# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2015

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_1
_database_code_depnum_ccdc_archive 'CCDC 1059844'
_audit_update_record             
;
2015-05-14 deposited with the CCDC.
2015-05-27 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C18 H17.80 Co2 N O10.90'
_chemical_formula_weight         540.39

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'
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'

_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                   13.5820(4)
_cell_length_b                   10.8173(3)
_cell_length_c                   14.7037(5)
_cell_angle_alpha                90.00
_cell_angle_beta                 110.6280(10)
_cell_angle_gamma                90.00
_cell_volume                     2021.77(11)
_cell_formula_units_Z            4
_cell_measurement_temperature    298(2)
_cell_measurement_reflns_used    11035
_cell_measurement_theta_min      2.395
_cell_measurement_theta_max      28.567

_exptl_crystal_description       plate
_exptl_crystal_colour            red
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.16
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.775
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1096
_exptl_absorpt_coefficient_mu    1.704
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6657
_exptl_absorpt_correction_T_max  0.7722
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      298(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini'
_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            11035
_diffrn_reflns_av_R_equivalents  0.0164
_diffrn_reflns_av_sigmaI/netI    0.0195
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         1.60
_diffrn_reflns_theta_max         26.37
_reflns_number_total             4101
_reflns_number_gt                3735
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_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)+(0.0454P)²+1.4093P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         4101
_refine_ls_number_parameters     293
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0330
_refine_ls_R_factor_gt           0.0299
_refine_ls_wR_factor_ref         0.0809
_refine_ls_wR_factor_gt          0.0782
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_restrained_S_all      1.060
_refine_ls_shift/su_max          0.024
_refine_ls_shift/su_mean         0.001

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 0.40941(2) 0.90254(3) 0.461141(19) 0.01832(9) Uani 1 1 d U . .
Co2 Co 0.50410(2) 1.01046(3) 0.292346(19) 0.01807(9) Uani 1 1 d . . .
O1 O 0.30172(12) 1.03083(14) 0.37160(11) 0.0261(3) Uani 1 1 d . . .
O1W O 0.49724(15) 0.73387(18) 0.54080(13) 0.0344(4) Uani 0.90 1 d PU . .
H1WA H 0.4545 0.6730 0.5332 0.052 Uiso 0.90 1 d PR . .
H1WB H 0.5255 0.7500 0.6017 0.052 Uiso 0.90 1 d PR . .
O2 O 0.38877(12) 1.13630(14) 0.29235(12) 0.0261(3) Uani 1 1 d . . .
O2W O 0.48134(14) 1.09614(18) 0.15192(12) 0.0390(4) Uani 1 1 d . . .
H2WA H 0.5402 1.1242 0.1507 0.058 Uiso 1 1 d R . .
H2WB H 0.4375 1.1566 0.1422 0.058 Uiso 1 1 d R . .
O3 O 0.38447(13) 1.40418(15) 0.23928(13) 0.0321(4) Uani 1 1 d . . .
O4 O 0.31142(13) 1.28408(18) 0.10944(12) 0.0363(4) Uani 1 1 d . . .
O5 O -0.36636(11) 1.27725(14) 0.15496(10) 0.0232(3) Uani 1 1 d . . .
O6 O -0.37018(11) 1.39602(14) 0.27882(11) 0.0231(3) Uani 1 1 d . . .
O7 O -0.37858(12) 1.14716(16) 0.34224(11) 0.0288(4) Uani 1 1 d . . .
O8 O -0.28447(12) 1.15317(16) 0.50142(11) 0.0275(4) Uani 1 1 d . . .
O9 O 0.53886(10) 0.95816(13) 0.43238(10) 0.0190(3) Uani 1 1 d . . .
C3 C 0.31113(15) 1.11726(19) 0.31921(15) 0.0193(4) Uani 1 1 d . . .
C4 C 0.22301(16) 1.2096(2) 0.28510(15) 0.0216(4) Uani 1 1 d . . .
C5 C 0.13865(16) 1.1959(2) 0.31731(16) 0.0244(5) Uani 1 1 d . . .
H5 H 0.1388 1.1301 0.3580 0.029 Uiso 1 1 calc R . .
C6 C 0.05419(16) 1.2777(2) 0.29054(16) 0.0242(5) Uani 1 1 d . . .
C7 C 0.05648(18) 1.3757(2) 0.22964(19) 0.0321(5) Uani 1 1 d . . .
H7 H 0.0012 1.4319 0.2106 0.038 Uiso 1 1 calc R . .
C8 C 0.14014(18) 1.3906(2) 0.19701(19) 0.0319(5) Uani 1 1 d . . .
H8 H 0.1399 1.4567 0.1565 0.038 Uiso 1 1 calc R . .
C9 C 0.22444(16) 1.3082(2) 0.22402(16) 0.0238(4) Uani 1 1 d . . .
C10 C 0.31480(16) 1.3317(2) 0.18789(17) 0.0250(5) Uani 1 1 d . . .
C11 C -0.03455(16) 1.2588(2) 0.32628(16) 0.0227(4) Uani 1 1 d . . .
C12 C -0.13718(16) 1.2938(2) 0.26968(16) 0.0228(4) Uani 1 1 d . . .
H12 H -0.1497 1.3328 0.2103 0.027 Uiso 1 1 calc R . .
C13 C -0.22048(15) 1.27067(19) 0.30137(14) 0.0190(4) Uani 1 1 d . . .
C14 C -0.20311(16) 1.20917(19) 0.38915(15) 0.0195(4) Uani 1 1 d . . .
C15 C -0.10104(16) 1.1787(2) 0.44720(15) 0.0237(4) Uani 1 1 d . . .
H15 H -0.0885 1.1416 0.5073 0.028 Uiso 1 1 calc R . .
C16 C -0.01772(16) 1.2030(2) 0.41637(16) 0.0246(5) Uani 1 1 d . . .
H16 H 0.0503 1.1820 0.4560 0.030 Uiso 1 1 calc R . .
C17 C -0.32856(15) 1.31693(19) 0.24067(15) 0.0190(4) Uani 1 1 d . . .
C18 C -0.29655(16) 1.16676(19) 0.41314(15) 0.0200(4) Uani 1 1 d . . .
N1 N 0.2516(2) 0.0383(3) 0.05511(19) 0.0562(7) Uani 1 1 d . . .
H1A H 0.2891 -0.0085 0.1062 0.067 Uiso 1 1 calc R . .
H1B H 0.2717 0.1174 0.0695 0.067 Uiso 1 1 calc R . .
C1 C 0.1404(3) 0.0275(4) 0.0417(3) 0.0790(13) Uani 1 1 d . . .
H1C H 0.0998 0.0781 -0.0121 0.119 Uiso 1 1 calc R . .
H1D H 0.1293 0.0543 0.0996 0.119 Uiso 1 1 calc R . .
H1E H 0.1188 -0.0572 0.0286 0.119 Uiso 1 1 calc R . .
C2 C 0.2772(4) -0.0002(4) -0.0319(3) 0.0838(13) Uani 1 1 d . . .
H2A H 0.2411 0.0528 -0.0858 0.126 Uiso 1 1 calc R . .
H2B H 0.2553 -0.0841 -0.0484 0.126 Uiso 1 1 calc R . .
H2C H 0.3517 0.0062 -0.0174 0.126 Uiso 1 1 calc R . .


