# Electronic Supplementary Material (ESI) for Chemical Communications
# This journal is © The Royal Society of Chemistry 2012


data_global

_journal_coden_Cambridge         182
_journal_volume                  ?
_journal_page_first              ?
_journal_year                    ?

loop_
_publ_author_name
'Turega, Simon'
'Whitehead, Martina'
'Hall, Ben'
'Haddow, Mairi'
'Hunter, Christopher'
'Ward, Mike'

_publ_contact_author_name        'Dr Mike Ward'
_publ_contact_author_address     
;
Department of Chemistry
University of Sheffield
SHEFFIELD
S3 7HF
;
_publ_contact_author_fax         '0114 2229346'
_publ_contact_author_email       m.d.ward@sheffield.ac.uk

_publ_section_title              
;
Selective guest recognition
by a self-assembled paramagnetic cage complex
;

_publ_contact_letter             
;
This CIF contains details of the crystal structure in the paper
?Selective guest recognition by a self-assembled...'
by S. Turega et al, submitted to Chem. Comm. for publication.
;

# Attachment '- Coumarin_Ward_Hunter_crystaldata.cif'

#========================================================
data_mikeward_1_0m
_database_code_depnum_ccdc_archive 'CCDC 855597'
#TrackingRef '- Coumarin_Ward_Hunter_crystaldata.cif'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         
'C336 H264 Co8 N72, 3(C2 H3 N), 16(Cl O4), 2(OH2)'
_chemical_formula_sum            'C342 H277 Cl16 Co8 N75 O66'
_chemical_formula_weight         7532.03

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Co Co -2.3653 3.6143 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           trigonal
_symmetry_space_group_name_H-M   R-3
_symmetry_space_group_name_Hall  '-R 3'

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'

_cell_length_a                   28.8897(14)
_cell_length_b                   28.8897(14)
_cell_length_c                   53.152(6)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_volume                     38418(5)
_cell_formula_units_Z            3
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9963
_cell_measurement_theta_min      2.43
_cell_measurement_theta_max      66.24

_exptl_crystal_description       block
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.10
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    0.977
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             11610
_exptl_absorpt_coefficient_mu    3.241
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.4527
_exptl_absorpt_correction_T_max  0.6254
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_type           CuK\a
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean 5.56
_diffrn_reflns_number            118146
_diffrn_reflns_av_R_equivalents  0.0748
_diffrn_reflns_av_sigmaI/netI    0.0465
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_l_min       -63
_diffrn_reflns_limit_l_max       57
_diffrn_reflns_theta_min         2.49
_diffrn_reflns_theta_max         66.65
_reflns_number_total             15004
_reflns_number_gt                11048
_reflns_threshold_expression     >2sigma(I)

__computing_data_collection      'Bruker Apex II'
_computing_cell_refinement       'Bruker Apex II'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'Bruker ShelXTL'
_computing_publication_material  'Bruker ShelXTL'

_refine_special_details          
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.

The structure is a [Co8L12](ClO4)16 cubic coordination cage with
3 (CH3CN) and 2 (OH2) solvent molecules per complex.
The structure was solved by direct methods and all hydrogens have
been added in calculated positions. The protons for the water molecules
could not be located in the data and therefore have not been included
in the refinement. Also, only 14 of the expected 16 ClO4 anions could
be located from the data. This has led to a difference in calculated and
reported formula and consequent alerts in the cif check.

The structure has a number of solvent accessible voids, which were
consequently dealt with by the Platon Squeeze program. The details of the
squeeze are:

loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.000 0.000 0.000 4852 1052 ' '
2 0.667 0.333 0.333 4856 1053 ' '
3 0.000 0.000 0.500 331 135 ' '
4 0.333 -0.333 0.667 4856 1053 ' '
5 0.667 0.333 0.833 324 135 ' '
6 0.333 0.667 0.167 324 134 ' '
_platon_squeeze_details

Global displacement restraints have been used to achieve a
consistent model. The occupancies of some anions and solvent molecules
have been changed to achieve more consistent thermal parameters. The anions
and solvent molecules have also benefitted from local restraints to improve
their appearance.

Attempts to obtain a better data set were hampered by rapid solvent
loss on removal of the crystals from the mother liquor. The crystals
were also weakily difracting due to the presence of large voids within the
structure and lattice.

