# Supplementary Material (ESI) for Dalton Transactions
# This journal is (c) The Royal Society of Chemistry 2010

data_global

_journal_name_full               'Dalton Trans.'
_journal_coden_cambridge         0222
_journal_year                    ?
_journal_volume                  ?
_journal_page_first              ?
_publ_contact_author_name        'Marius Andruh'
_publ_contact_author_email       marius.andruh@dnt.ro
loop_
_publ_author_name
'Catalin Maxim'
'Lorenzo Sorace'
'Panchanana Khuntia'
'Augustin M. Madalan'
'Victor Kravtsov'
;
A.Lascialfari
;
'Andrea Caneschi'
'Yves Journaux'
'Marius Andruh'

# Attachment 'crystal1.cif'

data_cmmn1
_database_code_depnum_ccdc_archive 'CCDC 755664'
#TrackingRef 'crystal1.cif'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C22 H40 Cl2 Cu2 N4 O15'
_chemical_formula_weight         798.56

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'
O O 0.0106 0.0060 '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'
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           orthorhombic
_symmetry_space_group_name_H-M   Fdd2

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z'
'-x+1/4, y+1/4, z+1/4'
'x+1/4, -y+1/4, z+1/4'
'x, y+1/2, z+1/2'
'-x, -y+1/2, z+1/2'
'-x+1/4, y+3/4, z+3/4'
'x+1/4, -y+3/4, z+3/4'
'x+1/2, y, z+1/2'
'-x+1/2, -y, z+1/2'
'-x+3/4, y+1/4, z+3/4'
'x+3/4, -y+1/4, z+3/4'
'x+1/2, y+1/2, z'
'-x+1/2, -y+1/2, z'
'-x+3/4, y+3/4, z+1/4'
'x+3/4, -y+3/4, z+1/4'

_cell_length_a                   17.5460(11)
_cell_length_b                   37.8030(11)
_cell_length_c                   9.994(2)
_cell_angle_alpha                90.000(5)
_cell_angle_beta                 90.000(4)
_cell_angle_gamma                90.000(5)
_cell_volume                     6628.9(15)
_cell_formula_units_Z            8
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    584
_cell_measurement_theta_min      2.5
_cell_measurement_theta_max      25.00

_exptl_crystal_description       prism
_exptl_crystal_colour            green
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_density_diffrn    1.600
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             3296
_exptl_absorpt_coefficient_mu    1.516
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.7514
_exptl_absorpt_correction_T_max  0.8632
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      150(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  'Nonius Kappa CCD'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            10387
_diffrn_reflns_av_R_equivalents  0.0675
_diffrn_reflns_av_sigmaI/netI    0.0666
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_k_min       -47
_diffrn_reflns_limit_k_max       47
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_theta_min         2.41
_diffrn_reflns_theta_max         26.50
_reflns_number_total             3249
_reflns_number_gt                2458
_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^)+(0.0563P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    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   0.008(19)
_refine_ls_number_reflns         3249
_refine_ls_number_parameters     234
_refine_ls_number_restraints     48
_refine_ls_R_factor_all          0.0643
_refine_ls_R_factor_gt           0.0440
_refine_ls_wR_factor_ref         0.1055
_refine_ls_wR_factor_gt          0.1002
_refine_ls_goodness_of_fit_ref   1.002
_refine_ls_restrained_S_all      1.018
_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 0.10655(3) -0.020999(15) 0.59654(5) 0.03607(17) Uani 1 1 d . . .
O1 O 0.10497(17) 0.02247(8) 0.5003(3) 0.0362(8) Uani 1 1 d . . .
O1W O 0.0393(2) -0.04174(9) 0.4602(4) 0.0419(9) Uani 1 1 d D . .
H1W1 H 0.060(2) -0.0372(14) 0.380(2) 0.063 Uiso 1 1 d D . .
H2W1 H -0.0055(15) -0.0320(16) 0.460(5) 0.063 Uiso 1 1 d D . .
O2W O 0.0000 0.0000 0.7383(5) 0.0513(14) Uani 1 2 d SD . .
H1W2 H 0.020(3) 0.0158(9) 0.801(2) 0.077 Uiso 1 1 d D . .
N1 N 0.1849(2) -0.00493(12) 0.7188(4) 0.0407(10) Uani 1 1 d . . .
N2 N 0.1184(3) -0.06849(12) 0.6907(5) 0.0508(12) Uani 1 1 d . . .
C1 C 0.1454(2) 0.05179(12) 0.5275(5) 0.0343(10) Uani 1 1 d . . .
C2 C 0.1357(3) 0.08103(13) 0.4420(6) 0.0401(12) Uani 1 1 d . . .
H2 H 0.1026 0.0790 0.3672 0.048 Uiso 1 1 calc R . .
C3 C 0.1728(3) 0.11232(15) 0.4643(6) 0.0516(14) Uani 1 1 d . . .
H3 H 0.1657 0.1317 0.4050 0.062 Uiso 1 1 calc R . .
C4 C 0.2214(3) 0.11573(16) 0.5752(8) 0.0681(19) Uani 1 1 d . . .
H4 H 0.2453 0.1378 0.5936 0.082 Uiso 1 1 calc R . .
C5 C 0.2341(3) 0.08798(18) 0.6546(6) 0.0562(15) Uani 1 1 d . . .
H5 H 0.2687 0.0903 0.7272 0.067 Uiso 1 1 calc R . .
C6 C 0.1971(3) 0.05483(14) 0.6333(5) 0.0395(12) Uani 1 1 d . . .
C7 C 0.2135(3) 0.02581(16) 0.7238(5) 0.0482(14) Uani 1 1 d . . .
H7 H 0.2491 0.0303 0.7934 0.058 Uiso 1 1 calc R . .
C8 C 0.2111(3) -0.03190(17) 0.8139(6) 0.0605(16) Uani 1 1 d . . .
H8A H 0.2211 -0.0211 0.9024 0.073 Uiso 1 1 calc R . .
H8B H 0.2588 -0.0430 0.7815 0.073 Uiso 1 1 calc R . .
C9 C 0.1478(3) -0.05975(17) 0.8251(6) 0.0634(18) Uani 1 1 d . . .
H9A H 0.1682 -0.0814 0.8682 0.076 Uiso 1 1 calc R . .
H9B H 0.1059 -0.0505 0.8814 0.076 Uiso 1 1 calc R . .
C10 C 0.1742(3) -0.08924(15) 0.6117(7) 0.0686(19) Uani 1 1 d . . .
H10A H 0.1855 -0.1114 0.6585 0.103 Uiso 1 1 calc R . .
H10B H 0.2212 -0.0755 0.6012 0.103 Uiso 1 1 calc R . .
H10C H 0.1527 -0.0945 0.5234 0.103 Uiso 1 1 calc R . .
C11 C 0.0457(3) -0.08943(16) 0.7011(7) 0.0688(19) Uani 1 1 d . . .
H11A H 0.0271 -0.0951 0.6112 0.103 Uiso 1 1 calc R . .
H11B H 0.0073 -0.0754 0.7486 0.103 Uiso 1 1 calc R . .
H11C H 0.0554 -0.1114 0.7504 0.103 Uiso 1 1 calc R . .
Cl1A Cl 0.09460(8) 0.05434(4) 0.03219(13) 0.0461(3) Uani 0.740(6) 1 d PD A 1
O1CL O 0.1352(8) 0.0363(3) 0.1275(12) 0.165(5) Uani 0.740(6) 1 d PD A 1
O2CL O 0.0535(7) 0.0266(3) -0.0285(9) 0.161(5) Uani 0.740(6) 1 d PD A 1
O3CL O 0.0346(6) 0.0743(3) 0.0820(11) 0.200(6) Uani 0.740(6) 1 d PD A 1
O4CL O 0.1335(6) 0.0727(2) -0.0686(11) 0.131(4) Uani 0.740(6) 1 d PD A 1
Cl1B Cl 0.09460(8) 0.05434(4) 0.03219(13) 0.0461(3) Uani 0.260(6) 1 d PD A 2
O5CL O 0.1492(10) 0.0276(5) 0.054(2) 0.069 Uiso 0.260(6) 1 d PD A 2
O6CL O 0.1300(9) 0.0860(3) 0.0762(17) 0.069 Uiso 0.260(6) 1 d PD A 2
O7CL O 0.0817(11) 0.0574(5) -0.1006(12) 0.069 Uiso 0.260(6) 1 d PD A 2
O8CL O 0.0396(8) 0.0498(5) 0.1302(15) 0.069 Uiso 0.260(6) 1 d PD A 2
O1WS O 0.0919(2) 0.96606(13) 0.2096(4) 0.0612(11) Uani 1 1 d D . .
H1WS H 0.089(3) 0.9887(7) 0.179(7) 0.092 Uiso 1 1 d D . .
H2WS H 0.053(3) 0.9557(12) 0.161(6) 0.092 Uiso 1 1 d D . .

