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

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_1
_database_code_depnum_ccdc_archive 'CCDC 1032234'
_audit_update_record             
;
2014-11-28 deposited with the CCDC.
2014-12-16 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C27 H27 Cd N O12'
_chemical_formula_sum            'C27 H27 Cd N O12'
_chemical_formula_weight         669.90

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           orthorhombic
_symmetry_space_group_name_H-M   Pnma

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

_cell_length_a                   11.4313(19)
_cell_length_b                   17.928(3)
_cell_length_c                   12.983(2)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     2660.8(8)
_cell_formula_units_Z            4
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    4584
_cell_measurement_theta_min      2.632
_cell_measurement_theta_max      27.138

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.09
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.672
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1360
_exptl_absorpt_coefficient_mu    0.889
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.8635
_exptl_absorpt_correction_T_max  0.9242
_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  ω
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean 0
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        0
_diffrn_reflns_number            12519
_diffrn_reflns_av_R_equivalents  0.0309
_diffrn_reflns_av_unetI/netI     0.0230
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         1.94
_diffrn_reflns_theta_max         25.00
_reflns_number_total             2423
_reflns_number_gt                2130
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'APEX2 (Bruker, 2005)'
_computing_cell_refinement       APEX2
_computing_data_reduction        APEX2
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    APEX2
_computing_publication_material  APEX2

_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)+(0.0866P)²+6.9628P] 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         2423
_refine_ls_number_parameters     201
_refine_ls_number_restraints     82
_refine_ls_R_factor_all          0.0480
_refine_ls_R_factor_gt           0.0415
_refine_ls_wR_factor_ref         0.1314
_refine_ls_wR_factor_gt          0.1242
_refine_ls_goodness_of_fit_ref   1.003
_refine_ls_restrained_S_all      0.999
_refine_ls_shift/su_max          0.021
_refine_ls_shift/su_mean         0.002

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 -0.208157(14) 0.7500 0.797846(13) 0.02662(5) Uani 1 2 d S . .
O1 O -0.06336(11) 0.83807(8) 0.83555(11) 0.0427(4) Uani 1 1 d . . .
O2 O -0.21170(9) 0.84957(7) 0.93966(11) 0.0358(3) Uani 1 1 d . . .
O3 O 0.62586(10) 0.89629(8) 1.06685(10) 0.0439(4) Uani 1 1 d . . .
H3 H 0.6730 0.8725 1.0324 0.066 Uiso 1 1 calc R . .
O4 O 0.51140(12) 0.88045(10) 0.92960(11) 0.0584(5) Uani 1 1 d . . .
O5 O -0.34601(13) 0.83754(8) 0.75607(14) 0.0606(5) Uani 1 1 d . . .
H5WA H -0.4107 0.8377 0.7287 0.073 Uiso 1 1 d R . .
H5WB H -0.3866 0.8497 0.8054 0.073 Uiso 1 1 d R . .
O6 O -0.1429(2) 0.7500 0.63243(16) 0.0683(8) Uani 1 2 d S . .
H6WA H -0.1966 0.7500 0.5906 0.082 Uiso 1 2 d SR . .
H6WB H -0.1012 0.7852 0.6158 0.082 Uiso 0.50 1 d PR . .
O7 O 0.1854(6) 0.7500 0.0034(3) 0.184(3) Uani 1 2 d SD . .
C1 C -0.11528(13) 0.87207(9) 0.90591(12) 0.0249(4) Uani 1 1 d . . .
C2 C 0.05333(13) 0.93126(9) 0.99588(12) 0.0236(4) Uani 1 1 d . . .
H2 H 0.0889 0.8847 0.9924 0.028 Uiso 1 1 calc R . .
C3 C -0.05771(13) 0.94034(9) 0.95193(11) 0.0223(4) Uani 1 1 d . . .
C4 C 0.11258(12) 0.98937(9) 1.04465(11) 0.0227(4) Uani 1 1 d . . .
C5 C 0.22868(13) 0.97479(9) 1.09458(13) 0.0248(4) Uani 1 1 d . . .
C6 C 0.24712(17) 0.99070(11) 1.19740(13) 0.0311(5) Uani 1 1 d . . .
H6 H 0.1874 1.0125 1.2356 0.037 Uiso 1 1 calc R . .
C7 C 0.35276(16) 0.97478(11) 1.24456(14) 0.0379(5) Uani 1 1 d . . .
H7 H 0.3630 0.9849 1.3142 0.045 Uiso 1 1 calc R . .
C8 C 0.44350(16) 0.94370(11) 1.18768(13) 0.0350(5) Uani 1 1 d . . .
H8 H 0.5151 0.9338 1.2189 0.042 Uiso 1 1 calc R . .
C9 C 0.42691(14) 0.92756(10) 1.08419(13) 0.0296(4) Uani 1 1 d . . .
C10 C 0.31885(14) 0.94231(9) 1.03790(13) 0.0273(4) Uani 1 1 d . . .
H10 H 0.3071 0.9304 0.9690 0.033 Uiso 1 1 calc R . .
C11 C 0.52438(14) 0.89804(10) 1.01892(14) 0.0335(5) Uani 1 1 d . . .
C12 C 0.1806(5) 0.7500 0.1000(3) 0.1665(8) Uani 1 2 d SDU . .
C13 C 0.2840(5) 0.7500 0.1726(4) 0.1674(8) Uani 1 2 d SDU . .
H13A H 0.3319 0.7060 0.1624 0.201 Uiso 0.50 1 calc PR . .
H13B H 0.3319 0.7940 0.1624 0.201 Uiso 0.50 1 calc PR . .
C14 C 0.2295(5) 0.7500 0.2783(4) 0.1703(8) Uani 1 2 d SDU . .
H14A H 0.2536 0.7939 0.3163 0.204 Uiso 0.50 1 calc PR . .
H14B H 0.2536 0.7061 0.3163 0.204 Uiso 0.50 1 calc PR . .
C15 C 0.0982(4) 0.7500 0.2637(4) 0.1680(8) Uani 1 2 d SDU . .
H15A H 0.0638 0.7060 0.2951 0.202 Uiso 0.50 1 calc PR . .
H15B H 0.0638 0.7940 0.2951 0.202 Uiso 0.50 1 calc PR . .
C16 C -0.0390(4) 0.7500 0.1126(5) 0.1826(13) Uani 1 2 d SDU . .
H16A H -0.0922 0.7758 0.1573 0.219 Uiso 0.50 1 calc PR . .
H16B H -0.0650 0.6995 0.1033 0.219 Uiso 0.50 1 calc PR . .
H16C H -0.0366 0.7747 0.0470 0.219 Uiso 0.50 1 calc PR . .
N1 N 0.0792(5) 0.7500 0.1588(5) 0.1686(7) Uani 1 2 d SDU . .


