
O4 Co1 N1 101.79(6) . 2_676 ?
O4 Co1 N1 78.21(6) 2_676 2_676 ?
N2 Co1 N1 92.09(7) . 2_676 ?
N2 Co1 N1 87.91(7) 2_676 2_676 ?
N1 Co1 N1 180.00(10) . 2_676 ?
C10 O2 H2A 109.5 . . ?
C11 O4 Co1 118.26(14) . . ?
C9 N1 C1 118.7(2) . . ?
C9 N1 Co1 109.21(13) . . ?
C1 N1 Co1 131.74(16) . . ?
C12 N2 C16 115.7(2) . . ?
C12 N2 Co1 118.33(15) . . ?
C16 N2 Co1 125.95(15) . . ?
C17 N3 C14 127.52(19) . . ?
C17 N3 H17 116.2 . . ?
C14 N3 H17 116.2 . . ?
N1 C9 C8 123.7(2) . . ?
N1 C9 C11 116.2(2) . . ?
C8 C9 C11 120.0(2) . . ?
C7 C8 C9 117.5(2) . . ?
C7 C8 C10 118.5(2) . . ?
C9 C8 C10 123.9(2) . . ?
C8 C7 C6 120.8(2) . . ?
C8 C7 H7 119.6 . . ?
C6 C7 H7 119.6 . . ?
C7 C6 C1 118.3(2) . . ?
C7 C6 C5 122.6(2) . . ?
C1 C6 C5 118.9(2) . . ?
N1 C1 C2 120.2(2) . . ?
N1 C1 C6 120.7(2) . . ?
C2 C1 C6 119.1(2) . . ?
C3 C2 C1 120.0(2) . . ?
C3 C2 H2 120.0 . . ?
C1 C2 H2 120.0 . . ?
C2 C3 C4 120.9(3) . . ?
C2 C3 H3 119.5 . . ?
C4 C3 H3 119.5 . . ?
C5 C4 C3 120.1(2) . . ?
C5 C4 H4 120.0 . . ?
C3 C4 H4 120.0 . . ?
C4 C5 C6 120.9(2) . . ?
C4 C5 H5 119.6 . . ?
C6 C5 H5 119.6 . . ?
O3 C11 O4 125.4(2) . . ?
O3 C11 C9 117.9(2) . . ?
O4 C11 C9 116.6(2) . . ?
O1 C10 O2 124.1(3) . . ?
O1 C10 C8 124.0(2) . . ?
O2 C10 C8 111.7(2) . . ?
N2 C12 C13 124.3(2) . . ?
N2 C12 H12 117.9 . . ?
C13 C12 H12 117.9 . . ?
C12 C13 C14 119.7(2) . . ?
C12 C13 H13 120.2 . . ?
C14 C13 H13 120.2 . . ?
C13 C14 N3 117.0(2) . . ?
C13 C14 C15 117.3(2) . . ?
N3 C14 C15 125.6(2) . . ?
N2 C16 C15 124.4(2) . . ?
N2 C16 H16 117.8 . . ?
C15 C16 H16 117.8 . . ?
O5 C17 N3 122.7(2) . . ?
O5 C17 C18 122.5(2) . . ?
N3 C17 C18 114.72(19) . . ?
C16 C15 C14 118.6(2) . . ?
C16 C15 H15 120.7 . . ?
C14 C15 H15 120.7 . . ?
C19 C18 C20 119.6(2) . . ?
C19 C18 C17 122.1(2) . . ?
C20 C18 C17 118.3(2) . . ?
C19 C20 C18 120.2(2) 2_475 . ?
C19 C20 H20 119.9 2_475 . ?
C18 C20 H20 119.9 . . ?
C20 C19 C18 120.2(2) 2_475 . ?
C20 C19 H19 119.9 2_475 . ?
C18 C19 H19 119.9 . . ?
H6B O6 H6A 109(2) . . ?
H7A O7 H7B 112(2) . . ?

_diffrn_measured_fraction_theta_max 0.905
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.905
_refine_diff_density_max         0.271
_refine_diff_density_min         -0.332
_refine_diff_density_rms         0.083

#===END
_database_code_depnum_ccdc_archive 'CCDC 975536'
