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

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#                                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_1

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C15 H20 N6 O5 Zn'
_chemical_formula_weight         429.74

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'
Zn Zn 0.2839 1.4301 '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           Tetragonal
_symmetry_space_group_name_H-M   'I4(1)/a  '
_symmetry_space_group_name_Hall  '-I 4ad'

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-y+3/4, x+1/4, z+1/4'
'y+3/4, -x+3/4, z+3/4'
'x+1/2, y+1/2, z+1/2'
'-x+1, -y+1/2, z+1'
'-y+5/4, x+3/4, z+3/4'
'y+5/4, -x+5/4, z+5/4'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'y-3/4, -x-1/4, -z-1/4'
'-y-3/4, x-3/4, -z-3/4'
'-x+1/2, -y+1/2, -z+1/2'
'x, y+1/2, -z'
'y-1/4, -x+1/4, -z+1/4'
'-y-1/4, x-1/4, -z-1/4'

_cell_length_a                   23.4346(12)
_cell_length_b                   23.4346(12)
_cell_length_c                   14.9150(15)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     8191.0(10)
_cell_formula_units_Z            16
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    3665
_cell_measurement_theta_min      2.37
_cell_measurement_theta_max      26.58

_exptl_crystal_description       octahedral
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.16
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.394
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             3552
_exptl_absorpt_coefficient_mu    1.236
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.7759
_exptl_absorpt_correction_T_max  0.8293
_exptl_absorpt_process_details   'SADABS; Brucker, 2000'

_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_decay_%        ?
_diffrn_reflns_number            20027
_diffrn_reflns_av_R_equivalents  0.1066
_diffrn_reflns_av_unetI/netI     0.0641
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         1.62
_diffrn_reflns_theta_max         25.00
_reflns_number_total             3602
_reflns_number_gt                2919
_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          
; 

 The following restraints were generated by SHELX. 
 DFIX for N5-H bond (0.90)
 FLAT for H C14 N5 C9.