;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[\s^2^(Fo^2^)+(0.2000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         15004
_refine_ls_number_parameters     791
_refine_ls_number_restraints     830
_refine_ls_R_factor_all          0.1124
_refine_ls_R_factor_gt           0.1003
_refine_ls_wR_factor_ref         0.2842
_refine_ls_wR_factor_gt          0.2655
_refine_ls_goodness_of_fit_ref   1.134
_refine_ls_restrained_S_all      1.130
_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 0.69276(2) 0.94083(2) 0.225762(10) 0.0617(2) Uani 1 1 d . . .
Co2 Co 0.3333 0.6667 0.340210(15) 0.0547(3) Uani 1 3 d S . .
N111 N 0.73908(11) 0.91762(12) 0.20295(6) 0.0699(7) Uani 1 1 d U . .
C112 C 0.74021(13) 0.87416(15) 0.21092(8) 0.0727(9) Uani 1 1 d U . .
C113 C 0.76869(16) 0.85430(18) 0.19815(9) 0.0858(11) Uani 1 1 d U . .
H113 H 0.7692 0.8243 0.2041 0.103 Uiso 1 1 calc R . .
C114 C 0.79554(19) 0.8791(2) 0.17694(10) 0.0973(13) Uani 1 1 d U . .
H114 H 0.8142 0.8659 0.1681 0.117 Uiso 1 1 calc R . .
C115 C 0.79518(18) 0.9240(2) 0.16848(9) 0.0951(13) Uani 1 1 d U . .
H115 H 0.8138 0.9418 0.1541 0.114 Uiso 1 1 calc R . .
C116 C 0.76615(16) 0.94194(18) 0.18218(8) 0.0823(10) Uani 1 1 d U . .
H116 H 0.7656 0.9722 0.1766 0.099 Uiso 1 1 calc R . .
N121 N 0.66160(12) 0.84185(13) 0.26541(6) 0.0749(8) Uani 1 1 d U . .
N122 N 0.68256(10) 0.87041(11) 0.24470(6) 0.0662(7) Uani 1 1 d U . .
C123 C 0.71096(13) 0.85021(14) 0.23359(8) 0.0714(9) Uani 1 1 d U . .
C124 C 0.70731(16) 0.80800(17) 0.24812(10) 0.0882(12) Uani 1 1 d U . .
H124 H 0.7234 0.7876 0.2449 0.106 Uiso 1 1 calc R . .
C125 C 0.67547(17) 0.80328(19) 0.26776(10) 0.0934(13) Uani 1 1 d U . .
H125 H 0.6649 0.7782 0.2806 0.112 Uiso 1 1 calc R . .
C126 C 0.62491(14) 0.84862(17) 0.28142(8) 0.0765(9) Uani 1 1 d U . .
H12A H 0.6357 0.8862 0.2820 0.092 Uiso 1 1 calc R . .
H12B H 0.6273 0.8375 0.2984 0.092 Uiso 1 1 calc R . .
N131 N 0.27236(12) 0.66933(12) 0.36280(5) 0.0684(7) Uani 1 1 d U . .
C132 C 0.26000(14) 0.70738(14) 0.35597(6) 0.0647(8) Uani 1 1 d U . .
C133 C 0.22410(17) 0.71583(17) 0.36924(8) 0.0808(10) Uani 1 1 d U . .
H133 H 0.2167 0.7424 0.3643 0.097 Uiso 1 1 calc R . .
C134 C 0.1991(2) 0.6843(2) 0.39005(9) 0.0942(13) Uani 1 1 d U . .
H134 H 0.1744 0.6891 0.3992 0.113 Uiso 1 1 calc R . .
C135 C 0.2111(2) 0.6465(2) 0.39678(9) 0.0982(13) Uani 1 1 d U . .
H135 H 0.1952 0.6255 0.4109 0.118 Uiso 1 1 calc R . .
C136 C 0.24709(18) 0.63875(19) 0.38277(8) 0.0882(11) Uani 1 1 d U . .
H136 H 0.2539 0.6116 0.3873 0.106 Uiso 1 1 calc R . .
N141 N 0.33824(10) 0.75906(10) 0.30164(5) 0.0575(6) Uani 1 1 d U . .
N142 N 0.32040(10) 0.72575(10) 0.32154(5) 0.0554(6) Uani 1 1 d U . .
C143 C 0.28752(13) 0.73793(13) 0.33378(6) 0.0599(7) Uani 1 1 d U . .
C144 C 0.28478(14) 0.77927(13) 0.32158(7) 0.0656(8) Uani 1 1 d U . .
H144 H 0.2647 0.7949 0.3263 0.079 Uiso 1 1 calc R . .
C145 C 0.31748(14) 0.79183(13) 0.30152(7) 0.0644(8) Uani 1 1 d U . .
H145 H 0.3245 0.8183 0.2897 0.077 Uiso 1 1 calc R . .
C146 C 0.37662(12) 0.75980(13) 0.28402(6) 0.0594(7) Uani 1 1 d U . .
H14A H 0.3715 0.7723 0.2679 0.071 Uiso 1 1 calc R . .
H14B H 0.3697 0.7236 0.2818 0.071 Uiso 1 1 calc R . .
C151 C 0.56817(14) 0.81757(14) 0.27277(7) 0.0685(8) Uani 1 1 d U . .
C152 C 0.55348(15) 0.78220(15) 0.25297(7) 0.0727(9) Uani 1 1 d U . .
H152 H 0.5792 0.7770 0.2450 0.087 Uiso 1 1 calc R . .
C153 C 0.50075(14) 0.75409(14) 0.24463(7) 0.0701(9) Uani 1 1 d U . .
H153 H 0.4921 0.7322 0.2306 0.084 Uiso 1 1 calc R . .
C154 C 0.46216(14) 0.75846(13) 0.25682(6) 0.0633(8) Uani 1 1 d U . .
H154 H 0.4270 0.7389 0.2512 0.076 Uiso 1 1 calc R . .
C155 C 0.47426(12) 0.79259(12) 0.27814(6) 0.0573(7) Uani 1 1 d U . .
C156 C 0.52812(14) 0.82308(13) 0.28599(6) 0.0645(8) Uani 1 1 d U . .
C161 C 0.53992(15) 0.85679(14) 0.30724(7) 0.0744(9) Uani 1 1 d U . .
H161 H 0.5752 0.8774 0.3125 0.089 Uiso 1 1 calc R . .
C162 C 0.50084(16) 0.85950(15) 0.31997(8) 0.0785(10) Uani 1 1 d U . .
H162 H 0.5096 0.8824 0.3337 0.094 Uiso 1 1 calc R . .
C163 C 0.44723(15) 0.82826(14) 0.31274(7) 0.0701(9) Uani 1 1 d U . .
H163 H 0.4206 0.8300 0.3218 0.084 Uiso 1 1 calc R . .
C164 C 0.43388(13) 0.79473(12) 0.29207(6) 0.0597(7) Uani 1 1 d U . .
N211 N 0.64036(12) 0.95674(12) 0.24792(6) 0.0710(7) Uani 1 1 d U . .
C212 C 0.58976(14) 0.93422(14) 0.23961(7) 0.0680(8) Uani 1 1 d U . .
C213 C 0.55108(17) 0.94066(18) 0.25200(9) 0.0832(11) Uani 1 1 d U . .
H213 H 0.5161 0.9240 0.2461 0.100 Uiso 1 1 calc R . .
C214 C 0.5656(2) 0.9724(2) 0.27340(11) 0.1028(14) Uani 1 1 d U . .
H214 H 0.5404 0.9773 0.2820 0.123 Uiso 1 1 calc R . .
C215 C 0.6177(2) 0.9966(2) 0.28173(10) 0.1052(14) Uani 1 1 d U . .
H215 H 0.6285 1.0184 0.2959 0.126 Uiso 1 1 calc R . .
C216 C 0.65333(19) 0.98739(19) 0.26852(9) 0.0893(11) Uani 1 1 d U . .
H216 H 0.6884 1.0034 0.2742 0.107 Uiso 1 1 calc R . .
N221 N 0.59734(11) 0.87248(11) 0.18340(6) 0.0647(7) Uani 1 1 d U . .
N222 N 0.61886(10) 0.90098(11) 0.20485(6) 0.0624(7) Uani 1 1 d U . .
C223 C 0.57874(13) 0.90322(13) 0.21665(7) 0.0653(8) Uani 1 1 d U . .
