# 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_1

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C7 H18 Co2 N3 O12 S'
_chemical_formula_weight         486.16

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'
S S 0.1246 0.1234 '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           triclinic
_symmetry_space_group_name_H-M   P-1

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   8.6065(3)
_cell_length_b                   9.5595(5)
_cell_length_c                   9.5987(5)
_cell_angle_alpha                77.884(4)
_cell_angle_beta                 82.744(4)
_cell_angle_gamma                87.356(4)
_cell_volume                     765.79(6)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    3415
_cell_measurement_theta_min      3.4210
_cell_measurement_theta_max      28.6590

_exptl_crystal_description       block
_exptl_crystal_colour            red
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.20
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.108
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             494
_exptl_absorpt_coefficient_mu    2.375
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.94783
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
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'
_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            5782
_diffrn_reflns_av_R_equivalents  0.0218
_diffrn_reflns_av_sigmaI/netI    0.0347
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_theta_min         3.20
_diffrn_reflns_theta_max         25.00
_reflns_number_total             2696
_reflns_number_gt                2374
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_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)+(0.0266P)²+0.2782P] 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         2696
_refine_ls_number_parameters     229
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0327
_refine_ls_R_factor_gt           0.0266
_refine_ls_wR_factor_ref         0.0638
_refine_ls_wR_factor_gt          0.0606
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_restrained_S_all      1.056
_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 0.34974(4) 0.09000(4) 0.23608(4) 0.01735(11) Uani 1 1 d . . .
Co2 Co 0.5000 0.5000 0.5000 0.01959(14) Uani 1 2 d S . .
Co3 Co 0.0000 0.5000 0.0000 0.01964(14) Uani 1 2 d S . .
S1 S 0.02013(7) 0.26796(7) 0.33143(7) 0.01587(15) Uani 1 1 d . . .
O1 O 0.1219(2) 0.1821(2) 0.2451(2) 0.0283(5) Uani 1 1 d . . .
O2 O -0.0350(2) 0.3958(2) 0.2366(2) 0.0326(5) Uani 1 1 d . . .
O3 O -0.1138(3) 0.1808(2) 0.4028(2) 0.0434(6) Uani 1 1 d . . .
O4 O 0.1048(2) 0.3092(2) 0.4396(2) 0.0282(5) Uani 1 1 d . . .
O5 O 0.5263(2) 0.4581(2) 0.29341(19) 0.0258(5) Uani 1 1 d . . .
O6 O 0.4576(2) 0.2897(2) 0.18403(19) 0.0258(5) Uani 1 1 d . . .
O7 O 0.4632(2) 0.27884(19) 0.54952(19) 0.0218(4) Uani 1 1 d . . .
O8 O 0.3956(2) 0.11277(19) 0.43728(19) 0.0216(4) Uani 1 1 d . . .
O9 O 0.5633(2) -0.0135(2) 0.16782(18) 0.0214(4) Uani 1 1 d . . .
O10 O 0.6801(2) -0.0879(2) -0.02615(19) 0.0231(4) Uani 1 1 d . . .
OW1 O 0.2798(2) -0.11984(19) 0.32748(19) 0.0237(4) Uani 1 1 d . . .
H1 H 0.2192 -0.1339 0.4054 0.036 Uiso 1 1 d R . .
H2 H 0.3611 -0.1708 0.3449 0.036 Uiso 1 1 d R . .
OW2 O 0.2588(2) 0.5340(2) 0.4949(2) 0.0362(5) Uani 1 1 d . . .
H3 H 0.2087 0.5580 0.5676 0.054 Uiso 1 1 d R . .
H4 H 0.2042 0.4722 0.4732 0.054 Uiso 1 1 d R . .
N2 N 0.0116(2) 0.7117(2) 0.0435(2) 0.0200(5) Uani 1 1 d . . .
H5 H -0.0354 0.7728 -0.0256 0.024 Uiso 1 1 calc R . .
N3 N -0.1661(2) 0.9153(2) 0.3240(2) 0.0222(5) Uani 1 1 d . . .
