# Electronic Supplementary Material (ESI) for CrystEngComm.
# This journal is © The Royal Society of Chemistry 2014

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#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
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#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
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#  except for the purpose of generating routine backup copies
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#  data retrieval see:
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data_55

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C20 H16 Cu2 N4 O44 Si W12, C10 H8 N2'
_chemical_formula_sum            'C30 H24 Cu2 N6 O44 Si W12'
_chemical_formula_weight         3533.82

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'
Si Si 0.0817 0.0704 '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           Monoclinic
_symmetry_space_group_name_H-M   P2(1)/c
_symmetry_space_group_name_hall  '-P 2ybc'

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

_cell_length_a                   11.622(5)
_cell_length_b                   22.213(5)
_cell_length_c                   11.896(5)
_cell_angle_alpha                90.000(5)
_cell_angle_beta                 112.738(5)
_cell_angle_gamma                90.000(5)
_cell_volume                     2832.4(18)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       ?
_exptl_crystal_colour            red
_exptl_crystal_size_max          0.43
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.21
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    4.144
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             3116.0
_exptl_absorpt_coefficient_mu    25.122
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.000
_exptl_absorpt_correction_T_max  0.005
_exptl_absorpt_process_details   adabs(Sheldrick,1996)

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71069
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'multiwire proportional'
_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            10642
_diffrn_reflns_av_R_equivalents  0.0572
_diffrn_reflns_av_sigmaI/netI    0.0813
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         3.26
_diffrn_reflns_theta_max         25.00
_reflns_number_total             4992
_reflns_number_gt                4046
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker XSCANS'
_computing_cell_refinement       'Bruker XSCANS'
_computing_data_reduction        'Bruker SHELXTL'
_computing_structure_solution    'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and
 goodness of fit S are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The threshold expression of
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
 not relevant to the choice of reflections for refinement.  R-factors based
 on F² are statistically about twice as large as those based on F, and R-
 factors based on ALL data will be even larger.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0413P)²+381.8426P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     SHELXL
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         4992
_refine_ls_number_parameters     430
_refine_ls_number_restraints     178
_refine_ls_R_factor_all          0.1126
_refine_ls_R_factor_gt           0.0943
_refine_ls_wR_factor_ref         0.2108
_refine_ls_wR_factor_gt          0.2013
_refine_ls_goodness_of_fit_ref   1.210
_refine_ls_restrained_S_all      1.198
_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
C2 C 0.888(6) 0.049(2) 0.523(6) 0.12(2) Uani 1 1 d DU . .
H2 H 0.9041 0.0835 0.4875 0.138 Uiso 1 1 calc R . .
C3 C 0.950(6) -0.004(3) 0.524(7) 0.11(2) Uani 1 1 d DU . .
C4 C 0.912(5) -0.057(2) 0.560(5) 0.10(2) Uani 1 1 d D . .
H4 H 0.9463 -0.0931 0.5496 0.123 Uiso 1 1 calc R . .
C6 C 0.539(4) 0.3038(16) 1.009(5) 0.057(13) Uani 1 1 d . . .
H6 H 0.4917 0.3235 1.0452 0.068 Uiso 1 1 calc R . .
C7 C 0.659(3) 0.3000(17) 1.073(5) 0.061(14) Uani 1 1 d . . .
H7 H 0.6940 0.3141 1.1525 0.073 Uiso 1 1 calc R . .
C8 C 0.738(3) 0.2731(16) 1.015(3) 0.035(8) Uani 1 1 d . . .
C9 C 0.677(3) 0.2533(17) 0.897(4) 0.042(10) Uani 1 1 d . . .
H9 H 0.7201 0.2377 0.8527 0.050 Uiso 1 1 calc R . .
C10 C 0.549(4) 0.2574(17) 0.848(4) 0.053(11) Uani 1 1 d . . .
H10 H 0.5092 0.2408 0.7706 0.064 Uiso 1 1 calc R . .
C11 C 0.879(2) 0.2708(18) 1.083(3) 0.051(12) Uani 1 1 d D . .
C12 C 0.940(3) 0.3058(16) 1.183(3) 0.060(12) Uani 1 1 d DU . .
H12 H 0.8998 0.3374 1.2040 0.072 Uiso 1 1 calc R . .
C13 C 1.064(3) 0.293(2) 1.252(4) 0.11(3) Uani 1 1 d D . .
H13 H 1.1053 0.3151 1.3236 0.127 Uiso 1 1 calc R . .
C14 C 1.063(3) 0.215(2) 1.118(4) 0.084(16) Uani 1 1 d DU . .
H14 H 1.1023 0.1823 1.0988 0.101 Uiso 1 1 calc R . .
C15 C 0.940(3) 0.2277(18) 1.045(3) 0.072(14) Uani 1 1 d DU . .
H15 H 0.9000 0.2075 0.9721 0.086 Uiso 1 1 calc R . .
N1 N 0.478(3) 0.2814(15) 0.895(3) 0.044(8) Uani 1 1 d . . .
N2 N 1.126(3) 0.250(2) 1.218(4) 0.100(16) Uani 1 1 d DU . .
O1 O 0.515(3) 0.0588(14) 1.087(3) 0.060(7) Uani 1 1 d U . .
O2 O 0.177(3) -0.0479(15) 0.788(3) 0.077(10) Uani 1 1 d U . .
O3 O 0.389(3) 0.0487(14) 0.932(3) 0.063(7) Uani 1 1 d U . .
O4 O 0.359(3) -0.0292(13) 0.961(3) 0.058(7) Uani 1 1 d U . .
O5 O 0.509(3) 0.0260(13) 0.873(3) 0.062(7) Uani 1 1 d U . .
O6 O 0.232(3) 0.0963(14) 0.972(2) 0.056(8) Uani 1 1 d . . .
O7 O 0.230(3) 0.0660(15) 0.758(3) 0.074(9) Uani 1 1 d U . .
O8 O 0.388(3) 0.0284(15) 0.671(3) 0.074(7) Uani 1 1 d U . .
O9 O 0.019(2) 0.0412(16) 0.812(3) 0.066(9) Uani 1 1 d . . .
O10 O 0.489(2) -0.0580(12) 0.576(2) 0.046(7) Uani 1 1 d . . .
O11 O 0.211(3) -0.1111(11) 1.176(3) 0.057(8) Uani 1 1 d . . .
O12 O 0.318(4) 0.1469(15) 0.634(3) 0.086(12) Uani 1 1 d . . .
O13 O 0.198(2) -0.1661(10) 0.745(3) 0.050(7) Uani 1 1 d . . .
O14 O 0.321(3) 0.2076(11) 1.059(3) 0.067(10) Uani 1 1 d . . .
O15 O 0.195(3) -0.0152(14) 1.013(3) 0.067(9) Uani 1 1 d U . .
O16 O 0.281(4) -0.1211(16) 0.983(3) 0.082(10) Uani 1 1 d U . .
O17 O 0.546(3) 0.1133(14) 0.808(3) 0.073(9) Uani 1 1 d U . .
O18 O 0.377(3) 0.1507(14) 0.883(3) 0.069(10) Uani 1 1 d . . .
O19 O 0.555(2) 0.1539(17) 1.102(3) 0.072(10) Uani 1 1 d . . .
O20 O 0.363(3) -0.0118(14) 1.231(4) 0.105(16) Uani 1 1 d . . .
O21 O 0.358(3) -0.0777(17) 0.714(2) 0.072(10) Uani 1 1 d . . .
O22 O 0.592(3) -0.1032(18) 0.810(3) 0.091(14) Uani 1 1 d . . .
Si1 Si 0.5000 0.0000 1.0000 0.020(2) Uani 1 2 d SU . .
Cu1 Cu 0.3007(6) 0.2682(4) 0.8089(8) 0.095(2) Uani 1 1 d . . .
W1 W 0.37150(14) 0.09942(7) 0.75056(14) 0.0376(4) Uani 1 1 d . . .
W2 W 0.17527(12) 0.02712(7) 0.87263(14) 0.0335(4) Uani 1 1 d . . .
W3 W 0.38239(13) 0.14066(6) 1.04221(14) 0.0341(4) Uani 1 1 d . . .
W4 W 0.29235(14) -0.11343(7) 0.82705(14) 0.0380(4) Uani 1 1 d . . .
W5 W 0.30273(15) -0.07415(7) 1.11835(16) 0.0392(4) Uani 1 1 d . . .
W6 W 0.49256(14) -0.04047(8) 0.71037(14) 0.0425(4) Uani 1 1 d U . .
C5 C 0.825(6) -0.055(2) 0.611(6) 0.11(2) Uani 1 1 d DU . .
H5 H 0.8084 -0.0896 0.6466 0.130 Uiso 1 1 calc R . .
N3 N 0.761(5) -0.003(3) 0.608(7) 0.16(2) Uani 1 1 d DU . .
C1 C 0.802(7) 0.050(2) 0.576(8) 0.16(2) Uani 1 1 d DU . .
H1 H 0.7710 0.0871 0.5906 0.189 Uiso 1 1 calc R . .


