# 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_volume                  ?
_journal_page_first              ?
_journal_year                    ?

_publ_contact_author_name        'Changwen Hu'
_publ_contact_author_email       CWHU@BIT.EDU.CN

_publ_section_title              
;
Transformation from [W6O19]2-
to [W6O22]8- Stabilized by Cu(II) Complexation
;
loop_
_publ_author_name
'Changwen Hu.'
'Ying Nan Chi.'
'Fengyun Cui.'
'Yuan-Ge Gao.'
;
Zhan-Gang Han
;
'Kun-Lin Huang.'
'Cong Li.'
'Xiao-Yu Ma.'

# Attachment 'compound1and2.cif'

data_compound1
_database_code_depnum_ccdc_archive 'CCDC 753690'
#TrackingRef 'compound1and2.cif'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C14 H15 Cu2 N5 O13 W3'
_chemical_formula_weight         1139.94

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'
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
W W -0.8490 6.8722 '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

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

_cell_length_a                   10.5450(17)
_cell_length_b                   10.8584(18)
_cell_length_c                   11.0244(19)
_cell_angle_alpha                83.531(2)
_cell_angle_beta                 70.2400(10)
_cell_angle_gamma                66.5540(10)
_cell_volume                     1089.6(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    298(2)
_cell_measurement_reflns_used    3054
_cell_measurement_theta_min      2.225
_cell_measurement_theta_max      27.926

_exptl_crystal_description       block
_exptl_crystal_colour            green
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    3.475
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1036
_exptl_absorpt_coefficient_mu    17.778
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.2242
_exptl_absorpt_correction_T_max  0.2694
_exptl_absorpt_process_details   sadabs

_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  'CCD area detector'
_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            5535
_diffrn_reflns_av_R_equivalents  0.0331
_diffrn_reflns_av_sigmaI/netI    0.0665
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_theta_min         1.96
_diffrn_reflns_theta_max         25.01
_reflns_number_total             3744
_reflns_number_gt                2931
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

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

_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^)+(0.0522P)^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         3744
_refine_ls_number_parameters     334
_refine_ls_number_restraints     24
_refine_ls_R_factor_all          0.0567
_refine_ls_R_factor_gt           0.0388
_refine_ls_wR_factor_ref         0.1006
_refine_ls_wR_factor_gt          0.0907
_refine_ls_goodness_of_fit_ref   1.002
_refine_ls_restrained_S_all      1.001
_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
W1 W -0.11235(5) 0.75466(5) 0.51990(5) 0.01541(15) Uani 1 1 d . . .
W2 W -0.28987(5) 1.06496(5) 0.64353(5) 0.01484(15) Uani 1 1 d . . .
W3 W -0.05270(5) 1.09160(5) 0.37521(5) 0.01382(15) Uani 1 1 d . . .
Cu2 Cu 0.23661(17) 0.53462(15) 0.33536(15) 0.0217(4) Uani 1 1 d . . .
Cu1 Cu -0.35092(17) 0.98280(15) 0.37057(15) 0.0194(4) Uani 1 1 d . . .
N1 N 0.4154(11) 0.3762(10) 0.2563(10) 0.019(2) Uani 1 1 d . . .
N2 N 0.5606(11) 0.1474(10) 0.2781(10) 0.017(2) Uani 1 1 d . . .
N3 N 0.4871(10) 0.3064(9) 0.4307(9) 0.012(2) Uani 1 1 d U . .
H3A H 0.4422 0.3877 0.4607 0.014 Uiso 1 1 calc R . .
H3B H 0.5325 0.2442 0.4741 0.014 Uiso 1 1 calc R . .
N4 N 0.2522(11) 0.5664(10) 0.1495(11) 0.022(3) Uani 1 1 d U . .
N5 N 0.7099(11) -0.1005(11) 0.2008(10) 0.023(3) Uani 1 1 d . . .
O1 O -0.0845(9) 0.9444(7) 0.4853(8) 0.0145(18) Uani 1 1 d . . .
O2 O -0.2774(9) 0.8935(8) 0.6700(8) 0.019(2) Uani 1 1 d . . .
O3 O 0.0553(10) 0.6792(8) 0.3951(9) 0.024(2) Uani 1 1 d . . .
O4 O -0.2386(9) 0.8180(8) 0.4346(8) 0.018(2) Uani 1 1 d . . .
O5 O -0.1428(9) 0.6168(8) 0.5989(9) 0.023(2) Uani 1 1 d . . .
O6 O -0.2272(8) 1.1863(7) 0.5225(8) 0.0137(18) Uani 1 1 d . . .
O7 O -0.4164(9) 1.0775(8) 0.5345(8) 0.0170(19) Uani 1 1 d . . .
O8 O -0.1355(9) 1.0330(8) 0.7122(8) 0.0178(19) Uani 1 1 d . . .
O9 O -0.4285(9) 1.1626(9) 0.7687(9) 0.026(2) Uani 1 1 d . . .
O10 O -0.1362(9) 1.1084(8) 0.2627(9) 0.022(2) Uani 1 1 d U . .
O11 O -0.0008(8) 1.2345(8) 0.3580(8) 0.0134(18) Uani 1 1 d U . .
O12 O 0.2881(12) 0.5471(10) 0.4904(11) 0.044(3) Uani 1 1 d . . .
H12B H 0.2078 0.5689 0.5521 0.053 Uiso 1 1 d R . .
H12C H 0.3113 0.6151 0.4788 0.053 Uiso 1 1 d R . .
O13 O 0.9608(17) 0.4799(13) 0.2239(15) 0.086(5) Uani 1 1 d . . .
H13C H 1.0157 0.4852 0.2628 0.103 Uiso 1 1 d R . .
H13D H 0.9478 0.4071 0.2456 0.103 Uiso 1 1 d R . .
C1 C 0.4864(13) 0.2794(12) 0.3263(12) 0.019(3) Uani 1 1 d . . .
C2 C 0.5771(13) 0.1226(12) 0.1559(11) 0.017(3) Uani 1 1 d . . .
C3 C 0.5157(14) 0.2243(13) 0.0789(13) 0.024(3) Uani 1 1 d . . .
H3 H 0.5339 0.2077 -0.0076 0.028 Uiso 1 1 calc R . .
C4 C 0.4293(14) 0.3473(13) 0.1335(12) 0.025(3) Uani 1 1 d . . .
C5 C 0.3458(12) 0.4606(13) 0.0718(12) 0.019(3) Uani 1 1 d . . .
C6 C 0.3620(16) 0.4626(14) -0.0567(13) 0.030(4) Uani 1 1 d . . .
H6 H 0.4273 0.3882 -0.1102 0.036 Uiso 1 1 calc R . .
C7 C 0.2779(16) 0.5793(16) -0.1060(15) 0.037(4) Uani 1 1 d . . .
H7 H 0.2853 0.5829 -0.1927 0.044 Uiso 1 1 calc R . .
C8 C 0.1847(16) 0.6878(16) -0.0251(16) 0.038(4) Uani 1 1 d . . .
H8 H 0.1278 0.7664 -0.0555 0.046 Uiso 1 1 calc R . .
C9 C 0.1775(15) 0.6775(15) 0.1017(14) 0.031(4) Uani 1 1 d . . .
H9 H 0.1172 0.7520 0.1565 0.038 Uiso 1 1 calc R . .
C10 C 0.6626(14) -0.0154(12) 0.1107(12) 0.019(3) Uani 1 1 d . . .
C11 C 0.6999(16) -0.0617(15) -0.0122(13) 0.032(4) Uani 1 1 d . . .
H11 H 0.6678 -0.0025 -0.0733 0.038 Uiso 1 1 calc R . .
C12 C 0.7835(16) -0.1934(14) -0.0460(14) 0.033(4) Uani 1 1 d . . .
H12 H 0.8098 -0.2251 -0.1294 0.040 Uiso 1 1 calc R . .
C13 C 0.8274(15) -0.2774(14) 0.0471(14) 0.029(3) Uani 1 1 d . . .
H13 H 0.8823 -0.3682 0.0273 0.034 Uiso 1 1 calc R . .
C14 C 0.7919(15) -0.2299(13) 0.1679(13) 0.027(3) Uani 1 1 d . . .
H14 H 0.8253 -0.2884 0.2288 0.033 Uiso 1 1 calc R . .

