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


data_960383(1)

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C18 H16 Cd2 N6 O7'
_chemical_formula_weight         653.17

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Tetragonal
_symmetry_space_group_name_H-M   P4(2)/n

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

_cell_length_a                   20.872(8)
_cell_length_b                   20.872(8)
_cell_length_c                   5.882(2)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     2562.4(16)
_cell_formula_units_Z            4
_cell_measurement_temperature    298(2)
_cell_measurement_reflns_used    1332
_cell_measurement_theta_min      2.76
_cell_measurement_theta_max      21.17

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.11
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.693
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1272
_exptl_absorpt_coefficient_mu    1.705
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.7055
_exptl_absorpt_correction_T_max  0.8346
_exptl_absorpt_process_details   
; 
SADABS (Sheldrick, G. M. (1998)). 
Program for Absorption Correction. 
University of Göttingen, Germany. 
;

_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  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            11891
_diffrn_reflns_av_R_equivalents  0.0683
_diffrn_reflns_av_sigmaI/netI    0.0477
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_l_min       -6
_diffrn_reflns_limit_l_max       5
_diffrn_reflns_theta_min         1.38
_diffrn_reflns_theta_max         24.68
_reflns_number_total             2173
_reflns_number_gt                1530
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_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)+(0.0725P)²+1.3529P] 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       0.00059(18)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         2173
_refine_ls_number_parameters     167
_refine_ls_number_restraints     4
_refine_ls_R_factor_all          0.0657
_refine_ls_R_factor_gt           0.0429
_refine_ls_wR_factor_ref         0.1351
_refine_ls_wR_factor_gt          0.1184
_refine_ls_goodness_of_fit_ref   1.089
_refine_ls_restrained_S_all      1.088
_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 0.32988(2) 0.76803(2) 0.04003(9) 0.0259(2) Uani 1 1 d . . .
O1 O 0.7011(2) 0.4044(2) 0.1544(8) 0.0403(13) Uani 1 1 d . . .
O2 O 0.6448(3) 0.4001(3) 0.4702(9) 0.0452(14) Uani 1 1 d . . .
O3 O 0.31242(19) 0.7666(2) -0.3346(8) 0.0238(10) Uani 1 1 d D . .
H3 H 0.345(3) 0.777(4) -0.411(14) 0.06(3) Uiso 1 1 d D . .
O4 O 0.610(2) 0.7584(16) 0.115(10) 0.51(6) Uani 0.50 1 d PD . .
H4A H 0.614(6) 0.761(4) 0.257(9) 0.53(3) Uiso 0.50 1 d PD . .
H4B H 0.612(7) 0.793(4) 0.040(12) 0.55(4) Uiso 0.50 1 d PD . .
N1 N 0.4201(3) 0.7002(3) -0.0360(10) 0.0375(15) Uani 1 1 d . . .
N2 N 0.5057(3) 0.6593(3) -0.2176(12) 0.0521(18) Uani 1 1 d . . .
N3 N 0.4984(3) 0.6320(3) -0.0089(10) 0.0379(15) Uani 1 1 d . . .
C1 C 0.4472(3) 0.6567(3) 0.0951(13) 0.0389(18) Uani 1 1 d . . .
H1 H 0.4327 0.6449 0.2388 0.047 Uiso 1 1 calc R . .
C2 C 0.4577(3) 0.7007(3) -0.2268(15) 0.046(2) Uani 1 1 d . . .
H2 H 0.4503 0.7275 -0.3504 0.055 Uiso 1 1 calc R . .
C3 C 0.5412(4) 0.5823(3) 0.0683(13) 0.0386(19) Uani 1 1 d . . .
C4 C 0.5364(5) 0.5594(5) 0.2789(16) 0.107(5) Uani 1 1 d . . .
H4 H 0.5079 0.5773 0.3824 0.129 Uiso 1 1 calc R . .
C5 C 0.5748(5) 0.5081(5) 0.3405(17) 0.104(5) Uani 1 1 d . . .
H5 H 0.5710 0.4922 0.4876 0.125 Uiso 1 1 calc R . .
C6 C 0.6170(3) 0.4801(3) 0.2009(12) 0.0343(17) Uani 1 1 d . . .
C7 C 0.6206(5) 0.5037(5) -0.0073(16) 0.082(4) Uani 1 1 d . . .
H7 H 0.6491 0.4854 -0.1101 0.098 Uiso 1 1 calc R . .
C8 C 0.5821(5) 0.5561(5) -0.0786(17) 0.093(4) Uani 1 1 d . . .
H8 H 0.5855 0.5719 -0.2259 0.111 Uiso 1 1 calc R . .
C9 C 0.6577(3) 0.4251(3) 0.2794(13) 0.0340(17) 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 O3 2.234(5) . ?
Cd1 O3 2.259(4) 3_465 ?
Cd1 O3 2.337(4) 2_655 ?
Cd1 O2 2.338(5) 6_576 ?
Cd1 N1 2.398(6) . ?
Cd1 O1 2.463(5) 6_576 ?
Cd1 C9 2.734(7) 6_576 ?
Cd1 Cd1 3.4183(15) 4_565 ?
O1 C9 1.244(8) . ?
O1 Cd1 2.463(5) 7_756 ?
O2 C9 1.266(8) . ?
O2 Cd1 2.338(5) 7_756 ?
O3 Cd1 2.259(4) 2_654 ?
O3 Cd1 2.337(4) 3_464 ?
O3 H3 0.835(10) . ?
O4 H4A 0.841(10) . ?
O4 H4B 0.840(10) . ?
N1 C1 1.319(9) . ?
N1 C2 1.370(10) . ?
N2 C2 1.324(8) . ?
N2 N3 1.362(9) . ?
N3 C1 1.335(9) . ?
N3 C3 1.441(9) . ?
C1 H1 0.9300 . ?
C2 H2 0.9300 . ?
C3 C4 1.332(11) . ?
C3 C8 1.333(11) . ?
C4 C5 1.385(11) . ?
C4 H4 0.9300 . ?
C5 C6 1.339(11) . ?
C5 H5 0.9300 . ?
C6 C7 1.322(11) . ?
C6 C9 1.502(9) . ?
C7 C8 1.421(11) . ?
C7 H7 0.9300 . ?
C8 H8 0.9300 . ?
C9 Cd1 2.734(7) 7_756 ?