 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^)+(0.0388P)^2^+0.0000P] 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         3602
_refine_ls_number_parameters     203
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0537
_refine_ls_R_factor_gt           0.0416
_refine_ls_wR_factor_ref         0.0956
_refine_ls_wR_factor_gt          0.0917
_refine_ls_goodness_of_fit_ref   0.998
_refine_ls_restrained_S_all      0.998
_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
Zn1 Zn 0.375758(14) 1.047272(15) 1.15967(2) 0.02237(13) Uani 1 1 d . . .
N1 N 0.35815(10) 0.96652(10) 1.19511(16) 0.0269(6) Uani 1 1 d . . .
N2 N 0.32072(10) 0.90392(10) 1.29173(15) 0.0242(6) Uani 1 1 d . . .
N3 N 0.19182(10) 0.87030(11) 0.88460(17) 0.0286(6) Uani 1 1 d . . .
N4 N 0.16938(10) 0.91103(10) 0.75414(15) 0.0252(6) Uani 1 1 d . . .
N5 N 0.45406(11) 0.93264(12) 0.77357(17) 0.0314(6) Uani 1 1 d D . .
H H 0.4290(18) 0.9327(18) 0.727(2) 0.15(2) Uiso 1 1 d D . .
N6 N 0.54150(10) 0.93725(11) 0.82949(16) 0.0305(6) Uani 1 1 d . . .
C1 C 0.34014(12) 0.91666(12) 1.04850(19) 0.0233(7) Uani 1 1 d . . .
C2 C 0.29085(12) 0.90662(13) 0.99919(19) 0.0256(7) Uani 1 1 d . . .
H2 H 0.2562 0.9024 1.0288 0.031 Uiso 1 1 calc R . .
C3 C 0.29262(12) 0.90273(12) 0.90641(18) 0.0219(6) Uani 1 1 d . . .
C4 C 0.34505(12) 0.90698(12) 0.86329(19) 0.0235(7) Uani 1 1 d . . .
H4 H 0.3468 0.9023 0.8014 0.028 Uiso 1 1 calc R . .
C5 C 0.39480(12) 0.91812(13) 0.91076(19) 0.0228(7) Uani 1 1 d . . .
C6 C 0.39145(12) 0.92347(12) 1.00375(19) 0.0250(7) Uani 1 1 d . . .
H6 H 0.4243 0.9318 1.0363 0.030 Uiso 1 1 calc R . .
C7 C 0.33683(12) 0.92099(12) 1.14707(19) 0.0238(7) Uani 1 1 d . . .
C8 C 0.23973(12) 0.89811(12) 0.85370(18) 0.0223(7) Uani 1 1 d . . .
C9 C 0.44950(12) 0.92600(13) 0.86478(19) 0.0244(7) Uani 1 1 d D . .
C10 C 0.31406(13) 0.88357(13) 1.2066(2) 0.0283(7) Uani 1 1 d . . .
H10 H 0.2966 0.8492 1.1917 0.034 Uiso 1 1 calc R . .
C11 C 0.34698(13) 0.95347(13) 1.2801(2) 0.0298(7) Uani 1 1 d . . .
H11 H 0.3568 0.9772 1.3276 0.036 Uiso 1 1 calc R . .
C12 C 0.15127(13) 0.87926(13) 0.8226(2) 0.0306(8) Uani 1 1 d . . .
H12 H 0.1144 0.8648 0.8270 0.037 Uiso 1 1 calc R . .
C13 C 0.22558(12) 0.92256(13) 0.77450(19) 0.0286(7) Uani 1 1 d . . .
H13 H 0.2502 0.9440 0.7390 0.034 Uiso 1 1 calc R . .
C14 C 0.50961(13) 0.93953(14) 0.7569(2) 0.0332(8) Uani 1 1 d D . .
H14 H 0.5243 0.9453 0.6997 0.040 Uiso 1 1 calc R . .
C15 C 0.50308(12) 0.92901(14) 0.8985(2) 0.0310(8) Uani 1 1 d . . .
H15 H 0.5125 0.9260 0.9589 0.037 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
Zn1 0.0185(2) 0.0306(2) 0.0181(2) 0.00118(15) 0.00101(14) -0.00141(15)
N1 0.0313(15) 0.0287(14) 0.0207(14) 0.0035(11) -0.0007(11) -0.0051(12)
N2 0.0307(14) 0.0270(14) 0.0149(13) 0.0025(11) -0.0007(11) -0.0037(12)
N3 0.0240(14) 0.0337(15) 0.0281(14) 0.0052(12) -0.0041(12) -0.0059(12)
N4 0.0175(13) 0.0346(15) 0.0235(14) 0.0055(12) -0.0065(11) 0.0002(11)
N5 0.0206(14) 0.0507(18) 0.0227(15) 0.0043(13) 0.0016(12) -0.0002(13)
N6 0.0179(13) 0.0449(17) 0.0288(15) 0.0043(13) 0.0000(11) -0.0022(12)
C1 0.0247(16) 0.0238(16) 0.0213(16) 0.0031(13) -0.0043(13) -0.0005(13)
C2 0.0207(15) 0.0338(18) 0.0223(17) 0.0002(14) 0.0037(13) -0.0021(14)
C3 0.0225(15) 0.0218(15) 0.0213(16) 0.0023(13) -0.0012(13) -0.0016(13)
C4 0.0236(16) 0.0277(17) 0.0193(15) 0.0011(13) 0.0013(13) 0.0010(14)
C5 0.0178(15) 0.0299(17) 0.0206(16) -0.0016(13) 0.0033(12) 0.0020(13)
C6 0.0203(16) 0.0301(17) 0.0245(17) -0.0011(13) -0.0028(13) -0.0022(14)
C7 0.0197(15) 0.0304(17) 0.0212(16) -0.0005(13) 0.0005(13) -0.0002(14)
C8 0.0185(15) 0.0280(17) 0.0204(16) -0.0006(13) 0.0019(12) -0.0016(13)
C9 0.0232(16) 0.0305(17) 0.0196(16) -0.0011(13) 0.0001(13) -0.0018(14)
C10 0.0281(17) 0.0321(18) 0.0245(17) 0.0009(14) -0.0026(14) -0.0068(14)
C11 0.0359(19) 0.0330(18) 0.0204(17) 0.0023(14) -0.0040(14) -0.0049(15)
C12 0.0221(17) 0.0348(19) 0.0351(19) 0.0058(15) -0.0032(14) -0.0051(15)
C13 0.0214(16) 0.0380(19) 0.0263(17) 0.0048(15) -0.0013(14) -0.0061(15)
C14 0.0271(18) 0.052(2) 0.0207(17) 0.0030(15) 0.0048(14) -0.0015(16)
C15 0.0201(16) 0.054(2) 0.0189(16) 0.0027(15) 0.0005(13) -0.0038(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 N2 1.970(2) 7_554 ?
Zn1 N6 1.979(2) 9_677 ?
Zn1 N1 2.008(2) . ?
Zn1 N4 2.015(2) 2_575 ?
N1 C11 1.330(4) . ?
N1 C7 1.379(4) . ?
N2 C11 1.326(4) . ?
N2 C10 1.365(4) . ?
N2 Zn1 1.970(2) 8_354 ?
N3 C12 1.342(4) . ?
N3 C8 1.378(4) . ?
N4 C12 1.333(4) . ?
N4 C13 1.378(3) . ?
N4 Zn1 2.015(2) 2_574 ?
N5 C14 1.335(4) . ?
N5 C9 1.373(4) . ?
N5 H 0.907(10) . ?
N6 C14 1.317(4) . ?
N6 C15 1.381(3) . ?
N6 Zn1 1.979(2) 9_677 ?
C1 C6 1.384(4) . ?
C1 C2 1.390(4) . ?
C1 C7 1.476(4) . ?
C2 C3 1.387(4) . ?
C2 H2 0.9300 . ?
C3 C4 1.391(4) . ?
C3 C8 1.472(4) . ?
C4 C5 1.389(4) . ?
C4 H4 0.9300 . ?
C5 C6 1.395(4) . ?
C5 C9 1.465(4) . ?
C6 H6 0.9300 . ?
C7 C10 1.358(4) . ?
C8 C13 1.354(4) . ?
C9 C15 1.354(4) . ?
C10 H10 0.9300 . ?
C11 H11 0.9300 . ?
C12 H12 0.9300 . ?
C13 H13 0.9300 . ?
C14 H14 0.9300 . ?
C15 H15 0.9300 . ?