_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 O6 2.274(2) . ?
Cd1 O5 2.2892(15) 7_575 ?
Cd1 O5 2.2892(15) . ?
Cd1 O1 2.3393(13) . ?
Cd1 O1 2.3393(13) 7_575 ?
Cd1 O2 2.5649(14) . ?
Cd1 O2 2.5649(14) 7_575 ?
O1 C1 1.248(2) . ?
O2 C1 1.2528(19) . ?
O3 C11 1.317(2) . ?
O3 H3 0.8200 . ?
O4 C11 1.211(2) . ?
O5 H5WA 0.8200 . ?
O5 H5WB 0.8200 . ?
O6 H6WA 0.8200 . ?
O6 H6WB 0.8200 . ?
O7 C12 1.256(6) . ?
C1 C3 1.513(2) . ?
C2 C4 1.395(2) . ?
C2 C3 1.401(2) . ?
C2 H2 0.9300 . ?
C3 C4 1.408(2) 5_577 ?
C4 C3 1.408(2) 5_577 ?
C4 C5 1.500(2) . ?
C5 C6 1.381(2) . ?
C5 C10 1.394(2) . ?
C6 C7 1.384(3) . ?
C6 H6 0.9300 . ?
C7 C8 1.390(3) . ?
C7 H7 0.9300 . ?
C8 C9 1.388(2) . ?
C8 H8 0.9300 . ?
C9 C10 1.399(2) . ?
C9 C11 1.497(2) . ?
C10 H10 0.9300 . ?
C12 N1 1.388(8) . ?
C12 C13 1.511(7) . ?
C13 C14 1.507(7) . ?
C13 H13A 0.9700 . ?
C13 H13B 0.9700 . ?
C14 C15 1.512(7) . ?
C14 H14A 0.9700 . ?
C14 H14B 0.9700 . ?
C15 N1 1.380(8) . ?
C15 H15A 0.9700 . ?
C15 H15B 0.9700 . ?
C16 N1 1.479(7) . ?
C16 H16A 0.9600 . ?
C16 H16B 0.9600 . ?
C16 H16C 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
O6 Cd1 O5 90.12(6) . 7_575 ?
O6 Cd1 O5 90.12(6) . . ?
O5 Cd1 O5 86.56(8) 7_575 . ?
O6 Cd1 O1 88.02(6) . . ?
O5 Cd1 O1 177.98(5) 7_575 . ?
O5 Cd1 O1 94.24(5) . . ?
O6 Cd1 O1 88.02(6) . 7_575 ?
O5 Cd1 O1 94.24(5) 7_575 7_575 ?
O5 Cd1 O1 177.98(5) . 7_575 ?
O1 Cd1 O1 84.90(7) . 7_575 ?
O6 Cd1 O2 133.10(4) . . ?
O5 Cd1 O2 129.52(5) 7_575 . ?
O5 Cd1 O2 71.46(5) . . ?
O1 Cd1 O2 52.50(4) . . ?
O1 Cd1 O2 109.31(4) 7_575 . ?
O6 Cd1 O2 133.10(4) . 7_575 ?
O5 Cd1 O2 71.46(5) 7_575 7_575 ?
O5 Cd1 O2 129.52(5) . 7_575 ?
O1 Cd1 O2 109.31(4) . 7_575 ?
O1 Cd1 O2 52.50(4) 7_575 7_575 ?
O2 Cd1 O2 88.21(6) . 7_575 ?
C1 O1 Cd1 98.41(10) . . ?
C1 O2 Cd1 87.65(10) . . ?
C11 O3 H3 109.5 . . ?
Cd1 O5 H5WA 136.5 . . ?
Cd1 O5 H5WB 112.8 . . ?
H5WA O5 H5WB 80.1 . . ?
Cd1 O6 H6WA 112.3 . . ?
Cd1 O6 H6WB 116.1 . . ?
H6WA O6 H6WB 105.1 . . ?
O1 C1 O2 121.14(15) . . ?
O1 C1 C3 118.51(14) . . ?
O2 C1 C3 120.33(14) . . ?
C4 C2 C3 122.55(14) . . ?
C4 C2 H2 118.7 . . ?
C3 C2 H2 118.7 . . ?
C2 C3 C4 119.65(14) . 5_577 ?
C2 C3 C1 117.45(13) . . ?
C4 C3 C1 122.86(13) 5_577 . ?
C2 C4 C3 117.80(13) . 5_577 ?
C2 C4 C5 119.72(14) . . ?
C3 C4 C5 122.44(14) 5_577 . ?
C6 C5 C10 118.92(15) . . ?
C6 C5 C4 121.12(14) . . ?
C10 C5 C4 119.93(14) . . ?
C5 C6 C7 121.22(17) . . ?
C5 C6 H6 119.4 . . ?
C7 C6 H6 119.4 . . ?
C6 C7 C8 119.93(17) . . ?
C6 C7 H7 120.0 . . ?
C8 C7 H7 120.0 . . ?
C9 C8 C7 119.74(16) . . ?
C9 C8 H8 120.1 . . ?
C7 C8 H8 120.1 . . ?
C8 C9 C10 119.82(15) . . ?
C8 C9 C11 121.35(15) . . ?
C10 C9 C11 118.75(15) . . ?
C5 C10 C9 120.34(15) . . ?
C5 C10 H10 119.8 . . ?
C9 C10 H10 119.8 . . ?
O4 C11 O3 123.67(16) . . ?
O4 C11 C9 122.89(16) . . ?
O3 C11 C9 113.37(15) . . ?
O7 C12 N1 125.9(6) . . ?
O7 C12 C13 126.0(5) . . ?
N1 C12 C13 108.1(4) . . ?
C14 C13 C12 104.1(4) . . ?
C14 C13 H13A 110.9 . . ?
C12 C13 H13A 110.9 . . ?
C14 C13 H13B 110.9 . . ?
C12 C13 H13B 110.9 . . ?
H13A C13 H13B 108.9 . . ?
C13 C14 C15 107.3(4) . . ?
C13 C14 H14A 110.3 . . ?
C15 C14 H14A 110.3 . . ?
C13 C14 H14B 110.3 . . ?
C15 C14 H14B 110.3 . . ?
H14A C14 H14B 108.5 . . ?
N1 C15 C14 106.2(4) . . ?
N1 C15 H15A 110.5 . . ?
C14 C15 H15A 110.5 . . ?
N1 C15 H15B 110.5 . . ?
C14 C15 H15B 110.5 . . ?
H15A C15 H15B 108.7 . . ?
N1 C16 H16A 109.5 . . ?
N1 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
N1 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C15 N1 C12 114.3(5) . . ?
C15 N1 C16 123.0(5) . . ?
C12 N1 C16 122.7(6) . . ?

