# Electronic Supplementary Material (ESI) for CrystEngComm.
# This journal is © The Royal Society of Chemistry 2015

####################################################################### 
# 
# 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_compd1
_database_code_depnum_ccdc_archive 'CCDC 987561'
_audit_update_record             
;
2014-02-18 deposited with the CCDC.
2015-03-26 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C28 H Cd2 N4 O9'
_chemical_formula_weight         762.13

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           monoclinic
_symmetry_space_group_name_H-M   P21/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                   13.3217(2)
_cell_length_b                   11.7975(2)
_cell_length_c                   23.3963(5)
_cell_angle_alpha                90.00
_cell_angle_beta                 123.480(2)
_cell_angle_gamma                90.00
_cell_volume                     3066.93(10)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    7023
_cell_measurement_theta_min      3.0528
_cell_measurement_theta_max      30.0098

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.651
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1460
_exptl_absorpt_coefficient_mu    1.442
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.89558
_exptl_absorpt_correction_T_max  1.00000
_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  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            10156
_diffrn_reflns_av_R_equivalents  0.0231
_diffrn_reflns_av_sigmaI/netI    0.0355
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         3.06
_diffrn_reflns_theta_max         25.20
_reflns_number_total             5483
_reflns_number_gt                5076
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_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)+(0.0276P)²+10.8918P] 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         5483
_refine_ls_number_parameters     391
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0423
_refine_ls_R_factor_gt           0.0382
_refine_ls_wR_factor_ref         0.0862
_refine_ls_wR_factor_gt          0.0838
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_restrained_S_all      1.041
_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 0.57983(3) 0.72421(3) 0.929063(15) 0.02011(10) Uani 1 1 d . . .
Cd2 Cd 0.93106(3) 0.74785(3) 1.058222(14) 0.01833(10) Uani 1 1 d . . .
C1 C 0.9061(4) 0.6417(4) 0.9223(2) 0.0218(9) Uani 1 1 d . . .
H1 H 0.8890 0.5759 0.9373 0.026 Uiso 1 1 calc R . .
C2 C 0.9019(4) 0.6375(4) 0.8622(2) 0.0194(9) Uani 1 1 d . . .
H2 H 0.8826 0.5703 0.8375 0.023 Uiso 1 1 calc R . .
C3 C 0.9269(4) 0.7353(3) 0.8388(2) 0.0185(8) Uani 1 1 d . . .
C4 C 0.9571(4) 0.8324(4) 0.8788(2) 0.0230(9) Uani 1 1 d . . .
H4 H 0.9758 0.8992 0.8654 0.028 Uiso 1 1 calc R . .
C5 C 0.9592(4) 0.8289(4) 0.9383(2) 0.0248(9) Uani 1 1 d . . .
H5 H 0.9794 0.8946 0.9645 0.030 Uiso 1 1 calc R . .
C6 C 0.9227(4) 0.7367(3) 0.7740(2) 0.0184(8) Uani 1 1 d . . .
C7 C 0.9546(4) 0.6422(4) 0.7516(2) 0.0236(9) Uani 1 1 d . . .
H7 H 0.9781 0.5754 0.7768 0.028 Uiso 1 1 calc R . .
C8 C 0.9508(4) 0.6488(4) 0.6919(2) 0.0241(9) Uani 1 1 d . . .
H8 H 0.9731 0.5853 0.6779 0.029 Uiso 1 1 calc R . .
C9 C 0.8859(4) 0.8329(4) 0.6743(2) 0.0206(9) Uani 1 1 d . . .
H9 H 0.8625 0.8984 0.6479 0.025 Uiso 1 1 calc R . .
C10 C 0.8873(3) 0.8341(3) 0.7336(2) 0.0185(8) Uani 1 1 d . . .
H10 H 0.8650 0.8990 0.7465 0.022 Uiso 1 1 calc R . .
C11 C 0.5703(4) 0.6508(4) 1.0586(2) 0.0302(11) Uani 1 1 d . . .
H11 H 0.5595 0.5804 1.0381 0.036 Uiso 1 1 calc R . .
C12 C 0.5736(4) 0.6568(4) 1.1184(2) 0.0264(10) Uani 1 1 d . . .
H12 H 0.5651 0.5913 1.1376 0.032 Uiso 1 1 calc R . .
C13 C 0.5898(4) 0.7610(4) 1.1500(2) 0.0226(9) Uani 1 1 d . . .
C14 C 0.6006(4) 0.8561(4) 1.1186(2) 0.0258(10) Uani 1 1 d . . .
H14 H 0.6105 0.9277 1.1377 0.031 Uiso 1 1 calc R . .
C15 C 0.5965(4) 0.8425(4) 1.0590(2) 0.0306(10) Uani 1 1 d . . .
H15 H 0.6042 0.9066 1.0386 0.037 Uiso 1 1 calc R . .
O1W O 0.2410(3) 0.5549(3) 0.74430(17) 0.0347(8) Uani 1 1 d G . .
H1WA H 0.2795 0.5947 0.7806 0.052 Uiso 1 1 d G . .
H1WB H 0.2136 0.5976 0.7095 0.052 Uiso 1 1 d G . .
C16 C 0.5939(4) 0.7696(4) 1.2148(2) 0.0209(9) Uani 1 1 d . . .
C17 C 0.6312(4) 0.6770(4) 1.2595(2) 0.0219(9) Uani 1 1 d . . .
H17 H 0.6558 0.6102 1.2498 0.026 Uiso 1 1 calc R . .
C18 C 0.6308(4) 0.6862(4) 1.3179(2) 0.0223(9) Uani 1 1 d . . .
H18 H 0.6566 0.6243 1.3474 0.027 Uiso 1 1 calc R . .
C19 C 0.5611(4) 0.8683(4) 1.2927(2) 0.0249(9) Uani 1 1 d . . .
H19 H 0.5372 0.9339 1.3041 0.030 Uiso 1 1 calc R . .
C20 C 0.5594(4) 0.8676(4) 1.2330(2) 0.0251(9) Uani 1 1 d . . .
H20 H 0.5355 0.9317 1.2053 0.030 Uiso 1 1 calc R . .
N1 N 0.9335(3) 0.7354(3) 0.96024(18) 0.0218(8) Uani 1 1 d . . .
N2 N 0.9166(3) 0.7417(3) 0.65276(17) 0.0195(7) Uani 1 1 d . . .
N3 N 0.5819(3) 0.7419(3) 1.02870(18) 0.0256(8) Uani 1 1 d . . .
N4 N 0.5955(3) 0.7793(3) 1.33469(18) 0.0245(8) Uani 1 1 d . . .
N5 N 1.1745(4) 0.6987(3) 1.13841(19) 0.0289(9) Uani 1 1 d . . .
N6 N 0.7896(4) 0.9429(4) 1.0006(2) 0.0410(11) Uani 1 1 d . . .
N7 N 0.3459(4) 0.8034(4) 0.8543(2) 0.0462(11) Uani 1 1 d . . .
N8 N 0.7245(4) 0.5191(4) 0.9901(2) 0.0464(12) Uani 1 1 d . . .
O1 O 0.8986(3) 0.9477(3) 1.04751(14) 0.0262(7) Uani 1 1 d . . .
O2 O 0.7375(3) 0.8471(3) 0.97824(17) 0.0351(8) Uani 1 1 d . . .
O3 O 0.4355(3) 0.8744(3) 0.88054(19) 0.0394(8) Uani 1 1 d . . .
O4 O 0.3689(3) 0.6989(3) 0.85972(17) 0.0360(8) Uani 1 1 d . . .
O5 O 0.6163(3) 0.5361(3) 0.94207(16) 0.0327(7) Uani 1 1 d . . .
O6 O 0.7987(4) 0.5955(4) 1.0221(2) 0.0559(12) Uani 1 1 d . . .
O7 O 1.0936(3) 0.6218(3) 1.11247(17) 0.0336(8) Uani 1 1 d . . .
O8 O 1.1410(3) 0.8025(3) 1.12823(17) 0.0336(8) Uani 1 1 d . . .
O9 O 0.7189(6) 1.0512(5) 0.9689(3) 0.111(2) Uani 1 1 d . . .
O10 O 0.2201(5) 0.8481(6) 0.8148(4) 0.124(2) Uani 1 1 d . . .
O11 O 0.7647(6) 0.3960(6) 1.0107(4) 0.124(2) Uani 1 1 d . . .
O12 O 1.3042(5) 0.6673(6) 1.1799(3) 0.112(2) Uani 1 1 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 O5 2.256(3) . ?
Cd1 O2 2.274(3) . ?
Cd1 N3 2.325(3) . ?
Cd1 N4 2.330(4) 4_575 ?
Cd1 O4 2.364(3) . ?
Cd1 O3 2.391(3) . ?
Cd2 N1 2.315(3) . ?
Cd2 O6 2.326(3) . ?
Cd2 N2 2.327(3) 4_576 ?
Cd2 O7 2.340(3) . ?
Cd2 O1 2.385(3) . ?
Cd2 O8 2.422(3) . ?
Cd2 O2 2.489(4) . ?
C1 N1 1.336(5) . ?
C1 C2 1.379(6) . ?
C1 H1 0.9300 . ?
C2 C3 1.392(6) . ?
C2 H2 0.9300 . ?
C3 C4 1.391(6) . ?
C3 C6 1.488(5) . ?
C4 C5 1.379(6) . ?
C4 H4 0.9300 . ?
C5 N1 1.339(5) . ?
C5 H5 0.9300 . ?
C6 C10 1.394(6) . ?
C6 C7 1.394(6) . ?
C7 C8 1.371(6) . ?
C7 H7 0.9300 . ?
C8 N2 1.337(5) . ?
C8 H8 0.9300 . ?
C9 N2 1.344(5) . ?
C9 C10 1.376(5) . ?
C9 H9 0.9300 . ?
C10 H10 0.9300 . ?
C11 N3 1.337(6) . ?
C11 C12 1.377(6) . ?
C11 H11 0.9300 . ?
C12 C13 1.389(6) . ?
C12 H12 0.9300 . ?
C13 C14 1.390(6) . ?
C13 C16 1.489(6) . ?
C14 C15 1.375(6) . ?
C14 H14 0.9300 . ?
C15 N3 1.340(6) . ?
C15 H15 0.9300 . ?
O1W H1WA 0.8500 . ?
O1W H1WB 0.8501 . ?
C16 C20 1.394(6) . ?
C16 C17 1.400(6) . ?
C17 C18 1.374(6) . ?
C17 H17 0.9300 . ?
C18 N4 1.336(5) . ?
C18 H18 0.9300 . ?
C19 N4 1.335(5) . ?
C19 C20 1.386(6) . ?
C19 H19 0.9300 . ?
C20 H20 0.9300 . ?
N2 Cd2 2.327(3) 4_575 ?
N4 Cd1 2.330(3) 4_576 ?
N5 O7 1.277(5) . ?
N5 O8 1.281(5) . ?
N5 O12 1.487(6) . ?
N6 O1 1.248(5) . ?
N6 O2 1.278(5) . ?
N6 O9 1.516(7) . ?
N7 O4 1.260(6) . ?
N7 O3 1.302(6) . ?
N7 O10 1.494(7) . ?
N8 O6 1.239(6) . ?
N8 O5 1.262(6) . ?
N8 O11 1.531(8) . ?

