# 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
# start Validation Reply Form
_vrf_CHEMW03_I                   
;
PROBLEM: The ratio of given/expected molecular weight as
calculated from the _atom_site* data lies outside
the range 0.90 <> 1.10
From the CIF: _cell_formula_units_Z 4
From the CIF: _chemical_formula_weight 770.30
TEST: Calculate formula weight from _atom_site_*
atom mass num sum
C 12.01 18.00 216.20
H 1.01 12.00 12.10
N 14.01 6.00 84.04
O 16.00 6.00 95.99
S 32.07 2.00 64.13
Ag 107.87 2.00 215.74
Calculated formula weight 688.20
RESPONSE: This is caused by the given molecular weight being increased
from the atom count to account for two disordered CH3CN omitted by SQUEEZE.
;
# end Validation Reply Form

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C18 H12 Ag2 N6 O6 S2, 2(CH3CN)'
_chemical_formula_sum            'C22 H18 Ag2 N8 O6 S2'
_chemical_formula_weight         770.30

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'
S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ag Ag 0.1306 4.2820 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21/c'

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

_cell_length_a                   12.3349(4)
_cell_length_b                   14.6190(5)
_cell_length_c                   13.7257(5)
_cell_angle_alpha                90.00
_cell_angle_beta                 94.045(3)
_cell_angle_gamma                90.00
_cell_volume                     2468.91(15)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    4855
_cell_measurement_theta_min      4.4208
_cell_measurement_theta_max      62.8771

_exptl_crystal_description       block
_exptl_crystal_colour            brown
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.16
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.072
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1520
_exptl_absorpt_coefficient_mu    14.830
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.1082
_exptl_absorpt_correction_T_max  0.2000
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
CrysAlisPro, Agilent Technologies,
Version 1.171.36.21 (release 14-08-2012 CrysAlis171 .NET)
(compiled Sep 14 2012,17:21:16)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_type           CuK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Xcalibur, Sapphire3, Gemini ultra'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            11929
_diffrn_reflns_av_R_equivalents  0.0746
_diffrn_reflns_av_unetI/netI     0.0550
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         4.42
_diffrn_reflns_theta_max         62.97
_reflns_number_total             3892
_reflns_number_gt                3188
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'CrysAlis Pro (Oxford Diffraction, 2009)'
_computing_cell_refinement       'CrysAlis Pro (Oxford Diffraction, 2009)'
_computing_data_reduction        'CrysAlis Pro (Oxford Diffraction, 2009)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'

_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. 
;

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 -0.007 0.500 0.000 310 90 ' '
2 -0.010 1.000 0.500 308 89 ' '
_platon_squeeze_details          
;
In order to subtract the contribution from the disordered solvent molecules,
the SQUEEZE command was applied.
SQUEEZE removed two disordered CH3CN per formula unit. This valueis calculated
See ref. Bi, Y. F.; Wang, X. T.; Liao, W. P.; Wang, X. F.; Wang, X. W.;
Zhang, H. J.; Gao, S. J. Am. Chem. Soc. 2009, 131, 11650.
;

_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)+(0.1594P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         3892
_refine_ls_number_parameters     307
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0813
_refine_ls_R_factor_gt           0.0730
_refine_ls_wR_factor_ref         0.2173
_refine_ls_wR_factor_gt          0.2049
_refine_ls_goodness_of_fit_ref   1.011
_refine_ls_restrained_S_all      1.011
_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
Ag1 Ag 0.79559(5) 0.47177(4) 0.59703(5) 0.0599(3) Uani 1 1 d . . .
Ag2 Ag 0.70025(5) 0.38129(4) 0.37726(5) 0.0623(3) Uani 1 1 d . . .
S2 S 0.91439(16) 0.53934(13) 0.36994(15) 0.0513(5) Uani 1 1 d . . .
N2 N 0.6018(5) 0.4476(5) 0.6247(4) 0.0499(15) Uani 1 1 d . . .
O6 O 0.8255(5) 0.5313(4) 0.4325(4) 0.0606(15) Uani 1 1 d . . .
N5 N 0.8923(5) 0.3591(4) 0.3577(4) 0.0483(14) Uani 1 1 d . . .
N3 N 0.7500(5) 0.3140(4) 0.6054(4) 0.0492(14) Uani 1 1 d . . .
N6 N 0.7424(6) 0.2256(4) 0.3673(5) 0.0526(15) Uani 1 1 d . . .
C6 C 0.6261(8) 0.1968(6) 0.6443(6) 0.066(2) Uani 1 1 d . . .
H6A H 0.5568 0.1806 0.6607 0.079 Uiso 1 1 calc R . .
C15 C 0.8701(8) 0.1089(6) 0.3305(6) 0.061(2) Uani 1 1 d . . .
H15A H 0.9406 0.0934 0.3172 0.074 Uiso 1 1 calc R . .
C5 C 0.6504(6) 0.2873(5) 0.6280(5) 0.0491(17) Uani 1 1 d . . .
C1 C 0.5309(6) 0.5133(5) 0.6323(5) 0.0487(18) Uani 1 1 d . . .
C14 C 0.8416(6) 0.1990(5) 0.3454(5) 0.0490(17) Uani 1 1 d . . .
C4 C 0.5689(6) 0.3617(5) 0.6378(5) 0.0499(18) Uani 1 1 d . . .
C10 C 0.9650(6) 0.4248(5) 0.3580(5) 0.0496(18) Uani 1 1 d . . .
C13 C 0.9254(7) 0.2736(5) 0.3413(5) 0.0523(19) Uani 1 1 d . . .
C9 C 0.8242(7) 0.2487(6) 0.5981(6) 0.060(2) Uani 1 1 d . . .
H9A H 0.8932 0.2655 0.5815 0.072 Uiso 1 1 calc R . .
C8 C 0.8034(8) 0.1567(6) 0.6141(6) 0.064(2) Uani 1 1 d . . .
H8A H 0.8582 0.1134 0.6094 0.077 Uiso 1 1 calc R . .
C18 C 0.6685(8) 0.1594(6) 0.3728(6) 0.062(2) Uani 1 1 d . . .
H18A H 0.5988 0.1767 0.3873 0.075 Uiso 1 1 calc R . .
C17 C 0.6871(9) 0.0671(7) 0.3585(7) 0.074(3) Uani 1 1 d . . .
H17A H 0.6324 0.0239 0.3640 0.088 Uiso 1 1 calc R . .
C3 C 0.4648(6) 0.3450(6) 0.6662(7) 0.061(2) Uani 1 1 d . . .
H3A H 0.4427 0.2865 0.6825 0.073 Uiso 1 1 calc R . .
C7 C 0.7035(9) 0.1307(6) 0.6363(7) 0.071(3) Uani 1 1 d . . .
H7A H 0.6874 0.0694 0.6460 0.085 Uiso 1 1 calc R . .
C16 C 0.7900(9) 0.0418(6) 0.3359(6) 0.067(2) Uani 1 1 d . . .
H16A H 0.8060 -0.0193 0.3244 0.080 Uiso 1 1 calc R . .
N4 N 1.0712(5) 0.4172(5) 0.3438(5) 0.0552(16) Uani 1 1 d . . .
N1 N 0.4256(5) 0.5041(5) 0.6528(5) 0.0598(17) Uani 1 1 d . . .
C11 C 1.1020(7) 0.3319(6) 0.3248(6) 0.058(2) Uani 1 1 d . . .
H11A H 1.1743 0.3216 0.3131 0.069 Uiso 1 1 d R . .
C12 C 1.0320(7) 0.2578(6) 0.3219(6) 0.065(2) Uani 1 1 d . . .
H12A H 1.0561 0.1995 0.3073 0.078 Uiso 1 1 calc R . .
C2 C 0.3959(8) 0.4186(7) 0.6693(7) 0.071(2) Uani 1 1 d . . .
H2A H 0.3245 0.4079 0.6837 0.085 Uiso 1 1 calc R . .
S1 S 0.58051(17) 0.62848(13) 0.62770(16) 0.0558(5) Uani 1 1 d . . .
O5 O 0.8777(5) 0.5645(5) 0.2712(4) 0.0702(16) Uani 1 1 d . . .
O4 O 1.0045(5) 0.5932(4) 0.4137(6) 0.081(2) Uani 1 1 d . . .
O3 O 0.6704(6) 0.6245(4) 0.5686(6) 0.0772(19) Uani 1 1 d . . .
O2 O 0.4908(5) 0.6828(5) 0.5855(6) 0.087(2) Uani 1 1 d . . .
O1 O 0.6109(6) 0.6474(5) 0.7287(5) 0.0837(19) Uani 1 1 d . . .


_geom_special_details            
; 
 All esds (except the esd in the dihedral angle between two l.s. planes) 
 are estimated using the full covariance matrix.  The cell esds are taken 
 into account individually in the estimation of esds in distances, angles 
 and torsion angles; correlations between esds in cell parameters are only 
 used when they are defined by crystal symmetry.  An approximate (isotropic) 
 treatment of cell esds is used for estimating esds involving l.s. planes. 
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ag1 N3 2.378(6) . ?
Ag1 N4 2.410(7) 3_766 ?
Ag1 N2 2.472(6) . ?
Ag1 O6 2.473(6) . ?
Ag2 N1 2.302(7) 3_666 ?
Ag2 N6 2.341(6) . ?
Ag2 N5 2.424(6) . ?
S2 O6 1.444(6) . ?
S2 O5 1.446(6) . ?
S2 O4 1.457(6) . ?
S2 C10 1.798(8) . ?
N2 C1 1.308(10) . ?
N2 C4 1.336(10) . ?
N5 C10 1.314(10) . ?
N5 C13 1.340(10) . ?
N3 C9 1.330(11) . ?
N3 C5 1.347(10) . ?
N6 C18 1.334(11) . ?
N6 C14 1.338(10) . ?
C6 C7 1.369(13) . ?
C6 C5 1.378(12) . ?
C6 H6A 0.9300 . ?
C15 C14 1.381(11) . ?
C15 C16 1.398(13) . ?
C15 H15A 0.9300 . ?
C5 C4 1.493(11) . ?
C1 N1 1.354(10) . ?
C1 S1 1.795(8) . ?
C14 C13 1.507(11) . ?
C4 C3 1.390(11) . ?
C10 N4 1.343(10) . ?
C13 C12 1.380(11) . ?
C9 C8 1.390(13) . ?
C9 H9A 0.9300 . ?
C8 C7 1.345(13) . ?
C8 H8A 0.9300 . ?
C18 C17 1.386(14) . ?
C18 H18A 0.9300 . ?
C17 C16 1.379(14) . ?
C17 H17A 0.9300 . ?
C3 C2 1.374(14) . ?
C3 H3A 0.9300 . ?
C7 H7A 0.9300 . ?
C16 H16A 0.9300 . ?
N4 C11 1.335(11) . ?
N4 Ag1 2.410(7) 3_766 ?
N1 C2 1.326(12) . ?
N1 Ag2 2.302(7) 3_666 ?
C11 C12 1.383(13) . ?
C11 H11A 0.9300 . ?
C12 H12A 0.9300 . ?
C2 H2A 0.9300 . ?
S1 O3 1.421(7) . ?
S1 O1 1.437(7) . ?
S1 O2 1.449(7) . ?