_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 O9 2.0386(14) . ?
Co1 O8 2.0503(15) 3_576 ?
Co1 O5 2.0952(15) 2_545 ?
Co1 O9 2.1072(14) 3_676 ?
Co1 O1 2.1075(15) . ?
Co1 O1W 2.2670(19) . ?
Co2 O9 2.0243(14) . ?
Co2 O2 2.0753(15) . ?
Co2 O3 2.0795(16) 2_645 ?
Co2 O7 2.1071(15) 1_655 ?
Co2 O6 2.1435(15) 2_545 ?
Co2 O2W 2.1837(17) . ?
O1 C3 1.246(3) . ?
O2 C3 1.266(2) . ?
O3 C10 1.256(3) . ?
O3 Co2 2.0795(15) 2_655 ?
O4 C10 1.249(3) . ?
O5 C17 1.257(2) . ?
O5 Co1 2.0952(15) 2 ?
O6 C17 1.261(3) . ?
O6 Co2 2.1435(14) 2 ?
O7 C18 1.247(3) . ?
O7 Co2 2.1071(15) 1_455 ?
O8 C18 1.258(3) . ?
O8 Co1 2.0503(15) 3_576 ?
O9 Co1 2.1072(14) 3_676 ?
C3 C4 1.503(3) . ?
C4 C5 1.393(3) . ?
C4 C9 1.398(3) . ?
C5 C6 1.391(3) . ?
C6 C7 1.395(3) . ?
C6 C11 1.489(3) . ?
C7 C8 1.390(3) . ?
C8 C9 1.394(3) . ?
C9 C10 1.521(3) . ?
C11 C16 1.399(3) . ?
C11 C12 1.400(3) . ?
C12 C13 1.389(3) . ?
C13 C14 1.396(3) . ?
C13 C17 1.509(3) . ?
C14 C15 1.388(3) . ?
C14 C18 1.504(3) . ?
C15 C16 1.385(3) . ?
N1 C1 1.458(4) . ?
N1 C2 1.499(5) . ?