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 0.0342(3) 0.0395(3) 0.0346(3) 0.0036(3) 0.0024(3) 0.0069(3)
O1 0.0376(18) 0.0326(18) 0.0383(19) 0.0009(14) -0.0053(16) -0.0034(15)
O1W 0.0379(19) 0.0389(19) 0.049(2) -0.0061(17) 0.0105(17) -0.0008(16)
O2W 0.043(3) 0.075(4) 0.037(3) 0.000 0.000 0.021(3)
N1 0.032(2) 0.058(3) 0.033(2) 0.008(2) -0.0058(19) 0.010(2)
N2 0.049(3) 0.050(3) 0.054(3) 0.019(2) 0.016(2) 0.009(2)
C1 0.027(2) 0.033(2) 0.042(3) -0.004(2) 0.003(2) 0.002(2)
C2 0.034(3) 0.037(3) 0.049(3) 0.003(2) 0.003(2) 0.001(2)
C3 0.040(3) 0.042(3) 0.073(4) 0.005(3) 0.007(3) 0.000(2)
C4 0.054(3) 0.048(3) 0.103(6) -0.014(4) -0.009(4) -0.010(3)
C5 0.041(3) 0.069(4) 0.059(3) -0.016(3) -0.003(3) -0.013(3)
C6 0.030(2) 0.054(3) 0.035(3) -0.009(2) 0.002(2) 0.002(2)
C7 0.034(3) 0.079(4) 0.031(3) -0.002(3) -0.009(2) 0.007(3)
C8 0.049(3) 0.081(4) 0.051(4) 0.019(3) -0.001(3) 0.021(3)
C9 0.056(3) 0.080(4) 0.055(4) 0.029(3) 0.010(3) 0.025(3)
C10 0.065(3) 0.050(3) 0.090(5) 0.025(4) 0.029(4) 0.026(3)
C11 0.062(4) 0.058(4) 0.087(5) 0.025(3) 0.036(4) -0.003(3)
Cl1A 0.0520(8) 0.0497(7) 0.0365(6) 0.0016(6) -0.0021(7) -0.0066(7)
O1CL 0.240(13) 0.108(8) 0.148(10) 0.033(7) -0.131(10) 0.011(7)
O2CL 0.250(14) 0.123(7) 0.110(7) 0.008(6) -0.082(9) -0.090(8)
O3CL 0.280(13) 0.133(7) 0.188(10) 0.084(8) 0.164(11) 0.135(8)
O4CL 0.132(7) 0.097(6) 0.165(8) 0.050(6) 0.098(7) 0.021(5)
Cl1B 0.0520(8) 0.0497(7) 0.0365(6) 0.0016(6) -0.0021(7) -0.0066(7)
O1WS 0.058(3) 0.076(3) 0.050(2) 0.006(2) 0.002(2) 0.015(2)

_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 1.904(3) . ?
Cu1 N1 1.937(4) . ?
Cu1 O1W 1.966(4) . ?
Cu1 N2 2.037(4) . ?
Cu1 O2W 2.477(3) . ?
O1 C1 1.344(5) . ?
O1W H1W1 0.891(12) . ?
O1W H2W1 0.87(3) . ?
O2W Cu1 2.477(3) 2 ?
O2W H1W2 0.934(14) . ?
N1 C7 1.267(7) . ?
N1 C8 1.468(7) . ?
N2 C9 1.477(8) . ?
N2 C10 1.481(7) . ?
N2 C11 1.505(7) . ?
C1 C6 1.398(7) . ?
C1 C2 1.407(7) . ?
C2 C3 1.369(7) . ?
C2 H2 0.9500 . ?
C3 C4 1.404(8) . ?
C3 H3 0.9500 . ?
C4 C5 1.334(9) . ?
C4 H4 0.9500 . ?
C5 C6 1.428(8) . ?
C5 H5 0.9500 . ?
C6 C7 1.451(8) . ?
C7 H7 0.9500 . ?
C8 C9 1.535(9) . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
Cl1A O1CL 1.370(7) . ?
Cl1A O3CL 1.388(7) . ?
Cl1A O4CL 1.400(7) . ?
Cl1A O2CL 1.410(7) . ?
O1WS H1WS 0.910(19) . ?
O1WS H2WS 0.928(17) . ?

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 93.34(16) . . ?
O1 Cu1 O1W 89.16(14) . . ?
N1 Cu1 O1W 171.28(16) . . ?
O1 Cu1 N2 174.29(16) . . ?
N1 Cu1 N2 85.0(2) . . ?
O1W Cu1 N2 91.72(18) . . ?
O1 Cu1 O2W 90.08(12) . . ?
N1 Cu1 O2W 94.27(14) . . ?
O1W Cu1 O2W 94.08(13) . . ?
N2 Cu1 O2W 95.48(14) . . ?
C1 O1 Cu1 127.0(3) . . ?
Cu1 O1W H1W1 108(3) . . ?
Cu1 O1W H2W1 112(4) . . ?
H1W1 O1W H2W1 106(3) . . ?
Cu1 O2W Cu1 110.19(19) 2 . ?
Cu1 O2W H1W2 117(4) 2 . ?
Cu1 O2W H1W2 108(4) . . ?
C7 N1 C8 119.2(5) . . ?
C7 N1 Cu1 126.4(4) . . ?
C8 N1 Cu1 114.4(4) . . ?
C9 N2 C10 111.9(5) . . ?
C9 N2 C11 110.5(5) . . ?
C10 N2 C11 108.6(5) . . ?
C9 N2 Cu1 105.0(4) . . ?
C10 N2 Cu1 106.8(3) . . ?
C11 N2 Cu1 114.1(4) . . ?
O1 C1 C6 124.3(4) . . ?
O1 C1 C2 117.5(4) . . ?
C6 C1 C2 118.2(4) . . ?
C3 C2 C1 121.5(5) . . ?
C3 C2 H2 119.3 . . ?
C1 C2 H2 119.3 . . ?
C2 C3 C4 119.8(6) . . ?
C2 C3 H3 120.1 . . ?
C4 C3 H3 120.1 . . ?
C5 C4 C3 119.9(5) . . ?
C5 C4 H4 120.1 . . ?
C3 C4 H4 120.1 . . ?
C4 C5 C6 121.7(5) . . ?
C4 C5 H5 119.1 . . ?
C6 C5 H5 119.1 . . ?
C1 C6 C5 118.7(5) . . ?
C1 C6 C7 122.6(5) . . ?
C5 C6 C7 118.7(5) . . ?
N1 C7 C6 126.2(5) . . ?
N1 C7 H7 116.9 . . ?
C6 C7 H7 116.9 . . ?
N1 C8 C9 107.3(5) . . ?
N1 C8 H8A 110.3 . . ?
C9 C8 H8A 110.3 . . ?
N1 C8 H8B 110.3 . . ?
C9 C8 H8B 110.3 . . ?
H8A C8 H8B 108.5 . . ?
N2 C9 C8 109.9(5) . . ?
N2 C9 H9A 109.7 . . ?
C8 C9 H9A 109.7 . . ?
N2 C9 H9B 109.7 . . ?
C8 C9 H9B 109.7 . . ?
H9A C9 H9B 108.2 . . ?
N2 C10 H10A 109.5 . . ?
N2 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
N2 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
N2 C11 H11A 109.5 . . ?
N2 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
N2 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
O1CL Cl1A O3CL 114.5(7) . . ?
O1CL Cl1A O4CL 119.5(7) . . ?
O3CL Cl1A O4CL 110.9(5) . . ?
O1CL Cl1A O2CL 101.2(6) . . ?
O3CL Cl1A O2CL 99.9(8) . . ?
O4CL Cl1A O2CL 108.0(7) . . ?
H1WS O1WS H2WS 100(3) . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O1W H1W1 O1WS 0.891(12) 1.802(14) 2.685(5) 171(5) 1_545
O1W H2W1 O1 0.87(3) 1.826(19) 2.664(5) 162(5) 2
O2W H1W2 O2CL 0.934(14) 1.847(17) 2.706(9) 152(2) 1_556
O1WS H1WS O1CL 0.910(19) 2.043(18) 2.883(12) 153(4) 1_565
O1WS H2WS O3CL 0.928(17) 2.065(16) 2.981(11) 169(5) 2_565

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        26.50
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         0.558
_refine_diff_density_min         -0.614
_refine_diff_density_rms         0.076