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 O3 102.53(16) . 3_465 ?
O3 Cd1 O3 100.12(15) . 2_655 ?
O3 Cd1 O3 71.83(17) 3_465 2_655 ?
O3 Cd1 O2 94.99(17) . 6_576 ?
O3 Cd1 O2 162.42(17) 3_465 6_576 ?
O3 Cd1 O2 103.91(17) 2_655 6_576 ?
O3 Cd1 N1 86.36(18) . . ?
O3 Cd1 N1 94.63(18) 3_465 . ?
O3 Cd1 N1 165.90(18) 2_655 . ?
O2 Cd1 N1 87.83(18) 6_576 . ?
O3 Cd1 O1 145.74(15) . 6_576 ?
O3 Cd1 O1 108.96(16) 3_465 6_576 ?
O3 Cd1 O1 102.16(15) 2_655 6_576 ?
O2 Cd1 O1 54.50(17) 6_576 6_576 ?
N1 Cd1 O1 78.13(18) . 6_576 ?
O3 Cd1 C9 120.6(2) . 6_576 ?
O3 Cd1 C9 136.0(2) 3_465 6_576 ?
O3 Cd1 C9 106.21(18) 2_655 6_576 ?
O2 Cd1 C9 27.51(19) 6_576 6_576 ?
N1 Cd1 C9 80.6(2) . 6_576 ?
O1 Cd1 C9 27.07(18) 6_576 6_576 ?
O3 Cd1 Cd1 80.68(11) . 4_565 ?
O3 Cd1 Cd1 42.83(11) 3_465 4_565 ?
O3 Cd1 Cd1 41.09(10) 2_655 4_565 ?
O2 Cd1 Cd1 141.56(14) 6_576 4_565 ?
N1 Cd1 Cd1 129.49(15) . 4_565 ?
O1 Cd1 Cd1 132.35(11) 6_576 4_565 ?
C9 Cd1 Cd1 146.47(15) 6_576 4_565 ?
C9 O1 Cd1 88.7(4) . 7_756 ?
C9 O2 Cd1 93.9(4) . 7_756 ?
Cd1 O3 Cd1 115.82(19) . 2_654 ?
Cd1 O3 Cd1 112.78(18) . 3_464 ?
Cd1 O3 Cd1 96.08(16) 2_654 3_464 ?
Cd1 O3 H3 113(7) . . ?
Cd1 O3 H3 105(6) 2_654 . ?
Cd1 O3 H3 112(6) 3_464 . ?
H4A O4 H4B 118(3) . . ?
C1 N1 C2 103.8(6) . . ?
C1 N1 Cd1 129.4(5) . . ?
C2 N1 Cd1 126.7(5) . . ?
C2 N2 N3 103.0(6) . . ?
C1 N3 N2 109.9(6) . . ?
C1 N3 C3 128.9(6) . . ?
N2 N3 C3 121.1(6) . . ?
N1 C1 N3 109.9(7) . . ?
N1 C1 H1 125.0 . . ?
N3 C1 H1 125.0 . . ?
N2 C2 N1 113.3(7) . . ?
N2 C2 H2 123.4 . . ?
N1 C2 H2 123.4 . . ?
C4 C3 C8 120.2(7) . . ?
C4 C3 N3 120.4(7) . . ?
C8 C3 N3 119.2(7) . . ?
C3 C4 C5 118.5(8) . . ?
C3 C4 H4 120.7 . . ?
C5 C4 H4 120.7 . . ?
C6 C5 C4 123.9(9) . . ?
C6 C5 H5 118.1 . . ?
C4 C5 H5 118.1 . . ?
C7 C6 C5 116.3(7) . . ?
C7 C6 C9 122.5(7) . . ?
C5 C6 C9 121.2(7) . . ?
C6 C7 C8 121.9(8) . . ?
C6 C7 H7 119.1 . . ?
C8 C7 H7 119.1 . . ?
C3 C8 C7 119.2(8) . . ?
C3 C8 H8 120.4 . . ?
C7 C8 H8 120.4 . . ?
O1 C9 O2 122.5(7) . . ?
O1 C9 C6 119.7(6) . . ?
O2 C9 C6 117.8(6) . . ?
O1 C9 Cd1 64.2(4) . 7_756 ?
O2 C9 Cd1 58.5(4) . 7_756 ?
C6 C9 Cd1 174.9(5) . 7_756 ?