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
O6 Cd1 O1 C1 149.56(11) . . . . ?
O5 Cd1 O1 C1 172.8(14) 7_575 . . . ?
O5 Cd1 O1 C1 59.58(11) . . . . ?
O1 Cd1 O1 C1 -122.25(9) 7_575 . . . ?
O2 Cd1 O1 C1 -3.11(9) . . . . ?
O2 Cd1 O1 C1 -75.02(11) 7_575 . . . ?
O6 Cd1 O2 C1 -35.86(13) . . . . ?
O5 Cd1 O2 C1 -176.74(9) 7_575 . . . ?
O5 Cd1 O2 C1 -107.77(10) . . . . ?
O1 Cd1 O2 C1 3.07(9) . . . . ?
O1 Cd1 O2 C1 70.26(10) 7_575 . . . ?
O2 Cd1 O2 C1 119.24(9) 7_575 . . . ?
Cd1 O1 C1 O2 5.91(17) . . . . ?
Cd1 O1 C1 C3 -175.66(11) . . . . ?
Cd1 O2 C1 O1 -5.33(15) . . . . ?
Cd1 O2 C1 C3 176.26(13) . . . . ?
C4 C2 C3 C4 0.7(3) . . . 5_577 ?
C4 C2 C3 C1 -177.05(14) . . . . ?
O1 C1 C3 C2 -58.3(2) . . . . ?
O2 C1 C3 C2 120.12(17) . . . . ?
O1 C1 C3 C4 124.00(17) . . . 5_577 ?
O2 C1 C3 C4 -57.6(2) . . . 5_577 ?
C3 C2 C4 C3 -0.7(2) . . . 5_577 ?
C3 C2 C4 C5 177.00(14) . . . . ?
C2 C4 C5 C6 -123.55(18) . . . . ?
C3 C4 C5 C6 54.0(2) 5_577 . . . ?
C2 C4 C5 C10 54.2(2) . . . . ?
C3 C4 C5 C10 -128.19(17) 5_577 . . . ?
C10 C5 C6 C7 -0.2(3) . . . . ?
C4 C5 C6 C7 177.60(16) . . . . ?
C5 C6 C7 C8 1.4(3) . . . . ?
C6 C7 C8 C9 -1.2(3) . . . . ?
C7 C8 C9 C10 -0.3(3) . . . . ?
C7 C8 C9 C11 176.57(17) . . . . ?
C6 C5 C10 C9 -1.3(2) . . . . ?
C4 C5 C10 C9 -179.12(15) . . . . ?
C8 C9 C10 C5 1.6(3) . . . . ?
C11 C9 C10 C5 -175.42(15) . . . . ?
C8 C9 C11 O4 176.77(19) . . . . ?
C10 C9 C11 O4 -6.3(3) . . . . ?
C8 C9 C11 O3 -6.0(2) . . . . ?
C10 C9 C11 O3 170.88(16) . . . . ?
O7 C12 C13 C14 180.0 . . . . ?
N1 C12 C13 C14 0.0 . . . . ?
C12 C13 C14 C15 0.0 . . . . ?
C13 C14 C15 N1 0.0 . . . . ?
C14 C15 N1 C12 0.0 . . . . ?
C14 C15 N1 C16 180.0 . . . . ?
O7 C12 N1 C15 180.0 . . . . ?
C13 C12 N1 C15 0.0 . . . . ?
O7 C12 N1 C16 0.0 . . . . ?
C13 C12 N1 C16 180.0 . . . . ?