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 O2 119.25(12) . . ?
O5 Cd1 N3 94.05(12) . . ?
O2 Cd1 N3 86.49(12) . . ?
O5 Cd1 N4 89.14(12) . 4_575 ?
O2 Cd1 N4 87.15(12) . 4_575 ?
N3 Cd1 N4 173.64(13) . 4_575 ?
O5 Cd1 O4 93.14(12) . . ?
O2 Cd1 O4 147.59(12) . . ?
N3 Cd1 O4 92.96(12) . . ?
N4 Cd1 O4 92.36(12) 4_575 . ?
O5 Cd1 O3 148.21(12) . . ?
O2 Cd1 O3 92.53(12) . . ?
N3 Cd1 O3 88.35(13) . . ?
N4 Cd1 O3 91.84(13) 4_575 . ?
O4 Cd1 O3 55.08(11) . . ?
N1 Cd2 O6 90.78(12) . . ?
N1 Cd2 N2 176.65(12) . 4_576 ?
O6 Cd2 N2 86.67(12) . 4_576 ?
N1 Cd2 O7 89.00(12) . . ?
O6 Cd2 O7 89.74(14) . . ?
N2 Cd2 O7 93.15(12) 4_576 . ?
N1 Cd2 O1 93.41(11) . . ?
O6 Cd2 O1 131.95(14) . . ?
N2 Cd2 O1 86.71(11) 4_576 . ?
O7 Cd2 O1 138.13(11) . . ?
N1 Cd2 O8 92.56(12) . . ?
O6 Cd2 O8 144.36(15) . . ?
N2 Cd2 O8 90.77(12) 4_576 . ?
O7 Cd2 O8 54.88(11) . . ?
O1 Cd2 O8 83.25(11) . . ?
N1 Cd2 O2 81.96(12) . . ?
O6 Cd2 O2 80.04(14) . . ?
N2 Cd2 O2 95.46(11) 4_576 . ?
O7 Cd2 O2 166.20(11) . . ?
O1 Cd2 O2 53.39(10) . . ?
O8 Cd2 O2 135.54(11) . . ?
N1 C1 C2 123.3(4) . . ?
N1 C1 H1 118.3 . . ?
C2 C1 H1 118.3 . . ?
C1 C2 C3 119.2(4) . . ?
C1 C2 H2 120.4 . . ?
C3 C2 H2 120.4 . . ?
C4 C3 C2 117.5(4) . . ?
C4 C3 C6 120.6(4) . . ?
C2 C3 C6 121.8(4) . . ?
C5 C4 C3 119.4(4) . . ?
C5 C4 H4 120.3 . . ?
C3 C4 H4 120.3 . . ?
N1 C5 C4 123.0(4) . . ?
N1 C5 H5 118.5 . . ?
C4 C5 H5 118.5 . . ?
C10 C6 C7 117.6(4) . . ?
C10 C6 C3 120.6(4) . . ?
C7 C6 C3 121.7(4) . . ?
C8 C7 C6 119.3(4) . . ?
C8 C7 H7 120.3 . . ?
C6 C7 H7 120.3 . . ?
N2 C8 C7 123.4(4) . . ?
N2 C8 H8 118.3 . . ?
C7 C8 H8 118.3 . . ?
N2 C9 C10 123.3(4) . . ?
N2 C9 H9 118.4 . . ?
C10 C9 H9 118.4 . . ?
C9 C10 C6 119.1(4) . . ?
C9 C10 H10 120.5 . . ?
C6 C10 H10 120.5 . . ?
N3 C11 C12 122.9(4) . . ?
N3 C11 H11 118.6 . . ?
C12 C11 H11 118.6 . . ?
C11 C12 C13 119.6(4) . . ?
C11 C12 H12 120.2 . . ?
C13 C12 H12 120.2 . . ?
C12 C13 C14 117.7(4) . . ?
C12 C13 C16 120.6(4) . . ?
C14 C13 C16 121.7(4) . . ?
C15 C14 C13 118.9(4) . . ?
C15 C14 H14 120.5 . . ?
C13 C14 H14 120.5 . . ?
N3 C15 C14 123.6(4) . . ?
N3 C15 H15 118.2 . . ?
C14 C15 H15 118.2 . . ?
H1WA O1W H1WB 109.5 . . ?
C20 C16 C17 117.4(4) . . ?
C20 C16 C13 122.2(4) . . ?
C17 C16 C13 120.4(4) . . ?
C18 C17 C16 119.2(4) . . ?
C18 C17 H17 120.4 . . ?
C16 C17 H17 120.4 . . ?
N4 C18 C17 123.5(4) . . ?
N4 C18 H18 118.3 . . ?
C17 C18 H18 118.3 . . ?
N4 C19 C20 123.1(4) . . ?
N4 C19 H19 118.5 . . ?
C20 C19 H19 118.5 . . ?
C19 C20 C16 119.2(4) . . ?
C19 C20 H20 120.4 . . ?
C16 C20 H20 120.4 . . ?
C1 N1 C5 117.5(3) . . ?
C1 N1 Cd2 124.2(3) . . ?
C5 N1 Cd2 118.2(3) . . ?
C8 N2 C9 117.3(3) . . ?
C8 N2 Cd2 121.2(3) . 4_575 ?
C9 N2 Cd2 121.1(3) . 4_575 ?
C11 N3 C15 117.3(4) . . ?
C11 N3 Cd1 120.8(3) . . ?
C15 N3 Cd1 121.9(3) . . ?
C19 N4 C18 117.6(4) . . ?
C19 N4 Cd1 122.5(3) . 4_576 ?
C18 N4 Cd1 119.6(3) . 4_576 ?
O7 N5 O8 118.3(4) . . ?
O7 N5 O12 120.4(4) . . ?
O8 N5 O12 121.3(4) . . ?
O1 N6 O2 120.4(4) . . ?
O1 N6 O9 120.0(5) . . ?
O2 N6 O9 119.6(5) . . ?
O4 N7 O3 118.2(4) . . ?
O4 N7 O10 122.4(5) . . ?
O3 N7 O10 119.3(5) . . ?
O6 N8 O5 124.1(5) . . ?
O6 N8 O11 118.4(5) . . ?
O5 N8 O11 117.4(5) . . ?
N6 O1 Cd2 95.9(3) . . ?
N6 O2 Cd1 155.9(3) . . ?
N6 O2 Cd2 90.3(3) . . ?
Cd1 O2 Cd2 111.41(14) . . ?
N7 O3 Cd1 92.0(3) . . ?
N7 O4 Cd1 94.4(3) . . ?
N8 O5 Cd1 109.4(3) . . ?
N8 O6 Cd2 167.0(3) . . ?
N5 O7 Cd2 95.3(2) . . ?
N5 O8 Cd2 91.4(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
N1 C1 C2 C3 -0.2(6) . . . . ?
C1 C2 C3 C4 1.1(6) . . . . ?
C1 C2 C3 C6 -179.4(4) . . . . ?
C2 C3 C4 C5 -1.1(6) . . . . ?
C6 C3 C4 C5 179.4(4) . . . . ?
C3 C4 C5 N1 0.2(7) . . . . ?
C4 C3 C6 C10 -33.3(6) . . . . ?
C2 C3 C6 C10 147.2(4) . . . . ?
C4 C3 C6 C7 146.3(4) . . . . ?
C2 C3 C6 C7 -33.3(6) . . . . ?
C10 C6 C7 C8 0.5(6) . . . . ?
C3 C6 C7 C8 -179.0(4) . . . . ?
C6 C7 C8 N2 -0.7(7) . . . . ?
N2 C9 C10 C6 0.3(6) . . . . ?
C7 C6 C10 C9 -0.3(6) . . . . ?
C3 C6 C10 C9 179.2(4) . . . . ?
N3 C11 C12 C13 -0.1(7) . . . . ?
C11 C12 C13 C14 0.7(6) . . . . ?
C11 C12 C13 C16 -179.9(4) . . . . ?
C12 C13 C14 C15 -0.8(6) . . . . ?
C16 C13 C14 C15 179.8(4) . . . . ?
C13 C14 C15 N3 0.3(7) . . . . ?
C12 C13 C16 C20 -152.3(4) . . . . ?