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
O9 Co1 O8 176.63(6) . 3_576 ?
O9 Co1 O5 92.03(6) . 2_545 ?
O8 Co1 O5 90.51(6) 3_576 2_545 ?
O9 Co1 O9 81.77(6) . 3_676 ?
O8 Co1 O9 95.83(6) 3_576 3_676 ?
O5 Co1 O9 172.86(6) 2_545 3_676 ?
O9 Co1 O1 97.79(6) . . ?
O8 Co1 O1 84.46(6) 3_576 . ?
O5 Co1 O1 89.08(6) 2_545 . ?
O9 Co1 O1 88.26(6) 3_676 . ?
O9 Co1 O1W 90.54(7) . . ?
O8 Co1 O1W 87.67(7) 3_576 . ?
O5 Co1 O1W 81.10(6) 2_545 . ?
O9 Co1 O1W 102.39(6) 3_676 . ?
O1 Co1 O1W 167.36(7) . . ?
O9 Co2 O2 95.10(6) . . ?
O9 Co2 O3 98.37(6) . 2_645 ?
O2 Co2 O3 166.28(7) . 2_645 ?
O9 Co2 O7 88.01(6) . 1_655 ?
O2 Co2 O7 91.03(7) . 1_655 ?
O3 Co2 O7 86.86(7) 2_645 1_655 ?
O9 Co2 O6 100.89(6) . 2_545 ?
O2 Co2 O6 82.43(6) . 2_545 ?
O3 Co2 O6 97.51(6) 2_645 2_545 ?
O7 Co2 O6 169.35(6) 1_655 2_545 ?
O9 Co2 O2W 170.08(7) . . ?
O2 Co2 O2W 82.31(7) . . ?
O3 Co2 O2W 83.97(7) 2_645 . ?
O7 Co2 O2W 82.48(6) 1_655 . ?
O6 Co2 O2W 88.30(6) 2_545 . ?
C3 O1 Co1 132.88(14) . . ?
C3 O2 Co2 127.21(14) . . ?
C10 O3 Co2 131.61(15) . 2_655 ?
C17 O5 Co1 119.61(14) . 2 ?
C17 O6 Co2 127.67(13) . 2 ?
C18 O7 Co2 138.92(14) . 1_455 ?
C18 O8 Co1 119.46(13) . 3_576 ?
Co2 O9 Co1 112.60(6) . . ?
Co2 O9 Co1 116.94(7) . 3_676 ?
Co1 O9 Co1 98.23(6) . 3_676 ?
O1 C3 O2 126.35(19) . . ?
O1 C3 C4 117.52(18) . . ?
O2 C3 C4 116.13(18) . . ?
C5 C4 C9 119.89(19) . . ?
C5 C4 C3 118.00(19) . . ?
C9 C4 C3 122.11(18) . . ?
C6 C5 C4 122.1(2) . . ?
C5 C6 C7 117.52(19) . . ?
C5 C6 C11 120.17(19) . . ?
C7 C6 C11 122.3(2) . . ?
C8 C7 C6 121.0(2) . . ?
C7 C8 C9 121.1(2) . . ?
C8 C9 C4 118.33(19) . . ?
C8 C9 C10 118.47(19) . . ?
C4 C9 C10 123.18(19) . . ?
O4 C10 O3 126.0(2) . . ?
O4 C10 C9 118.8(2) . . ?
O3 C10 C9 115.1(2) . . ?
C16 C11 C12 118.39(19) . . ?
C16 C11 C6 120.71(19) . . ?
C12 C11 C6 120.89(19) . . ?
C13 C12 C11 120.65(19) . . ?
C12 C13 C14 120.21(18) . . ?
C12 C13 C17 118.64(18) . . ?
C14 C13 C17 121.12(17) . . ?
C15 C14 C13 119.26(19) . . ?
C15 C14 C18 121.73(18) . . ?
C13 C14 C18 118.72(18) . . ?
C16 C15 C14 120.5(2) . . ?
C15 C16 C11 120.82(19) . . ?
O5 C17 O6 126.08(19) . . ?
O5 C17 C13 116.63(18) . . ?
O6 C17 C13 117.19(18) . . ?
O7 C18 O8 126.58(19) . . ?
O7 C18 C14 115.80(18) . . ?
O8 C18 C14 117.62(18) . . ?
C1 N1 C2 113.8(3) . . ?

_diffrn_measured_fraction_theta_max 0.991
_diffrn_reflns_theta_full        26.37
_diffrn_measured_fraction_theta_full 0.991
_refine_diff_density_max         0.716
_refine_diff_density_min         -0.357
_refine_diff_density_rms         0.075
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_1a
_database_code_depnum_ccdc_archive 'CCDC 1059845'
_audit_update_record             
;
2015-05-14 deposited with the CCDC.
2015-05-27 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C17.75 H16.72 Co2 N O10.13'
_chemical_formula_weight         524.02

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'
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'

_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                   13.5497(7)
_cell_length_b                   10.8567(4)
_cell_length_c                   14.6263(7)
_cell_angle_alpha                90.00
_cell_angle_beta                 109.784(6)
_cell_angle_gamma                90.00
_cell_volume                     2024.60(16)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    3571
_cell_measurement_theta_min      2.8425
_cell_measurement_theta_max      28.9756

_exptl_crystal_description       plate
_exptl_crystal_colour            purple
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.16
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.719
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1061
_exptl_absorpt_coefficient_mu    1.696
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6669
_exptl_absorpt_correction_T_max  0.7731
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_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  'Xcalibur, Eos, Gemini'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            7999
_diffrn_reflns_av_R_equivalents  0.0260
_diffrn_reflns_av_sigmaI/netI    0.0432
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_theta_min         2.85
_diffrn_reflns_theta_max         26.37
_reflns_number_total             4147
_reflns_number_gt                3735
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET)
(compiled Jul 11 2012,15:38:31)
;
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET)
(compiled Jul 11 2012,15:38:31)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET)
(compiled Jul 11 2012,15:38:31)
;
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_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)+(0.0000P)²+19.3694P] 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         4147
_refine_ls_number_parameters     299
_refine_ls_number_restraints     5
_refine_ls_R_factor_all          0.0767
_refine_ls_R_factor_gt           0.0706
_refine_ls_wR_factor_ref         0.1596
_refine_ls_wR_factor_gt          0.1574
_refine_ls_goodness_of_fit_ref   1.293
_refine_ls_restrained_S_all      1.292
_refine_ls_shift/su_max          0.021
_refine_ls_shift/su_mean         0.001

