# 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        'Yunling Liu'
_publ_contact_author_address     
;
College of Chemistry
Jilin University
2699 Qianjin Street
Changchun
Jilin
130012
CHINA
;

_publ_contact_author_email       YUNLING@JLU.EDU.CN

_publ_section_title              
;Assembly of two 3-D metal-organic frameworks from
Cd(II) and 4,5-imidazoledicarboxylic acid or
2-ethyl-4,5-imidazoledicarboxylic acid
;
loop_
_publ_author_name
'Yun Liu.'
'Minghui Bi.'
'Qisheng Huo.'
'Shuang Wang.'
'Li-rong Zhang.'

# Attachment 'Comp1.cif'

data_compound1
_database_code_depnum_ccdc_archive 'CCDC 668680'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          'not measured'
_chemical_formula_moiety         'C10 H6 Cd3 N4 O10, H2 O'
_chemical_formula_sum            'C10 H8 Cd3 N4 O11'
_chemical_formula_weight         697.40

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

_symmetry_cell_setting           Orthorhombic
_symmetry_space_group_name_H-M   Pbca
_symmetry_space_group_name_Hall  -P2ac2ab

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

_cell_length_a                   14.300(3)
_cell_length_b                   13.041(3)
_cell_length_c                   18.230(4)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     3399.7(13)
_cell_formula_units_Z            8
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    3861
_cell_measurement_theta_min      3.08
_cell_measurement_theta_max      27.42

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.23
_exptl_crystal_density_meas      none
_exptl_crystal_density_diffrn    2.725
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2624
_exptl_absorpt_coefficient_mu    3.788
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.3768
_exptl_absorpt_correction_T_max  0.4189
_exptl_absorpt_process_details   Process-auto

_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  'Rigaku RAXIS-RAPID'
_diffrn_measurement_method       omega-scan
_diffrn_detector_area_resol_mean 10.0
_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        0
_diffrn_reflns_number            31073
_diffrn_reflns_av_R_equivalents  0.0574
_diffrn_reflns_av_sigmaI/netI    0.0307
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_theta_min         3.08
_diffrn_reflns_theta_max         27.42
_reflns_number_total             3861
_reflns_number_gt                3317
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       Process-auto
_computing_cell_refinement       Process-auto
_computing_data_reduction        Process-auto
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_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.

The bond lengths of O(9) H(9A) and O(9) H(9B) in compound 1 were 1.07
and 1.17 angstrom in the Fourier maps. The bond lengths were found to be
a little longer when we checked the CIF via the IUCr CheckCIF, as a result,
we added two restraints. The bond lengths of O(9) H(9A) and O(9) H(9B) of 1
were restrained to 0.96(8) angstrom and 0.96(6) angstrom.'
;