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
N2 Zn1 N6 111.57(10) 7_554 9_677 ?
N2 Zn1 N1 115.18(10) 7_554 . ?
N6 Zn1 N1 110.64(10) 9_677 . ?
N2 Zn1 N4 107.69(10) 7_554 2_575 ?
N6 Zn1 N4 111.62(10) 9_677 2_575 ?
N1 Zn1 N4 99.51(10) . 2_575 ?
C11 N1 C7 104.2(2) . . ?
C11 N1 Zn1 120.5(2) . . ?
C7 N1 Zn1 131.84(19) . . ?
C11 N2 C10 103.8(2) . . ?
C11 N2 Zn1 123.7(2) . 8_354 ?
C10 N2 Zn1 132.5(2) . 8_354 ?
C12 N3 C8 105.8(2) . . ?
C12 N4 C13 104.2(2) . . ?
C12 N4 Zn1 129.7(2) . 2_574 ?
C13 N4 Zn1 124.11(19) . 2_574 ?
C14 N5 C9 105.9(3) . . ?
C14 N5 H 119(4) . . ?
C9 N5 H 135(4) . . ?
C14 N6 C15 104.4(2) . . ?
C14 N6 Zn1 128.0(2) . 9_677 ?
C15 N6 Zn1 127.1(2) . 9_677 ?
C6 C1 C2 119.1(3) . . ?
C6 C1 C7 121.2(3) . . ?
C2 C1 C7 119.7(3) . . ?
C3 C2 C1 120.9(3) . . ?
C3 C2 H2 119.5 . . ?
C1 C2 H2 119.5 . . ?
C2 C3 C4 118.9(3) . . ?
C2 C3 C8 120.8(3) . . ?
C4 C3 C8 120.2(2) . . ?
C5 C4 C3 121.3(3) . . ?
C5 C4 H4 119.3 . . ?
C3 C4 H4 119.3 . . ?
C4 C5 C6 118.5(3) . . ?
C4 C5 C9 121.3(2) . . ?
C6 C5 C9 120.2(3) . . ?
C1 C6 C5 121.2(3) . . ?
C1 C6 H6 119.4 . . ?
C5 C6 H6 119.4 . . ?
C10 C7 N1 107.6(3) . . ?
C10 C7 C1 128.9(3) . . ?
N1 C7 C1 123.5(3) . . ?
C13 C8 N3 107.0(3) . . ?
C13 C8 C3 129.9(3) . . ?
N3 C8 C3 122.8(2) . . ?
C15 C9 N5 106.9(3) . . ?
C15 C9 C5 130.1(3) . . ?
N5 C9 C5 123.1(3) . . ?
C7 C10 N2 109.8(3) . . ?
C7 C10 H10 125.1 . . ?
N2 C10 H10 125.1 . . ?
N2 C11 N1 114.7(3) . . ?
N2 C11 H11 122.7 . . ?
N1 C11 H11 122.7 . . ?
N4 C12 N3 112.9(3) . . ?
N4 C12 H12 123.5 . . ?
N3 C12 H12 123.5 . . ?
C8 C13 N4 110.1(3) . . ?
C8 C13 H13 125.0 . . ?
N4 C13 H13 125.0 . . ?
N6 C14 N5 113.3(3) . . ?
N6 C14 H14 123.4 . . ?
N5 C14 H14 123.4 . . ?
C9 C15 N6 109.5(3) . . ?
C9 C15 H15 125.2 . . ?
N6 C15 H15 125.2 . . ?