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 O3 Cd1 90.78(7) 3_465 . . 2_654 ?
O3 Cd1 O3 Cd1 17.3(2) 2_655 . . 2_654 ?
O2 Cd1 O3 Cd1 -87.8(2) 6_576 . . 2_654 ?
N1 Cd1 O3 Cd1 -175.3(2) . . . 2_654 ?
O1 Cd1 O3 Cd1 -112.6(3) 6_576 . . 2_654 ?
C9 Cd1 O3 Cd1 -98.5(2) 6_576 . . 2_654 ?
Cd1 Cd1 O3 Cd1 53.71(16) 4_565 . . 2_654 ?
O3 Cd1 O3 Cd1 -18.5(2) 3_465 . . 3_464 ?
O3 Cd1 O3 Cd1 -91.99(5) 2_655 . . 3_464 ?
O2 Cd1 O3 Cd1 162.9(2) 6_576 . . 3_464 ?
N1 Cd1 O3 Cd1 75.4(2) . . . 3_464 ?
O1 Cd1 O3 Cd1 138.0(2) 6_576 . . 3_464 ?
C9 Cd1 O3 Cd1 152.22(19) 6_576 . . 3_464 ?
Cd1 Cd1 O3 Cd1 -55.61(14) 4_565 . . 3_464 ?
O3 Cd1 N1 C1 -151.5(6) . . . . ?
O3 Cd1 N1 C1 -49.2(6) 3_465 . . . ?
O3 Cd1 N1 C1 -33.5(12) 2_655 . . . ?
O2 Cd1 N1 C1 113.4(6) 6_576 . . . ?
O1 Cd1 N1 C1 59.2(6) 6_576 . . . ?
C9 Cd1 N1 C1 86.7(6) 6_576 . . . ?
Cd1 Cd1 N1 C1 -76.7(7) 4_565 . . . ?
O3 Cd1 N1 C2 32.2(6) . . . . ?
O3 Cd1 N1 C2 134.5(6) 3_465 . . . ?
O3 Cd1 N1 C2 150.3(6) 2_655 . . . ?
O2 Cd1 N1 C2 -62.9(6) 6_576 . . . ?
O1 Cd1 N1 C2 -117.1(6) 6_576 . . . ?
C9 Cd1 N1 C2 -89.6(6) 6_576 . . . ?
Cd1 Cd1 N1 C2 107.0(6) 4_565 . . . ?
C2 N2 N3 C1 0.9(8) . . . . ?
C2 N2 N3 C3 178.8(7) . . . . ?
C2 N1 C1 N3 0.1(8) . . . . ?
Cd1 N1 C1 N3 -176.9(5) . . . . ?
N2 N3 C1 N1 -0.6(9) . . . . ?
C3 N3 C1 N1 -178.3(7) . . . . ?
N3 N2 C2 N1 -0.9(9) . . . . ?
C1 N1 C2 N2 0.6(9) . . . . ?
Cd1 N1 C2 N2 177.6(5) . . . . ?
C1 N3 C3 C4 -7.5(14) . . . . ?
N2 N3 C3 C4 175.1(9) . . . . ?
C1 N3 C3 C8 167.3(9) . . . . ?
N2 N3 C3 C8 -10.1(12) . . . . ?
C8 C3 C4 C5 0.1(19) . . . . ?
N3 C3 C4 C5 174.8(10) . . . . ?
C3 C4 C5 C6 0(2) . . . . ?
C4 C5 C6 C7 -0.6(18) . . . . ?
C4 C5 C6 C9 179.4(11) . . . . ?
C5 C6 C7 C8 0.5(17) . . . . ?
C9 C6 C7 C8 -179.5(10) . . . . ?
C4 C3 C8 C7 -0.2(18) . . . . ?
N3 C3 C8 C7 -175.0(10) . . . . ?
C6 C7 C8 C3 -0.1(19) . . . . ?
Cd1 O1 C9 O2 -6.0(7) 7_756 . . . ?
Cd1 O1 C9 C6 176.2(6) 7_756 . . . ?
Cd1 O2 C9 O1 6.3(7) 7_756 . . . ?
Cd1 O2 C9 C6 -175.8(5) 7_756 . . . ?
C7 C6 C9 O1 7.5(12) . . . . ?
C5 C6 C9 O1 -172.5(9) . . . . ?
C7 C6 C9 O2 -170.4(9) . . . . ?
C5 C6 C9 O2 9.6(12) . . . . ?
C7 C6 C9 Cd1 146(5) . . . 7_756 ?
C5 C6 C9 Cd1 -34(6) . . . 7_756 ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O3 H3 O1 0.835(10) 1.95(3) 2.770(6) 165(9) 6_575

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        24.68
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         0.847
_refine_diff_density_min         -0.663
_refine_diff_density_rms         0.149
_database_code_depnum_ccdc_archive 'CCDC 960383'
##################### END ######################

data_946743(1a)

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C9 H7 Cd N3 O3'
_chemical_formula_weight         317.58

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

_symmetry_cell_setting           Tetragonal
_symmetry_space_group_name_H-M   P4(2)/n

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

_cell_length_a                   20.8164(13)
_cell_length_b                   20.8164(13)
_cell_length_c                   5.8701(4)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     2543.6(3)
_cell_formula_units_Z            8
_cell_measurement_temperature    298(2)
_cell_measurement_reflns_used    3009
_cell_measurement_theta_min      2.77
_cell_measurement_theta_max      26.43

