# Electronic Supplementary Material (ESI) for Dalton Transactions
# This journal is © The Royal Society of Chemistry 2013

#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
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# 
#  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
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data_global

data_1


_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C28 H24 Cd N8 O8'
_chemical_formula_weight         712.95

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'
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'
Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_H-M   I-42d

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'y, -x, -z'
'-x, -y, z'
'-y, x, -z'
'x, -y+1/2, -z+1/4'
'-x, y+1/2, -z+1/4'
'-y, -x+1/2, z+1/4'
'y, x+1/2, z+1/4'
'x+1/2, y+1/2, z+1/2'
'y+1/2, -x+1/2, -z+1/2'
'-x+1/2, -y+1/2, z+1/2'
'-y+1/2, x+1/2, -z+1/2'
'x+1/2, -y+1, -z+3/4'
'-x+1/2, y+1, -z+3/4'
'-y+1/2, -x+1, z+3/4'
'y+1/2, x+1, z+3/4'

_cell_length_a                   25.749(4)
_cell_length_b                   25.749(4)
_cell_length_c                   8.3921(17)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     5563.9(16)
_cell_formula_units_Z            8
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       ?
_exptl_crystal_colour            ?
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.15
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.702
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2880
_exptl_absorpt_coefficient_mu    0.853
_exptl_absorpt_correction_type   none
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_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  ?
_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            23147
_diffrn_reflns_av_R_equivalents  0.0622
_diffrn_reflns_av_sigmaI/netI    0.0350
_diffrn_reflns_limit_h_min       -33
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_theta_min         3.16
_diffrn_reflns_theta_max         27.50
_reflns_number_total             3201
_reflns_number_gt                3165
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_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^)+(0.0449P)^2^+20.9166P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.03(4)
_refine_ls_number_reflns         3201
_refine_ls_number_parameters     202
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0459
_refine_ls_R_factor_gt           0.0453
_refine_ls_wR_factor_ref         0.1060
_refine_ls_wR_factor_gt          0.1056
_refine_ls_goodness_of_fit_ref   1.157
_refine_ls_restrained_S_all      1.157
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Cd1 Cd -1.918932(16) -1.2500 -0.3750 0.01951(12) Uani 1 2 d S . .
O1 O -1.89451(14) -1.12976(13) 0.3753(6) 0.0368(8) Uani 1 1 d . . .
O2 O -1.94073(13) -1.20218(12) 0.3981(4) 0.0269(7) Uani 1 1 d . . .
O3 O -1.99771(15) -1.08832(17) 0.4496(4) 0.0438(10) Uani 1 1 d . . .
O4 O -2.0510(2) -1.0452(3) 0.2950(7) 0.0783(17) Uiso 1 1 d . . .
H4 H -2.0619 -1.0347 0.3809 0.117 Uiso 1 1 calc RD . .
N1 N -1.85043(17) -1.19950(18) -0.2767(5) 0.0292(9) Uani 1 1 d . . .
N2 N -1.83683(17) -1.15248(17) -0.3369(6) 0.0361(12) Uani 1 1 d . . .