_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
C2 C3 1.372(19) . ?
C2 C1 1.375(19) . ?
C3 C4 1.377(19) . ?
C3 C3 1.50(8) 3_756 ?
C4 C5 1.371(18) . ?
C6 C7 1.31(5) . ?
C6 N1 1.36(6) . ?
C7 C8 1.47(6) . ?
C8 C9 1.37(5) . ?
C8 C11 1.52(4) . ?
C9 C10 1.37(5) . ?
C10 N1 1.28(5) . ?
C11 C12 1.370(18) . ?
C11 C15 1.370(19) . ?
C12 C13 1.378(18) . ?
C13 N2 1.361(18) . ?
C14 N2 1.375(18) . ?
C14 C15 1.378(19) . ?
N1 Cu1 1.94(3) . ?
N2 Cu1 1.94(3) 4_666 ?
O1 Si1 1.63(3) . ?
O1 W3 2.31(3) . ?
O1 W4 2.40(3) 3_657 ?
O1 W6 2.48(3) 3_657 ?
O2 W4 1.91(4) . ?
O2 W2 1.95(3) . ?
O3 Si1 1.64(3) . ?
O3 W2 2.35(3) . ?
O3 W1 2.37(3) . ?
O3 W3 2.44(3) . ?
O4 Si1 1.65(3) . ?
O4 W2 2.35(3) . ?
O4 W4 2.38(3) . ?
O4 W5 2.43(3) . ?
O5 Si1 1.66(3) . ?
O5 W1 2.36(3) . ?
O5 W6 2.38(3) . ?
O5 W5 2.40(3) 3_657 ?
O6 W2 1.89(3) . ?
O6 W3 1.90(3) . ?
O7 W1 1.83(3) . ?
O7 W2 1.92(3) . ?
O8 W1 1.89(3) . ?
O8 W6 1.89(3) . ?
O9 W2 1.70(2) . ?
O10 W6 1.63(3) . ?
O11 W5 1.69(2) . ?
O12 W1 1.66(3) . ?
O13 W4 1.64(2) . ?
O14 W3 1.69(2) . ?
O15 W2 1.85(3) . ?
O15 W5 1.91(3) . ?
O16 W5 1.85(4) . ?
O16 W4 1.92(4) . ?
O17 W5 1.85(3) 3_657 ?
O17 W1 1.89(3) . ?
O18 W3 1.89(3) . ?
O18 W1 1.92(3) . ?
O19 W3 1.87(3) . ?
O19 W4 1.87(3) 3_657 ?
O20 W5 1.86(3) . ?
O20 W6 1.93(3) 3_657 ?
O21 W6 1.78(3) . ?
O21 W4 1.95(3) . ?
O22 W3 1.86(3) 3_657 ?
O22 W6 1.90(3) . ?
Si1 O1 1.63(3) 3_657 ?
Si1 O3 1.64(3) 3_657 ?
Si1 O4 1.65(3) 3_657 ?
Si1 O5 1.66(3) 3_657 ?
Cu1 N2 1.94(3) 4_465 ?
W3 O22 1.86(3) 3_657 ?
W4 O19 1.87(3) 3_657 ?
W4 O1 2.40(3) 3_657 ?
W5 O17 1.85(3) 3_657 ?
W5 O5 2.40(3) 3_657 ?
W6 O20 1.93(3) 3_657 ?
W6 O1 2.48(3) 3_657 ?
C5 N3 1.376(19) . ?
N3 C1 1.379(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
C3 C2 C1 119(2) . . ?
C2 C3 C4 120(2) . . ?
C2 C3 C3 113(6) . 3_756 ?
C4 C3 C3 127(6) . 3_756 ?
C5 C4 C3 120(2) . . ?
C7 C6 N1 126(4) . . ?
C6 C7 C8 118(5) . . ?
C9 C8 C7 116(3) . . ?
C9 C8 C11 124(3) . . ?
C7 C8 C11 120(3) . . ?
C10 C9 C8 118(4) . . ?
N1 C10 C9 128(5) . . ?
C12 C11 C15 121(2) . . ?
C12 C11 C8 123(3) . . ?
C15 C11 C8 116(3) . . ?
C11 C12 C13 118.7(19) . . ?
N2 C13 C12 120.8(19) . . ?
N2 C14 C15 120(2) . . ?
C11 C15 C14 119(2) . . ?
C10 N1 C6 115(3) . . ?
C10 N1 Cu1 116(3) . . ?
C6 N1 Cu1 129(3) . . ?
C13 N2 C14 120(2) . . ?
C13 N2 Cu1 123(2) . 4_666 ?
C14 N2 Cu1 117(2) . 4_666 ?
Si1 O1 W3 125.9(16) . . ?
Si1 O1 W4 121.7(16) . 3_657 ?
W3 O1 W4 97.5(11) . 3_657 ?
Si1 O1 W6 116.7(15) . 3_657 ?
W3 O1 W6 94.8(11) . 3_657 ?
W4 O1 W6 92.7(10) 3_657 3_657 ?
W4 O2 W2 132.4(19) . . ?
Si1 O3 W2 123.6(16) . . ?
Si1 O3 W1 122.3(17) . . ?
W2 O3 W1 96.6(11) . . ?
Si1 O3 W3 118.0(15) . . ?
W2 O3 W3 94.8(11) . . ?
W1 O3 W3 94.7(11) . . ?
Si1 O4 W2 123.3(15) . . ?
Si1 O4 W4 122.1(15) . . ?
W2 O4 W4 96.6(11) . . ?
Si1 O4 W5 118.4(15) . . ?
W2 O4 W5 95.2(11) . . ?
W4 O4 W5 94.4(10) . . ?
Si1 O5 W1 122.3(16) . . ?
Si1 O5 W6 120.7(15) . . ?
W1 O5 W6 96.0(11) . . ?
Si1 O5 W5 119.7(15) . 3_657 ?
W1 O5 W5 96.2(11) . 3_657 ?
W6 O5 W5 95.7(11) . 3_657 ?
W2 O6 W3 137.2(17) . . ?
W1 O7 W2 140(2) . . ?
W1 O8 W6 137.0(19) . . ?
W2 O15 W5 140.0(18) . . ?
W5 O16 W4 139(2) . . ?
W5 O17 W1 141.3(19) 3_657 . ?
W3 O18 W1 136.9(18) . . ?
W3 O19 W4 142(2) . 3_657 ?
W5 O20 W6 138(2) . 3_657 ?
W6 O21 W4 142.0(16) . . ?
W3 O22 W6 139(2) 3_657 . ?
O1 Si1 O1 180.000(7) 3_657 . ?
O1 Si1 O3 69.8(15) 3_657 3_657 ?
O1 Si1 O3 110.2(15) . 3_657 ?
O1 Si1 O3 110.2(15) 3_657 . ?
O1 Si1 O3 69.8(15) . . ?
O3 Si1 O3 180.000(8) 3_657 . ?
O1 Si1 O4 69.9(14) 3_657 . ?
O1 Si1 O4 110.1(14) . . ?
O3 Si1 O4 112.8(15) 3_657 . ?
O3 Si1 O4 67.2(15) . . ?
O1 Si1 O4 110.1(14) 3_657 3_657 ?
O1 Si1 O4 69.9(14) . 3_657 ?
O3 Si1 O4 67.2(15) 3_657 3_657 ?
O3 Si1 O4 112.8(15) . 3_657 ?
O4 Si1 O4 180.000(4) . 3_657 ?
O1 Si1 O5 105.7(15) 3_657 3_657 ?
O1 Si1 O5 74.3(15) . 3_657 ?