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.659
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1232
_exptl_absorpt_coefficient_mu    1.712
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.7258
_exptl_absorpt_correction_T_max  0.8474
_exptl_absorpt_process_details   'SADABS (Shekldrick, 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  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            2288
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0264
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_limit_l_max       7
_diffrn_reflns_theta_min         1.38
_diffrn_reflns_theta_max         25.25
_reflns_number_total             2288
_reflns_number_gt                1831
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_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)+(0.0460P)²+3.0413P] 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         2288
_refine_ls_number_parameters     136
_refine_ls_number_restraints     48
_refine_ls_R_factor_all          0.0390
_refine_ls_R_factor_gt           0.0313
_refine_ls_wR_factor_ref         0.0904
_refine_ls_wR_factor_gt          0.0865
_refine_ls_goodness_of_fit_ref   1.081
_refine_ls_restrained_S_all      1.127
_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 0.268443(14) 0.670339(14) 0.03871(6) 0.02415(14) Uani 1 1 d . . .
O1 O -0.09574(14) 0.29904(15) 0.1571(5) 0.0365(8) Uani 1 1 d . . .
O2 O -0.09994(17) 0.35617(17) 0.4722(6) 0.0414(9) Uani 1 1 d . . .
O3 O 0.18788(13) 0.73321(13) 0.1640(5) 0.0238(7) Uani 1 1 d . . .
H3A H 0.158(2) 0.717(2) 0.088(10) 0.036 Uiso 1 1 d . . .
N1 N 0.13348(19) 0.50081(18) -0.0069(7) 0.0331(9) Uani 1 1 d . . .
N2 N 0.1611(2) 0.4934(2) -0.2172(8) 0.0469(11) Uani 1 1 d . . .
N3 N 0.20113(18) 0.58004(18) -0.0367(7) 0.0322(9) Uani 1 1 d . . .
C1 C -0.0752(2) 0.3433(2) 0.2816(9) 0.0310(10) Uani 1 1 d . . .
C3 C 0.0048(2) 0.3778(2) -0.0164(5) 0.081(2) Uani 1 1 d GU . .
H3 H -0.0137 0.3490 -0.1183 0.097 Uiso 1 1 calc R . .
C2 C -0.01870(15) 0.38258(16) 0.2045(5) 0.0315(10) Uani 1 1 d GU . .
C7 C 0.0090(2) 0.4255(2) 0.3568(5) 0.103(3) Uani 1 1 d GU . .
H7 H -0.0067 0.4288 0.5046 0.124 Uiso 1 1 calc R . .
C6 C 0.0603(2) 0.4637(2) 0.2881(5) 0.108(3) Uani 1 1 d GU . .
H6 H 0.0789 0.4924 0.3899 0.129 Uiso 1 1 calc R . .
C5 C 0.08385(16) 0.45885(17) 0.0671(6) 0.0341(11) Uani 1 1 d GU . .
C4 C 0.0561(2) 0.4159(2) -0.0851(5) 0.088(3) Uani 1 1 d GU . .
H4 H 0.0718 0.4127 -0.2329 0.105 Uiso 1 1 calc R . .
C8 C 0.2016(2) 0.5423(2) -0.2254(10) 0.0426(13) Uani 1 1 d . . .
H8 H 0.2281 0.5502 -0.3498 0.051 Uiso 1 1 calc R . .
C9 C 0.1574(2) 0.5528(2) 0.0935(9) 0.0352(11) Uani 1 1 d . . .
H9 H 0.1450 0.5678 0.2360 0.042 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 2.230(3) 3_654 ?
Cd1 O3 2.251(3) . ?
Cd1 O3 2.323(3) 2_565 ?
Cd1 O2 2.342(3) 7_566 ?
Cd1 N3 2.386(4) . ?
Cd1 O1 2.451(3) 7_566 ?
Cd1 C1 2.733(4) 7_566 ?
Cd1 Cd1 3.4042(6) 2_565 ?
O1 C1 1.252(5) . ?
O1 Cd1 2.451(3) 8_656 ?
O2 C1 1.260(6) . ?
O2 Cd1 2.342(3) 8_656 ?
O3 Cd1 2.230(3) 4_465 ?
O3 Cd1 2.323(3) 2_565 ?
O3 H3A 0.84(5) . ?
N1 C9 1.329(6) . ?
N1 N2 1.370(6) . ?
N1 C5 1.421(4) . ?
N2 C8 1.323(6) . ?
N3 C9 1.317(6) . ?
N3 C8 1.358(6) . ?
C1 C2 1.501(5) . ?
C1 Cd1 2.733(4) 8_656 ?
C3 C2 1.3900 . ?
C3 C4 1.3900 . ?
C3 H3 0.9300 . ?
C2 C7 1.3900 . ?
C7 C6 1.3900 . ?
C7 H7 0.9300 . ?
C6 C5 1.3900 . ?
C6 H6 0.9300 . ?
C5 C4 1.3900 . ?
C4 H4 0.9300 . ?
C8 H8 0.9300 . ?
C9 H9 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 O3 102.45(11) 3_654 . ?
O3 Cd1 O3 100.18(10) 3_654 2_565 ?
O3 Cd1 O3 71.69(12) . 2_565 ?
O3 Cd1 O2 95.02(11) 3_654 7_566 ?
O3 Cd1 O2 162.48(11) . 7_566 ?
O3 Cd1 O2 104.13(12) 2_565 7_566 ?
O3 Cd1 N3 86.39(12) 3_654 . ?
O3 Cd1 N3 94.65(12) . . ?
O3 Cd1 N3 165.77(12) 2_565 . ?
O2 Cd1 N3 87.70(12) 7_566 . ?
O3 Cd1 O1 145.74(10) 3_654 7_566 ?
O3 Cd1 O1 108.91(11) . 7_566 ?
O3 Cd1 O1 102.43(10) 2_565 7_566 ?
O2 Cd1 O1 54.61(11) 7_566 7_566 ?
N3 Cd1 O1 77.79(12) . 7_566 ?
O3 Cd1 C1 120.54(13) 3_654 7_566 ?
O3 Cd1 C1 136.10(13) . 7_566 ?
O3 Cd1 C1 106.33(12) 2_565 7_566 ?
O2 Cd1 C1 27.40(13) 7_566 7_566 ?
N3 Cd1 C1 80.53(13) . 7_566 ?
O1 Cd1 C1 27.27(12) 7_566 7_566 ?
O3 Cd1 Cd1 80.62(7) 3_654 2_565 ?
O3 Cd1 Cd1 42.73(7) . 2_565 ?
O3 Cd1 Cd1 41.10(7) 2_565 2_565 ?
O2 Cd1 Cd1 141.75(9) 7_566 2_565 ?
N3 Cd1 Cd1 129.43(10) . 2_565 ?
O1 Cd1 Cd1 132.53(7) 7_566 2_565 ?
C1 Cd1 Cd1 146.61(9) 7_566 2_565 ?
C1 O1 Cd1 89.0(3) . 8_656 ?
C1 O2 Cd1 93.8(3) . 8_656 ?
Cd1 O3 Cd1 115.80(13) 4_465 . ?
Cd1 O3 Cd1 112.93(13) 4_465 2_565 ?
Cd1 O3 Cd1 96.17(11) . 2_565 ?
Cd1 O3 H3A 113(4) 4_465 . ?
Cd1 O3 H3A 98(3) . . ?
Cd1 O3 H3A 118(4) 2_565 . ?
C9 N1 N2 109.5(4) . . ?
C9 N1 C5 129.6(4) . . ?
N2 N1 C5 120.8(3) . . ?
C8 N2 N1 102.3(4) . . ?
C9 N3 C8 103.2(4) . . ?
C9 N3 Cd1 129.6(3) . . ?
C8 N3 Cd1 127.1(3) . . ?
O1 C1 O2 122.3(4) . . ?
O1 C1 C2 119.5(4) . . ?
O2 C1 C2 118.2(4) . . ?
O1 C1 Cd1 63.7(2) . 8_656 ?
O2 C1 Cd1 58.8(2) . 8_656 ?
C2 C1 Cd1 173.9(3) . 8_656 ?
C2 C3 C4 120.0 . . ?
C2 C3 H3 120.0 . . ?
C4 C3 H3 120.0 . . ?
C7 C2 C3 120.0 . . ?
C7 C2 C1 118.8(3) . . ?
C3 C2 C1 121.2(3) . . ?
C2 C7 C6 120.0 . . ?
C2 C7 H7 120.0 . . ?
C6 C7 H7 120.0 . . ?
C5 C6 C7 120.0 . . ?
C5 C6 H6 120.0 . . ?
C7 C6 H6 120.0 . . ?
C4 C5 C6 120.0 . . ?
C4 C5 N1 120.1(3) . . ?
C6 C5 N1 119.8(3) . . ?
C5 C4 C3 120.0 . . ?
C5 C4 H4 120.0 . . ?
C3 C4 H4 120.0 . . ?
N2 C8 N3 114.3(4) . . ?
N2 C8 H8 122.9 . . ?
N3 C8 H8 122.9 . . ?
N3 C9 N1 110.6(4) . . ?
N3 C9 H9 124.7 . . ?
N1 C9 H9 124.7 . . ?