H2 H -1.8554 -1.1353 -0.4038 0.043 Uiso 1 1 calc R . .
N3 N -1.97508(16) -1.19286(16) -0.2417(5) 0.0249(9) Uani 1 1 d . . .
N4 N -2.04209(17) -1.13826(17) -0.2414(5) 0.0280(9) Uani 1 1 d . . .
H4A H -2.0687 -1.1214 -0.2756 0.034 Uiso 1 1 calc R . .
C1 C -1.8143(2) -1.2617(2) -0.0864(8) 0.0496(18) Uani 1 1 d . . .
H1A H -1.8103 -1.2902 -0.1592 0.074 Uiso 1 1 calc R . .
H1B H -1.8470 -1.2646 -0.0324 0.074 Uiso 1 1 calc R . .
H1C H -1.7866 -1.2625 -0.0097 0.074 Uiso 1 1 calc R . .
C2 C -1.81248(19) -1.2119(2) -0.1760(6) 0.0300(11) Uani 1 1 d . . .
C3 C -1.77409(17) -1.17304(19) -0.1733(6) 0.0286(11) Uani 1 1 d . . .
C4 C -1.7909(2) -1.1357(2) -0.2799(9) 0.0406(15) Uani 1 1 d . . .
C5 C -1.7663(3) -1.0865(3) -0.3330(11) 0.073(3) Uani 1 1 d . . .
H5A H -1.7824 -1.0578 -0.2793 0.109 Uiso 1 1 calc R . .
H5B H -1.7708 -1.0827 -0.4460 0.109 Uiso 1 1 calc R . .
H5C H -1.7300 -1.0872 -0.3082 0.109 Uiso 1 1 calc R . .
C6 C -1.92972(17) -1.16043(17) 0.3322(5) 0.0197(9) Uani 1 1 d . . .
C7 C -1.96047(17) -1.14833(18) 0.1807(6) 0.0215(9) Uani 1 1 d . . .
C8 C -1.94813(18) -1.17735(18) 0.0465(6) 0.0240(9) Uani 1 1 d . . .
H8 H -1.9208 -1.2009 0.0479 0.029 Uiso 1 1 calc R . .
C9 C -1.97812(17) -1.17005(17) -0.0915(5) 0.0205(9) Uani 1 1 d . . .
C10 C -2.02015(18) -1.13554(19) -0.0906(5) 0.0234(9) Uani 1 1 d . . .
C11 C -2.0325(2) -1.1060(2) 0.0406(6) 0.0294(11) Uani 1 1 d . . .
H11 H -2.0602 -1.0828 0.0384 0.035 Uiso 1 1 calc R . .
C12 C -2.0022(2) -1.1120(2) 0.1768(6) 0.0261(10) Uani 1 1 d . . .
C13 C -2.01625(19) -1.0819(2) 0.3196(6) 0.0287(10) Uani 1 1 d . . .
C14 C -2.01350(19) -1.17246(19) -0.3225(6) 0.0248(10) Uani 1 1 d . . .
H14 H -2.0203 -1.1811 -0.4280 0.030 Uiso 1 1 calc R . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Cd1 0.0185(2) 0.0221(2) 0.01792(19) -0.00066(18) 0.000 0.000
O1 0.0380(18) 0.0333(17) 0.039(2) 0.015(2) -0.016(2) -0.0150(14)
O2 0.0339(17) 0.0260(16) 0.0209(18) 0.0074(14) -0.0087(14) -0.0057(13)
O3 0.058(3) 0.044(2) 0.030(2) -0.0115(19) -0.0152(19) 0.013(2)
N1 0.026(2) 0.034(2) 0.028(2) 0.0000(18) -0.0087(18) -0.0056(17)
N2 0.029(2) 0.031(2) 0.048(3) 0.009(2) -0.015(2) 0.0029(18)
N3 0.025(2) 0.027(2) 0.023(2) 0.0002(17) -0.0025(17) 0.0055(17)
N4 0.030(2) 0.035(2) 0.019(2) -0.0018(18) -0.0058(17) 0.0114(18)
C1 0.044(3) 0.051(4) 0.053(4) 0.021(3) -0.021(3) -0.013(3)
C2 0.024(2) 0.038(3) 0.027(2) -0.002(2) -0.0067(19) -0.003(2)
C3 0.019(2) 0.029(2) 0.038(3) -0.003(2) -0.013(2) -0.0022(18)
C4 0.027(3) 0.035(3) 0.060(4) 0.012(3) -0.016(3) -0.004(2)
C5 0.061(4) 0.049(4) 0.107(8) 0.042(4) -0.042(4) -0.022(3)
C6 0.023(2) 0.020(2) 0.015(2) 0.0021(15) 0.0034(16) 0.0040(16)
C7 0.023(2) 0.021(2) 0.020(2) 0.0004(17) -0.0014(17) -0.0007(17)
C8 0.023(2) 0.027(2) 0.022(2) 0.0036(19) -0.0059(19) 0.0063(19)
C9 0.022(2) 0.022(2) 0.018(2) 0.0011(16) -0.0022(16) 0.0014(16)
C10 0.027(2) 0.030(2) 0.013(2) 0.0009(17) 0.0007(17) 0.0067(18)
C11 0.025(2) 0.037(3) 0.026(3) -0.002(2) -0.004(2) 0.012(2)
C12 0.029(2) 0.032(2) 0.017(2) -0.0040(19) 0.0006(18) 0.006(2)
C13 0.031(2) 0.036(3) 0.020(2) 0.001(2) -0.0028(18) 0.010(2)
C14 0.028(2) 0.025(2) 0.021(2) -0.0030(18) -0.0015(18) 0.0021(18)