_diffrn_measured_fraction_theta_max 0.997
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.997
_refine_diff_density_max         1.279
_refine_diff_density_min         -1.070
_refine_diff_density_rms         0.117

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_2
_database_code_depnum_ccdc_archive 'CCDC 1032235'
_audit_update_record             
;
2014-11-28 deposited with the CCDC.
2014-12-16 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C22 H20 Cd3 O14'
_chemical_formula_sum            'C22 H20 Cd3 O14'
_chemical_formula_weight         845.58

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'
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   P2(1)/c

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

_cell_length_a                   11.0483(18)
_cell_length_b                   6.6820(11)
_cell_length_c                   17.638(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 107.833(2)
_cell_angle_gamma                90.00
_cell_volume                     1239.6(4)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    3570
_cell_measurement_theta_min      3.538
_cell_measurement_theta_max      28.330

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.10
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.266
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             816
_exptl_absorpt_coefficient_mu    2.624
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6220
_exptl_absorpt_correction_T_max  0.7794
_exptl_absorpt_process_details   sadabs

_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  ω
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean 0
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        0
_diffrn_reflns_number            5881
_diffrn_reflns_av_R_equivalents  0.0410
_diffrn_reflns_av_unetI/netI     0.0443
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         1.94
_diffrn_reflns_theta_max         25.09
_reflns_number_total             2201
_reflns_number_gt                1857
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'APEX2 (Bruker, 2005)'
_computing_cell_refinement       APEX2
_computing_data_reduction        APEX2
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    APEX2
_computing_publication_material  APEX2

_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)+(0.0597P)²+3.8582P] 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         2201
_refine_ls_number_parameters     182
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0424
_refine_ls_R_factor_gt           0.0290
_refine_ls_wR_factor_ref         0.1118
_refine_ls_wR_factor_gt          0.0841
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_restrained_S_all      1.057
_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
Cd1 Cd 0.5000 0.0000 0.0000 0.01594(18) Uani 1 2 d S . .
Cd2 Cd 0.46532(3) 0.49647(4) 0.090266(19) 0.01865(17) Uani 1 1 d . . .
C1 C 0.2552(4) 0.1676(6) 0.0442(2) 0.0159(8) Uani 1 1 d . . .
C2 C 0.1225(4) 0.0811(7) 0.0237(2) 0.0172(8) Uani 1 1 d . . .
C3 C 0.0891(4) -0.0691(7) -0.0343(2) 0.0184(9) Uani 1 1 d . . .
H3 H 0.1498 -0.1161 -0.0567 0.022 Uiso 1 1 calc R . .
C4 C 0.0331(4) 0.1496(6) 0.0593(2) 0.0157(8) Uani 1 1 d . . .
C5 C 0.0700(4) 0.2970(6) 0.1261(2) 0.0167(8) Uani 1 1 d . . .
C6 C 0.1692(4) 0.2503(6) 0.1939(2) 0.0181(8) Uani 1 1 d . . .
H6 H 0.2107 0.1281 0.1968 0.022 Uiso 1 1 calc R . .
C7 C 0.2075(4) 0.3823(7) 0.2573(2) 0.0182(9) Uani 1 1 d . . .
C8 C 0.1445(5) 0.5649(8) 0.2528(3) 0.0254(10) Uani 1 1 d . . .
H8 H 0.1698 0.6551 0.2948 0.030 Uiso 1 1 calc R . .
C9 C 0.0446(5) 0.6121(7) 0.1860(3) 0.0296(11) Uani 1 1 d . . .
H9 H 0.0027 0.7338 0.1834 0.036 Uiso 1 1 calc R . .
C10 C 0.0062(5) 0.4781(7) 0.1224(3) 0.0258(11) Uani 1 1 d . . .
H10 H -0.0616 0.5098 0.0778 0.031 Uiso 1 1 calc R . .
C11 C 0.3153(4) 0.3255(7) 0.3301(2) 0.0214(9) Uani 1 1 d . . .
O1 O 0.3451(3) 0.0437(5) 0.0653(2) 0.0246(7) Uani 1 1 d . . .
O2 O 0.2673(3) 0.3513(5) 0.03856(19) 0.0252(7) Uani 1 1 d . . .
O3 O 0.3673(4) 0.1637(7) 0.3297(2) 0.0592(13) Uani 1 1 d . . .
O4 O 0.3415(4) 0.4448(7) 0.3872(2) 0.0535(12) Uani 1 1 d . . .
O5 O 0.3337(3) 0.7057(5) 0.1413(2) 0.0332(8) Uani 1 1 d . . .
H5WA H 0.3296 0.8175 0.1215 0.050 Uiso 1 1 calc R . .
H5WB H 0.3794 0.7290 0.1866 0.050 Uiso 1 1 d R . .
O6 O 0.5055(4) 0.2887(7) 0.1997(2) 0.0544(13) Uani 1 1 d . . .
H6WA H 0.4707 0.1804 0.1860 0.082 Uiso 1 1 calc R . .
H6WB H 0.5513 0.2658 0.2451 0.082 Uiso 1 1 d R . .
O7 O 0.5684(3) 0.3141(4) 0.02177(17) 0.0189(6) Uani 1 1 d D . .
H7 H 0.642(3) 0.307(11) 0.048(3) 0.06(2) Uiso 1 1 d D . .


_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 O7 2.224(3) 3_655 ?
Cd1 O7 2.224(3) . ?
Cd1 O4 2.243(4) 2_645 ?
Cd1 O4 2.243(4) 4_565 ?
Cd1 O1 2.356(3) 3_655 ?
Cd1 O1 2.356(3) . ?
Cd2 O3 2.250(4) 2_655 ?
Cd2 O7 2.255(3) . ?
Cd2 O7 2.279(3) 3_665 ?
Cd2 O6 2.307(4) . ?
Cd2 O2 2.310(3) . ?
Cd2 O5 2.383(3) . ?
C1 O2 1.242(5) . ?
C1 O1 1.258(5) . ?
C1 C2 1.514(6) . ?
C2 C3 1.399(6) . ?
C2 C4 1.400(6) . ?
C3 C4 1.393(6) 3 ?
C3 H3 0.9300 . ?
C4 C3 1.393(6) 3 ?
C4 C5 1.493(6) . ?
C5 C6 1.388(6) . ?
C5 C10 1.392(6) . ?
C6 C7 1.385(6) . ?
C6 H6 0.9300 . ?
C7 C8 1.395(7) . ?
C7 C11 1.509(6) . ?
C8 C9 1.382(7) . ?
C8 H8 0.9300 . ?
C9 C10 1.395(7) . ?
C9 H9 0.9300 . ?
C10 H10 0.9300 . ?
C11 O3 1.225(6) . ?
C11 O4 1.246(6) . ?
O3 Cd2 2.250(4) 2_645 ?
O4 Cd1 2.243(4) 2_655 ?
O5 H5WA 0.8200 . ?
O5 H5WB 0.8201 . ?
O6 H6WA 0.8200 . ?
O6 H6WB 0.8201 . ?
O7 Cd2 2.279(3) 3_665 ?
O7 H7 0.80(2) . ?