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 0.403598(18) 0.91509(3) 0.457131(17) 0.01938(6) Uani 1 1 d U . .
Co2 Co 0.504781(17) 1.02144(2) 0.294754(17) 0.01782(6) Uani 1 1 d . . .
O1 O 0.29680(10) 1.03794(13) 0.36946(9) 0.0186(4) Uani 0.90 1 d PU . .
O1W O 0.4959(4) 0.7327(5) 0.5395(3) 0.0400(15) Uani 0.33 1 d PG . .
H1WA H 0.4983 0.6663 0.5709 0.060 Uiso 0.33 1 d PG . .
H1WB H 0.5515 0.7740 0.5663 0.060 Uiso 0.33 1 d PG . .
O2 O 0.39120(9) 1.14730(13) 0.29933(11) 0.0303(4) Uani 1 1 d . . .
O2W O 0.48142(11) 1.10694(15) 0.15552(10) 0.0273(4) Uani 0.90 1 d P . .
H2WA H 0.4811 1.0515 0.1144 0.041 Uiso 0.90 1 d PR . .
H2WB H 0.5309 1.1575 0.1606 0.041 Uiso 0.90 1 d PR . .
O3 O 0.37994(10) 1.42022(15) 0.23512(10) 0.0324(4) Uani 1 1 d U . .
O4 O 0.31740(10) 1.28750(14) 0.11241(10) 0.0305(4) Uani 1 1 d . . .
O5 O -0.36693(9) 1.28409(12) 0.15489(9) 0.0209(4) Uani 1 1 d . . .
O6 O -0.37223(9) 1.40562(12) 0.27721(9) 0.0208(3) Uani 1 1 d U . .
O7 O -0.38351(10) 1.16122(14) 0.34814(10) 0.0338(4) Uani 1 1 d . . .
O8 O -0.28501(10) 1.15399(14) 0.50453(9) 0.0275(4) Uani 1 1 d . . .
O9 O 0.53840(8) 0.95638(11) 0.43331(8) 0.0157(3) Uani 1 1 d . . .
C3 C 0.31033(13) 1.12697(18) 0.32111(13) 0.0198(5) Uani 1 1 d . . .
C4 C 0.22212(13) 1.21774(18) 0.28523(13) 0.0192(5) Uani 1 1 d . . .
C5 C 0.13632(13) 1.20416(18) 0.31635(13) 0.0206(5) Uani 1 1 d . . .
H5 H 0.1355 1.1386 0.3570 0.025 Uiso 1 1 calc R . .
C6 C 0.05165(13) 1.28536(19) 0.28874(14) 0.0235(5) Uani 1 1 d . . .
C7 C 0.05525(14) 1.38263(19) 0.22808(15) 0.0296(6) Uani 1 1 d . . .
H7 H 0.0000 1.4385 0.2087 0.035 Uiso 1 1 calc R . .
C8 C 0.13960(14) 1.39770(19) 0.19614(15) 0.0289(5) Uani 1 1 d . . .
H8 H 0.1400 1.4634 0.1554 0.035 Uiso 1 1 calc R . .
C9 C 0.22458(13) 1.31568(17) 0.22406(13) 0.0200(5) Uani 1 1 d . . .
C10 C 0.31566(13) 1.34098(18) 0.18794(13) 0.0222(5) Uani 1 1 d U . .
C11 C -0.03751(13) 1.26643(18) 0.32567(13) 0.0210(5) Uani 1 1 d . . .
C12 C -0.13953(13) 1.30092(18) 0.26957(13) 0.0213(5) Uani 1 1 d . . .
H12 H -0.1516 1.3394 0.2100 0.026 Uiso 1 1 calc R . .
C13 C -0.22295(13) 1.27824(16) 0.30199(12) 0.0166(5) Uani 1 1 d U . .
C14 C -0.20682(13) 1.21686(17) 0.39036(12) 0.0171(5) Uani 1 1 d . . .
C15 C -0.10486(13) 1.18574(18) 0.44722(13) 0.0210(5) Uani 1 1 d . . .
H15 H -0.0927 1.1480 0.5071 0.025 Uiso 1 1 calc R . .
C16 C -0.02099(13) 1.21036(19) 0.41574(13) 0.0239(5) Uani 1 1 d . . .
H16 H 0.0467 1.1894 0.4549 0.029 Uiso 1 1 calc R . .
C17 C -0.33081(13) 1.32407(17) 0.24038(12) 0.0177(5) Uani 1 1 d U . .
C18 C -0.29905(13) 1.17488(17) 0.41692(13) 0.0195(5) Uani 1 1 d . . .
N1 N 0.25952(19) 0.0406(2) 0.05386(18) 0.0641(9) Uani 1 1 d . . .
H1A H 0.2803 0.1191 0.0687 0.077 Uiso 1 1 calc R . .
H1B H 0.2948 -0.0064 0.1052 0.077 Uiso 1 1 calc R . .
C1 C 0.1448(3) 0.0320(3) 0.0388(3) 0.0933(15) Uani 1 1 d . . .
H1C H 0.1056 0.0732 -0.0204 0.140 Uiso 1 1 calc R . .
H1D H 0.1309 0.0704 0.0924 0.140 Uiso 1 1 calc R . .
H1E H 0.1243 -0.0530 0.0349 0.140 Uiso 1 1 calc R . .
C2 C 0.2888(3) 0.0018(4) -0.0310(2) 0.0613(14) Uani 0.75 1 d P . .
H2A H 0.2593 0.0582 -0.0838 0.092 Uiso 0.75 1 calc PR . .
H2B H 0.2623 -0.0795 -0.0508 0.092 Uiso 0.75 1 calc PR . .
