# Electronic Supplementary Material (ESI) for Journal of Materials Chemistry A.
# 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_CoBDC_plate
#============================================================================== 

_audit_creation_date             2014-04-30T11:05:48-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.3
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic

#----------------------------------------------------------------------------#
#                   CHEMICAL INFORMATION                                     #
#----------------------------------------------------------------------------#

_chemical_name_systematic        
;
 ?
;
_chemical_formula_sum            'C36 H40 Co3 N4 O16'
_chemical_formula_weight         961.51

#----------------------------------------------------------------------------#
#                   UNIT CELL INFORMATION                                    #
#----------------------------------------------------------------------------#

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   'P 21/n'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_Int_Tables_number      14

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   16.182(3)
_cell_length_b                   9.4700(19)
_cell_length_c                   16.361(3)
_cell_angle_alpha                90
_cell_angle_beta                 111.28(3)
_cell_angle_gamma                90
_cell_volume                     2336.3(8)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)

#----------------------------------------------------------------------------#
#                   CRYSTAL INFORMATION                                      #
#----------------------------------------------------------------------------#

_exptl_crystal_description       plate
_exptl_crystal_colour            purple
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.05
_exptl_crystal_density_diffrn    1.367
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             986
_exptl_special_details           
;
 ?
;

#----------------------------------------------------------------------------#
#                   ABSORPTION CORRECTION                                    #
#----------------------------------------------------------------------------#

_exptl_absorpt_coefficient_mu    1.017
_exptl_absorpt_correction_type   none
_exptl_absorpt_correction_T_min  0.8877
_exptl_absorpt_correction_T_max  0.9509

#----------------------------------------------------------------------------#
#                   DATA COLLECTION                                          #
#----------------------------------------------------------------------------#

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.70002
_diffrn_radiation_monochromator  graphite
_diffrn_reflns_av_R_equivalents  0.0841
_diffrn_reflns_av_unetI/netI     0.0751
_diffrn_reflns_number            17122
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         2.59
_diffrn_reflns_theta_max         26
_diffrn_reflns_theta_full        26
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_reflns_number_total             4776
_reflns_number_gt                2785
_reflns_threshold_expression     >2sigma(I)

#----------------------------------------------------------------------------#
#                   COMPUTER PROGRAMS USED                                   #
#----------------------------------------------------------------------------#

_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'

#----------------------------------------------------------------------------#
#                   REFINEMENT INFORMATION                                   #
#----------------------------------------------------------------------------#

_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)+(0.1539P)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    riding
_refine_ls_extinction_method     SHELXL
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_coef       0.036(4)
_refine_ls_number_reflns         4776
_refine_ls_number_parameters     273
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1174
_refine_ls_R_factor_gt           0.0801
_refine_ls_wR_factor_ref         0.2357
_refine_ls_wR_factor_gt          0.216
_refine_ls_goodness_of_fit_ref   0.962
_refine_ls_restrained_S_all      0.962
_refine_ls_shift/su_max          0
_refine_ls_shift/su_mean         0
_refine_diff_density_max         1.681
_refine_diff_density_min         -0.647
_refine_diff_density_rms         0.11

#----------------------------------------------------------------------------#
#                   ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS         #
#----------------------------------------------------------------------------#