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
O7 Cd1 O7 180.0 3_655 . ?
O7 Cd1 O4 97.45(14) 3_655 2_645 ?
O7 Cd1 O4 82.55(14) . 2_645 ?
O7 Cd1 O4 82.55(14) 3_655 4_565 ?
O7 Cd1 O4 97.45(14) . 4_565 ?
O4 Cd1 O4 180.0 2_645 4_565 ?
O7 Cd1 O1 93.32(11) 3_655 3_655 ?
O7 Cd1 O1 86.68(11) . 3_655 ?
O4 Cd1 O1 85.81(16) 2_645 3_655 ?
O4 Cd1 O1 94.19(16) 4_565 3_655 ?
O7 Cd1 O1 86.68(11) 3_655 . ?
O7 Cd1 O1 93.32(11) . . ?
O4 Cd1 O1 94.19(16) 2_645 . ?
O4 Cd1 O1 85.81(16) 4_565 . ?
O1 Cd1 O1 180.0(2) 3_655 . ?
O3 Cd2 O7 98.74(16) 2_655 . ?
O3 Cd2 O7 98.80(12) 2_655 3_665 ?
O7 Cd2 O7 79.09(12) . 3_665 ?
O3 Cd2 O6 82.16(14) 2_655 . ?
O7 Cd2 O6 97.10(14) . . ?
O7 Cd2 O6 176.16(14) 3_665 . ?
O3 Cd2 O2 162.39(16) 2_655 . ?
O7 Cd2 O2 97.72(11) . . ?
O7 Cd2 O2 90.42(11) 3_665 . ?
O6 Cd2 O2 89.64(13) . . ?
O3 Cd2 O5 87.19(17) 2_655 . ?
O7 Cd2 O5 170.38(11) . . ?
O7 Cd2 O5 92.58(11) 3_665 . ?
O6 Cd2 O5 91.18(15) . . ?
O2 Cd2 O5 77.38(12) . . ?
O2 C1 O1 125.4(4) . . ?
O2 C1 C2 118.6(4) . . ?
O1 C1 C2 116.0(4) . . ?
C3 C2 C4 119.9(4) . . ?
C3 C2 C1 117.9(4) . . ?
C4 C2 C1 122.2(4) . . ?
C4 C3 C2 121.4(4) 3 . ?
C4 C3 H3 119.3 3 . ?
C2 C3 H3 119.3 . . ?
C3 C4 C2 118.7(4) 3 . ?
C3 C4 C5 120.5(4) 3 . ?
C2 C4 C5 120.7(4) . . ?
C6 C5 C10 119.4(4) . . ?
C6 C5 C4 119.0(4) . . ?
C10 C5 C4 121.6(4) . . ?
C7 C6 C5 121.2(4) . . ?
C7 C6 H6 119.4 . . ?
C5 C6 H6 119.4 . . ?
C6 C7 C8 119.2(4) . . ?
C6 C7 C11 119.6(4) . . ?
C8 C7 C11 121.2(4) . . ?
C9 C8 C7 120.2(4) . . ?
C9 C8 H8 119.9 . . ?
C7 C8 H8 119.9 . . ?
C8 C9 C10 120.4(4) . . ?
C8 C9 H9 119.8 . . ?
C10 C9 H9 119.8 . . ?
C5 C10 C9 119.7(4) . . ?
C5 C10 H10 120.2 . . ?
C9 C10 H10 120.2 . . ?
O3 C11 O4 125.2(4) . . ?
O3 C11 C7 117.8(4) . . ?
O4 C11 C7 117.0(4) . . ?
C1 O1 Cd1 124.2(3) . . ?
C1 O2 Cd2 119.7(3) . . ?
C11 O3 Cd2 137.0(3) . 2_645 ?
C11 O4 Cd1 138.3(4) . 2_655 ?
Cd2 O5 H5WA 109.5 . . ?
Cd2 O5 H5WB 102.4 . . ?
H5WA O5 H5WB 100.4 . . ?
Cd2 O6 H6WA 109.5 . . ?
Cd2 O6 H6WB 146.3 . . ?
H6WA O6 H6WB 102.5 . . ?
Cd1 O7 Cd2 113.69(13) . . ?
Cd1 O7 Cd2 114.69(12) . 3_665 ?
Cd2 O7 Cd2 100.91(12) . 3_665 ?
Cd1 O7 H7 106(5) . . ?
Cd2 O7 H7 108(5) . . ?
Cd2 O7 H7 114(5) 3_665 . ?

