# Electronic Supplementary Material for CrystEngComm
# This journal is (c) The Royal Society of Chemistry 2008

data_global
_journal_name_full               CrystEngComm

_journal_coden_Cambridge         1350

_publ_contact_author_name        'Junfeng Bai'
_publ_contact_author_email       BJUNFENG@NJU.EDU.CN

_publ_section_title              
;
An unprecedented nanoscale trilayered polythreading
coordination array hierarchically formed from 2D square grid networks
and induced by protonated 1,2-bis(4-pyridyl)ethane
;
loop_
_publ_author_name
'Junfeng Bai.'
'Bo Zheng.'

data_1
_database_code_depnum_ccdc_archive 'CCDC 693390'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C14 H19 Cd N2 O5, C8 H4 Cd O10'
_chemical_formula_sum            'C22 H23 Cd2 N2 O15'
_chemical_formula_weight         780.24

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

_symmetry_cell_setting           Triclinic
_symmetry_space_group_name_H-M   P-1
_symmetry_space_group_name_Hall  '-P 1'

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   8.2621(10)
_cell_length_b                   8.3419(10)
_cell_length_c                   19.247(2)
_cell_angle_alpha                101.726(2)
_cell_angle_beta                 92.286(2)
_cell_angle_gamma                92.437(2)
_cell_volume                     1296.1(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    291(2)
_cell_measurement_reflns_used    3855
_cell_measurement_theta_min      2.51
_cell_measurement_theta_max      28.26

_exptl_crystal_description       block
_exptl_crystal_colour            red
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.20
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.999
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             770
_exptl_absorpt_coefficient_mu    1.721
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.65
_exptl_absorpt_correction_T_max  0.71
_exptl_absorpt_process_details   'SADABA, (Bruker, 2000)'