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
W1 0.0176(3) 0.0148(3) 0.0148(3) 0.0025(2) -0.0090(2) -0.0047(2)
W2 0.0141(3) 0.0195(3) 0.0082(3) -0.0001(2) -0.0043(2) -0.0031(2)
W3 0.0156(3) 0.0180(3) 0.0092(3) 0.0043(2) -0.0074(2) -0.0060(2)
Cu2 0.0200(8) 0.0219(8) 0.0174(9) 0.0028(7) -0.0070(7) -0.0021(7)
Cu1 0.0224(8) 0.0202(8) 0.0129(8) -0.0006(6) -0.0095(7) -0.0021(7)
N1 0.015(5) 0.023(6) 0.016(6) 0.005(5) -0.010(5) -0.004(5)
N2 0.014(5) 0.020(6) 0.013(6) 0.008(4) -0.005(5) -0.005(5)
N3 0.013(3) 0.010(3) 0.009(3) 0.0008(18) -0.0066(19) 0.0011(19)
N4 0.021(3) 0.023(3) 0.021(3) 0.0028(19) -0.009(2) -0.007(2)
N5 0.020(6) 0.030(6) 0.016(6) -0.007(5) -0.007(5) -0.004(5)
O1 0.019(5) 0.014(4) 0.012(4) 0.000(3) -0.008(4) -0.006(4)
O2 0.015(4) 0.026(5) 0.013(5) 0.005(4) -0.006(4) -0.005(4)
O3 0.027(5) 0.024(5) 0.021(5) 0.001(4) -0.013(4) -0.005(4)
O4 0.016(4) 0.020(5) 0.024(5) 0.002(4) -0.016(4) -0.003(4)
O5 0.022(5) 0.021(5) 0.029(6) 0.007(4) -0.013(4) -0.009(4)
O6 0.014(4) 0.013(4) 0.012(4) -0.004(3) -0.006(4) -0.001(3)
O7 0.019(5) 0.015(4) 0.017(5) -0.001(4) -0.011(4) -0.001(4)
O8 0.020(5) 0.024(5) 0.014(5) -0.006(4) -0.011(4) -0.007(4)
O9 0.019(5) 0.028(5) 0.022(5) -0.001(4) -0.006(4) 0.000(4)
O10 0.022(3) 0.024(3) 0.021(3) 0.0008(18) -0.0101(18) -0.0079(18)
O11 0.009(4) 0.024(4) 0.008(4) 0.006(3) -0.007(3) -0.005(3)
O12 0.060(8) 0.033(6) 0.046(7) -0.003(5) -0.023(6) -0.020(5)
O13 0.130(14) 0.067(9) 0.095(12) 0.033(9) -0.078(11) -0.044(9)
C1 0.012(6) 0.024(7) 0.012(7) 0.001(5) 0.000(5) -0.001(5)
C2 0.013(6) 0.025(7) 0.007(6) 0.005(5) 0.003(5) -0.008(5)
C3 0.024(7) 0.026(7) 0.015(7) -0.007(6) -0.004(6) -0.003(6)
C4 0.021(7) 0.033(8) 0.010(7) 0.006(6) 0.002(6) -0.008(6)
C5 0.005(6) 0.040(8) 0.010(6) 0.009(6) -0.003(5) -0.008(6)
C6 0.044(9) 0.026(8) 0.016(7) 0.005(6) -0.010(7) -0.011(7)
C7 0.036(9) 0.055(10) 0.030(9) 0.031(8) -0.024(8) -0.026(8)
C8 0.028(8) 0.040(9) 0.045(10) 0.026(8) -0.024(8) -0.009(7)
C9 0.029(8) 0.039(9) 0.018(8) 0.014(7) -0.004(7) -0.011(7)
C10 0.022(7) 0.018(7) 0.012(7) 0.010(5) -0.004(6) -0.006(5)
C11 0.043(9) 0.048(10) 0.009(7) 0.013(7) -0.014(7) -0.021(8)
C12 0.035(9) 0.033(8) 0.014(7) 0.002(6) 0.001(7) -0.003(7)
C13 0.030(8) 0.027(8) 0.027(8) -0.005(6) -0.010(7) -0.008(6)
C14 0.038(9) 0.025(8) 0.019(7) -0.001(6) -0.016(7) -0.006(7)

