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

#######################################################################
#
#                 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
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# 
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#  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_b

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C54 H30 O20 Zn3, 6(O)'
_chemical_formula_sum            'C54 H30 O26 Zn3'
_chemical_formula_weight         1290.95

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'
Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Trigonal
_symmetry_space_group_name_H-M   P-31c

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

_cell_length_a                   16.6504(16)
_cell_length_b                   16.6504(16)
_cell_length_c                   14.521(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_volume                     3486.4(9)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    5312
_cell_measurement_theta_min      2.45
_cell_measurement_theta_max      24.76

_exptl_crystal_description       NEEDLE
_exptl_crystal_colour            YELLOW
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.15
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.230
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1304
_exptl_absorpt_coefficient_mu    1.094
_exptl_absorpt_correction_type   none
_exptl_absorpt_correction_T_min  0.7008
_exptl_absorpt_correction_T_max  0.8531
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  '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            17148
_diffrn_reflns_av_R_equivalents  0.0291
_diffrn_reflns_av_sigmaI/netI    0.0181
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         1.41
_diffrn_reflns_theta_max         25.01
_reflns_number_total             2060
_reflns_number_gt                1617
_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^)+(0.1473P)^2^+2.5095P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         2060
_refine_ls_number_parameters     128
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0792
_refine_ls_R_factor_gt           0.0658
_refine_ls_wR_factor_ref         0.2227
_refine_ls_wR_factor_gt          0.2014
_refine_ls_goodness_of_fit_ref   1.101
_refine_ls_restrained_S_all      1.101
_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
Zn1 Zn 0.3333 0.6667 0.2500 0.0422(4) Uani 1 6 d S . .
Zn2 Zn 0.3333 0.6667 0.00821(7) 0.0600(4) Uani 1 3 d S . .
O3 O 0.1828(2) 0.1334(2) 0.1405(2) 0.0635(9) Uani 1 1 d . . .
O1 O 0.3358(2) 0.5626(3) 0.1739(3) 0.0859(13) Uani 1 1 d . . .
O2 O 0.2870(3) 0.5383(2) 0.0297(3) 0.0786(11) Uani 1 1 d . . .
O4 O 0.3333 0.6667 -0.1281(7) 0.271(14) Uani 1 3 d S . .
C8 C 0.0898(3) 0.0691(3) 0.1338(3) 0.0476(9) Uani 1 1 d . . .
C9 C 0.0217(3) 0.0926(3) 0.1342(3) 0.0487(9) Uani 1 1 d . . .
H9 H 0.0360 0.1542 0.1347 0.058 Uiso 1 1 calc R . .
C3 C 0.2842(3) 0.3773(3) 0.1948(4) 0.0640(12) Uani 1 1 d . . .
H3 H 0.3142 0.4170 0.2440 0.077 Uiso 1 1 calc R . .
C5 C 0.2095(3) 0.2265(3) 0.1308(3) 0.0561(11) Uani 1 1 d . . .
C6 C 0.1957(3) 0.2599(3) 0.0505(3) 0.0663(13) Uani 1 1 d . . .
H6 H 0.1666 0.2202 0.0012 0.080 Uiso 1 1 calc R . .
C4 C 0.2551(3) 0.2841(3) 0.2024(3) 0.0635(12) Uani 1 1 d . . .
H4 H 0.2666 0.2609 0.2560 0.076 Uiso 1 1 calc R . .
C7 C 0.2249(4) 0.3522(3) 0.0429(4) 0.0650(12) Uani 1 1 d . . .
H7 H 0.2150 0.3753 -0.0116 0.078 Uiso 1 1 calc R . .
C2 C 0.2691(3) 0.4114(3) 0.1159(3) 0.0567(11) Uani 1 1 d . . .
C1 C 0.2993(3) 0.5119(3) 0.1064(4) 0.0677(14) Uani 1 1 d . . .
O5 O 0.515(3) 0.2575(15) 0.2500 0.86(7) Uani 1 2 d S . .
O6 O 1.0000 0.5000 0.0000 0.445(17) Uani 1 2 d S . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Zn1 0.0337(4) 0.0337(4) 0.0591(7) 0.000 0.000 0.0169(2)
Zn2 0.0568(5) 0.0568(5) 0.0666(7) 0.000 0.000 0.0284(2)
O3 0.0417(16) 0.0472(17) 0.096(2) -0.0004(15) -0.0074(15) 0.0183(13)
O1 0.070(2) 0.058(2) 0.133(4) -0.047(2) -0.030(2) 0.0349(18)
O2 0.077(2) 0.0493(19) 0.104(3) -0.0187(19) -0.012(2) 0.0272(17)
O4 0.38(2) 0.38(2) 0.063(7) 0.000 0.000 0.188(11)
C8 0.042(2) 0.048(2) 0.049(2) -0.0019(17) -0.0023(16) 0.0193(18)
C9 0.049(2) 0.042(2) 0.056(2) -0.0001(17) 0.0009(17) 0.0229(18)
C3 0.053(3) 0.057(3) 0.073(3) -0.023(2) -0.007(2) 0.021(2)
C5 0.039(2) 0.044(2) 0.079(3) -0.010(2) -0.001(2) 0.0167(18)
C6 0.071(3) 0.044(2) 0.070(3) -0.018(2) -0.014(2) 0.019(2)
C4 0.049(2) 0.066(3) 0.068(3) -0.006(2) -0.003(2) 0.024(2)
C7 0.069(3) 0.049(2) 0.071(3) -0.010(2) -0.010(2) 0.025(2)
C2 0.040(2) 0.045(2) 0.078(3) -0.017(2) 0.0002(19) 0.0170(18)
C1 0.042(2) 0.053(3) 0.109(4) -0.025(3) -0.008(3) 0.025(2)
O5 0.38(5) 1.09(14) 0.87(11) 0.55(11) 0.000 0.19(2)
O6 0.30(2) 0.212(16) 0.55(3) -0.25(2) -0.05(2) -0.071(15)