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      291(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker Smart Apex CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            7109
_diffrn_reflns_av_R_equivalents  0.0618
_diffrn_reflns_av_sigmaI/netI    0.0568
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_theta_min         2.16
_diffrn_reflns_theta_max         26.00
_reflns_number_total             4994
_reflns_number_gt                4187
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'SMART (Bruker, 2000)'
_computing_cell_refinement       SMART
_computing_data_reduction        'SAINT (Bruker, 2000)'
_computing_structure_solution    'SHELXTL (Bruker, 2000)'
_computing_structure_refinement  SHELXTL
_computing_molecular_graphics    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)+(0.0474P)²+0.0000P] 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     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         4994
_refine_ls_number_parameters     373
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0428
_refine_ls_R_factor_gt           0.0361
_refine_ls_wR_factor_ref         0.0894
_refine_ls_wR_factor_gt          0.0867
_refine_ls_goodness_of_fit_ref   0.986
_refine_ls_restrained_S_all      0.986
_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
C1 C 0.5866(4) 0.5576(5) 0.1913(2) 0.0254(8) Uani 1 1 d . . .
C2 C 0.6563(5) 0.6308(5) 0.2613(2) 0.0260(8) Uani 1 1 d . . .
C3 C 0.8203(5) 0.6120(5) 0.2343(2) 0.0283(9) Uani 1 1 d . . .
C4 C 0.7477(5) 0.5424(5) 0.1628(2) 0.0296(9) Uani 1 1 d . . .
C5 C 0.2461(4) 0.9823(5) 0.2297(2) 0.0257(8) Uani 1 1 d . . .
C6 C 0.1610(5) 1.0152(5) 0.1660(2) 0.0274(9) Uani 1 1 d . . .
C7 C 0.1727(5) 1.1908(5) 0.1983(2) 0.0260(8) Uani 1 1 d . . .
C8 C 0.2585(5) 1.1584(5) 0.2614(2) 0.0276(9) Uani 1 1 d . . .
C9 C 0.3852(4) 0.4440(4) 0.49500(19) 0.0220(8) Uani 1 1 d . . .
C10 C 0.4510(4) 0.6102(4) 0.4957(2) 0.0219(8) Uani 1 1 d . . .
C11 C 0.0469(5) 0.8320(5) 0.6170(2) 0.0348(10) Uani 1 1 d . . .
H11 H -0.0296 0.8665 0.5871 0.042 Uiso 1 1 calc R . .
C12 C 0.1024(5) 0.9398(5) 0.6784(2) 0.0337(10) Uani 1 1 d . . .
H12 H 0.0616 1.0436 0.6897 0.040 Uiso 1 1 calc R . .
C13 C 0.2196(5) 0.8934(5) 0.7235(2) 0.0296(9) Uani 1 1 d . . .
C14 C 0.2747(6) 0.7372(5) 0.7025(2) 0.0380(10) Uani 1 1 d . . .
H14 H 0.3547 0.7007 0.7300 0.046 Uiso 1 1 calc R . .
C15 C 0.2120(5) 0.6363(5) 0.6413(2) 0.0356(10) Uani 1 1 d . . .
H15 H 0.2505 0.5316 0.6288 0.043 Uiso 1 1 calc R . .
C16 C 0.2790(6) 1.0082(6) 0.7902(2) 0.0404(11) Uani 1 1 d . . .
H16A H 0.1963 1.0860 0.8042 0.048 Uiso 1 1 calc R . .
H16B H 0.3744 1.0697 0.7801 0.048 Uiso 1 1 calc R . .
C17 C 0.3209(6) 0.9315(5) 0.8519(2) 0.0420(11) Uani 1 1 d . . .
H17A H 0.4151 0.8667 0.8418 0.050 Uiso 1 1 calc R . .
H17B H 0.2312 0.8590 0.8593 0.050 Uiso 1 1 calc R . .
C18 C 0.3567(6) 1.0634(6) 0.9186(2) 0.0369(10) Uani 1 1 d . . .
C19 C 0.5026(6) 1.1498(6) 0.9326(3) 0.0465(12) Uani 1 1 d . . .
H19 H 0.5849 1.1259 0.9011 0.056 Uiso 1 1 calc R . .
C20 C 0.5298(6) 1.2707(7) 0.9921(3) 0.0508(13) Uani 1 1 d . . .
H20 H 0.6303 1.3274 1.0015 0.061 Uiso 1 1 calc R . .
C21 C 0.2667(6) 1.2282(7) 1.0240(3) 0.0507(13) Uani 1 1 d . . .
H21 H 0.1852 1.2580 1.0554 0.061 Uiso 1 1 calc R . .
C22 C 0.2366(6) 1.1044(6) 0.9659(2) 0.0463(12) Uani 1 1 d . . .
H22 H 0.1357 1.0481 0.9583 0.056 Uiso 1 1 calc R . .
Cd1 Cd 0.20042(3) 0.58677(3) 0.213477(14) 0.02339(10) Uani 1 1 d . . .