C224 C 0.53163(13) 0.87603(14) 0.20291(8) 0.0721(9) Uani 1 1 d U . .
H224 H 0.4984 0.8717 0.2070 0.087 Uiso 1 1 calc R . .
C225 C 0.54459(14) 0.85694(15) 0.18196(8) 0.0731(9) Uani 1 1 d U . .
H225 H 0.5214 0.8369 0.1691 0.088 Uiso 1 1 calc R . .
C226 C 0.62694(15) 0.85815(14) 0.16642(7) 0.0700(8) Uani 1 1 d U . .
H22A H 0.6637 0.8872 0.1658 0.084 Uiso 1 1 calc R . .
H22B H 0.6119 0.8536 0.1497 0.084 Uiso 1 1 calc R . .
N231 N 0.65653(12) 0.56245(12) 0.08360(6) 0.0698(7) Uani 1 1 d U . .
C232 C 0.70869(15) 0.58641(15) 0.08993(8) 0.0754(9) Uani 1 1 d U . .
C233 C 0.74538(18) 0.58103(18) 0.07538(9) 0.0892(12) Uani 1 1 d U . .
H233 H 0.7809 0.5969 0.0805 0.107 Uiso 1 1 calc R . .
C234 C 0.72936(19) 0.55239(19) 0.05351(10) 0.0931(12) Uani 1 1 d U . .
H234 H 0.7538 0.5492 0.0433 0.112 Uiso 1 1 calc R . .
C235 C 0.67645(19) 0.52844(18) 0.04691(9) 0.0881(11) Uani 1 1 d U . .
H235 H 0.6643 0.5084 0.0322 0.106 Uiso 1 1 calc R . .
C236 C 0.64173(17) 0.53445(15) 0.06236(7) 0.0754(9) Uani 1 1 d U . .
H236 H 0.6059 0.5181 0.0577 0.091 Uiso 1 1 calc R . .
N241 N 0.70942(12) 0.65359(14) 0.14535(7) 0.0798(9) Uani 1 1 d U . .
N242 N 0.68537(11) 0.62408(12) 0.12470(6) 0.0703(7) Uani 1 1 d U . .
C243 C 0.72292(15) 0.61799(16) 0.11302(8) 0.0792(10) Uani 1 1 d U . .
C244 C 0.77150(18) 0.6442(2) 0.12596(11) 0.1090(16) Uani 1 1 d U . .
H244 H 0.8036 0.6460 0.1218 0.131 Uiso 1 1 calc R . .
C245 C 0.76087(18) 0.6668(2) 0.14624(11) 0.1030(15) Uani 1 1 d U . .
H245 H 0.7853 0.6877 0.1585 0.124 Uiso 1 1 calc R . .
C246 C 0.68228(15) 0.67206(15) 0.16175(8) 0.0726(9) Uani 1 1 d U . .
H24A H 0.6982 0.6781 0.1783 0.087 Uiso 1 1 calc R . .
H24B H 0.6452 0.6441 0.1633 0.087 Uiso 1 1 calc R . .
C251 C 0.62651(13) 0.80747(13) 0.17388(7) 0.0641(8) Uani 1 1 d U . .
C252 C 0.59758(14) 0.77869(14) 0.19416(7) 0.0679(8) Uani 1 1 d U . .
H252 H 0.5772 0.7899 0.2031 0.081 Uiso 1 1 calc R . .
C253 C 0.59797(15) 0.73238(14) 0.20187(7) 0.0695(8) Uani 1 1 d U . .
H253 H 0.5779 0.7135 0.2158 0.083 Uiso 1 1 calc R . .
C254 C 0.62686(14) 0.71504(14) 0.18949(7) 0.0666(8) Uani 1 1 d U . .
H254 H 0.6279 0.6852 0.1953 0.080 Uiso 1 1 calc R . .
C255 C 0.65598(13) 0.74221(14) 0.16749(7) 0.0643(8) Uani 1 1 d U . .
C256 C 0.65574(13) 0.78888(14) 0.15967(6) 0.0641(8) Uani 1 1 d U . .
C261 C 0.68511(15) 0.81626(15) 0.13753(7) 0.0756(9) Uani 1 1 d U . .
H261 H 0.6861 0.8474 0.1323 0.091 Uiso 1 1 calc R . .
C262 C 0.71158(16) 0.79641(17) 0.12425(8) 0.0847(11) Uani 1 1 d U . .
H262 H 0.7299 0.8139 0.1097 0.102 Uiso 1 1 calc R . .
C263 C 0.71184(15) 0.75028(16) 0.13203(8) 0.0802(10) Uani 1 1 d U . .
H263 H 0.7311 0.7381 0.1229 0.096 Uiso 1 1 calc R . .
C264 C 0.68391(14) 0.72274(15) 0.15312(7) 0.0707(9) Uani 1 1 d U . .
Cl11 Cl 0.78793(5) 0.73229(6) 0.22017(3) 0.1113(5) Uani 1 1 d DU . .
O12 O 0.73390(16) 0.7204(2) 0.21973(10) 0.1508(18) Uani 1 1 d DU . .
O13 O 0.8174(2) 0.77705(19) 0.23445(10) 0.1609(19) Uani 1 1 d DU . .
O14 O 0.78769(18) 0.68643(19) 0.23021(14) 0.181(2) Uani 1 1 d DU . .
O15 O 0.8072(2) 0.7396(3) 0.19555(10) 0.193(3) Uani 1 1 d DU . .
Cl21 Cl 0.69848(8) 0.93074(13) 0.33479(4) 0.1323(9) Uani 0.67 1 d PDU . .
O22 O 0.71948(16) 0.8986(2) 0.32208(9) 0.1101(16) Uani 0.67 1 d PDU . .
O23 O 0.6944(3) 0.9644(3) 0.31723(11) 0.157(3) Uani 0.67 1 d PDU . .
O24 O 0.6447(2) 0.8925(4) 0.34321(11) 0.193(4) Uani 0.67 1 d PDU . .
O25 O 0.73110(19) 0.9574(2) 0.35671(9) 0.1106(15) Uani 0.67 1 d PDU . .
Cl31 Cl 0.39587(7) 0.87522(12) 0.23356(4) 0.1383(10) Uani 0.67 1 d PDU . .
O32 O 0.3742(3) 0.8450(4) 0.20972(12) 0.207(4) Uani 0.67 1 d PDU . .
O33 O 0.4227(2) 0.8502(3) 0.24435(13) 0.150(3) Uani 0.67 1 d PDU . .
O34 O 0.4314(2) 0.9282(3) 0.22894(15) 0.181(4) Uani 0.67 1 d PDU . .
O35 O 0.35313(17) 0.8665(2) 0.24945(10) 0.127(2) Uani 0.67 1 d PDU . .
C1S C 0.6289(6) 0.6304(6) 0.24649(19) 0.155(5) Uani 0.50 1 d PDU . .
H1S1 H 0.6391 0.6168 0.2606 0.232 Uiso 0.50 1 calc PR . .
H1S2 H 0.5948 0.6274 0.2497 0.232 Uiso 0.50 1 calc PR . .
H1S3 H 0.6552 0.6672 0.2438 0.232 Uiso 0.50 1 calc PR . .
C2S C 0.6252(5) 0.5995(5) 0.22406(18) 0.118(3) Uani 0.50 1 d PDU . .
N3S N 0.6253(3) 0.5767(3) 0.20614(15) 0.093(2) Uani 0.50 1 d PDU . .
O1 O 0.3333 0.6667 0.23352(11) 0.0992(15) Uani 1 3 d S . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Co1 0.0471(3) 0.0605(3) 0.0764(4) 0.0030(2) -0.0020(2) 0.0259(2)
Co2 0.0568(3) 0.0568(3) 0.0506(5) 0.000 0.000 0.02838(17)
N111 0.0489(14) 0.0727(18) 0.0850(19) 0.0011(14) -0.0005(13) 0.0282(13)
C112 0.0488(17) 0.072(2) 0.097(2) -0.0027(18) -0.0052(16) 0.0298(16)
C113 0.064(2) 0.087(3) 0.110(3) -0.012(2) -0.003(2) 0.040(2)
C114 0.078(3) 0.112(3) 0.109(3) -0.015(3) 0.003(2) 0.052(2)
C115 0.075(2) 0.116(3) 0.091(3) 0.001(2) 0.012(2) 0.045(2)
C116 0.070(2) 0.084(2) 0.089(3) 0.006(2) 0.0086(19) 0.0356(19)
N121 0.0576(16) 0.0783(19) 0.084(2) 0.0152(15) 0.0015(14) 0.0305(14)
N122 0.0485(14) 0.0607(15) 0.0828(19) 0.0088(13) -0.0020(12) 0.0225(12)
C123 0.0486(16) 0.0643(19) 0.101(3) 0.0014(17) -0.0063(16) 0.0283(15)
C124 0.062(2) 0.079(2) 0.130(3) 0.019(2) -0.001(2) 0.0396(19)