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
N3 Ag1 N4 142.6(2) . 3_766 ?
N3 Ag1 N2 67.6(2) . . ?
N4 Ag1 N2 133.5(2) 3_766 . ?
N3 Ag1 O6 115.89(19) . . ?
N4 Ag1 O6 85.9(2) 3_766 . ?
N2 Ag1 O6 113.5(2) . . ?
N1 Ag2 N6 147.9(2) 3_666 . ?
N1 Ag2 N5 136.8(2) 3_666 . ?
N6 Ag2 N5 69.0(2) . . ?
O6 S2 O5 112.2(4) . . ?
O6 S2 O4 112.8(4) . . ?
O5 S2 O4 115.3(4) . . ?
O6 S2 C10 105.2(3) . . ?
O5 S2 C10 103.8(4) . . ?
O4 S2 C10 106.3(4) . . ?
C1 N2 C4 117.9(7) . . ?
C1 N2 Ag1 124.5(5) . . ?
C4 N2 Ag1 117.5(5) . . ?
S2 O6 Ag1 137.7(4) . . ?
C10 N5 C13 117.8(7) . . ?
C10 N5 Ag2 125.0(5) . . ?
C13 N5 Ag2 117.1(5) . . ?
C9 N3 C5 117.0(7) . . ?
C9 N3 Ag1 121.7(6) . . ?
C5 N3 Ag1 121.0(5) . . ?
C18 N6 C14 116.2(7) . . ?
C18 N6 Ag2 123.1(6) . . ?
C14 N6 Ag2 120.4(5) . . ?
C7 C6 C5 120.3(9) . . ?
C7 C6 H6A 119.9 . . ?
C5 C6 H6A 119.9 . . ?
C14 C15 C16 118.2(8) . . ?
C14 C15 H15A 120.9 . . ?
C16 C15 H15A 120.9 . . ?
N3 C5 C6 121.8(7) . . ?
N3 C5 C4 116.2(7) . . ?
C6 C5 C4 122.0(8) . . ?
N2 C1 N1 126.9(8) . . ?
N2 C1 S1 117.0(6) . . ?
N1 C1 S1 115.8(6) . . ?
N6 C14 C15 123.8(7) . . ?
N6 C14 C13 116.0(7) . . ?
C15 C14 C13 120.1(7) . . ?
N2 C4 C3 119.9(8) . . ?
N2 C4 C5 117.4(7) . . ?
C3 C4 C5 122.6(7) . . ?
N5 C10 N4 127.7(7) . . ?
N5 C10 S2 116.1(6) . . ?
N4 C10 S2 116.0(6) . . ?
N5 C13 C12 119.6(8) . . ?
N5 C13 C14 116.8(7) . . ?
C12 C13 C14 123.6(7) . . ?
N3 C9 C8 123.2(9) . . ?
N3 C9 H9A 118.4 . . ?
C8 C9 H9A 118.4 . . ?
C7 C8 C9 119.4(8) . . ?
C7 C8 H8A 120.3 . . ?
C9 C8 H8A 120.3 . . ?
N6 C18 C17 125.2(10) . . ?
N6 C18 H18A 117.4 . . ?
C17 C18 H18A 117.4 . . ?
C16 C17 C18 117.2(9) . . ?
C16 C17 H17A 121.4 . . ?
C18 C17 H17A 121.4 . . ?
C2 C3 C4 117.2(8) . . ?
C2 C3 H3A 121.4 . . ?
C4 C3 H3A 121.4 . . ?
C8 C7 C6 118.3(9) . . ?
C8 C7 H7A 120.8 . . ?
C6 C7 H7A 120.8 . . ?
C17 C16 C15 119.3(8) . . ?
C17 C16 H16A 120.4 . . ?
C15 C16 H16A 120.4 . . ?
C11 N4 C10 113.6(7) . . ?
C11 N4 Ag1 119.9(5) . 3_766 ?
C10 N4 Ag1 123.0(5) . 3_766 ?
C2 N1 C1 114.2(8) . . ?
C2 N1 Ag2 121.7(6) . 3_666 ?
C1 N1 Ag2 122.4(5) . 3_666 ?
N4 C11 C12 123.5(8) . . ?
N4 C11 H11A 118.3 . . ?
C12 C11 H11A 118.2 . . ?
C13 C12 C11 117.8(8) . . ?
C13 C12 H12A 121.1 . . ?
C11 C12 H12A 121.1 . . ?
N1 C2 C3 123.6(9) . . ?
N1 C2 H2A 118.2 . . ?
C3 C2 H2A 118.2 . . ?
O3 S1 O1 113.4(5) . . ?
O3 S1 O2 113.5(5) . . ?
O1 S1 O2 114.8(5) . . ?
O3 S1 C1 105.3(4) . . ?
O1 S1 C1 102.3(4) . . ?
O2 S1 C1 106.0(4) . . ?

_diffrn_measured_fraction_theta_max 0.975
_diffrn_reflns_theta_full        62.97
_diffrn_measured_fraction_theta_full 0.975
_refine_diff_density_max         1.468
_refine_diff_density_min         -1.083
_refine_diff_density_rms         0.178

_database_code_depnum_ccdc_archive 'CCDC 1015423'
#######################################################################
#
#                 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         'C18 H16 Cl2 Cu N6 O11'
_chemical_formula_sum            'C18 H16 Cl2 Cu N6 O11'
_chemical_formula_weight         626.81

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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21/c'
_symmetry_space_group_name_Hall  '-P 2ybc'

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

_cell_length_a                   12.3685(9)
_cell_length_b                   15.4917(12)
_cell_length_c                   12.9541(10)
_cell_angle_alpha                90.00
_cell_angle_beta                 111.2950(10)
_cell_angle_gamma                90.00
_cell_volume                     2312.7(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    4044
_cell_measurement_theta_min      2.53
_cell_measurement_theta_max      25.10

_exptl_crystal_description       block
_exptl_crystal_colour            blue
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.18
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.800
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1268
_exptl_absorpt_coefficient_mu    1.250
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.7452
_exptl_absorpt_correction_T_max  0.8063
_exptl_absorpt_process_details   '(SADABS; Bruker, 2001)'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      296(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  'Bruker APEXII CCD area-detector'
_diffrn_measurement_method       'φ and ω'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            16010
_diffrn_reflns_av_R_equivalents  0.0279
_diffrn_reflns_av_unetI/netI     0.0263
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         2.14
_diffrn_reflns_theta_max         25.00
_reflns_number_total             4044
_reflns_number_gt                3303
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'APEX2 (Bruker, 2007)'
_computing_cell_refinement       'SAINT-Plus (Bruker, 2007)'
_computing_data_reduction        'SAINT-Plus (Bruker, 2007)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'

_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)+(0.1088P)²+1.8000P] 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         4044
_refine_ls_number_parameters     346
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0642
_refine_ls_R_factor_gt           0.0531
_refine_ls_wR_factor_ref         0.1643
_refine_ls_wR_factor_gt          0.1558
_refine_ls_goodness_of_fit_ref   1.068
_refine_ls_restrained_S_all      1.068
_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
Cu1 Cu 0.80442(4) 0.01822(3) 0.33423(4) 0.0331(2) Uani 1 1 d . . .
O11 O 0.9894(3) 0.0251(2) 0.3939(3) 0.0449(7) Uani 1 1 d . . .
N5 N 0.8171(3) -0.09869(19) 0.2763(3) 0.0339(7) Uani 1 1 d . . .
N3 N 0.7292(3) -0.0090(2) 0.4490(3) 0.0359(7) Uani 1 1 d . . .
N2 N 0.8041(3) 0.1350(2) 0.3955(3) 0.0331(7) Uani 1 1 d . . .
N6 N 0.7103(3) 0.0371(2) 0.1687(2) 0.0327(7) Uani 1 1 d . . .
O10 O 0.8795(3) 0.2036(2) 0.2807(3) 0.0553(8) Uani 1 1 d . . .
N4 N 0.8831(4) -0.2404(2) 0.2891(3) 0.0509(10) Uani 1 1 d . . .
H4A H 0.9147 -0.2846 0.3286 0.061 Uiso 1 1 calc R . .
C10 C 0.8735(4) -0.1658(3) 0.3436(4) 0.0403(9) Uani 1 1 d . . .
O9 O 0.9128(3) -0.16129(19) 0.4444(2) 0.0507(8) Uani 1 1 d . . .
C13 C 0.7772(3) -0.1065(2) 0.1651(3) 0.0345(8) Uani 1 1 d . . .
C12 C 0.7934(4) -0.1808(3) 0.1127(4) 0.0448(10) Uani 1 1 d . . .
H12A H 0.7690 -0.1844 0.0359 0.054 Uiso 1 1 calc R . .
N1 N 0.8564(3) 0.2802(2) 0.4209(3) 0.0499(9) Uani 1 1 d . . .
H1A H 0.8787 0.3267 0.3983 0.060 Uiso 1 1 calc R . .
C5 C 0.7238(3) 0.0600(3) 0.5106(3) 0.0374(9) Uani 1 1 d . . .
C14 C 0.7143(3) -0.0305(2) 0.1046(3) 0.0338(8) Uani 1 1 d . . .
C1 C 0.8484(4) 0.2059(3) 0.3600(4) 0.0411(9) Uani 1 1 d . . .
C15 C 0.6606(4) -0.0271(3) -0.0106(4) 0.0443(10) Uani 1 1 d . . .
H15A H 0.6657 -0.0731 -0.0547 0.053 Uiso 1 1 calc R . .
C4 C 0.7739(3) 0.1400(3) 0.4844(3) 0.0378(9) Uani 1 1 d . . .
C18 C 0.6502(4) 0.1067(3) 0.1221(3) 0.0393(9) Uani 1 1 d . . .
H18A H 0.6462 0.1523 0.1673 0.047 Uiso 1 1 calc R . .
C3 C 0.7907(4) 0.2153(3) 0.5474(4) 0.0521(11) Uani 1 1 d . . .
H3A H 0.7739 0.2172 0.6118 0.062 Uiso 1 1 calc R . .
C7 C 0.6278(5) -0.0240(4) 0.6052(5) 0.0629(14) Uani 1 1 d . . .
H7A H 0.5946 -0.0296 0.6587 0.076 Uiso 1 1 calc R . .
C9 C 0.6830(4) -0.0833(3) 0.4644(4) 0.0465(10) Uani 1 1 d . . .
H9A H 0.6857 -0.1307 0.4214 0.056 Uiso 1 1 calc R . .
C16 C 0.5994(4) 0.0472(3) -0.0575(4) 0.0486(11) Uani 1 1 d . . .
H16A H 0.5627 0.0513 -0.1339 0.058 Uiso 1 1 calc R . .
C17 C 0.5932(4) 0.1140(3) 0.0087(4) 0.0465(10) Uani 1 1 d . . .
H17A H 0.5514 0.1636 -0.0218 0.056 Uiso 1 1 calc R . .
C6 C 0.6743(4) 0.0552(3) 0.5900(4) 0.0519(11) Uani 1 1 d . . .
H6A H 0.6719 0.1032 0.6322 0.062 Uiso 1 1 calc R . .
C11 C 0.8468(4) -0.2483(3) 0.1792(4) 0.0529(12) Uani 1 1 d . . .
H11B H 0.8579 -0.3000 0.1479 0.064 Uiso 1 1 calc R . .
C8 C 0.6314(4) -0.0924(3) 0.5417(4) 0.0548(12) Uani 1 1 d . . .
H8A H 0.5994 -0.1450 0.5502 0.066 Uiso 1 1 calc R . .
C2 C 0.8318(4) 0.2843(3) 0.5121(5) 0.0588(13) Uani 1 1 d . . .
H2A H 0.8433 0.3357 0.5518 0.071 Uiso 1 1 calc R . .
Cl2 Cl 0.07883(12) 0.02262(7) 0.15367(12) 0.0579(3) Uani 1 1 d . . .
Cl1 Cl 0.47696(11) 0.23988(8) 0.24091(9) 0.0549(3) Uani 1 1 d . . .
O8 O 0.1018(4) 0.0640(3) 0.2587(3) 0.0773(12) Uani 1 1 d . A .
O7 O 0.0868(4) 0.0885(3) 0.0752(3) 0.0792(12) Uani 1 1 d . A .
O6 O -0.0460(5) -0.0064(4) 0.1118(5) 0.1011(17) Uani 1 1 d . A .
O5A O 0.1384(11) -0.0555(8) 0.1676(9) 0.101(4) Uiso 0.575(15) 1 d P A 1
O3A O 0.4265(7) 0.2234(5) 0.1256(6) 0.063(2) Uiso 0.575(15) 1 d P A 1
O2A O 0.5270(9) 0.1761(7) 0.3204(10) 0.093(3) Uiso 0.575(15) 1 d P A 1
O4A O 0.4159(7) 0.3063(7) 0.2752(7) 0.074(2) Uiso 0.575(15) 1 d P A 1
O5B O 0.1640(8) -0.0407(6) 0.1479(7) 0.046(2) Uiso 0.425(15) 1 d P A 2
O3B O 0.3792(14) 0.2107(9) 0.1507(11) 0.099(4) Uiso 0.425(15) 1 d P A 2
O2B O 0.5073(9) 0.1487(7) 0.2783(10) 0.065(3) Uiso 0.425(15) 1 d P A 2
O4B O 0.4108(9) 0.2726(9) 0.3020(9) 0.069(3) Uiso 0.425(15) 1 d P A 2
O1 O 0.5807(5) 0.2852(4) 0.2476(5) 0.1156(19) Uani 1 1 d . A .
HWA H 1.018(11) 0.038(7) 0.345(10) 0.173 Uiso 1 1 d . . .
HWB H 1.009(10) 0.070(7) 0.434(9) 0.173 Uiso 1 1 d . . .