Cd2 Cd 0.0000 0.5000 0.5000 0.02482(11) Uani 1 2 d S . .
Cd3 Cd 0.5000 1.0000 0.5000 0.02503(11) Uani 1 2 d S . .
N1 N 0.0985(4) 0.6805(4) 0.59860(17) 0.0293(8) Uani 1 1 d . . .
N2 N 0.4113(5) 1.3061(5) 1.03606(19) 0.0457(10) Uani 1 1 d . . .
H2 H 0.4317 1.3923 1.0696 0.055 Uiso 1 1 d R . .
O1 O 0.4453(3) 0.5188(4) 0.16326(15) 0.0362(7) Uani 1 1 d . . .
O2 O 0.6029(3) 0.6868(4) 0.32095(14) 0.0343(7) Uani 1 1 d . . .
O3 O 0.9582(3) 0.6460(4) 0.26271(15) 0.0348(7) Uani 1 1 d . . .
O4 O 0.7967(3) 0.4917(4) 0.10227(15) 0.0434(8) Uani 1 1 d . . .
O5 O 0.2900(4) 0.8551(3) 0.24996(16) 0.0358(7) Uani 1 1 d . . .
O6 O 0.1051(4) 0.9307(4) 0.10906(15) 0.0395(7) Uani 1 1 d . . .
O7 O 0.1231(3) 1.3154(3) 0.17825(15) 0.0333(7) Uani 1 1 d . . .
O8 O 0.3176(4) 1.2423(3) 0.31827(15) 0.0397(7) Uani 1 1 d . . .
O9 O 0.2458(3) 0.3752(3) 0.48930(14) 0.0253(6) Uani 1 1 d . . .
O10 O 0.3880(3) 0.7411(3) 0.49018(15) 0.0291(6) Uani 1 1 d . . .
O11 O 0.1102(3) 0.6038(4) 0.10232(15) 0.0324(6) Uani 1 1 d . . .
H11B H 0.0167 0.5557 0.0931 0.039 Uiso 1 1 d R . .
H11A H 0.1053 0.7041 0.0998 0.049 Uiso 1 1 d R . .
O12 O 0.2960(3) 0.5633(3) 0.32260(14) 0.0311(6) Uani 1 1 d . . .
H12B H 0.3883 0.6138 0.3319 0.037 Uiso 1 1 d R . .
H12A H 0.3043 0.4625 0.3235 0.047 Uiso 1 1 d R . .
O13 O 0.3739(5) 1.0070(4) 0.39391(17) 0.0586(11) Uani 1 1 d . . .
H13B H 0.4211 0.9456 0.3609 0.070 Uiso 1 1 d R . .
H13A H 0.3781 1.1049 0.3875 0.088 Uiso 1 1 d R . .
O14 O 0.7219(3) 0.8945(4) 0.44485(16) 0.0377(7) Uani 1 1 d . . .
H14B H 0.7739 0.8431 0.4717 0.045 Uiso 1 1 d R . .
H14A H 0.6920 0.8294 0.4061 0.056 Uiso 1 1 d R . .
O15 O 0.0637(4) 0.6990(4) 0.43256(17) 0.0417(7) Uani 1 1 d . . .
H15A H 0.0485 0.6570 0.3886 0.050 Uiso 1 1 d R . .
H15B H 0.1623 0.7328 0.4415 0.063 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
C1 O1 1.267(5) . ?
C1 C2 1.448(5) . ?
C1 C4 1.460(5) . ?
C2 O2 1.254(5) . ?
C2 C3 1.473(5) . ?
C3 O3 1.240(5) . ?
C3 C4 1.474(5) . ?
C4 O4 1.245(5) . ?
C5 O5 1.265(5) . ?
C5 C6 1.468(5) . ?
C5 C8 1.469(5) . ?
C6 O6 1.237(5) . ?
C6 C7 1.468(5) . ?
C7 O7 1.259(4) . ?
C7 C8 1.461(5) . ?
C8 O8 1.242(5) . ?
C9 O9 1.255(4) . ?
C9 C10 1.461(5) 2_666 ?
C9 C10 1.465(5) . ?
C10 O10 1.251(4) . ?
C10 C9 1.461(5) 2_666 ?
C11 N1 1.335(5) . ?
C11 C12 1.381(6) . ?
C11 H11 0.9300 . ?
C12 C13 1.394(6) . ?
C12 H12 0.9300 . ?
C13 C14 1.386(6) . ?
C13 C16 1.489(6) . ?
C14 C15 1.369(6) . ?
C14 H14 0.9300 . ?
C15 N1 1.335(5) . ?
C15 H15 0.9300 . ?
C16 C17 1.494(6) . ?
C16 H16A 0.9700 . ?
C16 H16B 0.9700 . ?
C17 C18 1.522(6) . ?
C17 H17A 0.9700 . ?
C17 H17B 0.9700 . ?
C18 C19 1.366(6) . ?
C18 C22 1.380(6) . ?
C19 C20 1.367(7) . ?
C19 H19 0.9300 . ?
C20 N2 1.324(6) . ?
C20 H20 0.9300 . ?
C21 N2 1.324(6) . ?
C21 C22 1.366(7) . ?
C21 H21 0.9300 . ?
C22 H22 0.9300 . ?
Cd1 O12 2.263(3) . ?
Cd1 O11 2.271(3) . ?
Cd1 O3 2.279(3) 1_455 ?
Cd1 O7 2.282(3) 1_545 ?
Cd1 O5 2.287(3) . ?
Cd1 O1 2.320(3) . ?
Cd2 N1 2.268(3) 2_566 ?
Cd2 N1 2.268(3) . ?
Cd2 O9 2.319(2) . ?
Cd2 O9 2.319(2) 2_566 ?
Cd2 O15 2.361(3) 2_566 ?
Cd2 O15 2.361(3) . ?
Cd3 O13 2.268(3) . ?
Cd3 O13 2.268(3) 2_676 ?
Cd3 O14 2.275(3) . ?
Cd3 O14 2.275(3) 2_676 ?
Cd3 O10 2.281(3) . ?
Cd3 O10 2.281(3) 2_676 ?
N2 H2 0.8688 . ?
O3 Cd1 2.279(3) 1_655 ?
O7 Cd1 2.282(3) 1_565 ?
O11 H11B 0.8500 . ?
O11 H11A 0.8500 . ?
O12 H12B 0.8500 . ?
O12 H12A 0.8501 . ?
O13 H13B 0.8500 . ?
O13 H13A 0.8500 . ?
O14 H14B 0.8501 . ?
O14 H14A 0.8500 . ?
O15 H15A 0.8499 . ?
O15 H15B 0.8501 . ?