O3 Si1 O5 68.8(15) 3_657 3_657 ?
O3 Si1 O5 111.2(15) . 3_657 ?
O4 Si1 O5 73.4(15) . 3_657 ?
O4 Si1 O5 106.6(15) 3_657 3_657 ?
O1 Si1 O5 74.3(15) 3_657 . ?
O1 Si1 O5 105.7(15) . . ?
O3 Si1 O5 111.2(15) 3_657 . ?
O3 Si1 O5 68.8(15) . . ?
O4 Si1 O5 106.6(15) . . ?
O4 Si1 O5 73.4(15) 3_657 . ?
O5 Si1 O5 180.000(7) 3_657 . ?
N2 Cu1 N1 176.1(19) 4_465 . ?
O12 W1 O7 104.0(17) . . ?
O12 W1 O8 101.0(17) . . ?
O7 W1 O8 87.3(15) . . ?
O12 W1 O17 101.5(17) . . ?
O7 W1 O17 154.3(15) . . ?
O8 W1 O17 90.7(14) . . ?
O12 W1 O18 100.9(17) . . ?
O7 W1 O18 87.2(13) . . ?
O8 W1 O18 158.1(15) . . ?
O17 W1 O18 85.2(13) . . ?
O12 W1 O5 154.5(17) . . ?
O7 W1 O5 95.6(13) . . ?
O8 W1 O5 63.5(13) . . ?
O17 W1 O5 60.9(13) . . ?
O18 W1 O5 96.0(13) . . ?
O12 W1 O3 159.0(17) . . ?
O7 W1 O3 61.8(13) . . ?
O8 W1 O3 94.0(13) . . ?
O17 W1 O3 92.8(13) . . ?
O18 W1 O3 64.7(12) . . ?
O5 W1 O3 46.5(11) . . ?
O9 W2 O15 102.6(15) . . ?
O9 W2 O6 99.8(14) . . ?
O15 W2 O6 87.6(12) . . ?
O9 W2 O7 102.2(16) . . ?
O15 W2 O7 155.2(15) . . ?
O6 W2 O7 87.0(12) . . ?
O9 W2 O2 99.4(15) . . ?
O15 W2 O2 90.5(14) . . ?
O6 W2 O2 160.8(14) . . ?
O7 W2 O2 86.8(14) . . ?
O9 W2 O4 157.7(14) . . ?
O15 W2 O4 63.3(12) . . ?
O6 W2 O4 96.8(12) . . ?
O7 W2 O4 93.4(13) . . ?
O2 W2 O4 65.4(13) . . ?
O9 W2 O3 156.6(14) . . ?
O15 W2 O3 94.6(13) . . ?
O6 W2 O3 65.0(11) . . ?
O7 W2 O3 61.3(13) . . ?
O2 W2 O3 96.2(13) . . ?
O4 W2 O3 45.6(10) . . ?
O14 W3 O22 101.5(19) . 3_657 ?
O14 W3 O19 104.6(15) . . ?
O22 W3 O19 87.5(12) 3_657 . ?
O14 W3 O18 99.5(17) . . ?
O22 W3 O18 158.9(18) 3_657 . ?
O19 W3 O18 88.7(12) . . ?
O14 W3 O6 98.7(14) . . ?
O22 W3 O6 88.1(12) 3_657 . ?
O19 W3 O6 156.7(16) . . ?
O18 W3 O6 87.3(10) . . ?
O14 W3 O1 159.6(14) . . ?
O22 W3 O1 65.3(15) 3_657 . ?
O19 W3 O1 61.0(14) . . ?
O18 W3 O1 94.8(14) . . ?
O6 W3 O1 96.4(12) . . ?
O14 W3 O3 154.1(14) . . ?
O22 W3 O3 96.1(16) 3_657 . ?
O19 W3 O3 94.9(14) . . ?
O18 W3 O3 63.6(12) . . ?
O6 W3 O3 62.9(12) . . ?
O1 W3 O3 46.3(10) . . ?
O13 W4 O19 103.0(15) . 3_657 ?
O13 W4 O2 98.9(14) . . ?
O19 W4 O2 158.1(16) 3_657 . ?
O13 W4 O16 103.5(16) . . ?
O19 W4 O16 85.9(14) 3_657 . ?
O2 W4 O16 90.0(15) . . ?
O13 W4 O21 103.3(14) . . ?
O19 W4 O21 87.0(13) 3_657 . ?
O2 W4 O21 87.1(15) . . ?
O16 W4 O21 153.1(15) . . ?
O13 W4 O4 158.0(12) . . ?
O19 W4 O4 93.9(14) 3_657 . ?
O2 W4 O4 65.2(13) . . ?
O16 W4 O4 63.3(13) . . ?
O21 W4 O4 91.4(13) . . ?
O13 W4 O1 155.7(13) . 3_657 ?
O19 W4 O1 59.0(13) 3_657 3_657 ?
O2 W4 O1 99.7(13) . 3_657 ?
O16 W4 O1 91.9(14) . 3_657 ?
O21 W4 O1 62.4(12) . 3_657 ?
O4 W4 O1 46.3(10) . 3_657 ?
O11 W5 O16 100.6(15) . . ?
O11 W5 O17 102.3(15) . 3_657 ?
O16 W5 O17 86.1(15) . 3_657 ?
O11 W5 O20 101.2(17) . . ?
O16 W5 O20 158.1(18) . . ?
O17 W5 O20 88.9(14) 3_657 . ?
O11 W5 O15 104.3(14) . . ?
O16 W5 O15 89.0(14) . . ?
O17 W5 O15 153.5(15) 3_657 . ?
O20 W5 O15 86.0(16) . . ?
O11 W5 O5 155.2(14) . 3_657 ?
O16 W5 O5 95.9(14) . 3_657 ?
O17 W5 O5 60.4(13) 3_657 3_657 ?
O20 W5 O5 63.3(13) . 3_657 ?
O15 W5 O5 94.3(12) . 3_657 ?
O11 W5 O4 156.3(13) . . ?
O16 W5 O4 63.0(13) . . ?
O17 W5 O4 93.9(13) 3_657 . ?
O20 W5 O4 96.2(16) . . ?
O15 W5 O4 60.8(12) . . ?
O5 W5 O4 48.4(10) 3_657 . ?
O10 W6 O21 102.9(13) . . ?
O10 W6 O8 100.2(14) . . ?
O21 W6 O8 84.2(16) . . ?
O10 W6 O22 102.4(16) . . ?
O21 W6 O22 88.4(14) . . ?
O8 W6 O22 157.2(17) . . ?
O10 W6 O20 101.0(17) . 3_657 ?
O21 W6 O20 155.9(16) . 3_657 ?
O8 W6 O20 89.2(14) . 3_657 ?
O22 W6 O20 88.9(15) . 3_657 ?
O10 W6 O5 155.2(12) . . ?
O21 W6 O5 93.7(13) . . ?
O8 W6 O5 62.8(12) . . ?
O22 W6 O5 96.3(15) . . ?
O20 W6 O5 62.9(14) 3_657 . ?
O10 W6 O1 156.5(12) . 3_657 ?
O21 W6 O1 62.5(10) . 3_657 ?
O8 W6 O1 96.5(13) . 3_657 ?
O22 W6 O1 61.1(14) . 3_657 ?
O20 W6 O1 95.5(16) 3_657 3_657 ?
O5 W6 O1 48.3(10) . 3_657 ?
C4 C5 N3 120(2) . . ?
C5 N3 C1 120(2) . . ?
C2 C1 N3 120(2) . . ?

