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


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#                                CCDC 
# 
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# 
#  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. 
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#  fide research purposes only. It may contain copyright material 
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data_9
_database_code_depnum_ccdc_archive 'CCDC 638086'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C43 H54 Cl3 Cu4 N10 O3 S4'
_chemical_formula_weight         1247.71

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'
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           hexagonal
_symmetry_space_group_name_H-M   R3c

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'-y, -x, z+1/2'
'-x+y, y, z+1/2'
'x, x-y, z+1/2'
'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'
'-y+2/3, -x+1/3, z+5/6'
'-x+y+2/3, y+1/3, z+5/6'
'x+2/3, x-y+1/3, z+5/6'
'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'
'-y+1/3, -x+2/3, z+7/6'
'-x+y+1/3, y+2/3, z+7/6'
'x+1/3, x-y+2/3, z+7/6'

_cell_length_a                   20.925(2)
_cell_length_b                   20.925(2)
_cell_length_c                   20.610(2)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_volume                     7815.2(13)
_cell_formula_units_Z            6
_cell_measurement_temperature    298(2)
_cell_measurement_reflns_used    3851
_cell_measurement_theta_min      2.3
_cell_measurement_theta_max      24.6

_exptl_crystal_description       block
_exptl_crystal_colour            blue
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.10
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.591
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             3822
_exptl_absorpt_coefficient_mu    1.973
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.5890
_exptl_absorpt_correction_T_max  0.8271
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1996)'

_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 SMART 1000 CCD area-detector'
_diffrn_measurement_method       '\w scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         0
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            19655
_diffrn_reflns_av_R_equivalents  0.0489
_diffrn_reflns_av_sigmaI/netI    0.0524
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_theta_min         1.95
_diffrn_reflns_theta_max         27.50
_reflns_number_total             3944
_reflns_number_gt                3180
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'SMART (Bruker, 1998)'
_computing_cell_refinement       SMART
_computing_data_reduction        'SAINT (Bruker, 1998)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 1997)'
_computing_publication_material  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.
;