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.003 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0059 0.0032 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0105 0.0059 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Co Co 0.3512 0.9494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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 0.5 1 0 0.0546(4) Uani 1 2 d S . .
Co2 Co 0.36562(6) 0.94125(8) 0.12448(5) 0.0555(3) Uani 1 1 d . . .
N1 N 0.1726(4) 0.8102(6) -0.0982(3) 0.0729(16) Uani 1 1 d . . .
N2 N 0.2077(4) 0.9173(5) 0.2821(3) 0.0619(13) Uani 1 1 d . . .
O1 O 0.5639(3) 1.0564(5) 0.1293(3) 0.0674(12) Uani 1 1 d . . .
O2 O 0.4757(3) 1.0414(5) 0.2075(3) 0.0605(11) Uani 1 1 d . . .
O3 O 0.8984(3) 1.3562(5) 0.4774(3) 0.0628(11) Uani 1 1 d . . .
O4 O 0.8038(3) 1.3918(4) 0.5475(3) 0.0589(10) Uani 1 1 d . . .
O5 O 0.4237(3) 0.8508(4) 0.0385(3) 0.0619(11) Uani 1 1 d . . .
O6 O 0.4298(3) 0.7273(5) 0.1522(3) 0.0712(12) Uani 1 1 d . . .
O7 O 0.2501(3) 0.8160(5) 0.0468(3) 0.0677(12) Uani 1 1 d . . .
O8 O 0.3100(3) 0.9640(5) 0.2192(3) 0.0642(11) Uani 1 1 d . . .
C1 C 0.5458(5) 1.0718(6) 0.1972(4) 0.0575(15) Uani 1 1 d . . .
C2 C 0.6184(4) 1.1414(6) 0.2737(4) 0.0562(14) Uani 1 1 d . . .
C3 C 0.6024(4) 1.1834(6) 0.3488(4) 0.0595(15) Uani 1 1 d . . .
H3 H 0.5456 1.1705 0.3523 0.071 Uiso 1 1 calc R . .
C4 C 0.6708(4) 1.2439(7) 0.4179(4) 0.0600(15) Uani 1 1 d . . .
H4 H 0.6605 1.2711 0.4692 0.072 Uiso 1 1 calc R . .
C5 C 0.7533(4) 1.2656(7) 0.4138(4) 0.0573(14) Uani 1 1 d . . .
C6 C 0.7677(5) 1.2213(9) 0.3398(5) 0.078(2) Uani 1 1 d . . .
H6 H 0.8245 1.2343 0.3363 0.094 Uiso 1 1 calc R . .
C7 C 0.7004(5) 1.1579(8) 0.2697(4) 0.0710(18) Uani 1 1 d . . .
H7 H 0.7119 1.1265 0.2197 0.085 Uiso 1 1 calc R . .
C8 C 0.8246(5) 1.3435(6) 0.4856(4) 0.0577(15) Uani 1 1 d . . .
C9 C 0.4427(5) 0.7390(7) 0.0821(5) 0.0672(17) Uani 1 1 d . . .
C10 C 0.4727(5) 0.6093(8) 0.0365(5) 0.0747(19) Uani 1 1 d . . .
C11 C 0.4633(5) 0.6181(8) -0.0503(5) 0.0732(18) Uani 1 1 d . . .
H11 H 0.4388 0.7002 -0.0836 0.088 Uiso 1 1 calc R . .
C12 C 0.4903(5) 0.5056(8) -0.0882(5) 0.0735(19) Uani 1 1 d . . .
H12 H 0.4834 0.5075 -0.1483 0.088 Uiso 1 1 calc R . .
C13 C 0.1952(5) 0.8657(8) -0.0215(4) 0.0693(17) Uani 1 1 d . . .
H13 H 0.1675 0.9522 -0.0167 0.083 Uiso 1 1 calc R . .
C14 C 0.2146(6) 0.6813(9) -0.1097(5) 0.091(2) Uani 1 1 d . . .
H14A H 0.2569 0.7024 -0.1384 0.136 Uiso 1 1 calc R . .
H14B H 0.1695 0.6157 -0.1462 0.136 Uiso 1 1 calc R . .
H14C H 0.2461 0.6381 -0.0524 0.136 Uiso 1 1 calc R . .
C15 C 0.1082(6) 0.8811(10) -0.1759(5) 0.090(2) Uani 1 1 d . . .
H15A H 0.0796 0.9589 -0.1567 0.135 Uiso 1 1 calc R . .
H15B H 0.0631 0.8129 -0.2096 0.135 Uiso 1 1 calc R . .
H15C H 0.1392 0.9183 -0.2128 0.135 Uiso 1 1 calc R . .
C16 C 0.2423(5) 0.9061(7) 0.2195(4) 0.0636(16) Uani 1 1 d . . .
H16 H 0.2115 0.8478 0.1707 0.076 Uiso 1 1 calc R . .
C17 C 0.1286(5) 0.8408(8) 0.2770(5) 0.078(2) Uani 1 1 d . . .
H17A H 0.1092 0.7812 0.2244 0.117 Uiso 1 1 calc R . .
H17B H 0.0814 0.908 0.2739 0.117 Uiso 1 1 calc R . .
H17C H 0.1414 0.7814 0.3292 0.117 Uiso 1 1 calc R . .
C18 C 0.2447(6) 1.0095(9) 0.3553(5) 0.081(2) Uani 1 1 d . . .
H18A H 0.3039 1.0397 0.3589 0.121 Uiso 1 1 calc R . .
H18B H 0.2493 0.9597 0.4093 0.121 Uiso 1 1 calc R . .
H18C H 0.2065 1.0924 0.3479 0.121 Uiso 1 1 calc R . .