_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)+(0.0255P)²+24.1540P] 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         3861
_refine_ls_number_parameters     271
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0471
_refine_ls_R_factor_gt           0.0382
_refine_ls_wR_factor_ref         0.0806
_refine_ls_wR_factor_gt          0.0776
_refine_ls_goodness_of_fit_ref   1.094
_refine_ls_restrained_S_all      1.094
_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 0.06042(3) 0.49452(3) 0.17910(2) 0.01878(10) Uani 1 1 d . . .
Cd2 Cd 0.03264(3) 0.21663(3) 0.12888(2) 0.01612(10) Uani 1 1 d . . .
Cd3 Cd 0.25689(3) 0.25123(3) -0.06673(2) 0.01681(10) Uani 1 1 d . . .
O1 O 0.0480(3) 0.3811(3) 0.08303(19) 0.0190(8) Uani 1 1 d . . .
O2 O 0.1295(3) 0.2704(3) 0.0179(2) 0.0235(9) Uani 1 1 d . . .
O3 O 0.0424(3) 0.6092(3) 0.0852(2) 0.0237(9) Uani 1 1 d . . .
O4 O 0.1168(3) 0.7244(3) 0.0171(2) 0.0304(10) Uani 1 1 d . . .
O5 O 0.0544(3) 0.6139(3) 0.2789(2) 0.0295(10) Uani 1 1 d . . .
O6 O 0.1285(3) 0.7351(3) 0.3398(2) 0.0187(8) Uani 1 1 d . . .
O7 O 0.4089(3) 0.8207(3) 0.2289(2) 0.0261(9) Uani 1 1 d . . .
O8 O 0.3325(3) 0.8040(3) 0.3334(2) 0.0305(10) Uani 1 1 d . . .
O9 O -0.0881(4) 0.4605(5) 0.2086(4) 0.0650(18) Uani 1 1 d D . .
O10 O -0.0031(5) 0.0851(5) 0.0553(3) 0.0629(17) Uani 1 1 d . . .
O1W O 0.0177(6) 0.8746(5) 0.1034(5) 0.086(3) Uani 1 1 d . . .
N1 N 0.2310(3) 0.4162(3) -0.0507(2) 0.0190(9) Uani 1 1 d . . .
N2 N 0.2263(3) 0.5863(3) -0.0481(2) 0.0206(10) Uani 1 1 d . . .
N3 N 0.2032(3) 0.5617(4) 0.1959(2) 0.0192(10) Uani 1 1 d . . .
N4 N 0.3394(3) 0.6421(4) 0.1761(2) 0.0183(9) Uani 1 1 d . . .
C1 C 0.2665(4) 0.5026(4) -0.0767(3) 0.0245(13) Uani 1 1 d . . .
H1 H 0.3143 0.5050 -0.1113 0.080 Uiso 1 1 calc . . .
C2 C 0.1613(4) 0.4458(4) -0.0031(3) 0.0157(10) Uani 1 1 d . . .
C3 C 0.1585(4) 0.5518(4) -0.0014(3) 0.0145(10) Uani 1 1 d . . .
C4 C 0.1096(4) 0.3622(4) 0.0344(3) 0.0152(10) Uani 1 1 d . . .
C5 C 0.1011(4) 0.6333(4) 0.0372(3) 0.0176(11) Uani 1 1 d . . .