H2C H 0.3638 0.0015 -0.0134 0.092 Uiso 0.75 1 calc PR . .
H9 H 0.5852(15) 0.8977(19) 0.4418(14) 0.023(5) Uiso 1 1 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 O8 2.0171(15) 3_576 ?
Co1 O9 2.0222(13) . ?
Co1 O1 2.0643(13) . ?
Co1 O9 2.0689(12) 3_676 ?
Co1 O5 2.0983(13) 2_545 ?
Co2 O9 2.0466(12) . ?
Co2 O3 2.0737(16) 2_645 ?
Co2 O2 2.0761(14) . ?
Co2 O7 2.0985(14) 1_655 ?
Co2 O6 2.1529(12) 2_545 ?
Co2 O2W 2.1617(16) . ?
O1 C3 1.247(2) . ?
O2 C3 1.260(2) . ?
O3 C10 1.252(2) . ?
O3 Co2 2.0737(16) 2_655 ?
O4 C10 1.255(3) . ?
O5 C17 1.256(2) . ?
O5 Co1 2.0983(13) 2 ?
O6 C17 1.262(2) . ?
O6 Co2 2.1529(12) 2 ?
O7 C18 1.251(2) . ?
O7 Co2 2.0985(14) 1_455 ?
O8 C18 1.251(2) . ?
O8 Co1 2.0171(15) 3_576 ?
O9 Co1 2.0689(12) 3_676 ?
C3 C4 1.500(2) . ?
C4 C5 1.392(3) . ?
C4 C9 1.397(3) . ?
C5 C6 1.394(3) . ?
C6 C7 1.391(3) . ?
C6 C11 1.495(3) . ?
C7 C8 1.383(3) . ?
C8 C9 1.403(3) . ?
C9 C10 1.523(3) . ?
C11 C12 1.399(2) . ?
C11 C16 1.399(3) . ?
C12 C13 1.388(3) . ?
C13 C14 1.404(3) . ?
C13 C17 1.518(2) . ?
C14 C15 1.392(2) . ?
C14 C18 1.500(3) . ?
C15 C16 1.389(3) . ?
N1 C2 1.487(5) . ?
N1 C1 1.498(4) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O8 Co1 O9 168.89(5) 3_576 . ?
O8 Co1 O1 87.48(6) 3_576 . ?
O9 Co1 O1 103.53(5) . . ?
O8 Co1 O9 99.50(5) 3_576 3_676 ?
O9 Co1 O9 81.69(6) . 3_676 ?
O1 Co1 O9 92.75(5) . 3_676 ?
O8 Co1 O5 87.98(6) 3_576 2_545 ?
O9 Co1 O5 90.27(5) . 2_545 ?
O1 Co1 O5 91.26(5) . 2_545 ?
O9 Co1 O5 171.66(5) 3_676 2_545 ?
O9 Co2 O3 95.43(5) . 2_645 ?
O9 Co2 O2 96.56(6) . . ?
O3 Co2 O2 167.18(6) 2_645 . ?
O9 Co2 O7 89.45(5) . 1_655 ?
O3 Co2 O7 87.81(6) 2_645 1_655 ?
O2 Co2 O7 87.78(6) . 1_655 ?
O9 Co2 O6 98.73(5) . 2_545 ?
O3 Co2 O6 98.67(5) 2_645 2_545 ?
O2 Co2 O6 83.99(5) . 2_545 ?
O7 Co2 O6 168.99(5) 1_655 2_545 ?
O9 Co2 O2W 173.53(5) . . ?
O3 Co2 O2W 84.81(6) 2_645 . ?
O2 Co2 O2W 82.76(6) . . ?
O7 Co2 O2W 84.10(6) 1_655 . ?
O6 Co2 O2W 87.61(5) 2_545 . ?
C3 O1 Co1 130.26(12) . . ?
C3 O2 Co2 127.63(13) . . ?
C10 O3 Co2 132.92(14) . 2_655 ?
C17 O5 Co1 116.92(12) . 2 ?
C17 O6 Co2 128.23(10) . 2 ?
C18 O7 Co2 137.17(13) . 1_455 ?
C18 O8 Co1 119.54(11) . 3_576 ?
Co1 O9 Co2 109.62(5) . . ?
Co1 O9 Co1 98.31(6) . 3_676 ?
Co2 O9 Co1 115.66(6) . 3_676 ?
O1 C3 O2 125.90(17) . . ?
O1 C3 C4 117.06(17) . . ?
O2 C3 C4 117.04(17) . . ?
C5 C4 C9 119.57(16) . . ?
C5 C4 C3 118.07(17) . . ?
C9 C4 C3 122.34(17) . . ?
C4 C5 C6 122.32(18) . . ?
C7 C6 C5 117.52(19) . . ?
C7 C6 C11 122.82(17) . . ?
C5 C6 C11 119.66(18) . . ?
C8 C7 C6 121.11(18) . . ?
C7 C8 C9 121.16(19) . . ?
C4 C9 C8 118.32(18) . . ?
C4 C9 C10 123.86(16) . . ?
C8 C9 C10 117.80(17) . . ?
O3 C10 O4 125.9(2) . . ?
O3 C10 C9 115.28(18) . . ?
O4 C10 C9 118.74(16) . . ?
C12 C11 C16 118.71(18) . . ?
C12 C11 C6 120.68(17) . . ?
C16 C11 C6 120.59(15) . . ?
C13 C12 C11 120.63(17) . . ?
C12 C13 C14 120.52(15) . . ?
C12 C13 C17 118.09(16) . . ?
C14 C13 C17 121.38(17) . . ?
C15 C14 C13 118.63(18) . . ?
C15 C14 C18 121.14(16) . . ?
C13 C14 C18 119.94(14) . . ?
C16 C15 C14 120.89(17) . . ?
C15 C16 C11 120.53(15) . . ?
O5 C17 O6 125.98(15) . . ?
O5 C17 C13 116.76(17) . . ?
O6 C17 C13 117.02(14) . . ?
O8 C18 O7 125.66(19) . . ?
O8 C18 C14 118.00(14) . . ?
O7 C18 C14 116.33(17) . . ?
C2 N1 C1 114.6(3) . . ?