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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Zn1 O1 2.073(3) 4_665 ?
Zn1 O1 2.073(3) 5_565 ?
Zn1 O1 2.073(3) 2_665 ?
Zn1 O1 2.073(3) . ?
Zn1 O1 2.073(3) 6 ?
Zn1 O1 2.073(3) 3_565 ?
Zn2 O2 1.900(4) 2_665 ?
Zn2 O2 1.900(4) 3_565 ?
Zn2 O2 1.900(4) . ?
Zn2 O4 1.979(10) . ?
O3 C8 1.377(5) . ?
O3 C5 1.390(5) . ?
O1 C1 1.236(6) . ?
O2 C1 1.251(7) . ?
C8 C9 1.373(6) . ?
C8 C9 1.381(6) 3 ?
C9 C8 1.381(6) 2 ?
C9 H9 0.9300 . ?
C3 C2 1.357(7) . ?
C3 C4 1.381(7) . ?
C3 H3 0.9300 . ?
C5 C4 1.359(6) . ?
C5 C6 1.360(7) . ?
C6 C7 1.365(6) . ?
C6 H6 0.9300 . ?
C4 H4 0.9300 . ?
C7 C2 1.382(6) . ?
C7 H7 0.9300 . ?
C2 C1 1.494(7) . ?

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 Zn1 O1 94.22(18) 4_665 5_565 ?
O1 Zn1 O1 87.2(2) 4_665 2_665 ?
O1 Zn1 O1 84.4(2) 5_565 2_665 ?
O1 Zn1 O1 84.4(2) 4_665 . ?
O1 Zn1 O1 178.07(19) 5_565 . ?
O1 Zn1 O1 94.22(18) 2_665 . ?
O1 Zn1 O1 94.22(18) 4_665 6 ?
O1 Zn1 O1 94.22(18) 5_565 6 ?
O1 Zn1 O1 178.07(19) 2_665 6 ?
O1 Zn1 O1 87.2(2) . 6 ?
O1 Zn1 O1 178.07(19) 4_665 3_565 ?
O1 Zn1 O1 87.2(2) 5_565 3_565 ?
O1 Zn1 O1 94.22(18) 2_665 3_565 ?
O1 Zn1 O1 94.22(18) . 3_565 ?
O1 Zn1 O1 84.4(2) 6 3_565 ?
O2 Zn2 O2 117.36(7) 2_665 3_565 ?
O2 Zn2 O2 117.35(7) 2_665 . ?
O2 Zn2 O2 117.35(7) 3_565 . ?
O2 Zn2 O4 99.46(13) 2_665 . ?
O2 Zn2 O4 99.46(13) 3_565 . ?
O2 Zn2 O4 99.46(13) . . ?
C8 O3 C5 118.0(3) . . ?
C1 O1 Zn1 141.7(4) . . ?
C1 O2 Zn2 119.7(3) . . ?
C9 C8 O3 123.0(4) . . ?
C9 C8 C9 122.9(4) . 3 ?
O3 C8 C9 113.8(4) . 3 ?
C8 C9 C8 117.1(4) . 2 ?
C8 C9 H9 121.5 . . ?
C8 C9 H9 121.5 2 . ?
C2 C3 C4 120.2(4) . . ?
C2 C3 H3 119.9 . . ?
C4 C3 H3 119.9 . . ?
C4 C5 C6 121.1(4) . . ?
C4 C5 O3 117.6(4) . . ?