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
N2 Zn1 N1 C11 -143.9(2) 7_554 . . . ?
N6 Zn1 N1 C11 88.4(2) 9_677 . . . ?
N4 Zn1 N1 C11 -29.1(2) 2_575 . . . ?
N2 Zn1 N1 C7 11.8(3) 7_554 . . . ?
N6 Zn1 N1 C7 -115.9(3) 9_677 . . . ?
N4 Zn1 N1 C7 126.6(3) 2_575 . . . ?
C6 C1 C2 C3 0.7(4) . . . . ?
C7 C1 C2 C3 179.6(3) . . . . ?
C1 C2 C3 C4 2.3(4) . . . . ?
C1 C2 C3 C8 -173.5(3) . . . . ?
C2 C3 C4 C5 -3.6(4) . . . . ?
C8 C3 C4 C5 172.3(3) . . . . ?
C3 C4 C5 C6 1.8(4) . . . . ?
C3 C4 C5 C9 -176.3(3) . . . . ?
C2 C1 C6 C5 -2.6(4) . . . . ?
C7 C1 C6 C5 178.6(3) . . . . ?
C4 C5 C6 C1 1.4(4) . . . . ?
C9 C5 C6 C1 179.5(3) . . . . ?
C11 N1 C7 C10 0.2(3) . . . . ?
Zn1 N1 C7 C10 -158.4(2) . . . . ?
C11 N1 C7 C1 -179.5(3) . . . . ?
Zn1 N1 C7 C1 21.9(4) . . . . ?
C6 C1 C7 C10 -127.6(3) . . . . ?
C2 C1 C7 C10 53.6(5) . . . . ?
C6 C1 C7 N1 52.0(4) . . . . ?
C2 C1 C7 N1 -126.8(3) . . . . ?
C12 N3 C8 C13 0.1(3) . . . . ?
C12 N3 C8 C3 174.6(3) . . . . ?
C2 C3 C8 C13 140.2(3) . . . . ?
C4 C3 C8 C13 -35.6(5) . . . . ?
C2 C3 C8 N3 -33.0(4) . . . . ?
C4 C3 C8 N3 151.2(3) . . . . ?
C14 N5 C9 C15 -0.3(4) . . . . ?
C14 N5 C9 C5 179.0(3) . . . . ?
C4 C5 C9 C15 -169.5(3) . . . . ?
C6 C5 C9 C15 12.5(5) . . . . ?
C4 C5 C9 N5 11.4(5) . . . . ?
C6 C5 C9 N5 -166.6(3) . . . . ?
N1 C7 C10 N2 -0.5(3) . . . . ?
C1 C7 C10 N2 179.2(3) . . . . ?
C11 N2 C10 C7 0.6(3) . . . . ?
Zn1 N2 C10 C7 178.4(2) 8_354 . . . ?
C10 N2 C11 N1 -0.5(4) . . . . ?
Zn1 N2 C11 N1 -178.58(19) 8_354 . . . ?
C7 N1 C11 N2 0.2(4) . . . . ?
Zn1 N1 C11 N2 161.8(2) . . . . ?
C13 N4 C12 N3 0.4(4) . . . . ?
Zn1 N4 C12 N3 -163.8(2) 2_574 . . . ?
C8 N3 C12 N4 -0.3(4) . . . . ?
N3 C8 C13 N4 0.1(3) . . . . ?
C3 C8 C13 N4 -173.9(3) . . . . ?
C12 N4 C13 C8 -0.3(3) . . . . ?
Zn1 N4 C13 C8 165.1(2) 2_574 . . . ?
C15 N6 C14 N5 -0.9(4) . . . . ?
Zn1 N6 C14 N5 -173.2(2) 9_677 . . . ?
C9 N5 C14 N6 0.7(4) . . . . ?
N5 C9 C15 N6 -0.3(4) . . . . ?
C5 C9 C15 N6 -179.5(3) . . . . ?
C14 N6 C15 C9 0.7(4) . . . . ?
Zn1 N6 C15 C9 173.1(2) 9_677 . . . ?

