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


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

data_1
_database_code_depnum_ccdc_archive 'CCDC 893800'
#TrackingRef 'CIF(893800).txt'


_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'Cu H42 N10 O61 W18'
_chemical_formula_weight         4531.28

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
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'
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'

_symmetry_cell_setting           Orthorhombic
_symmetry_space_group_name_H-M   I2mm

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

_cell_length_a                   13.5226(9)
_cell_length_b                   17.5596(12)
_cell_length_c                   17.9569(13)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     4263.9(5)
_cell_formula_units_Z            2
_cell_measurement_temperature    295(2)
_cell_measurement_reflns_used    5122
_cell_measurement_theta_min      3.0177
_cell_measurement_theta_max      27.4835

_exptl_crystal_description       block
_exptl_crystal_colour            green
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.15
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    3.529
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             3922
_exptl_absorpt_coefficient_mu    24.493
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.0842
_exptl_absorpt_correction_T_max  0.1203
_exptl_absorpt_process_details   ?

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      295(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  'Mercury 70'
_diffrn_measurement_method       CCD_Profile_fitting
_diffrn_detector_area_resol_mean 14.6306
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            15987
_diffrn_reflns_av_R_equivalents  0.0634
_diffrn_reflns_av_sigmaI/netI    0.0605
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_theta_min         2.99
_diffrn_reflns_theta_max         27.51
_reflns_number_total             4922
_reflns_number_gt                3942
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'CrystalClear (Rigaku Corp., 2000)'
_computing_cell_refinement       'CrystalClear (Rigaku Corp., 2000)'
_computing_data_reduction        'CrystalClear (Rigaku Corp., 2000)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Diamond 3.0'
_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^)+(0.0300P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   ?
_refine_ls_hydrogen_treatment    ?
_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   0.00(2)
_refine_ls_number_reflns         4922
_refine_ls_number_parameters     227
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0522
_refine_ls_R_factor_gt           0.0404
_refine_ls_wR_factor_ref         0.0814
_refine_ls_wR_factor_gt          0.0770
_refine_ls_goodness_of_fit_ref   0.983
_refine_ls_restrained_S_all      0.983
_refine_ls_shift/su_max          0.002
_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 0.48777(7) 0.0000 0.0000 0.0336(2) Uani 1 4 d S . .
W2 W 0.68145(5) 0.10575(4) 0.10481(3) 0.05155(17) Uani 1 1 d . . .
W3 W 0.46641(5) 0.19921(4) 0.10143(3) 0.05134(17) Uani 1 1 d . . .
W4 W 0.24060(6) 0.13393(5) 0.0000 0.0476(4) Uani 1 2 d S . .
W5 W 0.59536(8) 0.0000 0.27411(5) 0.0644(3) Uani 1 2 d S . .
W6 W 0.38053(6) 0.09457(4) 0.27008(3) 0.0634(2) Uani 1 1 d . . .
W7 W 0.20776(10) 0.0000 0.15252(7) 0.0560(4) Uani 0.50 2 d SP . .
Cu Cu 0.20776(10) 0.0000 0.15252(7) 0.0560(4) Uani 0.50 2 d SP . .
O1 O 0.3621(11) 0.0000 0.0000 0.037(4) Uani 1 4 d S . .
O2 O 0.5239(7) 0.0745(5) 0.0716(4) 0.039(2) Uani 1 1 d . . .
O3 O 0.6088(8) 0.2003(6) 0.1198(5) 0.053(2) Uani 1 1 d . . .
O4 O 0.6454(7) 0.0753(6) 0.2045(5) 0.051(2) Uani 1 1 d . . .
O5 O 0.7057(10) 0.0000 0.0853(7) 0.062(4) Uani 1 2 d S . .
O6 O 0.6915(11) 0.1222(9) 0.0000 0.059(4) Uani 1 2 d S . .
O7 O 0.4416(8) 0.1571(5) 0.1993(5) 0.049(2) Uani 1 1 d . . .
O8 O 0.3452(8) 0.1615(6) 0.0698(5) 0.059(3) Uani 1 1 d . . .
O9 O 0.4423(10) 0.2945(7) 0.1228(6) 0.079(4) Uani 1 1 d . . .
O10 O 0.4958(11) 0.2173(7) 0.0000 0.044(3) Uani 1 2 d S . .
O11 O 0.1703(14) 0.2198(10) 0.0000 0.084(6) Uani 1 2 d S . .
O12 O 0.6903(13) 0.0000 0.3398(8) 0.084(6) Uani 1 2 d S . .
O13 O 0.4579(9) 0.0000 0.2059(5) 0.037(3) Uani 1 2 d S . .
O14 O 0.5122(9) 0.0769(8) 0.3172(5) 0.074(3) Uani 1 1 d . . .
O15 O 0.3508(11) 0.0000 0.3217(5) 0.060(4) Uani 1 2 d S . .
O16 O 0.3322(10) 0.1647(8) 0.3306(6) 0.083(4) Uani 1 1 d . . .
O17 O 0.2737(8) 0.0732(7) 0.2079(5) 0.068(3) Uani 1 1 d . . .
O18 O 0.080(2) 0.0000 0.1927(14) 0.150(11) Uani 1 2 d S . .
O19 O 0.1862(8) 0.0764(6) 0.0761(6) 0.062(3) Uani 1 1 d . . .
O20 O 0.7942(9) 0.1397(7) 0.1269(7) 0.074(3) Uani 1 1 d . . .
N1 N -0.138(9) 0.0000 0.5000 0.15(3) Uiso 0.50 4 d SP . .
N2 N 0.008(7) 0.0000 0.0000 0.24(3) Uiso 1 4 d S . .
N3 N 0.335(3) 0.225(3) 0.5000 0.125(14) Uiso 0.75 2 d SP . .
N4 N 0.692(9) 0.0000 0.5000 0.16(4) Uiso 0.50 4 d SP . .
N5 N 1.09(4) 0.0000 0.5000 0.6(3) Uiso 0.50 4 d SP . .
N6 N 0.474(4) 0.201(3) 0.403(2) 0.129(15) Uiso 0.50 1 d P . .
N7 N 0.265(9) 0.445(6) 0.083(6) 0.33(6) Uiso 0.50 1 d P . .
N8 N -1.052(15) 0.246(10) 0.5000 0.39(11) Uiso 0.50 2 d SP . .
N9 N -0.010(11) 0.0000 0.328(8) 0.28(6) Uiso 0.50 2 d SP . .