# Attachment 'crystal2.cif'

data_shelxl_crystal2
_database_code_depnum_ccdc_archive 'CCDC 755665'
#TrackingRef 'crystal2.cif'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C72 H118 Cl3 Cu6 Fe N18 O32'
_chemical_formula_weight         2291.28

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'
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 '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'

_symmetry_cell_setting           Hexagonal
_symmetry_space_group_name_H-M   R-3c

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

_cell_length_a                   27.8777(16)
_cell_length_b                   27.8777(16)
_cell_length_c                   21.3690(13)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_volume                     14382.3(15)
_cell_formula_units_Z            6
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    8000
_cell_measurement_theta_min      2.5
_cell_measurement_theta_max      25.75

_exptl_crystal_description       needle
_exptl_crystal_colour            green
_exptl_crystal_size_max          0.7
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.15
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_density_diffrn    1.587
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             7098
_exptl_absorpt_coefficient_mu    1.623
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.5751
_exptl_absorpt_correction_T_max  0.6399
_exptl_absorpt_process_details   wingx

_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  'STOE-IPDS I'
_diffrn_measurement_method       'Oscillation, Phi. incr. = 0.8'
_diffrn_detector_area_resol_mean 6.6
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            26006
_diffrn_reflns_av_R_equivalents  0.0547
_diffrn_reflns_av_sigmaI/netI    0.0411
_diffrn_reflns_limit_h_min       -33
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_theta_min         2.43
_diffrn_reflns_theta_max         25.27
_reflns_number_total             2900
_reflns_number_gt                1754
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'EXPOSE [STOE-IPDS]'
_computing_cell_refinement       'SELECT, CELL [STOE-IPDS]'
_computing_data_reduction        'INTEGRATE [STOE-IPDS]'
_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^)+(0.1105P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     SHELXL
_refine_ls_extinction_coef       0.00063(10)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_number_reflns         2900
_refine_ls_number_parameters     215
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0959
_refine_ls_R_factor_gt           0.0573
_refine_ls_wR_factor_ref         0.1701
_refine_ls_wR_factor_gt          0.1488
_refine_ls_goodness_of_fit_ref   1.003
_refine_ls_restrained_S_all      1.003
_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
C1 C 0.2269(2) 0.1140(2) 0.1871(3) 0.0611(14) Uani 1 1 d . . .
C2 C 0.2333(3) 0.1623(3) 0.2145(3) 0.0782(18) Uani 1 1 d . . .
H2 H 0.2082 0.1740 0.2045 0.094 Uiso 1 1 calc R . .
C3 C 0.2755(3) 0.1930(3) 0.2556(4) 0.091(2) Uani 1 1 d . . .
H3 H 0.2778 0.2243 0.2742 0.109 Uiso 1 1 calc R . .
C4 C 0.3145(3) 0.1782(3) 0.2698(3) 0.0838(19) Uani 1 1 d . . .
H4 H 0.3426 0.1988 0.2983 0.101 Uiso 1 1 calc R . .
C5 C 0.3113(3) 0.1329(3) 0.2418(3) 0.0732(17) Uani 1 1 d . . .
H5 H 0.3386 0.1238 0.2499 0.088 Uiso 1 1 calc R . .
C6 C 0.2677(2) 0.0994(2) 0.2006(3) 0.0556(12) Uani 1 1 d . . .
C7 C 0.2686(3) 0.0538(3) 0.1724(3) 0.0724(17) Uani 1 1 d . . .
H7 H 0.2982 0.0487 0.1823 0.087 Uiso 1 1 calc R . .
C8 C 0.2410(3) -0.0236(3) 0.1051(5) 0.104(3) Uani 1 1 d . . .
H8A H 0.2638 -0.0087 0.0681 0.125 Uiso 1 1 calc R . .
H8B H 0.2600 -0.0352 0.1342 0.125 Uiso 1 1 calc R . .
C9 C 0.1882(5) -0.0702(4) 0.0886(6) 0.156(5) Uani 1 1 d . . .
H9A H 0.1713 -0.0920 0.1259 0.187 Uiso 1 1 calc R . .
H9B H 0.1941 -0.0933 0.0594 0.187 Uiso 1 1 calc R . .
C10 C 0.1586(5) -0.0422(4) -0.0055(4) 0.125(3) Uani 1 1 d . . .
H10A H 0.1327 -0.0315 -0.0199 0.187 Uiso 1 1 calc R . .
H10B H 0.1531 -0.0743 -0.0281 0.187 Uiso 1 1 calc R . .
H10C H 0.1957 -0.0123 -0.0122 0.187 Uiso 1 1 calc R . .
C11 C 0.0929(4) -0.1028(3) 0.0682(6) 0.147(4) Uani 1 1 d . . .
H11A H 0.0857 -0.1121 0.1117 0.220 Uiso 1 1 calc R . .
H11B H 0.0896 -0.1341 0.0455 0.220 Uiso 1 1 calc R . .
H11C H 0.0666 -0.0932 0.0522 0.220 Uiso 1 1 calc R . .
C12 C 0.0600(2) 0.00778(19) 0.0491(3) 0.0516(12) Uani 1 1 d . . .
Cu1 Cu 0.16356(3) 0.01505(3) 0.11071(3) 0.0546(3) Uani 1 1 d . . .
Fe1 Fe 0.0000 0.0000 0.0000 0.0423(4) Uani 1 6 d S . .
N1 N 0.2318(2) 0.0188(2) 0.1341(3) 0.0710(14) Uani 1 1 d . . .
N2 N 0.1501(2) -0.0549(2) 0.0605(3) 0.0798(16) Uani 1 1 d . . .
N3 N 0.09797(19) 0.01194(19) 0.0763(2) 0.0613(12) Uani 1 1 d . . .
O1 O 0.18399(16) 0.08430(17) 0.1498(2) 0.0712(11) Uani 1 1 d . . .
O2 O 0.1126(3) -0.0385(3) 0.1996(3) 0.136(2) Uani 1 1 d . . .
Cl1 Cl 0.3333 0.29181(9) 0.4167 0.0848(7) Uani 1 2 d S . .
O3 O 0.3333 0.2451(4) 0.4167 0.274(11) Uani 1 2 d S . .
O4 O 0.3647(13) 0.3410(11) 0.3836(14) 0.194(9) Uani 0.50 1 d P . .
O5 O 0.2803(8) 0.2719(11) 0.3921(16) 0.205(9) Uani 0.50 1 d P . .
O6 O 0.3310(13) 0.3050(9) 0.3549(7) 0.145(7) Uani 0.50 1 d P . .
O1W O -0.0034(2) -0.0881(3) 0.1848(3) 0.144(3) Uani 1 1 d . . .
O2W O 0.0000 0.0000 0.1677(9) 0.180(6) 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
C1 0.050(3) 0.071(3) 0.062(3) -0.006(3) -0.002(3) 0.030(3)
C2 0.071(4) 0.078(4) 0.094(5) -0.028(4) -0.014(3) 0.043(3)
C3 0.079(4) 0.078(4) 0.102(6) -0.026(4) -0.005(4) 0.029(4)
C4 0.068(4) 0.091(5) 0.081(5) -0.018(4) -0.022(3) 0.031(4)
C5 0.067(4) 0.087(4) 0.072(4) -0.010(3) -0.014(3) 0.043(3)
C6 0.050(3) 0.060(3) 0.054(3) -0.003(2) -0.004(2) 0.026(2)
C7 0.060(3) 0.086(4) 0.082(4) -0.007(3) -0.013(3) 0.045(3)
C8 0.092(5) 0.108(6) 0.147(7) -0.053(5) -0.050(5) 0.076(5)
C9 0.174(9) 0.145(8) 0.220(12) -0.095(8) -0.123(9) 0.134(8)
C10 0.188(10) 0.152(8) 0.088(6) -0.032(6) -0.025(6) 0.127(8)
C11 0.122(7) 0.062(5) 0.239(13) -0.030(6) -0.026(8) 0.033(5)
C12 0.048(3) 0.041(2) 0.066(3) -0.002(2) 0.004(2) 0.023(2)
Cu1 0.0509(4) 0.0592(4) 0.0631(5) -0.0044(3) -0.0078(3) 0.0346(3)
Fe1 0.0333(5) 0.0333(5) 0.0602(11) 0.000 0.000 0.0167(3)
N1 0.070(3) 0.075(3) 0.086(4) -0.018(3) -0.015(3) 0.050(3)
N2 0.076(3) 0.069(3) 0.111(5) -0.018(3) -0.033(3) 0.048(3)
N3 0.060(3) 0.057(3) 0.070(3) -0.005(2) -0.005(2) 0.032(2)
O1 0.057(2) 0.080(3) 0.090(3) -0.023(2) -0.020(2) 0.044(2)
O2 0.116(5) 0.178(6) 0.108(4) 0.053(4) 0.008(4) 0.067(5)
Cl1 0.1027(19) 0.0780(10) 0.0819(17) -0.0014(7) -0.0028(14) 0.0514(10)
O3 0.54(3) 0.192(8) 0.207(14) -0.079(9) -0.158(17) 0.270(16)
O4 0.22(3) 0.17(2) 0.18(2) 0.078(17) 0.059(18) 0.082(18)
O5 0.128(14) 0.25(2) 0.25(2) -0.08(2) -0.061(17) 0.103(16)
O6 0.24(2) 0.124(13) 0.071(9) 0.019(9) -0.011(11) 0.088(15)
O1W 0.087(4) 0.132(5) 0.146(6) 0.051(4) -0.037(4) 0.006(3)
O2W 0.110(5) 0.110(5) 0.32(2) 0.000 0.000 0.055(3)

