# 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
#  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_y

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C96 H72 Cd6 N4 O29'
_chemical_formula_weight         2419.98

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'
Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   C2/c

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                   19.524(4)
_cell_length_b                   10.049(2)
_cell_length_c                   25.359(5)
_cell_angle_alpha                90.00
_cell_angle_beta                 95.409(4)
_cell_angle_gamma                90.00
_cell_volume                     4953.2(17)
_cell_formula_units_Z            2
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    1076
_cell_measurement_theta_min      2.39
_cell_measurement_theta_max      20.05

_exptl_crystal_description       block
_exptl_crystal_colour            ?
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.20
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.623
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2392
_exptl_absorpt_coefficient_mu    1.343
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.7476
_exptl_absorpt_correction_T_max  0.7751
_exptl_absorpt_process_details   sadabs

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      296(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 5.0cm
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            17595
_diffrn_reflns_av_R_equivalents  0.1021
_diffrn_reflns_av_sigmaI/netI    0.1278
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_theta_min         1.61
_diffrn_reflns_theta_max         28.21
_reflns_number_total             6090
_reflns_number_gt                3121
_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 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)+(0.0913P)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         6090
_refine_ls_number_parameters     311
_refine_ls_number_restraints     7
_refine_ls_R_factor_all          0.1487
_refine_ls_R_factor_gt           0.0704
_refine_ls_wR_factor_ref         0.2050
_refine_ls_wR_factor_gt          0.1698
_refine_ls_goodness_of_fit_ref   1.013
_refine_ls_restrained_S_all      1.014
_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
Cd1 Cd 0.589277(18) 1.04870(3) 0.983691(14) 0.03959(9) Uani 1 1 d . . .
Cd2 Cd 0.7500 1.2500 1.0000 0.04276(14) Uani 1 2 d S . .
O1 O 0.68891(19) 1.1072(4) 0.94280(13) 0.0673(12) Uani 1 1 d . . .
O2 O 0.60674(19) 1.0125(5) 0.89424(14) 0.0700(13) Uani 1 1 d . . .
O3 O 1.02415(17) 0.5832(3) 0.54768(13) 0.0409(9) Uani 1 1 d . . .
O4 O 1.10823(17) 0.6675(3) 0.50662(13) 0.0467(10) Uani 1 1 d . . .
O5 O 1.07473(18) 1.2824(3) 0.53538(12) 0.0435(9) Uani 1 1 d . . .
O6 O 1.15180(16) 1.1438(4) 0.50677(14) 0.0522(10) Uani 1 1 d . . .
O7 O 0.7782(2) 1.4123(4) 0.94248(16) 0.0655(12) Uani 1 1 d . . .
C1 C 0.6659(2) 1.0598(5) 0.89936(18) 0.0382(13) Uani 1 1 d . . .
C2 C 0.7090(2) 1.0520(5) 0.85408(18) 0.0386(13) Uani 1 1 d . . .
C3 C 0.6864(3) 0.9852(6) 0.80831(18) 0.0510(16) Uani 1 1 d . . .
H3 H 0.6427 0.9475 0.8044 0.061 Uiso 1 1 calc R . .
C4 C 0.7292(3) 0.9748(6) 0.7683(2) 0.0488(16) Uani 1 1 d . . .
H4 H 0.7134 0.9303 0.7373 0.059 Uiso 1 1 calc R . .
C5 C 0.7954(3) 1.0286(5) 0.77246(18) 0.0417(14) Uani 1 1 d . . .
C6 C 0.8171(3) 1.0975(6) 0.8181(2) 0.0588(18) Uani 1 1 d . . .
H6 H 0.8604 1.1366 0.8218 0.071 Uiso 1 1 calc R . .
C7 C 0.7736(3) 1.1085(7) 0.8589(2) 0.065(2) Uani 1 1 d . . .
H7 H 0.7886 1.1546 0.8896 0.078 Uiso 1 1 calc R . .
C8 C 0.8416(2) 1.0147(5) 0.72875(19) 0.0441(14) Uani 1 1 d . . .
C9 C 0.8335(3) 0.9106(5) 0.6923(2) 0.0507(15) Uani 1 1 d . . .
H9 H 0.7975 0.8509 0.6943 0.061 Uiso 1 1 calc R . .
C10 C 0.8775(3) 0.8941(5) 0.65374(19) 0.0524(15) Uani 1 1 d . . .
H10 H 0.8716 0.8218 0.6308 0.063 Uiso 1 1 calc R . .
C11 C 0.9311(2) 0.9843(5) 0.64821(18) 0.0386(13) Uani 1 1 d . . .
C12 C 0.9360(3) 1.0876(5) 0.6838(2) 0.0536(16) Uani 1 1 d . . .
H12 H 0.9711 1.1492 0.6814 0.064 Uiso 1 1 calc R . .
C13 C 0.8926(3) 1.1064(5) 0.7229(2) 0.0474(15) Uani 1 1 d . . .
H13 H 0.8977 1.1802 0.7450 0.057 Uiso 1 1 calc R . .
C14 C 0.9813(2) 0.9634(5) 0.60852(17) 0.0327(12) Uani 1 1 d . . .
C15 C 0.9980(2) 0.8356(5) 0.59157(17) 0.0369(12) Uani 1 1 d . . .
H15 H 0.9766 0.7619 0.6049 0.044 Uiso 1 1 calc R . .
C16 C 1.0461(2) 0.8173(5) 0.55509(17) 0.0325(12) Uani 1 1 d . . .
C17 C 1.0797(2) 0.9259(4) 0.53749(18) 0.0342(12) Uani 1 1 d . . .
H17 H 1.1142 0.9134 0.5151 0.041 Uiso 1 1 calc R . .
C18 C 1.0636(2) 1.0539(5) 0.55232(17) 0.0310(11) Uani 1 1 d . . .
C19 C 1.0149(2) 1.0719(4) 0.58816(18) 0.0352(12) Uani 1 1 d . . .
H19 H 1.0045 1.1576 0.5988 0.042 Uiso 1 1 calc R . .
C20 C 1.0599(2) 0.6801(5) 0.53544(18) 0.0361(13) Uani 1 1 d . . .
C21 C 1.0993(2) 1.1707(5) 0.52976(18) 0.0360(12) Uani 1 1 d . . .
C22 C 0.7469(4) 1.5203(7) 0.9416(3) 0.085(2) Uani 1 1 d . . .
H22 H 0.7144 1.5331 0.9657 0.102 Uiso 1 1 calc R . .
N1 N 0.7573(2) 1.6175(5) 0.90845(18) 0.0673(17) Uani 1 1 d D . .
C23 C 0.7186(5) 1.7371(9) 0.9137(4) 0.134(4) Uani 1 1 d . . .
H23A H 0.6836 1.7215 0.9372 0.201 Uiso 1 1 calc R . .
H23B H 0.6975 1.7636 0.8796 0.201 Uiso 1 1 calc R . .
H23C H 0.7488 1.8064 0.9279 0.201 Uiso 1 1 calc R . .
C24 C 0.8023(3) 1.6275(11) 0.8704(2) 0.130(4) Uani 1 1 d D . .
H24A H 0.8288 1.5472 0.8697 0.195 Uiso 1 1 calc R . .
H24B H 0.8326 1.7016 0.8783 0.195 Uiso 1 1 calc R . .
H24C H 0.7771 1.6409 0.8364 0.195 Uiso 1 1 calc R . .
O1W O 0.0000 0.421(2) 0.2500 0.152(6) Uani 0.50 2 d SPU . .