H6 H -0.1639 1.0069 0.3297 0.033 Uiso 1 1 calc R . .
H7 H -0.1328 0.8607 0.4020 0.033 Uiso 1 1 calc R . .
H8 H -0.2637 0.8925 0.3177 0.033 Uiso 1 1 calc R . .
N1 N 0.2427(3) 0.4981(3) 0.0038(2) 0.0255(5) Uani 1 1 d . . .
H9 H 0.2755 0.4129 0.0520 0.031 Uiso 1 1 calc R . .
H10 H 0.2927 0.5139 -0.0861 0.031 Uiso 1 1 calc R . .
C1 C 0.4785(3) 0.3364(3) 0.2929(3) 0.0194(6) Uani 1 1 d . . .
C2 C 0.4428(3) 0.2329(3) 0.4387(3) 0.0174(6) Uani 1 1 d . . .
C3 C 0.5701(3) -0.0296(3) 0.0416(3) 0.0169(6) Uani 1 1 d . . .
C4 C 0.2749(3) 0.6134(3) 0.0766(3) 0.0302(7) Uani 1 1 d . . .
H11 H 0.3857 0.6341 0.0599 0.036 Uiso 1 1 calc R . .
H12 H 0.2452 0.5841 0.1793 0.036 Uiso 1 1 calc R . .
C5 C 0.1812(3) 0.7442(3) 0.0172(3) 0.0274(7) Uani 1 1 d . . .
H13 H 0.2010 0.8219 0.0630 0.033 Uiso 1 1 calc R . .
H14 H 0.2126 0.7741 -0.0850 0.033 Uiso 1 1 calc R . .
C6 C -0.0647(3) 0.7360(3) 0.1827(3) 0.0226(6) Uani 1 1 d . . .
H15 H -0.0118 0.6779 0.2589 0.027 Uiso 1 1 calc R . .
H16 H -0.1724 0.7055 0.1959 0.027 Uiso 1 1 calc R . .
C7 C -0.0628(3) 0.8918(3) 0.1951(3) 0.0192(6) Uani 1 1 d . . .
H17 H 0.0433 0.9178 0.2012 0.023 Uiso 1 1 calc R . .
H18 H -0.0981 0.9523 0.1101 0.023 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 O10 2.0676(18) 2_655 ?
Co1 O8 2.0760(18) . ?
Co1 OW1 2.0964(19) . ?
Co1 O6 2.0977(19) . ?
Co1 O1 2.1108(17) . ?
Co1 O9 2.1419(17) . ?
Co2 O5 2.0871(18) . ?
Co2 O5 2.0871(18) 2_666 ?
Co2 OW2 2.0911(18) 2_666 ?
Co2 OW2 2.0911(18) . ?
Co2 O7 2.0971(18) . ?
Co2 O7 2.0971(18) 2_666 ?
Co3 N1 2.093(2) 2_565 ?
Co3 N1 2.093(2) . ?
Co3 N2 2.159(2) 2_565 ?
Co3 N2 2.159(2) . ?
Co3 O2 2.2685(19) 2_565 ?
Co3 O2 2.2685(19) . ?
S1 O2 1.462(2) . ?
S1 O3 1.463(2) . ?
S1 O4 1.468(2) . ?
S1 O1 1.4712(17) . ?
O5 C1 1.253(3) . ?
O6 C1 1.255(3) . ?
O7 C2 1.267(3) . ?
O8 C2 1.239(3) . ?
O9 C3 1.247(3) . ?
O10 C3 1.256(3) . ?
O10 Co1 2.0676(18) 2_655 ?
OW1 H1 0.8461 . ?
OW1 H2 0.8475 . ?
OW2 H3 0.8419 . ?
OW2 H4 0.8454 . ?
N2 C6 1.472(3) . ?
N2 C5 1.485(3) . ?
N2 H5 0.9100 . ?
N3 C7 1.481(3) . ?
N3 H6 0.8900 . ?
N3 H7 0.8900 . ?
N3 H8 0.8900 . ?
N1 C4 1.476(4) . ?
N1 H9 0.9000 . ?