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 O3 Cd1 179.83(12) 3_654 . . 4_465 ?
O3 Cd1 O3 Cd1 -83.42(10) 2_565 . . 4_465 ?
O2 Cd1 O3 Cd1 -4.6(5) 7_566 . . 4_465 ?
N3 Cd1 O3 Cd1 92.51(15) . . . 4_465 ?
O1 Cd1 O3 Cd1 13.84(16) 7_566 . . 4_465 ?
C1 Cd1 O3 Cd1 11.3(2) 7_566 . . 4_465 ?
Cd1 Cd1 O3 Cd1 -119.17(18) 2_565 . . 4_465 ?
O3 Cd1 O3 Cd1 -61.00(14) 3_654 . . 2_565 ?
O3 Cd1 O3 Cd1 35.76(14) 2_565 . . 2_565 ?
O2 Cd1 O3 Cd1 114.6(4) 7_566 . . 2_565 ?
N3 Cd1 O3 Cd1 -148.32(13) . . . 2_565 ?
O1 Cd1 O3 Cd1 133.01(11) 7_566 . . 2_565 ?
C1 Cd1 O3 Cd1 130.52(15) 7_566 . . 2_565 ?
C9 N1 N2 C8 1.1(5) . . . . ?
C5 N1 N2 C8 177.1(4) . . . . ?
O3 Cd1 N3 C9 -151.0(4) 3_654 . . . ?
O3 Cd1 N3 C9 -48.8(4) . . . . ?
O3 Cd1 N3 C9 -32.9(7) 2_565 . . . ?
O2 Cd1 N3 C9 113.8(4) 7_566 . . . ?
O1 Cd1 N3 C9 59.6(4) 7_566 . . . ?
C1 Cd1 N3 C9 87.2(4) 7_566 . . . ?
Cd1 Cd1 N3 C9 -76.3(4) 2_565 . . . ?
O3 Cd1 N3 C8 32.5(4) 3_654 . . . ?
O3 Cd1 N3 C8 134.7(4) . . . . ?
O3 Cd1 N3 C8 150.6(4) 2_565 . . . ?
O2 Cd1 N3 C8 -62.7(4) 7_566 . . . ?
O1 Cd1 N3 C8 -117.0(4) 7_566 . . . ?
C1 Cd1 N3 C8 -89.3(4) 7_566 . . . ?
Cd1 Cd1 N3 C8 107.2(4) 2_565 . . . ?
Cd1 O1 C1 O2 -5.3(4) 8_656 . . . ?
Cd1 O1 C1 C2 174.2(4) 8_656 . . . ?
Cd1 O2 C1 O1 5.5(5) 8_656 . . . ?
Cd1 O2 C1 C2 -173.9(3) 8_656 . . . ?
C4 C3 C2 C7 0.0 . . . . ?
C4 C3 C2 C1 178.3(4) . . . . ?
O1 C1 C2 C7 -171.3(4) . . . . ?
O2 C1 C2 C7 8.1(6) . . . . ?
Cd1 C1 C2 C7 -51(3) 8_656 . . . ?
O1 C1 C2 C3 10.3(6) . . . . ?
O2 C1 C2 C3 -170.2(4) . . . . ?
Cd1 C1 C2 C3 131(3) 8_656 . . . ?
C3 C2 C7 C6 0.0 . . . . ?
C1 C2 C7 C6 -178.3(4) . . . . ?
C2 C7 C6 C5 0.0 . . . . ?
C7 C6 C5 C4 0.0 . . . . ?
C7 C6 C5 N1 175.9(4) . . . . ?
C9 N1 C5 C4 165.4(4) . . . . ?
N2 N1 C5 C4 -9.6(6) . . . . ?
C9 N1 C5 C6 -10.5(6) . . . . ?
N2 N1 C5 C6 174.5(4) . . . . ?
C6 C5 C4 C3 0.0 . . . . ?
N1 C5 C4 C3 -175.9(4) . . . . ?
C2 C3 C4 C5 0.0 . . . . ?
N1 N2 C8 N3 -0.4(6) . . . . ?
C9 N3 C8 N2 -0.5(6) . . . . ?
Cd1 N3 C8 N2 176.7(3) . . . . ?
C8 N3 C9 N1 1.2(5) . . . . ?
Cd1 N3 C9 N1 -175.9(3) . . . . ?
N2 N1 C9 N3 -1.5(6) . . . . ?
C5 N1 C9 N3 -177.0(4) . . . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O3 H3A O1 0.84(5) 1.97(6) 2.771(4) 161(5) 5_565