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        26.37
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         1.202
_refine_diff_density_min         -0.891
_refine_diff_density_rms         0.124
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_2
_database_code_depnum_ccdc_archive 'CCDC 1059846'
_audit_update_record             
;
2015-05-14 deposited with the CCDC.
2015-05-27 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C17.50 H15.50 Co2 N0.75 O9.75'
_chemical_formula_weight         510.17

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'
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'

_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                   13.4701(13)
_cell_length_b                   10.8298(6)
_cell_length_c                   14.6883(11)
_cell_angle_alpha                90.00
_cell_angle_beta                 109.830(10)
_cell_angle_gamma                90.00
_cell_volume                     2015.7(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    2580
_cell_measurement_theta_min      3.4210
_cell_measurement_theta_max      28.6670

_exptl_crystal_description       plate
_exptl_crystal_colour            purple
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.16
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.681
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1031
_exptl_absorpt_coefficient_mu    1.699
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6664
_exptl_absorpt_correction_T_max  0.7727
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;

_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  'Xcalibur, Eos, Gemini'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            8111
_diffrn_reflns_av_R_equivalents  0.0295
_diffrn_reflns_av_sigmaI/netI    0.0506
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         2.95
_diffrn_reflns_theta_max         26.37
_reflns_number_total             4112
_reflns_number_gt                3459
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_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)+(0.0324P)²+11.4182P] 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         4112
_refine_ls_number_parameters     291
_refine_ls_number_restraints     9
_refine_ls_R_factor_all          0.0790
_refine_ls_R_factor_gt           0.0657
_refine_ls_wR_factor_ref         0.1573
_refine_ls_wR_factor_gt          0.1518
_refine_ls_goodness_of_fit_ref   1.264
_refine_ls_restrained_S_all      1.263
_refine_ls_shift/su_max          0.012
_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 0.40150(6) 0.91712(8) 0.45566(6) 0.0213(2) Uani 1 1 d . . .
Co2 Co 0.50557(6) 1.02088(8) 0.29887(6) 0.0218(2) Uani 1 1 d . . .
O1 O 0.2965(4) 1.0387(4) 0.3680(3) 0.0339(11) Uani 1 1 d . . .