N1 H10 0.9000 . ?
C1 C2 1.539(4) . ?
C3 C3 1.551(5) 2_655 ?
C4 C5 1.504(4) . ?
C4 H11 0.9700 . ?
C4 H12 0.9700 . ?
C5 H13 0.9700 . ?
C5 H14 0.9700 . ?
C6 C7 1.519(4) . ?
C6 H15 0.9700 . ?
C6 H16 0.9700 . ?
C7 H17 0.9700 . ?
C7 H18 0.9700 . ?

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
O10 Co1 O8 173.35(8) 2_655 . ?
O10 Co1 OW1 97.68(8) 2_655 . ?
O8 Co1 OW1 88.66(7) . . ?
O10 Co1 O6 94.21(7) 2_655 . ?
O8 Co1 O6 79.24(7) . . ?
OW1 Co1 O6 165.73(7) . . ?
O10 Co1 O1 84.40(7) 2_655 . ?
O8 Co1 O1 96.96(7) . . ?
OW1 Co1 O1 95.85(8) . . ?
O6 Co1 O1 93.12(8) . . ?
O10 Co1 O9 78.90(7) 2_655 . ?
O8 Co1 O9 99.98(7) . . ?
OW1 Co1 O9 83.49(7) . . ?
O6 Co1 O9 91.13(7) . . ?
O1 Co1 O9 163.02(7) . . ?
O5 Co2 O5 180.0 . 2_666 ?
O5 Co2 OW2 89.04(8) . 2_666 ?
O5 Co2 OW2 90.96(8) 2_666 2_666 ?
O5 Co2 OW2 90.96(8) . . ?
O5 Co2 OW2 89.04(8) 2_666 . ?
OW2 Co2 OW2 180.000(1) 2_666 . ?
O5 Co2 O7 80.14(7) . . ?
O5 Co2 O7 99.86(7) 2_666 . ?
OW2 Co2 O7 91.00(7) 2_666 . ?
OW2 Co2 O7 89.00(7) . . ?
O5 Co2 O7 99.86(7) . 2_666 ?
O5 Co2 O7 80.14(7) 2_666 2_666 ?
OW2 Co2 O7 89.00(7) 2_666 2_666 ?
OW2 Co2 O7 91.00(7) . 2_666 ?
O7 Co2 O7 180.0 . 2_666 ?
N1 Co3 N1 180.00(13) 2_565 . ?
N1 Co3 N2 83.56(8) 2_565 2_565 ?
N1 Co3 N2 96.44(8) . 2_565 ?
N1 Co3 N2 96.44(8) 2_565 . ?
N1 Co3 N2 83.56(8) . . ?
N2 Co3 N2 180.00(10) 2_565 . ?
N1 Co3 O2 90.50(8) 2_565 2_565 ?
N1 Co3 O2 89.50(8) . 2_565 ?
N2 Co3 O2 92.79(8) 2_565 2_565 ?
N2 Co3 O2 87.21(8) . 2_565 ?
N1 Co3 O2 89.50(8) 2_565 . ?
N1 Co3 O2 90.50(8) . . ?
N2 Co3 O2 87.21(8) 2_565 . ?
N2 Co3 O2 92.79(8) . . ?
O2 Co3 O2 180.0 2_565 . ?
O2 S1 O3 109.55(14) . . ?
O2 S1 O4 109.91(12) . . ?
O3 S1 O4 109.59(12) . . ?
O2 S1 O1 109.14(11) . . ?
O3 S1 O1 107.85(13) . . ?
O4 S1 O1 110.77(11) . . ?
S1 O1 Co1 139.35(12) . . ?
S1 O2 Co3 138.04(11) . . ?
C1 O5 Co2 111.68(16) . . ?
C1 O6 Co1 112.69(17) . . ?
C2 O7 Co2 111.21(17) . . ?
C2 O8 Co1 113.54(17) . . ?
C3 O9 Co1 112.57(16) . . ?
C3 O10 Co1 115.12(16) . 2_655 ?
Co1 OW1 H1 118.2 . . ?