_diffrn_measured_fraction_theta_max 1.000
_diffrn_reflns_theta_full        25.25
_diffrn_measured_fraction_theta_full 1.000
_refine_diff_density_max         0.759
_refine_diff_density_min         -0.758
_refine_diff_density_rms         0.096
_database_code_depnum_ccdc_archive 'CCDC 946743'
##################### END ######################


data_960384(1b)

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C9 H7 Cd I N3 O3'
_chemical_formula_weight         444.48

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'
I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Tetragonal
_symmetry_space_group_name_H-M   'P 42/n'

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

_cell_length_a                   21.23(6)
_cell_length_b                   21.23(6)
_cell_length_c                   6.029(17)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     2717(13)
_cell_formula_units_Z            8
_cell_measurement_temperature    298(2)
_cell_measurement_reflns_used    2647
_cell_measurement_theta_min      2.71
_cell_measurement_theta_max      24.53

_exptl_crystal_description       block
_exptl_crystal_colour            brown
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.08
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.173
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1656
_exptl_absorpt_coefficient_mu    3.879
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.483
_exptl_absorpt_correction_T_max  0.733
_exptl_absorpt_process_details   'SADABS (Shekldrick, 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  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            11206
_diffrn_reflns_av_R_equivalents  0.0603
_diffrn_reflns_av_sigmaI/netI    0.0463
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_l_min       -3
_diffrn_reflns_limit_l_max       7
_diffrn_reflns_theta_min         1.92
_diffrn_reflns_theta_max         24.73
_reflns_number_total             2284
_reflns_number_gt                1613
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_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)+(0.1294P)²+2.8496P] 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       0.0042(9)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         2284
_refine_ls_number_parameters     167
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0830
_refine_ls_R_factor_gt           0.0611
_refine_ls_wR_factor_ref         0.2029
_refine_ls_wR_factor_gt          0.1790
_refine_ls_goodness_of_fit_ref   1.086
_refine_ls_restrained_S_all      1.086
_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 0.32981(3) 0.76936(3) 0.96341(13) 0.0348(5) Uani 1 1 d . . .
I1 I 0.7652(12) 0.8640(11) 0.484(3) 0.525(13) Uani 0.50 1 d P . .
I2 I 0.7386(11) 0.8647(14) 0.921(5) 0.70(2) Uani 0.50 1 d P . .
O1 O 0.4002(4) 0.8567(4) 0.9749(13) 0.056(2) Uani 1 1 d . . .
O2 O 0.4040(3) 0.8009(3) 0.6589(12) 0.0508(19) Uani 1 1 d . . .
O3 O 0.3128(3) 0.7674(3) 1.3422(12) 0.0376(16) Uani 1 1 d . . .
H3A H 0.347(5) 0.797(5) 1.34(2) 0.056 Uiso 1 1 d . . .
N1 N 0.6354(5) 1.0009(4) 0.4955(16) 0.050(2) Uani 1 1 d . . .
N2 N 0.6632(5) 0.9922(4) 0.2865(18) 0.063(3) Uani 1 1 d . . .