_geom_special_details            
; 
 All esds (except the esd in the dihedral angle between two l.s. planes) 
 are estimated using the full covariance matrix.  The cell esds are taken 
 into account individually in the estimation of esds in distances, angles 
 and torsion angles; correlations between esds in cell parameters are only 
 used when they are defined by crystal symmetry.  An approximate (isotropic) 
 treatment of cell esds is used for estimating esds involving l.s. planes. 
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cu1 N2 1.977(3) . ?
Cu1 N5 1.988(3) . ?
Cu1 N6 2.056(3) . ?
Cu1 N3 2.064(3) . ?
Cu1 O11 2.136(3) . ?
O11 HWA 0.86(12) . ?
O11 HWB 0.85(11) . ?
N5 C13 1.347(5) . ?
N5 C10 1.373(5) . ?
N3 C9 1.332(5) . ?
N3 C5 1.350(5) . ?
N2 C4 1.336(5) . ?
N2 C1 1.379(5) . ?
N6 C18 1.323(5) . ?
N6 C14 1.349(5) . ?
O10 C1 1.221(5) . ?
N4 C11 1.333(6) . ?
N4 C10 1.382(5) . ?
N4 H4A 0.8600 . ?
C10 O9 1.218(5) . ?
C13 C12 1.388(6) . ?
C13 C14 1.471(6) . ?
C12 C11 1.364(6) . ?
C12 H12A 0.9300 . ?
N1 C2 1.323(6) . ?
N1 C1 1.378(6) . ?
N1 H1A 0.8600 . ?
C5 C6 1.376(6) . ?
C5 C4 1.479(6) . ?
C14 C15 1.397(6) . ?
C15 C16 1.389(7) . ?
C15 H15A 0.9300 . ?
C4 C3 1.395(6) . ?
C18 C17 1.385(6) . ?
C18 H18A 0.9300 . ?
C3 C2 1.335(7) . ?
C3 H3A 0.9300 . ?
C7 C8 1.352(8) . ?
C7 C6 1.399(8) . ?
C7 H7A 0.9300 . ?
C9 C8 1.376(7) . ?
C9 H9A 0.9300 . ?
C16 C17 1.364(7) . ?
C16 H16A 0.9300 . ?
C17 H17A 0.9300 . ?
C6 H6A 0.9300 . ?
C11 H11B 0.9300 . ?
C8 H8A 0.9300 . ?
C2 H2A 0.9300 . ?
Cl2 O5A 1.394(11) . ?
Cl2 O8 1.436(4) . ?
Cl2 O5B 1.461(9) . ?
Cl2 O7 1.469(4) . ?
Cl2 O6 1.507(5) . ?
Cl1 O2A 1.399(9) . ?
Cl1 O3B 1.416(14) . ?
Cl1 O3A 1.418(7) . ?
Cl1 O4B 1.422(10) . ?
Cl1 O1 1.437(5) . ?
Cl1 O4A 1.439(8) . ?
Cl1 O2B 1.496(10) . ?

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
N2 Cu1 N5 175.88(13) . . ?
N2 Cu1 N6 101.86(13) . . ?
N5 Cu1 N6 80.13(13) . . ?
N2 Cu1 N3 80.24(13) . . ?
N5 Cu1 N3 101.76(13) . . ?
N6 Cu1 N3 123.21(13) . . ?
N2 Cu1 O11 88.09(12) . . ?
N5 Cu1 O11 87.80(12) . . ?
N6 Cu1 O11 119.82(13) . . ?
N3 Cu1 O11 116.97(13) . . ?
Cu1 O11 HWA 115(8) . . ?
Cu1 O11 HWB 107(8) . . ?
HWA O11 HWB 99(9) . . ?
C13 N5 C10 121.0(3) . . ?
C13 N5 Cu1 115.9(2) . . ?
C10 N5 Cu1 122.7(3) . . ?
C9 N3 C5 118.6(4) . . ?
C9 N3 Cu1 128.0(3) . . ?
C5 N3 Cu1 113.3(3) . . ?
C4 N2 C1 120.7(3) . . ?
C4 N2 Cu1 116.2(3) . . ?
C1 N2 Cu1 122.4(3) . . ?
C18 N6 C14 119.4(3) . . ?
C18 N6 Cu1 127.1(3) . . ?
C14 N6 Cu1 113.5(3) . . ?
C11 N4 C10 124.4(4) . . ?
C11 N4 H4A 117.8 . . ?
C10 N4 H4A 117.8 . . ?
O9 C10 N5 123.4(4) . . ?
O9 C10 N4 121.4(4) . . ?
N5 C10 N4 115.2(4) . . ?
N5 C13 C12 122.4(4) . . ?
N5 C13 C14 114.5(3) . . ?
C12 C13 C14 123.1(4) . . ?
C11 C12 C13 116.7(4) . . ?
C11 C12 H12A 121.6 . . ?
C13 C12 H12A 121.6 . . ?
C2 N1 C1 124.1(4) . . ?
C2 N1 H1A 118.0 . . ?
C1 N1 H1A 118.0 . . ?
N3 C5 C6 122.0(4) . . ?
N3 C5 C4 114.4(3) . . ?
C6 C5 C4 123.6(4) . . ?
N6 C14 C15 121.3(4) . . ?
N6 C14 C13 115.1(3) . . ?
C15 C14 C13 123.7(4) . . ?
O10 C1 N1 121.9(4) . . ?
O10 C1 N2 122.8(4) . . ?
N1 C1 N2 115.3(4) . . ?
C16 C15 C14 118.0(4) . . ?
C16 C15 H15A 121.0 . . ?
C14 C15 H15A 121.0 . . ?
N2 C4 C3 121.6(4) . . ?
N2 C4 C5 114.9(3) . . ?
C3 C4 C5 123.5(4) . . ?
N6 C18 C17 122.4(4) . . ?
N6 C18 H18A 118.8 . . ?
C17 C18 H18A 118.8 . . ?
C2 C3 C4 117.6(4) . . ?
C2 C3 H3A 121.2 . . ?
C4 C3 H3A 121.2 . . ?
C8 C7 C6 119.7(5) . . ?
C8 C7 H7A 120.2 . . ?
C6 C7 H7A 120.2 . . ?
N3 C9 C8 122.4(4) . . ?
N3 C9 H9A 118.8 . . ?
C8 C9 H9A 118.8 . . ?
C17 C16 C15 120.0(4) . . ?
C17 C16 H16A 120.0 . . ?
C15 C16 H16A 120.0 . . ?
C16 C17 C18 118.8(4) . . ?
C16 C17 H17A 120.6 . . ?
C18 C17 H17A 120.6 . . ?
C5 C6 C7 118.0(5) . . ?
C5 C6 H6A 121.0 . . ?
C7 C6 H6A 121.0 . . ?
N4 C11 C12 120.1(4) . . ?
N4 C11 H11B 119.9 . . ?
C12 C11 H11B 119.9 . . ?
C7 C8 C9 119.3(5) . . ?
C7 C8 H8A 120.4 . . ?
C9 C8 H8A 120.4 . . ?
N1 C2 C3 120.4(4) . . ?
N1 C2 H2A 119.8 . . ?
C3 C2 H2A 119.8 . . ?
O5A Cl2 O8 110.6(5) . . ?
O5A Cl2 O5B 21.1(5) . . ?
O8 Cl2 O5B 116.7(4) . . ?
O5A Cl2 O7 121.9(6) . . ?
O8 Cl2 O7 107.8(2) . . ?
O5B Cl2 O7 101.6(5) . . ?
O5A Cl2 O6 102.2(6) . . ?
O8 Cl2 O6 107.4(3) . . ?
O5B Cl2 O6 116.4(4) . . ?
O7 Cl2 O6 106.0(3) . . ?
O2A Cl1 O3B 113.5(9) . . ?
O2A Cl1 O3A 123.8(7) . . ?
O3B Cl1 O3A 32.4(6) . . ?
O2A Cl1 O4B 91.9(6) . . ?
O3B Cl1 O4B 94.6(8) . . ?
O3A Cl1 O4B 121.9(5) . . ?
O2A Cl1 O1 98.8(5) . . ?
O3B Cl1 O1 133.0(8) . . ?
O3A Cl1 O1 101.2(5) . . ?
O4B Cl1 O1 118.3(6) . . ?
O2A Cl1 O4A 114.9(5) . . ?
O3B Cl1 O4A 95.5(7) . . ?
O3A Cl1 O4A 112.0(4) . . ?
O4B Cl1 O4A 26.0(5) . . ?
O1 Cl1 O4A 100.9(5) . . ?
O2A Cl1 O2B 26.2(5) . . ?
O3B Cl1 O2B 90.3(8) . . ?
O3A Cl1 O2B 97.7(6) . . ?
O4B Cl1 O2B 106.5(7) . . ?
O1 Cl1 O2B 109.1(5) . . ?
O4A Cl1 O2B 132.4(5) . . ?