Co1 OW1 H2 108.2 . . ?
H1 OW1 H2 105.6 . . ?
Co2 OW2 H3 116.0 . . ?
Co2 OW2 H4 120.4 . . ?
H3 OW2 H4 106.1 . . ?
C6 N2 C5 113.6(2) . . ?
C6 N2 Co3 117.64(16) . . ?
C5 N2 Co3 104.47(16) . . ?
C6 N2 H5 106.8 . . ?
C5 N2 H5 106.8 . . ?
Co3 N2 H5 106.8 . . ?
C7 N3 H6 109.5 . . ?
C7 N3 H7 109.5 . . ?
H6 N3 H7 109.5 . . ?
C7 N3 H8 109.5 . . ?
H6 N3 H8 109.5 . . ?
H7 N3 H8 109.5 . . ?
C4 N1 Co3 106.57(16) . . ?
C4 N1 H9 110.4 . . ?
Co3 N1 H9 110.4 . . ?
C4 N1 H10 110.4 . . ?
Co3 N1 H10 110.4 . . ?
H9 N1 H10 108.6 . . ?
O5 C1 O6 126.1(3) . . ?
O5 C1 C2 117.5(2) . . ?
O6 C1 C2 116.3(2) . . ?
O8 C2 O7 125.9(2) . . ?
O8 C2 C1 117.2(2) . . ?
O7 C2 C1 117.0(2) . . ?
O9 C3 O10 126.6(2) . . ?
O9 C3 C3 117.1(3) . 2_655 ?
O10 C3 C3 116.3(3) . 2_655 ?
N1 C4 C5 108.2(2) . . ?
N1 C4 H11 110.1 . . ?
C5 C4 H11 110.1 . . ?
N1 C4 H12 110.1 . . ?
C5 C4 H12 110.1 . . ?
H11 C4 H12 108.4 . . ?
N2 C5 C4 109.7(2) . . ?
N2 C5 H13 109.7 . . ?
C4 C5 H13 109.7 . . ?
N2 C5 H14 109.7 . . ?
C4 C5 H14 109.7 . . ?
H13 C5 H14 108.2 . . ?
N2 C6 C7 112.8(2) . . ?
N2 C6 H15 109.0 . . ?
C7 C6 H15 109.0 . . ?
N2 C6 H16 109.0 . . ?
C7 C6 H16 109.0 . . ?
H15 C6 H16 107.8 . . ?
N3 C7 C6 110.5(2) . . ?
N3 C7 H17 109.5 . . ?
C6 C7 H17 109.5 . . ?
N3 C7 H18 109.5 . . ?
C6 C7 H18 109.5 . . ?
H17 C7 H18 108.1 . . ?

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         0.336
_refine_diff_density_min         -0.301
_refine_diff_density_rms         0.071
_database_code_depnum_ccdc_archive 'CCDC 1003128'
#######################################################################
#
#                 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_2

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C8 H16 Co1.50 N3 O8 S'
_chemical_formula_weight         402.69

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'
S S 0.1246 0.1234 '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           triclinic
_symmetry_space_group_name_H-M   P-1

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   8.4331(6)
_cell_length_b                   9.4691(5)
_cell_length_c                   9.5144(5)
_cell_angle_alpha                71.522(5)
_cell_angle_beta                 64.356(6)
_cell_angle_gamma                89.622(5)
_cell_volume                     642.00(7)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    2677
_cell_measurement_theta_min      3.2750
_cell_measurement_theta_max      28.3560

_exptl_crystal_description       block
_exptl_crystal_colour            red
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.18
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.083
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             411
_exptl_absorpt_coefficient_mu    2.171
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.97721
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
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'
_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            4709
_diffrn_reflns_av_R_equivalents  0.0253
_diffrn_reflns_av_sigmaI/netI    0.0423
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_theta_min         3.26
_diffrn_reflns_theta_max         25.00
_reflns_number_total             2256
_reflns_number_gt                1936
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_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)+(0.0271P)²+0.2513P] 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         2256
_refine_ls_number_parameters     196
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0390
_refine_ls_R_factor_gt           0.0311
_refine_ls_wR_factor_ref         0.0704
_refine_ls_wR_factor_gt          0.0674
_refine_ls_goodness_of_fit_ref   1.084
_refine_ls_restrained_S_all      1.084
_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 0.80920(5) 0.98575(5) 0.32827(5) 0.01321(13) Uani 1 1 d . . .