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
O1 C1 C2 136.4(4) . . ?
O1 C1 C4 132.6(4) . . ?
C2 C1 C4 91.0(3) . . ?
O2 C2 C1 136.0(4) . . ?
O2 C2 C3 134.0(4) . . ?
C1 C2 C3 90.0(3) . . ?
O3 C3 C2 133.1(4) . . ?
O3 C3 C4 137.4(4) . . ?
C2 C3 C4 89.5(3) . . ?
O4 C4 C1 133.4(4) . . ?
O4 C4 C3 137.1(4) . . ?
C1 C4 C3 89.5(3) . . ?
O5 C5 C6 135.2(4) . . ?
O5 C5 C8 134.2(4) . . ?
C6 C5 C8 90.6(3) . . ?
O6 C6 C5 135.3(4) . . ?
O6 C6 C7 135.5(4) . . ?
C5 C6 C7 89.1(3) . . ?
O7 C7 C8 136.0(4) . . ?
O7 C7 C6 133.1(4) . . ?
C8 C7 C6 90.9(3) . . ?
O8 C8 C7 136.0(4) . . ?
O8 C8 C5 134.7(4) . . ?
C7 C8 C5 89.4(3) . . ?
O9 C9 C10 134.4(3) . 2_666 ?
O9 C9 C10 135.3(3) . . ?
C10 C9 C10 90.3(3) 2_666 . ?
O10 C10 C9 136.7(4) . 2_666 ?
O10 C10 C9 133.6(3) . . ?
C9 C10 C9 89.7(3) 2_666 . ?
N1 C11 C12 122.7(4) . . ?
N1 C11 H11 118.7 . . ?
C12 C11 H11 118.7 . . ?
C11 C12 C13 120.1(4) . . ?
C11 C12 H12 119.9 . . ?
C13 C12 H12 119.9 . . ?
C14 C13 C12 116.2(4) . . ?
C14 C13 C16 123.3(4) . . ?
C12 C13 C16 120.5(4) . . ?
C15 C14 C13 120.3(4) . . ?
C15 C14 H14 119.9 . . ?
C13 C14 H14 119.9 . . ?
N1 C15 C14 123.3(4) . . ?
N1 C15 H15 118.3 . . ?
C14 C15 H15 118.3 . . ?
C13 C16 C17 116.0(4) . . ?
C13 C16 H16A 108.3 . . ?
C17 C16 H16A 108.3 . . ?
C13 C16 H16B 108.3 . . ?
C17 C16 H16B 108.3 . . ?
H16A C16 H16B 107.4 . . ?
C16 C17 C18 110.2(4) . . ?
C16 C17 H17A 109.6 . . ?
C18 C17 H17A 109.6 . . ?
C16 C17 H17B 109.6 . . ?
C18 C17 H17B 109.6 . . ?
H17A C17 H17B 108.1 . . ?
C19 C18 C22 117.7(4) . . ?
C19 C18 C17 122.5(4) . . ?
C22 C18 C17 119.7(4) . . ?
C18 C19 C20 121.2(4) . . ?
C18 C19 H19 119.4 . . ?
C20 C19 H19 119.4 . . ?
N2 C20 C19 119.1(5) . . ?
N2 C20 H20 120.4 . . ?
C19 C20 H20 120.4 . . ?
N2 C21 C22 120.4(5) . . ?
N2 C21 H21 119.8 . . ?
C22 C21 H21 119.8 . . ?
C21 C22 C18 119.6(5) . . ?
C21 C22 H22 120.2 . . ?
C18 C22 H22 120.2 . . ?
O12 Cd1 O11 178.09(10) . . ?
O12 Cd1 O3 87.29(10) . 1_455 ?
O11 Cd1 O3 94.35(10) . 1_455 ?
O12 Cd1 O7 94.46(10) . 1_545 ?