_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 O2 2.336(3) 1_554 ?
Cd1 O2 2.336(3) 5_525 ?
Cd1 N1 2.341(4) . ?
Cd1 N1 2.341(4) 5_524 ?
Cd1 N3 2.347(4) 5_524 ?
Cd1 N3 2.347(4) . ?
O1 C6 1.255(5) . ?
O2 C6 1.242(5) . ?
O2 Cd1 2.336(3) 1_556 ?
O3 C13 1.203(6) . ?
O4 C13 1.317(7) . ?
N1 C2 1.331(6) . ?
N1 N2 1.358(6) . ?
N2 C4 1.347(7) . ?
N3 C14 1.309(6) . ?
N3 C9 1.393(6) . ?
N4 C14 1.334(6) . ?
N4 C10 1.387(6) . ?
C1 C2 1.488(8) . ?
C2 C3 1.407(7) . ?
C3 C4 1.382(7) . ?
C3 C3 1.482(9) 14_144 ?
C4 C5 1.485(8) . ?
C6 C7 1.530(6) . ?
C7 C8 1.388(6) . ?
C7 C12 1.426(6) . ?
C8 C9 1.404(6) . ?
C9 C10 1.400(6) . ?
C10 C11 1.376(7) . ?
C11 C12 1.392(7) . ?
C12 C13 1.472(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
O2 Cd1 O2 152.19(17) 1_554 5_525 ?
O2 Cd1 N1 100.10(14) 1_554 . ?
O2 Cd1 N1 100.76(15) 5_525 . ?
O2 Cd1 N1 100.76(15) 1_554 5_524 ?
O2 Cd1 N1 100.10(14) 5_525 5_524 ?
N1 Cd1 N1 82.2(2) . 5_524 ?
O2 Cd1 N3 78.11(13) 1_554 5_524 ?
O2 Cd1 N3 84.83(14) 5_525 5_524 ?
N1 Cd1 N3 168.60(16) . 5_524 ?
N1 Cd1 N3 87.02(15) 5_524 5_524 ?
O2 Cd1 N3 84.83(14) 1_554 . ?
O2 Cd1 N3 78.11(13) 5_525 . ?
N1 Cd1 N3 87.02(15) . . ?
N1 Cd1 N3 168.60(16) 5_524 . ?
N3 Cd1 N3 103.9(2) 5_524 . ?
C6 O2 Cd1 139.9(3) . 1_556 ?
C2 N1 N2 105.1(4) . . ?
C2 N1 Cd1 130.1(4) . . ?
N2 N1 Cd1 124.0(3) . . ?
C4 N2 N1 112.4(4) . . ?
C14 N3 C9 104.9(4) . . ?
C14 N3 Cd1 118.1(3) . . ?
C9 N3 Cd1 136.9(3) . . ?
C14 N4 C10 105.9(4) . . ?
N1 C2 C3 110.8(5) . . ?
N1 C2 C1 120.3(5) . . ?
C3 C2 C1 128.8(5) . . ?
C4 C3 C2 105.3(4) . . ?
C4 C3 C3 128.0(4) . 14_144 ?
C2 C3 C3 126.7(4) . 14_144 ?
N2 C4 C3 106.3(5) . . ?
N2 C4 C5 122.7(5) . . ?
C3 C4 C5 130.9(5) . . ?
O2 C6 O1 125.5(4) . . ?
O2 C6 C7 115.4(4) . . ?
O1 C6 C7 119.0(4) . . ?
C8 C7 C12 120.5(4) . . ?
C8 C7 C6 116.5(4) . . ?
C12 C7 C6 122.9(4) . . ?
C7 C8 C9 118.1(4) . . ?
N3 C9 C10 108.4(4) . . ?
N3 C9 C8 131.2(4) . . ?
C10 C9 C8 120.4(4) . . ?
C11 C10 N4 131.6(4) . . ?
C11 C10 C9 122.2(4) . . ?
N4 C10 C9 106.2(4) . . ?
C10 C11 C12 117.8(4) . . ?
C11 C12 C7 120.9(4) . . ?
C11 C12 C13 118.2(4) . . ?
C7 C12 C13 120.8(4) . . ?
O3 C13 O4 120.7(5) . . ?
O3 C13 C12 124.7(5) . . ?
O4 C13 C12 114.6(5) . . ?
N3 C14 N4 114.7(4) . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O4 H4 O3 0.82 1.78 2.595(5) 170.6 2_426
N2 H2 O1 0.86 2.11 2.895(6) 150.8 1_554
N4 H4A O1 0.86 1.83 2.659(5) 161.9 2_425

_diffrn_measured_fraction_theta_max 0.997
_diffrn_reflns_theta_full        27.50
_diffrn_measured_fraction_theta_full 0.997
_refine_diff_density_max         1.216
_refine_diff_density_min         -0.816
_refine_diff_density_rms         0.089



_database_code_depnum_ccdc_archive 'CCDC 912974'