#----------------------------------------------------------------------------#
#                   MOLECULAR GEOMETRY                                       #
#----------------------------------------------------------------------------#

_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 2.059(4) 3_675 ?
Co1 O1 2.059(4) . ?
Co1 O3 2.063(4) 4_585 ?
Co1 O3 2.063(4) 2_645 ?
Co1 O5 2.117(4) 3_675 ?
Co1 O5 2.117(4) . ?
Co2 O2 2.040(4) . ?
Co2 O4 2.043(4) 4_585 ?
Co2 O8 2.067(5) . ?
Co2 O5 2.134(4) . ?
Co2 O7 2.189(5) . ?
Co2 O6 2.247(5) . ?
Co2 C9 2.517(7) . ?
N1 C13 1.285(8) . ?
N1 C14 1.443(10) . ?
N1 C15 1.480(9) . ?
N2 C16 1.337(8) . ?
N2 C18 1.427(9) . ?
N2 C17 1.447(9) . ?
O1 C1 1.257(7) . ?
O2 C1 1.238(8) . ?
O3 C8 1.255(8) . ?
O3 Co1 2.063(4) 2_655 ?
O4 C8 1.262(7) . ?
O4 Co2 2.043(4) 4_686 ?
O5 C9 1.252(8) . ?
O6 C9 1.243(8) . ?
O7 C13 1.242(7) . ?
O8 C16 1.227(8) . ?
C1 C2 1.521(8) . ?
C2 C7 1.361(9) . ?
C2 C3 1.403(8) . ?
C3 C4 1.387(9) . ?
C4 C5 1.375(9) . ?
C5 C6 1.379(9) . ?
C5 C8 1.508(9) . ?
C6 C7 1.398(9) . ?
C9 C10 1.601(11) . ?
C10 C11 1.374(10) . ?
C10 C12 1.375(10) 3_665 ?
C11 C12 1.381(11) . ?
C12 C10 1.375(10) 3_665 ?