# SQUEEZE RESULTS (APPEND TO CIF)
# Note: Data are Listed for all Voids in the P1 Unit Cell
# i.e. Centre of Gravity, Solvent Accessible Volume,
# Recovered number of Electrons in the Void and
# Details about the Squeezed Material

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 -0.015 -0.001 -0.010 3494.4 787.4

_platon_squeeze_details          
;
Calculations from SQUEEZE routine from Platon indicated large solvent 
accessible voids accounting for 42.5% of the unit-cell volume 
(voids measuring 3481 \%A3 with 787.4 electrons each unit cell). The diffuse 
electron density was treated with the SQUEEZE routine from the PLATON
software package. Because these guest solvents in the crystal is highly
disordered and impossible to refine using conventional discrete-atom models,
we were unable to identify or model specific solvent molecules within the 
voids. The analysis showed that the void was occupied by 49.21(787.4/16) 
electrons per formula, corresponding to five water molecules.
;

_diffrn_measured_fraction_theta_max 1.000
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 1.000
_refine_diff_density_max         0.483
_refine_diff_density_min         -0.303
_refine_diff_density_rms         0.065
_database_code_depnum_ccdc_archive 'CCDC 974506'
#######################################################################
#
#                 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_2
_audit_creation_date             2013-12-19
_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
;
'C30 H42 Cd Cl2 N12 O18.50'
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C30 H42 Cd Cl2 N12 O18.50'
_chemical_formula_sum            'C30 H42 Cd Cl2 N12 O18.50'
_chemical_formula_weight         1050.05

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'
Cl Cl 0.1484 0.1585 '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'

_space_group_crystal_system      cubic
_space_group_IT_number           205
_space_group_name_H-M_alt        'P a -3'
_space_group_name_Hall           '-P 2ac 2ab 3'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

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

_cell_length_a                   17.542(5)
_cell_length_b                   17.542(5)
_cell_length_c                   17.542(5)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     5398(5)
_cell_formula_units_Z            4
_cell_measurement_temperature    200
_cell_measurement_reflns_used    14861
_cell_measurement_theta_min      3.3
_cell_measurement_theta_max      27.5