C14 C13 C16 C20 27.1(6) . . . . ?
C12 C13 C16 C17 26.5(6) . . . . ?
C14 C13 C16 C17 -154.1(4) . . . . ?
C20 C16 C17 C18 0.7(6) . . . . ?
C13 C16 C17 C18 -178.1(4) . . . . ?
C16 C17 C18 N4 0.6(6) . . . . ?
N4 C19 C20 C16 0.6(7) . . . . ?
C17 C16 C20 C19 -1.3(6) . . . . ?
C13 C16 C20 C19 177.6(4) . . . . ?
C2 C1 N1 C5 -0.7(6) . . . . ?
C2 C1 N1 Cd2 176.4(3) . . . . ?
C4 C5 N1 C1 0.7(6) . . . . ?
C4 C5 N1 Cd2 -176.6(3) . . . . ?
O6 Cd2 N1 C1 -22.7(3) . . . . ?
N2 Cd2 N1 C1 -63(2) 4_576 . . . ?
O7 Cd2 N1 C1 67.0(3) . . . . ?
O1 Cd2 N1 C1 -154.8(3) . . . . ?
O8 Cd2 N1 C1 121.8(3) . . . . ?
O2 Cd2 N1 C1 -102.6(3) . . . . ?
O6 Cd2 N1 C5 154.4(3) . . . . ?
N2 Cd2 N1 C5 114(2) 4_576 . . . ?
O7 Cd2 N1 C5 -115.9(3) . . . . ?
O1 Cd2 N1 C5 22.3(3) . . . . ?
O8 Cd2 N1 C5 -61.1(3) . . . . ?
O2 Cd2 N1 C5 74.6(3) . . . . ?
C7 C8 N2 C9 0.7(6) . . . . ?
C7 C8 N2 Cd2 173.7(3) . . . 4_575 ?
C10 C9 N2 C8 -0.5(6) . . . . ?
C10 C9 N2 Cd2 -173.5(3) . . . 4_575 ?
C12 C11 N3 C15 -0.5(7) . . . . ?
C12 C11 N3 Cd1 178.6(3) . . . . ?
C14 C15 N3 C11 0.3(7) . . . . ?
C14 C15 N3 Cd1 -178.7(3) . . . . ?
O5 Cd1 N3 C11 -17.2(4) . . . . ?
O2 Cd1 N3 C11 -136.3(4) . . . . ?
N4 Cd1 N3 C11 -137.2(11) 4_575 . . . ?
O4 Cd1 N3 C11 76.2(4) . . . . ?
O3 Cd1 N3 C11 131.1(4) . . . . ?
O5 Cd1 N3 C15 161.8(3) . . . . ?
O2 Cd1 N3 C15 42.7(4) . . . . ?
N4 Cd1 N3 C15 41.8(14) 4_575 . . . ?
O4 Cd1 N3 C15 -104.9(4) . . . . ?
O3 Cd1 N3 C15 -50.0(3) . . . . ?
C20 C19 N4 C18 0.7(7) . . . . ?
C20 C19 N4 Cd1 -173.8(3) . . . 4_576 ?
C17 C18 N4 C19 -1.4(6) . . . . ?
C17 C18 N4 Cd1 173.3(3) . . . 4_576 ?
O2 N6 O1 Cd2 1.8(4) . . . . ?
O9 N6 O1 Cd2 -176.9(4) . . . . ?
N1 Cd2 O1 N6 76.3(3) . . . . ?
O6 Cd2 O1 N6 -17.8(3) . . . . ?
N2 Cd2 O1 N6 -100.3(3) 4_576 . . . ?
O7 Cd2 O1 N6 168.6(2) . . . . ?
O8 Cd2 O1 N6 168.5(3) . . . . ?
O2 Cd2 O1 N6 -1.0(2) . . . . ?
O1 N6 O2 Cd1 152.9(5) . . . . ?
O9 N6 O2 Cd1 -28.3(10) . . . . ?
O1 N6 O2 Cd2 -1.7(4) . . . . ?
O9 N6 O2 Cd2 177.0(4) . . . . ?
O5 Cd1 O2 N6 -163.0(7) . . . . ?
N3 Cd1 O2 N6 -70.3(7) . . . . ?
N4 Cd1 O2 N6 109.6(7) 4_575 . . . ?
O4 Cd1 O2 N6 19.7(8) . . . . ?
O3 Cd1 O2 N6 17.9(7) . . . . ?
O5 Cd1 O2 Cd2 -10.32(18) . . . . ?
N3 Cd1 O2 Cd2 82.36(14) . . . . ?
N4 Cd1 O2 Cd2 -97.74(14) 4_575 . . . ?
O4 Cd1 O2 Cd2 172.35(16) . . . . ?
O3 Cd1 O2 Cd2 170.55(14) . . . . ?
N1 Cd2 O2 N6 -99.4(3) . . . . ?
O6 Cd2 O2 N6 168.4(3) . . . . ?
N2 Cd2 O2 N6 82.8(3) 4_576 . . . ?
O7 Cd2 O2 N6 -148.9(4) . . . . ?
O1 Cd2 O2 N6 1.0(2) . . . . ?
O8 Cd2 O2 N6 -13.9(3) . . . . ?
N1 Cd2 O2 Cd1 91.45(14) . . . . ?
O6 Cd2 O2 Cd1 -0.77(13) . . . . ?
N2 Cd2 O2 Cd1 -86.41(14) 4_576 . . . ?
O7 Cd2 O2 Cd1 42.0(5) . . . . ?
O1 Cd2 O2 Cd1 -168.19(19) . . . . ?
O8 Cd2 O2 Cd1 176.89(12) . . . . ?
O4 N7 O3 Cd1 -5.0(5) . . . . ?
O10 N7 O3 Cd1 179.2(5) . . . . ?
O5 Cd1 O3 N7 3.2(4) . . . . ?
O2 Cd1 O3 N7 -178.3(3) . . . . ?
N3 Cd1 O3 N7 -91.9(3) . . . . ?
N4 Cd1 O3 N7 94.5(3) 4_575 . . . ?
O4 Cd1 O3 N7 2.9(3) . . . . ?
O3 N7 O4 Cd1 5.1(5) . . . . ?
O10 N7 O4 Cd1 -179.2(5) . . . . ?
O5 Cd1 O4 N7 177.1(3) . . . . ?
O2 Cd1 O4 N7 -5.2(4) . . . . ?
N3 Cd1 O4 N7 82.9(3) . . . . ?
N4 Cd1 O4 N7 -93.6(3) 4_575 . . . ?
O3 Cd1 O4 N7 -3.0(3) . . . . ?
O6 N8 O5 Cd1 -3.2(5) . . . . ?
O11 N8 O5 Cd1 175.5(4) . . . . ?
O2 Cd1 O5 N8 15.5(3) . . . . ?
N3 Cd1 O5 N8 -72.7(3) . . . . ?
N4 Cd1 O5 N8 101.7(3) 4_575 . . . ?
O4 Cd1 O5 N8 -165.9(3) . . . . ?
O3 Cd1 O5 N8 -166.2(3) . . . . ?
O5 N8 O6 Cd2 -64(2) . . . . ?
O11 N8 O6 Cd2 117.4(18) . . . . ?
N1 Cd2 O6 N8 -16.7(19) . . . . ?
N2 Cd2 O6 N8 161.1(19) 4_576 . . . ?
O7 Cd2 O6 N8 -105.7(19) . . . . ?
O1 Cd2 O6 N8 78.6(19) . . . . ?
O8 Cd2 O6 N8 -112.2(18) . . . . ?
O2 Cd2 O6 N8 65.0(19) . . . . ?
O8 N5 O7 Cd2 1.9(4) . . . . ?
O12 N5 O7 Cd2 -178.7(4) . . . . ?
N1 Cd2 O7 N5 92.8(2) . . . . ?
O6 Cd2 O7 N5 -176.5(2) . . . . ?
N2 Cd2 O7 N5 -89.8(2) 4_576 . . . ?
O1 Cd2 O7 N5 -1.2(3) . . . . ?
O8 Cd2 O7 N5 -1.1(2) . . . . ?
O2 Cd2 O7 N5 141.6(4) . . . . ?
O7 N5 O8 Cd2 -1.8(4) . . . . ?
O12 N5 O8 Cd2 178.7(4) . . . . ?
N1 Cd2 O8 N5 -85.9(2) . . . . ?
O6 Cd2 O8 N5 9.0(3) . . . . ?
N2 Cd2 O8 N5 94.4(2) 4_576 . . . ?
O7 Cd2 O8 N5 1.1(2) . . . . ?
O1 Cd2 O8 N5 -179.0(2) . . . . ?
O2 Cd2 O8 N5 -167.0(2) . . . . ?