_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
C1 O1 1.327(7) . ?
C1 C2 1.397(8) . ?
C1 C6 1.415(8) . ?
C2 C3 1.373(10) . ?
C2 H2 0.9300 . ?
C3 C4 1.377(10) . ?
C3 H3 0.9300 . ?
C4 C5 1.359(9) . ?
C4 H4 0.9300 . ?
C5 C6 1.411(8) . ?
C5 H5 0.9300 . ?
C6 C7 1.417(8) . ?
C7 N1 1.294(8) . ?
C7 H7 0.9300 . ?
C8 C9 1.437(12) . ?
C8 N1 1.468(8) . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C9 N2 1.459(9) . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C10 N2 1.445(10) . ?
C10 H10A 0.9600 . ?
C10 H10B 0.9600 . ?
C10 H10C 0.9600 . ?
C11 N2 1.490(10) . ?
C11 H11A 0.9600 . ?
C11 H11B 0.9600 . ?
C11 H11C 0.9600 . ?
C12 N3 1.161(6) . ?
C12 Fe1 1.893(5) . ?
Cu1 O1 1.910(4) . ?
Cu1 N1 1.919(5) . ?
Cu1 N3 1.932(5) . ?
Cu1 N2 2.088(5) . ?
Cu1 O2 2.395(6) . ?
Fe1 C12 1.893(6) 4 ?
Fe1 C12 1.893(5) 19 ?
Fe1 C12 1.893(5) 2 ?
Fe1 C12 1.893(5) 20 ?
Fe1 C12 1.893(6) 22 ?
Cl1 O3 1.302(10) . ?
Cl1 O6 1.381(14) . ?
Cl1 O6 1.381(14) 11 ?
Cl1 O4 1.394(19) . ?
Cl1 O4 1.395(19) 11 ?
Cl1 O5 1.396(17) 11 ?
Cl1 O5 1.396(17) . ?
O4 O6 1.15(3) . ?
O4 O5 1.53(3) 11 ?
O5 O6 1.48(3) . ?
O5 O4 1.53(3) 11 ?

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 C1 C2 119.5(5) . . ?
O1 C1 C6 123.2(5) . . ?
C2 C1 C6 117.3(5) . . ?
C3 C2 C1 121.7(6) . . ?
C3 C2 H2 119.2 . . ?
C1 C2 H2 119.2 . . ?
C2 C3 C4 120.9(7) . . ?
C2 C3 H3 119.6 . . ?
C4 C3 H3 119.6 . . ?
C5 C4 C3 119.2(6) . . ?
C5 C4 H4 120.4 . . ?
C3 C4 H4 120.4 . . ?
C4 C5 C6 121.6(6) . . ?
C4 C5 H5 119.2 . . ?
C6 C5 H5 119.2 . . ?
C5 C6 C1 119.2(5) . . ?
C5 C6 C7 117.6(5) . . ?
C1 C6 C7 123.2(5) . . ?
N1 C7 C6 125.6(5) . . ?
N1 C7 H7 117.2 . . ?
C6 C7 H7 117.2 . . ?
C9 C8 N1 108.6(6) . . ?
C9 C8 H8A 110.0 . . ?
N1 C8 H8A 110.0 . . ?
C9 C8 H8B 110.0 . . ?
N1 C8 H8B 110.0 . . ?
H8A C8 H8B 108.4 . . ?
C8 C9 N2 113.9(7) . . ?
C8 C9 H9A 108.8 . . ?
N2 C9 H9A 108.8 . . ?
C8 C9 H9B 108.8 . . ?
N2 C9 H9B 108.8 . . ?
H9A C9 H9B 107.7 . . ?
N2 C10 H10A 109.5 . . ?
N2 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
N2 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
N2 C11 H11A 109.5 . . ?
N2 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
N2 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
N3 C12 Fe1 176.1(5) . . ?
O1 Cu1 N1 92.53(18) . . ?
O1 Cu1 N3 90.53(18) . . ?
N1 Cu1 N3 172.7(2) . . ?
O1 Cu1 N2 172.6(2) . . ?
N1 Cu1 N2 84.0(2) . . ?
N3 Cu1 N2 92.16(19) . . ?
O1 Cu1 O2 93.8(2) . . ?
N1 Cu1 O2 95.1(2) . . ?
N3 Cu1 O2 91.2(2) . . ?
N2 Cu1 O2 93.0(3) . . ?
C12 Fe1 C12 87.8(2) 4 19 ?
C12 Fe1 C12 92.2(2) 4 2 ?
C12 Fe1 C12 87.8(2) 19 2 ?
C12 Fe1 C12 92.2(2) 4 . ?
C12 Fe1 C12 180.0(4) 19 . ?
C12 Fe1 C12 92.2(2) 2 . ?
C12 Fe1 C12 87.8(2) 4 20 ?
C12 Fe1 C12 92.2(2) 19 20 ?
C12 Fe1 C12 180.0(4) 2 20 ?
C12 Fe1 C12 87.8(2) . 20 ?
C12 Fe1 C12 180.0(6) 4 22 ?
C12 Fe1 C12 92.2(2) 19 22 ?
C12 Fe1 C12 87.8(2) 2 22 ?
C12 Fe1 C12 87.8(2) . 22 ?
C12 Fe1 C12 92.2(2) 20 22 ?
C7 N1 C8 118.9(5) . . ?
C7 N1 Cu1 126.6(4) . . ?
C8 N1 Cu1 114.5(4) . . ?
C10 N2 C9 114.7(8) . . ?
C10 N2 C11 107.3(8) . . ?
C9 N2 C11 107.6(7) . . ?
C10 N2 Cu1 110.0(5) . . ?
C9 N2 Cu1 104.2(5) . . ?
C11 N2 Cu1 113.2(5) . . ?
C12 N3 Cu1 171.9(5) . . ?
C1 O1 Cu1 127.8(4) . . ?
O3 Cl1 O6 106.8(8) . . ?
O3 Cl1 O6 106.8(8) . 11 ?
O6 Cl1 O6 146.4(15) . 11 ?
O3 Cl1 O4 132.0(10) . . ?
O6 Cl1 O4 49.0(11) . . ?
O6 Cl1 O4 105.6(14) 11 . ?
O3 Cl1 O4 132.0(10) . 11 ?
O6 Cl1 O4 105.6(13) . 11 ?
O6 Cl1 O4 48.9(11) 11 11 ?
O4 Cl1 O4 96(2) . 11 ?
O3 Cl1 O5 97.5(10) . 11 ?
O6 Cl1 O5 111.0(12) . 11 ?
O6 Cl1 O5 64.2(13) 11 11 ?
O4 Cl1 O5 66.7(13) . 11 ?
O4 Cl1 O5 102.7(15) 11 11 ?
O3 Cl1 O5 97.5(10) . . ?
O6 Cl1 O5 64.2(13) . . ?
O6 Cl1 O5 111.0(12) 11 . ?
O4 Cl1 O5 102.7(15) . . ?
O4 Cl1 O5 66.7(13) 11 . ?
O5 Cl1 O5 165(2) 11 . ?
O6 O4 Cl1 64.9(14) . . ?
O6 O4 O5 116(2) . 11 ?
Cl1 O4 O5 56.7(10) . 11 ?
Cl1 O5 O6 57.4(9) . . ?
Cl1 O5 O4 56.6(11) . 11 ?
O6 O5 O4 94.5(15) . 11 ?
O4 O6 Cl1 66.1(13) . . ?
O4 O6 O5 112(2) . . ?
Cl1 O6 O5 58.4(10) . . ?