_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^)+(0.0323P)^2^+1.3632P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.021(15)
_refine_ls_number_reflns         3944
_refine_ls_number_parameters     204
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0519
_refine_ls_R_factor_gt           0.0373
_refine_ls_wR_factor_ref         0.0858
_refine_ls_wR_factor_gt          0.0799
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_restrained_S_all      1.033
_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 0.75954(2) 0.25247(2) 0.78802(2) 0.04381(12) Uani 1 1 d . . .
Cu2 Cu 0.6667 0.3333 0.54480(4) 0.0612(3) Uani 1 3 d S . .
Cl1 Cl 0.61011(7) 0.00344(7) 1.06109(6) 0.0764(4) Uani 1 1 d . . .
S1 S 0.65808(7) 0.22023(6) 0.57806(5) 0.0606(3) Uani 1 1 d . . .
S2 S 0.6667 0.3333 0.31379(8) 0.0496(4) Uani 1 3 d S . .
O1 O 0.68388(15) 0.15513(14) 0.81169(12) 0.0495(6) Uani 1 1 d . . .
N1 N 0.79102(17) 0.27701(17) 0.87645(15) 0.0441(7) Uani 1 1 d . . .
N2 N 0.86319(16) 0.33977(17) 0.76516(16) 0.0445(7) Uani 1 1 d . . .
N3 N 0.7248(2) 0.24004(19) 0.69897(18) 0.0529(8) Uani 1 1 d . . .
N4 N 0.6667 0.3333 0.4487(3) 0.0542(15) Uani 1 3 d S . .
C1 C 0.7032(2) 0.1626(2) 0.92664(18) 0.0436(9) Uani 1 1 d . . .
C2 C 0.6682(2) 0.1254(2) 0.86837(17) 0.0425(8) Uani 1 1 d . . .
C3 C 0.6132(2) 0.0514(2) 0.8745(2) 0.0495(9) Uani 1 1 d . . .
H3 H 0.5885 0.0255 0.8374 0.059 Uiso 1 1 calc R . .
C4 C 0.5943(2) 0.0153(2) 0.9333(2) 0.0567(11) Uani 1 1 d . . .
H4 H 0.5573 -0.0340 0.9355 0.068 Uiso 1 1 calc R . .
C5 C 0.6302(2) 0.0524(2) 0.9887(2) 0.0535(10) Uani 1 1 d . . .
C6 C 0.6828(2) 0.1247(2) 0.9856(2) 0.0514(10) Uani 1 1 d . . .
H6 H 0.7058 0.1495 1.0236 0.062 Uiso 1 1 calc R . .
C7 C 0.7631(2) 0.2373(2) 0.9268(2) 0.0475(9) Uani 1 1 d . . .
H7 H 0.7831 0.2584 0.9668 0.057 Uiso 1 1 calc R . .
C8 C 0.8536(2) 0.3525(2) 0.8815(2) 0.0637(12) Uani 1 1 d . . .
H8A H 0.8788 0.3593 0.9226 0.076 Uiso 1 1 calc R . .
H8B H 0.8367 0.3879 0.8786 0.076 Uiso 1 1 calc R . .
C9 C 0.9043(3) 0.3627(3) 0.8264(2) 0.0763(15) Uani 1 1 d . . .
H9A H 0.9424 0.4142 0.8236 0.092 Uiso 1 1 calc R . .
H9B H 0.9280 0.3337 0.8341 0.092 Uiso 1 1 calc R . .
C10 C 0.8559(2) 0.4003(2) 0.7355(2) 0.0595(11) Uani 1 1 d . . .
H10A H 0.8355 0.4189 0.7678 0.071 Uiso 1 1 calc R . .
H10B H 0.8205 0.3798 0.7003 0.071 Uiso 1 1 calc R . .
C11 C 0.9266(3) 0.4652(2) 0.7091(3) 0.0675(13) Uani 1 1 d . . .
H11A H 0.9639 0.4833 0.7422 0.101 Uiso 1 1 calc R . .
H11B H 0.9172 0.5038 0.6961 0.101 Uiso 1 1 calc R . .
H11C H 0.9433 0.4494 0.6723 0.101 Uiso 1 1 calc R . .