C6 C 0.2821(4) 0.5659(4) 0.1563(3) 0.0194(11) Uani 1 1 d . . .
H6 H 0.2957 0.5202 0.1187 0.080 Uiso 1 1 calc . . .
C7 C 0.2108(4) 0.6403(4) 0.2460(3) 0.0156(10) Uani 1 1 d . . .
C8 C 0.2961(4) 0.6901(4) 0.2343(3) 0.0151(10) Uani 1 1 d . . .
C9 C 0.1280(3) 0.6645(4) 0.2911(3) 0.0145(10) Uani 1 1 d . . .
C10 C 0.3480(4) 0.7781(4) 0.2687(3) 0.0182(11) Uani 1 1 d . . .
H1A H -0.024(7) 0.875(8) 0.137(5) 0.080 Uiso 1 1 d . . .
H1B H 0.050(7) 0.822(8) 0.090(6) 0.080 Uiso 1 1 d . . .
H9A H -0.116(6) 0.496(6) 0.249(4) 0.080 Uiso 1 1 d D . .
H9B H -0.109(7) 0.394(4) 0.192(5) 0.080 Uiso 1 1 d D . .
H10A H -0.007(7) 0.129(8) 0.011(5) 0.080 Uiso 1 1 d . . .
H10B H 0.014(7) 0.011(8) 0.056(5) 0.080 Uiso 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 O9 2.236(6) . ?
Cd1 N3 2.243(5) . ?
Cd1 O3 2.287(4) . ?
Cd1 O1 2.300(4) . ?
Cd1 O5 2.395(4) . ?
Cd1 O7 2.482(4) 8_655 ?
Cd2 O10 2.237(6) . ?
Cd2 N4 2.243(5) 8_655 ?
Cd2 O1 2.312(4) . ?
Cd2 O6 2.385(4) 3_545 ?
Cd2 O7 2.422(4) 8_655 ?
Cd2 O5 2.485(4) 3_545 ?
Cd2 O2 2.550(4) . ?
Cd3 N2 2.191(4) 8_655 ?
Cd3 N1 2.202(4) . ?
Cd3 O8 2.338(4) 2_564 ?
Cd3 O6 2.371(4) 2_564 ?
Cd3 O4 2.391(4) 8_655 ?
Cd3 O2 2.400(4) . ?
O1 C4 1.274(6) . ?
O2 C4 1.268(6) . ?
O3 C5 1.254(7) . ?
O4 C5 1.263(6) . ?
O4 Cd3 2.391(4) 8_665 ?
O5 C9 1.262(6) . ?
O5 Cd2 2.485(4) 3 ?
O6 C9 1.279(6) . ?
O6 Cd3 2.371(4) 2_565 ?
O6 Cd2 2.385(4) 3 ?
O7 C10 1.262(6) . ?
O7 Cd2 2.422(4) 8_665 ?
O7 Cd1 2.482(4) 8_665 ?
O8 C10 1.247(6) . ?
O8 Cd3 2.338(4) 2_565 ?
O9 H9A 0.96(8) . ?
O9 H9B 0.96(6) . ?
O10 H10A 0.99(10) . ?
O10 H10B 1.00(10) . ?
O1W H1A 0.86(10) . ?
O1W H1B 0.86(11) . ?
N1 C1 1.324(7) . ?
N1 C2 1.377(7) . ?
N2 C1 1.340(7) . ?
N2 C3 1.366(7) . ?
N2 Cd3 2.191(4) 8_665 ?
N3 C6 1.341(7) . ?
N3 C7 1.376(7) . ?
N4 C6 1.337(7) . ?
N4 C8 1.378(6) . ?
N4 Cd2 2.243(5) 8_665 ?
C1 H1 0.9300 . ?
C2 C3 1.384(7) . ?
C2 C4 1.483(7) . ?
C3 C5 1.515(7) . ?
C6 H6 0.9300 . ?
C7 C8 1.398(7) . ?
C7 C9 1.477(7) . ?
C8 C10 1.504(7) . ?