_diffrn_measured_fraction_theta_max 0.994
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.994
_refine_diff_density_max         0.985
_refine_diff_density_min         -1.000
_refine_diff_density_rms         0.099
_database_code_depnum_ccdc_archive 'CCDC 1015424'
#######################################################################
#
#                 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_3
# start Validation Reply Form
_vrf_CHEMW03_I                   
;
PROBLEM: The ratio of given/expected molecular weight as
            calculated from the _atom_site* data lies outside
            the range 0.90 <> 1.10
           From the CIF: _cell_formula_units_Z                   16
           From the CIF: _chemical_formula_weight           681.06
           TEST: Calculate formula weight from _atom_site_*
           atom     mass    num     sum
           C        12.01   18.00  216.20
           H         1.01   12.00   12.10
           Cl       35.45    1.00   35.45
           Co       58.93    1.00   58.93
           N        14.01    6.00   84.04
           O        16.00    4.00   64.00
           S        32.07    4.00  128.26
           Calculated formula weight              598.98
RESPONSE: This is caused by the given molecular weight being increased
from the atom count to account for two disordered CH3OH and one H2O omitted by SQUEEZE.
;
# end Validation Reply Form

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C18 H12 Cl Co N6 O4 S4, 2(CH4O), H2O'
_chemical_formula_sum            'C20 H22 Cl Co N6 O7 S4'
_chemical_formula_weight         681.06

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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Tetragonal
_symmetry_space_group_name_H-M   'I4/m '

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

_cell_length_a                   18.573(16)
_cell_length_b                   18.573(16)
_cell_length_c                   31.35(5)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     10814(22)
_cell_formula_units_Z            16
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    6114
_cell_measurement_theta_min      2.53
_cell_measurement_theta_max      24.97

_exptl_crystal_description       block
_exptl_crystal_colour            black
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.22
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.673
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             5568
_exptl_absorpt_coefficient_mu    1.096
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.7490
_exptl_absorpt_correction_T_max  0.7946
_exptl_absorpt_process_details   sadabs

_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  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            30193
_diffrn_reflns_av_R_equivalents  0.0558
_diffrn_reflns_av_unetI/netI     0.0399
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_theta_min         1.27
_diffrn_reflns_theta_max         25.01
_reflns_number_total             4884
_reflns_number_gt                3475
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_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 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. 
Because the ClO4- disorded, some refine orders have been used, such as isor, sadi,simu
et. Although the ClO4- do not refined to the standard model, we have confirmed with IR. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0000P)²+350.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         4884
_refine_ls_number_parameters     265
_refine_ls_number_restraints     55
_refine_ls_R_factor_all          0.1386
_refine_ls_R_factor_gt           0.1186
_refine_ls_wR_factor_ref         0.2626
_refine_ls_wR_factor_gt          0.2553
_refine_ls_goodness_of_fit_ref   1.187
_refine_ls_restrained_S_all      1.288
_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 0.17794(3) 0.41779(3) 0.17216(2) 0.04211(16) Uani 1 1 d . . .
C1 C 0.1310(3) 0.5284(3) 0.10874(17) 0.0579(16) Uani 1 1 d . . .
H1 H 0.1050 0.4920 0.0954 0.069 Uiso 1 1 calc R . .
C2 C 0.1298(3) 0.5970(3) 0.09159(19) 0.0730(19) Uani 1 1 d . . .
H2 H 0.1024 0.6067 0.0674 0.088 Uiso 1 1 calc R . .
C3 C 0.1682(3) 0.6495(3) 0.1100(2) 0.077(2) Uani 1 1 d . . .
H3 H 0.1679 0.6956 0.0985 0.093 Uiso 1 1 calc R . .
C4 C 0.2072(3) 0.6355(3) 0.14520(19) 0.0631(17) Uani 1 1 d . . .
H4 H 0.2339 0.6718 0.1581 0.076 Uiso 1 1 calc R . .
C5 C 0.2074(2) 0.5658(2) 0.16222(16) 0.0497(14) Uani 1 1 d . . .
C6 C 0.2449(2) 0.5445(2) 0.19994(15) 0.0465(13) Uani 1 1 d . . .
C7 C 0.2857(3) 0.5862(3) 0.2262(2) 0.0680(18) Uani 1 1 d . . .
H7 H 0.2940 0.6344 0.2198 0.082 Uiso 1 1 calc R . .
C8 C 0.3136(3) 0.5567(3) 0.2616(2) 0.080(2) Uani 1 1 d . . .
H8 H 0.3431 0.5853 0.2786 0.096 Uiso 1 1 calc R . .
N1 N 0.3019(2) 0.4895(3) 0.27384(15) 0.0730(16) Uani 1 1 d . . .
C10 C 0.3262(2) 0.4161(3) 0.13295(18) 0.0564(16) Uani 1 1 d . . .
H10 H 0.3420 0.4420 0.1565 0.068 Uiso 1 1 calc R . .
C11 C 0.3742(3) 0.3998(3) 0.10148(19) 0.0700(18) Uani 1 1 d . . .
H11 H 0.4215 0.4161 0.1031 0.084 Uiso 1 1 calc R . .
C12 C 0.3525(3) 0.3594(4) 0.0676(2) 0.084(2) Uani 1 1 d . . .
H12 H 0.3847 0.3481 0.0460 0.100 Uiso 1 1 calc R . .
C13 C 0.2830(3) 0.3358(4) 0.0658(2) 0.079(2) Uani 1 1 d . . .
H13 H 0.2681 0.3061 0.0436 0.095 Uiso 1 1 calc R . .
C14 C 0.2348(3) 0.3565(3) 0.09729(17) 0.0558(15) Uani 1 1 d . . .
C15 C 0.1209(4) 0.2929(4) 0.0710(2) 0.100(2) Uani 1 1 d . . .
H15 H 0.1445 0.2734 0.0476 0.120 Uiso 1 1 calc R . .
C16 C 0.0502(4) 0.2786(4) 0.0775(3) 0.119(3) Uani 1 1 d . . .
H16 H 0.0261 0.2489 0.0584 0.143 Uiso 1 1 calc R . .
N4 N 0.0139(3) 0.3059(3) 0.1107(2) 0.102(2) Uani 1 1 d . . .
C51 C 0.1578(3) 0.3361(3) 0.09907(18) 0.0622(16) Uani 1 1 d . . .
Cl2 Cl 0.0000 0.0000 0.30248(12) 0.0851(11) Uani 1 4 d SD . .
C9 C 0.2622(3) 0.4490(3) 0.24724(18) 0.0571(15) Uani 1 1 d . . .
N2 N 0.23361(19) 0.47315(19) 0.21099(12) 0.0442(11) Uani 1 1 d . . .
N3 N 0.16808(19) 0.51299(18) 0.14355(12) 0.0441(11) Uani 1 1 d . . .
C17 C 0.0513(3) 0.3472(3) 0.13813(19) 0.0617(16) Uani 1 1 d . . .
N5 N 0.1224(2) 0.36358(19) 0.13339(14) 0.0511(12) Uani 1 1 d . . .
N6 N 0.2576(2) 0.3960(2) 0.13101(13) 0.0493(11) Uani 1 1 d . . .
Cl1 Cl 0.2341 0.1388 0.0000 0.126 Uani 1 2 d SD . .
O1 O 0.2298 0.1050 0.0344 0.123 Uani 1 1 d DU . .
O2 O 0.2830 0.1891 0.0000 0.129 Uani 1 2 d SDU . .
O3 O 0.1712 0.1785 0.0000 0.129 Uani 1 2 d SDU . .
O5 O 0.0443 0.0521 0.2951 0.124 Uani 0.75 1 d PD . .
O4 O 0.0000 0.0000 0.3463 0.172 Uani 1 4 d SD . .
S1 S 0.08047(7) 0.43977(7) 0.21148(5) 0.0602(4) Uani 1 1 d . . .
S2 S 0.00470(7) 0.37959(9) 0.18070(6) 0.0802(5) Uani 1 1 d . . .
S3 S 0.20392(8) 0.31707(7) 0.20799(5) 0.0672(4) Uani 1 1 d . . .
S4 S 0.24153(9) 0.36213(8) 0.26363(5) 0.0765(5) Uani 1 1 d . . .
Cl3 Cl 0.0000 0.5000 1.0000 0.126 Uani 1 4 d SD . .
O8 O 0.0757 0.5133 1.0000 0.129 Uani 1 2 d SDU . .
O6 O -0.0253 0.5383 1.0362 0.132 Uani 0.25 1 d PD . .
O7 O 0.0000 0.5000 0.9546 0.127 Uani 0.50 2 d SPDU . .


_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 N2 1.900(4) . ?
Co1 N5 1.885(4) . ?
Co1 N3 1.991(4) . ?
Co1 N6 2.004(4) . ?
Co1 S1 2.228(2) . ?
Co1 S3 2.235(2) . ?
C1 N3 1.321(7) . ?
C1 C2 1.384(8) . ?
C1 H1 0.9300 . ?
C2 C3 1.339(8) . ?
C2 H2 0.9300 . ?
C3 C4 1.344(9) . ?
C3 H3 0.9300 . ?
C4 C5 1.400(7) . ?
C4 H4 0.9300 . ?
C5 N3 1.355(6) . ?
C5 C6 1.429(7) . ?
C6 N2 1.385(6) . ?
C6 C7 1.361(7) . ?
C7 C8 1.342(9) . ?
C7 H7 0.9300 . ?
C8 N1 1.324(8) . ?
C8 H8 0.9300 . ?
N1 C9 1.343(7) . ?
C10 N6 1.329(6) . ?
C10 C11 1.364(8) . ?
C10 H10 0.9300 . ?
C11 C12 1.360(9) . ?
C11 H11 0.9300 . ?
C12 C13 1.364(9) . ?
C12 H12 0.9300 . ?
C13 C14 1.388(8) . ?
C13 H13 0.9300 . ?
C14 N6 1.354(7) . ?
C14 C51 1.480(7) . ?
C15 C51 1.373(9) . ?
C15 C16 1.356(10) . ?
C15 H15 0.9300 . ?
C16 N4 1.337(10) . ?
C16 H16 0.9300 . ?
N4 C17 1.346(8) . ?
C51 N5 1.360(7) . ?
Cl2 O5 1.2907(13) . ?
Cl2 O5 1.2908(13) 3 ?
Cl2 O5 1.2908(13) 2 ?
Cl2 O5 1.2908(13) 4 ?
Cl2 O4 1.373(4) . ?
C9 N2 1.332(7) . ?
C9 S4 1.737(6) . ?
C17 N5 1.365(6) . ?
C17 S2 1.700(6) . ?
Cl1 O1 1.2514 11 ?
Cl1 O1 1.2514 . ?
Cl1 O2 1.3031 . ?
Cl1 O3 1.3827 . ?
O5 O5 1.7959 4 ?
O5 O5 1.7959 2 ?
S1 S2 2.040(3) . ?
S3 S4 2.057(3) . ?
Cl3 O6 1.4196 9_567 ?
Cl3 O6 1.4196 11_557 ?
Cl3 O6 1.4196 3_565 ?
Cl3 O6 1.4197 . ?
Cl3 O7 1.4241 9_567 ?
Cl3 O7 1.4241 . ?
Cl3 O8 1.4283 . ?
Cl3 O8 1.4284 9_567 ?
O8 O6 1.7558 9_567 ?
O8 O6 1.7558 3_565 ?
O6 O7 0.9005 9_567 ?
O6 O6 1.7056 3_565 ?
O6 O8 1.7559 9_567 ?
O7 O6 0.9005 11_557 ?
O7 O6 0.9005 9_567 ?