O2 O 0.3916(3) 1.1468(4) 0.2970(4) 0.0397(12) Uani 1 1 d . . .
O2W O 0.4803(5) 1.1072(7) 0.1565(5) 0.0433(16) Uani 0.75 1 d P . .
H2WA H 0.4518 1.0540 0.1088 0.065 Uiso 0.75 1 d PRU . .
H2WB H 0.5403 1.1333 0.1507 0.065 Uiso 0.75 1 d PRU . .
O3 O 0.3805(3) 1.4243(4) 0.2345(3) 0.0346(11) Uani 1 1 d . . .
O4 O 0.3155(4) 1.2915(5) 0.1115(4) 0.0413(12) Uani 1 1 d . . .
O5 O -0.3671(3) 1.2839(4) 0.1541(3) 0.0264(9) Uani 1 1 d . . .
O6 O -0.3756(3) 1.4051(4) 0.2754(3) 0.0252(9) Uani 1 1 d . . .
O7 O -0.3852(3) 1.1624(4) 0.3502(3) 0.0360(11) Uani 1 1 d . . .
O8 O -0.2855(4) 1.1559(5) 0.5050(3) 0.0427(13) Uani 1 1 d . . .
O9 O 0.5403(3) 0.9539(4) 0.4364(3) 0.0220(9) Uani 1 1 d . . .
C3 C 0.3106(4) 1.1283(5) 0.3198(4) 0.0227(12) Uani 1 1 d . . .
C4 C 0.2223(5) 1.2202(6) 0.2848(4) 0.0252(13) Uani 1 1 d . . .
C5 C 0.1364(4) 1.2064(6) 0.3163(4) 0.0253(13) Uani 1 1 d . . .
H5 H 0.1357 1.1399 0.3562 0.030 Uiso 1 1 calc R . .
C6 C 0.0518(4) 1.2875(6) 0.2907(4) 0.0245(12) Uani 1 1 d . . .
C7 C 0.0548(5) 1.3869(6) 0.2298(5) 0.0338(15) Uani 1 1 d . . .
H7 H -0.0010 1.4427 0.2108 0.041 Uiso 1 1 calc R . .
C8 C 0.1389(5) 1.4029(6) 0.1979(5) 0.0358(16) Uani 1 1 d . . .
H8 H 0.1396 1.4695 0.1581 0.043 Uiso 1 1 calc R . .
C9 C 0.2245(5) 1.3188(5) 0.2249(4) 0.0254(13) Uani 1 1 d . . .
C10 C 0.3154(5) 1.3442(6) 0.1877(4) 0.0279(13) Uani 1 1 d . . .
C11 C -0.0376(4) 1.2687(6) 0.3271(4) 0.0250(13) Uani 1 1 d . . .
C12 C -0.1397(5) 1.3011(5) 0.2710(4) 0.0250(13) Uani 1 1 d . . .
H12 H -0.1516 1.3387 0.2113 0.030 Uiso 1 1 calc R . .
C13 C -0.2248(4) 1.2786(5) 0.3023(4) 0.0196(11) Uani 1 1 d . . .
C14 C -0.2081(5) 1.2189(5) 0.3906(4) 0.0220(12) Uani 1 1 d . . .
C15 C -0.1052(5) 1.1893(6) 0.4487(4) 0.0275(13) Uani 1 1 d . . .
H15 H -0.0930 1.1528 0.5089 0.033 Uiso 1 1 calc R . .
C16 C -0.0212(5) 1.2139(6) 0.4173(4) 0.0279(13) Uani 1 1 d . . .
H16 H 0.0470 1.1938 0.4567 0.033 Uiso 1 1 calc R . .
C17 C -0.3317(4) 1.3234(5) 0.2400(4) 0.0209(12) Uani 1 1 d . . .
C18 C -0.3003(5) 1.1759(5) 0.4178(4) 0.0226(12) Uani 1 1 d . . .
N1 N 0.2670(11) 1.0431(8) 0.0560(7) 0.082(4) Uani 0.75 1 d P . .
H1A H 0.2888 1.1219 0.0680 0.099 Uiso 0.75 1 calc PRU . .
H1B H 0.3051 0.9961 0.1062 0.099 Uiso 0.75 1 calc PRU . .
C1 C 0.1423(12) 1.0324(13) 0.0408(13) 0.101(6) Uani 0.75 1 d P . .
H1C H 0.1220 0.9470 0.0357 0.152 Uiso 0.75 1 calc PRU . .
H1D H 0.1021 1.0749 -0.0173 0.152 Uiso 0.75 1 calc PRU . .
H1E H 0.1289 1.0688 0.0951 0.152 Uiso 0.75 1 calc PRU . .
C2 C 0.2787(14) 1.0042(13) -0.0251(9) 0.092(5) Uani 0.75 1 d P . .
H2A H 0.2373 1.0549 -0.0780 0.138 Uiso 0.75 1 calc PRU . .
H2C H 0.2555 0.9200 -0.0369 0.138 Uiso 0.75 1 calc PRU . .
H2B H 0.3517 1.0094 -0.0194 0.138 Uiso 0.75 1 calc PRU . .
H9A H 0.570(8) 0.906(10) 0.436(7) 0.08(3) Uiso 1 1 d U . .
H9B H 0.559(8) 1.035(10) 0.465(7) 0.09(3) Uiso 1 1 d U . .