_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
W1 O5 1.732(8) . ?
W1 O4 1.761(8) . ?
W1 O3 1.774(9) . ?
W1 O11 2.117(8) 2_576 ?
W1 O2 2.137(8) . ?
W1 O1 2.169(8) . ?
W2 O9 1.702(8) . ?
W2 O2 1.810(8) . ?
W2 O6 1.912(8) . ?
W2 O8 1.915(8) . ?
W2 O7 2.037(9) . ?
W2 O1 2.270(8) . ?
W2 W3 3.2356(8) . ?
W3 O10 1.705(9) . ?
W3 O11 1.811(8) . ?
W3 O8 1.887(8) 2_576 ?
W3 O1 1.963(8) . ?
W3 O6 1.982(7) . ?
W3 O1 2.352(8) 2_576 ?
Cu2 O3 1.883(8) . ?
Cu2 N1 1.979(10) . ?
Cu2 O12 1.993(11) . ?
Cu2 N4 2.000(11) . ?
Cu2 O5 2.179(8) 2_566 ?
Cu1 O4 1.923(8) . ?
Cu1 O7 1.952(8) . ?
Cu1 N5 1.960(11) 1_465 ?
Cu1 N2 2.003(10) 1_465 ?
N1 C1 1.358(16) . ?
N1 C4 1.370(17) . ?
N2 C2 1.343(16) . ?
N2 C1 1.396(16) . ?
N2 Cu1 2.002(10) 1_645 ?
N3 C1 1.222(16) . ?
N4 C9 1.317(16) . ?
N4 C5 1.333(16) . ?
N5 C14 1.338(16) . ?
N5 C10 1.360(16) . ?
N5 Cu1 1.960(11) 1_645 ?
O1 W3 2.352(8) 2_576 ?
O5 Cu2 2.179(8) 2_566 ?
O8 W3 1.887(8) 2_576 ?
O11 W1 2.117(8) 2_576 ?
C2 C3 1.397(18) . ?
C2 C10 1.447(17) . ?
C3 C4 1.349(18) . ?
C4 C5 1.451(17) . ?
C5 C6 1.367(19) . ?
C6 C7 1.401(19) . ?
C7 C8 1.37(2) . ?
C8 C9 1.37(2) . ?
C10 C11 1.371(19) . ?
C11 C12 1.362(19) . ?
C12 C13 1.37(2) . ?
C13 C14 1.357(19) . ?