Co2 Co 0.5000 0.5000 1.0000 0.01620(16) Uani 1 2 d S . .
S1 S 0.46340(10) 0.76785(8) 0.68722(8) 0.01389(19) Uani 1 1 d . . .
O1 O 0.6045(3) 0.8150(2) 0.5131(2) 0.0197(5) Uani 1 1 d . . .
O2 O 0.5443(3) 0.7031(2) 0.7984(2) 0.0203(5) Uani 1 1 d . . .
O3 O 0.3274(3) 0.6560(2) 0.7094(2) 0.0220(5) Uani 1 1 d . . .
O4 O 0.3841(3) 0.8994(2) 0.7239(3) 0.0219(5) Uani 1 1 d . . .
O5 O 0.9910(3) 0.8703(2) 0.4081(3) 0.0206(5) Uani 1 1 d . . .
O6 O 1.1601(3) 0.8938(2) 0.5292(2) 0.0187(5) Uani 1 1 d . . .
O7 O 0.8221(3) 0.8676(2) 0.1667(2) 0.0184(5) Uani 1 1 d . . .
O8 O 0.9668(3) 0.8864(2) -0.1004(2) 0.0215(5) Uani 1 1 d . . .
N1 N 0.5826(4) 0.2459(3) 0.6564(3) 0.0240(7) Uani 1 1 d . . .
H1 H 0.4901 0.2210 0.6409 0.029 Uiso 1 1 calc R . .
H2 H 0.6793 0.2169 0.5887 0.029 Uiso 1 1 calc R . .
N2 N 0.7129(3) 0.3845(3) 0.8272(3) 0.0157(6) Uani 1 1 d . . .
N3 N 0.7343(3) 0.5918(3) 0.9882(3) 0.0175(6) Uani 1 1 d . . .
H3 H 0.7328 0.6901 0.9749 0.021 Uiso 1 1 calc R . .
H4 H 0.7395 0.5446 1.0841 0.021 Uiso 1 1 calc R . .
C1 C 1.0432(4) 0.9325(3) 0.4814(3) 0.0146(7) Uani 1 1 d . . .
C2 C 0.9393(4) 0.9289(3) 0.0190(4) 0.0150(7) Uani 1 1 d . . .
C3 C 0.5445(5) 0.1655(4) 0.8310(4) 0.0267(8) Uani 1 1 d . . .
H5 H 0.5406 0.0583 0.8509 0.032 Uiso 1 1 calc R . .
H6 H 0.4285 0.1816 0.9041 0.032 Uiso 1 1 calc R . .
C4 C 0.6821(4) 0.2175(3) 0.8722(4) 0.0200(7) Uani 1 1 d . . .
H7 H 0.6442 0.1700 0.9905 0.024 Uiso 1 1 calc R . .
H8 H 0.7936 0.1849 0.8136 0.024 Uiso 1 1 calc R . .
C5 C 0.6142(5) 0.4116(4) 0.6124(4) 0.0248(8) Uani 1 1 d . . .
H9 H 0.5057 0.4450 0.6759 0.030 Uiso 1 1 calc R . .
H10 H 0.6478 0.4611 0.4952 0.030 Uiso 1 1 calc R . .
C6 C 0.7591(4) 0.4539(4) 0.6491(4) 0.0207(7) Uani 1 1 d . . .
H11 H 0.8677 0.4219 0.5837 0.025 Uiso 1 1 calc R . .
H12 H 0.7811 0.5626 0.6165 0.025 Uiso 1 1 calc R . .
C7 C 0.8715(4) 0.4163(4) 0.8509(4) 0.0212(7) Uani 1 1 d . . .
H13 H 0.9777 0.4018 0.7632 0.025 Uiso 1 1 calc R . .