_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 O8 2.003(4) 3_576 ?
Co1 O9 2.023(4) . ?
Co1 O1 2.039(4) . ?
Co1 O9 2.058(4) 3_676 ?
Co1 O5 2.096(4) 2_545 ?
Co2 O9 2.046(4) . ?
Co2 O2 2.047(4) . ?
Co2 O3 2.050(4) 2_645 ?
Co2 O7 2.081(4) 1_655 ?
Co2 O6 2.129(4) 2_545 ?
Co2 O2W 2.210(6) . ?
O1 C3 1.253(7) . ?
O2 C3 1.261(7) . ?
O3 C10 1.259(8) . ?
O3 Co2 2.050(4) 2_655 ?
O4 C10 1.257(7) . ?
O5 C17 1.262(7) . ?
O5 Co1 2.096(4) 2 ?
O6 C17 1.270(7) . ?
O6 Co2 2.129(4) 2 ?
O7 C18 1.242(7) . ?
O7 Co2 2.081(4) 1_455 ?
O8 C18 1.247(7) . ?
O8 Co1 2.003(4) 3_576 ?
O9 Co1 2.058(4) 3_676 ?
C3 C4 1.501(8) . ?
C4 C9 1.391(8) . ?
C4 C5 1.392(8) . ?
C5 C6 1.386(8) . ?
C6 C7 1.410(8) . ?
C6 C11 1.489(7) . ?
C7 C8 1.376(8) . ?
C8 C9 1.416(8) . ?
C9 C10 1.526(8) . ?
C11 C12 1.387(8) . ?
C11 C16 1.399(8) . ?
C12 C13 1.393(7) . ?
C13 C14 1.397(8) . ?
C13 C17 1.501(8) . ?
C14 C15 1.396(8) . ?
C14 C18 1.502(7) . ?
C15 C16 1.386(8) . ?
N1 C2 1.323(17) . ?
N1 C1 1.623(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
O8 Co1 O9 165.1(2) 3_576 . ?
O8 Co1 O1 89.7(2) 3_576 . ?
O9 Co1 O1 105.11(18) . . ?
O8 Co1 O9 100.17(18) 3_576 3_676 ?
O9 Co1 O9 81.08(18) . 3_676 ?
O1 Co1 O9 92.85(18) . 3_676 ?
O8 Co1 O5 87.70(18) 3_576 2_545 ?
O9 Co1 O5 90.10(17) . 2_545 ?
O1 Co1 O5 91.94(18) . 2_545 ?
O9 Co1 O5 170.80(16) 3_676 2_545 ?
O9 Co2 O2 99.69(19) . . ?
O9 Co2 O3 96.71(18) . 2_645 ?
O2 Co2 O3 162.95(19) . 2_645 ?
O9 Co2 O7 90.39(17) . 1_655 ?
O2 Co2 O7 87.11(19) . 1_655 ?
O3 Co2 O7 88.15(19) 2_645 1_655 ?
O9 Co2 O6 99.80(16) . 2_545 ?
O2 Co2 O6 84.41(17) . 2_545 ?
O3 Co2 O6 97.40(17) 2_645 2_545 ?
O7 Co2 O6 167.70(17) 1_655 2_545 ?
O9 Co2 O2W 174.3(2) . . ?
O2 Co2 O2W 80.3(2) . . ?
O3 Co2 O2W 82.9(2) 2_645 . ?
O7 Co2 O2W 83.9(2) 1_655 . ?
O6 Co2 O2W 85.9(2) 2_545 . ?
C3 O1 Co1 130.6(4) . . ?
C3 O2 Co2 127.1(4) . . ?
C10 O3 Co2 131.3(4) . 2_655 ?
C17 O5 Co1 116.4(4) . 2 ?
C17 O6 Co2 128.1(4) . 2 ?
C18 O7 Co2 136.2(4) . 1_455 ?
C18 O8 Co1 119.7(4) . 3_576 ?
Co1 O9 Co2 107.2(2) . . ?
Co1 O9 Co1 98.92(17) . 3_676 ?
Co2 O9 Co1 114.8(2) . 3_676 ?
O1 C3 O2 125.7(5) . . ?
O1 C3 C4 116.9(5) . . ?
O2 C3 C4 117.4(5) . . ?
C9 C4 C5 119.4(5) . . ?
C9 C4 C3 122.7(5) . . ?
C5 C4 C3 117.8(5) . . ?
C6 C5 C4 122.8(5) . . ?
C5 C6 C7 117.3(5) . . ?
C5 C6 C11 120.4(5) . . ?
C7 C6 C11 122.3(5) . . ?
C8 C7 C6 121.1(6) . . ?
C7 C8 C9 120.6(6) . . ?
C4 C9 C8 118.8(5) . . ?
C4 C9 C10 123.9(5) . . ?
C8 C9 C10 117.3(5) . . ?
O4 C10 O3 126.0(5) . . ?
O4 C10 C9 118.8(6) . . ?
O3 C10 C9 115.1(5) . . ?
C12 C11 C16 118.5(5) . . ?
C12 C11 C6 120.8(5) . . ?
C16 C11 C6 120.7(5) . . ?
C11 C12 C13 121.4(5) . . ?
C12 C13 C14 119.7(5) . . ?
C12 C13 C17 117.9(5) . . ?
C14 C13 C17 122.3(5) . . ?
C15 C14 C13 119.2(5) . . ?
C15 C14 C18 120.3(5) . . ?
C13 C14 C18 120.2(5) . . ?
C16 C15 C14 120.4(5) . . ?
C15 C16 C11 120.8(6) . . ?
O5 C17 O6 125.1(5) . . ?
O5 C17 C13 117.3(5) . . ?
O6 C17 C13 117.3(5) . . ?
O7 C18 O8 125.8(5) . . ?
O7 C18 C14 116.3(5) . . ?
O8 C18 C14 117.9(5) . . ?
C2 N1 C1 106.7(12) . . ?

_diffrn_measured_fraction_theta_max 0.996
_diffrn_reflns_theta_full        26.37
_diffrn_measured_fraction_theta_full 0.996
_refine_diff_density_max         1.340
_refine_diff_density_min         -0.514
_refine_diff_density_rms         0.123

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