N3 N 0.7026(4) 1.0799(5) 0.4603(15) 0.049(2) Uani 1 1 d . . .
C1 C 0.4249(6) 0.8448(6) 0.783(2) 0.062(3) Uani 1 1 d U . .
C2 C 0.4821(6) 0.8821(6) 0.707(2) 0.069(2) Uani 1 1 d U . .
C3 C 0.5104(7) 0.9224(7) 0.847(3) 0.086(2) Uani 1 1 d U . .
H3 H 0.4966 0.9237 0.9929 0.103 Uiso 1 1 calc R . .
C4 C 0.5615(7) 0.9641(7) 0.781(2) 0.087(3) Uani 1 1 d U . .
H4 H 0.5776 0.9938 0.8798 0.105 Uiso 1 1 calc R . .
C5 C 0.5856(7) 0.9584(7) 0.567(2) 0.070(2) Uani 1 1 d U . .
C6 C 0.5539(7) 0.9185(7) 0.427(2) 0.083(2) Uani 1 1 d U . .
H6 H 0.5654 0.9172 0.2787 0.100 Uiso 1 1 calc R . .
C7 C 0.5055(8) 0.8802(8) 0.499(2) 0.080(2) Uani 1 1 d U . .
H7 H 0.4881 0.8517 0.3992 0.096 Uiso 1 1 calc R . .
C8 C 0.6586(6) 1.0505(7) 0.595(2) 0.070(3) Uani 1 1 d U . .
H8 H 0.6472 1.0640 0.7358 0.084 Uiso 1 1 calc R . .
C9 C 0.7029(6) 1.0410(6) 0.274(2) 0.063(3) Uani 1 1 d U . .
H9 H 0.7285 1.0483 0.1510 0.076 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 2.309(9) 3_464 ?
Cd1 O3 2.312(10) . ?
Cd1 O3 2.375(9) 2_654 ?
Cd1 O1 2.381(10) . ?
Cd1 N3 2.428(12) 7_757 ?
Cd1 O2 2.510(9) . ?
I1 I2 2.70(3) . ?
I1 I2 3.09(4) 6_577 ?
I2 I1 3.09(4) 7_757 ?
O1 C1 1.297(14) . ?
O2 C1 1.274(13) . ?
O3 Cd1 2.309(9) 2_655 ?
O3 Cd1 2.375(9) 3_465 ?
O3 H3A 0.96(11) . ?
N1 C8 1.307(15) . ?
N1 N2 1.404(14) . ?
N1 C5 1.456(16) . ?
N2 C9 1.337(14) . ?
N3 C8 1.385(15) . ?
N3 C9 1.397(15) . ?
N3 Cd1 2.428(12) 6_577 ?
C1 C2 1.521(16) . ?
C2 C3 1.342(17) . ?
C2 C7 1.348(18) . ?
C3 C4 1.454(18) . ?
C3 H3 0.9300 . ?
C4 C5 1.394(18) . ?
C4 H4 0.9300 . ?
C5 C6 1.373(19) . ?
C6 C7 1.379(19) . ?
C6 H6 0.9300 . ?
C7 H7 0.9300 . ?
C8 H8 0.9300 . ?
C9 H9 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 O3 102.1(3) 3_464 . ?
O3 Cd1 O3 72.4(3) 3_464 2_654 ?
O3 Cd1 O3 100.1(2) . 2_654 ?
O3 Cd1 O1 163.1(3) 3_464 . ?
O3 Cd1 O1 94.8(3) . . ?
O3 Cd1 O1 104.6(3) 2_654 . ?
O3 Cd1 N3 94.1(3) 3_464 7_757 ?
O3 Cd1 N3 85.7(3) . 7_757 ?
O3 Cd1 N3 166.1(3) 2_654 7_757 ?
O1 Cd1 N3 87.4(3) . 7_757 ?
O3 Cd1 O2 109.3(3) 3_464 . ?
O3 Cd1 O2 145.6(2) . . ?
O3 Cd1 O2 102.5(3) 2_654 . ?
O1 Cd1 O2 54.6(3) . . ?
N3 Cd1 O2 78.4(3) 7_757 . ?
I2 I1 I2 88.0(9) . 6_577 ?
I1 I2 I1 109.0(12) . 7_757 ?
C1 O1 Cd1 94.4(7) . . ?
C1 O2 Cd1 89.1(7) . . ?
Cd1 O3 Cd1 114.8(3) 2_655 . ?
Cd1 O3 Cd1 96.2(3) 2_655 3_465 ?
Cd1 O3 Cd1 112.4(3) . 3_465 ?
Cd1 O3 H3A 101(6) 2_655 . ?
Cd1 O3 H3A 83(8) . . ?
Cd1 O3 H3A 150(7) 3_465 . ?
C8 N1 N2 111.0(10) . . ?
C8 N1 C5 129.5(11) . . ?
N2 N1 C5 119.4(9) . . ?
C9 N2 N1 102.5(9) . . ?
C8 N3 C9 102.0(10) . . ?
C8 N3 Cd1 129.7(8) . 6_577 ?
C9 N3 Cd1 128.1(7) . 6_577 ?
O2 C1 O1 121.7(10) . . ?
O2 C1 C2 118.8(11) . . ?
O1 C1 C2 119.4(11) . . ?
C3 C2 C7 116.0(12) . . ?
C3 C2 C1 120.0(12) . . ?
C7 C2 C1 123.9(12) . . ?
C2 C3 C4 123.5(13) . . ?
C2 C3 H3 118.3 . . ?
C4 C3 H3 118.3 . . ?
C5 C4 C3 118.1(13) . . ?
C5 C4 H4 121.0 . . ?
C3 C4 H4 121.0 . . ?
C6 C5 C4 116.3(12) . . ?
C6 C5 N1 123.8(11) . . ?
C4 C5 N1 119.2(11) . . ?
C5 C6 C7 122.4(13) . . ?
C5 C6 H6 118.8 . . ?
C7 C6 H6 118.8 . . ?
C2 C7 C6 123.2(13) . . ?
C2 C7 H7 118.4 . . ?
C6 C7 H7 118.4 . . ?
N1 C8 N3 110.5(11) . . ?
N1 C8 H8 124.8 . . ?
N3 C8 H8 124.8 . . ?
N2 C9 N3 114.0(10) . . ?
N2 C9 H9 123.0 . . ?
N3 C9 H9 123.0 . . ?