O11 Cd1 O7 84.49(10) . 1_545 ?
O3 Cd1 O7 92.08(10) 1_455 1_545 ?
O12 Cd1 O5 84.00(10) . . ?
O11 Cd1 O5 96.99(10) . . ?
O3 Cd1 O5 90.08(11) 1_455 . ?
O7 Cd1 O5 177.28(10) 1_545 . ?
O12 Cd1 O1 92.41(10) . . ?
O11 Cd1 O1 85.93(10) . . ?
O3 Cd1 O1 178.41(11) 1_455 . ?
O7 Cd1 O1 86.39(11) 1_545 . ?
O5 Cd1 O1 91.44(11) . . ?
N1 Cd2 N1 180.000(1) 2_566 . ?
N1 Cd2 O9 89.12(11) 2_566 . ?
N1 Cd2 O9 90.88(11) . . ?
N1 Cd2 O9 90.88(11) 2_566 2_566 ?
N1 Cd2 O9 89.12(11) . 2_566 ?
O9 Cd2 O9 180.000(1) . 2_566 ?
N1 Cd2 O15 88.58(12) 2_566 2_566 ?
N1 Cd2 O15 91.42(12) . 2_566 ?
O9 Cd2 O15 83.64(9) . 2_566 ?
O9 Cd2 O15 96.36(9) 2_566 2_566 ?
N1 Cd2 O15 91.42(12) 2_566 . ?
N1 Cd2 O15 88.58(12) . . ?
O9 Cd2 O15 96.36(9) . . ?
O9 Cd2 O15 83.64(9) 2_566 . ?
O15 Cd2 O15 180.0 2_566 . ?
O13 Cd3 O13 180.000(1) . 2_676 ?
O13 Cd3 O14 90.95(13) . . ?
O13 Cd3 O14 89.05(13) 2_676 . ?
O13 Cd3 O14 89.05(13) . 2_676 ?
O13 Cd3 O14 90.95(13) 2_676 2_676 ?
O14 Cd3 O14 180.000(1) . 2_676 ?
O13 Cd3 O10 88.31(11) . . ?
O13 Cd3 O10 91.69(11) 2_676 . ?
O14 Cd3 O10 89.84(10) . . ?
O14 Cd3 O10 90.16(10) 2_676 . ?
O13 Cd3 O10 91.69(11) . 2_676 ?
O13 Cd3 O10 88.31(11) 2_676 2_676 ?
O14 Cd3 O10 90.16(10) . 2_676 ?
O14 Cd3 O10 89.84(10) 2_676 2_676 ?
O10 Cd3 O10 180.000(1) . 2_676 ?
C11 N1 C15 117.3(3) . . ?
C11 N1 Cd2 122.7(3) . . ?
C15 N1 Cd2 120.0(3) . . ?
C21 N2 C20 121.9(4) . . ?
C21 N2 H2 122.9 . . ?
C20 N2 H2 114.6 . . ?
C1 O1 Cd1 127.4(2) . . ?
C3 O3 Cd1 127.8(3) . 1_655 ?
C5 O5 Cd1 130.6(3) . . ?
C7 O7 Cd1 131.3(3) . 1_565 ?
C9 O9 Cd2 127.4(2) . . ?
C10 O10 Cd3 131.0(2) . . ?
Cd1 O11 H11B 109.7 . . ?
Cd1 O11 H11A 109.3 . . ?
H11B O11 H11A 109.8 . . ?
Cd1 O12 H12B 109.7 . . ?
Cd1 O12 H12A 109.3 . . ?
H12B O12 H12A 109.8 . . ?
Cd3 O13 H13B 109.3 . . ?
Cd3 O13 H13A 109.4 . . ?
H13B O13 H13A 109.8 . . ?
Cd3 O14 H14B 109.5 . . ?
Cd3 O14 H14A 109.4 . . ?
H14B O14 H14A 109.8 . . ?
Cd2 O15 H15A 109.6 . . ?
Cd2 O15 H15B 109.4 . . ?
H15A O15 H15B 109.8 . . ?