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         2.884
_refine_diff_density_min         -2.588
_refine_diff_density_rms         0.480
_database_code_depnum_ccdc_archive 'CCDC 1011203'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_44

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C32 H8 Cu N4 O2, O40 Si W12, C16 H12 N2, 4(O)'
_chemical_formula_sum            'C48 H20 Cu N6 O46 Si W12'
_chemical_formula_weight         3714.42

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'
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'
Si Si 0.0817 0.0704 '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'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           ?
_symmetry_space_group_name_H-M   'C 2/m'
_symmetry_space_group_name_Hall  '-C 2y '

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

_cell_length_a                   16.044(5)
_cell_length_b                   21.276(5)
_cell_length_c                   11.001(5)
_cell_angle_alpha                90.000(5)
_cell_angle_beta                 110.460(5)
_cell_angle_gamma                90.000(5)
_cell_volume                     3518(2)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       ?
_exptl_crystal_colour            blue
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.34
_exptl_crystal_size_min          0.27
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    3.507
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             3298
_exptl_absorpt_coefficient_mu    19.947
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.000
_exptl_absorpt_correction_T_max  0.005
_exptl_absorpt_process_details   ?

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71069
_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            12233
_diffrn_reflns_av_R_equivalents  0.0436
_diffrn_reflns_av_sigmaI/netI    0.0358
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_theta_min         1.66
_diffrn_reflns_theta_max         25.00
_reflns_number_total             3198
_reflns_number_gt                2653
_reflns_threshold_expression     >2sigma(I)

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

_refine_special_details          
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and
 goodness of fit S are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The threshold expression of
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
 not relevant to the choice of reflections for refinement.  R-factors based
 on F² are statistically about twice as large as those based on F, and R-
 factors based on ALL data will be even larger.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0798P)²+106.5321P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         3186
_refine_ls_number_parameters     319
_refine_ls_number_restraints     28
_refine_ls_R_factor_all          0.0573
_refine_ls_R_factor_gt           0.0423
_refine_ls_wR_factor_ref         0.1424
_refine_ls_wR_factor_gt          0.1203
_refine_ls_goodness_of_fit_ref   1.107
_refine_ls_restrained_S_all      1.107
_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 0.9390(14) 0.2332(9) 0.408(2) 0.074(6) Uani 1 1 d . . .
H1 H 0.8966 0.2550 0.3412 0.089 Uiso 1 1 calc R . .
C2 C 0.9370(12) 0.1704(8) 0.4076(16) 0.059(5) Uani 1 1 d . . .
H2 H 0.8917 0.1498 0.3432 0.071 Uiso 1 1 calc R . .
C3 C 1.0000 0.1355(11) 0.5000 0.045(5) Uani 1 2 d S . .
C4 C 1.0000 0.0665(10) 0.5000 0.034(4) Uani 1 2 d S . .
C5 C 1.0721(11) 0.0336(8) 0.5776(17) 0.060(5) Uani 1 1 d . . .
H5 H 1.1218 0.0551 0.6312 0.072 Uiso 1 1 calc R . .
C6A C 1.0292(18) 0.1196(13) 0.155(2) 0.047(6) Uani 0.60 1 d P . .
C6B C 1.1016(19) 0.1185(12) 0.086(2) 0.021(6) Uani 0.40 1 d PDU . .
C7A C 1.097(2) 0.0551(14) 0.252(3) 0.027(7) Uani 0.40 1 d P . .
C7B C 1.1595(19) 0.0667(13) 0.179(3) 0.052(7) Uani 0.60 1 d P . .
C8A C 1.206(2) 0.1137(13) 0.271(3) 0.065(10) Uani 0.60 1 d PD . .
C8B C 1.148(2) 0.0988(15) 0.346(3) 0.026(7) Uani 0.40 1 d PU . .
C9A C 1.1503(15) 0.1633(10) 0.1734(17) 0.043(8) Uani 0.50 1 d PD . .
C9B C 1.0666(16) 0.1641(14) 0.239(3) 0.039(7) Uani 0.50 1 d PD . .
C10 C 1.1660(10) 0.1577(7) 0.3032(13) 0.038(3) Uani 1 1 d D . .
C11 C 1.2109(9) 0.2050(7) 0.4021(13) 0.037(3) Uani 1 1 d . . .
C12 C 1.2754(10) 0.1871(6) 0.5222(15) 0.042(4) Uani 1 1 d . . .
H12 H 1.2920 0.1451 0.5375 0.050 Uiso 1 1 calc R . .
C13 C 1.1863(11) 0.2686(7) 0.3839(14) 0.050(4) Uani 1 1 d . . .
H13 H 1.1430 0.2811 0.3064 0.060 Uiso 1 1 calc R . .
N1 N 1.0000 0.2651(9) 0.5000 0.049(5) Uani 1 2 d S . .
N2 N 1.0718(8) 0.0678(5) 0.1232(11) 0.033(3) Uani 1 1 d . . .
O1 O 0.8005(8) -0.1186(7) 0.1191(12) 0.069(4) Uani 1 1 d . . .
O2 O 0.6585(9) -0.0873(8) -0.1084(11) 0.078(5) Uani 1 1 d . . .
O1W O 1.096(2) 0.0000 -0.117(3) 0.125(10) Uani 1 2 d S . .
O3 O 0.6229(9) -0.1499(9) 0.0784(10) 0.082(5) Uani 1 1 d . . .
O4 O 0.5000 -0.2447(7) 0.0000 0.077(6) Uani 1 2 d S . .
O5 O 0.5444(11) -0.0637(7) -0.0284(14) 0.020(3) Uani 0.50 1 d P . .
O6 O 0.5708(8) -0.0623(6) 0.332(2) 0.105(7) Uani 1 1 d . . .
O7 O 0.5093(8) -0.1500(9) -0.1651(11) 0.084(5) Uani 1 1 d . . .
O8 O 0.6094(18) 0.0000 0.083(3) 0.107(9) Uani 1 2 d S . .
O9 O 0.7313(16) 0.0000 0.0575(19) 0.078(5) Uani 1 2 d SU . .
O10 O 0.7267(11) 0.0000 0.4712(14) 0.058(5) Uani 1 2 d S . .
O11 O 0.6958(12) -0.0622(8) 0.2396(17) 0.030(4) Uani 0.50 1 d PU . .
O12 O 0.5716(8) -0.1240(6) -0.3595(12) 0.059(3) Uani 1 1 d . . .
O13 O 0.5799(11) 0.0000 -0.268(3) 0.111(11) Uani 1 2 d S . .
O14 O 0.5062(17) 0.0000 0.154(3) 0.104(8) Uani 1 2 d S . .
Si1 Si 0.5000 0.0000 0.0000 0.0162(13) Uani 1 4 d S . .
Cu1 Cu 1.0000 0.0000 0.0000 0.0299(7) Uani 1 4 d S . .
W1 W 0.5000 -0.16632(3) 0.0000 0.0334(2) Uani 1 2 d S . .
W2 W 0.70105(4) -0.08340(3) 0.07683(6) 0.0392(2) Uani 1 1 d . . .
W3 W 0.54892(4) -0.08295(3) -0.24468(6) 0.0405(2) Uani 1 1 d . . .
W4 W 0.65214(6) 0.0000 0.32297(8) 0.0475(3) Uani 1 2 d S . .
O2W O 0.781(8) 0.263(3) 0.123(5) 0.74(11) Uani 1 1 d . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 N1 1.32(2) . ?
C1 C2 1.34(2) . ?
C2 C3 1.37(2) . ?
C3 C2 1.37(2) 2_756 ?
C3 C4 1.47(3) . ?
C4 C5 1.366(19) . ?
C4 C5 1.366(19) 2_756 ?
C5 C5 1.43(3) 6 ?
C6A C9B 1.31(4) . ?
C6A N2 1.40(3) . ?
C6A C6B 1.59(4) . ?
C6A C7A 1.84(4) . ?
C6B N2 1.30(3) . ?
C6B C9A 1.386(18) . ?
C6B C7B 1.57(4) . ?
C7A N2 1.36(3) . ?
C7A C8B 1.42(4) . ?
C7A C7B 1.51(5) . ?
C7B N2 1.33(3) . ?
C7B C8A 1.43(4) . ?
C7B C8B 2.03(4) . ?
C8A C10 1.25(3) . ?
C8A C8B 1.48(5) . ?
C8A C9A 1.545(18) . ?
C8B C10 1.41(4) . ?
C8B C9B 1.99(4) . ?
C9A C10 1.366(17) . ?
C9A C9B 1.732(19) . ?
C9B C10 1.51(3) . ?
C10 C11 1.47(2) . ?
C11 C13 1.41(2) . ?
C11 C12 1.416(19) . ?
C12 C13 1.38(2) 7_756 ?
C13 C12 1.38(2) 7_756 ?
N1 C1 1.32(2) 2_756 ?
N2 Cu1 2.037(11) . ?
O1 W2 1.674(11) . ?
O2 W3 1.872(12) . ?
O2 W2 1.911(12) . ?
O1W Cu1 2.32(3) . ?
O3 W1 1.888(12) . ?
O3 W2 1.895(14) . ?
O4 W1 1.668(16) . ?
O5 Si1 1.611(16) . ?
O5 O5 1.74(3) 2_655 ?
O5 W1 2.351(15) . ?
O5 W2 2.408(16) . ?
O5 W3 2.441(15) . ?
O6 W3 1.875(13) 2_655 ?
O6 W4 1.887(14) . ?
O7 W3 1.895(14) . ?
O7 W1 1.906(12) . ?
O8 Si1 1.67(3) . ?
O8 W2 2.322(19) 6 ?
O8 W2 2.322(19) . ?
O8 W4 2.48(3) . ?
O9 W2 1.871(7) 6 ?
O9 W2 1.871(7) . ?
O10 W4 1.652(14) . ?
O11 W2 1.877(18) . ?
O11 W4 1.879(18) . ?
O12 W3 1.676(11) . ?
O13 W3 1.876(9) 6 ?
O13 W3 1.876(9) . ?
O14 Si1 1.67(3) . ?
O14 W3 2.34(2) 5_655 ?
O14 W3 2.34(2) 2_655 ?
O14 W4 2.43(3) . ?
Si1 O5 1.611(16) 5_655 ?
Si1 O5 1.611(16) 6 ?
Si1 O5 1.611(16) 2_655 ?
Si1 O14 1.67(3) 5_655 ?
Si1 O8 1.67(3) 5_655 ?
Cu1 N2 2.037(11) 5_755 ?
Cu1 N2 2.037(11) 2_755 ?
Cu1 N2 2.037(11) 6 ?
Cu1 O1W 2.32(3) 5_755 ?
W1 O3 1.888(12) 2_655 ?
W1 O7 1.906(12) 2_655 ?
W1 O5 2.351(15) 2_655 ?
W3 O6 1.875(13) 2_655 ?
W3 O14 2.34(2) 5_655 ?
W4 O11 1.879(18) 6 ?
W4 O6 1.887(14) 6 ?