C12 C 0.9009(3) 0.3158(3) 0.7173(3) 0.0746(14) Uani 1 1 d . . .
H12A H 0.8818 0.3159 0.6744 0.089 Uiso 1 1 calc R . .
H12B H 0.9531 0.3522 0.7172 0.089 Uiso 1 1 calc R . .
C13 C 0.8930(3) 0.2439(3) 0.7284(3) 0.096(2) Uani 1 1 d . . .
H13A H 0.9124 0.2430 0.7704 0.144 Uiso 1 1 calc R . .
H13B H 0.9197 0.2342 0.6957 0.144 Uiso 1 1 calc R . .
H13C H 0.8418 0.2069 0.7265 0.144 Uiso 1 1 calc R . .
C14 C 0.6977(2) 0.2332(2) 0.64862(19) 0.0455(9) Uani 1 1 d . . .
C15 C 0.6667 0.3333 0.3934(3) 0.0404(14) 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
Cu1 0.0431(3) 0.0464(3) 0.0381(2) 0.0070(2) -0.0009(2) 0.0196(2)
Cu2 0.0761(4) 0.0761(4) 0.0313(5) 0.000 0.000 0.0380(2)
Cl1 0.0846(8) 0.0885(9) 0.0606(7) 0.0355(6) 0.0285(6) 0.0465(7)
S1 0.0842(8) 0.0642(7) 0.0366(5) -0.0041(5) -0.0074(5) 0.0395(6)
S2 0.0602(7) 0.0602(7) 0.0284(8) 0.000 0.000 0.0301(3)
O1 0.0583(16) 0.0459(14) 0.0366(14) 0.0039(12) 0.0017(12) 0.0203(12)
N1 0.0454(18) 0.0435(17) 0.0414(19) 0.0028(14) 0.0010(15) 0.0208(16)
N2 0.0396(16) 0.0441(17) 0.0512(19) 0.0113(14) 0.0012(14) 0.0220(14)
N3 0.055(2) 0.065(2) 0.0346(19) 0.0081(16) -0.0039(16) 0.0267(17)
N4 0.064(2) 0.064(2) 0.034(3) 0.000 0.000 0.0322(12)
C1 0.049(2) 0.048(2) 0.042(2) 0.0041(17) 0.0068(17) 0.0298(18)
C2 0.046(2) 0.048(2) 0.043(2) 0.0035(17) 0.0031(17) 0.0312(19)
C3 0.048(2) 0.044(2) 0.056(3) 0.0056(18) 0.0009(18) 0.0224(19)
C4 0.050(2) 0.047(2) 0.070(3) 0.014(2) 0.013(2) 0.023(2)
C5 0.055(2) 0.064(3) 0.049(3) 0.019(2) 0.019(2) 0.035(2)
C6 0.057(2) 0.063(3) 0.040(2) 0.0051(19) 0.0071(18) 0.035(2)
C7 0.060(2) 0.056(2) 0.036(2) -0.0010(18) 0.0021(18) 0.036(2)
C8 0.065(3) 0.047(2) 0.056(3) 0.000(2) -0.006(2) 0.011(2)
C9 0.060(3) 0.067(3) 0.075(4) 0.022(2) -0.008(2) 0.011(2)
C10 0.052(2) 0.059(2) 0.068(3) 0.025(2) 0.010(2) 0.028(2)
C11 0.065(3) 0.060(3) 0.073(3) 0.023(2) 0.018(2) 0.028(2)
C12 0.054(3) 0.067(3) 0.109(4) 0.022(3) 0.029(3) 0.035(2)
C13 0.078(4) 0.080(4) 0.147(6) 0.028(4) 0.029(4) 0.052(3)
C14 0.046(2) 0.048(2) 0.043(2) 0.0061(17) 0.0145(18) 0.0242(18)
C15 0.043(2) 0.043(2) 0.035(4) 0.000 0.000 0.0215(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
Cu1 O1 1.915(3) . ?
Cu1 N1 1.919(3) . ?
Cu1 N3 1.943(4) . ?
Cu1 N2 2.074(3) . ?
Cu2 N4 1.980(6) . ?
Cu2 S1 2.3829(12) . ?
Cu2 S1 2.3829(12) 2_655 ?
Cu2 S1 2.3829(12) 3_665 ?
Cl1 C5 1.739(4) . ?
S1 C14 1.628(4) . ?
S2 C15 1.641(7) . ?
O1 C2 1.286(4) . ?
N1 C7 1.274(5) . ?
N1 C8 1.467(5) . ?
N2 C9 1.467(6) . ?
N2 C10 1.481(5) . ?
N2 C12 1.497(5) . ?
N3 C14 1.157(5) . ?
N4 C15 1.139(8) . ?
C1 C6 1.397(5) . ?
C1 C2 1.419(5) . ?
C1 C7 1.433(5) . ?