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 O1 179.9990(10) 3_675 . ?
O1 Co1 O3 85.23(18) 3_675 4_585 ?
O1 Co1 O3 94.77(18) . 4_585 ?
O1 Co1 O3 94.77(18) 3_675 2_645 ?
O1 Co1 O3 85.23(18) . 2_645 ?
O3 Co1 O3 180 4_585 2_645 ?
O1 Co1 O5 89.84(17) 3_675 3_675 ?
O1 Co1 O5 90.16(17) . 3_675 ?
O3 Co1 O5 91.12(17) 4_585 3_675 ?
O3 Co1 O5 88.88(17) 2_645 3_675 ?
O1 Co1 O5 90.16(17) 3_675 . ?
O1 Co1 O5 89.84(17) . . ?
O3 Co1 O5 88.88(18) 4_585 . ?
O3 Co1 O5 91.13(17) 2_645 . ?
O5 Co1 O5 180 3_675 . ?
O2 Co2 O4 99.47(17) . 4_585 ?
O2 Co2 O8 88.01(18) . . ?
O4 Co2 O8 97.65(18) 4_585 . ?
O2 Co2 O5 97.97(18) . . ?
O4 Co2 O5 97.92(17) 4_585 . ?
O8 Co2 O5 162.15(18) . . ?
O2 Co2 O7 173.61(17) . . ?
O4 Co2 O7 86.44(17) 4_585 . ?
O8 Co2 O7 88.80(18) . . ?
O5 Co2 O7 83.52(17) . . ?
O2 Co2 O6 93.25(17) . . ?
O4 Co2 O6 155.42(17) 4_585 . ?
O8 Co2 O6 103.77(19) . . ?
O5 Co2 O6 59.29(17) . . ?
O7 Co2 O6 82.14(17) . . ?
O2 Co2 C9 97.9(2) . . ?
O4 Co2 C9 126.9(2) 4_585 . ?
O8 Co2 C9 132.9(2) . . ?
O5 Co2 C9 29.8(2) . . ?
O7 Co2 C9 80.3(2) . . ?
O6 Co2 C9 29.55(19) . . ?
C13 N1 C14 119.6(6) . . ?
C13 N1 C15 121.0(7) . . ?
C14 N1 C15 119.3(6) . . ?
C16 N2 C18 121.7(6) . . ?
C16 N2 C17 121.6(6) . . ?
C18 N2 C17 116.7(6) . . ?
C1 O1 Co1 138.4(4) . . ?
C1 O2 Co2 129.7(4) . . ?
C8 O3 Co1 140.5(4) . 2_655 ?
C8 O4 Co2 124.2(4) . 4_686 ?
C9 O5 Co1 133.2(4) . . ?
C9 O5 Co2 92.3(4) . . ?
Co1 O5 Co2 111.84(18) . . ?
C9 O6 Co2 87.4(4) . . ?
C13 O7 Co2 119.9(4) . . ?
C16 O8 Co2 126.1(4) . . ?
O2 C1 O1 127.7(6) . . ?
O2 C1 C2 117.5(5) . . ?
O1 C1 C2 114.7(6) . . ?
C7 C2 C3 120.2(6) . . ?
C7 C2 C1 119.2(6) . . ?
C3 C2 C1 120.6(6) . . ?
C4 C3 C2 119.0(6) . . ?
C5 C4 C3 121.6(6) . . ?
C4 C5 C6 118.3(6) . . ?
C4 C5 C8 121.1(6) . . ?
C6 C5 C8 120.5(6) . . ?
C5 C6 C7 121.4(7) . . ?
C2 C7 C6 119.5(6) . . ?
O3 C8 O4 126.3(6) . . ?
O3 C8 C5 116.9(5) . . ?
O4 C8 C5 116.8(6) . . ?
O6 C9 O5 120.8(6) . . ?
O6 C9 C10 122.9(6) . . ?
O5 C9 C10 115.9(6) . . ?
O6 C9 Co2 63.1(4) . . ?
O5 C9 Co2 57.9(3) . . ?
C10 C9 Co2 167.6(5) . . ?
C11 C10 C12 122.9(8) . 3_665 ?
C11 C10 C9 119.8(6) . . ?
C12 C10 C9 117.3(7) 3_665 . ?
C10 C11 C12 118.8(7) . . ?
C10 C12 C11 118.2(7) 3_665 . ?
O7 C13 N1 125.5(7) . . ?
O8 C16 N2 126.2(7) . . ?
#=============================================================================#
#     End of CIF
#=============================================================================# 

_database_code_depnum_ccdc_archive 'CCDC 1000305'
#######################################################################
#
#                 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_CoBDC_rod
#============================================================================== 

_audit_creation_date             2014-04-30T11:53:42-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.3
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic

#----------------------------------------------------------------------------#
#                   CHEMICAL INFORMATION                                     #
#----------------------------------------------------------------------------#

_chemical_name_systematic        
;
 ?
;
_chemical_formula_sum            'C20 H20 Co2 O10 S2'
_chemical_formula_weight         602.34

#----------------------------------------------------------------------------#
#                   UNIT CELL INFORMATION                                    #
#----------------------------------------------------------------------------#