H14 H 0.8577 0.3461 0.9565 0.025 Uiso 1 1 calc R . .
C8 C 0.8928(4) 0.5745(4) 0.8480(4) 0.0234(8) Uani 1 1 d . . .
H15 H 0.9991 0.5948 0.8584 0.028 Uiso 1 1 calc R . .
H16 H 0.9046 0.6454 0.7436 0.028 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 O1 2.072(2) . ?
Co1 O4 2.103(2) 2_676 ?
Co1 O6 2.120(2) 2_776 ?
Co1 O8 2.134(2) 2_775 ?
Co1 O7 2.139(2) . ?
Co1 O5 2.141(2) . ?
Co2 N3 2.107(3) . ?
Co2 N3 2.107(3) 2_667 ?
Co2 O2 2.137(2) 2_667 ?
Co2 O2 2.137(2) . ?
Co2 N2 2.384(3) 2_667 ?
Co2 N2 2.384(3) . ?
S1 O3 1.465(2) . ?
S1 O2 1.472(2) . ?
S1 O4 1.478(2) . ?
S1 O1 1.481(2) . ?
O4 Co1 2.103(2) 2_676 ?
O5 C1 1.248(3) . ?
O6 C1 1.262(4) . ?
O6 Co1 2.120(2) 2_776 ?
O7 C2 1.256(3) . ?
O8 C2 1.252(3) . ?
O8 Co1 2.134(2) 2_775 ?
N1 C3 1.477(4) . ?
N1 C5 1.484(4) . ?
N1 H1 0.9000 . ?
N1 H2 0.9000 . ?
N2 C6 1.477(4) . ?
N2 C4 1.494(4) . ?
N2 C7 1.497(4) . ?
N3 C8 1.478(4) . ?
N3 H3 0.9000 . ?
N3 H4 0.9000 . ?
C1 C1 1.530(6) 2_776 ?
C2 C2 1.543(6) 2_775 ?
C3 C4 1.506(5) . ?
C3 H5 0.9700 . ?
C3 H6 0.9700 . ?
C4 H7 0.9700 . ?
C4 H8 0.9700 . ?
C5 C6 1.496(4) . ?
C5 H9 0.9700 . ?
C5 H10 0.9700 . ?
C6 H11 0.9700 . ?
C6 H12 0.9700 . ?
C7 C8 1.500(4) . ?
C7 H13 0.9700 . ?
C7 H14 0.9700 . ?
C8 H15 0.9700 . ?
C8 H16 0.9700 . ?

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 Co1 O4 87.63(9) . 2_676 ?
O1 Co1 O6 100.47(8) . 2_776 ?
O4 Co1 O6 97.60(8) 2_676 2_776 ?
O1 Co1 O8 162.66(8) . 2_775 ?
O4 Co1 O8 96.41(9) 2_676 2_775 ?
O6 Co1 O8 95.70(8) 2_776 2_775 ?
O1 Co1 O7 85.79(8) . . ?
O4 Co1 O7 88.85(8) 2_676 . ?
O6 Co1 O7 171.15(8) 2_776 . ?
O8 Co1 O7 77.47(8) 2_775 . ?
O1 Co1 O5 89.32(9) . . ?
O4 Co1 O5 173.71(8) 2_676 . ?
O6 Co1 O5 77.55(8) 2_776 . ?
O8 Co1 O5 88.11(9) 2_775 . ?
O7 Co1 O5 96.41(8) . . ?
N3 Co2 N3 180.00(6) . 2_667 ?
N3 Co2 O2 95.05(9) . 2_667 ?
N3 Co2 O2 84.95(9) 2_667 2_667 ?
N3 Co2 O2 84.95(9) . . ?
N3 Co2 O2 95.05(9) 2_667 . ?
O2 Co2 O2 180.0 2_667 . ?
N3 Co2 N2 99.99(9) . 2_667 ?
N3 Co2 N2 80.01(9) 2_667 2_667 ?
O2 Co2 N2 93.97(8) 2_667 2_667 ?
O2 Co2 N2 86.03(8) . 2_667 ?