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 0.0332(6) 0.0415(6) 0.0262(4) 0.000 0.000 0.000
W2 0.0406(4) 0.0651(4) 0.0490(3) -0.0082(3) -0.0069(3) -0.0112(3)
W3 0.0589(4) 0.0481(3) 0.0470(3) -0.0107(2) -0.0020(3) -0.0008(3)
W4 0.0441(6) 0.0566(6) 0.0421(5) 0.000 0.000 0.0123(4)
W5 0.0678(7) 0.0870(8) 0.0385(4) 0.000 -0.0215(4) 0.000
W6 0.0783(5) 0.0760(5) 0.0361(3) -0.0134(3) 0.0097(3) 0.0044(4)
W7 0.0485(9) 0.0725(10) 0.0470(6) 0.000 0.0010(6) 0.000
Cu 0.0485(9) 0.0725(10) 0.0470(6) 0.000 0.0010(6) 0.000
O1 0.010(8) 0.075(13) 0.025(7) 0.000 0.000 0.000
O2 0.047(6) 0.044(5) 0.026(4) 0.003(3) -0.007(4) -0.002(4)
O3 0.047(6) 0.050(6) 0.061(6) -0.006(5) 0.009(5) -0.007(5)
O4 0.050(6) 0.063(7) 0.040(5) 0.000(4) -0.013(4) 0.002(5)
O5 0.026(8) 0.121(14) 0.038(7) 0.000 0.004(6) 0.000
O6 0.038(9) 0.081(11) 0.060(8) 0.000 0.000 -0.016(8)
O7 0.068(7) 0.037(5) 0.041(4) -0.011(4) -0.010(5) 0.004(5)
O8 0.054(7) 0.068(7) 0.054(5) 0.003(5) 0.001(5) 0.003(6)
O9 0.080(9) 0.081(9) 0.075(7) -0.031(6) -0.004(6) 0.006(7)
O10 0.055(9) 0.038(7) 0.037(6) 0.000 0.000 -0.011(7)
O11 0.091(14) 0.066(11) 0.095(12) 0.000 0.000 0.052(10)
O12 0.070(12) 0.132(16) 0.052(8) 0.000 -0.040(8) 0.000
O13 0.042(7) 0.052(7) 0.019(5) 0.000 0.001(5) 0.000
O14 0.073(8) 0.125(10) 0.024(4) -0.002(5) 0.009(5) -0.011(7)
O15 0.060(10) 0.108(13) 0.012(5) 0.000 0.016(6) 0.000
O16 0.070(8) 0.123(11) 0.056(6) -0.027(7) 0.013(6) -0.008(7)
O17 0.062(8) 0.107(9) 0.034(5) 0.013(5) 0.004(5) 0.010(7)
O18 0.13(2) 0.20(3) 0.126(19) 0.000 0.092(17) 0.000
O19 0.057(7) 0.062(7) 0.065(6) -0.029(5) 0.014(6) -0.004(6)
O20 0.055(7) 0.092(10) 0.075(7) -0.021(6) 0.002(6) -0.015(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 O1 1.699(15) . ?
W1 O2 1.898(8) . ?
W1 O2 1.898(8) 2 ?
W1 O2 1.898(8) 4 ?
W1 O2 1.898(8) 3 ?
W2 O20 1.684(11) . ?
W2 O6 1.909(3) . ?
W2 O5 1.918(3) . ?
W2 O4 1.931(9) . ?
W2 O3 1.948(11) . ?
W2 O2 2.280(9) . ?
W3 O9 1.747(12) . ?
W3 O8 1.857(11) . ?
W3 O10 1.891(4) . ?
W3 O7 1.936(9) . ?
W3 O3 1.953(11) . ?
W3 N8 2.08(8) 6_655 ?
W3 O2 2.385(9) . ?
W4 O11 1.783(15) . ?
W4 O19 1.852(11) 3 ?
W4 O19 1.852(11) . ?
W4 O8 1.950(11) . ?
W4 O8 1.950(11) 3 ?
W5 O12 1.743(14) . ?
W5 O14 1.920(13) 4 ?
W5 O14 1.920(13) . ?
W5 O4 1.942(10) . ?
W5 O4 1.942(10) 4 ?
W5 O13 2.226(12) . ?
W6 O16 1.767(12) . ?
W6 O17 1.864(11) . ?
W6 O7 1.872(10) . ?
W6 O15 1.944(5) . ?
W6 O14 1.995(12) . ?
W6 O13 2.276(8) . ?
Cu/W7 O17 1.853(13) . ?
Cu/W7 O17 1.853(13) 4 ?
Cu/W7 O18 1.88(2) . ?
Cu/W7 O19 1.941(12) 4 ?
Cu/W7 O19 1.941(12) . ?
O5 W2 1.918(3) 4 ?
O6 W2 1.909(3) 3 ?
O10 N8 0.92(18) 6_655 ?
O10 W3 1.891(4) 3 ?
O13 W6 2.276(8) 4 ?
O15 W6 1.944(5) 4 ?
N8 O10 0.92(18) 6_355 ?
N8 W3 2.08(8) 8_355 ?
N8 W3 2.08(8) 6_355 ?