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
O9 Cd1 N3 155.4(2) . . ?
O9 Cd1 O3 101.7(2) . . ?
N3 Cd1 O3 87.10(16) . . ?
O9 Cd1 O1 88.99(18) . . ?
N3 Cd1 O1 115.20(15) . . ?
O3 Cd1 O1 80.91(14) . . ?
O9 Cd1 O5 84.95(18) . . ?
N3 Cd1 O5 71.04(15) . . ?
O3 Cd1 O5 98.01(15) . . ?
O1 Cd1 O5 173.50(14) . . ?
O9 Cd1 O7 84.2(2) . 8_655 ?
N3 Cd1 O7 98.39(15) . 8_655 ?
O3 Cd1 O7 153.01(13) . 8_655 ?
O1 Cd1 O7 72.81(13) . 8_655 ?
O5 Cd1 O7 108.79(14) . 8_655 ?
O10 Cd2 N4 94.8(2) . 8_655 ?
O10 Cd2 O1 121.1(2) . . ?
N4 Cd2 O1 117.56(15) 8_655 . ?
O10 Cd2 O6 90.0(2) . 3_545 ?
N4 Cd2 O6 137.71(14) 8_655 3_545 ?
O1 Cd2 O6 94.86(13) . 3_545 ?
O10 Cd2 O7 163.7(2) . 8_655 ?
N4 Cd2 O7 70.86(14) 8_655 8_655 ?
O1 Cd2 O7 73.73(13) . 8_655 ?
O6 Cd2 O7 95.56(13) 3_545 8_655 ?
O10 Cd2 O5 83.0(2) . 3_545 ?
N4 Cd2 O5 85.14(15) 8_655 3_545 ?
O1 Cd2 O5 142.44(13) . 3_545 ?
O6 Cd2 O5 53.77(12) 3_545 3_545 ?
O7 Cd2 O5 88.01(15) 8_655 3_545 ?
O10 Cd2 O2 81.92(19) . . ?
N4 Cd2 O2 88.86(14) 8_655 . ?
O1 Cd2 O2 53.60(12) . . ?
O6 Cd2 O2 133.36(13) 3_545 . ?
O7 Cd2 O2 104.83(14) 8_655 . ?
O5 Cd2 O2 163.20(13) 3_545 . ?
N2 Cd3 N1 163.08(17) 8_655 . ?
N2 Cd3 O8 83.03(16) 8_655 2_564 ?
N1 Cd3 O8 108.21(16) . 2_564 ?
N2 Cd3 O6 96.29(15) 8_655 2_564 ?
N1 Cd3 O6 97.94(14) . 2_564 ?
O8 Cd3 O6 80.91(14) 2_564 2_564 ?
N2 Cd3 O4 70.98(15) 8_655 8_655 ?
N1 Cd3 O4 100.64(15) . 8_655 ?
O8 Cd3 O4 149.93(15) 2_564 8_655 ?
O6 Cd3 O4 87.02(14) 2_564 8_655 ?
N2 Cd3 O2 94.90(15) 8_655 . ?
N1 Cd3 O2 71.67(14) . . ?
O8 Cd3 O2 96.74(15) 2_564 . ?
O6 Cd3 O2 168.19(13) 2_564 . ?
O4 Cd3 O2 100.22(15) 8_655 . ?
C4 O1 Cd1 127.0(3) . . ?
C4 O1 Cd2 98.0(3) . . ?
Cd1 O1 Cd2 109.19(14) . . ?
C4 O2 Cd3 114.9(3) . . ?
C4 O2 Cd2 87.1(3) . . ?
Cd3 O2 Cd2 153.34(17) . . ?
C5 O3 Cd1 127.7(3) . . ?
C5 O4 Cd3 117.2(3) . 8_665 ?
C9 O5 Cd1 116.4(3) . . ?
C9 O5 Cd2 90.9(3) . 3 ?
Cd1 O5 Cd2 151.95(18) . 3 ?