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
N2 Co1 N5 179.52(17) . . ?
N2 Co1 N3 81.84(17) . . ?
N5 Co1 N3 97.68(17) . . ?
N2 Co1 N6 96.89(17) . . ?
N5 Co1 N6 83.15(18) . . ?
N3 Co1 N6 87.56(16) . . ?
N2 Co1 S1 89.34(14) . . ?
N5 Co1 S1 90.59(15) . . ?
N3 Co1 S1 90.68(12) . . ?
N6 Co1 S1 173.20(12) . . ?
N2 Co1 S3 90.77(14) . . ?
N5 Co1 S3 89.71(14) . . ?
N3 Co1 S3 171.75(12) . . ?
N6 Co1 S3 89.71(14) . . ?
S1 Co1 S3 92.91(8) . . ?
N3 C1 C2 121.9(5) . . ?
N3 C1 H1 119.0 . . ?
C2 C1 H1 119.0 . . ?
C3 C2 C1 119.6(6) . . ?
C3 C2 H2 120.2 . . ?
C1 C2 H2 120.2 . . ?
C4 C3 C2 120.0(5) . . ?
C4 C3 H3 120.0 . . ?
C2 C3 H3 120.0 . . ?
C3 C4 C5 119.5(5) . . ?
C3 C4 H4 120.2 . . ?
C5 C4 H4 120.2 . . ?
N3 C5 C4 120.2(5) . . ?
N3 C5 C6 114.8(4) . . ?
C4 C5 C6 124.9(4) . . ?
N2 C6 C7 118.5(5) . . ?
N2 C6 C5 113.4(4) . . ?
C7 C6 C5 127.9(5) . . ?
C8 C7 C6 118.9(5) . . ?
C8 C7 H7 120.6 . . ?
C6 C7 H7 120.6 . . ?
N1 C8 C7 124.2(6) . . ?
N1 C8 H8 117.9 . . ?
C7 C8 H8 117.9 . . ?
C8 N1 C9 116.0(5) . . ?
N6 C10 C11 122.1(5) . . ?
N6 C10 H10 118.9 . . ?
C11 C10 H10 118.9 . . ?
C12 C11 C10 119.4(5) . . ?
C12 C11 H11 120.3 . . ?
C10 C11 H11 120.3 . . ?
C11 C12 C13 119.5(6) . . ?
C11 C12 H12 120.2 . . ?
C13 C12 H12 120.2 . . ?
C12 C13 C14 119.3(6) . . ?
C12 C13 H13 120.3 . . ?
C14 C13 H13 120.3 . . ?
N6 C14 C13 120.3(5) . . ?
N6 C14 C51 114.2(4) . . ?
C13 C14 C51 125.4(5) . . ?
C51 C15 C16 120.1(6) . . ?
C51 C15 H15 119.9 . . ?
C16 C15 H15 119.9 . . ?
N4 C16 C15 122.0(7) . . ?
N4 C16 H16 119.0 . . ?
C15 C16 H16 119.0 . . ?
C16 N4 C17 117.0(5) . . ?
N5 C51 C15 118.9(5) . . ?
N5 C51 C14 113.6(4) . . ?
C15 C51 C14 127.4(5) . . ?
O5 Cl2 O5 159.4(3) . 3 ?
O5 Cl2 O5 88.16(6) . 2 ?
O5 Cl2 O5 88.16(6) 3 2 ?
O5 Cl2 O5 88.16(6) . 4 ?
O5 Cl2 O5 88.16(6) 3 4 ?
O5 Cl2 O5 159.4(3) 2 4 ?
O5 Cl2 O4 100.32(16) . . ?
O5 Cl2 O4 100.32(16) 3 . ?
O5 Cl2 O4 100.32(16) 2 . ?
O5 Cl2 O4 100.32(16) 4 . ?
N2 C9 N1 124.1(5) . . ?
N2 C9 S4 118.5(4) . . ?
N1 C9 S4 117.3(4) . . ?
C9 N2 C6 118.3(4) . . ?
C9 N2 Co1 125.6(3) . . ?
C6 N2 Co1 116.1(3) . . ?
C1 N3 C5 118.8(4) . . ?
C1 N3 Co1 127.7(3) . . ?
C5 N3 Co1 113.5(3) . . ?
N5 C17 N4 123.8(5) . . ?
N5 C17 S2 120.0(4) . . ?
N4 C17 S2 116.2(4) . . ?
C17 N5 C51 118.1(4) . . ?
C17 N5 Co1 125.3(4) . . ?
C51 N5 Co1 116.5(3) . . ?
C14 N6 C10 119.1(4) . . ?
C14 N6 Co1 112.4(3) . . ?
C10 N6 Co1 128.4(4) . . ?
O1 Cl1 O1 119.2 11 . ?
O1 Cl1 O2 113.9 11 . ?
O1 Cl1 O2 113.9 . . ?
O1 Cl1 O3 102.3 11 . ?
O1 Cl1 O3 102.3 . . ?
O2 Cl1 O3 101.9 . . ?
Cl2 O5 O5 45.92(3) . 4 ?
Cl2 O5 O5 45.92(3) . 2 ?
O5 O5 O5 90.0 4 2 ?
S2 S1 Co1 101.44(10) . . ?
C17 S2 S1 102.4(2) . . ?
S4 S3 Co1 99.15(10) . . ?
C9 S4 S3 101.7(2) . . ?
O6 Cl3 O6 73.8 9_567 11_557 ?
O6 Cl3 O6 106.2 9_567 3_565 ?
O6 Cl3 O6 180.0 11_557 3_565 ?
O6 Cl3 O6 180.0 9_567 . ?
O6 Cl3 O6 106.2 11_557 . ?
O6 Cl3 O6 73.8 3_565 . ?
O6 Cl3 O7 143.1 9_567 9_567 ?
O6 Cl3 O7 143.1 11_557 9_567 ?
O6 Cl3 O7 36.9 3_565 9_567 ?
O6 Cl3 O7 36.9 . 9_567 ?
O6 Cl3 O7 36.9 9_567 . ?
O6 Cl3 O7 36.9 11_557 . ?
O6 Cl3 O7 143.1 3_565 . ?
O6 Cl3 O7 143.1 . . ?
O7 Cl3 O7 180.0 9_567 . ?
O6 Cl3 O8 76.1 9_567 . ?
O6 Cl3 O8 103.9 11_557 . ?
O6 Cl3 O8 76.1 3_565 . ?
O6 Cl3 O8 103.9 . . ?
O7 Cl3 O8 90.0 9_567 . ?
O7 Cl3 O8 90.0 . . ?
O6 Cl3 O8 103.9 9_567 9_567 ?
O6 Cl3 O8 76.1 11_557 9_567 ?
O6 Cl3 O8 103.9 3_565 9_567 ?
O6 Cl3 O8 76.1 . 9_567 ?
O7 Cl3 O8 90.0 9_567 9_567 ?
O7 Cl3 O8 90.0 . 9_567 ?
O8 Cl3 O8 180.0 . 9_567 ?
Cl3 O8 O6 51.7 . 9_567 ?
Cl3 O8 O6 51.7 . 3_565 ?
O6 O8 O6 80.5 9_567 3_565 ?
O7 O6 Cl3 71.8 9_567 . ?
O7 O6 O6 18.7 9_567 3_565 ?
Cl3 O6 O6 53.1 . 3_565 ?
O7 O6 O8 93.2 9_567 9_567 ?
Cl3 O6 O8 52.2 . 9_567 ?
O6 O6 O8 80.7 3_565 9_567 ?
O6 O7 O6 142.5 11_557 9_567 ?
O6 O7 Cl3 71.3 11_557 . ?
O6 O7 Cl3 71.3 9_567 . ?