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
O5 W1 O4 104.8(4) . . ?
O5 W1 O3 102.5(4) . . ?
O4 W1 O3 102.3(4) . . ?
O5 W1 O11 92.0(4) . 2_576 ?
O4 W1 O11 155.8(3) . 2_576 ?
O3 W1 O11 90.6(4) . 2_576 ?
O5 W1 O2 93.7(4) . . ?
O4 W1 O2 85.4(4) . . ?
O3 W1 O2 159.4(4) . . ?
O11 W1 O2 76.1(3) 2_576 . ?
O5 W1 O1 161.1(4) . . ?
O4 W1 O1 86.9(3) . . ?
O3 W1 O1 89.1(4) . . ?
O11 W1 O1 72.8(3) 2_576 . ?
O2 W1 O1 72.1(3) . . ?
O9 W2 O2 108.2(4) . . ?
O9 W2 O6 105.8(4) . . ?
O2 W2 O6 145.4(4) . . ?
O9 W2 O8 96.9(4) . . ?
O2 W2 O8 91.9(4) . . ?
O6 W2 O8 90.5(4) . . ?
O9 W2 O7 95.9(4) . . ?
O2 W2 O7 85.5(4) . . ?
O6 W2 O7 84.5(3) . . ?
O8 W2 O7 167.1(3) . . ?
O9 W2 O1 172.0(4) . . ?
O2 W2 O1 75.9(3) . . ?
O6 W2 O1 71.2(3) . . ?
O8 W2 O1 75.8(3) . . ?
O7 W2 O1 91.3(3) . . ?
O9 W2 W3 140.1(3) . . ?
O2 W2 W3 111.7(3) . . ?
O6 W2 W3 34.5(2) . . ?
O8 W2 W3 83.3(3) . . ?
O7 W2 W3 85.9(2) . . ?
O1 W2 W3 36.76(19) . . ?
O10 W3 O11 106.2(4) . . ?
O10 W3 O8 100.0(4) . 2_576 ?
O11 W3 O8 95.8(4) . 2_576 ?
O10 W3 O1 106.3(4) . . ?
O11 W3 O1 146.2(4) . . ?
O8 W3 O1 87.6(3) 2_576 . ?
O10 W3 O6 98.9(4) . . ?
O11 W3 O6 89.2(3) . . ?
O8 W3 O6 158.3(3) 2_576 . ?
O1 W3 O6 76.9(3) . . ?
O10 W3 O1 174.2(3) . 2_576 ?
O11 W3 O1 74.1(3) . 2_576 ?
O8 W3 O1 74.3(3) 2_576 2_576 ?
O1 W3 O1 74.6(3) . 2_576 ?
O6 W3 O1 86.9(3) . 2_576 ?
O10 W3 W2 104.0(3) . . ?
O11 W3 W2 118.0(2) . . ?
O8 W3 W2 130.0(3) 2_576 . ?
O1 W3 W2 43.8(2) . . ?
O6 W3 W2 33.1(2) . . ?
O1 W3 W2 80.68(19) 2_576 . ?
O3 Cu2 N1 171.9(4) . . ?
O3 Cu2 O12 92.1(4) . . ?
N1 Cu2 O12 95.6(4) . . ?
O3 Cu2 N4 93.9(4) . . ?
N1 Cu2 N4 80.5(4) . . ?
O12 Cu2 N4 152.2(5) . . ?
O3 Cu2 O5 93.7(4) . 2_566 ?
N1 Cu2 O5 82.7(4) . 2_566 ?
O12 Cu2 O5 98.9(4) . 2_566 ?
N4 Cu2 O5 107.7(4) . 2_566 ?
O4 Cu1 O7 92.0(4) . . ?
O4 Cu1 N5 91.8(4) . 1_465 ?
O7 Cu1 N5 176.2(4) . 1_465 ?
O4 Cu1 N2 170.7(4) . 1_465 ?
O7 Cu1 N2 94.7(4) . 1_465 ?
N5 Cu1 N2 81.5(4) 1_465 1_465 ?
C1 N1 C4 120.0(11) . . ?
C1 N1 Cu2 123.2(9) . . ?
C4 N1 Cu2 112.7(8) . . ?
C2 N2 C1 118.8(10) . . ?
C2 N2 Cu1 113.6(8) . 1_645 ?
C1 N2 Cu1 127.6(9) . 1_645 ?
C9 N4 C5 119.9(12) . . ?
C9 N4 Cu2 126.2(10) . . ?
C5 N4 Cu2 113.9(8) . . ?
C14 N5 C10 119.0(11) . . ?
C14 N5 Cu1 126.1(9) . 1_645 ?
C10 N5 Cu1 114.9(8) . 1_645 ?
W3 O1 W1 153.2(4) . . ?
W3 O1 W2 99.5(3) . . ?
W1 O1 W2 96.7(3) . . ?
W3 O1 W3 105.4(3) . 2_576 ?
W1 O1 W3 95.8(3) . 2_576 ?
W2 O1 W3 89.9(3) . 2_576 ?
W2 O2 W1 114.1(4) . . ?
W1 O3 Cu2 149.1(5) . . ?
W1 O4 Cu1 141.5(5) . . ?
W1 O5 Cu2 160.4(5) . 2_566 ?
W2 O6 W3 112.4(4) . . ?
Cu1 O7 W2 126.1(4) . . ?
W3 O8 W2 118.4(4) 2_576 . ?
W3 O11 W1 117.1(4) . 2_576 ?
N3 C1 N1 120.9(12) . . ?
N3 C1 N2 119.5(11) . . ?
N1 C1 N2 119.6(12) . . ?
N2 C2 C3 121.6(11) . . ?
N2 C2 C10 115.4(11) . . ?
C3 C2 C10 123.0(12) . . ?
C4 C3 C2 118.0(13) . . ?
C3 C4 N1 121.1(12) . . ?
C3 C4 C5 125.4(13) . . ?
N1 C4 C5 113.5(11) . . ?
N4 C5 C6 121.3(12) . . ?
N4 C5 C4 115.0(12) . . ?
C6 C5 C4 123.7(13) . . ?
C5 C6 C7 118.5(14) . . ?
C8 C7 C6 119.2(14) . . ?
C7 C8 C9 118.2(14) . . ?
N4 C9 C8 122.8(15) . . ?
N5 C10 C11 120.3(12) . . ?
N5 C10 C2 114.4(11) . . ?
C11 C10 C2 125.2(12) . . ?
C12 C11 C10 120.8(13) . . ?
C11 C12 C13 117.7(14) . . ?
C14 C13 C12 120.9(13) . . ?
N5 C14 C13 121.2(13) . . ?

_diffrn_measured_fraction_theta_max 0.977
_diffrn_reflns_theta_full        25.01
_diffrn_measured_fraction_theta_full 0.977
_refine_diff_density_max         2.447
_refine_diff_density_min         -2.032
_refine_diff_density_rms         0.358
#===END

data_compound2
_database_code_depnum_ccdc_archive 'CCDC 753691'
#TrackingRef 'compound1and2.cif'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C56 H38 Cl2 Cu2 N18 O19 W6'
_chemical_formula_weight         2568.12

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'
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
W W -0.8490 6.8722 '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'

_symmetry_cell_setting           Triclinic
_symmetry_space_group_name_H-M   P-1

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

_cell_length_a                   12.0461(13)
_cell_length_b                   12.8977(14)
_cell_length_c                   13.7956(13)
_cell_angle_alpha                98.0720(10)
_cell_angle_beta                 109.9870(10)
_cell_angle_gamma                117.834(2)
_cell_volume                     1661.1(3)
_cell_formula_units_Z            1
_cell_measurement_temperature    298(2)
_cell_measurement_reflns_used    5542
_cell_measurement_theta_min      3.402
_cell_measurement_theta_max      28.277

_exptl_crystal_description       block
_exptl_crystal_colour            green
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.10
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.567
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1188
_exptl_absorpt_coefficient_mu    11.134
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.3047
_exptl_absorpt_correction_T_max  0.4023
_exptl_absorpt_process_details   sadabs

_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            8798
_diffrn_reflns_av_R_equivalents  0.0285
_diffrn_reflns_av_sigmaI/netI    0.0347
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         1.68
_diffrn_reflns_theta_max         25.02
_reflns_number_total             5786
_reflns_number_gt                4690
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