_diffrn_measured_fraction_theta_max 0.997
_diffrn_reflns_theta_full        25.27
_diffrn_measured_fraction_theta_full 0.997
_refine_diff_density_max         0.526
_refine_diff_density_min         -0.734
_refine_diff_density_rms         0.094


# Attachment 'Crystal3.cif'

data_shelxl_crystal3
_database_code_depnum_ccdc_archive 'CCDC 755666'
#TrackingRef 'Crystal3.cif'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C72 H118 Cl3 Co Cu6 N18 O32'
_chemical_formula_weight         2294.36

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'
Cu Cu 0.3201 1.2651 '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'

_symmetry_cell_setting           Hexagonal
_symmetry_space_group_name_H-M   R-3c

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

_cell_length_a                   27.9545(19)
_cell_length_b                   27.9545(19)
_cell_length_c                   21.3938(16)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_volume                     14478.4(18)
_cell_formula_units_Z            6
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    396
_cell_measurement_theta_min      2.5
_cell_measurement_theta_max      26

_exptl_crystal_description       prism
_exptl_crystal_colour            green
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_density_diffrn    1.579
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             7104
_exptl_absorpt_coefficient_mu    1.634
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.725
_exptl_absorpt_correction_T_max  0.895
_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  'Nonius Kappa CCD'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            25955
_diffrn_reflns_av_R_equivalents  0.1310
_diffrn_reflns_av_sigmaI/netI    0.0903
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         2.93
_diffrn_reflns_theta_max         25.01
_reflns_number_total             2831
_reflns_number_gt                1748
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       KappaCCD
_computing_cell_refinement       'Dirax/lsq (Duisenberg & Schreurs, 1989-2000)'
_computing_data_reduction        'Denzo and Scalepak'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_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^)+(0.0223P)^2^+172.7003P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         2831
_refine_ls_number_parameters     214
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1266
_refine_ls_R_factor_gt           0.0623
_refine_ls_wR_factor_ref         0.1166
_refine_ls_wR_factor_gt          0.0993
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_restrained_S_all      1.056
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.2291(2) 0.1158(3) 0.1848(3) 0.0306(15) Uani 1 1 d . . .
C2 C 0.2361(3) 0.1644(3) 0.2126(3) 0.0480(19) Uani 1 1 d . . .
H2 H 0.2121 0.1770 0.2017 0.058 Uiso 1 1 calc R . .
C3 C 0.2771(3) 0.1940(3) 0.2552(4) 0.055(2) Uani 1 1 d . . .
H3 H 0.2798 0.2256 0.2731 0.066 Uiso 1 1 calc R . .
C4 C 0.3142(3) 0.1779(3) 0.2720(3) 0.054(2) Uani 1 1 d . . .
H4 H 0.3414 0.1975 0.3017 0.064 Uiso 1 1 calc R . .
C5 C 0.3104(3) 0.1322(3) 0.2440(3) 0.049(2) Uani 1 1 d . . .
H5 H 0.3359 0.1213 0.2543 0.058 Uiso 1 1 calc R . .
C6 C 0.2689(2) 0.1011(3) 0.2002(3) 0.0343(16) Uani 1 1 d . . .
C7 C 0.2700(2) 0.0553(3) 0.1715(3) 0.0379(17) Uani 1 1 d . . .
H7 H 0.2994 0.0500 0.1816 0.046 Uiso 1 1 calc R . .
C8 C 0.2430(3) -0.0210(3) 0.1035(4) 0.069(3) Uani 1 1 d . . .
H8A H 0.2628 -0.0320 0.1319 0.083 Uiso 1 1 calc R . .
H8B H 0.2650 -0.0062 0.0660 0.083 Uiso 1 1 calc R . .
C9 C 0.1894(4) -0.0687(3) 0.0878(4) 0.076(3) Uani 1 1 d . . .
H9A H 0.1728 -0.0900 0.1254 0.091 Uiso 1 1 calc R . .
H9B H 0.1949 -0.0922 0.0588 0.091 Uiso 1 1 calc R . .
C10 C 0.1643(4) -0.0377(4) -0.0064(4) 0.074(3) Uani 1 1 d . . .
H10A H 0.1394 -0.0267 -0.0230 0.111 Uiso 1 1 calc R . .
H10B H 0.1605 -0.0690 -0.0293 0.111 Uiso 1 1 calc R . .
H10C H 0.2016 -0.0077 -0.0100 0.111 Uiso 1 1 calc R . .
C11 C 0.0950(3) -0.1001(3) 0.0622(4) 0.075(3) Uani 1 1 d . . .
H11A H 0.0853 -0.1114 0.1049 0.112 Uiso 1 1 calc R . .
H11B H 0.0933 -0.1301 0.0385 0.112 Uiso 1 1 calc R . .
H11C H 0.0697 -0.0899 0.0450 0.112 Uiso 1 1 calc R . .
C12 C 0.0605(2) 0.0093(2) 0.0486(3) 0.0201(13) Uani 1 1 d . . .
Co1 Co 0.0000 0.0000 0.0000 0.0158(4) Uani 1 6 d S . .
Cu1 Cu 0.16504(3) 0.01677(3) 0.11021(3) 0.0274(2) Uani 1 1 d . . .
N1 N 0.2339(2) 0.0208(2) 0.1328(3) 0.0379(14) Uani 1 1 d . . .
N2 N 0.1514(2) -0.0526(2) 0.0596(3) 0.0392(14) Uani 1 1 d . . .
N3 N 0.0990(2) 0.01412(19) 0.0739(2) 0.0279(12) Uani 1 1 d . . .
O1 O 0.18755(16) 0.08801(17) 0.1461(2) 0.0374(11) Uani 1 1 d . . .
O2 O 0.11483(19) -0.0375(2) 0.1966(2) 0.0568(14) Uani 1 1 d . . .
Cl1 Cl 0.3333 0.29258(10) 0.4167 0.0592(8) Uani 1 2 d S . .
O3 O 0.3333 0.2475(4) 0.4167 0.294(13) Uani 1 2 d S . .
O4 O 0.3649(11) 0.3439(9) 0.3841(11) 0.153(8) Uani 0.50 1 d P . .
O5 O 0.2795(7) 0.2689(10) 0.3924(13) 0.187(10) Uani 0.50 1 d P . .
O6 O 0.3344(10) 0.3056(7) 0.3556(7) 0.110(7) Uani 0.50 1 d P . .
O1W O 0.00020(17) -0.09881(17) 0.1843(2) 0.0463(12) Uani 1 1 d . . .
O2W O 0.0000 0.0000 0.1861(3) 0.043(2) 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
C1 0.021(3) 0.034(4) 0.030(3) 0.000(3) 0.002(3) 0.008(3)
C2 0.039(4) 0.043(4) 0.062(5) -0.018(4) -0.009(4) 0.021(4)
C3 0.045(5) 0.039(4) 0.072(6) -0.024(4) -0.010(4) 0.014(4)
C4 0.048(5) 0.053(5) 0.044(5) -0.019(4) -0.015(4) 0.013(4)
C5 0.038(4) 0.062(5) 0.040(4) 0.001(4) -0.012(3) 0.021(4)
C6 0.028(4) 0.037(4) 0.033(4) 0.000(3) -0.002(3) 0.013(3)
C7 0.026(4) 0.045(4) 0.048(4) 0.000(3) -0.009(3) 0.021(3)
C8 0.054(5) 0.074(6) 0.110(7) -0.041(5) -0.040(5) 0.056(5)
C9 0.087(7) 0.078(6) 0.104(7) -0.034(6) -0.047(6) 0.072(6)
C10 0.114(7) 0.094(7) 0.052(5) -0.027(5) -0.009(5) 0.081(6)
C11 0.067(6) 0.046(5) 0.111(7) -0.019(5) -0.014(5) 0.028(5)
C12 0.026(3) 0.012(3) 0.019(3) 0.000(2) 0.003(3) 0.006(3)
Co1 0.0153(6) 0.0153(6) 0.0166(9) 0.000 0.000 0.0077(3)
Cu1 0.0251(4) 0.0332(5) 0.0300(4) -0.0048(4) -0.0064(4) 0.0191(4)
N1 0.031(3) 0.040(3) 0.052(4) -0.013(3) -0.010(3) 0.025(3)
N2 0.039(3) 0.038(3) 0.049(4) -0.013(3) -0.016(3) 0.025(3)
N3 0.026(3) 0.033(3) 0.028(3) -0.004(2) -0.004(2) 0.017(3)
O1 0.030(2) 0.039(3) 0.049(3) -0.015(2) -0.013(2) 0.021(2)
O2 0.048(3) 0.076(4) 0.038(3) 0.014(3) 0.003(2) 0.025(3)
Cl1 0.077(2) 0.0580(14) 0.0489(18) 0.0010(8) 0.0020(17) 0.0386(12)
O3 0.63(4) 0.198(10) 0.195(16) -0.104(10) -0.21(2) 0.32(2)
O4 0.21(2) 0.107(15) 0.139(19) 0.072(14) 0.087(17) 0.079(17)
O5 0.081(13) 0.23(2) 0.22(2) -0.10(2) -0.046(15) 0.058(15)
O6 0.20(2) 0.069(10) 0.051(9) 0.023(8) 0.013(11) 0.062(13)
O1W 0.036(3) 0.039(3) 0.054(3) -0.002(2) -0.006(2) 0.011(2)
O2W 0.047(3) 0.047(3) 0.036(4) 0.000 0.000 0.0235(15)