_diffrn_measured_fraction_theta_max 0.993
_diffrn_reflns_theta_full        25.20
_diffrn_measured_fraction_theta_full 0.993
_refine_diff_density_max         0.770
_refine_diff_density_min         -0.741
_refine_diff_density_rms         0.098
####################################################################### 
# 
# 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_compd2
_database_code_depnum_ccdc_archive 'CCDC 987562'
_audit_update_record             
;
2014-02-18 deposited with the CCDC.
2015-03-26 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C7 H8 Cd N O7'
_chemical_formula_weight         330.54

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           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                   21.032(2)
_cell_length_b                   7.9734(8)
_cell_length_c                   12.5404(13)
_cell_angle_alpha                90.00
_cell_angle_beta                 110.1920(10)
_cell_angle_gamma                90.00
_cell_volume                     1973.7(4)
_cell_formula_units_Z            8
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    4262
_cell_measurement_theta_min      2.76
_cell_measurement_theta_max      28.37

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.225
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1288
_exptl_absorpt_coefficient_mu    2.234
_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      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  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            4888
_diffrn_reflns_av_R_equivalents  0.0199
_diffrn_reflns_av_sigmaI/netI    0.0215
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         2.06
_diffrn_reflns_theta_max         25.18
_reflns_number_total             1783
_reflns_number_gt                1683
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_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)+(0.0274P)²+5.7363P] 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     SHELXL
_refine_ls_extinction_coef       0.00236(13)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         1783
_refine_ls_number_parameters     148
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0223
_refine_ls_R_factor_gt           0.0209
_refine_ls_wR_factor_ref         0.0543
_refine_ls_wR_factor_gt          0.0534
_refine_ls_goodness_of_fit_ref   0.982
_refine_ls_restrained_S_all      0.982
_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 0.340021(10) 0.11034(2) 0.720920(17) 0.02761(11) Uani 1 1 d . . .
O2 O 0.43078(12) 0.2934(3) 0.8170(2) 0.0445(6) Uani 1 1 d . . .
O1 O 0.33072(11) 0.4028(2) 0.72915(19) 0.0366(5) Uani 1 1 d . . .
C1 C 0.39331(15) 0.4177(3) 0.7852(2) 0.0288(6) Uani 1 1 d . . .
O3 O 0.25590(12) -0.1067(3) 0.6043(2) 0.0441(6) Uani 1 1 d . . .
O4 O 0.22426(12) 0.1494(3) 0.5971(2) 0.0471(6) Uani 1 1 d . . .
N2 N 0.20961(13) 0.0004(4) 0.5659(2) 0.0368(6) Uani 1 1 d . . .
C2 C 0.42337(15) 0.5894(3) 0.8145(2) 0.0275(6) Uani 1 1 d . . .
C5 C 0.47347(15) 0.9068(4) 0.8596(3) 0.0310(6) Uani 1 1 d . . .
H6 H 0.4907 1.0150 0.8751 0.037 Uiso 1 1 calc R . .
C6 C 0.38397(14) 0.7301(3) 0.7743(3) 0.0294(6) Uani 1 1 d . . .
H7 H 0.3386 0.7149 0.7306 0.035 Uiso 1 1 calc R . .
C3 C 0.49104(16) 0.6123(3) 0.8798(3) 0.0307(6) Uani 1 1 d . . .
H4 H 0.5192 0.5204 0.9072 0.037 Uiso 1 1 calc R . .
C4 C 0.51599(15) 0.7738(4) 0.9035(2) 0.0334(7) Uani 1 1 d . . .
H5 H 0.5609 0.7921 0.9485 0.040 Uiso 1 1 calc R . .
N1 N 0.40765(12) 0.8868(3) 0.7949(2) 0.0282(5) Uani 1 1 d . . .
O5 O 0.29007(11) 0.0702(3) 0.86376(18) 0.0347(5) Uani 1 1 d . . .
H5A H 0.2824 0.1664 0.8889 0.052 Uiso 1 1 d R . .
H5B H 0.3171 0.0134 0.9201 0.052 Uiso 1 1 d R . .
O6 O 0.37063(13) 0.1249(3) 0.5588(2) 0.0445(6) Uani 1 1 d . . .
H6A H 0.4139 0.1262 0.5778 0.067 Uiso 1 1 d R . .
H6B H 0.3544 0.2148 0.5220 0.067 Uiso 1 1 d R . .
O7 O 0.15320(12) -0.0371(4) 0.5022(2) 0.0652(8) Uani 1 1 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 N1 2.269(2) 1_545 ?
Cd1 O6 2.337(2) . ?
Cd1 O1 2.345(2) . ?
Cd1 O2 2.374(2) . ?
Cd1 O5 2.390(2) . ?
Cd1 O4 2.414(2) . ?
Cd1 O3 2.545(2) . ?
O2 C1 1.243(4) . ?
O1 C1 1.266(4) . ?
C1 C2 1.499(4) . ?
O3 N2 1.259(3) . ?
O4 N2 1.256(4) . ?
N2 O7 1.217(3) . ?
C2 C6 1.382(4) . ?
C2 C3 1.387(4) . ?
C5 N1 1.351(4) . ?
C5 C4 1.373(4) . ?
C6 N1 1.337(3) . ?
C3 C4 1.384(4) . ?
N1 Cd1 2.269(2) 1_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
N1 Cd1 O6 94.16(9) 1_545 . ?
N1 Cd1 O1 144.38(8) 1_545 . ?
O6 Cd1 O1 92.35(8) . . ?
N1 Cd1 O2 89.69(8) 1_545 . ?
O6 Cd1 O2 89.77(9) . . ?
O1 Cd1 O2 55.33(7) . . ?
N1 Cd1 O5 87.94(8) 1_545 . ?
O6 Cd1 O5 169.29(8) . . ?
O1 Cd1 O5 92.02(8) . . ?
O2 Cd1 O5 100.75(8) . . ?
N1 Cd1 O4 135.66(8) 1_545 . ?
O6 Cd1 O4 87.34(9) . . ?
O1 Cd1 O4 79.57(8) . . ?
O2 Cd1 O4 134.65(8) . . ?
O5 Cd1 O4 83.84(8) . . ?
N1 Cd1 O3 85.08(8) 1_545 . ?
O6 Cd1 O3 83.09(9) . . ?
O1 Cd1 O3 130.50(7) . . ?
O2 Cd1 O3 170.81(8) . . ?
O5 Cd1 O3 86.64(8) . . ?
O4 Cd1 O3 51.05(8) . . ?
C1 O2 Cd1 91.03(19) . . ?
C1 O1 Cd1 91.81(17) . . ?
O2 C1 O1 121.7(3) . . ?
O2 C1 C2 118.8(3) . . ?
O1 C1 C2 119.5(2) . . ?
N2 O3 Cd1 92.92(17) . . ?
N2 O4 Cd1 99.36(17) . . ?
O7 N2 O4 121.0(3) . . ?
O7 N2 O3 122.3(3) . . ?
O4 N2 O3 116.7(3) . . ?
C6 C2 C3 118.2(3) . . ?
C6 C2 C1 120.2(3) . . ?
C3 C2 C1 121.6(3) . . ?
N1 C5 C4 122.7(3) . . ?
N1 C6 C2 123.5(3) . . ?
C4 C3 C2 119.0(3) . . ?
C5 C4 C3 119.1(3) . . ?
C6 N1 C5 117.5(2) . . ?
C6 N1 Cd1 121.06(19) . 1_565 ?
C5 N1 Cd1 121.40(17) . 1_565 ?