_symmetry_cell_setting           Triclinic
_symmetry_space_group_name_H-M   'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_Int_Tables_number      2

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

_cell_length_a                   7.3489(15)
_cell_length_b                   10.969(2)
_cell_length_c                   16.002(3)
_cell_angle_alpha                72.51(3)
_cell_angle_beta                 78.52(3)
_cell_angle_gamma                73.12(3)
_cell_volume                     1168.5(4)
_cell_formula_units_Z            2
_cell_measurement_temperature    173(2)

#----------------------------------------------------------------------------#
#                   CRYSTAL INFORMATION                                      #
#----------------------------------------------------------------------------#

_exptl_crystal_description       rod
_exptl_crystal_colour            pink
_exptl_crystal_size_max          0.06
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.04
_exptl_crystal_density_diffrn    1.712
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             612
_exptl_absorpt_correction_T_min  0.9446
_exptl_absorpt_correction_T_max  0.9625
_exptl_absorpt_process_details   'Rigaku Rapid Auto'

_exptl_special_details           
;
 ?
;

#----------------------------------------------------------------------------#
#                   ABSORPTION CORRECTION                                    #
#----------------------------------------------------------------------------#

_exptl_absorpt_coefficient_mu    1.652
_exptl_absorpt_correction_type   empirical

#----------------------------------------------------------------------------#
#                   DATA COLLECTION                                          #
#----------------------------------------------------------------------------#

_diffrn_ambient_temperature      173(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  'image plate'
_diffrn_measurement_method       'omega scans'
_diffrn_reflns_av_R_equivalents  0.0983
_diffrn_reflns_av_unetI/netI     0.1295
_diffrn_reflns_number            11151
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         3.02
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_full        25
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.988
_reflns_number_total             5300
_reflns_number_gt                3194
_reflns_threshold_expression     >2sigma(I)

#----------------------------------------------------------------------------#
#                   COMPUTER PROGRAMS USED                                   #
#----------------------------------------------------------------------------#
_computing_data_collection       'Rigaku RAPID-II'
_computing_cell_refinement       'Rigaku RAPID-II'
_computing_data_reduction        'Rigaku RAPID-II'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_publication_material  WinGX

#----------------------------------------------------------------------------#
#                   REFINEMENT INFORMATION                                   #
#----------------------------------------------------------------------------#

_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)+(0.2000P)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    riding
_refine_ls_extinction_method     none
_refine_ls_number_reflns         5300
_refine_ls_number_parameters     311
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.175
_refine_ls_R_factor_gt           0.1242
_refine_ls_wR_factor_ref         0.3591
_refine_ls_wR_factor_gt          0.3121
_refine_ls_goodness_of_fit_ref   1.183
_refine_ls_restrained_S_all      1.183
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0
_refine_diff_density_max         6.444
_refine_diff_density_min         -1.655
_refine_diff_density_rms         0.288

#----------------------------------------------------------------------------#
#                   ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS         #
#----------------------------------------------------------------------------#

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 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.006 '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'