_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
C1 O1 1.318(7) . ?
C1 C2 1.404(9) . ?
C1 C6 1.404(8) . ?
C2 C3 1.372(9) . ?
C2 H2 0.9300 . ?
C3 C4 1.370(10) . ?
C3 H3 0.9300 . ?
C4 C5 1.365(9) . ?
C4 H4 0.9300 . ?
C5 C6 1.403(9) . ?
C5 H5 0.9300 . ?
C6 C7 1.436(8) . ?
C7 N1 1.287(7) . ?
C7 H7 0.9300 . ?
C8 N1 1.456(8) . ?
C8 C9 1.463(10) . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C9 N2 1.475(8) . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C10 N2 1.464(9) . ?
C10 H10A 0.9600 . ?
C10 H10B 0.9600 . ?
C10 H10C 0.9600 . ?
C11 N2 1.469(9) . ?
C11 H11A 0.9600 . ?
C11 H11B 0.9600 . ?
C11 H11C 0.9600 . ?
C12 N3 1.153(6) . ?
C12 Co1 1.888(6) . ?
Co1 C12 1.888(6) 19 ?
Co1 C12 1.888(6) 2 ?
Co1 C12 1.888(6) 22 ?
Co1 C12 1.888(6) 20 ?
Co1 C12 1.888(6) 4 ?
Cu1 O1 1.923(4) . ?
Cu1 N1 1.934(5) . ?
Cu1 N3 1.968(5) . ?
Cu1 N2 2.083(5) . ?
Cu1 O2 2.357(4) . ?
Cl1 O3 1.261(12) . ?
Cl1 O6 1.353(14) . ?
Cl1 O6 1.353(14) 11 ?
Cl1 O5 1.406(17) 11 ?
Cl1 O5 1.407(17) . ?
Cl1 O4 1.435(16) . ?
Cl1 O4 1.435(16) 11 ?
O4 O6 1.16(2) . ?
O4 O5 1.61(3) 11 ?
O5 O6 1.57(2) . ?
O5 O4 1.61(3) 11 ?

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 C1 C2 119.5(6) . . ?
O1 C1 C6 124.7(6) . . ?
C2 C1 C6 115.8(6) . . ?
C3 C2 C1 122.4(7) . . ?
C3 C2 H2 118.8 . . ?
C1 C2 H2 118.8 . . ?
C4 C3 C2 121.1(7) . . ?
C4 C3 H3 119.4 . . ?
C2 C3 H3 119.4 . . ?
C5 C4 C3 118.4(7) . . ?
C5 C4 H4 120.8 . . ?
C3 C4 H4 120.8 . . ?
C4 C5 C6 121.7(7) . . ?
C4 C5 H5 119.2 . . ?
C6 C5 H5 119.2 . . ?
C5 C6 C1 120.5(6) . . ?
C5 C6 C7 117.3(6) . . ?
C1 C6 C7 122.2(6) . . ?
N1 C7 C6 125.8(6) . . ?
N1 C7 H7 117.1 . . ?
C6 C7 H7 117.1 . . ?
N1 C8 C9 108.7(6) . . ?
N1 C8 H8A 110.0 . . ?
C9 C8 H8A 110.0 . . ?
N1 C8 H8B 110.0 . . ?
C9 C8 H8B 110.0 . . ?
H8A C8 H8B 108.3 . . ?
C8 C9 N2 112.4(6) . . ?
C8 C9 H9A 109.1 . . ?
N2 C9 H9A 109.1 . . ?
C8 C9 H9B 109.1 . . ?
N2 C9 H9B 109.1 . . ?
H9A C9 H9B 107.8 . . ?
N2 C10 H10A 109.5 . . ?
N2 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
N2 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
N2 C11 H11A 109.5 . . ?
N2 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
N2 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
N3 C12 Co1 174.4(5) . . ?
C12 Co1 C12 180.0(4) 19 . ?
C12 Co1 C12 87.4(2) 19 2 ?
C12 Co1 C12 92.6(2) . 2 ?
C12 Co1 C12 92.6(2) 19 22 ?
C12 Co1 C12 87.4(2) . 22 ?
C12 Co1 C12 87.4(2) 2 22 ?
C12 Co1 C12 92.6(2) 19 20 ?
C12 Co1 C12 87.4(2) . 20 ?
C12 Co1 C12 180.0(4) 2 20 ?
C12 Co1 C12 92.6(2) 22 20 ?
C12 Co1 C12 87.4(2) 19 4 ?
C12 Co1 C12 92.6(2) . 4 ?
C12 Co1 C12 92.6(2) 2 4 ?
C12 Co1 C12 180.0(7) 22 4 ?
C12 Co1 C12 87.4(2) 20 4 ?
O1 Cu1 N1 92.24(19) . . ?
O1 Cu1 N3 90.67(18) . . ?
N1 Cu1 N3 171.2(2) . . ?
O1 Cu1 N2 169.9(2) . . ?
N1 Cu1 N2 84.1(2) . . ?
N3 Cu1 N2 91.62(19) . . ?
O1 Cu1 O2 97.77(18) . . ?
N1 Cu1 O2 95.5(2) . . ?
N3 Cu1 O2 92.29(18) . . ?
N2 Cu1 O2 92.0(2) . . ?
C7 N1 C8 119.4(5) . . ?
C7 N1 Cu1 126.1(4) . . ?
C8 N1 Cu1 114.5(4) . . ?
C10 N2 C11 107.1(6) . . ?
C10 N2 C9 111.6(6) . . ?
C11 N2 C9 108.6(6) . . ?
C10 N2 Cu1 109.4(4) . . ?
C11 N2 Cu1 115.9(4) . . ?
C9 N2 Cu1 104.3(4) . . ?
C12 N3 Cu1 173.7(5) . . ?
C1 O1 Cu1 126.7(4) . . ?
O3 Cl1 O6 105.0(7) . . ?
O3 Cl1 O6 105.0(7) . 11 ?
O6 Cl1 O6 150.0(14) . 11 ?
O3 Cl1 O5 93.7(10) . 11 ?
O6 Cl1 O5 108.8(11) . 11 ?
O6 Cl1 O5 69.1(12) 11 11 ?
O3 Cl1 O5 93.7(10) . . ?
O6 Cl1 O5 69.1(12) . . ?
O6 Cl1 O5 108.8(11) 11 . ?
O5 Cl1 O5 173(2) 11 . ?
O3 Cl1 O4 133.9(8) . . ?
O6 Cl1 O4 48.9(9) . . ?
O6 Cl1 O4 107.4(13) 11 . ?
O5 Cl1 O4 68.9(12) 11 . ?
O5 Cl1 O4 105.6(15) . . ?
O3 Cl1 O4 133.9(8) . 11 ?
O6 Cl1 O4 107.4(13) . 11 ?
O6 Cl1 O4 48.9(9) 11 11 ?
O5 Cl1 O4 105.6(15) 11 11 ?
O5 Cl1 O4 68.9(12) . 11 ?
O4 Cl1 O4 92.2(16) . 11 ?
O6 O4 Cl1 61.9(11) . . ?
O6 O4 O5 107.5(18) . 11 ?
Cl1 O4 O5 54.7(9) . 11 ?
Cl1 O5 O6 53.8(8) . . ?
Cl1 O5 O4 56.4(10) . 11 ?
O6 O5 O4 90.1(13) . 11 ?
O4 O6 Cl1 69.3(12) . . ?
O4 O6 O5 111.7(18) . . ?
Cl1 O6 O5 57.0(10) . . ?