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
N1 C1 C2 121.6(17) . . ?
C1 C2 C3 121.9(17) . . ?
C2 C3 C2 115(2) 2_756 . ?
C2 C3 C4 122.7(11) 2_756 . ?
C2 C3 C4 122.7(11) . . ?
C5 C4 C5 118(2) . 2_756 ?
C5 C4 C3 120.8(10) . . ?
C5 C4 C3 120.8(10) 2_756 . ?
C4 C5 C5 120.8(10) . 6 ?
C9B C6A N2 127(2) . . ?
C9B C6A C6B 97(2) . . ?
N2 C6A C6B 51.1(15) . . ?
C9B C6A C7A 96(2) . . ?
N2 C6A C7A 47.1(13) . . ?
C6B C6A C7A 83.5(19) . . ?
N2 C6B C9A 122(2) . . ?
N2 C6B C7B 53.9(15) . . ?
C9A C6B C7B 88(2) . . ?
N2 C6B C6A 56.9(16) . . ?
C9A C6B C6A 89(2) . . ?
C7B C6B C6A 93(2) . . ?
N2 C7A C8B 121(3) . . ?
N2 C7A C7B 54.8(16) . . ?
C8B C7A C7B 87(2) . . ?
N2 C7A C6A 49.3(14) . . ?
C8B C7A C6A 91(2) . . ?
C7B C7A C6A 86.5(19) . . ?
N2 C7B C8A 122(3) . . ?
N2 C7B C7A 56.8(17) . . ?
C8A C7B C7A 91(3) . . ?
N2 C7B C6B 52.7(14) . . ?
C8A C7B C6B 91(2) . . ?
C7A C7B C6B 96(2) . . ?
N2 C7B C8B 90(2) . . ?
C8A C7B C8B 47(2) . . ?
C7A C7B C8B 44.6(17) . . ?
C6B C7B C8B 98(2) . . ?
C10 C8A C7B 122(3) . . ?
C10 C8A C8B 61(2) . . ?
C7B C8A C8B 88(3) . . ?
C10 C8A C9A 57.3(11) . . ?
C7B C8A C9A 87.6(18) . . ?
C8B C8A C9A 102(2) . . ?
C10 C8B C7A 118(2) . . ?
C10 C8B C8A 51.4(16) . . ?
C7A C8B C8A 93(2) . . ?
C10 C8B C9B 49.2(14) . . ?
C7A C8B C9B 86(2) . . ?
C8A C8B C9B 85.8(18) . . ?
C10 C8B C7B 84.3(17) . . ?
C7A C8B C7B 48.0(18) . . ?
C8A C8B C7B 44.8(15) . . ?
C9B C8B C7B 86.9(16) . . ?
C10 C9A C6B 121(2) . . ?
C10 C9A C8A 50.6(14) . . ?
C6B C9A C8A 94(2) . . ?
C10 C9A C9B 56.8(13) . . ?
C6B C9A C9B 88(2) . . ?
C8A C9A C9B 93.6(19) . . ?
C6A C9B C10 114(2) . . ?
C6A C9B C9A 86(2) . . ?
C10 C9B C9A 49.3(9) . . ?
C6A C9B C8B 88(2) . . ?
C10 C9B C8B 44.9(13) . . ?
C9A C9B C8B 78.3(14) . . ?
C8A C10 C9A 72.1(13) . . ?
C8A C10 C8B 67(2) . . ?
C9A C10 C8B 116.5(18) . . ?
C8A C10 C11 123.6(18) . . ?
C9A C10 C11 125.3(15) . . ?
C8B C10 C11 117.6(16) . . ?
C8A C10 C9B 120(2) . . ?
C9A C10 C9B 74.0(12) . . ?
C8B C10 C9B 86.0(19) . . ?
C11 C10 C9B 116.7(16) . . ?
C13 C11 C12 118.0(13) . . ?
C13 C11 C10 120.8(12) . . ?
C12 C11 C10 121.0(13) . . ?
C13 C12 C11 120.4(13) 7_756 . ?
C12 C13 C11 121.6(13) 7_756 . ?
C1 N1 C1 118(2) . 2_756 ?
C6B N2 C7B 73.4(17) . . ?
C6B N2 C7A 119.2(18) . . ?
C7B N2 C7A 68(2) . . ?
C6B N2 C6A 72.0(19) . . ?
C7B N2 C6A 115.3(19) . . ?
C7A N2 C6A 83.7(18) . . ?
C6B N2 Cu1 124.0(12) . . ?
C7B N2 Cu1 124.0(15) . . ?
C7A N2 Cu1 116.4(14) . . ?
C6A N2 Cu1 120.7(13) . . ?
W3 O2 W2 137.5(9) . . ?
W1 O3 W2 136.2(9) . . ?
Si1 O5 O5 57.3(6) . 2_655 ?
Si1 O5 W1 125.5(9) . . ?
O5 O5 W1 68.2(4) 2_655 . ?
Si1 O5 W2 120.7(8) . . ?
O5 O5 W2 132.4(11) 2_655 . ?
W1 O5 W2 95.1(5) . . ?
Si1 O5 W3 119.7(7) . . ?
O5 O5 W3 131.0(11) 2_655 . ?
W1 O5 W3 95.0(5) . . ?
W2 O5 W3 93.3(6) . . ?
W3 O6 W4 137.8(10) 2_655 . ?
W3 O7 W1 136.7(9) . . ?
Si1 O8 W2 122.5(8) . 6 ?
Si1 O8 W2 122.5(8) . . ?
W2 O8 W2 99.7(11) 6 . ?
Si1 O8 W4 115.5(16) . . ?
W2 O8 W4 95.2(8) 6 . ?
W2 O8 W4 95.2(8) . . ?
W2 O9 W2 143.0(13) 6 . ?
W2 O11 W4 141.6(10) . . ?
W3 O13 W3 140.4(16) 6 . ?
Si1 O14 W3 122.3(8) . 5_655 ?
Si1 O14 W3 122.3(8) . 2_655 ?
W3 O14 W3 97.7(11) 5_655 2_655 ?
Si1 O14 W4 118.5(14) . . ?
W3 O14 W4 94.8(8) 5_655 . ?
W3 O14 W4 94.8(8) 2_655 . ?
O5 Si1 O5 65.5(11) 5_655 6 ?
O5 Si1 O5 180.0(15) 5_655 . ?
O5 Si1 O5 114.5(11) 6 . ?
O5 Si1 O5 114.5(11) 5_655 2_655 ?
O5 Si1 O5 180.0(12) 6 2_655 ?
O5 Si1 O5 65.5(11) . 2_655 ?
O5 Si1 O14 71.1(6) 5_655 . ?
O5 Si1 O14 108.9(6) 6 . ?
O5 Si1 O14 108.9(6) . . ?
O5 Si1 O14 71.1(6) 2_655 . ?
O5 Si1 O14 108.9(6) 5_655 5_655 ?
O5 Si1 O14 71.1(6) 6 5_655 ?
O5 Si1 O14 71.1(6) . 5_655 ?
O5 Si1 O14 108.9(6) 2_655 5_655 ?
O14 Si1 O14 180.0(18) . 5_655 ?
O5 Si1 O8 110.1(7) 5_655 . ?
O5 Si1 O8 69.9(7) 6 . ?
O5 Si1 O8 69.9(7) . . ?
O5 Si1 O8 110.1(7) 2_655 . ?
O14 Si1 O8 76.3(14) . . ?
O14 Si1 O8 103.7(14) 5_655 . ?
O5 Si1 O8 69.9(7) 5_655 5_655 ?
O5 Si1 O8 110.1(7) 6 5_655 ?
O5 Si1 O8 110.1(7) . 5_655 ?
O5 Si1 O8 69.9(7) 2_655 5_655 ?
O14 Si1 O8 103.7(14) . 5_655 ?
O14 Si1 O8 76.3(14) 5_655 5_655 ?
O8 Si1 O8 180(3) . 5_655 ?
N2 Cu1 N2 180.0(11) . 5_755 ?
N2 Cu1 N2 89.9(7) . 2_755 ?
N2 Cu1 N2 90.1(7) 5_755 2_755 ?
N2 Cu1 N2 90.1(7) . 6 ?
N2 Cu1 N2 89.9(7) 5_755 6 ?
N2 Cu1 N2 180.0(8) 2_755 6 ?
N2 Cu1 O1W 87.7(7) . 5_755 ?
N2 Cu1 O1W 92.3(7) 5_755 5_755 ?
N2 Cu1 O1W 92.3(7) 2_755 5_755 ?
N2 Cu1 O1W 87.7(7) 6 5_755 ?
N2 Cu1 O1W 92.3(7) . . ?
N2 Cu1 O1W 87.7(7) 5_755 . ?
N2 Cu1 O1W 87.7(7) 2_755 . ?
N2 Cu1 O1W 92.3(7) 6 . ?
O1W Cu1 O1W 180.0(9) 5_755 . ?
O4 W1 O3 100.6(6) . 2_655 ?
O4 W1 O3 100.6(6) . . ?
O3 W1 O3 158.7(11) 2_655 . ?
O4 W1 O7 100.5(6) . 2_655 ?
O3 W1 O7 89.1(5) 2_655 2_655 ?
O3 W1 O7 87.0(6) . 2_655 ?
O4 W1 O7 100.5(6) . . ?
O3 W1 O7 87.0(6) 2_655 . ?
O3 W1 O7 89.1(5) . . ?
O7 W1 O7 159.0(12) 2_655 . ?
O4 W1 O5 158.2(4) . 2_655 ?
O3 W1 O5 64.7(6) 2_655 2_655 ?
O3 W1 O5 94.8(7) . 2_655 ?
O7 W1 O5 64.9(6) 2_655 2_655 ?
O7 W1 O5 94.9(7) . 2_655 ?
O4 W1 O5 158.2(4) . . ?
O3 W1 O5 94.8(7) 2_655 . ?
O3 W1 O5 64.7(6) . . ?
O7 W1 O5 94.9(7) 2_655 . ?
O7 W1 O5 64.9(6) . . ?
O5 W1 O5 43.5(8) 2_655 . ?
O1 W2 O9 101.3(9) . . ?
O1 W2 O11 101.5(7) . . ?
O9 W2 O11 88.8(8) . . ?
O1 W2 O3 103.5(7) . . ?
O9 W2 O3 155.2(9) . . ?
O11 W2 O3 85.5(7) . . ?
O1 W2 O2 103.2(7) . . ?
O9 W2 O2 86.0(7) . . ?
O11 W2 O2 155.4(7) . . ?
O3 W2 O2 89.2(5) . . ?
O1 W2 O8 152.3(8) . . ?
O9 W2 O8 58.1(9) . . ?
O11 W2 O8 63.0(9) . . ?
O3 W2 O8 98.2(8) . . ?
O2 W2 O8 94.1(9) . . ?
O1 W2 O5 160.8(7) . . ?
O9 W2 O5 92.8(8) . . ?
O11 W2 O5 91.7(7) . . ?
O3 W2 O5 63.4(6) . . ?
O2 W2 O5 64.6(6) . . ?
O8 W2 O5 46.8(7) . . ?
O12 W3 O2 100.8(7) . . ?
O12 W3 O6 100.9(8) . 2_655 ?
O2 W3 O6 158.3(8) . 2_655 ?
O12 W3 O13 104.4(11) . . ?
O2 W3 O13 86.4(8) . . ?
O6 W3 O13 88.9(6) 2_655 . ?
O12 W3 O7 98.8(7) . . ?
O2 W3 O7 88.0(5) . . ?
O6 W3 O7 88.0(6) 2_655 . ?
O13 W3 O7 156.8(11) . . ?
O12 W3 O14 157.6(8) . 5_655 ?
O2 W3 O14 94.9(8) . 5_655 ?
O6 W3 O14 64.5(8) 2_655 5_655 ?
O13 W3 O14 60.5(10) . 5_655 ?
O7 W3 O14 97.7(8) . 5_655 ?
O12 W3 O5 155.5(6) . . ?
O2 W3 O5 64.3(6) . . ?
O6 W3 O5 94.9(8) 2_655 . ?
O13 W3 O5 94.4(11) . . ?
O7 W3 O5 63.0(6) . . ?
O14 W3 O5 46.9(7) 5_655 . ?
O10 W4 O11 102.5(7) . . ?
O10 W4 O11 102.5(7) . 6 ?
O11 W4 O11 89.5(11) . 6 ?
O10 W4 O6 102.9(8) . 6 ?
O11 W4 O6 154.6(8) . 6 ?
O11 W4 O6 85.1(8) 6 6 ?
O10 W4 O6 102.9(8) . . ?
O11 W4 O6 85.1(8) . . ?
O11 W4 O6 154.6(8) 6 . ?
O6 W4 O6 89.2(8) 6 . ?
O10 W4 O14 158.0(9) . . ?
O11 W4 O14 93.0(7) . . ?
O11 W4 O14 93.0(7) 6 . ?
O6 W4 O14 62.6(7) 6 . ?
O6 W4 O14 62.6(7) . . ?
O10 W4 O8 152.3(9) . . ?
O11 W4 O8 59.6(6) . . ?
O11 W4 O8 59.6(6) 6 . ?
O6 W4 O8 96.7(8) 6 . ?
O6 W4 O8 96.7(8) . . ?
O14 W4 O8 49.7(10) . . ?