C9 O6 Cd3 123.8(3) . 2_565 ?
C9 O6 Cd2 95.1(3) . 3 ?
Cd3 O6 Cd2 120.24(15) 2_565 3 ?
C10 O7 Cd2 115.1(3) . 8_665 ?
C10 O7 Cd1 137.2(4) . 8_665 ?
Cd2 O7 Cd1 100.09(14) 8_665 8_665 ?
C10 O8 Cd3 138.6(4) . 2_565 ?
Cd1 O9 H9A 119(6) . . ?
Cd1 O9 H9B 113(6) . . ?
H9A O9 H9B 123(8) . . ?
Cd2 O10 H10A 93(6) . . ?
Cd2 O10 H10B 133(6) . . ?
H10A O10 H10B 125(8) . . ?
H1A O1W H1B 126(10) . . ?
C1 N1 C2 105.4(4) . . ?
C1 N1 Cd3 136.0(4) . . ?
C2 N1 Cd3 118.6(3) . . ?
C1 N2 C3 106.2(4) . . ?
C1 N2 Cd3 133.8(4) . 8_665 ?
C3 N2 Cd3 119.9(4) . 8_665 ?
C6 N3 C7 105.0(4) . . ?
C6 N3 Cd1 135.1(4) . . ?
C7 N3 Cd1 117.0(3) . . ?
C6 N4 C8 105.6(4) . . ?
C6 N4 Cd2 135.9(3) . 8_665 ?
C8 N4 Cd2 117.7(3) . 8_665 ?
N1 C1 N2 112.9(5) . . ?
N1 C1 H1 123.6 . . ?
N2 C1 H1 123.6 . . ?
N1 C2 C3 108.4(4) . . ?
N1 C2 C4 116.5(5) . . ?
C3 C2 C4 135.2(5) . . ?
N2 C3 C2 107.1(4) . . ?
N2 C3 C5 116.2(4) . . ?
C2 C3 C5 136.6(5) . . ?
O2 C4 O1 120.2(5) . . ?
O2 C4 C2 118.2(5) . . ?
O1 C4 C2 121.6(5) . . ?
O3 C5 O4 123.9(5) . . ?
O3 C5 C3 120.7(5) . . ?
O4 C5 C3 115.4(5) . . ?
N4 C6 N3 113.7(5) . . ?
N4 C6 H6 123.2 . . ?
N3 C6 H6 123.2 . . ?
N3 C7 C8 108.3(4) . . ?
N3 C7 C9 117.7(4) . . ?
C8 C7 C9 133.3(5) . . ?
N4 C8 C7 107.4(4) . . ?
N4 C8 C10 116.5(4) . . ?
C7 C8 C10 136.2(5) . . ?
O5 C9 O6 120.3(5) . . ?
O5 C9 C7 117.2(5) . . ?
O6 C9 C7 122.5(5) . . ?
O8 C10 O7 123.1(5) . . ?
O8 C10 C8 121.0(5) . . ?
O7 C10 C8 115.9(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
O1W H1A O8 0.86(10) 2.31(11) 3.031(9) 141(9) 6_556
O1W H1B O4 0.86(11) 2.07(11) 2.885(8) 157(10) .
O9 H9A N4 0.96(8) 2.43(4) 3.333(7) 157(8) 6_556
O9 H9B O6 0.96(6) 2.18(3) 3.123(7) 169(9) 3_545
O10 H10A O1W 0.99(10) 2.10(10) 2.949(11) 143(8) 5_565
O10 H10A O4 0.99(10) 2.53(10) 3.250(9) 130(7) 5_565
O10 H10B O1W 1.00(10) 1.98(10) 2.896(10) 152(8) 1_545
O10 H10B O10 1.00(10) 2.38(10) 3.000(11) 119(7) 5