C125 0.071(2) 0.086(3) 0.122(3) 0.031(2) 0.003(2) 0.038(2)
C126 0.0608(19) 0.081(2) 0.079(2) 0.0130(18) 0.0036(16) 0.0290(17)
N131 0.0704(17) 0.0749(18) 0.0572(16) 0.0027(13) 0.0135(13) 0.0343(15)
C132 0.0677(19) 0.0600(18) 0.0657(19) -0.0088(14) 0.0054(15) 0.0314(15)
C133 0.081(2) 0.079(2) 0.082(2) -0.0081(19) 0.0190(19) 0.040(2)
C134 0.101(3) 0.095(3) 0.091(3) -0.004(2) 0.033(2) 0.053(2)
C135 0.103(3) 0.110(3) 0.078(3) 0.009(2) 0.034(2) 0.051(3)
C136 0.098(3) 0.090(3) 0.074(2) 0.007(2) 0.022(2) 0.045(2)
N141 0.0585(14) 0.0535(13) 0.0602(15) 0.0001(11) 0.0003(11) 0.0278(12)
N142 0.0551(14) 0.0541(13) 0.0563(14) -0.0027(11) 0.0038(11) 0.0267(11)
C143 0.0577(16) 0.0565(16) 0.0664(18) -0.0137(14) 0.0004(14) 0.0292(14)
C144 0.0651(19) 0.0585(18) 0.075(2) -0.0099(15) -0.0047(16) 0.0324(15)
C145 0.0655(19) 0.0550(17) 0.074(2) 0.0009(15) -0.0029(16) 0.0314(15)
C146 0.0574(17) 0.0549(16) 0.0606(18) 0.0010(13) 0.0027(14) 0.0241(14)
C151 0.0577(18) 0.0622(18) 0.074(2) 0.0105(15) 0.0042(15) 0.0214(15)
C152 0.066(2) 0.071(2) 0.074(2) 0.0001(17) 0.0102(16) 0.0292(17)
C153 0.0625(19) 0.0618(19) 0.069(2) -0.0076(15) 0.0082(15) 0.0188(15)
C154 0.0606(18) 0.0555(17) 0.0603(18) 0.0005(14) 0.0017(14) 0.0190(14)
C155 0.0549(16) 0.0495(15) 0.0594(17) 0.0089(13) 0.0033(13) 0.0199(13)
C156 0.0601(18) 0.0543(17) 0.0671(19) 0.0048(14) 0.0018(15) 0.0196(14)
C161 0.0586(19) 0.064(2) 0.080(2) -0.0044(16) -0.0025(16) 0.0145(16)
C162 0.078(2) 0.060(2) 0.080(2) -0.0186(17) -0.0033(18) 0.0219(17)
C163 0.067(2) 0.0596(18) 0.080(2) -0.0058(16) 0.0010(16) 0.0281(16)
C164 0.0613(17) 0.0474(15) 0.0664(19) 0.0036(13) 0.0002(14) 0.0244(13)
N211 0.0617(16) 0.0702(17) 0.086(2) -0.0083(15) -0.0022(14) 0.0369(14)
C212 0.0599(18) 0.0635(19) 0.088(2) 0.0072(16) 0.0039(16) 0.0361(15)
C213 0.072(2) 0.090(3) 0.100(3) 0.010(2) 0.010(2) 0.050(2)
C214 0.105(3) 0.111(3) 0.115(4) 0.002(3) 0.023(3) 0.071(3)
C215 0.109(3) 0.110(3) 0.108(3) -0.023(3) 0.004(3) 0.062(3)
C216 0.083(3) 0.090(3) 0.101(3) -0.015(2) -0.001(2) 0.048(2)
N221 0.0556(14) 0.0577(15) 0.0793(18) -0.0013(13) -0.0072(13) 0.0271(12)
N222 0.0502(14) 0.0564(14) 0.0797(18) 0.0004(13) -0.0035(12) 0.0260(12)
C223 0.0532(17) 0.0580(17) 0.087(2) 0.0097(15) 0.0033(15) 0.0295(14)
C224 0.0477(16) 0.067(2) 0.102(3) 0.0072(18) -0.0070(16) 0.0290(15)
C225 0.0582(18) 0.067(2) 0.092(3) -0.0010(18) -0.0188(17) 0.0294(16)
C226 0.0673(19) 0.0639(19) 0.073(2) -0.0013(16) -0.0065(16) 0.0283(16)
N231 0.0707(17) 0.0635(16) 0.0844(19) -0.0093(14) -0.0021(14) 0.0403(14)
C232 0.072(2) 0.070(2) 0.095(2) -0.0150(18) -0.0013(18) 0.0435(18)
C233 0.075(2) 0.089(3) 0.113(3) -0.020(2) 0.005(2) 0.047(2)
C234 0.090(3) 0.092(3) 0.106(3) -0.020(2) 0.011(2) 0.052(2)
C235 0.096(3) 0.083(2) 0.092(3) -0.019(2) 0.003(2) 0.049(2)
C236 0.084(2) 0.067(2) 0.081(2) -0.0146(17) -0.0058(18) 0.0423(18)
N241 0.0642(17) 0.084(2) 0.097(2) -0.0292(17) -0.0130(15) 0.0417(15)
N242 0.0609(16) 0.0685(17) 0.088(2) -0.0213(14) -0.0090(14) 0.0370(14)
C243 0.0615(19) 0.082(2) 0.102(3) -0.025(2) -0.0089(18) 0.0414(18)
C244 0.072(2) 0.128(4) 0.145(4) -0.057(3) -0.022(2) 0.064(3)
C245 0.071(2) 0.118(3) 0.131(4) -0.052(3) -0.027(2) 0.055(2)
C246 0.0609(19) 0.073(2) 0.087(2) -0.0183(18) -0.0077(17) 0.0358(17)
C251 0.0572(17) 0.0583(17) 0.069(2) -0.0043(14) -0.0040(14) 0.0235(14)
C252 0.0616(18) 0.0655(19) 0.076(2) -0.0009(16) 0.0081(16) 0.0317(16)
C253 0.069(2) 0.0634(19) 0.074(2) -0.0006(16) 0.0066(16) 0.0312(16)
C254 0.0624(18) 0.0576(18) 0.075(2) -0.0005(15) 0.0021(15) 0.0267(15)
C255 0.0528(16) 0.0608(18) 0.072(2) -0.0122(15) -0.0022(14) 0.0227(14)
C256 0.0549(17) 0.0603(18) 0.0659(19) -0.0097(14) -0.0042(14) 0.0204(14)
C261 0.068(2) 0.0610(19) 0.081(2) -0.0034(17) 0.0065(17) 0.0198(16)
C262 0.071(2) 0.078(2) 0.082(2) -0.0105(19) 0.0137(18) 0.0204(19)
C263 0.062(2) 0.076(2) 0.091(3) -0.0166(19) 0.0129(18) 0.0258(18)
C264 0.0549(17) 0.068(2) 0.080(2) -0.0189(17) -0.0040(16) 0.0238(15)
Cl11 0.0969(8) 0.1250(9) 0.1450(11) -0.0635(8) -0.0530(7) 0.0803(7)
O12 0.117(3) 0.176(4) 0.204(4) -0.067(3) -0.061(3) 0.107(3)
O13 0.151(4) 0.151(4) 0.186(4) -0.088(3) -0.079(3) 0.081(3)
O14 0.103(3) 0.125(3) 0.339(8) -0.007(4) 0.009(4) 0.076(3)
O15 0.150(4) 0.276(7) 0.129(4) -0.079(4) -0.034(3) 0.088(4)
Cl21 0.0829(11) 0.228(3) 0.0916(12) 0.0362(14) -0.0040(9) 0.0815(15)
O22 0.049(2) 0.151(4) 0.100(3) -0.010(3) -0.027(2) 0.027(2)
O23 0.184(7) 0.250(8) 0.102(4) 0.004(4) -0.013(4) 0.157(7)
O24 0.067(3) 0.363(12) 0.102(4) 0.026(5) -0.017(3) 0.073(5)
O25 0.087(3) 0.148(4) 0.101(3) 0.002(3) -0.005(2) 0.062(3)
Cl31 0.0664(9) 0.213(2) 0.1300(16) 0.1075(17) 0.0245(9) 0.0653(12)
O32 0.112(5) 0.342(12) 0.114(5) 0.070(6) 0.006(4) 0.073(6)
O33 0.080(3) 0.170(6) 0.179(6) 0.098(5) 0.010(3) 0.047(3)
O34 0.104(4) 0.213(7) 0.203(7) 0.146(6) 0.035(4) 0.063(4)
O35 0.059(2) 0.153(5) 0.117(4) 0.063(3) 0.007(2) 0.012(3)
C1S 0.143(10) 0.198(14) 0.103(8) 0.029(7) -0.002(8) 0.070(10)
C2S 0.102(7) 0.129(9) 0.113(7) 0.033(6) -0.019(7) 0.049(6)
N3S 0.076(4) 0.094(5) 0.088(5) 0.021(4) -0.020(4) 0.026(4)
O1 0.096(2) 0.096(2) 0.106(4) 0.000 0.000 0.0480(11)