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
O11 H11A O6 0.85 1.86 2.705(4) 171.1 .
O12 H12B O2 0.85 1.88 2.700(4) 160.5 .
O13 H13B O5 0.85 2.32 2.847(4) 120.3 .
O13 H13A O8 0.85 1.99 2.715(4) 142.9 .
O14 H14A O2 0.85 1.92 2.765(4) 174.4 .
O15 H15A O12 0.85 2.52 2.996(4) 116.5 .
O15 H15B O10 0.85 2.05 2.838(4) 155.0 .
N2 H2 O1 0.87 1.89 2.712(5) 157.1 1_566
O11 H11B O4 0.85 1.90 2.716(4) 161.0 1_455
O12 H12A O8 0.85 1.83 2.676(4) 175.7 1_545
O14 H14B O9 0.85 2.11 2.814(4) 140.1 2_666
O15 H15A O3 0.85 2.49 3.286(4) 156.5 1_455

_diffrn_measured_fraction_theta_max 0.981
_diffrn_reflns_theta_full        26.00
_diffrn_measured_fraction_theta_full 0.981
_refine_diff_density_max         0.975
_refine_diff_density_min         -1.519
_refine_diff_density_rms         0.148

data_complex_2
_database_code_depnum_ccdc_archive 'CCDC 693391'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C8 H4 Cd O10, 2(C6 H7 N)'
_chemical_formula_sum            'C20 H18 Cd N2 O10'
_chemical_formula_weight         558.76

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'
Cd Cd -0.8075 1.2024 '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'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Triclinic
_symmetry_space_group_name_H-M   'P -1 '
_symmetry_space_group_name_Hall  '-P 1'

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   8.0087(16)
_cell_length_b                   8.1857(16)
_cell_length_c                   8.3767(17)
_cell_angle_alpha                85.300(2)
_cell_angle_beta                 71.493(2)
_cell_angle_gamma                83.153(2)
_cell_volume                     516.47(18)
_cell_formula_units_Z            1
_cell_measurement_temperature    291(2)
_cell_measurement_reflns_used    1893
_cell_measurement_theta_min      2.57
_cell_measurement_theta_max      27.59

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.20
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.797
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             280
_exptl_absorpt_coefficient_mu    1.120
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.732
_exptl_absorpt_correction_T_max  0.801
_exptl_absorpt_process_details   'SADABA, (Bruker, 2000)'