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
O2 C1 C2 C3 124.3(4) . . . . ?
O1 C1 C2 C3 -55.2(5) . . . . ?
O2 C1 C2 C4 -54.3(6) . . . . ?
O1 C1 C2 C4 126.3(4) . . . . ?
C4 C2 C3 C4 1.7(7) . . . 3 ?
C1 C2 C3 C4 -176.9(4) . . . 3 ?
C3 C2 C4 C3 -1.6(7) . . . 3 ?
C1 C2 C4 C3 176.9(4) . . . 3 ?
C3 C2 C4 C5 174.7(4) . . . . ?
C1 C2 C4 C5 -6.7(6) . . . . ?
C3 C4 C5 C6 119.6(5) 3 . . . ?
C2 C4 C5 C6 -56.7(6) . . . . ?
C3 C4 C5 C10 -59.5(6) 3 . . . ?
C2 C4 C5 C10 124.2(5) . . . . ?
C10 C5 C6 C7 -1.3(6) . . . . ?
C4 C5 C6 C7 179.6(4) . . . . ?
C5 C6 C7 C8 0.3(6) . . . . ?
C5 C6 C7 C11 179.7(4) . . . . ?
C6 C7 C8 C9 0.4(7) . . . . ?
C11 C7 C8 C9 -178.9(4) . . . . ?
C7 C8 C9 C10 -0.3(8) . . . . ?
C6 C5 C10 C9 1.4(7) . . . . ?
C4 C5 C10 C9 -179.5(4) . . . . ?
C8 C9 C10 C5 -0.7(8) . . . . ?
C6 C7 C11 O3 1.5(7) . . . . ?
C8 C7 C11 O3 -179.2(5) . . . . ?
C6 C7 C11 O4 -176.2(5) . . . . ?
C8 C7 C11 O4 3.1(7) . . . . ?
O2 C1 O1 Cd1 -58.2(5) . . . . ?
C2 C1 O1 Cd1 121.2(3) . . . . ?
O7 Cd1 O1 C1 -119.5(3) 3_655 . . . ?
O7 Cd1 O1 C1 60.5(3) . . . . ?
O4 Cd1 O1 C1 143.2(3) 2_645 . . . ?
O4 Cd1 O1 C1 -36.8(3) 4_565 . . . ?
O1 Cd1 O1 C1 34(100) 3_655 . . . ?
O1 C1 O2 Cd2 -11.5(6) . . . . ?
C2 C1 O2 Cd2 169.1(3) . . . . ?
O3 Cd2 O2 C1 -102.4(5) 2_655 . . . ?
O7 Cd2 O2 C1 56.6(3) . . . . ?
O7 Cd2 O2 C1 135.7(3) 3_665 . . . ?
O6 Cd2 O2 C1 -40.5(3) . . . . ?
O5 Cd2 O2 C1 -131.8(3) . . . . ?
O4 C11 O3 Cd2 -7.5(10) . . . 2_645 ?
C7 C11 O3 Cd2 175.1(4) . . . 2_645 ?
O3 C11 O4 Cd1 17.0(10) . . . 2_655 ?
C7 C11 O4 Cd1 -165.5(4) . . . 2_655 ?
O7 Cd1 O7 Cd2 -1.0(15) 3_655 . . . ?
O4 Cd1 O7 Cd2 -93.20(18) 2_645 . . . ?
O4 Cd1 O7 Cd2 86.80(18) 4_565 . . . ?
O1 Cd1 O7 Cd2 -179.40(14) 3_655 . . . ?
O1 Cd1 O7 Cd2 0.60(14) . . . . ?
O7 Cd1 O7 Cd2 -116.4(13) 3_655 . . 3_665 ?
O4 Cd1 O7 Cd2 151.38(19) 2_645 . . 3_665 ?
O4 Cd1 O7 Cd2 -28.62(19) 4_565 . . 3_665 ?
O1 Cd1 O7 Cd2 65.18(14) 3_655 . . 3_665 ?
O1 Cd1 O7 Cd2 -114.82(14) . . . 3_665 ?
O3 Cd2 O7 Cd1 139.33(15) 2_655 . . . ?
O7 Cd2 O7 Cd1 -123.31(18) 3_665 . . . ?
O6 Cd2 O7 Cd1 56.22(16) . . . . ?
O2 Cd2 O7 Cd1 -34.38(14) . . . . ?
O5 Cd2 O7 Cd1 -93.1(7) . . . . ?
O3 Cd2 O7 Cd2 -97.36(13) 2_655 . . 3_665 ?
O7 Cd2 O7 Cd2 0.0 3_665 . . 3_665 ?
O6 Cd2 O7 Cd2 179.53(13) . . . 3_665 ?
O2 Cd2 O7 Cd2 88.93(12) . . . 3_665 ?
O5 Cd2 O7 Cd2 30.2(7) . . . 3_665 ?

_diffrn_measured_fraction_theta_max 0.997
_diffrn_reflns_theta_full        25.09
_diffrn_measured_fraction_theta_full 0.997
_refine_diff_density_max         1.063
_refine_diff_density_min         -1.845
_refine_diff_density_rms         0.293
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_3
_database_code_depnum_ccdc_archive 'CCDC 1032236'
_audit_update_record             
;
2014-11-28 deposited with the CCDC.
2014-12-16 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C11 H9 Cd O6'
_chemical_formula_sum            'C11 H9 Cd O6'
_chemical_formula_weight         349.58

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'
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   I4(1)/a

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                   18.1586(14)
_cell_length_b                   18.1586(14)
_cell_length_c                   14.416(2)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     4753.4(9)
_cell_formula_units_Z            16
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    5043
_cell_measurement_theta_min      2.392
_cell_measurement_theta_max      28.764

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.24
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.954
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2736
_exptl_absorpt_coefficient_mu    1.854
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6063
_exptl_absorpt_correction_T_max  0.6646
_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  ω
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean 0
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        0
_diffrn_reflns_number            11566
_diffrn_reflns_av_R_equivalents  0.0231
_diffrn_reflns_av_unetI/netI     0.0164
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       7
_diffrn_reflns_theta_min         1.80
_diffrn_reflns_theta_max         25.08
_reflns_number_total             2105
_reflns_number_gt                1964
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'APEX2 (Bruker, 2005)'
_computing_cell_refinement       APEX2
_computing_data_reduction        APEX2
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    APEX2
_computing_publication_material  APEX2