_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
Cd1 O5 2.180(3) 8_476 ?
Cd1 O4 2.270(3) 8_466 ?
Cd1 O3 2.308(3) 4_656 ?
Cd1 O2 2.354(4) . ?
Cd1 O1 2.363(4) . ?
Cd1 O3 2.529(3) 8_466 ?
Cd1 C1 2.726(5) . ?
Cd1 C20 2.735(5) 8_466 ?
Cd2 O6 2.215(3) 2_756 ?
Cd2 O6 2.215(3) 8_476 ?
Cd2 O7 2.289(4) . ?
Cd2 O7 2.289(4) 7_677 ?
Cd2 O1 2.293(4) . ?
Cd2 O1 2.294(4) 7_677 ?
O1 C1 1.244(6) . ?
O2 C1 1.245(6) . ?
O3 C20 1.255(6) . ?
O3 Cd1 2.308(3) 4_646 ?
O3 Cd1 2.529(3) 8_565 ?
O4 C20 1.253(6) . ?
O4 Cd1 2.270(3) 8_565 ?
O5 C21 1.233(6) . ?
O5 Cd1 2.180(3) 8_575 ?
O6 C21 1.256(5) . ?
O6 Cd2 2.215(3) 2_756 ?
O7 C22 1.244(8) . ?
C1 C2 1.488(6) . ?
C2 C3 1.377(7) . ?
C2 C7 1.378(8) . ?
C3 C4 1.379(7) . ?
C3 H3 0.9300 . ?
C4 C5 1.396(7) . ?
C4 H4 0.9300 . ?
C5 C6 1.381(7) . ?
C5 C8 1.499(7) . ?
C6 C7 1.402(7) . ?
C6 H6 0.9300 . ?
C7 H7 0.9300 . ?
C8 C13 1.376(7) . ?
C8 C9 1.394(7) . ?
C9 C10 1.371(7) . ?
C9 H9 0.9300 . ?
C10 C11 1.403(7) . ?
C10 H10 0.9300 . ?
C11 C12 1.373(7) . ?
C11 C14 1.484(6) . ?
C12 C13 1.374(7) . ?
C12 H12 0.9300 . ?
C13 H13 0.9300 . ?
C14 C19 1.396(6) . ?
C14 C15 1.402(7) . ?
C15 C16 1.391(6) . ?
C15 H15 0.9300 . ?
C16 C17 1.370(6) . ?
C16 C20 1.499(6) . ?
C17 C18 1.385(6) . ?
C17 H17 0.9300 . ?
C18 C19 1.387(6) . ?
C18 C21 1.506(6) . ?
C19 H19 0.9300 . ?
C20 Cd1 2.735(5) 8_565 ?
C22 N1 1.317(8) . ?
C22 H22 0.9300 . ?
N1 C24 1.369(6) . ?
N1 C23 1.433(10) . ?
C23 H23A 0.9600 . ?
C23 H23B 0.9600 . ?
C23 H23C 0.9600 . ?
C24 H24A 0.9600 . ?
C24 H24B 0.9600 . ?
C24 H24C 0.9600 . ?