C2 C3 1.399(5) . ?
C3 C4 1.378(6) . ?
C3 H3 0.9300 . ?
C4 C5 1.373(6) . ?
C4 H4 0.9300 . ?
C5 C6 1.356(6) . ?
C6 H6 0.9300 . ?
C7 H7 0.9300 . ?
C8 C9 1.493(7) . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C10 C11 1.523(6) . ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
C11 H11A 0.9600 . ?
C11 H11B 0.9600 . ?
C11 H11C 0.9600 . ?
C12 C13 1.447(6) . ?
C12 H12A 0.9700 . ?
C12 H12B 0.9700 . ?
C13 H13A 0.9600 . ?
C13 H13B 0.9600 . ?
C13 H13C 0.9600 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Cu1 N1 91.91(12) . . ?
O1 Cu1 N3 92.48(13) . . ?
N1 Cu1 N3 171.31(14) . . ?
O1 Cu1 N2 159.86(12) . . ?
N1 Cu1 N2 84.96(13) . . ?
N3 Cu1 N2 93.42(14) . . ?
N4 Cu2 S1 106.72(4) . . ?
N4 Cu2 S1 106.72(4) . 2_655 ?
S1 Cu2 S1 112.07(3) . 2_655 ?
N4 Cu2 S1 106.72(4) . 3_665 ?
S1 Cu2 S1 112.07(3) . 3_665 ?
S1 Cu2 S1 112.07(3) 2_655 3_665 ?
C14 S1 Cu2 108.17(14) . . ?
C2 O1 Cu1 128.4(2) . . ?
C7 N1 C8 121.1(3) . . ?
C7 N1 Cu1 128.0(3) . . ?
C8 N1 Cu1 110.9(2) . . ?
C9 N2 C10 111.7(4) . . ?
C9 N2 C12 110.8(4) . . ?
C10 N2 C12 108.1(3) . . ?
C9 N2 Cu1 106.1(2) . . ?
C10 N2 Cu1 109.7(2) . . ?
C12 N2 Cu1 110.4(3) . . ?
C14 N3 Cu1 172.5(3) . . ?
C15 N4 Cu2 180.000(1) . . ?
C6 C1 C2 119.8(4) . . ?
C6 C1 C7 118.0(4) . . ?
C2 C1 C7 122.0(3) . . ?
O1 C2 C3 119.1(3) . . ?
O1 C2 C1 124.5(3) . . ?
C3 C2 C1 116.4(3) . . ?
C4 C3 C2 122.6(4) . . ?
C4 C3 H3 118.7 . . ?
C2 C3 H3 118.7 . . ?
C5 C4 C3 119.7(4) . . ?
C5 C4 H4 120.2 . . ?
C3 C4 H4 120.2 . . ?
C6 C5 C4 120.1(4) . . ?
C6 C5 Cl1 121.3(3) . . ?
C4 C5 Cl1 118.5(3) . . ?
C5 C6 C1 121.4(4) . . ?
C5 C6 H6 119.3 . . ?
C1 C6 H6 119.3 . . ?
N1 C7 C1 125.1(4) . . ?
N1 C7 H7 117.5 . . ?
C1 C7 H7 117.5 . . ?
N1 C8 C9 106.8(4) . . ?
N1 C8 H8A 110.4 . . ?
C9 C8 H8A 110.4 . . ?
N1 C8 H8B 110.4 . . ?
C9 C8 H8B 110.4 . . ?
H8A C8 H8B 108.6 . . ?
N2 C9 C8 110.4(4) . . ?
N2 C9 H9A 109.6 . . ?
C8 C9 H9A 109.6 . . ?
N2 C9 H9B 109.6 . . ?
C8 C9 H9B 109.6 . . ?
H9A C9 H9B 108.1 . . ?
N2 C10 C11 116.1(4) . . ?
N2 C10 H10A 108.3 . . ?
C11 C10 H10A 108.3 . . ?
N2 C10 H10B 108.3 . . ?
C11 C10 H10B 108.3 . . ?
H10A C10 H10B 107.4 . . ?
C10 C11 H11A 109.5 . . ?
C10 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
C10 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
C13 C12 N2 116.1(4) . . ?
C13 C12 H12A 108.3 . . ?
N2 C12 H12A 108.3 . . ?
C13 C12 H12B 108.3 . . ?
N2 C12 H12B 108.3 . . ?
H12A C12 H12B 107.4 . . ?
C12 C13 H13A 109.5 . . ?
C12 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C12 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
N3 C14 S1 177.8(4) . . ?
N4 C15 S2 180.000(1) . . ?