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        25.18
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         0.513
_refine_diff_density_min         -0.556
_refine_diff_density_rms         0.076
####################################################################### 
# 
# 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_compd3
_database_code_depnum_ccdc_archive 'CCDC 987563'
_audit_update_record             
;
2014-02-18 deposited with the CCDC.
2015-03-26 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C27 H29 Cd2 N7 O15'
_chemical_formula_weight         916.37

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           monoclinic
_symmetry_space_group_name_H-M   P21/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                   15.5653(18)
_cell_length_b                   15.3856(18)
_cell_length_c                   14.8364(17)
_cell_angle_alpha                90.00
_cell_angle_beta                 109.7250(10)
_cell_angle_gamma                90.00
_cell_volume                     3344.6(7)
_cell_formula_units_Z            4
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    2810
_cell_measurement_theta_min      2.65
_cell_measurement_theta_max      22.61

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.820
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1824
_exptl_absorpt_coefficient_mu    1.353
_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      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  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            14198
_diffrn_reflns_av_R_equivalents  0.0446
_diffrn_reflns_av_sigmaI/netI    0.0513
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         1.39
_diffrn_reflns_theta_max         23.22
_reflns_number_total             4767
_reflns_number_gt                3687
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_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)+(0.1209P)²+39.4230P] 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         4767
_refine_ls_number_parameters     477
_refine_ls_number_restraints     1476
_refine_ls_R_factor_all          0.0846
_refine_ls_R_factor_gt           0.0664
_refine_ls_wR_factor_ref         0.2030
_refine_ls_wR_factor_gt          0.1844
_refine_ls_goodness_of_fit_ref   0.980
_refine_ls_restrained_S_all      1.541
_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 0.62229(8) 0.85035(8) 0.74346(8) 0.0334(5) Uani 1 1 d U . .
Cd2 Cd 0.82242(8) 0.67823(8) 0.76684(8) 0.0308(4) Uani 1 1 d U . .
N1 N 0.4714(9) 0.2545(9) 0.3518(10) 0.038(3) Uani 1 1 d U . .
N2 N 0.7279(9) 0.9431(9) 0.8465(9) 0.036(2) Uani 1 1 d U . .
N3 N 0.7393(9) 0.5756(9) 0.6615(9) 0.033(2) Uani 1 1 d U . .
N4 N 0.8194(8) 0.5952(9) 0.9042(8) 0.030(2) Uani 1 1 d U . .
N5 N 1.0659(9) 1.2286(9) 1.1379(10) 0.038(3) Uani 1 1 d U . .
N6 N 0.3031(19) 0.837(2) 0.668(2) 0.117(7) Uani 1 1 d U . .
N7 N 0.9865(11) 0.6216(12) 0.7302(11) 0.053(3) Uani 1 1 d U . .
C1 C 0.4856(12) 0.3306(11) 0.3181(12) 0.038(3) Uani 1 1 d U . .
H1 H 0.4573 0.3418 0.2532 0.046 Uiso 1 1 calc R . .
C2 C 0.5406(11) 0.3944(11) 0.3748(11) 0.037(3) Uani 1 1 d U . .
H2 H 0.5478 0.4473 0.3480 0.045 Uiso 1 1 calc R . .
C3 C 0.5849(11) 0.3792(11) 0.4718(12) 0.035(3) Uani 1 1 d U . .
C4 C 0.5715(12) 0.2986(12) 0.5049(12) 0.042(3) Uani 1 1 d U . .
H4 H 0.6011 0.2842 0.5687 0.050 Uiso 1 1 calc R . .
C5 C 0.5145(12) 0.2389(12) 0.4443(12) 0.043(3) Uani 1 1 d U . .
H5 H 0.5058 0.1854 0.4691 0.052 Uiso 1 1 calc R . .
C6 C 0.7910(11) 0.9175(11) 0.9279(12) 0.040(3) Uani 1 1 d U . .
H6 H 0.7910 0.8596 0.9458 0.048 Uiso 1 1 calc R . .
C7 C 0.8559(11) 0.9718(12) 0.9869(12) 0.040(3) Uani 1 1 d U . .
H7 H 0.8994 0.9498 1.0418 0.048 Uiso 1 1 calc R . .
C8 C 0.8569(11) 1.0590(11) 0.9648(12) 0.035(3) Uani 1 1 d U . .
C9 C 0.7902(11) 1.0868(12) 0.8809(12) 0.043(3) Uani 1 1 d U . .
H9 H 0.7871 1.1449 0.8632 0.052 Uiso 1 1 calc R . .
C10 C 0.7287(12) 1.0280(12) 0.8242(13) 0.044(3) Uani 1 1 d U . .
H10 H 0.6856 1.0479 0.7678 0.053 Uiso 1 1 calc R . .
C11 C 1.0249(12) 1.2420(13) 1.0438(12) 0.044(3) Uani 1 1 d U . .
H11 H 1.0435 1.2892 1.0157 0.053 Uiso 1 1 calc R . .
C12 C 0.9565(12) 1.1892(12) 0.9867(12) 0.044(3) Uani 1 1 d U . .