C6 C5 O3 121.2(4) . . ?
C5 C6 C7 119.5(4) . . ?
C5 C6 H6 120.3 . . ?
C7 C6 H6 120.3 . . ?
C5 C4 C3 119.3(5) . . ?
C5 C4 H4 120.3 . . ?
C3 C4 H4 120.3 . . ?
C6 C7 C2 120.2(5) . . ?
C6 C7 H7 119.9 . . ?
C2 C7 H7 119.9 . . ?
C3 C2 C7 119.6(4) . . ?
C3 C2 C1 121.1(4) . . ?
C7 C2 C1 119.3(5) . . ?
O1 C1 O2 125.2(5) . . ?
O1 C1 C2 117.8(6) . . ?
O2 C1 C2 116.9(4) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O1 Zn1 O1 C1 -178.5(8) 4_665 . . . ?
O1 Zn1 O1 C1 -135.0(7) 5_565 . . . ?
O1 Zn1 O1 C1 -91.7(6) 2_665 . . . ?
O1 Zn1 O1 C1 87.0(7) 6 . . . ?
O1 Zn1 O1 C1 2.8(7) 3_565 . . . ?
O2 Zn2 O2 C1 54.8(5) 2_665 . . . ?
O2 Zn2 O2 C1 -93.4(4) 3_565 . . . ?
O4 Zn2 O2 C1 160.7(4) . . . . ?
C5 O3 C8 C9 -11.6(6) . . . . ?
C5 O3 C8 C9 173.3(4) . . . 3 ?
O3 C8 C9 C8 -175.4(2) . . . 2 ?
C9 C8 C9 C8 -0.8(9) 3 . . 2 ?
C8 O3 C5 C4 120.7(4) . . . . ?
C8 O3 C5 C6 -63.4(6) . . . . ?
C4 C5 C6 C7 -2.6(7) . . . . ?
O3 C5 C6 C7 -178.4(4) . . . . ?
C6 C5 C4 C3 2.9(7) . . . . ?
O3 C5 C4 C3 178.9(4) . . . . ?
C2 C3 C4 C5 -1.4(7) . . . . ?
C5 C6 C7 C2 0.8(8) . . . . ?
C4 C3 C2 C7 -0.3(7) . . . . ?
C4 C3 C2 C1 179.5(4) . . . . ?
C6 C7 C2 C3 0.7(7) . . . . ?
C6 C7 C2 C1 -179.1(5) . . . . ?
Zn1 O1 C1 O2 46.8(9) . . . . ?
Zn1 O1 C1 C2 -134.7(5) . . . . ?
Zn2 O2 C1 O1 4.2(7) . . . . ?
Zn2 O2 C1 C2 -174.4(3) . . . . ?
C3 C2 C1 O1 -2.3(7) . . . . ?
C7 C2 C1 O1 177.5(4) . . . . ?
C3 C2 C1 O2 176.4(4) . . . . ?
C7 C2 C1 O2 -3.8(7) . . . . ?

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        25.01
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         0.853
_refine_diff_density_min         -0.292
_refine_diff_density_rms         0.153
_database_code_depnum_ccdc_archive 'CCDC 971950'