_diffrn_measured_fraction_theta_max 0.996
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.996
_refine_diff_density_max         3.259
_refine_diff_density_min         -2.344
_refine_diff_density_rms         0.472
_database_code_depnum_ccdc_archive 'CCDC 1011204'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_1313

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C12 H10 Cu N4 O40 Si W12, C12 H10 N4, 2(O)'
_chemical_formula_sum            'C24 H20 Cu N8 O42 Si W12'
_chemical_formula_weight         3390.20

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'
Si Si 0.0817 0.0704 '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           ?
_symmetry_space_group_name_H-M   'C 2/c'
_symmetry_space_group_name_Hall  '-C 2yc'

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

_cell_length_a                   24.737(5)
_cell_length_b                   10.601(5)
_cell_length_c                   20.038(5)
_cell_angle_alpha                90.000(5)
_cell_angle_beta                 99.405(5)
_cell_angle_gamma                90.000(5)
_cell_volume                     5184(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       ?
_exptl_crystal_colour            green
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.34
_exptl_crystal_size_min          0.27
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    4.344
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             5948
_exptl_absorpt_coefficient_mu    27.045
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.000
_exptl_absorpt_correction_T_max  0.001
_exptl_absorpt_process_details   ?

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71069
_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            8583
_diffrn_reflns_av_R_equivalents  0.0478
_diffrn_reflns_av_sigmaI/netI    0.0605
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         3.16
_diffrn_reflns_theta_max         25.00
_reflns_number_total             4554
_reflns_number_gt                3808
_reflns_threshold_expression     >2sigma(I)