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      291(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker Smart Apex CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            2631
_diffrn_reflns_av_R_equivalents  0.0450
_diffrn_reflns_av_sigmaI/netI    0.0499
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_theta_min         2.51
_diffrn_reflns_theta_max         25.00
_reflns_number_total             1795
_reflns_number_gt                1772
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'SMART (Bruker, 2000)'
_computing_cell_refinement       SMART
_computing_data_reduction        'SAINT (Bruker, 2000)'
_computing_structure_solution    'SHELXTL (Bruker, 2000)'
_computing_structure_refinement  SHELXTL
_computing_molecular_graphics    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)+(0.0323P)²] 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     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         1795
_refine_ls_number_parameters     151
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0280
_refine_ls_R_factor_gt           0.0269
_refine_ls_wR_factor_ref         0.0663
_refine_ls_wR_factor_gt          0.0660
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_restrained_S_all      1.055
_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
C1 C 0.5429(4) 0.1065(4) 0.5239(4) 0.0293(7) Uani 1 1 d . . .
C2 C 0.6259(4) -0.0601(4) 0.4817(4) 0.0303(7) Uani 1 1 d . . .
C3 C 0.4476(4) 0.5243(4) 0.9024(4) 0.0262(6) Uani 1 1 d . . .
C4 C 0.6272(4) 0.4812(4) 0.9134(4) 0.0279(7) Uani 1 1 d . . .
C5 C 1.0093(5) 0.8264(5) 0.7377(5) 0.0501(10) Uani 1 1 d . . .
H5 H 1.0805 0.8207 0.6259 0.060 Uiso 1 1 calc R . .
C6 C 0.8601(4) 0.9331(5) 0.7789(4) 0.0444(9) Uani 1 1 d . . .
H6 H 0.8324 1.0045 0.6967 0.053 Uiso 1 1 calc R . .
C7 C 0.7501(4) 0.9349(4) 0.9430(4) 0.0334(7) Uani 1 1 d . . .
C8 C 0.5792(4) 1.0466(4) 0.9925(5) 0.0427(8) Uani 1 1 d . . .
H8A H 0.5852 1.1365 0.9085 0.051 Uiso 1 1 calc R . .
H8B H 0.5641 1.0934 1.0995 0.051 Uiso 1 1 calc R . .
C9 C 0.7987(5) 0.8290(5) 1.0613(4) 0.0493(10) Uani 1 1 d . . .
H9 H 0.7256 0.8259 1.1725 0.059 Uiso 1 1 calc R . .
C10 C 0.9534(5) 0.7291(5) 1.0156(5) 0.0535(10) Uani 1 1 d . . .
H10 H 0.9879 0.6607 1.0961 0.064 Uiso 1 1 calc R . .
Cd1 Cd 0.5000 0.5000 0.5000 0.02419(12) Uani 1 2 d S . .
N1 N 1.0541(3) 0.7301(4) 0.8565(4) 0.0466(8) Uani 1 1 d . . .
H1 H 1.1513 0.6665 0.8288 0.056 Uiso 1 1 calc R . .
O1 O 0.5969(3) 0.2351(2) 0.5538(3) 0.0368(5) Uani 1 1 d . . .
O2 O 0.7785(3) -0.1312(3) 0.4577(3) 0.0400(6) Uani 1 1 d . . .
O3 O 0.3800(3) 0.5545(3) 0.7845(2) 0.0344(5) Uani 1 1 d . . .
O4 O 0.7777(3) 0.4595(3) 0.8119(3) 0.0421(6) Uani 1 1 d . . .
O5 O 0.7778(3) 0.5409(3) 0.4881(3) 0.0342(5) Uani 1 1 d . . .
H5B H 0.7790 0.6387 0.5144 0.051 Uiso 1 1 d R . .
H5A H 0.8114 0.4731 0.5569 0.051 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
C1 O1 1.257(4) . ?
C1 C2 1.463(4) 2_656 ?
C1 C2 1.463(4) . ?
C2 O2 1.251(4) . ?
C2 C1 1.463(4) 2_656 ?
C3 O3 1.264(3) . ?
C3 C4 1.466(4) 2_667 ?
C3 C4 1.469(4) . ?
C4 O4 1.237(3) . ?
C4 C3 1.466(4) 2_667 ?
C5 N1 1.331(5) . ?
C5 C6 1.360(5) . ?
C5 H5 0.9300 . ?
C6 C7 1.378(5) . ?
C6 H6 0.9300 . ?
C7 C9 1.381(5) . ?
C7 C8 1.511(4) . ?
C8 C8 1.524(7) 2_677 ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C9 C10 1.363(5) . ?
C9 H9 0.9300 . ?
C10 N1 1.321(5) . ?
C10 H10 0.9300 . ?
Cd1 O5 2.259(2) . ?
Cd1 O5 2.259(2) 2_666 ?
Cd1 O1 2.273(2) 2_666 ?
Cd1 O1 2.273(2) . ?
Cd1 O3 2.328(2) . ?
Cd1 O3 2.328(2) 2_666 ?
N1 H1 0.8600 . ?
O5 H5B 0.8500 . ?
O5 H5A 0.8500 . ?