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 W1 O2 104.9(3) . . ?
O1 W1 O2 104.9(3) . 2 ?
O2 W1 O2 150.2(6) . 2 ?
O1 W1 O2 104.9(3) . 4 ?
O2 W1 O2 87.1(5) . 4 ?
O2 W1 O2 85.3(5) 2 4 ?
O1 W1 O2 104.9(3) . 3 ?
O2 W1 O2 85.3(5) . 3 ?
O2 W1 O2 87.1(5) 2 3 ?
O2 W1 O2 150.2(6) 4 3 ?
O20 W2 O6 96.6(6) . . ?
O20 W2 O5 103.3(6) . . ?
O6 W2 O5 87.4(6) . . ?
O20 W2 O4 96.2(5) . . ?
O6 W2 O4 166.9(5) . . ?
O5 W2 O4 86.8(5) . . ?
O20 W2 O3 97.0(5) . . ?
O6 W2 O3 92.5(6) . . ?
O5 W2 O3 159.5(5) . . ?
O4 W2 O3 88.9(4) . . ?
O20 W2 O2 173.1(5) . . ?
O6 W2 O2 81.1(5) . . ?
O5 W2 O2 83.1(5) . . ?
O4 W2 O2 86.6(4) . . ?
O3 W2 O2 76.7(4) . . ?
O9 W3 O8 104.1(6) . . ?
O9 W3 O10 95.1(6) . . ?
O8 W3 O10 87.2(5) . . ?
O9 W3 O7 97.7(5) . . ?
O8 W3 O7 89.4(4) . . ?
O10 W3 O7 167.2(5) . . ?
O9 W3 O3 97.9(5) . . ?
O8 W3 O3 157.7(4) . . ?
O10 W3 O3 87.4(5) . . ?
O7 W3 O3 91.2(4) . . ?
O9 W3 N8 74(4) . 6_655 ?
O8 W3 N8 78(5) . 6_655 ?
O10 W3 N8 26(5) . 6_655 ?
O7 W3 N8 162(5) . 6_655 ?
O3 W3 N8 105(6) . 6_655 ?
O9 W3 O2 171.7(5) . . ?
O8 W3 O2 83.8(4) . . ?
O10 W3 O2 82.5(5) . . ?
O7 W3 O2 84.8(3) . . ?
O3 W3 O2 74.1(4) . . ?
N8 W3 O2 106(4) 6_655 . ?
O11 W4 O19 104.5(6) . 3 ?
O11 W4 O19 104.5(6) . . ?
O19 W4 O19 95.1(6) 3 . ?
O11 W4 O8 100.2(6) . . ?
O19 W4 O8 153.8(5) 3 . ?
O19 W4 O8 87.1(5) . . ?
O11 W4 O8 100.2(6) . 3 ?
O19 W4 O8 87.1(5) 3 3 ?
O19 W4 O8 153.8(5) . 3 ?
O8 W4 O8 79.9(6) . 3 ?
O12 W5 O14 99.1(5) . 4 ?
O12 W5 O14 99.1(5) . . ?
O14 W5 O14 89.4(7) 4 . ?
O12 W5 O4 100.3(5) . . ?
O14 W5 O4 160.5(4) 4 . ?
O14 W5 O4 89.1(5) . . ?
O12 W5 O4 100.3(5) . 4 ?
O14 W5 O4 89.1(5) 4 4 ?
O14 W5 O4 160.5(4) . 4 ?
O4 W5 O4 85.9(6) . 4 ?
O12 W5 O13 170.8(7) . . ?