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

_refine_special_details          
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and
 goodness of fit S are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The threshold expression of
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
 not relevant to the choice of reflections for refinement.  R-factors based
 on F² are statistically about twice as large as those based on F, and R-
 factors based on ALL data will be even larger.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0472P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         4545
_refine_ls_number_parameters     399
_refine_ls_number_restraints     48
_refine_ls_R_factor_all          0.0550
_refine_ls_R_factor_gt           0.0455
_refine_ls_wR_factor_ref         0.1163
_refine_ls_wR_factor_gt          0.1095
_refine_ls_goodness_of_fit_ref   1.133
_refine_ls_restrained_S_all      1.127
_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 0.1075(6) -0.1197(14) 0.4964(7) 0.018(3) Uani 1 1 d . . .
H1 H 0.0985 -0.1921 0.5184 0.021 Uiso 1 1 calc R . .
C2 C 0.1517(7) 0.0158(14) 0.4443(8) 0.021(4) Uani 1 1 d U . .
H2 H 0.1783 0.0553 0.4238 0.025 Uiso 1 1 calc R . .
C3 C 0.1026(6) 0.0590(17) 0.4487(7) 0.022(4) Uani 1 1 d . . .
H3 H 0.0890 0.1364 0.4316 0.026 Uiso 1 1 calc R . .
C5 C 0.2429(6) -0.1661(14) 0.4475(7) 0.018(3) Uani 1 1 d U . .
H5 H 0.2376 -0.1088 0.4119 0.021 Uiso 1 1 calc R . .
C6 C 0.2100(6) -0.2666(14) 0.5402(7) 0.018(3) Uani 1 1 d U . .
H6 H 0.1831 -0.2774 0.5671 0.022 Uiso 1 1 calc R . .
C7 C 0.2895(8) 0.208(2) 0.4636(9) 0.046(5) Uani 1 1 d . . .
H7 H 0.3166 0.1810 0.4399 0.055 Uiso 1 1 calc R . .
C8 C 0.2246(7) 0.3622(16) 0.4847(8) 0.031(4) Uani 1 1 d . . .
H8 H 0.2077 0.4399 0.4753 0.037 Uiso 1 1 calc R . .
C9 C 0.2615(7) 0.3251(17) 0.4471(8) 0.033(4) Uani 1 1 d . . .
C10 C 0.3321(7) 0.411(2) 0.3821(10) 0.052(6) Uani 1 1 d . . .
H10 H 0.3630 0.3684 0.4034 0.063 Uiso 1 1 calc R . .
C11 C 0.2442(8) 0.4783(18) 0.3565(10) 0.042(5) Uani 1 1 d . . .
H11 H 0.2069 0.4887 0.3570 0.050 Uiso 1 1 calc R . .
N1 N 0.0740(5) -0.0244(11) 0.4816(6) 0.015(3) Uani 1 1 d . . .
N2 N 0.1558(5) -0.1021(12) 0.4767(5) 0.017(3) Uani 1 1 d U . .
N4 N 0.2778(6) 0.4010(14) 0.3955(7) 0.035(4) Uani 1 1 d . . .
N5 N 0.2744(7) 0.5396(17) 0.3155(9) 0.050(5) Uani 1 1 d . . .
C12 C 0.3287(9) 0.4984(17) 0.3302(12) 0.048(6) Uani 1 1 d . . .
H12 H 0.3574 0.5250 0.3090 0.058 Uiso 1 1 calc R . .
O1 O -0.0452(4) 0.4119(9) 0.2775(4) 0.014(2) Uani 1 1 d . . .
O2 O -0.0299(3) 0.5871(9) 0.1882(4) 0.009(2) Uani 1 1 d . . .
O1W O 0.2536(5) 0.2521(12) 0.2489(7) 0.059(5) Uani 1 1 d . . .
O3 O 0.0370(4) 0.8565(9) 0.0819(5) 0.022(2) Uani 1 1 d . . .
O4 O 0.0550(4) 0.7769(10) 0.2180(5) 0.023(3) Uani 1 1 d . . .
O5 O 0.0681(4) 0.6070(10) 0.1293(4) 0.016(2) Uani 1 1 d . . .
O6 O -0.0319(3) 0.6445(9) 0.0627(4) 0.014(2) Uani 1 1 d . . .
O7 O -0.0490(4) 0.8168(9) 0.1533(4) 0.015(2) Uani 1 1 d . . .
O8 O 0.1533(4) 0.8394(10) 0.3074(5) 0.021(2) Uani 1 1 d . . .
O9 O 0.1268(4) 0.6000(9) 0.2488(5) 0.018(2) Uani 1 1 d . . .
O10 O 0.1768(4) 0.5188(9) 0.1411(5) 0.018(2) Uani 1 1 d U . .
O11 O 0.0864(3) 0.3527(9) 0.1156(4) 0.012(2) Uani 1 1 d . . .
O12 O 0.1483(3) 0.3605(9) 0.2377(4) 0.012(2) Uani 1 1 d . . .
O13 O -0.1138(4) 0.4799(10) 0.0081(5) 0.023(3) Uani 1 1 d . . .
O14 O -0.1239(3) 0.6392(9) 0.1169(4) 0.011(2) Uani 1 1 d U . .
O15 O -0.1106(3) 0.3932(9) 0.1419(4) 0.014(2) Uani 1 1 d . . .
O16 O 0.1499(4) 0.1616(10) 0.3241(5) 0.022(2) Uani 1 1 d . . .
O17 O 0.0364(4) 0.2210(9) 0.3227(4) 0.012(2) Uani 1 1 d . . .
O18 O -0.0735(4) 0.1790(9) 0.2935(4) 0.017(2) Uani 1 1 d . . .
O19 O 0.0199(3) 0.3923(9) 0.4082(4) 0.013(2) Uani 1 1 d . . .
O20 O -0.0183(4) 0.1437(10) 0.4261(5) 0.020(2) Uani 1 1 d . . .
Si1 Si 0.0000 0.4979(5) 0.2500 0.0064(11) Uani 1 2 d SU . .
Cu1 Cu 0.0000 0.0000 0.5000 0.0130(6) Uani 1 2 d S . .
W1 W 0.01464(2) 0.74051(6) 0.13230(3) 0.01269(17) Uani 1 1 d . . .
W2 W 0.10168(2) 0.72897(6) 0.30128(3) 0.01289(17) Uani 1 1 d . . .
W3 W 0.11849(2) 0.48828(5) 0.17177(3) 0.01106(17) Uani 1 1 d . . .
W4 W -0.07682(2) 0.51137(6) 0.08523(3) 0.01278(17) Uani 1 1 d . . .
W5 W 0.10336(2) 0.26986(6) 0.28945(3) 0.01191(17) Uani 1 1 d . . .
W6 W -0.02440(2) 0.25840(6) 0.36331(3) 0.01156(17) Uani 1 1 d . . .
C4 C 0.2026(5) -0.1814(13) 0.4872(6) 0.013(3) Uani 1 1 d U . .