H12 H 0.9301 1.2014 0.9218 0.053 Uiso 1 1 calc R . .
C13 C 0.9273(11) 1.1188(11) 1.0253(12) 0.036(3) Uani 1 1 d U . .
C14 C 0.9690(12) 1.1054(13) 1.1233(12) 0.046(3) Uani 1 1 d U . .
H14 H 0.9512 1.0591 1.1532 0.056 Uiso 1 1 calc R . .
C15 C 1.0367(12) 1.1610(12) 1.1757(13) 0.045(3) Uani 1 1 d U . .
H15 H 1.0635 1.1509 1.2411 0.054 Uiso 1 1 calc R . .
C16 C 0.6721(11) 0.5966(11) 0.5806(11) 0.036(3) Uani 1 1 d U . .
H16 H 0.6589 0.6549 0.5662 0.043 Uiso 1 1 calc R . .
C17 C 0.6215(11) 0.5343(11) 0.5177(11) 0.035(3) Uani 1 1 d U . .
H17 H 0.5749 0.5512 0.4625 0.042 Uiso 1 1 calc R . .
C18 C 0.6399(11) 0.4467(11) 0.5366(11) 0.035(3) Uani 1 1 d U . .
C19 C 0.7117(12) 0.4259(11) 0.6190(12) 0.043(3) Uani 1 1 d U . .
H19 H 0.7282 0.3681 0.6334 0.051 Uiso 1 1 calc R . .
C20 C 0.7583(12) 0.4909(12) 0.6794(12) 0.043(3) Uani 1 1 d U . .
H20 H 0.8051 0.4755 0.7352 0.052 Uiso 1 1 calc R . .
C21 C 0.7040(10) 0.7024(11) 0.9049(11) 0.030(2) Uani 1 1 d U . .
C22 C 0.7711(10) 0.6309(10) 0.9550(10) 0.028(2) Uani 1 1 d U . .
C23 C 0.7784(10) 0.6033(10) 1.0466(11) 0.030(2) Uani 1 1 d U . .
C24 C 0.8342(12) 0.5321(12) 1.0827(12) 0.043(3) Uani 1 1 d U . .
H24 H 0.8401 0.5106 1.1430 0.051 Uiso 1 1 calc R . .
C25 C 0.8809(12) 0.4934(11) 1.0294(12) 0.041(3) Uani 1 1 d U . .
H25 H 0.9178 0.4452 1.0527 0.049 Uiso 1 1 calc R . .
C26 C 0.8719(11) 0.5274(11) 0.9413(11) 0.038(3) Uani 1 1 d U . .
H26 H 0.9042 0.5016 0.9059 0.045 Uiso 1 1 calc R . .
C27 C 0.7325(11) 0.6456(11) 1.1107(11) 0.034(3) Uani 1 1 d U . .
O1 O 0.7124(7) 0.7342(7) 0.8284(7) 0.034(2) Uani 1 1 d U . .
O2 O 0.6458(8) 0.7236(9) 0.9397(8) 0.048(3) Uani 1 1 d U . .
O3 O 0.5263(10) 0.8430(11) 0.8335(11) 0.065(3) Uani 1 1 d U . .
H3A H 0.5065 0.7868 0.8405 0.097 Uiso 1 1 d R . .
H3B H 0.4731 0.8749 0.8067 0.097 Uiso 1 1 d R . .
O4 O 0.5116(10) 0.9621(10) 0.6784(10) 0.065(4) Uani 1 1 d U . .
H4A H 0.5365 1.0142 0.6930 0.098 Uiso 1 1 d R . .
H4B H 0.4661 0.9585 0.7013 0.098 Uiso 1 1 d R . .
O5 O 0.6688(9) 0.6022(9) 1.1228(9) 0.050(2) Uani 1 1 d U . .
O6 O 0.7646(9) 0.7139(9) 1.1515(9) 0.055(3) Uani 1 1 d U . .
O7 O 0.9384(10) 0.6802(10) 0.6791(10) 0.059(3) Uani 1 1 d U . .
O8 O 0.9564(9) 0.5821(10) 0.7864(9) 0.058(3) Uani 1 1 d U . .
O12 O 0.3397(19) 0.908(2) 0.651(3) 0.185(7) Uani 1 1 d U . .
O10 O 0.2254(16) 0.818(2) 0.626(3) 0.194(8) Uani 1 1 d U . .
O11 O 0.3517(15) 0.7885(18) 0.7343(17) 0.125(6) Uani 1 1 d U . .
O1W O 0.597(4) 0.449(4) 0.043(4) 0.340(16) Uani 1 1 d GU . .
H1WA H 0.6134 0.4118 0.0099 0.509 Uiso 1 1 d G . .
H1B H 0.6401 0.4854 0.0667 0.509 Uiso 1 1 d G . .
O9 O 1.0606(12) 0.6019(16) 0.7246(15) 0.112(5) Uani 1 1 d U . .
O2W O 0.764(6) 0.185(5) 0.607(10) 0.466(10) Uani 1 1 d U . .
H2WB H 0.7476 0.2317 0.6278 0.6(10) Uani 1 1 d R . .
H2WA H 0.7797 0.1981 0.5592 0.6(9) Uani 1 1 d R . .
O3W O 0.9215(9) 0.3476(8) 0.8237(9) 0.050(3) Uani 1 1 d U . .
H3WB H 0.8975 0.3881 0.8461 0.060 Uiso 1 1 d R . .
H3WA H 0.9793 0.3448 0.8408 0.060 Uiso 1 1 d 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 2.266(12) 4_575 ?
Cd1 N1 2.310(13) 3_666 ?
Cd1 O3 2.318(14) . ?
Cd1 N2 2.320(13) . ?
Cd1 O1 2.357(11) . ?
Cd1 O4 2.395(14) . ?
Cd2 N3 2.290(13) . ?
Cd2 N5 2.327(13) 3_777 ?
Cd2 O6 2.336(12) 4_575 ?
Cd2 O1 2.359(11) . ?
Cd2 N4 2.420(12) . ?
Cd2 O8 2.492(14) . ?
Cd2 O7 2.558(14) . ?
N1 C1 1.32(2) . ?
N1 C5 1.33(2) . ?
N1 Cd1 2.310(13) 3_666 ?
N2 C6 1.33(2) . ?
N2 C10 1.35(2) . ?
N3 C16 1.34(2) . ?
N3 C20 1.34(2) . ?
N4 C26 1.33(2) . ?
N4 C22 1.35(2) . ?
N5 C15 1.33(2) . ?
N5 C11 1.34(2) . ?
N5 Cd2 2.327(13) 3_777 ?
N6 O10 1.20(3) . ?
N6 O11 1.27(3) . ?
N6 O12 1.29(4) . ?
N7 O9 1.22(2) . ?
N7 O8 1.25(2) . ?
N7 O7 1.25(2) . ?
C1 C2 1.38(2) . ?
C2 C3 1.39(2) . ?
C3 C4 1.38(2) . ?
C3 C18 1.48(2) . ?
C4 C5 1.38(2) . ?
C6 C7 1.37(2) . ?
C7 C8 1.38(2) . ?
C8 C9 1.39(2) . ?
C8 C13 1.48(2) . ?
C9 C10 1.38(2) . ?
C11 C12 1.38(2) . ?
C12 C13 1.37(2) . ?
C13 C14 1.39(2) . ?
C14 C15 1.38(2) . ?
C16 C17 1.38(2) . ?
C17 C18 1.39(2) . ?
C18 C19 1.39(2) . ?
C19 C20 1.38(2) . ?
C21 O2 1.229(19) . ?
C21 O1 1.282(19) . ?
C21 C22 1.53(2) . ?
C22 C23 1.39(2) . ?
C23 C24 1.39(2) . ?
C23 C27 1.52(2) . ?
C24 C25 1.38(2) . ?
C25 C26 1.37(2) . ?
C27 O6 1.23(2) . ?
C27 O5 1.26(2) . ?
O5 Cd1 2.266(12) 4_576 ?
O6 Cd2 2.336(12) 4_576 ?