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
N3 C1 C2 C3 1.4(9) . . . . ?
C1 C2 C3 C4 -0.6(9) . . . . ?
C2 C3 C4 C5 0.1(9) . . . . ?
C3 C4 C5 N3 -0.5(8) . . . . ?
C3 C4 C5 C6 -178.3(5) . . . . ?
N3 C5 C6 N2 -0.7(6) . . . . ?
C4 C5 C6 N2 177.2(5) . . . . ?
N3 C5 C6 C7 -176.9(5) . . . . ?
C4 C5 C6 C7 1.0(8) . . . . ?
N2 C6 C7 C8 0.4(8) . . . . ?
C5 C6 C7 C8 176.4(5) . . . . ?
C6 C7 C8 N1 -2.8(9) . . . . ?
C7 C8 N1 C9 3.4(9) . . . . ?
N6 C10 C11 C12 -2.5(9) . . . . ?
C10 C11 C12 C13 -0.1(9) . . . . ?
C11 C12 C13 C14 3.4(10) . . . . ?
C12 C13 C14 N6 -4.1(9) . . . . ?
C12 C13 C14 C51 178.9(6) . . . . ?
C51 C15 C16 N4 0.5(12) . . . . ?
C15 C16 N4 C17 -1.4(11) . . . . ?
C16 C15 C51 N5 0.5(10) . . . . ?
C16 C15 C51 C14 179.1(6) . . . . ?
N6 C14 C51 N5 2.9(7) . . . . ?
C13 C14 C51 N5 180.0(5) . . . . ?
N6 C14 C51 C15 -175.8(6) . . . . ?
C13 C14 C51 C15 1.3(10) . . . . ?
C8 N1 C9 N2 -1.8(8) . . . . ?
C8 N1 C9 S4 -176.5(4) . . . . ?
N1 C9 N2 C6 -0.3(7) . . . . ?
S4 C9 N2 C6 174.3(3) . . . . ?
N1 C9 N2 Co1 179.4(4) . . . . ?
S4 C9 N2 Co1 -6.0(6) . . . . ?
C7 C6 N2 C9 1.0(6) . . . . ?
C5 C6 N2 C9 -175.6(4) . . . . ?
C7 C6 N2 Co1 -178.7(4) . . . . ?
C5 C6 N2 Co1 4.7(5) . . . . ?
N5 Co1 N2 C9 167(100) . . . . ?
N3 Co1 N2 C9 175.2(4) . . . . ?
N6 Co1 N2 C9 -98.3(4) . . . . ?
S1 Co1 N2 C9 84.4(4) . . . . ?
S3 Co1 N2 C9 -8.5(4) . . . . ?
N5 Co1 N2 C6 -14(23) . . . . ?
N3 Co1 N2 C6 -5.1(3) . . . . ?
N6 Co1 N2 C6 81.4(3) . . . . ?
S1 Co1 N2 C6 -95.9(3) . . . . ?
S3 Co1 N2 C6 171.2(3) . . . . ?
C2 C1 N3 C5 -1.7(7) . . . . ?
C2 C1 N3 Co1 -178.7(4) . . . . ?
C4 C5 N3 C1 1.3(7) . . . . ?
C6 C5 N3 C1 179.3(4) . . . . ?
C4 C5 N3 Co1 178.7(4) . . . . ?
C6 C5 N3 Co1 -3.3(5) . . . . ?
N2 Co1 N3 C1 -178.3(4) . . . . ?
N5 Co1 N3 C1 1.6(4) . . . . ?
N6 Co1 N3 C1 84.4(4) . . . . ?
S1 Co1 N3 C1 -89.1(4) . . . . ?
S3 Co1 N3 C1 155.1(7) . . . . ?
N2 Co1 N3 C5 4.6(3) . . . . ?
N5 Co1 N3 C5 -175.5(3) . . . . ?
N6 Co1 N3 C5 -92.7(3) . . . . ?
S1 Co1 N3 C5 93.8(3) . . . . ?
S3 Co1 N3 C5 -22.0(10) . . . . ?
C16 N4 C17 N5 1.4(9) . . . . ?
C16 N4 C17 S2 -178.5(5) . . . . ?
N4 C17 N5 C51 -0.4(8) . . . . ?
S2 C17 N5 C51 179.5(4) . . . . ?
N4 C17 N5 Co1 -177.2(4) . . . . ?
S2 C17 N5 Co1 2.7(6) . . . . ?
C15 C51 N5 C17 -0.6(8) . . . . ?
C14 C51 N5 C17 -179.3(4) . . . . ?
C15 C51 N5 Co1 176.5(5) . . . . ?
C14 C51 N5 Co1 -2.3(6) . . . . ?
N2 Co1 N5 C17 -87(23) . . . . ?
N3 Co1 N5 C17 -95.7(4) . . . . ?
N6 Co1 N5 C17 177.7(4) . . . . ?
S1 Co1 N5 C17 -4.9(4) . . . . ?
S3 Co1 N5 C17 88.0(4) . . . . ?
N2 Co1 N5 C51 96(22) . . . . ?
N3 Co1 N5 C51 87.5(4) . . . . ?
N6 Co1 N5 C51 0.9(4) . . . . ?
S1 Co1 N5 C51 178.3(4) . . . . ?
S3 Co1 N5 C51 -88.8(4) . . . . ?
C13 C14 N6 C10 1.6(7) . . . . ?
C51 C14 N6 C10 178.8(4) . . . . ?
C13 C14 N6 Co1 -179.4(4) . . . . ?
C51 C14 N6 Co1 -2.1(5) . . . . ?
C11 C10 N6 C14 1.8(7) . . . . ?
C11 C10 N6 Co1 -177.1(4) . . . . ?
N2 Co1 N6 C14 -178.8(3) . . . . ?
N5 Co1 N6 C14 0.8(3) . . . . ?
N3 Co1 N6 C14 -97.3(3) . . . . ?
S1 Co1 N6 C14 -22.2(12) . . . . ?
S3 Co1 N6 C14 90.5(3) . . . . ?
N2 Co1 N6 C10 0.2(4) . . . . ?
N5 Co1 N6 C10 179.7(4) . . . . ?
N3 Co1 N6 C10 81.6(4) . . . . ?
S1 Co1 N6 C10 156.7(8) . . . . ?
S3 Co1 N6 C10 -90.6(4) . . . . ?
O5 Cl2 O5 O5 -79.84(15) 3 . . 4 ?
O5 Cl2 O5 O5 -159.7(3) 2 . . 4 ?
O4 Cl2 O5 O5 100.15(15) . . . 4 ?
O5 Cl2 O5 O5 79.85(15) 3 . . 2 ?
O5 Cl2 O5 O5 159.7(3) 4 . . 2 ?
O4 Cl2 O5 O5 -100.15(15) . . . 2 ?
N2 Co1 S1 S2 -175.93(13) . . . . ?
N5 Co1 S1 S2 4.55(14) . . . . ?
N3 Co1 S1 S2 102.24(15) . . . . ?
N6 Co1 S1 S2 27.4(10) . . . . ?
S3 Co1 S1 S2 -85.20(11) . . . . ?
N5 C17 S2 S1 1.6(5) . . . . ?
N4 C17 S2 S1 -178.5(4) . . . . ?
Co1 S1 S2 C17 -4.1(2) . . . . ?
N2 Co1 S3 S4 15.63(13) . . . . ?
N5 Co1 S3 S4 -164.33(14) . . . . ?
N3 Co1 S3 S4 41.9(9) . . . . ?
N6 Co1 S3 S4 112.53(15) . . . . ?
S1 Co1 S3 S4 -73.75(10) . . . . ?
N2 C9 S4 S3 18.1(4) . . . . ?
N1 C9 S4 S3 -166.9(4) . . . . ?
Co1 S3 S4 C9 -19.59(19) . . . . ?
O6 Cl3 O8 O6 -69.1 11_557 . . 9_567 ?
O6 Cl3 O8 O6 110.9 3_565 . . 9_567 ?
O6 Cl3 O8 O6 180.0 . . . 9_567 ?
O7 Cl3 O8 O6 145.4 9_567 . . 9_567 ?
O7 Cl3 O8 O6 -34.6 . . . 9_567 ?
O8 Cl3 O8 O6 -124.6 9_567 . . 9_567 ?
O6 Cl3 O8 O6 -110.9 9_567 . . 3_565 ?
O6 Cl3 O8 O6 180.0 11_557 . . 3_565 ?
O6 Cl3 O8 O6 69.1 . . . 3_565 ?
O7 Cl3 O8 O6 34.6 9_567 . . 3_565 ?
O7 Cl3 O8 O6 -145.4 . . . 3_565 ?
O8 Cl3 O8 O6 124.6 9_567 . . 3_565 ?
O6 Cl3 O6 O7 -139.8 9_567 . . 9_567 ?
O6 Cl3 O6 O7 180.0 11_557 . . 9_567 ?
O6 Cl3 O6 O7 0.0 3_565 . . 9_567 ?
O7 Cl3 O6 O7 180.0 . . . 9_567 ?
O8 Cl3 O6 O7 -70.8 . . . 9_567 ?
O8 Cl3 O6 O7 109.2 9_567 . . 9_567 ?
O6 Cl3 O6 O6 -139.7 9_567 . . 3_565 ?
O6 Cl3 O6 O6 180.0 11_557 . . 3_565 ?
O7 Cl3 O6 O6 0.0 9_567 . . 3_565 ?
O7 Cl3 O6 O6 180.0 . . . 3_565 ?
O8 Cl3 O6 O6 -70.8 . . . 3_565 ?
O8 Cl3 O6 O6 109.2 9_567 . . 3_565 ?
O6 Cl3 O6 O8 111.1 9_567 . . 9_567 ?
O6 Cl3 O6 O8 70.8 11_557 . . 9_567 ?
O6 Cl3 O6 O8 -109.2 3_565 . . 9_567 ?
O7 Cl3 O6 O8 -109.2 9_567 . . 9_567 ?
O7 Cl3 O6 O8 70.8 . . . 9_567 ?
O8 Cl3 O6 O8 180.0 . . . 9_567 ?
O6 Cl3 O7 O6 180.0 9_567 . . 11_557 ?
O6 Cl3 O7 O6 180.0 3_565 . . 11_557 ?
O6 Cl3 O7 O6 0.0 . . . 11_557 ?
O7 Cl3 O7 O6 -33.5 9_567 . . 11_557 ?
O8 Cl3 O7 O6 -113.5 . . . 11_557 ?
O8 Cl3 O7 O6 66.5 9_567 . . 11_557 ?
O6 Cl3 O7 O6 180.0 11_557 . . 9_567 ?
O6 Cl3 O7 O6 0.0 3_565 . . 9_567 ?
O6 Cl3 O7 O6 180.0 . . . 9_567 ?
O7 Cl3 O7 O6 146.5 9_567 . . 9_567 ?
O8 Cl3 O7 O6 66.5 . . . 9_567 ?
O8 Cl3 O7 O6 -113.5 9_567 . . 9_567 ?

_diffrn_measured_fraction_theta_max 1.000
_diffrn_reflns_theta_full        25.01
_diffrn_measured_fraction_theta_full 1.000
_refine_diff_density_max         2.016
_refine_diff_density_min         -4.178
_refine_diff_density_rms         0.204

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 0.000 760 228 ' '
2 0.000 0.000 0.500 379 129 ' '
3 0.500 0.500 0.000 379 129 ' '
4 0.500 0.500 0.500 760 228 ' '
_platon_squeeze_details          
;
In order to subtract the contribution from the disordered solvent molecules,
the SQUEEZE command was applied.
SQUEEZE removed eleven disordered H2O per formula unit. This valueis calculated
See ref. Bi, Y. F.; Wang, X. T.; Liao, W. P.; Wang, X. F.; Wang, X. W.;
Zhang, H. J.; Gao, S. J. Am. Chem. Soc. 2009, 131, 11650.
;

_database_code_depnum_ccdc_archive 'CCDC 1015425'
#######################################################################
#
#                 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_x

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C36 H24 Cu4 I2 N12 S4'
_chemical_formula_sum            'C36 H24 Cu4 I2 N12 S4'
_chemical_formula_weight         1260.87

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'
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.4742 1.8119 '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'
_symmetry_space_group_name_Hall  '-P 1'

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

_cell_length_a                   7.360(4)
_cell_length_b                   17.468(9)
_cell_length_c                   17.955(9)
_cell_angle_alpha                63.248(5)
_cell_angle_beta                 82.315(6)
_cell_angle_gamma                86.261(6)
_cell_volume                     2043.0(19)
_cell_formula_units_Z            2
_cell_measurement_temperature    298(2)
_cell_measurement_reflns_used    7045
_cell_measurement_theta_min      2.5
_cell_measurement_theta_max      25.0

_exptl_crystal_description       block
_exptl_crystal_colour            black
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.22
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.050
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1220
_exptl_absorpt_coefficient_mu    3.815
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.302
_exptl_absorpt_correction_T_max  0.432
_exptl_absorpt_process_details   '(SADABS; Bruker, 2001)'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      298(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  'Bruker APEXII CCD area-detector'
_diffrn_measurement_method       'φ and ω'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            14115
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0379
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         2.20
_diffrn_reflns_theta_max         25.02
_reflns_number_total             7046
_reflns_number_gt                5945
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'APEX2 (Bruker, 2007)'
_computing_cell_refinement       'SAINT-Plus (Bruker, 2007)'
_computing_data_reduction        'SAINT-Plus (Bruker, 2007)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'