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 Cd1 O4 128.21(12) 8_476 8_466 ?
O5 Cd1 O3 85.13(12) 8_476 4_656 ?
O4 Cd1 O3 111.10(12) 8_466 4_656 ?
O5 Cd1 O2 137.65(15) 8_476 . ?
O4 Cd1 O2 93.66(15) 8_466 . ?
O3 Cd1 O2 84.98(12) 4_656 . ?
O5 Cd1 O1 103.27(14) 8_476 . ?
O4 Cd1 O1 103.26(14) 8_466 . ?
O3 Cd1 O1 127.89(12) 4_656 . ?
O2 Cd1 O1 54.24(13) . . ?
O5 Cd1 O3 85.43(11) 8_476 8_466 ?
O4 Cd1 O3 54.11(11) 8_466 8_466 ?
O3 Cd1 O3 77.04(12) 4_656 8_466 ?
O2 Cd1 O3 131.65(14) . 8_466 ?
O1 Cd1 O3 153.68(13) . 8_466 ?
O5 Cd1 C1 123.53(14) 8_476 . ?
O4 Cd1 C1 98.73(13) 8_466 . ?
O3 Cd1 C1 107.67(13) 4_656 . ?
O2 Cd1 C1 27.14(14) . . ?
O1 Cd1 C1 27.12(13) . . ?
O3 Cd1 C1 150.62(13) 8_466 . ?
O5 Cd1 C20 108.73(13) 8_476 8_466 ?
O4 Cd1 C20 27.00(13) 8_466 8_466 ?
O3 Cd1 C20 93.10(13) 4_656 8_466 ?
O2 Cd1 C20 112.85(16) . 8_466 ?
O1 Cd1 C20 129.65(15) . 8_466 ?
O3 Cd1 C20 27.22(12) 8_466 8_466 ?
C1 Cd1 C20 124.49(14) . 8_466 ?
O6 Cd2 O6 180.00(18) 2_756 8_476 ?
O6 Cd2 O7 91.84(13) 2_756 . ?
O6 Cd2 O7 88.15(13) 8_476 . ?
O6 Cd2 O7 88.15(13) 2_756 7_677 ?
O6 Cd2 O7 91.85(13) 8_476 7_677 ?
O7 Cd2 O7 180.000(1) . 7_677 ?
O6 Cd2 O1 92.98(14) 2_756 . ?
O6 Cd2 O1 87.02(14) 8_476 . ?
O7 Cd2 O1 100.63(14) . . ?
O7 Cd2 O1 79.37(14) 7_677 . ?
O6 Cd2 O1 87.02(14) 2_756 7_677 ?
O6 Cd2 O1 92.98(14) 8_476 7_677 ?
O7 Cd2 O1 79.37(14) . 7_677 ?
O7 Cd2 O1 100.63(14) 7_677 7_677 ?
O1 Cd2 O1 180.00(13) . 7_677 ?
C1 O1 Cd2 157.2(4) . . ?
C1 O1 Cd1 92.9(3) . . ?
Cd2 O1 Cd1 106.18(14) . . ?
C1 O2 Cd1 93.3(3) . . ?
C20 O3 Cd1 124.7(3) . 4_646 ?
C20 O3 Cd1 85.6(3) . 8_565 ?
Cd1 O3 Cd1 102.96(12) 4_646 8_565 ?
C20 O4 Cd1 97.6(3) . 8_565 ?
C21 O5 Cd1 124.4(3) . 8_575 ?
C21 O6 Cd2 133.1(3) . 2_756 ?
C22 O7 Cd2 119.1(4) . . ?
O1 C1 O2 119.5(4) . . ?
O1 C1 C2 121.4(4) . . ?
O2 C1 C2 119.1(4) . . ?
O1 C1 Cd1 60.0(3) . . ?
O2 C1 Cd1 59.6(2) . . ?
C2 C1 Cd1 174.5(3) . . ?
C3 C2 C7 119.6(5) . . ?
C3 C2 C1 121.1(4) . . ?
C7 C2 C1 119.3(4) . . ?
C2 C3 C4 119.3(5) . . ?
C2 C3 H3 120.4 . . ?
C4 C3 H3 120.4 . . ?
C3 C4 C5 122.4(5) . . ?
C3 C4 H4 118.8 . . ?
C5 C4 H4 118.8 . . ?