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 N1 92.6(5) 4_575 3_666 ?
O5 Cd1 O3 155.6(6) 4_575 . ?
N1 Cd1 O3 85.5(5) 3_666 . ?
O5 Cd1 N2 88.7(5) 4_575 . ?
N1 Cd1 N2 173.6(5) 3_666 . ?
O3 Cd1 N2 95.8(5) . . ?
O5 Cd1 O1 112.1(4) 4_575 . ?
N1 Cd1 O1 86.4(5) 3_666 . ?
O3 Cd1 O1 92.2(5) . . ?
N2 Cd1 O1 87.3(4) . . ?
O5 Cd1 O4 80.1(5) 4_575 . ?
N1 Cd1 O4 92.0(5) 3_666 . ?
O3 Cd1 O4 75.6(6) . . ?
N2 Cd1 O4 94.4(5) . . ?
O1 Cd1 O4 167.7(5) . . ?
N3 Cd2 N5 166.7(5) . 3_777 ?
N3 Cd2 O6 90.0(5) . 4_575 ?
N5 Cd2 O6 91.8(5) 3_777 4_575 ?
N3 Cd2 O1 101.5(4) . . ?
N5 Cd2 O1 91.7(4) 3_777 . ?
O6 Cd2 O1 82.8(4) 4_575 . ?
N3 Cd2 N4 92.5(4) . . ?
N5 Cd2 N4 92.1(5) 3_777 . ?
O6 Cd2 N4 151.7(5) 4_575 . ?
O1 Cd2 N4 69.1(4) . . ?
N3 Cd2 O8 85.9(5) . . ?
N5 Cd2 O8 82.6(5) 3_777 . ?
O6 Cd2 O8 127.4(5) 4_575 . ?
O1 Cd2 O8 149.3(4) . . ?
N4 Cd2 O8 80.9(4) . . ?
N3 Cd2 O7 89.6(5) . . ?
N5 Cd2 O7 78.0(5) 3_777 . ?
O6 Cd2 O7 77.4(5) 4_575 . ?
O1 Cd2 O7 157.2(4) . . ?
N4 Cd2 O7 130.8(4) . . ?
O8 Cd2 O7 50.2(4) . . ?
C1 N1 C5 117.4(14) . . ?
C1 N1 Cd1 122.6(11) . 3_666 ?
C5 N1 Cd1 120.0(11) . 3_666 ?
C6 N2 C10 116.3(14) . . ?
C6 N2 Cd1 123.8(11) . . ?
C10 N2 Cd1 119.8(11) . . ?
C16 N3 C20 117.7(14) . . ?
C16 N3 Cd2 122.5(11) . . ?
C20 N3 Cd2 119.9(10) . . ?
C26 N4 C22 118.1(13) . . ?
C26 N4 Cd2 125.5(10) . . ?
C22 N4 Cd2 115.4(10) . . ?
C15 N5 C11 116.7(14) . . ?
C15 N5 Cd2 121.0(11) . 3_777 ?
C11 N5 Cd2 122.2(11) . 3_777 ?
O10 N6 O11 119(3) . . ?
O10 N6 O12 123(3) . . ?
O11 N6 O12 118(3) . . ?
O9 N7 O8 120.1(18) . . ?
O9 N7 O7 121.6(17) . . ?
O8 N7 O7 118.3(16) . . ?
N1 C1 C2 123.1(16) . . ?
C1 C2 C3 120.0(16) . . ?
C4 C3 C2 116.0(15) . . ?
C4 C3 C18 121.8(15) . . ?
C2 C3 C18 122.2(16) . . ?
C3 C4 C5 120.7(16) . . ?
N1 C5 C4 122.8(17) . . ?
N2 C6 C7 123.8(17) . . ?
C6 C7 C8 120.2(16) . . ?
C7 C8 C9 116.4(15) . . ?
C7 C8 C13 121.6(16) . . ?
C9 C8 C13 121.9(16) . . ?
C10 C9 C8 120.0(17) . . ?
N2 C10 C9 123.2(17) . . ?
N5 C11 C12 123.1(17) . . ?
C13 C12 C11 120.3(16) . . ?
C12 C13 C14 116.6(15) . . ?
C12 C13 C8 121.3(15) . . ?
C14 C13 C8 122.1(16) . . ?
C15 C14 C13 119.8(17) . . ?
N5 C15 C14 123.5(17) . . ?
N3 C16 C17 122.2(16) . . ?
C16 C17 C18 120.4(15) . . ?
C17 C18 C19 116.9(15) . . ?
C17 C18 C3 121.1(15) . . ?
C19 C18 C3 121.9(16) . . ?
C20 C19 C18 119.8(16) . . ?
N3 C20 C19 123.0(15) . . ?
O2 C21 O1 125.5(15) . . ?
O2 C21 C22 117.8(14) . . ?
O1 C21 C22 116.7(14) . . ?
N4 C22 C23 122.9(14) . . ?
N4 C22 C21 116.1(13) . . ?
C23 C22 C21 120.9(14) . . ?
C24 C23 C22 116.9(15) . . ?
C24 C23 C27 117.6(14) . . ?
C22 C23 C27 125.5(14) . . ?
C25 C24 C23 120.3(16) . . ?
C26 C25 C24 118.5(16) . . ?
N4 C26 C25 123.2(15) . . ?
O6 C27 O5 126.3(16) . . ?
O6 C27 C23 118.4(16) . . ?
O5 C27 C23 115.0(15) . . ?
C21 O1 Cd1 122.9(10) . . ?
C21 O1 Cd2 120.5(10) . . ?
Cd1 O1 Cd2 116.6(4) . . ?
C27 O5 Cd1 114.8(11) . 4_576 ?
C27 O6 Cd2 163.5(12) . 4_576 ?
N7 O7 Cd2 93.7(10) . . ?
N7 O8 Cd2 97.0(11) . . ?

_diffrn_measured_fraction_theta_max 0.996
_diffrn_reflns_theta_full        23.22
_diffrn_measured_fraction_theta_full 0.996
_refine_diff_density_max         1.086
_refine_diff_density_min         -6.952
_refine_diff_density_rms         0.169
####################################################################### 
# 
# 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_c
_database_code_depnum_ccdc_archive 'CCDC 1050812'
_audit_update_record             
;
2015-02-21 deposited with the CCDC.
2015-03-26 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C7 H3 Cd N O4'
_chemical_formula_weight         277.50

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           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                   10.72120(10)
_cell_length_b                   7.72590(10)
_cell_length_c                   8.67800(10)
_cell_angle_alpha                90.00
_cell_angle_beta                 110.0370(10)
_cell_angle_gamma                90.00
_cell_volume                     675.298(13)
_cell_formula_units_Z            4
_cell_measurement_temperature    298(2)
_cell_measurement_reflns_used    2579
_cell_measurement_theta_min      3.32
_cell_measurement_theta_max      29.12