_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)+(0.0797P)²+2.8090P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         7046
_refine_ls_number_parameters     524
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0469
_refine_ls_R_factor_gt           0.0381
_refine_ls_wR_factor_ref         0.1244
_refine_ls_wR_factor_gt          0.1160
_refine_ls_goodness_of_fit_ref   0.998
_refine_ls_restrained_S_all      0.998
_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
Cu1 Cu 0.49350(11) 0.73750(5) -0.06586(4) 0.03958(19) Uani 1 1 d . . .
Cu2 Cu 0.38091(11) 0.82880(4) 0.00215(4) 0.03881(19) Uani 1 1 d . . .
Cu3 Cu 0.16367(11) 0.35837(5) 0.45013(4) 0.03975(19) Uani 1 1 d . . .
Cu4 Cu 0.14306(11) 0.20792(5) 0.48621(5) 0.04050(19) Uani 1 1 d . . .
I1 I 0.11591(6) 0.72727(3) -0.00387(3) 0.04766(14) Uani 1 1 d . . .
I2 I 0.48904(6) 0.27818(3) 0.43728(3) 0.04786(14) Uani 1 1 d . . .
S1 S 0.5207(2) 0.74505(10) 0.11517(10) 0.0453(4) Uani 1 1 d . . .
S2 S 0.5314(3) 0.85050(11) -0.19096(11) 0.0600(5) Uani 1 1 d . . .
S3 S 0.0281(3) 0.17916(11) 0.61755(10) 0.0539(4) Uani 1 1 d . . .
S4 S -0.0039(2) 0.39259(10) 0.34556(10) 0.0410(4) Uani 1 1 d . . .
N1 N 0.6830(9) 0.5936(3) 0.1721(4) 0.0538(15) Uani 1 1 d . . .
N2 N 0.6059(6) 0.6510(3) 0.0326(3) 0.0329(10) Uani 1 1 d . . .
N3 N 0.5726(7) 0.6483(3) -0.1105(3) 0.0400(12) Uani 1 1 d . . .
N4 N 0.2665(7) 0.9128(3) 0.0471(3) 0.0387(11) Uani 1 1 d . . .
N5 N 0.3911(7) 0.9353(3) -0.1050(3) 0.0369(11) Uani 1 1 d . . .
N6 N 0.4534(9) 1.0151(4) -0.2542(3) 0.0576(16) Uani 1 1 d . . .
N7 N 0.2384(7) 0.4767(3) 0.4320(3) 0.0402(12) Uani 1 1 d . . .
N8 N 0.1369(7) 0.3392(3) 0.5689(3) 0.0365(11) Uani 1 1 d . . .
N9 N 0.0667(8) 0.2529(4) 0.7155(3) 0.0491(14) Uani 1 1 d . . .
N10 N 0.1930(7) 0.0894(3) 0.4908(3) 0.0415(12) Uani 1 1 d . . .
N11 N 0.0703(6) 0.2311(3) 0.3755(3) 0.0343(11) Uani 1 1 d . . .
N12 N -0.0536(8) 0.3199(4) 0.2484(3) 0.0488(14) Uani 1 1 d . . .
C1 C 0.5475(10) 0.6513(4) -0.1843(4) 0.0498(16) Uani 1 1 d . . .
H1B H 0.4834 0.6974 -0.2214 0.060 Uiso 1 1 calc R . .
C2 C 0.6143(10) 0.5876(4) -0.2074(4) 0.0518(17) Uani 1 1 d . . .
H2A H 0.5958 0.5910 -0.2590 0.062 Uiso 1 1 calc R . .
C3 C 0.7088(10) 0.5191(4) -0.1516(5) 0.0540(17) Uani 1 1 d . . .
H3A H 0.7530 0.4752 -0.1651 0.065 Uiso 1 1 calc R . .
C4 C 0.7370(9) 0.5162(4) -0.0764(4) 0.0460(15) Uani 1 1 d . . .
H4A H 0.8036 0.4713 -0.0393 0.055 Uiso 1 1 calc R . .
C5 C 0.6646(8) 0.5811(4) -0.0560(4) 0.0355(13) Uani 1 1 d . . .
C6 C 0.6835(8) 0.5824(4) 0.0239(4) 0.0375(13) Uani 1 1 d . . .
C7 C 0.7672(9) 0.5187(4) 0.0892(4) 0.0484(16) Uani 1 1 d . . .
H7A H 0.8242 0.4717 0.0845 0.058 Uiso 1 1 calc R . .
C8 C 0.7621(11) 0.5282(4) 0.1612(5) 0.060(2) Uani 1 1 d . . .
H8A H 0.8179 0.4860 0.2054 0.072 Uiso 1 1 calc R . .
C9 C 0.6105(8) 0.6559(4) 0.1053(4) 0.0400(14) Uani 1 1 d . . .
C10 C 0.2052(9) 0.8955(4) 0.1262(4) 0.0495(16) Uani 1 1 d . . .
H10A H 0.2068 0.8389 0.1671 0.059 Uiso 1 1 calc R . .
C11 C 0.1392(10) 0.9577(5) 0.1503(5) 0.0538(17) Uani 1 1 d . . .
H11A H 0.0965 0.9432 0.2061 0.065 Uiso 1 1 calc R . .
C12 C 0.1380(9) 1.0423(4) 0.0898(4) 0.0506(16) Uani 1 1 d . . .
H12B H 0.0963 1.0857 0.1044 0.061 Uiso 1 1 calc R . .
C13 C 0.1998(9) 1.0611(4) 0.0074(4) 0.0455(15) Uani 1 1 d . . .
H13A H 0.1995 1.1174 -0.0343 0.055 Uiso 1 1 calc R . .
C14 C 0.2621(8) 0.9956(4) -0.0127(4) 0.0375(13) Uani 1 1 d . . .
C15 C 0.3319(8) 1.0079(4) -0.0993(4) 0.0363(13) Uani 1 1 d . . .
C16 C 0.3356(10) 1.0856(4) -0.1703(4) 0.0488(16) Uani 1 1 d . . .
H16A H 0.2979 1.1360 -0.1670 0.059 Uiso 1 1 calc R . .
C17 C 0.3973(11) 1.0857(4) -0.2461(4) 0.060(2) Uani 1 1 d . . .
H17A H 0.4000 1.1376 -0.2944 0.072 Uiso 1 1 calc R . .
C18 C 0.4512(9) 0.9410(4) -0.1822(4) 0.0459(15) Uani 1 1 d . . .
C19 C 0.2906(10) 0.5441(4) 0.3577(4) 0.0489(16) Uani 1 1 d . . .
H19A H 0.2916 0.5386 0.3085 0.059 Uiso 1 1 calc R . .
C20 C 0.3425(10) 0.6212(4) 0.3525(4) 0.0504(16) Uani 1 1 d . . .
H20A H 0.3787 0.6667 0.3006 0.060 Uiso 1 1 calc R . .
C21 C 0.3399(9) 0.6295(4) 0.4251(4) 0.0476(16) Uani 1 1 d . . .
H21A H 0.3722 0.6811 0.4230 0.057 Uiso 1 1 calc R . .
C22 C 0.2888(8) 0.5605(4) 0.5009(4) 0.0430(14) Uani 1 1 d . . .
H22A H 0.2886 0.5649 0.5507 0.052 Uiso 1 1 calc R . .
C23 C 0.2377(7) 0.4847(4) 0.5032(4) 0.0338(12) Uani 1 1 d . . .
C24 C 0.1806(8) 0.4060(4) 0.5817(4) 0.0364(13) Uani 1 1 d . . .
C25 C 0.1702(9) 0.3976(4) 0.6621(4) 0.0453(15) Uani 1 1 d . . .
H25A H 0.2011 0.4424 0.6725 0.054 Uiso 1 1 calc R . .
C26 C 0.1116(11) 0.3194(5) 0.7268(4) 0.0539(18) Uani 1 1 d . . .
H26A H 0.1029 0.3128 0.7815 0.065 Uiso 1 1 calc R . .
C27 C 0.0828(8) 0.2639(4) 0.6358(4) 0.0408(14) Uani 1 1 d . . .
C28 C 0.2610(9) 0.0199(4) 0.5529(4) 0.0482(16) Uani 1 1 d . . .
H28A H 0.2791 0.0222 0.6021 0.058 Uiso 1 1 calc R . .
C29 C 0.3048(9) -0.0548(4) 0.5453(5) 0.0547(19) Uani 1 1 d . . .
H29A H 0.3503 -0.1024 0.5890 0.066 Uiso 1 1 calc R . .
C30 C 0.2796(9) -0.0575(4) 0.4723(5) 0.0570(19) Uani 1 1 d . . .
H30A H 0.3086 -0.1072 0.4663 0.068 Uiso 1 1 calc R . .
C31 C 0.2114(9) 0.0133(4) 0.4071(5) 0.0516(17) Uani 1 1 d . . .
H31A H 0.1966 0.0125 0.3568 0.062 Uiso 1 1 calc R . .
C32 C 0.1659(8) 0.0856(4) 0.4198(4) 0.0380(13) Uani 1 1 d . . .
C33 C 0.0876(8) 0.1648(4) 0.3558(4) 0.0383(13) Uani 1 1 d . . .
C34 C 0.0295(10) 0.1743(4) 0.2824(4) 0.0494(16) Uani 1 1 d . . .
H34A H 0.0373 0.1292 0.2680 0.059 Uiso 1 1 calc R . .
C35 C -0.0409(10) 0.2531(5) 0.2309(4) 0.0534(18) Uani 1 1 d . . .
H35A H -0.0815 0.2599 0.1814 0.064 Uiso 1 1 calc R . .
C36 C 0.0032(8) 0.3075(4) 0.3209(4) 0.0378(13) Uani 1 1 d . . .


_geom_special_details            
; 
 All esds (except the esd in the dihedral angle between two l.s. planes) 
 are estimated using the full covariance matrix.  The cell esds are taken 
 into account individually in the estimation of esds in distances, angles 
 and torsion angles; correlations between esds in cell parameters are only 
 used when they are defined by crystal symmetry.  An approximate (isotropic) 
 treatment of cell esds is used for estimating esds involving l.s. planes. 
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cu1 N2 1.979(4) . ?
Cu1 N3 2.072(5) . ?
Cu1 S2 2.221(2) . ?
Cu1 Cu2 2.4562(13) . ?
Cu1 I1 2.8379(16) . ?
Cu2 N5 1.981(5) . ?
Cu2 N4 2.059(5) . ?
Cu2 S1 2.2377(18) . ?
Cu2 I1 2.7645(13) . ?
Cu3 N8 1.988(5) . ?
Cu3 N7 2.044(5) . ?
Cu3 S4 2.2172(18) . ?
Cu3 Cu4 2.4172(17) . ?
Cu3 I2 2.7307(14) . ?
Cu4 N11 1.984(5) . ?
Cu4 N10 2.046(5) . ?
Cu4 S3 2.233(2) . ?
Cu4 I2 2.7571(15) . ?
S1 C9 1.726(6) . ?
S2 C18 1.718(7) . ?
S3 C27 1.736(7) . ?
S4 C36 1.727(6) . ?
N1 C8 1.330(9) . ?
N1 C9 1.351(7) . ?
N2 C9 1.351(8) . ?
N2 C6 1.357(7) . ?
N3 C1 1.340(8) . ?
N3 C5 1.354(8) . ?
N4 C10 1.331(8) . ?
N4 C14 1.360(8) . ?
N5 C18 1.358(8) . ?
N5 C15 1.358(8) . ?
N6 C17 1.339(9) . ?
N6 C18 1.355(8) . ?
N7 C23 1.347(7) . ?
N7 C19 1.349(8) . ?
N8 C24 1.353(8) . ?
N8 C27 1.359(8) . ?
N9 C26 1.334(9) . ?
N9 C27 1.344(8) . ?
N10 C32 1.347(8) . ?
N10 C28 1.349(8) . ?
N11 C33 1.350(8) . ?
N11 C36 1.361(7) . ?
N12 C35 1.333(9) . ?
N12 C36 1.340(7) . ?
C1 C2 1.392(10) . ?
C1 H1B 0.9300 . ?
C2 C3 1.385(10) . ?
C2 H2A 0.9300 . ?
C3 C4 1.371(10) . ?
C3 H3A 0.9300 . ?
C4 C5 1.396(8) . ?
C4 H4A 0.9300 . ?
C5 C6 1.470(8) . ?
C6 C7 1.387(8) . ?
C7 C8 1.370(10) . ?
C7 H7A 0.9300 . ?
C8 H8A 0.9300 . ?
C10 C11 1.380(10) . ?
C10 H10A 0.9300 . ?
C11 C12 1.385(10) . ?
C11 H11A 0.9300 . ?
C12 C13 1.381(9) . ?
C12 H12B 0.9300 . ?
C13 C14 1.382(9) . ?
C13 H13A 0.9300 . ?
C14 C15 1.491(9) . ?
C15 C16 1.381(8) . ?
C16 C17 1.375(10) . ?
C16 H16A 0.9300 . ?
C17 H17A 0.9300 . ?
C19 C20 1.382(9) . ?
C19 H19A 0.9300 . ?
C20 C21 1.372(9) . ?
C20 H20A 0.9300 . ?
C21 C22 1.376(9) . ?
C21 H21A 0.9300 . ?
C22 C23 1.382(9) . ?
C22 H22A 0.9300 . ?
C23 C24 1.491(9) . ?
C24 C25 1.376(8) . ?
C25 C26 1.384(10) . ?
C25 H25A 0.9300 . ?
C26 H26A 0.9300 . ?
C28 C29 1.386(10) . ?
C28 H28A 0.9300 . ?
C29 C30 1.370(11) . ?
C29 H29A 0.9300 . ?
C30 C31 1.387(10) . ?
C30 H30A 0.9300 . ?
C31 C32 1.395(9) . ?
C31 H31A 0.9300 . ?
C32 C33 1.486(8) . ?
C33 C34 1.374(9) . ?
C34 C35 1.381(10) . ?
C34 H34A 0.9300 . ?
C35 H35A 0.9300 . ?