N3 Co2 N2 80.01(9) . . ?
N3 Co2 N2 99.99(9) 2_667 . ?
O2 Co2 N2 86.03(8) 2_667 . ?
O2 Co2 N2 93.97(8) . . ?
N2 Co2 N2 180.000(1) 2_667 . ?
O3 S1 O2 110.87(12) . . ?
O3 S1 O4 110.32(13) . . ?
O2 S1 O4 108.66(12) . . ?
O3 S1 O1 108.32(12) . . ?
O2 S1 O1 108.47(13) . . ?
O4 S1 O1 110.18(13) . . ?
S1 O1 Co1 143.50(14) . . ?
S1 O2 Co2 137.61(14) . . ?
S1 O4 Co1 131.91(13) . 2_676 ?
C1 O5 Co1 113.62(19) . . ?
C1 O6 Co1 114.23(19) . 2_776 ?
C2 O7 Co1 114.22(19) . . ?
C2 O8 Co1 114.41(19) . 2_775 ?
C3 N1 C5 111.5(2) . . ?
C3 N1 H1 109.3 . . ?
C5 N1 H1 109.3 . . ?
C3 N1 H2 109.3 . . ?
C5 N1 H2 109.3 . . ?
H1 N1 H2 108.0 . . ?
C6 N2 C4 107.7(2) . . ?
C6 N2 C7 108.9(2) . . ?
C4 N2 C7 105.3(2) . . ?
C6 N2 Co2 113.84(19) . . ?
C4 N2 Co2 119.16(19) . . ?
C7 N2 Co2 101.05(16) . . ?
C8 N3 Co2 110.44(19) . . ?
C8 N3 H3 109.6 . . ?
Co2 N3 H3 109.6 . . ?
C8 N3 H4 109.6 . . ?
Co2 N3 H4 109.6 . . ?
H3 N3 H4 108.1 . . ?
O5 C1 O6 126.0(3) . . ?
O5 C1 C1 117.4(3) . 2_776 ?
O6 C1 C1 116.6(3) . 2_776 ?
O8 C2 O7 126.4(3) . . ?
O8 C2 C2 116.9(3) . 2_775 ?
O7 C2 C2 116.8(3) . 2_775 ?
N1 C3 C4 112.2(3) . . ?
N1 C3 H5 109.2 . . ?
C4 C3 H5 109.2 . . ?
N1 C3 H6 109.2 . . ?
C4 C3 H6 109.2 . . ?
H5 C3 H6 107.9 . . ?
N2 C4 C3 113.2(3) . . ?
N2 C4 H7 108.9 . . ?
C3 C4 H7 108.9 . . ?
N2 C4 H8 108.9 . . ?
C3 C4 H8 108.9 . . ?
H7 C4 H8 107.8 . . ?
N1 C5 C6 110.0(3) . . ?
N1 C5 H9 109.7 . . ?
C6 C5 H9 109.7 . . ?
N1 C5 H10 109.7 . . ?
C6 C5 H10 109.7 . . ?
H9 C5 H10 108.2 . . ?
N2 C6 C5 111.9(3) . . ?
N2 C6 H11 109.2 . . ?
C5 C6 H11 109.2 . . ?
N2 C6 H12 109.2 . . ?
C5 C6 H12 109.2 . . ?
H11 C6 H12 107.9 . . ?
N2 C7 C8 111.0(3) . . ?
N2 C7 H13 109.4 . . ?
C8 C7 H13 109.4 . . ?
N2 C7 H14 109.4 . . ?
C8 C7 H14 109.4 . . ?
H13 C7 H14 108.0 . . ?
N3 C8 C7 108.6(3) . . ?
N3 C8 H15 110.0 . . ?
C7 C8 H15 110.0 . . ?
N3 C8 H16 110.0 . . ?
C7 C8 H16 110.0 . . ?
H15 C8 H16 108.4 . . ?

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         0.466
_refine_diff_density_min         -0.469
_refine_diff_density_rms         0.083
_database_code_depnum_ccdc_archive 'CCDC 1003129'