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

_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^)+(0.0660P)^2^+0.2457P] 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         5786
_refine_ls_number_parameters     466
_refine_ls_number_restraints     42
_refine_ls_R_factor_all          0.0457
_refine_ls_R_factor_gt           0.0331
_refine_ls_wR_factor_ref         0.0981
_refine_ls_wR_factor_gt          0.0911
_refine_ls_goodness_of_fit_ref   1.012
_refine_ls_restrained_S_all      1.020
_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
W1 W 0.50462(4) 0.32867(3) 0.52848(3) 0.03966(12) Uani 1 1 d . . .
W2 W 0.48229(4) 0.54477(3) 0.66086(3) 0.04040(12) Uani 1 1 d . . .
W3 W 0.25539(3) 0.37295(3) 0.39977(3) 0.03950(11) Uani 1 1 d . . .
Cu1 Cu 0.63113(10) 0.86566(9) 0.92823(8) 0.0348(2) Uani 1 1 d . . .
Cl1 Cl 0.7900(2) 1.08456(19) 1.05256(17) 0.0461(5) Uani 1 1 d . . .
N1 N 0.8934(6) 0.8531(6) 0.9250(5) 0.0336(14) Uani 1 1 d . . .
H1 H 0.9740 0.8656 0.9358 0.040 Uiso 1 1 calc R . .
N2 N 0.7277(6) 0.9000(6) 0.8369(5) 0.0314(13) Uani 1 1 d . . .
N3 N 0.9273(7) 0.9561(6) 0.8091(5) 0.0346(14) Uani 1 1 d . . .
N4 N 0.4930(7) 0.8810(6) 0.8036(5) 0.0356(14) Uani 1 1 d . . .
N5 N 0.9495(8) 1.1265(8) 0.6274(7) 0.056(2) Uani 1 1 d . . .
N6 N 0.7252(7) 0.7818(6) 0.9898(5) 0.0335(14) Uani 1 1 d . . .
N7 N 0.8920(7) 0.7238(6) 1.0223(6) 0.0448(17) Uani 1 1 d . . .
N8 N 0.5288(7) 0.7973(6) 1.0142(5) 0.0400(15) Uani 1 1 d . . .
O1 O 0.5000 0.5000 0.5000 0.0368(17) Uani 1 2 d S . .
O2 O 0.4879(6) 0.3982(5) 0.6520(4) 0.0443(14) Uani 1 1 d . . .
O3 O 0.5168(6) 0.3265(5) 0.3934(5) 0.0430(13) Uani 1 1 d . . .
O4 O 0.3069(6) 0.2603(5) 0.4417(4) 0.0397(13) Uani 1 1 d . . .
O5 O 0.7000(6) 0.4644(6) 0.6044(5) 0.0507(15) Uani 1 1 d . . .
O6 O 0.5053(7) 0.2010(6) 0.5491(6) 0.0601(18) Uani 1 1 d . . .
O7 O 0.2897(6) 0.4346(5) 0.5490(5) 0.0449(14) Uani 1 1 d . . .
O8 O 0.6827(6) 0.6383(5) 0.7101(4) 0.0448(14) Uani 1 1 d . . .
O9 O 0.4711(8) 0.5765(6) 0.7791(5) 0.067(2) Uani 1 1 d . . .
O10 O 0.0756(6) 0.2810(6) 0.3288(6) 0.0605(18) Uani 1 1 d . . .
C1 C 0.8451(8) 0.9043(7) 0.8558(6) 0.0326(16) Uani 1 1 d . . .
C2 C 0.8858(8) 1.0053(7) 0.7377(6) 0.0334(17) Uani 1 1 d . . .
C3 C 0.7634(8) 1.0027(7) 0.7108(6) 0.0381(18) Uani 1 1 d . . .
H3 H 0.7355 1.0373 0.6604 0.046 Uiso 1 1 calc R . .
C4 C 0.6851(8) 0.9472(7) 0.7613(6) 0.0337(16) Uani 1 1 d . . .
C5 C 0.5464(8) 0.9275(7) 0.7384(7) 0.0364(17) Uani 1 1 d . . .
C6 C 0.4748(10) 0.9520(9) 0.6534(7) 0.052(2) Uani 1 1 d . . .
H6 H 0.5160 0.9883 0.6111 0.063 Uiso 1 1 calc R . .
C7 C 0.3399(10) 0.9215(11) 0.6319(8) 0.062(3) Uani 1 1 d . . .
H7 H 0.2883 0.9355 0.5738 0.074 Uiso 1 1 calc R . .
C8 C 0.2848(10) 0.8716(10) 0.6961(8) 0.059(3) Uani 1 1 d . . .
H8 H 0.1937 0.8488 0.6821 0.071 Uiso 1 1 calc R . .
C9 C 0.3633(10) 0.8548(9) 0.7813(8) 0.053(2) Uani 1 1 d . . .
H9 H 0.3254 0.8235 0.8270 0.064 Uiso 1 1 calc R . .
C10 C 0.9787(8) 1.0615(7) 0.6867(6) 0.0358(17) Uani 1 1 d . . .
C11 C 1.0893(9) 1.0476(8) 0.7035(8) 0.048(2) Uani 1 1 d . . .
H11 H 1.1052 0.9998 0.7443 0.057 Uiso 1 1 calc R . .
C12 C 1.1754(10) 1.1060(9) 0.6585(8) 0.056(2) Uani 1 1 d . . .
H12 H 1.2522 1.0996 0.6694 0.067 Uiso 1 1 calc R . .
C13 C 1.1485(11) 1.1730(10) 0.5984(9) 0.069(3) Uani 1 1 d . . .
H13 H 1.2049 1.2119 0.5660 0.083 Uiso 1 1 calc R . .
C14 C 1.0379(12) 1.1822(11) 0.5864(9) 0.071(3) Uani 1 1 d . . .
H14 H 1.0221 1.2307 0.5467 0.085 Uiso 1 1 calc R . .
C15 C 0.8320(8) 0.7842(7) 0.9803(6) 0.0356(17) Uani 1 1 d . . .
C16 C 0.8321(9) 0.6539(8) 1.0745(8) 0.051(2) Uani 1 1 d . . .
C17 C 0.7194(9) 0.6438(8) 1.0875(7) 0.047(2) Uani 1 1 d . . .
H17 H 0.6803 0.5938 1.1242 0.056 Uiso 1 1 calc R . .
C18 C 0.6670(8) 0.7102(7) 1.0441(6) 0.0386(18) Uani 1 1 d . . .
C19 C 0.5579(8) 0.7216(7) 1.0593(6) 0.0387(18) Uani 1 1 d . . .
C20 C 0.4955(10) 0.6653(9) 1.1195(8) 0.056(2) Uani 1 1 d . . .
H20 H 0.5161 0.6120 1.1486 0.067 Uiso 1 1 calc R . .
C21 C 0.4022(11) 0.6884(11) 1.1363(8) 0.068(3) Uani 1 1 d . . .
H21 H 0.3573 0.6496 1.1758 0.082 Uiso 1 1 calc R . .
C22 C 0.3755(11) 0.7694(10) 1.0943(8) 0.061(3) Uani 1 1 d . . .
H22 H 0.3146 0.7881 1.1067 0.074 Uiso 1 1 calc R . .
C23 C 0.4396(10) 0.8216(9) 1.0344(7) 0.052(2) Uani 1 1 d . . .
H23 H 0.4214 0.8764 1.0061 0.062 Uiso 1 1 calc R . .
C24 C 0.8925(11) 0.5881(10) 1.1236(11) 0.075(4) Uani 1 1 d . . .
N9 N 0.8301(12) 0.5134(10) 1.1673(10) 0.104(4) Uani 1 1 d . . .
C25 C 0.995(2) 0.5901(19) 1.1076(18) 0.161(7) Uani 1 1 d U . .
H25 H 1.0431 0.6489 1.0808 0.194 Uiso 1 1 calc R . .
C26 C 1.035(3) 0.498(2) 1.132(2) 0.186(8) Uani 1 1 d U . .
H26 H 1.0902 0.4811 1.1080 0.223 Uiso 1 1 calc R . .
C27 C 0.979(2) 0.4428(19) 1.1959(18) 0.158(7) Uani 1 1 d U . .
H27 H 1.0119 0.3993 1.2311 0.189 Uiso 1 1 calc R . .
C28 C 0.875(2) 0.4502(16) 1.2089(15) 0.132(6) Uani 1 1 d U . .
H28 H 0.8356 0.4076 1.2496 0.158 Uiso 1 1 calc R . .