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        27.50
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         0.315
_refine_diff_density_min         -0.244
_refine_diff_density_rms         0.053


data_1
_database_code_depnum_ccdc_archive 'CCDC 889124'
#TrackingRef '1.cif'


_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C43 H57 Cu4 N10 O3 S4'
_chemical_formula_weight         1144.39

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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'

_symmetry_cell_setting           hexagonal
_symmetry_space_group_name_H-M   R3c

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'-y, -x, z+1/2'
'-x+y, y, z+1/2'
'x, x-y, z+1/2'
'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'
'-y+2/3, -x+1/3, z+5/6'
'-x+y+2/3, y+1/3, z+5/6'
'x+2/3, x-y+1/3, z+5/6'
'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'
'-y+1/3, -x+2/3, z+7/6'
'-x+y+1/3, y+2/3, z+7/6'
'x+1/3, x-y+2/3, z+7/6'

_cell_length_a                   20.6498(8)
_cell_length_b                   20.6498(8)
_cell_length_c                   20.3322(13)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_volume                     7508.4(6)
_cell_formula_units_Z            6
_cell_measurement_temperature    298(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       block
_exptl_crystal_colour            blue
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.519
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             3534
_exptl_absorpt_coefficient_mu    1.892
_exptl_absorpt_correction_type   ?
_exptl_absorpt_correction_T_min  0.6702
_exptl_absorpt_correction_T_max  0.7035
_exptl_absorpt_process_details   ?