_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 N211 2.142(3) . ?
Co1 N111 2.147(3) . ?
Co1 N242 2.153(3) 15 ?
Co1 N122 2.154(3) . ?
Co1 N222 2.159(3) . ?
Co1 N231 2.169(3) 15 ?
Co2 N142 2.162(3) . ?
Co2 N142 2.162(3) 2_665 ?
Co2 N142 2.162(3) 3_565 ?
Co2 N131 2.165(3) 3_565 ?
Co2 N131 2.165(3) 2_665 ?
Co2 N131 2.165(3) . ?
N111 C116 1.332(5) . ?
N111 C112 1.341(5) . ?
C112 C113 1.392(6) . ?
C112 C123 1.436(6) . ?
C113 C114 1.353(7) . ?
C113 H113 0.9300 . ?
C114 C115 1.376(7) . ?
C114 H114 0.9300 . ?
C115 C116 1.392(6) . ?
C115 H115 0.9300 . ?
C116 H116 0.9300 . ?
N121 N122 1.327(4) . ?
N121 C125 1.366(6) . ?
N121 C126 1.446(5) . ?
N122 C123 1.357(5) . ?
C123 C124 1.402(6) . ?
C124 C125 1.352(7) . ?
C124 H124 0.9300 . ?
C125 H125 0.9300 . ?
C126 C151 1.494(5) . ?
C126 H12A 0.9700 . ?
C126 H12B 0.9700 . ?
N131 C136 1.340(5) . ?
N131 C132 1.364(5) . ?
C132 C133 1.373(5) . ?
C132 C143 1.449(5) . ?
C133 C134 1.385(6) . ?
C133 H133 0.9300 . ?
C134 C135 1.350(7) . ?
C134 H134 0.9300 . ?
C135 C136 1.384(6) . ?
C135 H135 0.9300 . ?
C136 H136 0.9300 . ?
N141 N142 1.347(4) . ?
N141 C145 1.350(4) . ?
N141 C146 1.443(4) . ?
N142 C143 1.336(4) . ?
C143 C144 1.396(5) . ?
C144 C145 1.348(5) . ?
C144 H144 0.9300 . ?
C145 H145 0.9300 . ?
C146 C164 1.506(5) . ?
C146 H14A 0.9700 . ?
C146 H14B 0.9700 . ?
C151 C152 1.378(5) . ?
C151 C156 1.429(5) . ?
C152 C153 1.393(5) . ?
C152 H152 0.9300 . ?
C153 C154 1.349(5) . ?
C153 H153 0.9300 . ?
C154 C155 1.426(5) . ?
C154 H154 0.9300 . ?
C155 C164 1.409(5) . ?
C155 C156 1.414(5) . ?
C156 C161 1.417(5) . ?
C161 C162 1.351(6) . ?
C161 H161 0.9300 . ?
C162 C163 1.401(5) . ?
C162 H162 0.9300 . ?
C163 C164 1.386(5) . ?
C163 H163 0.9300 . ?
N211 C216 1.338(5) . ?
N211 C212 1.343(5) . ?
C212 C213 1.387(5) . ?
C212 C223 1.452(5) . ?
C213 C214 1.387(7) . ?
C213 H213 0.9300 . ?
C214 C215 1.378(8) . ?
C214 H214 0.9300 . ?
C215 C216 1.376(7) . ?
C215 H215 0.9300 . ?
C216 H216 0.9300 . ?
N221 C225 1.359(4) . ?
N221 N222 1.361(4) . ?
N221 C226 1.439(5) . ?
N222 C223 1.348(4) . ?
C223 C224 1.390(5) . ?
C224 C225 1.375(6) . ?
C224 H224 0.9300 . ?
C225 H225 0.9300 . ?
C226 C251 1.511(5) . ?
C226 H22A 0.9700 . ?
C226 H22B 0.9700 . ?
N231 C236 1.328(5) . ?
N231 C232 1.349(5) . ?
N231 Co1 2.170(3) 14_455 ?
C232 C233 1.383(6) . ?
C232 C243 1.460(6) . ?
C233 C234 1.366(7) . ?
C233 H233 0.9300 . ?
C234 C235 1.371(7) . ?
C234 H234 0.9300 . ?
C235 C236 1.373(6) . ?
C235 H235 0.9300 . ?
C236 H236 0.9300 . ?
N241 C245 1.338(5) . ?
N241 N242 1.350(4) . ?
N241 C246 1.442(5) . ?
N242 C243 1.336(5) . ?
N242 Co1 2.153(3) 14_455 ?
C243 C244 1.398(6) . ?
C244 C245 1.371(7) . ?
C244 H244 0.9300 . ?
C245 H245 0.9300 . ?
C246 C264 1.512(6) . ?
C246 H24A 0.9700 . ?
C246 H24B 0.9700 . ?
C251 C252 1.363(5) . ?
C251 C256 1.423(5) . ?
C252 C253 1.405(5) . ?
C252 H252 0.9300 . ?
C253 C254 1.341(5) . ?
C253 H253 0.9300 . ?
C254 C255 1.425(5) . ?
C254 H254 0.9300 . ?
C255 C256 1.414(5) . ?
C255 C264 1.416(5) . ?
C256 C261 1.435(5) . ?
C261 C262 1.360(6) . ?
C261 H261 0.9300 . ?
C262 C263 1.399(6) . ?
C262 H262 0.9300 . ?
C263 C264 1.378(6) . ?
C263 H263 0.9300 . ?
Cl11 O13 1.369(4) . ?
Cl11 O15 1.396(5) . ?
Cl11 O12 1.421(4) . ?
Cl11 O14 1.425(5) . ?
Cl21 O23 1.394(7) . ?
Cl21 O25 1.453(5) . ?
Cl21 O24 1.455(6) . ?
Cl21 O22 1.499(6) . ?
Cl31 O34 1.374(7) . ?
Cl31 O35 1.410(5) . ?
Cl31 O33 1.420(6) . ?
Cl31 O32 1.488(8) . ?
C1S C2S 1.461(2) . ?
C1S H1S1 0.9600 . ?
C1S H1S2 0.9600 . ?
C1S H1S3 0.9600 . ?
C2S N3S 1.159(2) . ?