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
N2 Cu1 N3 81.1(2) . . ?
N2 Cu1 S2 148.01(15) . . ?
N3 Cu1 S2 95.07(15) . . ?
N2 Cu1 Cu2 94.62(15) . . ?
N3 Cu1 Cu2 173.04(14) . . ?
S2 Cu1 Cu2 91.44(7) . . ?
N2 Cu1 I1 102.65(14) . . ?
N3 Cu1 I1 112.91(15) . . ?
S2 Cu1 I1 107.97(6) . . ?
Cu2 Cu1 I1 62.47(3) . . ?
N5 Cu2 N4 80.8(2) . . ?
N5 Cu2 S1 146.79(15) . . ?
N4 Cu2 S1 96.30(15) . . ?
N5 Cu2 Cu1 93.88(16) . . ?
N4 Cu2 Cu1 172.83(14) . . ?
S1 Cu2 Cu1 90.77(6) . . ?
N5 Cu2 I1 106.30(14) . . ?
N4 Cu2 I1 111.13(15) . . ?
S1 Cu2 I1 105.55(6) . . ?
Cu1 Cu2 I1 65.55(4) . . ?
N8 Cu3 N7 80.6(2) . . ?
N8 Cu3 S4 140.21(15) . . ?
N7 Cu3 S4 101.38(14) . . ?
N8 Cu3 Cu4 94.18(14) . . ?
N7 Cu3 Cu4 166.34(15) . . ?
S4 Cu3 Cu4 90.73(5) . . ?
N8 Cu3 I2 102.23(14) . . ?
N7 Cu3 I2 104.12(15) . . ?
S4 Cu3 I2 115.36(6) . . ?
Cu4 Cu3 I2 64.43(4) . . ?
N11 Cu4 N10 80.8(2) . . ?
N11 Cu4 S3 142.38(15) . . ?
N10 Cu4 S3 103.75(16) . . ?
N11 Cu4 Cu3 93.36(14) . . ?
N10 Cu4 Cu3 162.88(15) . . ?
S3 Cu4 Cu3 90.73(6) . . ?
N11 Cu4 I2 100.20(14) . . ?
N10 Cu4 I2 101.68(15) . . ?
S3 Cu4 I2 114.89(6) . . ?
Cu3 Cu4 I2 63.31(3) . . ?
Cu2 I1 Cu1 51.99(3) . . ?
Cu3 I2 Cu4 52.27(4) . . ?
C9 S1 Cu2 109.4(2) . . ?
C18 S2 Cu1 109.6(2) . . ?
C27 S3 Cu4 107.7(2) . . ?
C36 S4 Cu3 108.2(2) . . ?
C8 N1 C9 116.2(6) . . ?
C9 N2 C6 119.3(5) . . ?
C9 N2 Cu1 125.2(4) . . ?
C6 N2 Cu1 115.5(4) . . ?
C1 N3 C5 119.3(5) . . ?
C1 N3 Cu1 128.4(4) . . ?
C5 N3 Cu1 112.3(4) . . ?
C10 N4 C14 118.4(5) . . ?
C10 N4 Cu2 127.7(4) . . ?
C14 N4 Cu2 113.9(4) . . ?
C18 N5 C15 118.3(5) . . ?
C18 N5 Cu2 125.6(4) . . ?
C15 N5 Cu2 116.1(4) . . ?
C17 N6 C18 116.4(6) . . ?
C23 N7 C19 118.9(5) . . ?
C23 N7 Cu3 114.4(4) . . ?
C19 N7 Cu3 126.7(4) . . ?
C24 N8 C27 119.6(5) . . ?
C24 N8 Cu3 116.1(4) . . ?
C27 N8 Cu3 124.2(4) . . ?
C26 N9 C27 116.6(6) . . ?
C32 N10 C28 119.0(6) . . ?
C32 N10 Cu4 113.6(4) . . ?
C28 N10 Cu4 127.2(5) . . ?
C33 N11 C36 119.7(5) . . ?
C33 N11 Cu4 116.0(4) . . ?
C36 N11 Cu4 124.3(4) . . ?
C35 N12 C36 116.8(6) . . ?
N3 C1 C2 122.1(6) . . ?
N3 C1 H1B 118.9 . . ?
C2 C1 H1B 118.9 . . ?
C3 C2 C1 118.5(6) . . ?
C3 C2 H2A 120.8 . . ?
C1 C2 H2A 120.8 . . ?
C4 C3 C2 119.7(6) . . ?
C4 C3 H3A 120.1 . . ?
C2 C3 H3A 120.1 . . ?
C3 C4 C5 119.4(6) . . ?
C3 C4 H4A 120.3 . . ?
C5 C4 H4A 120.3 . . ?
N3 C5 C4 121.0(6) . . ?
N3 C5 C6 115.7(5) . . ?
C4 C5 C6 123.3(5) . . ?
N2 C6 C7 119.8(6) . . ?
N2 C6 C5 115.2(5) . . ?
C7 C6 C5 125.0(6) . . ?
C8 C7 C6 116.8(6) . . ?
C8 C7 H7A 121.6 . . ?
C6 C7 H7A 121.6 . . ?
N1 C8 C7 124.6(6) . . ?
N1 C8 H8A 117.7 . . ?
C7 C8 H8A 117.7 . . ?
N2 C9 N1 123.1(6) . . ?
N2 C9 S1 119.5(4) . . ?
N1 C9 S1 117.4(5) . . ?
N4 C10 C11 123.0(6) . . ?
N4 C10 H10A 118.5 . . ?
C11 C10 H10A 118.5 . . ?
C10 C11 C12 118.7(7) . . ?
C10 C11 H11A 120.6 . . ?
C12 C11 H11A 120.6 . . ?
C13 C12 C11 118.9(6) . . ?
C13 C12 H12B 120.6 . . ?
C11 C12 H12B 120.6 . . ?
C12 C13 C14 119.5(6) . . ?
C12 C13 H13A 120.3 . . ?
C14 C13 H13A 120.3 . . ?
N4 C14 C13 121.5(6) . . ?
N4 C14 C15 114.2(5) . . ?
C13 C14 C15 124.4(6) . . ?
N5 C15 C16 120.5(6) . . ?
N5 C15 C14 114.9(5) . . ?
C16 C15 C14 124.6(6) . . ?
C17 C16 C15 117.4(6) . . ?
C17 C16 H16A 121.3 . . ?
C15 C16 H16A 121.3 . . ?
N6 C17 C16 123.6(6) . . ?
N6 C17 H17A 118.2 . . ?
C16 C17 H17A 118.2 . . ?
N6 C18 N5 123.7(6) . . ?
N6 C18 S2 117.0(5) . . ?
N5 C18 S2 119.2(4) . . ?
N7 C19 C20 122.0(6) . . ?
N7 C19 H19A 119.0 . . ?
C20 C19 H19A 119.0 . . ?
C21 C20 C19 119.0(6) . . ?
C21 C20 H20A 120.5 . . ?
C19 C20 H20A 120.5 . . ?
C20 C21 C22 119.1(6) . . ?
C20 C21 H21A 120.5 . . ?
C22 C21 H21A 120.5 . . ?
C21 C22 C23 120.0(6) . . ?
C21 C22 H22A 120.0 . . ?
C23 C22 H22A 120.0 . . ?
N7 C23 C22 121.0(6) . . ?
N7 C23 C24 114.5(5) . . ?
C22 C23 C24 124.5(5) . . ?
N8 C24 C25 119.9(6) . . ?
N8 C24 C23 114.4(5) . . ?
C25 C24 C23 125.7(6) . . ?
C24 C25 C26 116.9(6) . . ?
C24 C25 H25A 121.5 . . ?
C26 C25 H25A 121.5 . . ?
N9 C26 C25 124.1(6) . . ?
N9 C26 H26A 118.0 . . ?
C25 C26 H26A 118.0 . . ?
N9 C27 N8 122.8(6) . . ?
N9 C27 S3 118.5(5) . . ?
N8 C27 S3 118.6(4) . . ?
N10 C28 C29 121.7(7) . . ?
N10 C28 H28A 119.1 . . ?
C29 C28 H28A 119.1 . . ?
C30 C29 C28 118.8(6) . . ?
C30 C29 H29A 120.6 . . ?
C28 C29 H29A 120.6 . . ?
C29 C30 C31 120.7(7) . . ?
C29 C30 H30A 119.7 . . ?
C31 C30 H30A 119.7 . . ?
C30 C31 C32 117.5(7) . . ?
C30 C31 H31A 121.3 . . ?
C32 C31 H31A 121.3 . . ?
N10 C32 C31 122.3(6) . . ?
N10 C32 C33 114.9(5) . . ?
C31 C32 C33 122.8(6) . . ?
N11 C33 C34 119.4(6) . . ?
N11 C33 C32 114.3(5) . . ?
C34 C33 C32 126.2(6) . . ?
C33 C34 C35 117.7(6) . . ?
C33 C34 H34A 121.1 . . ?
C35 C34 H34A 121.1 . . ?
N12 C35 C34 123.5(6) . . ?
N12 C35 H35A 118.3 . . ?
C34 C35 H35A 118.3 . . ?
N12 C36 N11 122.9(6) . . ?
N12 C36 S4 118.9(5) . . ?
N11 C36 S4 118.3(4) . . ?

_diffrn_measured_fraction_theta_max 0.977
_diffrn_reflns_theta_full        25.02
_diffrn_measured_fraction_theta_full 0.977
_refine_diff_density_max         0.576
_refine_diff_density_min         -1.203
_refine_diff_density_rms         0.118
_database_code_depnum_ccdc_archive 'CCDC 881171'