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
W1 0.0473(2) 0.03098(18) 0.03374(19) 0.01366(14) 0.01384(15) 0.01979(16)
W2 0.0493(2) 0.03524(19) 0.02623(18) 0.00896(14) 0.01787(15) 0.01650(16)
W3 0.03448(19) 0.03438(19) 0.03258(19) 0.00821(14) 0.00856(14) 0.01316(15)
Cu1 0.0419(5) 0.0422(5) 0.0346(5) 0.0205(4) 0.0223(4) 0.0283(5)
Cl1 0.0445(11) 0.0448(11) 0.0438(11) 0.0070(9) 0.0169(9) 0.0260(10)
N1 0.032(3) 0.033(3) 0.035(3) 0.013(3) 0.015(3) 0.018(3)
N2 0.034(3) 0.034(3) 0.029(3) 0.012(3) 0.014(3) 0.021(3)
N3 0.036(3) 0.037(3) 0.024(3) 0.008(3) 0.012(3) 0.018(3)
N4 0.042(4) 0.042(4) 0.033(3) 0.016(3) 0.021(3) 0.027(3)
N5 0.054(5) 0.065(5) 0.064(5) 0.039(4) 0.034(4) 0.035(4)
N6 0.038(3) 0.032(3) 0.037(4) 0.016(3) 0.018(3) 0.023(3)
N7 0.047(4) 0.039(4) 0.052(4) 0.021(3) 0.017(3) 0.029(3)
N8 0.046(4) 0.047(4) 0.038(4) 0.020(3) 0.025(3) 0.029(3)
O1 0.041(4) 0.032(4) 0.025(4) 0.010(3) 0.012(3) 0.015(3)
O2 0.058(4) 0.038(3) 0.029(3) 0.015(2) 0.019(3) 0.021(3)
O3 0.051(3) 0.031(3) 0.039(3) 0.008(2) 0.018(3) 0.021(3)
O4 0.042(3) 0.029(3) 0.034(3) 0.011(2) 0.015(2) 0.012(2)
O5 0.044(3) 0.051(4) 0.047(3) 0.019(3) 0.009(3) 0.027(3)
O6 0.074(4) 0.040(3) 0.062(4) 0.027(3) 0.025(4) 0.032(3)
O7 0.038(3) 0.041(3) 0.044(3) 0.014(3) 0.022(3) 0.012(3)
O8 0.043(3) 0.041(3) 0.028(3) 0.007(2) 0.008(2) 0.014(3)
O9 0.078(5) 0.060(4) 0.043(4) 0.011(3) 0.037(4) 0.019(4)
O10 0.035(3) 0.050(4) 0.059(4) 0.009(3) 0.005(3) 0.012(3)
C1 0.041(4) 0.030(4) 0.023(4) 0.006(3) 0.014(3) 0.019(3)
C2 0.035(4) 0.028(4) 0.029(4) 0.010(3) 0.015(3) 0.012(3)
C3 0.045(5) 0.041(4) 0.038(4) 0.020(4) 0.021(4) 0.027(4)
C4 0.042(4) 0.033(4) 0.032(4) 0.012(3) 0.018(3) 0.024(4)
C5 0.040(4) 0.039(4) 0.041(4) 0.017(4) 0.020(4) 0.028(4)
C6 0.065(6) 0.077(6) 0.046(5) 0.035(5) 0.030(5) 0.054(6)
C7 0.060(6) 0.110(9) 0.056(6) 0.047(6) 0.035(5) 0.066(6)
C8 0.038(5) 0.086(7) 0.058(6) 0.027(5) 0.019(4) 0.039(5)
C9 0.049(5) 0.073(6) 0.052(5) 0.031(5) 0.029(4) 0.037(5)
C10 0.029(4) 0.040(4) 0.031(4) 0.011(3) 0.014(3) 0.015(3)
C11 0.054(5) 0.049(5) 0.055(5) 0.023(4) 0.037(5) 0.029(4)
C12 0.049(5) 0.059(6) 0.069(6) 0.027(5) 0.038(5) 0.027(5)
C13 0.062(7) 0.071(7) 0.082(8) 0.041(6) 0.057(6) 0.024(6)
C14 0.076(7) 0.081(7) 0.080(8) 0.059(6) 0.049(6) 0.044(6)
C15 0.034(4) 0.032(4) 0.032(4) 0.008(3) 0.006(3) 0.019(3)
C16 0.049(5) 0.040(5) 0.058(6) 0.025(4) 0.012(4) 0.026(4)
C17 0.045(5) 0.040(4) 0.048(5) 0.024(4) 0.021(4) 0.017(4)
C18 0.040(4) 0.035(4) 0.029(4) 0.010(3) 0.009(3) 0.017(4)
C19 0.041(4) 0.043(4) 0.035(4) 0.021(4) 0.021(4) 0.022(4)
C20 0.059(6) 0.068(6) 0.051(5) 0.039(5) 0.031(5) 0.034(5)
C21 0.062(6) 0.096(8) 0.058(6) 0.047(6) 0.043(5) 0.036(6)
C22 0.058(6) 0.083(7) 0.053(6) 0.031(5) 0.036(5) 0.037(6)
C23 0.061(6) 0.069(6) 0.043(5) 0.023(5) 0.029(5) 0.044(5)
C24 0.051(6) 0.066(7) 0.119(10) 0.062(7) 0.031(6) 0.038(6)
N9 0.090(7) 0.088(7) 0.128(10) 0.082(7) 0.026(7) 0.050(6)
C25 0.157(10) 0.147(9) 0.208(11) 0.108(8) 0.060(7) 0.108(8)
C26 0.173(11) 0.189(11) 0.211(12) 0.083(9) 0.066(8) 0.124(9)
C27 0.160(10) 0.141(9) 0.173(10) 0.101(8) 0.046(7) 0.094(8)
C28 0.128(9) 0.117(8) 0.145(10) 0.085(7) 0.039(6) 0.071(7)