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 0.45886(17) 0.25186(11) 0.24126(8) 0.0212(4) Uani 1 1 d . . .
Co2 Co -0.04505(17) 0.24384(10) 0.25689(8) 0.0208(4) Uani 1 1 d . . .
O1 O 0.3021(11) 0.3151(8) 0.3475(5) 0.0387(18) Uani 1 1 d . . .
O2 O 0.0103(11) 0.2766(7) 0.3681(5) 0.0368(17) Uani 1 1 d . . .
O3 O 0.4100(10) 0.0669(6) 0.2863(5) 0.0319(16) Uani 1 1 d . . .
O4 O 0.1195(10) 0.0531(6) 0.2783(5) 0.0356(17) Uani 1 1 d . . .
O5 O 0.7924(11) -0.5645(6) 0.2343(6) 0.0391(18) Uani 1 1 d . . .
O6 O 0.5163(11) -0.5660(6) 0.1998(5) 0.0354(17) Uani 1 1 d . . .
O7 O -0.0924(10) 0.2168(7) 0.1430(5) 0.0351(17) Uani 1 1 d . . .
O8 O -0.3754(11) 0.1839(8) 0.1376(5) 0.0371(17) Uani 1 1 d . . .
C1 C 0.1303(15) 0.3304(9) 0.3797(6) 0.027(2) Uani 1 1 d . . .
C2 C 0.0621(15) 0.4166(9) 0.4428(6) 0.027(2) Uani 1 1 d . . .
C3 C 0.1878(16) 0.4660(12) 0.4694(8) 0.043(3) Uani 1 1 d . . .
H3 H 0.3168 0.4444 0.4476 0.052 Uiso 1 1 calc R . .
C4 C -0.1310(16) 0.4551(11) 0.4738(8) 0.039(3) Uani 1 1 d . . .
H4 H -0.2213 0.427 0.4558 0.046 Uiso 1 1 calc R . .
C5 C 0.2941(15) 0.0098(9) 0.2764(6) 0.029(2) Uani 1 1 d . . .
C6 C 0.3803(13) -0.1276(8) 0.2632(7) 0.027(2) Uani 1 1 d . . .
C7 C 0.5748(17) -0.1739(11) 0.2492(10) 0.049(3) Uani 1 1 d . . .
H7 H 0.6533 -0.1194 0.2464 0.058 Uiso 1 1 calc R . .
C8 C 0.6582(18) -0.3009(11) 0.2392(10) 0.051(3) Uani 1 1 d . . .
H8 H 0.7906 -0.3332 0.234 0.061 Uiso 1 1 calc R . .
C9 C 0.5391(15) -0.3794(9) 0.2371(7) 0.032(2) Uani 1 1 d . . .
C10 C 0.3420(17) -0.3292(10) 0.2487(8) 0.041(3) Uani 1 1 d . . .
H10 H 0.2622 -0.3803 0.2471 0.05 Uiso 1 1 calc R . .
C11 C 0.2615(17) -0.2056(11) 0.2625(9) 0.046(3) Uani 1 1 d . . .
H11 H 0.1291 -0.1747 0.2713 0.055 Uiso 1 1 calc R . .
C12 C 0.6245(14) -0.5159(9) 0.2241(6) 0.027(2) Uani 1 1 d . . .
C13 C -0.1957(15) 0.1653(9) 0.1181(6) 0.027(2) Uani 1 1 d . . .
C14 C -0.0935(17) 0.0786(10) 0.0563(7) 0.035(2) Uani 1 1 d . . .
C15 C 0.0992(17) 0.0415(13) 0.0453(9) 0.050(3) Uani 1 1 d . . .
H15 H 0.1672 0.0699 0.0759 0.06 Uiso 1 1 calc R . .
C16 C -0.200(2) 0.0386(12) 0.0109(9) 0.050(3) Uani 1 1 d . . .
H16 H -0.3334 0.0642 0.0178 0.06 Uiso 1 1 calc R . .
S1 S 0.6371(4) 0.0873(3) 0.41390(17) 0.0378(7) Uani 1 1 d . . .
O1D O 0.6940(10) 0.1754(7) 0.3234(4) 0.0295(15) Uani 1 1 d . . .
C17 C 0.682(4) 0.151(2) 0.4936(10) 0.111(9) Uani 1 1 d . . .
H17A H 0.8098 0.1635 0.4801 0.166 Uiso 1 1 calc R . .
H17B H 0.6686 0.0911 0.5508 0.166 Uiso 1 1 calc R . .
H17C H 0.5919 0.2347 0.4937 0.166 Uiso 1 1 calc R . .
C18 C 0.816(3) -0.0634(19) 0.4237(13) 0.129(10) Uani 1 1 d . . .
H18A H 0.796 -0.1121 0.387 0.194 Uiso 1 1 calc R . .
H18B H 0.8098 -0.1146 0.484 0.194 Uiso 1 1 calc R . .
H18C H 0.9404 -0.0451 0.4053 0.194 Uiso 1 1 calc R . .
S2 S 0.1395(4) 0.4137(3) 0.08613(18) 0.0389(7) Uani 1 1 d . . .
O2D O 0.1968(9) 0.3217(7) 0.1747(4) 0.0282(15) Uani 1 1 d . . .
C19 C 0.184(3) 0.5657(15) 0.0807(12) 0.095(7) Uani 1 1 d . . .
H19A H 0.2984 0.5497 0.1072 0.142 Uiso 1 1 calc R . .
H19B H 0.0779 0.6155 0.112 0.142 Uiso 1 1 calc R . .
H19C H 0.2015 0.6146 0.0202 0.142 Uiso 1 1 calc R . .
C20 C 0.319(3) 0.361(2) 0.0091(9) 0.112(9) Uani 1 1 d . . .
H20A H 0.4402 0.3584 0.0241 0.168 Uiso 1 1 calc R . .
H20B H 0.2995 0.4204 -0.048 0.168 Uiso 1 1 calc R . .
H20C H 0.3171 0.2741 0.0081 0.168 Uiso 1 1 calc R . .