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.292
_exptl_crystal_F_000             2144
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.250
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.200
_exptl_absorpt_coefficient_mu    0.574
_shelx_estimated_absorpt_T_min   0.870
_shelx_estimated_absorpt_T_max   0.894
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.8719
_exptl_absorpt_correction_T_max  0.8956
_exptl_absorpt_process_details   
;
    Higashi, T. (1995). Program for Absorption Correction.
    Rigaku Corporation, Tokyo, Japan.
;
_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      200
_diffrn_radiation_wavelength     0.71075
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Rigaku RAXIS-RAPID'
_diffrn_measurement_method       \w
_diffrn_detector_area_resol_mean 10.00
_diffrn_reflns_number            37771
_diffrn_reflns_av_unetI/netI     0.0313
_diffrn_reflns_av_R_equivalents  0.1075
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         3.285
_diffrn_reflns_theta_max         24.995
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measured_fraction_theta_full 0.968
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_Laue_measured_fraction_full 0.968
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_point_group_measured_fraction_full 0.968
_reflns_number_total             1586
_reflns_number_gt                1082
_reflns_threshold_expression     'I > 2\s(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.

 The following restraints were generated by SHELX. 
 ISOR for O1, O2, O3, O11, O12, O13, O14, CL1 CL1B; 
 SADI for O...O distances among O11, O12, O13, O14, and O14B;
 DFIX for CL-O (O11-O14, Cl1, Cl1B) bonds (1.42).
;

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
;
 ?
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[\s^2^(Fo^2^)+(0.1153P)^2^+9.8220P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         1586
_refine_ls_number_parameters     151
_refine_ls_number_restraints     86
_refine_ls_R_factor_all          0.1010
_refine_ls_R_factor_gt           0.0705
_refine_ls_wR_factor_ref         0.2183
_refine_ls_wR_factor_gt          0.1981
_refine_ls_goodness_of_fit_ref   1.092
_refine_ls_restrained_S_all      1.115
_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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Cd1 Cd 0.5000 0.5000 0.0000 0.0382(4) Uani 1 6 d S T P . .
N11 N 0.5416(4) 0.6522(4) 0.1997(3) 0.092(2) Uani 1 1 d . . . . .
H2 H 0.5280 0.6706 0.2444 0.111 Uiso 1 1 calc R U . . .
N12 N 0.5420(2) 0.5794(2) 0.0984(2) 0.0452(11) Uani 1 1 d . . . . .
C1 C 0.6447(3) 0.7467(3) 0.1728(3) 0.0577(15) Uani 1 1 d . . . . .
C2 C 0.6281(3) 0.7922(3) 0.2359(3) 0.0577(15) Uani 1 1 d . . . . .
H1 H 0.5858 0.7799 0.2674 0.069 Uiso 1 1 calc R U . . .
C11 C 0.5979(3) 0.6801(3) 0.1542(3) 0.0521(14) Uani 1 1 d . . . . .
C12 C 0.5961(3) 0.6345(3) 0.0919(3) 0.0513(14) Uani 1 1 d . . . . .
H3 H 0.6286 0.6403 0.0490 0.062 Uiso 1 1 calc R U . . .
C13 C 0.5105(4) 0.5915(4) 0.1644(4) 0.076(2) Uani 1 1 d . . . . .
H4 H 0.4705 0.5614 0.1850 0.091 Uiso 1 1 calc R U . . .
Cl1 Cl 0.8390(11) 0.6004(10) 0.1789(12) 0.263(12) Uani 0.250(7) 1 d D U P . .
Cl1B Cl 0.8411(10) 0.5704(10) 0.1353(13) 0.087(10) Uani 0.084(7) 1 d D U P . .
O11 O 0.8615(14) 0.6451(13) 0.1145(17) 0.229(15) Uani 0.3333 1 d D U P . .
O12 O 0.8935(12) 0.5410(15) 0.1897(18) 0.235(14) Uani 0.3333 1 d D U P . .
O13 O 0.7663(10) 0.5679(14) 0.1657(19) 0.197(11) Uani 0.3333 1 d D U P . .
O14 O 0.837(2) 0.648(2) 0.2446(17) 0.30(3) Uani 0.250(7) 1 d D U P . .
O14B O 0.844(2) 0.523(2) 0.0696(19) 0.8(5) Uani 0.084(7) 1 d D U P . .
O1 O 0.8138(18) 0.6862(18) 0.3138(18) 0.169(17) Uani 0.25(2) 3 d S TU P . .
O2 O 0.6712(10) 0.5325(10) 0.2801(9) 0.344(10) Uani 1 1 d . U . . .
O3 O 0.553(2) 0.413(2) 0.319(2) 0.387(18) Uani 0.6667 1 d . U P . .