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
N211 Co1 N111 174.69(12) . . ?
N211 Co1 N242 91.34(12) . 15 ?
N111 Co1 N242 92.58(12) . 15 ?
N211 Co1 N122 99.68(12) . . ?
N111 Co1 N122 77.36(12) . . ?
N242 Co1 N122 162.66(11) 15 . ?
N211 Co1 N222 77.35(12) . . ?
N111 Co1 N222 98.47(11) . . ?
N242 Co1 N222 99.44(10) 15 . ?
N122 Co1 N222 96.03(11) . . ?
N211 Co1 N231 92.46(12) . 15 ?
N111 Co1 N231 91.93(12) . 15 ?
N242 Co1 N231 76.45(11) 15 15 ?
N122 Co1 N231 89.65(11) . 15 ?
N222 Co1 N231 169.02(11) . 15 ?
N142 Co2 N142 100.61(8) . 2_665 ?
N142 Co2 N142 100.61(8) . 3_565 ?
N142 Co2 N142 100.60(8) 2_665 3_565 ?
N142 Co2 N131 91.36(11) . 3_565 ?
N142 Co2 N131 168.00(11) 2_665 3_565 ?
N142 Co2 N131 76.20(10) 3_565 3_565 ?
N142 Co2 N131 168.01(11) . 2_665 ?
N142 Co2 N131 76.20(10) 2_665 2_665 ?
N142 Co2 N131 91.36(11) 3_565 2_665 ?
N131 Co2 N131 92.22(12) 3_565 2_665 ?
N142 Co2 N131 76.20(10) . . ?
N142 Co2 N131 91.37(11) 2_665 . ?
N142 Co2 N131 168.01(11) 3_565 . ?
N131 Co2 N131 92.22(12) 3_565 . ?
N131 Co2 N131 92.22(12) 2_665 . ?
C116 N111 C112 118.2(3) . . ?
C116 N111 Co1 126.6(3) . . ?
C112 N111 Co1 115.1(3) . . ?
N111 C112 C113 121.9(4) . . ?
N111 C112 C123 115.6(3) . . ?
C113 C112 C123 122.5(4) . . ?
C114 C113 C112 119.2(4) . . ?
C114 C113 H113 120.4 . . ?
C112 C113 H113 120.4 . . ?
C113 C114 C115 119.9(4) . . ?
C113 C114 H114 120.0 . . ?
C115 C114 H114 120.0 . . ?
C114 C115 C116 118.0(4) . . ?
C114 C115 H115 121.0 . . ?
C116 C115 H115 121.0 . . ?
N111 C116 C115 122.8(4) . . ?
N111 C116 H116 118.6 . . ?
C115 C116 H116 118.6 . . ?
N122 N121 C125 110.8(3) . . ?
N122 N121 C126 122.8(3) . . ?
C125 N121 C126 126.2(3) . . ?
N121 N122 C123 106.2(3) . . ?
N121 N122 Co1 141.2(3) . . ?
C123 N122 Co1 112.1(2) . . ?
N122 C123 C124 109.6(4) . . ?
N122 C123 C112 119.7(3) . . ?
C124 C123 C112 130.7(4) . . ?
C125 C124 C123 105.3(4) . . ?
C125 C124 H124 127.3 . . ?
C123 C124 H124 127.3 . . ?
C124 C125 N121 108.0(4) . . ?
C124 C125 H125 126.0 . . ?
N121 C125 H125 126.0 . . ?
N121 C126 C151 113.3(3) . . ?
N121 C126 H12A 108.9 . . ?
C151 C126 H12A 108.9 . . ?
N121 C126 H12B 108.9 . . ?
C151 C126 H12B 108.9 . . ?
H12A C126 H12B 107.7 . . ?
C136 N131 C132 117.8(3) . . ?
C136 N131 Co2 126.9(3) . . ?
C132 N131 Co2 115.3(2) . . ?
N131 C132 C133 122.1(3) . . ?
N131 C132 C143 115.0(3) . . ?
C133 C132 C143 122.9(3) . . ?
C132 C133 C134 119.1(4) . . ?
C132 C133 H133 120.5 . . ?
C134 C133 H133 120.5 . . ?
C135 C134 C133 118.9(4) . . ?
C135 C134 H134 120.6 . . ?
C133 C134 H134 120.6 . . ?
C134 C135 C136 120.4(4) . . ?
C134 C135 H135 119.8 . . ?
C136 C135 H135 119.8 . . ?
N131 C136 C135 121.7(4) . . ?
N131 C136 H136 119.2 . . ?
C135 C136 H136 119.2 . . ?
N142 N141 C145 111.0(3) . . ?
N142 N141 C146 122.5(3) . . ?
C145 N141 C146 126.4(3) . . ?
C143 N142 N141 105.2(3) . . ?
C143 N142 Co2 114.3(2) . . ?
N141 N142 Co2 140.25(19) . . ?
N142 C143 C144 110.6(3) . . ?
N142 C143 C132 118.8(3) . . ?
C144 C143 C132 130.6(3) . . ?
C145 C144 C143 105.4(3) . . ?
C145 C144 H144 127.3 . . ?
C143 C144 H144 127.3 . . ?
C144 C145 N141 107.8(3) . . ?
C144 C145 H145 126.1 . . ?
N141 C145 H145 126.1 . . ?
N141 C146 C164 113.8(3) . . ?
N141 C146 H14A 108.8 . . ?
C164 C146 H14A 108.8 . . ?
N141 C146 H14B 108.8 . . ?
C164 C146 H14B 108.8 . . ?
H14A C146 H14B 107.7 . . ?
C152 C151 C156 119.5(3) . . ?
C152 C151 C126 121.2(4) . . ?
C156 C151 C126 119.2(3) . . ?
C151 C152 C153 121.1(3) . . ?
C151 C152 H152 119.4 . . ?
C153 C152 H152 119.4 . . ?
C154 C153 C152 120.5(3) . . ?
C154 C153 H153 119.8 . . ?
C152 C153 H153 119.8 . . ?
C153 C154 C155 121.2(3) . . ?
C153 C154 H154 119.4 . . ?
C155 C154 H154 119.4 . . ?
C164 C155 C156 119.7(3) . . ?
C164 C155 C154 121.7(3) . . ?
C156 C155 C154 118.6(3) . . ?
C155 C156 C161 118.3(3) . . ?
C155 C156 C151 119.0(3) . . ?
C161 C156 C151 122.6(3) . . ?
C162 C161 C156 121.2(3) . . ?
C162 C161 H161 119.4 . . ?
C156 C161 H161 119.4 . . ?
C161 C162 C163 120.8(3) . . ?
C161 C162 H162 119.6 . . ?
C163 C162 H162 119.6 . . ?
C164 C163 C162 120.0(3) . . ?
C164 C163 H163 120.0 . . ?
C162 C163 H163 120.0 . . ?
C163 C164 C155 120.0(3) . . ?
C163 C164 C146 121.5(3) . . ?
C155 C164 C146 118.5(3) . . ?
C216 N211 C212 117.8(3) . . ?
C216 N211 Co1 126.7(3) . . ?
C212 N211 Co1 115.5(2) . . ?
N211 C212 C213 122.2(4) . . ?
N211 C212 C223 115.2(3) . . ?
C213 C212 C223 122.6(3) . . ?
C214 C213 C212 118.7(4) . . ?
C214 C213 H213 120.7 . . ?
C212 C213 H213 120.7 . . ?
C215 C214 C213 119.4(4) . . ?
C215 C214 H214 120.3 . . ?
C213 C214 H214 120.3 . . ?
C216 C215 C214 118.1(5) . . ?
C216 C215 H215 121.0 . . ?
C214 C215 H215 121.0 . . ?
N211 C216 C215 123.8(4) . . ?
N211 C216 H216 118.1 . . ?
C215 C216 H216 118.1 . . ?
C225 N221 N222 110.2(3) . . ?
C225 N221 C226 126.8(3) . . ?
N222 N221 C226 122.8(3) . . ?
C223 N222 N221 106.0(3) . . ?
C223 N222 Co1 112.3(2) . . ?
N221 N222 Co1 141.7(2) . . ?
N222 C223 C224 110.6(3) . . ?
N222 C223 C212 119.5(3) . . ?
C224 C223 C212 129.9(3) . . ?
C225 C224 C223 105.4(3) . . ?
C225 C224 H224 127.3 . . ?
C223 C224 H224 127.3 . . ?
N221 C225 C224 107.9(3) . . ?
N221 C225 H225 126.1 . . ?
C224 C225 H225 126.1 . . ?
N221 C226 C251 113.3(3) . . ?
N221 C226 H22A 108.9 . . ?
C251 C226 H22A 108.9 . . ?
N221 C226 H22B 108.9 . . ?
C251 C226 H22B 108.9 . . ?
H22A C226 H22B 107.7 . . ?
C236 N231 C232 117.5(3) . . ?
C236 N231 Co1 126.9(3) . 14_455 ?
C232 N231 Co1 115.2(2) . 14_455 ?
N231 C232 C233 121.7(4) . . ?
N231 C232 C243 115.1(3) . . ?
C233 C232 C243 123.3(4) . . ?
C234 C233 C232 119.8(4) . . ?
C234 C233 H233 120.1 . . ?
C232 C233 H233 120.1 . . ?
C233 C234 C235 118.5(4) . . ?
C233 C234 H234 120.7 . . ?
C235 C234 H234 120.7 . . ?
C234 C235 C236 118.9(4) . . ?
C234 C235 H235 120.5 . . ?
C236 C235 H235 120.5 . . ?
N231 C236 C235 123.5(4) . . ?
N231 C236 H236 118.2 . . ?
C235 C236 H236 118.2 . . ?