_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  ?
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            13212
_diffrn_reflns_av_R_equivalents  0.0430
_diffrn_reflns_av_sigmaI/netI    0.0424
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_theta_min         2.30
_diffrn_reflns_theta_max         25.49
_reflns_number_total             3012
_reflns_number_gt                2282
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
;
Refinement of 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.
;

_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^)+(0.0323P)^2^+8.9356P] 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    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.016(18)
_refine_ls_number_reflns         3012
_refine_ls_number_parameters     196
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0592
_refine_ls_R_factor_gt           0.0358
_refine_ls_wR_factor_ref         0.0816
_refine_ls_wR_factor_gt          0.0722
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_restrained_S_all      1.029
_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 0.83908(3) 0.42346(3) 0.62017(3) 0.05655(18) Uani 1 1 d . . .
Cu2 Cu 0.6667 0.3333 0.86308(4) 0.0531(3) Uani 1 3 d S . .
N1 N 0.83613(17) 0.38817(19) 0.53182(19) 0.0430(8) Uani 1 1 d . . .
N2 N 0.8929(3) 0.3688(3) 0.65707(19) 0.0670(12) Uani 1 1 d . . .
N3 N 0.8081(2) 0.4388(2) 0.7056(2) 0.0663(11) Uani 1 1 d . . .
N4 N 0.6667 0.3333 0.9598(3) 0.0389(14) Uani 1 3 d S . .
O1 O 0.87115(17) 0.52393(16) 0.59337(15) 0.0562(8) Uani 1 1 d . . .
S1 S 0.75710(7) 0.45628(7) 0.82748(6) 0.0553(3) Uani 1 1 d . . .
S2 S 0.6667 0.3333 1.09747(8) 0.0483(5) Uani 1 3 d S . .
C1 C 0.8662(2) 0.5047(2) 0.4769(2) 0.0402(10) Uani 1 1 d . . .
C2 C 0.8805(2) 0.5497(2) 0.5341(2) 0.0432(10) Uani 1 1 d . . .
C3 C 0.9050(2) 0.6264(2) 0.5242(2) 0.0521(12) Uani 1 1 d . . .
C4 C 0.9119(3) 0.6548(3) 0.4613(3) 0.0675(14) Uani 1 1 d . . .
H4 H 0.9276 0.7053 0.4558 0.081 Uiso 1 1 calc R . .
C5 C 0.8959(3) 0.6093(3) 0.4061(3) 0.0677(14) Uani 1 1 d . . .
H5 H 0.8999 0.6290 0.3642 0.081 Uiso 1 1 calc R . .
C6 C 0.8744(2) 0.5363(3) 0.4140(2) 0.0538(12) Uani 1 1 d . . .
H6 H 0.8648 0.5063 0.3770 0.065 Uiso 1 1 calc R . .
C7 C 0.9243(3) 0.6759(3) 0.5843(3) 0.0794(18) Uani 1 1 d . . .
H7A H 0.8799 0.6615 0.6095 0.119 Uiso 1 1 calc R . .
H7B H 0.9456 0.7271 0.5708 0.119 Uiso 1 1 calc R . .
H7C H 0.9599 0.6705 0.6108 0.119 Uiso 1 1 calc R . .
C8 C 0.8447(2) 0.4275(2) 0.4802(2) 0.0408(11) Uani 1 1 d . . .
H8 H 0.8358 0.4027 0.4402 0.049 Uiso 1 1 calc R . .
C9 C 0.8136(3) 0.3089(2) 0.5230(2) 0.0567(13) Uani 1 1 d . . .
H9A H 0.8102 0.2977 0.4764 0.068 Uiso 1 1 calc R . .
H9B H 0.7645 0.2780 0.5421 0.068 Uiso 1 1 calc R . .
C10 C 0.8678(3) 0.2901(3) 0.5545(2) 0.0602(13) Uani 1 1 d . . .
H10A H 0.9176 0.3239 0.5378 0.072 Uiso 1 1 calc R . .
H10B H 0.8549 0.2397 0.5418 0.072 Uiso 1 1 calc R . .
C11 C 0.8693(3) 0.2949(3) 0.6290(3) 0.0817(17) Uani 1 1 d . . .
H11A H 0.8195 0.2602 0.6453 0.098 Uiso 1 1 calc R . .
H11B H 0.9026 0.2781 0.6454 0.098 Uiso 1 1 calc R . .
C12 C 0.9732(4) 0.4221(3) 0.6383(3) 0.100(2) Uani 1 1 d . . .
H12A H 1.0039 0.4019 0.6522 0.151 Uiso 1 1 calc R . .
H12B H 0.9899 0.4694 0.6595 0.151 Uiso 1 1 calc R . .
H12C H 0.9768 0.4289 0.5915 0.151 Uiso 1 1 calc R . .
C13 C 0.8936(5) 0.3636(5) 0.7293(3) 0.124(3) Uani 1 1 d . . .
H13A H 0.9271 0.3462 0.7422 0.186 Uiso 1 1 calc R . .
H13B H 0.8441 0.3291 0.7447 0.186 Uiso 1 1 calc R . .
H13C H 0.9101 0.4120 0.7482 0.186 Uiso 1 1 calc R . .
C14 C 0.7861(2) 0.4449(2) 0.7554(2) 0.0465(11) Uani 1 1 d . . .
C15 C 0.6667 0.3333 1.0167(4) 0.0346(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
Cu1 0.0806(4) 0.0639(4) 0.0345(3) 0.0032(3) 0.0159(3) 0.0431(4)
Cu2 0.0653(4) 0.0653(4) 0.0286(5) 0.000 0.000 0.0327(2)
N1 0.0389(19) 0.039(2) 0.046(2) -0.0035(17) 0.0083(16) 0.0164(16)
N2 0.082(3) 0.078(3) 0.052(3) 0.008(2) 0.012(2) 0.049(3)
N3 0.082(3) 0.080(3) 0.037(2) -0.007(2) 0.013(2) 0.041(3)
N4 0.044(2) 0.044(2) 0.029(3) 0.000 0.000 0.0219(11)
O1 0.074(2) 0.0509(18) 0.0407(18) -0.0083(14) 0.0056(15) 0.0292(16)
S1 0.0700(8) 0.0597(7) 0.0341(6) -0.0011(5) 0.0115(6) 0.0309(6)
S2 0.0599(7) 0.0599(7) 0.0253(9) 0.000 0.000 0.0299(3)
C1 0.034(2) 0.048(2) 0.040(2) -0.003(2) -0.0024(19) 0.022(2)
C2 0.036(2) 0.046(3) 0.048(3) -0.005(2) 0.0003(19) 0.020(2)
C3 0.041(3) 0.045(3) 0.067(3) -0.010(2) -0.004(2) 0.019(2)
C4 0.062(3) 0.048(3) 0.094(5) 0.008(3) -0.009(3) 0.028(2)
C5 0.074(3) 0.079(4) 0.060(3) 0.013(3) -0.002(3) 0.046(3)
C6 0.050(3) 0.066(3) 0.044(3) 0.002(2) -0.005(2) 0.028(3)
C7 0.079(4) 0.057(3) 0.105(5) -0.020(3) -0.003(3) 0.035(3)
C8 0.031(2) 0.051(3) 0.036(2) -0.010(2) 0.0022(17) 0.017(2)
C9 0.055(3) 0.046(3) 0.061(3) -0.004(2) 0.006(2) 0.020(2)
C10 0.064(3) 0.050(3) 0.072(4) 0.001(2) 0.006(3) 0.033(2)
C11 0.084(4) 0.078(4) 0.088(5) 0.026(3) 0.014(3) 0.044(3)
C12 0.084(5) 0.094(5) 0.124(6) -0.009(4) -0.012(4) 0.046(4)
C13 0.193(8) 0.193(8) 0.058(4) 0.011(4) -0.010(4) 0.151(7)
C14 0.056(3) 0.056(3) 0.034(3) 0.003(2) 0.003(2) 0.032(2)
C15 0.038(2) 0.038(2) 0.029(4) 0.000 0.000 0.0189(12)