O14 W5 O13 74.5(4) 4 . ?
O14 W5 O13 74.5(4) . . ?
O4 W5 O13 86.4(3) . . ?
O4 W5 O13 86.4(3) 4 . ?
O16 W6 O17 102.9(5) . . ?
O16 W6 O7 99.9(5) . . ?
O17 W6 O7 93.0(4) . . ?
O16 W6 O15 103.0(5) . . ?
O17 W6 O15 87.3(6) . . ?
O7 W6 O15 156.4(4) . . ?
O16 W6 O14 100.2(5) . . ?
O17 W6 O14 156.1(5) . . ?
O7 W6 O14 89.2(5) . . ?
O15 W6 O14 81.4(6) . . ?
O16 W6 O13 171.7(5) . . ?
O17 W6 O13 84.6(5) . . ?
O7 W6 O13 83.2(3) . . ?
O15 W6 O13 73.3(3) . . ?
O14 W6 O13 72.0(5) . . ?
O17 W7 O17 87.8(7) . 4 ?
O17 W7 O18 103.8(7) . . ?
O17 W7 O18 103.8(7) 4 . ?
O17 W7 O19 158.5(5) . 4 ?
O17 W7 O19 88.4(4) 4 4 ?
O18 W7 O19 97.7(7) . 4 ?
O17 W7 O19 88.4(4) . . ?
O17 W7 O19 158.5(5) 4 . ?
O18 W7 O19 97.7(7) . . ?
O19 W7 O19 87.5(5) 4 . ?
W1 O2 W2 125.7(5) . . ?
W1 O2 W3 134.5(4) . . ?
W2 O2 W3 91.4(3) . . ?
W2 O3 W3 117.8(5) . . ?
W2 O4 W5 150.8(6) . . ?
W2 O5 W2 151.0(7) . 4 ?
W2 O6 W2 160.8(9) 3 . ?
W6 O7 W3 156.5(5) . . ?
W3 O8 W4 157.7(6) . . ?
N8 O10 W3 88(3) 6_655 3 ?
N8 O10 W3 88(3) 6_655 . ?
W3 O10 W3 148.8(8) 3 . ?
W5 O13 W6 96.1(3) . . ?
W5 O13 W6 96.1(3) . 4 ?
W6 O13 W6 93.7(4) . 4 ?
W5 O14 W6 117.5(5) . . ?
W6 O15 W6 117.4(5) 4 . ?
Cu/W7 O17 W6 146.5(7) . . ?
W4 O19 Cu/W7 147.1(7) . . ?
O10 N8 W3 66(5) 6_355 8_355 ?
O10 N8 W3 66(5) 6_355 6_355 ?
W3 N8 W3 123(8) 8_355 6_355 ?

_diffrn_measured_fraction_theta_max 0.964
_diffrn_reflns_theta_full        27.51
_diffrn_measured_fraction_theta_full 0.964
_refine_diff_density_max         1.178
_refine_diff_density_min         -1.013
_refine_diff_density_rms         0.202

loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
1 -0.031 0.094 0.101 1224.8 222.2
_platon_squeeze_details          
; ?
;