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.18
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.729
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             528
_exptl_absorpt_coefficient_mu    3.206
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.4895
_exptl_absorpt_correction_T_max  0.5961
_exptl_absorpt_process_details   'SADABS (Shldrick, 1996)'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      298(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_reflns_number            3745
_diffrn_reflns_av_R_equivalents  0.0183
_diffrn_reflns_av_sigmaI/netI    0.0202
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_theta_min         3.32
_diffrn_reflns_theta_max         25.50
_reflns_number_total             1253
_reflns_number_gt                1163
_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, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_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)+(0.0311P)²+1.6705P] where P=(Fo²+2Fc²)/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     SHELXL
_refine_ls_extinction_coef       0.0050(6)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         1253
_refine_ls_number_parameters     119
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0255
_refine_ls_R_factor_gt           0.0235
_refine_ls_wR_factor_ref         0.0610
_refine_ls_wR_factor_gt          0.0596
_refine_ls_goodness_of_fit_ref   1.082
_refine_ls_restrained_S_all      1.082
_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 0.36399(3) 1.14230(3) 0.03929(3) 0.01847(14) Uani 1 1 d . . .
O1 O 0.4939(3) 0.6299(4) 0.1897(3) 0.0241(6) Uani 1 1 d . . .
O2 O 0.4406(3) 0.8453(3) 0.0067(3) 0.0237(6) Uani 1 1 d . . .
O3 O 0.2719(3) 0.4014(4) 0.0287(3) 0.0281(7) Uani 1 1 d . . .
O4 O 0.2458(3) 0.3482(3) 0.2673(3) 0.0246(6) Uani 1 1 d . . .
N1 N 0.2452(3) 0.9345(4) 0.1279(4) 0.0175(6) Uani 1 1 d . . .
C1 C 0.4179(4) 0.7424(5) 0.1078(4) 0.0179(8) Uani 1 1 d . . .
C2 C 0.2850(3) 0.7695(5) 0.1296(4) 0.0152(7) Uani 1 1 d . . .
C3 C 0.2117(4) 0.6349(5) 0.1624(4) 0.0181(8) Uani 1 1 d . . .
C4 C 0.2477(4) 0.4470(5) 0.1536(4) 0.0194(8) Uani 1 1 d . . .
C5 C 0.1014(4) 0.6664(4) 0.1981(4) 0.0146(7) Uani 1 1 d . . .
H5 H 0.0520 0.5769 0.2202 0.017 Uiso 1 1 calc R . .
C6 C 0.0663(4) 0.8278(6) 0.2003(6) 0.0302(10) Uani 1 1 d . . .
H6 H -0.0089 0.8525 0.2266 0.036 Uiso 1 1 calc R . .
C7 C 0.1366(4) 0.9645(5) 0.1649(5) 0.0235(8) Uani 1 1 d . . .
H7 H 0.1075 1.0775 0.1671 0.028 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 O3 2.220(3) 1_565 ?
Cd1 O2 2.265(3) 3_675 ?
Cd1 O4 2.266(3) 4_575 ?
Cd1 O1 2.325(3) 2_655 ?
Cd1 N1 2.336(3) . ?
Cd1 O2 2.486(3) . ?
O1 C1 1.236(5) . ?
O1 Cd1 2.325(3) 2_645 ?
O2 C1 1.268(4) . ?
O2 Cd1 2.265(3) 3_675 ?
O3 C4 1.248(4) . ?
O3 Cd1 2.220(3) 1_545 ?
O4 C4 1.253(5) . ?
O4 Cd1 2.266(3) 4_576 ?
N1 C7 1.330(5) . ?
N1 C2 1.343(5) . ?
C1 C2 1.515(5) . ?
C2 C3 1.390(5) . ?
C3 C5 1.344(5) . ?
C3 C4 1.510(5) . ?
C5 C6 1.304(6) . ?
C5 H5 0.9300 . ?
C6 C7 1.392(6) . ?
C6 H6 0.9300 . ?
C7 H7 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
O3 Cd1 O2 112.32(10) 1_565 3_675 ?
O3 Cd1 O4 81.12(10) 1_565 4_575 ?
O2 Cd1 O4 92.08(10) 3_675 4_575 ?
O3 Cd1 O1 101.96(10) 1_565 2_655 ?
O2 Cd1 O1 81.64(10) 3_675 2_655 ?
O4 Cd1 O1 173.66(10) 4_575 2_655 ?
O3 Cd1 N1 110.38(11) 1_565 . ?
O2 Cd1 N1 136.73(10) 3_675 . ?
O4 Cd1 N1 101.04(10) 4_575 . ?
O1 Cd1 N1 83.17(10) 2_655 . ?
O3 Cd1 O2 170.84(10) 1_565 . ?
O2 Cd1 O2 69.96(10) 3_675 . ?
O4 Cd1 O2 89.99(9) 4_575 . ?
O1 Cd1 O2 87.11(10) 2_655 . ?
N1 Cd1 O2 69.02(9) . . ?
C1 O1 Cd1 128.9(2) . 2_645 ?
C1 O2 Cd1 123.9(2) . 3_675 ?
C1 O2 Cd1 110.5(2) . . ?
Cd1 O2 Cd1 110.04(10) 3_675 . ?
C4 O3 Cd1 116.1(2) . 1_545 ?
C4 O4 Cd1 130.3(2) . 4_576 ?
C7 N1 C2 117.6(3) . . ?
C7 N1 Cd1 125.5(3) . . ?
C2 N1 Cd1 116.7(2) . . ?
O1 C1 O2 126.4(3) . . ?
O1 C1 C2 119.2(3) . . ?
O2 C1 C2 114.3(3) . . ?
N1 C2 C3 120.9(3) . . ?
N1 C2 C1 116.0(3) . . ?
C3 C2 C1 122.9(3) . . ?
C5 C3 C2 121.0(3) . . ?
C5 C3 C4 116.5(3) . . ?
C2 C3 C4 122.5(3) . . ?
O3 C4 O4 125.1(4) . . ?
O3 C4 C3 116.6(3) . . ?
O4 C4 C3 118.2(3) . . ?
C6 C5 C3 117.2(3) . . ?
C6 C5 H5 121.4 . . ?
C3 C5 H5 121.4 . . ?
C5 C6 C7 122.8(4) . . ?
C5 C6 H6 118.6 . . ?
C7 C6 H6 118.6 . . ?
N1 C7 C6 120.5(4) . . ?
N1 C7 H7 119.8 . . ?
C6 C7 H7 119.8 . . ?

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
O3 Cd1 O2 C1 -113.6(6) 1_565 . . . ?
O2 Cd1 O2 C1 140.3(3) 3_675 . . . ?
O4 Cd1 O2 C1 -127.5(3) 4_575 . . . ?
O1 Cd1 O2 C1 58.2(3) 2_655 . . . ?
N1 Cd1 O2 C1 -25.6(2) . . . . ?
O3 Cd1 O2 Cd1 106.1(6) 1_565 . . 3_675 ?
O2 Cd1 O2 Cd1 0.0 3_675 . . 3_675 ?
O4 Cd1 O2 Cd1 92.21(12) 4_575 . . 3_675 ?
O1 Cd1 O2 Cd1 -82.15(12) 2_655 . . 3_675 ?
N1 Cd1 O2 Cd1 -165.95(15) . . . 3_675 ?
O3 Cd1 N1 C7 0.9(3) 1_565 . . . ?
O2 Cd1 N1 C7 171.2(3) 3_675 . . . ?
O4 Cd1 N1 C7 -83.6(3) 4_575 . . . ?
O1 Cd1 N1 C7 101.2(3) 2_655 . . . ?
O2 Cd1 N1 C7 -169.3(3) . . . . ?
O3 Cd1 N1 C2 175.7(2) 1_565 . . . ?
O2 Cd1 N1 C2 -13.9(3) 3_675 . . . ?
O4 Cd1 N1 C2 91.2(2) 4_575 . . . ?
O1 Cd1 N1 C2 -84.0(2) 2_655 . . . ?
O2 Cd1 N1 C2 5.5(2) . . . . ?
Cd1 O1 C1 O2 98.0(4) 2_645 . . . ?
Cd1 O1 C1 C2 -79.9(4) 2_645 . . . ?
Cd1 O2 C1 O1 -3.5(5) 3_675 . . . ?
Cd1 O2 C1 O1 -137.3(3) . . . . ?
Cd1 O2 C1 C2 174.4(2) 3_675 . . . ?
Cd1 O2 C1 C2 40.6(3) . . . . ?
C7 N1 C2 C3 2.6(5) . . . . ?
Cd1 N1 C2 C3 -172.7(3) . . . . ?
C7 N1 C2 C1 -172.7(3) . . . . ?
Cd1 N1 C2 C1 12.1(4) . . . . ?
O1 C1 C2 N1 140.4(3) . . . . ?
O2 C1 C2 N1 -37.7(4) . . . . ?
O1 C1 C2 C3 -34.8(5) . . . . ?
O2 C1 C2 C3 147.2(3) . . . . ?
N1 C2 C3 C5 -2.0(5) . . . . ?
C1 C2 C3 C5 172.9(3) . . . . ?
N1 C2 C3 C4 175.5(3) . . . . ?
C1 C2 C3 C4 -9.6(5) . . . . ?
Cd1 O3 C4 O4 -15.2(5) 1_545 . . . ?
Cd1 O3 C4 C3 167.9(2) 1_545 . . . ?
Cd1 O4 C4 O3 122.3(4) 4_576 . . . ?
Cd1 O4 C4 C3 -60.9(5) 4_576 . . . ?
C5 C3 C4 O3 129.8(4) . . . . ?
C2 C3 C4 O3 -47.8(5) . . . . ?
C5 C3 C4 O4 -47.3(5) . . . . ?
C2 C3 C4 O4 135.1(4) . . . . ?
C2 C3 C5 C6 0.1(6) . . . . ?
C4 C3 C5 C6 -177.6(4) . . . . ?
C3 C5 C6 C7 1.1(7) . . . . ?
C2 N1 C7 C6 -1.4(6) . . . . ?
Cd1 N1 C7 C6 173.4(3) . . . . ?
C5 C6 C7 N1 -0.5(7) . . . . ?

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        25.50
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         0.793
_refine_diff_density_min         -1.013
_refine_diff_density_rms         0.116