_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 O1 1.915(3) . ?
Cu1 N1 1.928(4) . ?
Cu1 N3 1.932(4) . ?
Cu1 N2 2.080(4) . ?
Cu2 N4 1.967(6) . ?
Cu2 S1 2.3908(13) 3_665 ?
Cu2 S1 2.3908(13) . ?
Cu2 S1 2.3908(13) 2_655 ?
N1 C8 1.284(5) . ?
N1 C9 1.471(6) . ?
N2 C11 1.467(7) . ?
N2 C13 1.474(7) . ?
N2 C12 1.510(7) . ?
N3 C14 1.142(5) . ?
N4 C15 1.157(8) . ?
O1 C2 1.292(5) . ?
S1 C14 1.643(4) . ?
S2 C15 1.641(7) . ?
C1 C6 1.407(6) . ?
C1 C2 1.424(5) . ?
C1 C8 1.426(5) . ?
C2 C3 1.417(6) . ?
C3 C4 1.384(7) . ?
C3 C7 1.513(6) . ?
C4 C5 1.393(7) . ?
C4 H4 0.9300 . ?
C5 C6 1.352(7) . ?
C5 H5 0.9300 . ?
C6 H6 0.9300 . ?
C7 H7A 0.9600 . ?
C7 H7B 0.9600 . ?
C7 H7C 0.9600 . ?
C8 H8 0.9300 . ?
C9 C10 1.500(6) . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C10 C11 1.517(7) . ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
C12 H12A 0.9600 . ?
C12 H12B 0.9600 . ?
C12 H12C 0.9600 . ?
C13 H13A 0.9600 . ?
C13 H13B 0.9600 . ?
C13 H13C 0.9600 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Cu1 N1 94.18(14) . . ?
O1 Cu1 N3 92.40(16) . . ?
N1 Cu1 N3 161.72(17) . . ?
O1 Cu1 N2 134.54(17) . . ?
N1 Cu1 N2 93.19(16) . . ?
N3 Cu1 N2 94.31(18) . . ?
N4 Cu2 S1 107.62(4) . 3_665 ?
N4 Cu2 S1 107.62(4) . . ?
S1 Cu2 S1 111.25(4) 3_665 . ?
N4 Cu2 S1 107.62(4) . 2_655 ?
S1 Cu2 S1 111.25(4) 3_665 2_655 ?
S1 Cu2 S1 111.25(4) . 2_655 ?
C8 N1 C9 118.2(4) . . ?
C8 N1 Cu1 123.6(3) . . ?
C9 N1 Cu1 117.8(3) . . ?
C11 N2 C13 108.7(5) . . ?
C11 N2 C12 109.5(4) . . ?
C13 N2 C12 104.9(5) . . ?
C11 N2 Cu1 115.8(3) . . ?
C13 N2 Cu1 115.3(4) . . ?
C12 N2 Cu1 101.7(3) . . ?
C14 N3 Cu1 176.5(4) . . ?
C15 N4 Cu2 180.000(3) . . ?
C2 O1 Cu1 127.6(3) . . ?
C14 S1 Cu2 105.37(17) . . ?
C6 C1 C2 120.2(4) . . ?
C6 C1 C8 117.4(4) . . ?
C2 C1 C8 122.5(4) . . ?
O1 C2 C3 119.2(4) . . ?
O1 C2 C1 123.7(4) . . ?
C3 C2 C1 117.1(4) . . ?
C4 C3 C2 120.5(4) . . ?
C4 C3 C7 121.6(5) . . ?
C2 C3 C7 117.8(4) . . ?
C3 C4 C5 121.3(4) . . ?
C3 C4 H4 119.4 . . ?
C5 C4 H4 119.4 . . ?
C6 C5 C4 119.5(5) . . ?
C6 C5 H5 120.3 . . ?
C4 C5 H5 120.3 . . ?
C5 C6 C1 121.4(4) . . ?
C5 C6 H6 119.3 . . ?
C1 C6 H6 119.3 . . ?
C3 C7 H7A 109.5 . . ?
C3 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
C3 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
N1 C8 C1 127.9(4) . . ?
N1 C8 H8 116.1 . . ?
C1 C8 H8 116.1 . . ?
N1 C9 C10 112.0(4) . . ?
N1 C9 H9A 109.2 . . ?
C10 C9 H9A 109.2 . . ?
N1 C9 H9B 109.2 . . ?
C10 C9 H9B 109.2 . . ?
H9A C9 H9B 107.9 . . ?
C9 C10 C11 113.7(4) . . ?
C9 C10 H10A 108.8 . . ?
C11 C10 H10A 108.8 . . ?
C9 C10 H10B 108.8 . . ?
C11 C10 H10B 108.8 . . ?
H10A C10 H10B 107.7 . . ?
N2 C11 C10 116.2(4) . . ?
N2 C11 H11A 108.2 . . ?
C10 C11 H11A 108.2 . . ?
N2 C11 H11B 108.2 . . ?
C10 C11 H11B 108.2 . . ?
H11A C11 H11B 107.4 . . ?
N2 C12 H12A 109.5 . . ?
N2 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
N2 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
N2 C13 H13A 109.5 . . ?
N2 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
N2 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
N3 C14 S1 178.1(5) . . ?
N4 C15 S2 180.000(2) . . ?

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        25.49
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         0.289
_refine_diff_density_min         -0.226
_refine_diff_density_rms         0.054