C6 C5 C4 117.8(5) . . ?
C6 C5 C8 120.6(5) . . ?
C4 C5 C8 121.6(4) . . ?
C5 C6 C7 119.9(5) . . ?
C5 C6 H6 120.0 . . ?
C7 C6 H6 120.0 . . ?
C2 C7 C6 121.0(5) . . ?
C2 C7 H7 119.5 . . ?
C6 C7 H7 119.5 . . ?
C13 C8 C9 117.9(5) . . ?
C13 C8 C5 120.7(5) . . ?
C9 C8 C5 121.4(5) . . ?
C10 C9 C8 121.6(5) . . ?
C10 C9 H9 119.2 . . ?
C8 C9 H9 119.2 . . ?
C9 C10 C11 121.1(5) . . ?
C9 C10 H10 119.4 . . ?
C11 C10 H10 119.4 . . ?
C12 C11 C10 115.4(4) . . ?
C12 C11 C14 123.0(4) . . ?
C10 C11 C14 121.6(4) . . ?
C11 C12 C13 124.7(5) . . ?
C11 C12 H12 117.7 . . ?
C13 C12 H12 117.7 . . ?
C12 C13 C8 119.2(5) . . ?
C12 C13 H13 120.4 . . ?
C8 C13 H13 120.4 . . ?
C19 C14 C15 118.1(4) . . ?
C19 C14 C11 120.2(4) . . ?
C15 C14 C11 121.7(4) . . ?
C16 C15 C14 121.1(4) . . ?
C16 C15 H15 119.5 . . ?
C14 C15 H15 119.5 . . ?
C17 C16 C15 119.1(4) . . ?
C17 C16 C20 121.2(4) . . ?
C15 C16 C20 119.8(4) . . ?
C16 C17 C18 121.5(4) . . ?
C16 C17 H17 119.2 . . ?
C18 C17 H17 119.2 . . ?
C17 C18 C19 119.1(4) . . ?
C17 C18 C21 119.7(4) . . ?
C19 C18 C21 121.2(4) . . ?
C18 C19 C14 121.0(4) . . ?
C18 C19 H19 119.5 . . ?
C14 C19 H19 119.5 . . ?
O4 C20 O3 122.2(4) . . ?
O4 C20 C16 117.1(4) . . ?
O3 C20 C16 120.6(4) . . ?
O4 C20 Cd1 55.4(2) . 8_565 ?
O3 C20 Cd1 67.2(2) . 8_565 ?
C16 C20 Cd1 170.1(3) . 8_565 ?
O5 C21 O6 126.4(4) . . ?
O5 C21 C18 117.8(4) . . ?
O6 C21 C18 115.9(4) . . ?
O7 C22 N1 123.6(6) . . ?
O7 C22 H22 118.2 . . ?
N1 C22 H22 118.2 . . ?
C22 N1 C24 130.8(7) . . ?
C22 N1 C23 116.6(6) . . ?
C24 N1 C23 112.5(7) . . ?
N1 C23 H23A 109.5 . . ?
N1 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
N1 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
N1 C24 H24A 109.5 . . ?
N1 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
N1 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?

_diffrn_measured_fraction_theta_max 0.996
_diffrn_reflns_theta_full        28.21
_diffrn_measured_fraction_theta_full 0.996
_refine_diff_density_max         1.612
_refine_diff_density_min         -1.183
_refine_diff_density_rms         0.182
_database_code_depnum_ccdc_archive 'CCDC 1014198'