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 0.0382(4) 0.0382(4) 0.0382(4) 0.0011(2) -0.0011(2) -0.0011(2)
N11 0.110(5) 0.097(4) 0.070(4) -0.036(3) 0.036(3) -0.057(4)
N12 0.044(3) 0.048(3) 0.044(3) -0.003(2) 0.000(2) -0.004(2)
C1 0.058(3) 0.055(3) 0.060(4) -0.006(3) 0.008(3) -0.013(3)
C2 0.050(3) 0.064(4) 0.059(4) -0.011(3) 0.016(3) -0.011(3)
C11 0.053(3) 0.056(3) 0.048(3) -0.012(3) 0.010(3) -0.012(3)
C12 0.049(3) 0.058(3) 0.047(3) -0.004(3) 0.009(3) -0.013(3)
C13 0.083(5) 0.081(5) 0.065(4) -0.019(4) 0.023(4) -0.044(4)
Cl1 0.291(19) 0.241(18) 0.256(19) 0.026(16) -0.068(15) 0.057(16)
Cl1B 0.088(14) 0.041(11) 0.132(18) 0.019(11) -0.028(12) -0.023(9)
O11 0.23(2) 0.20(2) 0.26(2) 0.067(17) 0.018(17) -0.010(17)
O12 0.22(2) 0.23(2) 0.26(2) 0.046(18) -0.045(17) -0.007(18)
O13 0.174(18) 0.164(17) 0.25(2) 0.038(16) -0.013(16) 0.033(15)
O14 0.30(3) 0.30(3) 0.28(3) 0.01(2) -0.02(2) 0.03(2)
O14B 0.8(5) 0.8(5) 0.8(5) 0.00(2) 0.00(2) 0.00(2)
O1 0.169(17) 0.169(17) 0.169(17) 0.022(11) -0.022(11) 0.022(11)
O2 0.330(18) 0.370(16) 0.333(16) -0.109(15) -0.175(15) 0.209(15)
O3 0.39(2) 0.36(2) 0.41(2) 0.007(18) 0.012(18) 0.017(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 N12 2.337(4) 13_665 ?
Cd1 N12 2.337(4) 18_665 ?
Cd1 N12 2.337(4) 6 ?
Cd1 N12 2.337(4) 23_565 ?
Cd1 N12 2.337(4) 11_655 ?
Cd1 N12 2.338(4) . ?
N11 C13 1.348(8) . ?
N11 C11 1.362(7) . ?
N11 H2 0.8800 . ?
N12 C13 1.299(8) . ?
N12 C12 1.359(7) . ?
C1 C2 1.390(8) 17_765 ?
C1 C2 1.396(8) . ?
C1 C11 1.464(7) . ?
C2 C1 1.390(8) 8_566 ?
C2 H1 0.9500 . ?
C11 C12 1.355(7) . ?
C12 H3 0.9500 . ?
C13 H4 0.9500 . ?
Cl1 Cl1B 0.93(2) . ?
Cl1 O13 1.416(10) . ?
Cl1 O14 1.421(10) . ?
Cl1 O12 1.427(10) . ?
Cl1 O11 1.431(10) . ?
Cl1 O3 1.84(4) 6 ?
Cl1B O3 0.97(4) 6 ?
Cl1B O11 1.407(10) . ?
Cl1B O13 1.417(10) . ?
Cl1B O14B 1.420(11) . ?
Cl1B O12 1.422(10) . ?
O13 O3 1.68(4) 6 ?
O14 O1 1.45(2) . ?
O14B O3 0.74(5) 6 ?
O1 O14 1.45(2) 17_765 ?
O1 O14 1.45(2) 8_566 ?
O3 O14B 0.74(5) 23_565 ?
O3 Cl1B 0.97(4) 23_565 ?
O3 O13 1.68(4) 23_565 ?
O3 Cl1 1.84(4) 23_565 ?