_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)+(0.0673P)²+24.4033P] 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         2105
_refine_ls_number_parameters     164
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0306
_refine_ls_R_factor_gt           0.0283
_refine_ls_wR_factor_ref         0.1006
_refine_ls_wR_factor_gt          0.0986
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_restrained_S_all      1.038
_refine_ls_shift/su_max          0.005
_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 0.204553(15) 0.015159(15) 1.047679(19) 0.02199(16) Uani 1 1 d . . .
O1 O 0.13401(19) 0.10414(19) 0.9673(2) 0.0376(8) Uani 1 1 d . . .
O2 O 0.14563(15) -0.00221(17) 0.8966(2) 0.0276(6) Uani 1 1 d . . .
O3 O 0.30262(17) 0.0182(2) 0.9475(3) 0.0448(9) Uani 1 1 d . . .
O4 O 0.2288(2) -0.10722(19) 1.0716(2) 0.0463(9) Uani 1 1 d . . .
O5 O 0.1003(2) 0.0098(3) 1.1328(3) 0.0648(13) Uani 1 1 d . . .
H5WA H 0.1126 0.0129 1.1874 0.078 Uiso 1 1 d R . .
H5WB H 0.0659 0.0384 1.1246 0.078 Uiso 1 1 d R . .
O6 O 0.9838(5) 0.1098(7) 0.1107(13) 0.326(12) Uani 1 1 d . . .
H6WA H 0.9488 0.0812 0.1104 0.391 Uiso 1 1 d R . .
H6WB H 1.0182 0.0813 0.1189 0.391 Uiso 1 1 d R . .
C1 C 0.1173(2) 0.0623(2) 0.9019(3) 0.0245(8) Uani 1 1 d . . .
C2 C 0.0615(2) 0.0853(2) 0.8310(3) 0.0245(8) Uani 1 1 d . . .
C3 C 0.0155(3) 0.1451(3) 0.8481(3) 0.0393(11) Uani 1 1 d . . .
H3 H 0.0209 0.1724 0.9023 0.047 Uiso 1 1 calc R . .
C4 C -0.0380(3) 0.1639(3) 0.7847(4) 0.0446(13) Uani 1 1 d . . .
H4 H -0.0703 0.2024 0.7976 0.053 Uiso 1 1 calc R . .
C5 C -0.0440(3) 0.1256(3) 0.7011(3) 0.0311(10) Uani 1 1 d . . .
H5 H -0.0787 0.1398 0.6571 0.037 Uiso 1 1 calc R . .
C6 C 0.0013(2) 0.0669(2) 0.6842(3) 0.0193(8) Uani 1 1 d . . .
C7 C 0.0538(2) 0.0451(2) 0.7491(3) 0.0221(8) Uani 1 1 d . . .
H7 H 0.0834 0.0043 0.7380 0.026 Uiso 1 1 calc R . .
C8 C -0.0013(2) 0.0283(2) 0.5916(3) 0.0193(8) Uani 1 1 d . . .
C9 C -0.0671(2) 0.0070(2) 0.5481(3) 0.0194(8) Uani 1 1 d . . .
C10 C -0.1403(2) 0.0020(2) 0.5969(3) 0.0246(9) Uani 1 1 d . . .
C11 C 0.0644(2) 0.0201(2) 0.5424(3) 0.0201(8) Uani 1 1 d . . .
H11 H 0.1083 0.0332 0.5713 0.024 Uiso 1 1 calc R . .


_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 2.259(4) . ?
Cd1 O4 2.292(3) . ?
Cd1 O3 2.293(3) . ?
Cd1 O2 2.297(3) 8_444 ?
Cd1 O1 2.365(3) . ?
Cd1 O2 2.447(3) . ?
O1 C1 1.249(5) . ?
O2 C1 1.281(5) . ?
O2 Cd1 2.297(3) 7_444 ?
O3 C10 1.253(5) 10_657 ?
O4 C10 1.248(6) 11_657 ?
O5 H5WA 0.8199 . ?
O5 H5WB 0.8200 . ?
O6 H6WA 0.8201 . ?
O6 H6WB 0.8199 . ?
C1 C2 1.498(6) . ?
C2 C3 1.393(6) . ?
C2 C7 1.394(6) . ?
C3 C4 1.378(7) . ?
C3 H3 0.9300 . ?
C4 C5 1.396(6) . ?
C4 H4 0.9300 . ?
C5 C6 1.368(6) . ?
C5 H5 0.9300 . ?
C6 C7 1.393(6) . ?
C6 C8 1.509(5) . ?
C7 H7 0.9300 . ?
C8 C11 1.396(5) . ?
C8 C9 1.403(5) . ?
C9 C11 1.395(5) 9_556 ?
C9 C10 1.507(5) . ?
C10 O4 1.248(6) 16_557 ?
C10 O3 1.253(5) 10_557 ?
C11 C9 1.395(5) 9_556 ?
C11 H11 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
O5 Cd1 O4 92.18(17) . . ?
O5 Cd1 O3 173.82(15) . . ?
O4 Cd1 O3 88.22(14) . . ?
O5 Cd1 O2 88.82(16) . 8_444 ?
O4 Cd1 O2 121.63(12) . 8_444 ?
O3 Cd1 O2 96.22(13) . 8_444 ?
O5 Cd1 O1 80.87(15) . . ?
O4 Cd1 O1 147.19(13) . . ?
O3 Cd1 O1 95.48(13) . . ?
O2 Cd1 O1 90.44(11) 8_444 . ?
O5 Cd1 O2 96.40(13) . . ?
O4 Cd1 O2 95.36(12) . . ?
O3 Cd1 O2 77.43(12) . . ?
O2 Cd1 O2 142.48(9) 8_444 . ?
O1 Cd1 O2 54.21(10) . . ?
C1 O1 Cd1 94.9(3) . . ?
C1 O2 Cd1 129.3(3) . 7_444 ?
C1 O2 Cd1 90.3(2) . . ?
Cd1 O2 Cd1 106.76(11) 7_444 . ?
C10 O3 Cd1 163.3(3) 10_657 . ?
C10 O4 Cd1 103.9(3) 11_657 . ?
Cd1 O5 H5WA 106.8 . . ?
Cd1 O5 H5WB 122.3 . . ?
H5WA O5 H5WB 107.6 . . ?
H6WA O6 H6WB 101.0 . . ?
O1 C1 O2 120.2(4) . . ?
O1 C1 C2 120.6(4) . . ?
O2 C1 C2 119.1(4) . . ?
C3 C2 C7 119.8(4) . . ?
C3 C2 C1 120.1(4) . . ?
C7 C2 C1 120.0(4) . . ?
C4 C3 C2 119.9(4) . . ?
C4 C3 H3 120.0 . . ?
C2 C3 H3 120.0 . . ?
C3 C4 C5 120.3(4) . . ?
C3 C4 H4 119.9 . . ?
C5 C4 H4 119.9 . . ?
C6 C5 C4 119.7(4) . . ?
C6 C5 H5 120.2 . . ?
C4 C5 H5 120.2 . . ?
C5 C6 C7 120.9(4) . . ?
C5 C6 C8 120.0(4) . . ?
C7 C6 C8 119.0(3) . . ?
C6 C7 C2 119.3(4) . . ?
C6 C7 H7 120.4 . . ?
C2 C7 H7 120.4 . . ?
C11 C8 C9 118.1(4) . . ?
C11 C8 C6 118.1(3) . . ?
C9 C8 C6 123.4(3) . . ?
C11 C9 C8 119.0(4) 9_556 . ?
C11 C9 C10 116.5(3) 9_556 . ?
C8 C9 C10 124.0(4) . . ?
O4 C10 O3 122.1(4) 16_557 10_557 ?
O4 C10 C9 119.4(4) 16_557 . ?
O3 C10 C9 118.5(4) 10_557 . ?
C9 C11 C8 122.8(4) 9_556 . ?
C9 C11 H11 118.6 9_556 . ?
C8 C11 H11 118.6 . . ?