_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 N1 1.310(18) . ?
C1 N2 1.331(16) . ?
C2 C3 1.32(2) . ?
C2 N2 1.405(18) . ?
C3 N1 1.367(19) . ?
C5 C6 1.35(2) 7_546 ?
C5 C4 1.382(17) . ?
C6 C5 1.35(2) 7_546 ?
C6 C4 1.384(19) . ?
C7 C8 1.37(2) 7_556 ?
C7 C9 1.43(3) . ?
C8 C9 1.33(2) . ?
C8 C7 1.37(2) 7_556 ?
C9 N4 1.42(2) . ?
C10 C12 1.39(3) . ?
C10 N4 1.41(2) . ?
C11 N4 1.33(2) . ?
C11 N5 1.36(2) . ?
N1 Cu1 1.943(12) . ?
N2 C4 1.419(17) . ?
N5 C12 1.40(3) . ?
O1 Si1 1.607(9) . ?
O1 W5 2.347(9) 2 ?
O1 W3 2.362(8) 2 ?
O1 W6 2.363(9) . ?
O2 Si1 1.636(9) . ?
O2 W4 2.338(8) . ?
O2 W1 2.349(9) . ?
O2 W2 2.362(8) 2 ?
O3 W1 1.737(10) . ?
O3 Cu1 2.314(10) 2_565 ?
O4 W1 1.880(10) . ?
O4 W2 1.935(10) . ?
O5 W3 1.875(10) . ?
O5 W1 1.944(10) . ?
O6 W4 1.896(9) . ?
O6 W1 1.944(9) . ?
O7 W1 1.877(9) . ?
O7 W2 1.944(9) 2 ?
O8 W2 1.722(10) . ?
O9 W2 1.891(9) . ?
O9 W3 1.930(9) . ?
O10 W3 1.690(10) . ?
O11 W3 1.916(9) . ?
O11 W6 1.935(9) 2 ?
O12 W5 1.900(8) . ?
O12 W3 1.951(9) . ?
O13 W4 1.695(11) . ?
O14 W2 1.898(9) 2 ?
O14 W4 1.959(9) . ?
O15 W5 1.886(9) 2 ?
O15 W4 1.966(9) . ?
O16 W5 1.693(10) . ?
O17 W6 1.865(8) . ?
O17 W5 1.954(9) . ?
O18 W6 1.894(10) . ?
O18 W5 1.958(9) 2 ?
O19 W4 1.880(9) 2 ?
O19 W6 1.924(9) . ?
O20 W6 1.738(9) . ?
O20 Cu1 2.121(9) . ?
Si1 O1 1.607(9) 2 ?
Si1 O2 1.636(9) 2 ?
Cu1 N1 1.943(12) 5_556 ?
Cu1 O20 2.121(10) 5_556 ?
Cu1 O3 2.314(10) 6_566 ?
Cu1 O3 2.314(10) 2_545 ?
W2 O14 1.898(9) 2 ?
W2 O7 1.944(9) 2 ?
W2 O2 2.362(9) 2 ?
W3 O1 2.362(9) 2 ?
W4 O19 1.880(9) 2 ?
W5 O15 1.886(9) 2 ?
W5 O18 1.958(9) 2 ?
W5 O1 2.347(9) 2 ?
W6 O11 1.935(9) 2 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 C1 N2 113.0(12) . . ?
C3 C2 N2 106.1(14) . . ?
C2 C3 N1 111.3(15) . . ?
C6 C5 C4 120.9(14) 7_546 . ?
C5 C6 C4 119.0(13) 7_546 . ?
C8 C7 C9 118.3(17) 7_556 . ?
C9 C8 C7 123.3(17) . 7_556 ?
C8 C9 N4 123.1(16) . . ?
C8 C9 C7 118.3(16) . . ?
N4 C9 C7 118.3(15) . . ?
C12 C10 N4 104.4(17) . . ?
N4 C11 N5 107.3(17) . . ?
C1 N1 C3 104.5(12) . . ?
C1 N1 Cu1 129.9(10) . . ?
C3 N1 Cu1 125.6(10) . . ?
C1 N2 C2 105.1(12) . . ?
C1 N2 C4 128.6(12) . . ?
C2 N2 C4 126.3(12) . . ?
C11 N4 C10 111.5(16) . . ?
C11 N4 C9 123.6(15) . . ?
C10 N4 C9 124.8(16) . . ?
C11 N5 C12 109.0(18) . . ?
C10 C12 N5 107.9(17) . . ?
Si1 O1 W5 124.3(4) . 2 ?
Si1 O1 W3 125.4(5) . 2 ?
W5 O1 W3 91.4(3) 2 2 ?
Si1 O1 W6 124.0(5) . . ?
W5 O1 W6 90.8(3) 2 . ?
W3 O1 W6 90.8(3) 2 . ?
Si1 O2 W4 124.5(5) . . ?
Si1 O2 W1 124.9(5) . . ?
W4 O2 W1 91.2(3) . . ?
Si1 O2 W2 123.7(4) . 2 ?
W4 O2 W2 91.5(3) . 2 ?
W1 O2 W2 91.1(3) . 2 ?
W1 O3 Cu1 138.7(5) . 2_565 ?
W1 O4 W2 152.5(6) . . ?
W3 O5 W1 151.7(5) . . ?
W4 O6 W1 121.4(4) . . ?
W1 O7 W2 123.3(5) . 2 ?
W2 O9 W3 152.5(6) . . ?
W3 O11 W6 121.7(4) . 2 ?
W5 O12 W3 122.0(4) . . ?
W2 O14 W4 121.5(4) 2 . ?
W5 O15 W4 149.8(5) 2 . ?
W6 O17 W5 151.8(5) . . ?
W6 O18 W5 121.0(5) . 2 ?
W4 O19 W6 153.0(5) 2 . ?
W6 O20 Cu1 172.3(6) . . ?
O1 Si1 O1 111.0(7) . 2 ?
O1 Si1 O2 108.8(4) . 2 ?
O1 Si1 O2 109.5(5) 2 2 ?
O1 Si1 O2 109.5(5) . . ?
O1 Si1 O2 108.8(4) 2 . ?
O2 Si1 O2 109.3(7) 2 . ?
N1 Cu1 N1 180.000(2) . 5_556 ?
N1 Cu1 O20 86.3(4) . 5_556 ?
N1 Cu1 O20 93.7(4) 5_556 5_556 ?
N1 Cu1 O20 93.7(4) . . ?
N1 Cu1 O20 86.3(4) 5_556 . ?
O20 Cu1 O20 180.000(1) 5_556 . ?
N1 Cu1 O3 86.9(4) . 6_566 ?
N1 Cu1 O3 93.1(4) 5_556 6_566 ?
O20 Cu1 O3 87.9(4) 5_556 6_566 ?
O20 Cu1 O3 92.1(4) . 6_566 ?
N1 Cu1 O3 93.1(4) . 2_545 ?
N1 Cu1 O3 86.9(4) 5_556 2_545 ?
O20 Cu1 O3 92.1(4) 5_556 2_545 ?
O20 Cu1 O3 87.9(4) . 2_545 ?
O3 Cu1 O3 180.000(1) 6_566 2_545 ?
O3 W1 O7 100.6(4) . . ?
O3 W1 O4 102.4(5) . . ?
O7 W1 O4 92.7(4) . . ?
O3 W1 O6 99.2(4) . . ?
O7 W1 O6 88.1(4) . . ?
O4 W1 O6 157.9(4) . . ?
O3 W1 O5 102.4(4) . . ?
O7 W1 O5 156.8(4) . . ?
O4 W1 O5 85.1(4) . . ?
O6 W1 O5 85.6(4) . . ?
O3 W1 O2 170.3(4) . . ?
O7 W1 O2 73.5(4) . . ?
O4 W1 O2 85.8(4) . . ?
O6 W1 O2 73.2(3) . . ?
O5 W1 O2 83.4(3) . . ?
O8 W2 O9 102.9(4) . . ?
O8 W2 O14 99.9(4) . 2 ?
O9 W2 O14 92.4(4) . 2 ?
O8 W2 O4 102.3(5) . . ?
O9 W2 O4 85.1(4) . . ?
O14 W2 O4 157.6(4) 2 . ?
O8 W2 O7 100.8(4) . 2 ?
O9 W2 O7 155.9(4) . 2 ?
O14 W2 O7 87.6(4) 2 2 ?
O4 W2 O7 85.8(4) . 2 ?
O8 W2 O2 170.4(4) . 2 ?
O9 W2 O2 84.8(4) . 2 ?
O14 W2 O2 73.7(3) 2 2 ?
O4 W2 O2 83.8(4) . 2 ?
O7 W2 O2 72.1(3) 2 2 ?
O10 W3 O5 104.5(4) . . ?
O10 W3 O11 103.0(4) . . ?
O5 W3 O11 93.2(4) . . ?
O10 W3 O9 100.8(4) . . ?
O5 W3 O9 85.8(4) . . ?
O11 W3 O9 155.5(4) . . ?
O10 W3 O12 97.4(4) . . ?
O5 W3 O12 157.3(4) . . ?
O11 W3 O12 87.3(4) . . ?
O9 W3 O12 84.5(4) . . ?
O10 W3 O1 169.6(4) . 2 ?
O5 W3 O1 85.7(3) . 2 ?
O11 W3 O1 73.9(3) . 2 ?
O9 W3 O1 81.7(3) . 2 ?
O12 W3 O1 72.7(3) . 2 ?
O13 W4 O19 102.6(4) . 2 ?
O13 W4 O6 100.3(4) . . ?
O19 W4 O6 93.2(4) 2 . ?
O13 W4 O14 99.8(4) . . ?
O19 W4 O14 156.9(4) 2 . ?
O6 W4 O14 88.0(4) . . ?
O13 W4 O15 100.6(4) . . ?
O19 W4 O15 85.2(4) 2 . ?
O6 W4 O15 158.8(4) . . ?
O14 W4 O15 85.6(4) . . ?
O13 W4 O2 171.2(4) . . ?
O19 W4 O2 84.9(4) 2 . ?
O6 W4 O2 74.2(3) . . ?
O14 W4 O2 73.3(3) . . ?
O15 W4 O2 84.6(3) . . ?
O16 W5 O15 101.2(4) . 2 ?
O16 W5 O12 98.4(4) . . ?
O15 W5 O12 93.0(4) 2 . ?
O16 W5 O17 103.8(4) . . ?
O15 W5 O17 85.4(4) 2 . ?
O12 W5 O17 157.6(4) . . ?
O16 W5 O18 98.7(5) . 2 ?
O15 W5 O18 159.8(4) 2 2 ?
O12 W5 O18 87.7(4) . 2 ?
O17 W5 O18 86.3(4) . 2 ?
O16 W5 O1 169.2(4) . 2 ?
O15 W5 O1 87.0(4) 2 2 ?
O12 W5 O1 73.9(3) . 2 ?
O17 W5 O1 83.7(3) . 2 ?
O18 W5 O1 73.7(4) 2 2 ?
O20 W6 O17 100.7(4) . . ?
O20 W6 O18 101.1(4) . . ?
O17 W6 O18 92.8(4) . . ?
O20 W6 O19 101.7(4) . . ?
O17 W6 O19 85.5(4) . . ?
O18 W6 O19 157.0(4) . . ?
O20 W6 O11 100.4(4) . 2 ?
O17 W6 O11 158.4(4) . 2 ?
O18 W6 O11 87.4(4) . 2 ?
O19 W6 O11 85.9(4) . 2 ?
O20 W6 O1 172.5(4) . . ?
O17 W6 O1 85.6(3) . . ?
O18 W6 O1 74.4(4) . . ?
O19 W6 O1 82.6(4) . . ?
O11 W6 O1 73.6(3) 2 . ?
C5 C4 C6 120.1(13) . . ?
C5 C4 N2 119.5(13) . . ?
C6 C4 N2 120.2(12) . . ?

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         2.600
_refine_diff_density_min         -2.936
_refine_diff_density_rms         0.493
_database_code_depnum_ccdc_archive 'CCDC 1011205'