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
O1 C1 C2 135.6(3) . 2_656 ?
O1 C1 C2 134.0(3) . . ?
C2 C1 C2 90.5(2) 2_656 . ?
O2 C2 C1 135.5(3) . 2_656 ?
O2 C2 C1 134.9(3) . . ?
C1 C2 C1 89.5(2) 2_656 . ?
O3 C3 C4 133.2(3) . 2_667 ?
O3 C3 C4 135.7(3) . . ?
C4 C3 C4 91.2(2) 2_667 . ?
O4 C4 C3 135.2(3) . 2_667 ?
O4 C4 C3 136.0(3) . . ?
C3 C4 C3 88.8(2) 2_667 . ?
N1 C5 C6 120.3(3) . . ?
N1 C5 H5 119.8 . . ?
C6 C5 H5 119.8 . . ?
C5 C6 C7 119.6(3) . . ?
C5 C6 H6 120.2 . . ?
C7 C6 H6 120.2 . . ?
C6 C7 C9 118.1(3) . . ?
C6 C7 C8 121.2(3) . . ?
C9 C7 C8 120.7(3) . . ?
C7 C8 C8 111.4(3) . 2_677 ?
C7 C8 H8A 109.4 . . ?
C8 C8 H8A 109.4 2_677 . ?
C7 C8 H8B 109.4 . . ?
C8 C8 H8B 109.4 2_677 . ?
H8A C8 H8B 108.0 . . ?
C10 C9 C7 120.3(3) . . ?
C10 C9 H9 119.9 . . ?
C7 C9 H9 119.9 . . ?
N1 C10 C9 119.7(3) . . ?
N1 C10 H10 120.2 . . ?
C9 C10 H10 120.2 . . ?
O5 Cd1 O5 180.00(10) . 2_666 ?
O5 Cd1 O1 98.25(8) . 2_666 ?
O5 Cd1 O1 81.75(8) 2_666 2_666 ?
O5 Cd1 O1 81.75(8) . . ?
O5 Cd1 O1 98.25(8) 2_666 . ?
O1 Cd1 O1 180.0 2_666 . ?
O5 Cd1 O3 94.06(7) . . ?
O5 Cd1 O3 85.94(7) 2_666 . ?
O1 Cd1 O3 86.68(8) 2_666 . ?
O1 Cd1 O3 93.32(8) . . ?
O5 Cd1 O3 85.94(7) . 2_666 ?
O5 Cd1 O3 94.06(7) 2_666 2_666 ?
O1 Cd1 O3 93.32(8) 2_666 2_666 ?
O1 Cd1 O3 86.68(8) . 2_666 ?
O3 Cd1 O3 180.0 . 2_666 ?
C10 N1 C5 121.9(3) . . ?
C10 N1 H1 119.0 . . ?
C5 N1 H1 119.0 . . ?
C1 O1 Cd1 127.26(19) . . ?
C3 O3 Cd1 129.61(18) . . ?
Cd1 O5 H5B 109.3 . . ?
Cd1 O5 H5A 109.4 . . ?
H5B O5 H5A 109.5 . . ?

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
N1 H1 O3 0.86 1.89 2.737(3) 170.1 1_655
O5 H5B O2 0.85 1.90 2.676(3) 150.4 1_565
O5 H5A O4 0.85 2.06 2.740(3) 136.2 .

_diffrn_measured_fraction_theta_max 0.982
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.982
_refine_diff_density_max         0.424
_refine_diff_density_min         -0.544
_refine_diff_density_rms         0.091