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
O5 Cd1 O1 C1 -101.3(3) . . . . ?
O4 Cd1 O1 C1 -21.6(4) . . . . ?
O3 Cd1 O1 C1 73.6(3) . . . . ?
O2 Cd1 O1 C1 169.9(3) 8_444 . . . ?
O2 Cd1 O1 C1 3.4(2) . . . . ?
O5 Cd1 O2 C1 70.5(2) . . . . ?
O4 Cd1 O2 C1 163.3(2) . . . . ?
O3 Cd1 O2 C1 -109.7(3) . . . . ?
O2 Cd1 O2 C1 -25.9(3) 8_444 . . . ?
O1 Cd1 O2 C1 -3.3(2) . . . . ?
O5 Cd1 O2 Cd1 -157.96(17) . . . 7_444 ?
O4 Cd1 O2 Cd1 -65.15(15) . . . 7_444 ?
O3 Cd1 O2 Cd1 21.82(14) . . . 7_444 ?
O2 Cd1 O2 Cd1 105.61(9) 8_444 . . 7_444 ?
O1 Cd1 O2 Cd1 128.16(18) . . . 7_444 ?
O5 Cd1 O3 C10 -105.6(17) . . . 10_657 ?
O4 Cd1 O3 C10 -11.8(12) . . . 10_657 ?
O2 Cd1 O3 C10 109.9(12) 8_444 . . 10_657 ?
O1 Cd1 O3 C10 -159.1(12) . . . 10_657 ?
O2 Cd1 O3 C10 -107.7(12) . . . 10_657 ?
O5 Cd1 O4 C10 -75.7(3) . . . 11_657 ?
O3 Cd1 O4 C10 110.5(3) . . . 11_657 ?
O2 Cd1 O4 C10 14.3(3) 8_444 . . 11_657 ?
O1 Cd1 O4 C10 -152.1(3) . . . 11_657 ?
O2 Cd1 O4 C10 -172.3(3) . . . 11_657 ?
Cd1 O1 C1 O2 -6.2(4) . . . . ?
Cd1 O1 C1 C2 171.2(3) . . . . ?
Cd1 O2 C1 O1 -106.2(4) 7_444 . . . ?
Cd1 O2 C1 O1 5.9(4) . . . . ?
Cd1 O2 C1 C2 76.4(4) 7_444 . . . ?
Cd1 O2 C1 C2 -171.5(3) . . . . ?
O1 C1 C2 C3 -14.9(6) . . . . ?
O2 C1 C2 C3 162.5(4) . . . . ?
O1 C1 C2 C7 167.3(4) . . . . ?
O2 C1 C2 C7 -15.3(6) . . . . ?
C7 C2 C3 C4 0.8(8) . . . . ?
C1 C2 C3 C4 -176.9(5) . . . . ?
C2 C3 C4 C5 -3.2(9) . . . . ?
C3 C4 C5 C6 3.0(8) . . . . ?
C4 C5 C6 C7 -0.4(7) . . . . ?
C4 C5 C6 C8 -175.9(4) . . . . ?
C5 C6 C7 C2 -2.0(6) . . . . ?
C8 C6 C7 C2 173.6(4) . . . . ?
C3 C2 C7 C6 1.8(6) . . . . ?
C1 C2 C7 C6 179.5(4) . . . . ?
C5 C6 C8 C11 126.3(4) . . . . ?
C7 C6 C8 C11 -49.3(5) . . . . ?
C5 C6 C8 C9 -47.0(6) . . . . ?
C7 C6 C8 C9 137.4(4) . . . . ?
C11 C8 C9 C11 -1.2(6) . . . 9_556 ?
C6 C8 C9 C11 172.1(4) . . . 9_556 ?
C11 C8 C9 C10 170.6(4) . . . . ?
C6 C8 C9 C10 -16.1(6) . . . . ?
C11 C9 C10 O4 134.2(4) 9_556 . . 16_557 ?
C8 C9 C10 O4 -37.7(6) . . . 16_557 ?
C11 C9 C10 O3 -42.6(6) 9_556 . . 10_557 ?
C8 C9 C10 O3 145.4(4) . . . 10_557 ?
C9 C8 C11 C9 1.2(7) . . . 9_556 ?
C6 C8 C11 C9 -172.4(4) . . . 9_556 ?

_diffrn_measured_fraction_theta_max 0.995
_diffrn_reflns_theta_full        25.08
_diffrn_measured_fraction_theta_full 0.995
_refine_diff_density_max         1.671
_refine_diff_density_min         -0.548
_refine_diff_density_rms         0.118