C245 N241 N242 110.9(3) . . ?
C245 N241 C246 127.3(3) . . ?
N242 N241 C246 121.5(3) . . ?
C243 N242 N241 105.4(3) . . ?
C243 N242 Co1 114.4(2) . 14_455 ?
N241 N242 Co1 140.0(2) . 14_455 ?
N242 C243 C244 111.2(3) . . ?
N242 C243 C232 118.6(3) . . ?
C244 C243 C232 130.2(3) . . ?
C245 C244 C243 104.0(4) . . ?
C245 C244 H244 128.0 . . ?
C243 C244 H244 128.0 . . ?
N241 C245 C244 108.5(4) . . ?
N241 C245 H245 125.7 . . ?
C244 C245 H245 125.7 . . ?
N241 C246 C264 114.6(3) . . ?
N241 C246 H24A 108.6 . . ?
C264 C246 H24A 108.6 . . ?
N241 C246 H24B 108.6 . . ?
C264 C246 H24B 108.6 . . ?
H24A C246 H24B 107.6 . . ?
C252 C251 C256 119.2(3) . . ?
C252 C251 C226 120.3(3) . . ?
C256 C251 C226 120.5(3) . . ?
C251 C252 C253 121.1(3) . . ?
C251 C252 H252 119.4 . . ?
C253 C252 H252 119.4 . . ?
C254 C253 C252 121.0(3) . . ?
C254 C253 H253 119.5 . . ?
C252 C253 H253 119.5 . . ?
C253 C254 C255 120.2(3) . . ?
C253 C254 H254 119.9 . . ?
C255 C254 H254 119.9 . . ?
C256 C255 C264 119.7(3) . . ?
C256 C255 C254 118.9(3) . . ?
C264 C255 C254 121.4(3) . . ?
C255 C256 C251 119.4(3) . . ?
C255 C256 C261 118.9(3) . . ?
C251 C256 C261 121.7(3) . . ?
C262 C261 C256 119.7(4) . . ?
C262 C261 H261 120.2 . . ?
C256 C261 H261 120.2 . . ?
C261 C262 C263 121.3(4) . . ?
C261 C262 H262 119.3 . . ?
C263 C262 H262 119.3 . . ?
C264 C263 C262 120.7(4) . . ?
C264 C263 H263 119.7 . . ?
C262 C263 H263 119.7 . . ?
C263 C264 C255 119.7(4) . . ?
C263 C264 C246 122.1(3) . . ?
C255 C264 C246 118.2(3) . . ?
O13 Cl11 O15 111.3(4) . . ?
O13 Cl11 O12 109.1(3) . . ?
O15 Cl11 O12 109.1(3) . . ?
O13 Cl11 O14 112.4(3) . . ?
O15 Cl11 O14 108.0(4) . . ?
O12 Cl11 O14 106.7(3) . . ?
O23 Cl21 O25 115.2(5) . . ?
O23 Cl21 O24 107.7(4) . . ?
O25 Cl21 O24 108.6(3) . . ?
O23 Cl21 O22 109.3(4) . . ?
O25 Cl21 O22 109.5(3) . . ?
O24 Cl21 O22 106.1(5) . . ?
O34 Cl31 O35 114.0(5) . . ?
O34 Cl31 O33 110.2(4) . . ?
O35 Cl31 O33 108.6(3) . . ?
O34 Cl31 O32 111.3(4) . . ?
O35 Cl31 O32 109.3(4) . . ?
O33 Cl31 O32 102.8(5) . . ?
C2S C1S H1S1 109.5 . . ?
C2S C1S H1S2 109.5 . . ?
H1S1 C1S H1S2 109.5 . . ?
C2S C1S H1S3 109.5 . . ?
H1S1 C1S H1S3 109.5 . . ?
H1S2 C1S H1S3 109.5 . . ?
N3S C2S C1S 176.2(14) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N211 Co1 N111 C116 122.7(13) . . . . ?
N242 Co1 N111 C116 -15.0(3) 15 . . . ?
N122 Co1 N111 C116 179.3(3) . . . . ?
N222 Co1 N111 C116 84.9(3) . . . . ?
N231 Co1 N111 C116 -91.5(3) 15 . . . ?
N211 Co1 N111 C112 -57.5(14) . . . . ?
N242 Co1 N111 C112 164.9(3) 15 . . . ?
N122 Co1 N111 C112 -0.9(2) . . . . ?
N222 Co1 N111 C112 -95.2(3) . . . . ?
N231 Co1 N111 C112 88.3(3) 15 . . . ?
C116 N111 C112 C113 0.1(5) . . . . ?
Co1 N111 C112 C113 -179.8(3) . . . . ?
C116 N111 C112 C123 179.1(3) . . . . ?
Co1 N111 C112 C123 -0.8(4) . . . . ?
N111 C112 C113 C114 -0.7(6) . . . . ?
C123 C112 C113 C114 -179.7(4) . . . . ?
C112 C113 C114 C115 1.1(7) . . . . ?
C113 C114 C115 C116 -0.8(7) . . . . ?
C112 N111 C116 C115 0.3(6) . . . . ?
Co1 N111 C116 C115 -179.9(3) . . . . ?
C114 C115 C116 N111 0.1(7) . . . . ?
C125 N121 N122 C123 -0.6(4) . . . . ?
C126 N121 N122 C123 -175.0(3) . . . . ?
C125 N121 N122 Co1 -171.9(3) . . . . ?
C126 N121 N122 Co1 13.7(6) . . . . ?
N211 Co1 N122 N121 -11.1(4) . . . . ?
N111 Co1 N122 N121 173.4(4) . . . . ?
N242 Co1 N122 N121 117.7(5) 15 . . . ?
N222 Co1 N122 N121 -89.2(4) . . . . ?
N231 Co1 N122 N121 81.4(4) 15 . . . ?
N211 Co1 N122 C123 177.9(2) . . . . ?
N111 Co1 N122 C123 2.4(2) . . . . ?
N242 Co1 N122 C123 -53.3(5) 15 . . . ?
N222 Co1 N122 C123 99.8(2) . . . . ?
N231 Co1 N122 C123 -89.6(2) 15 . . . ?
N121 N122 C123 C124 -0.2(4) . . . . ?
Co1 N122 C123 C124 173.9(3) . . . . ?
N121 N122 C123 C112 -177.9(3) . . . . ?
Co1 N122 C123 C112 -3.8(4) . . . . ?
N111 C112 C123 N122 3.2(5) . . . . ?
C113 C112 C123 N122 -177.8(3) . . . . ?
N111 C112 C123 C124 -174.0(4) . . . . ?
C113 C112 C123 C124 5.0(6) . . . . ?
N122 C123 C124 C125 1.0(5) . . . . ?
C112 C123 C124 C125 178.3(4) . . . . ?
C123 C124 C125 N121 -1.3(5) . . . . ?
N122 N121 C125 C124 1.2(5) . . . . ?
C126 N121 C125 C124 175.3(4) . . . . ?
N122 N121 C126 C151 84.5(4) . . . . ?
C125 N121 C126 C151 -88.9(5) . . . . ?
N142 Co2 N131 C136 176.6(4) . . . . ?
N142 Co2 N131 C136 76.0(3) 2_665 . . . ?
N142 Co2 N131 C136 -107.5(6) 3_565 . . . ?
N131 Co2 N131 C136 -92.5(3) 3_565 . . . ?
N131 Co2 N131 C136 -0.2(4) 2_665 . . . ?
N142 Co2 N131 C132 -5.1(2) . . . . ?
N142 Co2 N131 C132 -105.7(3) 2_665 . . . ?
N142 Co2 N131 C132 70.8(6) 3_565 . . . ?
N131 Co2 N131 C132 85.8(3) 3_565 . . . ?
N131 Co2 N131 C132 178.1(2) 2_665 . . . ?
C136 N131 C132 C133 1.8(5) . . . . ?
Co2 N131 C132 C133 -176.6(3) . . . . ?
C136 N131 C132 C143 -178.2(3) . . . . ?
Co2 N131 C132 C143 3.4(4) . . . . ?
N131 C132 C133 C134 -0.8(6) . . . . ?
C143 C132 C133 C134 179.2(4) . . . . ?
C132 C133 C134 C135 0.6(7) . . . . ?
C133 C134 C135 C136 -1.3(8) . . . . ?
C132 N131 C136 C135 -2.5(6) . . . . ?
Co2 N131 C136 C135 175.7(4) . . . . ?
C134 C135 C136 N131 2.3(8) . . . . ?
C145 N141 N142 C143 0.7(3) . . . . ?
C146 N141 N142 C143 177.8(3) . . . . ?
C145 N141 N142 Co2 -172.8(2) . . . . ?
C146 N141 N142 Co2 4.3(5) . . . . ?
N142 Co2 N142 C143 95.0(3) 2_665 . . . ?
N142 Co2 N142 C143 -162.0(2) 3_565 . . . ?
N131 Co2 N142 C143 -85.7(2) 3_565 . . . ?
N131 Co2 N142 C143 21.6(6) 2_665 . . . ?
N131 Co2 N142 C143 6.2(2) . . . . ?
N142 Co2 N142 N141 -91.9(2) 2_665 . . . ?
N142 Co2 N142 N141 11.1(3) 3_565 . . . ?
N131 Co2 N142 N141 87.3(3) 3_565 . . . ?
N131 Co2 N142 N141 -165.3(5) 2_665 . . . ?
N131 Co2 N142 N141 179.3(3) . . . . ?
N141 N142 C143 C144 -0.2(3) . . . . ?
Co2 N142 C143 C144 175.2(2) . . . . ?
N141 N142 C143 C132 177.9(3) . . . . ?
Co2 N142 C143 C132 -6.7(4) . . . . ?
N131 C132 C143 N142 2.3(4) . . . . ?
C133 C132 C143 N142 -177.7(3) . . . . ?
N131 C132 C143 C144 180.0(3) . . . . ?