_diffrn_measured_fraction_theta_max 0.996
_diffrn_reflns_theta_full        25.01
_diffrn_measured_fraction_theta_full 0.996
_refine_diff_density_max         0.733
_refine_diff_density_min         -0.520
_refine_diff_density_rms         0.103

# Attachment 'Crystal4.cif'

data_shelxl_crystal4
_database_code_depnum_ccdc_archive 'CCDC 755667'
#TrackingRef 'Crystal4.cif'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C72 H118 Cl3 Cr Cu6 N18 O32'
_chemical_formula_weight         2287.43

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'
Cr Cr 0.3209 0.6236 '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'
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'

_symmetry_cell_setting           Hexagonal
_symmetry_space_group_name_H-M   R-3c

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

_cell_length_a                   28.100(2)
_cell_length_b                   28.100(2)
_cell_length_c                   21.656(2)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_volume                     14809(2)
_cell_formula_units_Z            6
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    500
_cell_measurement_theta_min      2.5
_cell_measurement_theta_max      26

_exptl_crystal_description       prism
_exptl_crystal_colour            green
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.05
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_density_diffrn    1.539
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             7086
_exptl_absorpt_coefficient_mu    1.539
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.7431
_exptl_absorpt_correction_T_max  0.8180
_exptl_absorpt_process_details   wingx

_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  'Nonius Kappa CCD'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            15650
_diffrn_reflns_av_R_equivalents  0.1606
_diffrn_reflns_av_sigmaI/netI    0.1708
_diffrn_reflns_limit_h_min       -35
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_k_max       35
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_theta_min         11.61
_diffrn_reflns_theta_max         27.00
_reflns_number_total             3265
_reflns_number_gt                1676
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       KappaCCD
_computing_cell_refinement       'Dirax/lsq (Duisenberg & Schreurs, 1989-2000)'
_computing_data_reduction        'Denzo and Scalepak'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_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^)+(0.0372P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         3265
_refine_ls_number_parameters     214
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1529
_refine_ls_R_factor_gt           0.0568
_refine_ls_wR_factor_ref         0.1097
_refine_ls_wR_factor_gt          0.0880
_refine_ls_goodness_of_fit_ref   0.981
_refine_ls_restrained_S_all      0.981
_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
C1 C 0.23246(18) 0.1176(2) 0.18837(18) 0.0379(11) Uani 1 1 d . . .
C2 C 0.2380(2) 0.1646(2) 0.2165(3) 0.0592(14) Uani 1 1 d . . .
H2 H 0.2134 0.1763 0.2064 0.071 Uiso 1 1 calc R . .
C3 C 0.2785(3) 0.1941(2) 0.2586(3) 0.0639(16) Uani 1 1 d . . .
H3 H 0.2803 0.2248 0.2772 0.077 Uiso 1 1 calc R . .
C4 C 0.3164(3) 0.1789(3) 0.2738(2) 0.0643(16) Uani 1 1 d . . .
H4 H 0.3436 0.1987 0.3029 0.077 Uiso 1 1 calc R . .
C5 C 0.3137(2) 0.1346(3) 0.2457(2) 0.0552(14) Uani 1 1 d . . .
H5 H 0.3403 0.1251 0.2547 0.066 Uiso 1 1 calc R . .
C6 C 0.27134(19) 0.1022(2) 0.20283(17) 0.0384(11) Uani 1 1 d . . .
C7 C 0.2733(2) 0.0577(2) 0.1741(2) 0.0468(12) Uani 1 1 d . . .
H7 H 0.3032 0.0533 0.1836 0.056 Uiso 1 1 calc R . .
C8 C 0.2472(3) -0.0176(3) 0.1062(4) 0.080(2) Uani 1 1 d . . .
H8A H 0.2700 -0.0017 0.0700 0.095 Uiso 1 1 calc R . .
H8B H 0.2661 -0.0295 0.1342 0.095 Uiso 1 1 calc R . .
C9 C 0.1948(4) -0.0640(3) 0.0884(4) 0.092(2) Uani 1 1 d . . .
H9A H 0.1778 -0.0867 0.1245 0.110 Uiso 1 1 calc R . .
H9B H 0.2013 -0.0860 0.0587 0.110 Uiso 1 1 calc R . .
C10 C 0.1689(4) -0.0325(4) -0.0039(3) 0.087(2) Uani 1 1 d . . .
H10A H 0.1436 -0.0218 -0.0192 0.130 Uiso 1 1 calc R . .
H10B H 0.1653 -0.0630 -0.0275 0.130 Uiso 1 1 calc R . .
H10C H 0.2058 -0.0022 -0.0074 0.130 Uiso 1 1 calc R . .
C11 C 0.0997(3) -0.0966(3) 0.0644(4) 0.088(2) Uani 1 1 d . . .
H11A H 0.0901 -0.1077 0.1066 0.132 Uiso 1 1 calc R . .
H11B H 0.0977 -0.1265 0.0410 0.132 Uiso 1 1 calc R . .
H11C H 0.0745 -0.0863 0.0475 0.132 Uiso 1 1 calc R . .
C12 C 0.06592(17) 0.01217(16) 0.05168(15) 0.0228(8) Uani 1 1 d . . .
Cr1 Cr 0.0000 0.0000 0.0000 0.0187(3) Uani 1 6 d S . .
Cu1 Cu 0.16938(2) 0.01941(2) 0.11313(2) 0.0317(2) Uani 1 1 d . . .
N1 N 0.23789(17) 0.02324(18) 0.13642(17) 0.0453(10) Uani 1 1 d . . .
N2 N 0.15664(18) -0.04870(18) 0.06141(18) 0.0463(10) Uani 1 1 d . . .
N3 N 0.10480(16) 0.01755(15) 0.07602(15) 0.0362(8) Uani 1 1 d . . .
O1 O 0.19056(13) 0.08953(14) 0.15035(13) 0.0458(8) Uani 1 1 d . . .
O2 O 0.11607(16) -0.0367(2) 0.19688(14) 0.0707(11) Uani 1 1 d . . .
Cl1 Cl 0.3333 0.29190(9) 0.4167 0.0621(6) Uani 1 2 d S . .
O3 O 0.3333 0.2453(5) 0.4167 0.282(17) Uani 1 2 d S . .
O4 O 0.3630(15) 0.3402(14) 0.3834(15) 0.160(8) Uani 0.50 1 d P . .
O5 O 0.2822(9) 0.2743(10) 0.3858(11) 0.151(7) Uani 0.50 1 d P . .
O6 O 0.3339(10) 0.3052(8) 0.3570(5) 0.102(5) Uani 0.50 1 d P . .
O1W O 0.00020(14) -0.09903(14) 0.18468(15) 0.0545(9) Uani 1 1 d . . .
O2W O 0.0000 0.0000 0.1867(2) 0.0506(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
C1 0.028(3) 0.044(3) 0.038(2) -0.0096(19) -0.0022(18) 0.016(2)
C2 0.047(3) 0.054(3) 0.077(3) -0.024(3) -0.007(3) 0.026(3)
C3 0.058(4) 0.059(4) 0.072(3) -0.033(3) -0.012(3) 0.026(3)
C4 0.056(4) 0.059(4) 0.060(3) -0.021(3) -0.013(3) 0.015(3)
C5 0.041(3) 0.068(4) 0.052(3) -0.007(3) -0.015(2) 0.024(3)
C6 0.029(3) 0.046(3) 0.035(2) 0.0023(19) 0.0019(18) 0.015(2)
C7 0.033(3) 0.064(3) 0.055(3) -0.011(2) -0.016(2) 0.033(3)
C8 0.066(4) 0.096(5) 0.113(5) -0.049(4) -0.043(4) 0.068(4)
C9 0.094(6) 0.076(5) 0.137(6) -0.052(4) -0.063(5) 0.066(5)
C10 0.138(7) 0.104(5) 0.057(3) -0.024(3) -0.001(4) 0.089(5)
C11 0.079(5) 0.046(4) 0.129(5) -0.019(4) -0.012(4) 0.023(4)
C12 0.025(2) 0.024(2) 0.0230(16) -0.0014(15) -0.0016(16) 0.0147(19)
Cr1 0.0179(5) 0.0179(5) 0.0202(6) 0.000 0.000 0.0090(3)
Cu1 0.0280(3) 0.0385(4) 0.0356(3) -0.0061(2) -0.0073(2) 0.0218(3)
N1 0.037(2) 0.055(3) 0.057(2) -0.016(2) -0.0137(18) 0.033(2)
N2 0.047(3) 0.045(3) 0.062(2) -0.0159(18) -0.0202(19) 0.034(2)
N3 0.036(2) 0.038(2) 0.0398(17) -0.0058(15) -0.0030(17) 0.0219(19)
O1 0.0343(18) 0.050(2) 0.0617(17) -0.0208(15) -0.0158(15) 0.0271(17)
O2 0.054(2) 0.105(3) 0.0446(16) 0.0167(18) 0.0052(15) 0.034(2)
Cl1 0.0817(17) 0.0605(11) 0.0512(11) 0.0017(5) 0.0034(11) 0.0409(9)
O3 0.61(5) 0.212(13) 0.161(10) -0.083(9) -0.166(19) 0.30(3)
O4 0.21(2) 0.139(19) 0.165(16) 0.057(16) 0.065(19) 0.116(19)
O5 0.131(16) 0.164(15) 0.174(14) -0.036(14) -0.066(14) 0.086(14)
O6 0.165(16) 0.072(9) 0.068(7) 0.014(6) 0.000(8) 0.058(10)
O1W 0.047(2) 0.046(2) 0.0608(18) 0.0008(15) -0.0078(15) 0.0153(17)
O2W 0.054(2) 0.054(2) 0.044(3) 0.000 0.000 0.0270(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
C1 O1 1.326(5) . ?
C1 C2 1.391(7) . ?
C1 C6 1.398(7) . ?
C2 C3 1.367(8) . ?
C2 H2 0.9300 . ?
C3 C4 1.372(10) . ?
C3 H3 0.9300 . ?
C4 C5 1.352(9) . ?
C4 H4 0.9300 . ?
C5 C6 1.424(7) . ?
C5 H5 0.9300 . ?
C6 C7 1.422(7) . ?
C7 N1 1.276(6) . ?
C7 H7 0.9300 . ?
C8 C9 1.449(11) . ?
C8 N1 1.452(8) . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C9 N2 1.464(8) . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C10 N2 1.472(8) . ?
C10 H10A 0.9600 . ?
C10 H10B 0.9600 . ?
C10 H10C 0.9600 . ?
C11 N2 1.491(10) . ?
C11 H11A 0.9600 . ?
C11 H11B 0.9600 . ?
C11 H11C 0.9600 . ?
C12 N3 1.153(5) . ?
C12 Cr1 2.042(4) . ?
Cr1 C12 2.042(4) 2 ?
Cr1 C12 2.042(4) 4 ?
Cr1 C12 2.042(4) 20 ?
Cr1 C12 2.042(4) 22 ?
Cr1 C12 2.042(4) 19 ?
Cu1 O1 1.927(3) . ?
Cu1 N1 1.940(4) . ?
Cu1 N3 1.961(4) . ?
Cu1 N2 2.088(4) . ?
Cu1 O2 2.379(3) . ?
Cl1 O3 1.310(14) . ?
Cl1 O6 1.344(10) . ?
Cl1 O6 1.344(10) 11 ?
Cl1 O4 1.39(2) . ?
Cl1 O4 1.39(2) 11 ?
Cl1 O5 1.431(16) 11 ?
Cl1 O5 1.431(16) . ?
O4 O6 1.08(3) . ?
O4 O5 1.65(4) 11 ?
O5 O6 1.41(3) . ?
O5 O4 1.65(4) 11 ?