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
I2 I1 I2 I1 -88.6(3) 6_577 . . 7_757 ?
O3 Cd1 O1 C1 -20.7(14) 3_464 . . . ?
O3 Cd1 O1 C1 160.3(8) . . . . ?
O3 Cd1 O1 C1 -98.0(8) 2_654 . . . ?
N3 Cd1 O1 C1 74.8(8) 7_757 . . . ?
O2 Cd1 O1 C1 -2.8(7) . . . . ?
O3 Cd1 O2 C1 177.4(7) 3_464 . . . ?
O3 Cd1 O2 C1 -28.0(9) . . . . ?
O3 Cd1 O2 C1 102.0(7) 2_654 . . . ?
O1 Cd1 O2 C1 2.9(7) . . . . ?
N3 Cd1 O2 C1 -92.2(8) 7_757 . . . ?
O3 Cd1 O3 Cd1 -90.80(10) 3_464 . . 2_655 ?
O3 Cd1 O3 Cd1 -16.9(4) 2_654 . . 2_655 ?
O1 Cd1 O3 Cd1 88.9(3) . . . 2_655 ?
N3 Cd1 O3 Cd1 175.9(3) 7_757 . . 2_655 ?
O2 Cd1 O3 Cd1 113.7(4) . . . 2_655 ?
O3 Cd1 O3 Cd1 17.8(4) 3_464 . . 3_465 ?
O3 Cd1 O3 Cd1 91.77(8) 2_654 . . 3_465 ?
O1 Cd1 O3 Cd1 -162.5(3) . . . 3_465 ?
N3 Cd1 O3 Cd1 -75.5(3) 7_757 . . 3_465 ?
O2 Cd1 O3 Cd1 -137.7(4) . . . 3_465 ?
C8 N1 N2 C9 -1.0(14) . . . . ?
C5 N1 N2 C9 176.4(12) . . . . ?
Cd1 O2 C1 O1 -5.0(13) . . . . ?
Cd1 O2 C1 C2 172.3(12) . . . . ?
Cd1 O1 C1 O2 5.3(14) . . . . ?
Cd1 O1 C1 C2 -172.0(11) . . . . ?
O2 C1 C2 C3 -170.7(15) . . . . ?
O1 C1 C2 C3 7(2) . . . . ?
O2 C1 C2 C7 13(2) . . . . ?
O1 C1 C2 C7 -169.6(16) . . . . ?
C7 C2 C3 C4 3(3) . . . . ?
C1 C2 C3 C4 -174.1(15) . . . . ?
C2 C3 C4 C5 -5(3) . . . . ?
C3 C4 C5 C6 7(3) . . . . ?
C3 C4 C5 N1 178.1(14) . . . . ?
C8 N1 C5 C6 161.9(16) . . . . ?
N2 N1 C5 C6 -15(2) . . . . ?
C8 N1 C5 C4 -8(2) . . . . ?
N2 N1 C5 C4 175.1(14) . . . . ?
C4 C5 C6 C7 -8(3) . . . . ?
N1 C5 C6 C7 -177.9(16) . . . . ?
C3 C2 C7 C6 -2(3) . . . . ?
C1 C2 C7 C6 174.1(16) . . . . ?
C5 C6 C7 C2 5(3) . . . . ?
N2 N1 C8 N3 1.3(16) . . . . ?
C5 N1 C8 N3 -175.7(13) . . . . ?
C9 N3 C8 N1 -1.1(14) . . . . ?
Cd1 N3 C8 N1 -176.1(8) 6_577 . . . ?
N1 N2 C9 N3 0.3(14) . . . . ?
C8 N3 C9 N2 0.4(15) . . . . ?
Cd1 N3 C9 N2 175.6(8) 6_577 . . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O3 H3A O2 0.96(11) 2.26(12) 2.812(11) 115(9) 1_556

_diffrn_measured_fraction_theta_max 0.987
_diffrn_reflns_theta_full        24.73
_diffrn_measured_fraction_theta_full 0.987
_refine_diff_density_max         1.098
_refine_diff_density_min         -0.992
_refine_diff_density_rms         0.213
##################### END ######################
_database_code_depnum_ccdc_archive 'CCDC 960384'