_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
W1 O6 1.713(6) . ?
W1 O5 1.911(6) . ?
W1 O4 1.918(6) . ?
W1 O3 1.917(6) . ?
W1 O2 1.929(6) . ?
W1 O1 2.3204(4) . ?
W2 O9 1.692(6) . ?
W2 O7 1.908(6) . ?
W2 O3 1.911(5) 2_666 ?
W2 O2 1.911(6) . ?
W2 O8 1.917(6) . ?
W2 O1 2.3200(4) . ?
W3 O10 1.697(6) . ?
W3 O4 1.913(5) . ?
W3 O8 1.920(6) 2_666 ?
W3 O7 1.922(6) . ?
W3 O5 1.922(6) 2_666 ?
W3 O1 2.3128(4) . ?
Cu1 N2 1.953(6) . ?
Cu1 N6 1.979(6) . ?
Cu1 N8 1.995(7) . ?
Cu1 N4 2.052(6) . ?
Cu1 Cl1 2.434(2) . ?
N1 C1 1.358(9) . ?
N1 C15 1.371(10) . ?
N2 C1 1.320(10) . ?
N2 C4 1.351(9) . ?
N3 C2 1.326(10) . ?
N3 C1 1.335(10) . ?
N4 C9 1.341(11) . ?
N4 C5 1.330(10) . ?
N5 C14 1.335(12) . ?
N5 C10 1.331(10) . ?
N6 C15 1.324(10) . ?
N6 C18 1.361(10) . ?
N7 C16 1.335(11) . ?
N7 C15 1.354(9) . ?
N8 C19 1.344(10) . ?
N8 C23 1.352(11) . ?
O1 W3 2.3128(4) 2_666 ?
O1 W2 2.3200(4) 2_666 ?
O1 W1 2.3204(4) 2_666 ?
O3 W2 1.911(5) 2_666 ?
O5 W3 1.922(6) 2_666 ?
O8 W3 1.920(6) 2_666 ?
C2 C3 1.375(11) . ?
C2 C10 1.481(10) . ?
C3 C4 1.359(11) . ?
C4 C5 1.475(11) . ?
C5 C6 1.372(11) . ?
C6 C7 1.388(12) . ?
C7 C8 1.343(13) . ?
C8 C9 1.351(12) . ?
C10 C11 1.372(11) . ?
C11 C12 1.368(12) . ?
C12 C13 1.348(14) . ?
C13 C14 1.349(15) . ?
C16 C17 1.378(13) . ?
C16 C24 1.453(12) . ?
C17 C18 1.372(11) . ?
C18 C19 1.467(12) . ?
C19 C20 1.367(11) . ?
C20 C21 1.371(14) . ?
C21 C22 1.374(15) . ?
C22 C23 1.355(12) . ?
C24 N9 1.286(15) . ?
C24 C25 1.31(2) . ?
N9 C28 1.271(17) . ?
C25 C26 1.52(3) . ?
C26 C27 1.36(3) . ?
C27 C28 1.37(3) . ?