C133 C132 C143 C144 0.0(6) . . . . ?
N142 C143 C144 C145 -0.3(4) . . . . ?
C132 C143 C144 C145 -178.1(3) . . . . ?
C143 C144 C145 N141 0.7(4) . . . . ?
N142 N141 C145 C144 -0.8(4) . . . . ?
C146 N141 C145 C144 -177.8(3) . . . . ?
N142 N141 C146 C164 -85.4(3) . . . . ?
C145 N141 C146 C164 91.2(4) . . . . ?
N121 C126 C151 C152 6.4(5) . . . . ?
N121 C126 C151 C156 -176.3(3) . . . . ?
C156 C151 C152 C153 3.9(5) . . . . ?
C126 C151 C152 C153 -178.7(3) . . . . ?
C151 C152 C153 C154 -4.1(6) . . . . ?
C152 C153 C154 C155 1.3(5) . . . . ?
C153 C154 C155 C164 -175.6(3) . . . . ?
C153 C154 C155 C156 1.5(5) . . . . ?
C164 C155 C156 C161 -2.6(5) . . . . ?
C154 C155 C156 C161 -179.8(3) . . . . ?
C164 C155 C156 C151 175.5(3) . . . . ?
C154 C155 C156 C151 -1.7(5) . . . . ?
C152 C151 C156 C155 -1.0(5) . . . . ?
C126 C151 C156 C155 -178.4(3) . . . . ?
C152 C151 C156 C161 177.0(3) . . . . ?
C126 C151 C156 C161 -0.4(5) . . . . ?
C155 C156 C161 C162 0.8(5) . . . . ?
C151 C156 C161 C162 -177.3(4) . . . . ?
C156 C161 C162 C163 1.1(6) . . . . ?
C161 C162 C163 C164 -1.0(6) . . . . ?
C162 C163 C164 C155 -0.9(5) . . . . ?
C162 C163 C164 C146 178.8(3) . . . . ?
C156 C155 C164 C163 2.7(5) . . . . ?
C154 C155 C164 C163 179.7(3) . . . . ?
C156 C155 C164 C146 -177.0(3) . . . . ?
C154 C155 C164 C146 0.0(4) . . . . ?
N141 C146 C164 C163 -8.5(4) . . . . ?
N141 C146 C164 C155 171.2(3) . . . . ?
N111 Co1 N211 C216 145.9(12) . . . . ?
N242 Co1 N211 C216 -76.4(4) 15 . . . ?
N122 Co1 N211 C216 90.2(4) . . . . ?
N222 Co1 N211 C216 -175.7(4) . . . . ?
N231 Co1 N211 C216 0.1(4) 15 . . . ?
N111 Co1 N211 C212 -35.7(14) . . . . ?
N242 Co1 N211 C212 102.0(3) 15 . . . ?
N122 Co1 N211 C212 -91.4(3) . . . . ?
N222 Co1 N211 C212 2.6(2) . . . . ?
N231 Co1 N211 C212 178.5(3) 15 . . . ?
C216 N211 C212 C213 -1.8(5) . . . . ?
Co1 N211 C212 C213 179.7(3) . . . . ?
C216 N211 C212 C223 177.7(4) . . . . ?
Co1 N211 C212 C223 -0.9(4) . . . . ?
N211 C212 C213 C214 1.4(6) . . . . ?
C223 C212 C213 C214 -178.0(4) . . . . ?
C212 C213 C214 C215 0.0(7) . . . . ?
C213 C214 C215 C216 -1.0(8) . . . . ?
C212 N211 C216 C215 0.7(7) . . . . ?
Co1 N211 C216 C215 179.1(4) . . . . ?
C214 C215 C216 N211 0.6(8) . . . . ?
C225 N221 N222 C223 -0.4(4) . . . . ?
C226 N221 N222 C223 -175.6(3) . . . . ?
C225 N221 N222 Co1 177.9(3) . . . . ?
C226 N221 N222 Co1 2.8(5) . . . . ?
N211 Co1 N222 C223 -4.0(2) . . . . ?
N111 Co1 N222 C223 172.6(2) . . . . ?
N242 Co1 N222 C223 -93.3(2) 15 . . . ?
N122 Co1 N222 C223 94.6(2) . . . . ?
N231 Co1 N222 C223 -26.2(7) 15 . . . ?
N211 Co1 N222 N221 177.7(4) . . . . ?
N111 Co1 N222 N221 -5.6(4) . . . . ?
N242 Co1 N222 N221 88.4(3) 15 . . . ?
N122 Co1 N222 N221 -83.7(3) . . . . ?
N231 Co1 N222 N221 155.5(5) 15 . . . ?
N221 N222 C223 C224 0.4(4) . . . . ?
Co1 N222 C223 C224 -178.5(2) . . . . ?
N221 N222 C223 C212 -176.0(3) . . . . ?
Co1 N222 C223 C212 5.1(4) . . . . ?
N211 C212 C223 N222 -2.9(5) . . . . ?
C213 C212 C223 N222 176.5(3) . . . . ?
N211 C212 C223 C224 -178.5(3) . . . . ?
C213 C212 C223 C224 0.9(6) . . . . ?
N222 C223 C224 C225 -0.2(4) . . . . ?
C212 C223 C224 C225 175.7(3) . . . . ?
N222 N221 C225 C224 0.3(4) . . . . ?
C226 N221 C225 C224 175.2(3) . . . . ?
C223 C224 C225 N221 -0.1(4) . . . . ?
C225 N221 C226 C251 -89.4(4) . . . . ?
N222 N221 C226 C251 84.9(4) . . . . ?
C236 N231 C232 C233 -1.8(6) . . . . ?
Co1 N231 C232 C233 -175.5(3) 14_455 . . . ?
C236 N231 C232 C243 178.1(4) . . . . ?
Co1 N231 C232 C243 4.5(5) 14_455 . . . ?
N231 C232 C233 C234 2.3(7) . . . . ?
C243 C232 C233 C234 -177.6(4) . . . . ?
C232 C233 C234 C235 -1.6(7) . . . . ?
C233 C234 C235 C236 0.5(7) . . . . ?
C232 N231 C236 C235 0.6(6) . . . . ?
Co1 N231 C236 C235 173.5(3) 14_455 . . . ?
C234 C235 C236 N231 0.0(7) . . . . ?
C245 N241 N242 C243 1.6(5) . . . . ?
C246 N241 N242 C243 175.0(4) . . . . ?
C245 N241 N242 Co1 175.6(4) . . . 14_455 ?
C246 N241 N242 Co1 -11.0(6) . . . 14_455 ?
N241 N242 C243 C244 -0.8(5) . . . . ?
Co1 N242 C243 C244 -176.6(4) 14_455 . . . ?
N241 N242 C243 C232 178.7(4) . . . . ?
Co1 N242 C243 C232 3.0(5) 14_455 . . . ?
N231 C232 C243 N242 -5.0(6) . . . . ?
C233 C232 C243 N242 174.9(4) . . . . ?
N231 C232 C243 C244 174.4(5) . . . . ?
C233 C232 C243 C244 -5.7(8) . . . . ?
N242 C243 C244 C245 -0.2(6) . . . . ?
C232 C243 C244 C245 -179.7(5) . . . . ?
N242 N241 C245 C244 -1.7(6) . . . . ?
C246 N241 C245 C244 -174.7(5) . . . . ?
C243 C244 C245 N241 1.1(7) . . . . ?
C245 N241 C246 C264 89.3(5) . . . . ?
N242 N241 C246 C264 -82.9(4) . . . . ?
N221 C226 C251 C252 3.3(5) . . . . ?
N221 C226 C251 C256 -177.4(3) . . . . ?
C256 C251 C252 C253 2.7(5) . . . . ?
C226 C251 C252 C253 -178.0(3) . . . . ?
C251 C252 C253 C254 0.0(6) . . . . ?
C252 C253 C254 C255 -2.8(5) . . . . ?
C253 C254 C255 C256 2.8(5) . . . . ?
C253 C254 C255 C264 -175.8(3) . . . . ?
C264 C255 C256 C251 178.5(3) . . . . ?
C254 C255 C256 C251 -0.1(5) . . . . ?
C264 C255 C256 C261 -1.5(5) . . . . ?
C254 C255 C256 C261 179.9(3) . . . . ?
C252 C251 C256 C255 -2.6(5) . . . . ?
C226 C251 C256 C255 178.1(3) . . . . ?
C252 C251 C256 C261 177.4(3) . . . . ?
C226 C251 C256 C261 -1.9(5) . . . . ?
C255 C256 C261 C262 1.3(5) . . . . ?
C251 C256 C261 C262 -178.6(3) . . . . ?
C256 C261 C262 C263 -1.5(6) . . . . ?
C261 C262 C263 C264 1.8(6) . . . . ?
C262 C263 C264 C255 -1.9(6) . . . . ?
C262 C263 C264 C246 178.6(3) . . . . ?
C256 C255 C264 C263 1.8(5) . . . . ?
C254 C255 C264 C263 -179.7(3) . . . . ?
C256 C255 C264 C246 -178.7(3) . . . . ?
C254 C255 C264 C246 -0.2(5) . . . . ?
N241 C246 C264 C263 -3.6(5) . . . . ?
N241 C246 C264 C255 176.9(3) . . . . ?

_diffrn_measured_fraction_theta_max 0.993
_diffrn_reflns_theta_full        66.65
_diffrn_measured_fraction_theta_full 0.993
_refine_diff_density_max         1.599
_refine_diff_density_min         -0.367
_refine_diff_density_rms         0.107
#===END