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        27.42
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         0.881
_refine_diff_density_min         -1.545
_refine_diff_density_rms         0.173

# Attachment 'Comp2.cif'

data_compound2
_database_code_depnum_ccdc_archive 'CCDC 668681'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          'not measured'
_chemical_formula_moiety         'C7 H5 Cd K N2 O4'
_chemical_formula_sum            'C7 H5 Cd K N2 O4'
_chemical_formula_weight         332.63

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'
K K 0.2009 0.2494 '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   P-42(1)c

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

_cell_length_a                   16.0901(15)
_cell_length_b                   16.0901(15)
_cell_length_c                   6.7807(9)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     1755.5(3)
_cell_formula_units_Z            8
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    2189
_cell_measurement_theta_min      1.79
_cell_measurement_theta_max      28.31

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.18
_exptl_crystal_density_meas      none
_exptl_crystal_density_diffrn    2.517
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1280
_exptl_absorpt_coefficient_mu    2.954
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.4971
_exptl_absorpt_correction_T_max  0.5884
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean 9.00cm
_diffrn_standards_number         none
_diffrn_standards_interval_count none
_diffrn_standards_interval_time  none
_diffrn_standards_decay_%        none
_diffrn_reflns_number            10288
_diffrn_reflns_av_R_equivalents  0.0942
_diffrn_reflns_av_sigmaI/netI    0.0660
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_l_min       -7
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_theta_min         1.79
_diffrn_reflns_theta_max         28.31
_reflns_number_total             2189
_reflns_number_gt                1887
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_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)+(0.0278P)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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.06(5)
_refine_ls_number_reflns         2189
_refine_ls_number_parameters     131
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0453
_refine_ls_R_factor_gt           0.0351
_refine_ls_wR_factor_ref         0.0683
_refine_ls_wR_factor_gt          0.0647
_refine_ls_goodness_of_fit_ref   0.977
_refine_ls_restrained_S_all      0.977
_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 0.82333(2) 0.23935(2) 0.51981(6) 0.01346(10) Uani 1 1 d . . .
K1 K 0.61936(8) 0.03252(8) 1.2790(2) 0.0247(3) Uani 1 1 d . . .
O1 O 0.7716(2) 0.2112(2) 0.8352(5) 0.0177(8) Uani 1 1 d . . .
O2 O 0.6886(2) 0.1251(2) 1.0059(7) 0.0254(9) Uani 1 1 d . . .
O3 O 0.6057(2) -0.0329(2) 0.9024(6) 0.0228(9) Uani 1 1 d . . .