#----------------------------------------------------------------------------#
#                   MOLECULAR GEOMETRY                                       #
#----------------------------------------------------------------------------#

_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 2.041(7) . ?
Co1 O6 2.047(7) 1_565 ?
Co1 O8 2.051(7) 1_655 ?
Co1 O3 2.051(6) . ?
Co1 O1D 2.195(7) . ?
Co1 O2D 2.213(6) . ?
Co2 O7 2.041(7) . ?
Co2 O2 2.055(7) . ?
Co2 O4 2.055(7) . ?
Co2 O5 2.058(7) 1_465 ?
Co2 O2D 2.212(6) . ?
Co2 O1D 2.218(7) 1_455 ?
O1 C1 1.248(12) . ?
O2 C1 1.262(12) . ?
O3 C5 1.251(12) . ?
O4 C5 1.230(12) . ?
O5 C12 1.216(12) . ?
O5 Co2 2.058(7) 1_645 ?
O6 C12 1.261(12) . ?
O6 Co1 2.047(7) 1_545 ?
O7 C13 1.248(12) . ?
O8 C13 1.266(12) . ?
O8 Co1 2.051(7) 1_455 ?
C1 C2 1.504(13) . ?
C2 C3 1.383(15) . ?
C2 C4 1.391(15) . ?
C3 C4 1.365(15) 2_566 ?
C4 C3 1.365(15) 2_566 ?
C5 C6 1.517(12) . ?
C6 C7 1.368(15) . ?
C6 C11 1.392(14) . ?
C7 C8 1.393(15) . ?
C8 C9 1.405(15) . ?
C9 C10 1.388(16) . ?
C9 C12 1.507(13) . ?
C10 C11 1.378(14) . ?
C13 C14 1.518(14) . ?
C14 C15 1.346(17) . ?
C14 C16 1.398(16) . ?
C15 C16 1.400(16) 2 ?
C16 C15 1.400(16) 2 ?
S1 O1D 1.536(6) . ?
S1 C17 1.753(18) . ?
S1 C18 1.777(16) . ?
O1D Co2 2.218(7) 1_655 ?
S2 O2D 1.529(6) . ?
S2 C20 1.712(17) . ?
S2 C19 1.765(16) . ?