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 C1 C2 118.8(4) . . ?
O1 C1 C6 123.7(4) . . ?
C2 C1 C6 117.5(4) . . ?
C3 C2 C1 122.2(6) . . ?
C3 C2 H2 118.9 . . ?
C1 C2 H2 118.9 . . ?
C2 C3 C4 120.8(5) . . ?
C2 C3 H3 119.6 . . ?
C4 C3 H3 119.6 . . ?
C5 C4 C3 119.0(5) . . ?
C5 C4 H4 120.5 . . ?
C3 C4 H4 120.5 . . ?
C4 C5 C6 121.8(5) . . ?
C4 C5 H5 119.1 . . ?
C6 C5 H5 119.1 . . ?
C1 C6 C7 123.7(4) . . ?
C1 C6 C5 118.7(5) . . ?
C7 C6 C5 117.4(4) . . ?
N1 C7 C6 126.0(4) . . ?
N1 C7 H7 117.0 . . ?
C6 C7 H7 117.0 . . ?
C9 C8 N1 109.2(5) . . ?
C9 C8 H8A 109.8 . . ?
N1 C8 H8A 109.8 . . ?
C9 C8 H8B 109.8 . . ?
N1 C8 H8B 109.8 . . ?
H8A C8 H8B 108.3 . . ?
C8 C9 N2 113.9(6) . . ?
C8 C9 H9A 108.8 . . ?
N2 C9 H9A 108.8 . . ?
C8 C9 H9B 108.8 . . ?
N2 C9 H9B 108.8 . . ?
H9A C9 H9B 107.7 . . ?
N2 C10 H10A 109.5 . . ?
N2 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
N2 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
N2 C11 H11A 109.5 . . ?
N2 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
N2 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
N3 C12 Cr1 173.5(3) . . ?
C12 Cr1 C12 92.82(13) 2 4 ?
C12 Cr1 C12 92.82(13) 2 . ?
C12 Cr1 C12 92.82(13) 4 . ?
C12 Cr1 C12 180.0(3) 2 20 ?
C12 Cr1 C12 87.18(13) 4 20 ?
C12 Cr1 C12 87.18(13) . 20 ?
C12 Cr1 C12 87.18(13) 2 22 ?
C12 Cr1 C12 180.0(5) 4 22 ?
C12 Cr1 C12 87.18(13) . 22 ?
C12 Cr1 C12 92.82(13) 20 22 ?
C12 Cr1 C12 87.18(13) 2 19 ?
C12 Cr1 C12 87.18(13) 4 19 ?
C12 Cr1 C12 180.0(3) . 19 ?
C12 Cr1 C12 92.82(13) 20 19 ?
C12 Cr1 C12 92.82(13) 22 19 ?
O1 Cu1 N1 92.51(15) . . ?
O1 Cu1 N3 90.42(14) . . ?
N1 Cu1 N3 170.79(15) . . ?
O1 Cu1 N2 170.15(16) . . ?
N1 Cu1 N2 84.32(16) . . ?
N3 Cu1 N2 91.34(15) . . ?
O1 Cu1 O2 97.41(15) . . ?
N1 Cu1 O2 96.72(16) . . ?
N3 Cu1 O2 91.55(14) . . ?
N2 Cu1 O2 92.23(17) . . ?
C7 N1 C8 120.4(4) . . ?
C7 N1 Cu1 125.8(3) . . ?
C8 N1 Cu1 113.9(3) . . ?
C9 N2 C10 112.4(6) . . ?
C9 N2 C11 109.4(6) . . ?
C10 N2 C11 107.4(5) . . ?
C9 N2 Cu1 103.9(3) . . ?
C10 N2 Cu1 109.0(4) . . ?
C11 N2 Cu1 114.7(4) . . ?
C12 N3 Cu1 173.9(3) . . ?
C1 O1 Cu1 126.6(3) . . ?
O3 Cl1 O6 105.9(7) . . ?
O3 Cl1 O6 105.9(7) . 11 ?
O6 Cl1 O6 148.3(15) . 11 ?
O3 Cl1 O4 132.7(10) . . ?
O6 Cl1 O4 46.4(13) . . ?
O6 Cl1 O4 108.6(19) 11 . ?
O3 Cl1 O4 132.7(10) . 11 ?
O6 Cl1 O4 108.6(19) . 11 ?
O6 Cl1 O4 46.4(14) 11 11 ?
O4 Cl1 O4 94.6(19) . 11 ?
O3 Cl1 O5 99.0(9) . 11 ?
O6 Cl1 O5 113.5(13) . 11 ?
O6 Cl1 O5 61.0(12) 11 11 ?
O4 Cl1 O5 72(2) . 11 ?
O4 Cl1 O5 96(2) 11 11 ?
O3 Cl1 O5 99.0(9) . . ?
O6 Cl1 O5 61.0(12) . . ?
O6 Cl1 O5 113.5(12) 11 . ?
O4 Cl1 O5 96(2) . . ?
O4 Cl1 O5 72(2) 11 . ?
O5 Cl1 O5 162.0(17) 11 . ?
O6 O4 Cl1 64.7(17) . . ?
O6 O4 O5 115.2(18) . 11 ?
Cl1 O4 O5 55.4(11) . 11 ?
O6 O5 Cl1 56.4(9) . . ?
O6 O5 O4 92.6(14) . 11 ?
Cl1 O5 O4 53.0(15) . 11 ?
O4 O6 Cl1 69.0(12) . . ?
O4 O6 O5 114.0(18) . . ?
Cl1 O6 O5 62.5(9) . . ?

_diffrn_measured_fraction_theta_max 0.906
_diffrn_reflns_theta_full        27.00
_diffrn_measured_fraction_theta_full 0.906
_refine_diff_density_max         0.435
_refine_diff_density_min         -0.522
_refine_diff_density_rms         0.079