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
O6 W1 O5 104.5(3) . . ?
O6 W1 O4 103.1(3) . . ?
O5 W1 O4 152.4(2) . . ?
O6 W1 O3 104.3(3) . . ?
O5 W1 O3 87.4(3) . . ?
O4 W1 O3 86.2(2) . . ?
O6 W1 O2 103.6(3) . . ?
O5 W1 O2 86.7(3) . . ?
O4 W1 O2 86.4(2) . . ?
O3 W1 O2 152.1(2) . . ?
O6 W1 O1 179.1(2) . . ?
O5 W1 O1 76.30(17) . . ?
O4 W1 O1 76.08(15) . . ?
O3 W1 O1 76.05(16) . . ?
O2 W1 O1 76.02(16) . . ?
O9 W2 O7 104.3(3) . . ?
O9 W2 O3 104.6(3) . 2_666 ?
O7 W2 O3 86.9(2) . 2_666 ?
O9 W2 O2 102.8(3) . . ?
O7 W2 O2 86.5(3) . . ?
O3 W2 O2 152.5(2) 2_666 . ?
O9 W2 O8 103.2(3) . . ?
O7 W2 O8 152.6(2) . . ?
O3 W2 O8 86.5(3) 2_666 . ?
O2 W2 O8 87.2(3) . . ?
O9 W2 O1 179.0(3) . . ?
O7 W2 O1 76.28(17) . . ?
O3 W2 O1 76.16(17) 2_666 . ?
O2 W2 O1 76.36(16) . . ?
O8 W2 O1 76.28(16) . . ?
O10 W3 O4 103.9(3) . . ?
O10 W3 O8 104.9(3) . 2_666 ?
O4 W3 O8 86.6(2) . 2_666 ?
O10 W3 O7 102.5(3) . . ?
O4 W3 O7 87.2(2) . . ?
O8 W3 O7 152.6(2) 2_666 . ?
O10 W3 O5 103.5(3) . 2_666 ?
O4 W3 O5 152.6(2) . 2_666 ?
O8 W3 O5 86.4(3) 2_666 2_666 ?
O7 W3 O5 87.0(3) . 2_666 ?
O10 W3 O1 178.7(3) . . ?
O4 W3 O1 76.35(16) . . ?
O8 W3 O1 76.40(16) 2_666 . ?
O7 W3 O1 76.20(16) . . ?
O5 W3 O1 76.29(17) 2_666 . ?
N2 Cu1 N6 89.6(3) . . ?
N2 Cu1 N8 168.4(3) . . ?
N6 Cu1 N8 81.4(3) . . ?
N2 Cu1 N4 80.5(2) . . ?
N6 Cu1 N4 153.6(3) . . ?
N8 Cu1 N4 104.6(3) . . ?
N2 Cu1 Cl1 90.94(19) . . ?
N6 Cu1 Cl1 105.06(19) . . ?
N8 Cu1 Cl1 98.4(2) . . ?
N4 Cu1 Cl1 99.50(19) . . ?
C1 N1 C15 129.2(7) . . ?
C1 N2 C4 117.3(6) . . ?
C1 N2 Cu1 126.1(5) . . ?
C4 N2 Cu1 115.3(5) . . ?
C2 N3 C1 116.9(7) . . ?
C9 N4 C5 117.4(7) . . ?
C9 N4 Cu1 130.2(6) . . ?
C5 N4 Cu1 112.3(5) . . ?
C14 N5 C10 115.7(8) . . ?
C15 N6 C18 117.9(6) . . ?
C15 N6 Cu1 127.6(5) . . ?
C18 N6 Cu1 114.4(5) . . ?
C16 N7 C15 114.7(7) . . ?
C19 N8 C23 117.7(7) . . ?
C19 N8 Cu1 114.4(5) . . ?
C23 N8 Cu1 127.8(6) . . ?
W3 O1 W3 180.0 . 2_666 ?
W3 O1 W2 90.023(13) . 2_666 ?
W3 O1 W2 89.977(13) 2_666 2_666 ?
W3 O1 W2 89.977(13) . . ?
W3 O1 W2 90.023(13) 2_666 . ?
W2 O1 W2 180.0 2_666 . ?
W3 O1 W1 90.005(13) . . ?
W3 O1 W1 89.995(13) 2_666 . ?
W2 O1 W1 89.917(12) 2_666 . ?
W2 O1 W1 90.083(12) . . ?
W3 O1 W1 89.995(13) . 2_666 ?
W3 O1 W1 90.005(13) 2_666 2_666 ?
W2 O1 W1 90.083(12) 2_666 2_666 ?
W2 O1 W1 89.917(12) . 2_666 ?
W1 O1 W1 180.0 . 2_666 ?
W2 O2 W1 117.5(3) . . ?
W2 O3 W1 117.9(3) 2_666 . ?
W3 O4 W1 117.6(3) . . ?
W1 O5 W3 117.4(3) . 2_666 ?
W2 O7 W3 117.5(3) . . ?
W2 O8 W3 117.3(3) . 2_666 ?
N2 C1 N3 124.8(7) . . ?
N2 C1 N1 122.4(7) . . ?
N3 C1 N1 112.8(7) . . ?
N3 C2 C3 122.4(7) . . ?
N3 C2 C10 115.7(7) . . ?
C3 C2 C10 121.9(7) . . ?
C4 C3 C2 117.0(7) . . ?
N2 C4 C3 121.5(7) . . ?
N2 C4 C5 113.3(7) . . ?
C3 C4 C5 125.2(7) . . ?
N4 C5 C6 122.0(8) . . ?
N4 C5 C4 115.6(7) . . ?
C6 C5 C4 122.4(8) . . ?
C5 C6 C7 118.8(9) . . ?
C8 C7 C6 119.1(8) . . ?
C7 C8 C9 119.2(9) . . ?
N4 C9 C8 123.5(9) . . ?
N5 C10 C11 123.5(8) . . ?
N5 C10 C2 116.0(7) . . ?
C11 C10 C2 120.5(7) . . ?
C10 C11 C12 118.0(9) . . ?
C13 C12 C11 119.7(9) . . ?
C12 C13 C14 118.4(9) . . ?
N5 C14 C13 124.7(9) . . ?
N6 C15 N7 125.8(7) . . ?
N6 C15 N1 120.6(6) . . ?
N7 C15 N1 113.6(7) . . ?
N7 C16 C17 123.9(7) . . ?
N7 C16 C24 117.9(9) . . ?
C17 C16 C24 118.2(9) . . ?
C18 C17 C16 117.4(8) . . ?
N6 C18 C17 120.2(8) . . ?
N6 C18 C19 114.3(7) . . ?
C17 C18 C19 125.2(8) . . ?
N8 C19 C20 122.1(8) . . ?
N8 C19 C18 114.8(7) . . ?
C20 C19 C18 123.0(8) . . ?
C21 C20 C19 119.2(9) . . ?
C20 C21 C22 119.4(9) . . ?
C23 C22 C21 118.8(10) . . ?
N8 C23 C22 122.8(9) . . ?
N9 C24 C25 120.8(12) . . ?
N9 C24 C16 118.6(11) . . ?
C25 C24 C16 119.7(12) . . ?
C24 N9 C28 122.0(15) . . ?
C24 C25 C26 121(2) . . ?
C27 C26 C25 110(2) . . ?
C26 C27 C28 121.7(19) . . ?
N9 C28 C27 122.1(19) . . ?

_diffrn_measured_fraction_theta_max 0.984
_diffrn_reflns_theta_full        25.02
_diffrn_measured_fraction_theta_full 0.984
_refine_diff_density_max         1.484
_refine_diff_density_min         -1.184
_refine_diff_density_rms         0.175