O4 O 0.6834(3) -0.1373(2) 0.7892(6) 0.0264(10) Uani 1 1 d . . .
N1 N 0.7985(2) 0.0956(2) 0.5464(7) 0.0155(9) Uani 1 1 d . . .
N2 N 0.7581(2) -0.0376(2) 0.5191(7) 0.0164(8) Uani 1 1 d . . .
C1 C 0.7482(3) 0.0767(3) 0.7054(7) 0.0132(10) Uani 1 1 d . . .
C2 C 0.7225(3) -0.0056(3) 0.6874(7) 0.0126(10) Uani 1 1 d . . .
C3 C 0.8029(3) 0.0251(3) 0.4402(8) 0.0165(12) Uani 1 1 d . . .
C4 C 0.7338(3) 0.1403(3) 0.8620(8) 0.0150(11) Uani 1 1 d . . .
C5 C 0.6665(3) -0.0615(3) 0.8058(8) 0.0164(11) Uani 1 1 d . . .
C6 C 0.8493(5) 0.0124(4) 0.2501(10) 0.0400(13) Uani 1 1 d . . .
H6A H 0.8854 -0.0354 0.2651 0.080 Uiso 1 1 calc . . .
H6B H 0.8094 -0.0006 0.1475 0.080 Uiso 1 1 calc . . .
C7 C 0.9008(5) 0.0843(4) 0.1823(10) 0.0400(13) Uani 1 1 d . . .
H7A H 0.8662 0.1324 0.1679 0.080 Uiso 1 1 calc R . .
H7B H 0.9259 0.0711 0.0577 0.080 Uiso 1 1 calc R . .
H7C H 0.9435 0.0954 0.2777 0.080 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 N2 2.254(4) 3_666 ?
Cd1 O1 2.257(3) 8_544 ?
Cd1 O1 2.339(4) . ?
Cd1 N1 2.354(4) . ?
Cd1 O4 2.372(4) 5_656 ?
Cd1 O4 2.517(4) 3_666 ?
K1 O2 2.625(4) . ?
K1 O3 2.754(4) 7 ?
K1 O3 2.771(4) . ?
K1 O3 2.844(4) 8_545 ?
K1 O2 2.946(4) 8_545 ?
K1 N2 2.985(4) 1_556 ?
K1 C3 3.151(5) 1_556 ?
K1 C2 3.286(5) 1_556 ?
K1 C4 3.303(6) 8_545 ?
K1 C5 3.340(5) 7 ?
K1 K1 3.9242(14) 8_544 ?
K1 K1 3.9242(14) 8_545 ?
O1 C4 1.305(6) . ?
O1 Cd1 2.257(3) 8_545 ?
O2 C4 1.241(6) . ?
O2 K1 2.946(4) 8_544 ?
O3 C5 1.265(6) . ?
O3 K1 2.754(4) 7_554 ?
O3 K1 2.844(4) 8_544 ?
O4 C5 1.255(6) . ?
O4 Cd1 2.372(4) 5_646 ?
O4 Cd1 2.517(4) 4_646 ?
N1 C3 1.346(6) . ?
N1 C1 1.381(6) . ?
N2 C3 1.349(6) . ?
N2 C2 1.377(6) . ?
N2 Cd1 2.254(4) 4_646 ?
N2 K1 2.985(4) 1_554 ?
C1 C2 1.393(7) . ?
C1 C4 1.493(7) . ?
C2 C5 1.504(7) . ?
C2 K1 3.286(5) 1_554 ?
C3 C6 1.504(8) . ?
C3 K1 3.151(5) 1_554 ?
C4 K1 3.303(6) 8_544 ?
C5 K1 3.340(5) 7_554 ?
C6 C7 1.494(9) . ?
C6 H6A 0.9700 . ?
C6 H6B 0.9700 . ?
C7 H7A 0.9600 . ?
C7 H7B 0.9600 . ?
C7 H7C 0.9600 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N2 Cd1 O1 136.46(15) 3_666 8_544 ?
N2 Cd1 O1 117.66(15) 3_666 . ?
O1 Cd1 O1 105.47(11) 8_544 . ?
N2 Cd1 N1 101.26(13) 3_666 . ?
O1 Cd1 N1 97.61(14) 8_544 . ?
O1 Cd1 N1 71.28(13) . . ?
N2 Cd1 O4 95.41(14) 3_666 5_656 ?
O1 Cd1 O4 94.25(15) 8_544 5_656 ?
O1 Cd1 O4 69.32(13) . 5_656 ?
N1 Cd1 O4 140.56(14) . 5_656 ?
N2 Cd1 O4 69.14(14) 3_666 3_666 ?
O1 Cd1 O4 68.03(12) 8_544 3_666 ?
O1 Cd1 O4 161.13(13) . 3_666 ?
N1 Cd1 O4 126.27(15) . 3_666 ?
O4 Cd1 O4 93.04(12) 5_656 3_666 ?
O2 K1 O3 152.52(13) . 7 ?
O2 K1 O3 66.35(12) . . ?
O3 K1 O3 86.17(9) 7 . ?
O2 K1 O3 109.76(11) . 8_545 ?
O3 K1 O3 79.04(13) 7 8_545 ?
O3 K1 O3 111.11(13) . 8_545 ?
O2 K1 O2 82.61(9) . 8_545 ?
O3 K1 O2 123.07(12) 7 8_545 ?
O3 K1 O2 143.85(13) . 8_545 ?
O3 K1 O2 61.35(10) 8_545 8_545 ?
O2 K1 N2 106.38(12) . 1_556 ?
O3 K1 N2 84.66(12) 7 1_556 ?
O3 K1 N2 114.74(12) . 1_556 ?
O3 K1 N2 129.82(13) 8_545 1_556 ?
O2 K1 N2 90.79(11) 8_545 1_556 ?
O2 K1 C3 82.46(13) . 1_556 ?
O3 K1 C3 109.71(13) 7 1_556 ?
O3 K1 C3 112.31(13) . 1_556 ?