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
N12 Cd1 N12 91.14(15) 13_665 18_665 ?
N12 Cd1 N12 88.86(15) 13_665 6 ?
N12 Cd1 N12 180.00(19) 18_665 6 ?
N12 Cd1 N12 88.86(15) 13_665 23_565 ?
N12 Cd1 N12 91.14(15) 18_665 23_565 ?
N12 Cd1 N12 88.86(15) 6 23_565 ?
N12 Cd1 N12 91.14(15) 13_665 11_655 ?
N12 Cd1 N12 88.86(15) 18_665 11_655 ?
N12 Cd1 N12 91.14(15) 6 11_655 ?
N12 Cd1 N12 180.00(19) 23_565 11_655 ?
N12 Cd1 N12 180.0 13_665 . ?
N12 Cd1 N12 88.86(15) 18_665 . ?
N12 Cd1 N12 91.14(15) 6 . ?
N12 Cd1 N12 91.14(15) 23_565 . ?
N12 Cd1 N12 88.86(15) 11_655 . ?
C13 N11 C11 107.9(5) . . ?
C13 N11 H2 126.0 . . ?
C11 N11 H2 126.0 . . ?
C13 N12 C12 104.8(5) . . ?
C13 N12 Cd1 128.4(4) . . ?
C12 N12 Cd1 125.5(4) . . ?
C2 C1 C2 119.1(6) 17_765 . ?
C2 C1 C11 119.7(5) 17_765 . ?
C2 C1 C11 121.1(5) . . ?
C1 C2 C1 120.8(6) 8_566 . ?
C1 C2 H1 119.6 8_566 . ?
C1 C2 H1 119.6 . . ?
C12 C11 N11 104.1(5) . . ?
C12 C11 C1 131.6(5) . . ?
N11 C11 C1 124.2(5) . . ?
C11 C12 N12 111.6(5) . . ?
C11 C12 H3 124.2 . . ?
N12 C12 H3 124.2 . . ?
N12 C13 N11 111.5(5) . . ?
N12 C13 H4 124.3 . . ?
N11 C13 H4 124.3 . . ?
O13 Cl1 O14 109.9(8) . . ?
O13 Cl1 O12 109.4(7) . . ?
O14 Cl1 O12 109.8(7) . . ?
O13 Cl1 O11 109.9(7) . . ?
O14 Cl1 O11 109.2(7) . . ?
O12 Cl1 O11 108.7(7) . . ?
O11 Cl1B O13 111.2(10) . . ?
O11 Cl1B O14B 109.0(10) . . ?
O13 Cl1B O14B 108.5(10) . . ?
O11 Cl1B O12 110.3(10) . . ?
O13 Cl1B O12 109.6(10) . . ?
O14B Cl1B O12 108.2(10) . . ?

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
C2 C1 C2 C1 1.6(13) 17_765 . . 8_566 ?
C11 C1 C2 C1 180.0(4) . . . 8_566 ?
C13 N11 C11 C12 1.3(8) . . . . ?
C13 N11 C11 C1 179.4(7) . . . . ?
C2 C1 C11 C12 -11.9(11) 17_765 . . . ?
C2 C1 C11 C12 169.8(7) . . . . ?
C2 C1 C11 N11 170.6(7) 17_765 . . . ?
C2 C1 C11 N11 -7.7(10) . . . . ?
N11 C11 C12 N12 -1.0(7) . . . . ?
C1 C11 C12 N12 -178.9(6) . . . . ?
C13 N12 C12 C11 0.3(7) . . . . ?
Cd1 N12 C12 C11 168.4(4) . . . . ?
C12 N12 C13 N11 0.6(8) . . . . ?
Cd1 N12 C13 N11 -167.1(5) . . . . ?
C11 N11 C13 N12 -1.3(9) . . . . ?

_refine_diff_density_max         0.573
_refine_diff_density_min         -0.372
_refine_diff_density_rms         0.108

#====END
_database_code_depnum_ccdc_archive 'CCDC 974507'