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 O6 85.0(3) . 1_565 ?
O1 Co1 O8 177.8(3) . 1_655 ?
O6 Co1 O8 95.6(3) 1_565 1_655 ?
O1 Co1 O3 94.6(3) . . ?
O6 Co1 O3 177.6(3) 1_565 . ?
O8 Co1 O3 84.8(3) 1_655 . ?
O1 Co1 O1D 84.6(3) . . ?
O6 Co1 O1D 91.0(3) 1_565 . ?
O8 Co1 O1D 93.2(3) 1_655 . ?
O3 Co1 O1D 86.5(3) . . ?
O1 Co1 O2D 89.3(3) . . ?
O6 Co1 O2D 92.9(3) 1_565 . ?
O8 Co1 O2D 92.9(3) 1_655 . ?
O3 Co1 O2D 89.5(3) . . ?
O1D Co1 O2D 172.4(2) . . ?
O7 Co2 O2 177.4(3) . . ?
O7 Co2 O4 85.4(3) . . ?
O2 Co2 O4 95.4(3) . . ?
O7 Co2 O5 94.4(3) . 1_465 ?
O2 Co2 O5 84.8(3) . 1_465 ?
O4 Co2 O5 179.4(3) . 1_465 ?
O7 Co2 O2D 85.2(3) . . ?
O2 Co2 O2D 92.4(3) . . ?
O4 Co2 O2D 91.9(3) . . ?
O5 Co2 O2D 87.5(3) 1_465 . ?
O7 Co2 O1D 88.4(3) . 1_455 ?
O2 Co2 O1D 94.1(3) . 1_455 ?
O4 Co2 O1D 91.3(3) . 1_455 ?
O5 Co2 O1D 89.3(3) 1_465 1_455 ?
O2D Co2 O1D 172.5(2) . 1_455 ?
C1 O1 Co1 134.5(7) . . ?
C1 O2 Co2 131.7(7) . . ?
C5 O3 Co1 137.0(6) . . ?
C5 O4 Co2 130.4(7) . . ?
C12 O5 Co2 132.2(7) . 1_645 ?
C12 O6 Co1 132.9(6) . 1_545 ?
C13 O7 Co2 139.2(7) . . ?
C13 O8 Co1 127.5(6) . 1_455 ?
O1 C1 O2 126.9(9) . . ?
O1 C1 C2 116.3(9) . . ?
O2 C1 C2 116.6(9) . . ?
C3 C2 C4 117.0(9) . . ?
C3 C2 C1 121.4(9) . . ?
C4 C2 C1 121.5(9) . . ?
C4 C3 C2 123.0(10) 2_566 . ?
C3 C4 C2 119.9(10) 2_566 . ?
O4 C5 O3 126.5(9) . . ?
O4 C5 C6 117.8(9) . . ?
O3 C5 C6 115.7(9) . . ?
C7 C6 C11 119.7(9) . . ?
C7 C6 C5 120.2(9) . . ?
C11 C6 C5 120.1(9) . . ?
C6 C7 C8 121.5(10) . . ?
C7 C8 C9 119.0(11) . . ?
C10 C9 C8 118.6(9) . . ?
C10 C9 C12 121.0(9) . . ?
C8 C9 C12 120.4(10) . . ?
C11 C10 C9 121.7(11) . . ?
C10 C11 C6 119.4(11) . . ?
O5 C12 O6 126.5(9) . . ?
O5 C12 C9 117.0(8) . . ?
O6 C12 C9 116.4(9) . . ?
O7 C13 O8 125.4(9) . . ?
O7 C13 C14 115.7(9) . . ?
O8 C13 C14 118.8(9) . . ?
C15 C14 C16 120.6(10) . . ?
C15 C14 C13 119.6(10) . . ?
C16 C14 C13 119.7(11) . . ?
C14 C15 C16 121.8(12) . 2 ?
C14 C16 C15 117.5(12) . 2 ?
O1D S1 C17 106.8(6) . . ?
O1D S1 C18 105.0(7) . . ?
C17 S1 C18 102.5(13) . . ?
S1 O1D Co1 111.8(4) . . ?
S1 O1D Co2 135.3(4) . 1_655 ?
Co1 O1D Co2 112.9(3) . 1_655 ?
O2D S2 C20 104.8(6) . . ?
O2D S2 C19 105.8(6) . . ?
C20 S2 C19 100.5(12) . . ?
S2 O2D Co2 111.5(4) . . ?
S2 O2D Co1 135.6(4) . . ?
Co2 O2D Co1 112.8(3) . . ?
#=============================================================================#
#     End of CIF
#=============================================================================# 


_database_code_depnum_ccdc_archive 'CCDC 1000296'