O3 K1 C3 136.13(13) 8_545 1_556 ?
O2 K1 C3 79.75(12) 8_545 1_556 ?
N2 K1 C3 25.22(11) 1_556 1_556 ?
O2 K1 C2 119.11(14) . 1_556 ?
O3 K1 C2 81.27(13) 7 1_556 ?
O3 K1 C2 138.23(12) . 1_556 ?
O3 K1 C2 105.32(12) 8_545 1_556 ?
O2 K1 C2 72.74(12) 8_545 1_556 ?
N2 K1 C2 24.77(11) 1_556 1_556 ?
C3 K1 C2 39.42(13) 1_556 1_556 ?
O2 K1 C4 61.36(12) . 8_545 ?
O3 K1 C4 142.31(12) 7 8_545 ?
O3 K1 C4 122.50(13) . 8_545 ?
O3 K1 C4 68.40(12) 8_545 8_545 ?
O2 K1 C4 21.96(12) 8_545 8_545 ?
N2 K1 C4 101.61(12) 1_556 8_545 ?
C3 K1 C4 83.27(13) 1_556 8_545 ?
C2 K1 C4 89.32(12) 1_556 8_545 ?
O2 K1 C5 134.48(13) . 7 ?
O3 K1 C5 21.29(12) 7 7 ?
O3 K1 C5 70.35(12) . 7 ?
O3 K1 C5 98.11(12) 8_545 7 ?
O2 K1 C5 142.90(13) 8_545 7 ?
N2 K1 C5 79.42(12) 1_556 7 ?
C3 K1 C5 101.87(13) 1_556 7 ?
C2 K1 C5 85.17(13) 1_556 7 ?
C4 K1 C5 163.52(13) 8_545 7 ?
O2 K1 K1 48.65(9) . 8_544 ?
O3 K1 K1 111.73(9) 7 8_544 ?
O3 K1 K1 46.43(8) . 8_544 ?
O3 K1 K1 78.46(9) 8_545 8_544 ?
O2 K1 K1 99.13(9) 8_545 8_544 ?
N2 K1 K1 150.72(10) 1_556 8_544 ?
C3 K1 K1 130.31(10) 1_556 8_544 ?
C2 K1 K1 167.00(9) 1_556 8_544 ?
C4 K1 K1 80.47(9) 8_545 8_544 ?
C5 K1 K1 106.81(9) 7 8_544 ?
O2 K1 K1 123.96(9) . 8_545 ?
O3 K1 K1 81.09(8) 7 8_545 ?
O3 K1 K1 154.59(9) . 8_545 ?
O3 K1 K1 44.90(9) 8_545 8_545 ?
O2 K1 K1 41.98(8) 8_545 8_545 ?
N2 K1 K1 85.96(9) 1_556 8_545 ?
C3 K1 K1 92.72(10) 1_556 8_545 ?
C2 K1 K1 61.19(8) 1_556 8_545 ?
C4 K1 K1 62.62(9) 8_545 8_545 ?
C5 K1 K1 101.26(9) 7 8_545 ?
K1 K1 K1 119.53(7) 8_544 8_545 ?
C4 O1 Cd1 121.0(3) . 8_545 ?
C4 O1 Cd1 117.6(3) . . ?
Cd1 O1 Cd1 115.71(14) 8_545 . ?
C4 O2 K1 156.2(3) . . ?
C4 O2 K1 95.4(3) . 8_544 ?
K1 O2 K1 89.37(10) . 8_544 ?
C5 O3 K1 106.5(3) . 7_554 ?
C5 O3 K1 123.7(3) . . ?
K1 O3 K1 122.41(14) 7_554 . ?
C5 O3 K1 118.8(3) . 8_544 ?
K1 O3 K1 90.65(12) 7_554 8_544 ?
K1 O3 K1 88.67(11) . 8_544 ?
C5 O4 Cd1 139.0(4) . 5_646 ?
C5 O4 Cd1 115.2(3) . 4_646 ?
Cd1 O4 Cd1 105.47(14) 5_646 4_646 ?
C3 N1 C1 105.2(4) . . ?
C3 N1 Cd1 141.1(4) . . ?
C1 N1 Cd1 112.1(3) . . ?
C3 N2 C2 105.8(4) . . ?
C3 N2 Cd1 133.3(3) . 4_646 ?
C2 N2 Cd1 118.4(3) . 4_646 ?
C3 N2 K1 84.3(3) . 1_554 ?
C2 N2 K1 90.0(3) . 1_554 ?
Cd1 N2 K1 108.95(15) 4_646 1_554 ?
N1 C1 C2 108.4(4) . . ?
N1 C1 C4 119.7(4) . . ?
C2 C1 C4 131.9(5) . . ?
N2 C2 C1 107.7(4) . . ?
N2 C2 C5 117.9(4) . . ?
C1 C2 C5 134.4(5) . . ?
N2 C2 K1 65.3(2) . 1_554 ?
C1 C2 K1 92.7(3) . 1_554 ?
C5 C2 K1 105.0(3) . 1_554 ?
N1 C3 N2 112.9(4) . . ?
N1 C3 C6 126.8(5) . . ?
N2 C3 C6 120.3(5) . . ?
N1 C3 K1 96.0(3) . 1_554 ?
N2 C3 K1 70.5(3) . 1_554 ?
C6 C3 K1 100.0(4) . 1_554 ?
O2 C4 O1 123.7(5) . . ?
O2 C4 C1 121.0(4) . . ?
O1 C4 C1 115.3(4) . . ?
O2 C4 K1 62.6(3) . 8_544 ?
O1 C4 K1 121.5(3) . 8_544 ?
C1 C4 K1 87.8(3) . 8_544 ?
O4 C5 O3 124.6(5) . . ?
O4 C5 C2 113.9(5) . . ?
O3 C5 C2 121.4(4) . . ?
O4 C5 K1 86.1(3) . 7_554 ?
O3 C5 K1 52.2(3) . 7_554 ?
C2 C5 K1 135.3(3) . 7_554 ?
C7 C6 C3 115.8(5) . . ?
C7 C6 H6A 108.3 . . ?
C3 C6 H6A 108.3 . . ?
C7 C6 H6B 108.3 . . ?
C3 C6 H6B 108.3 . . ?
H6A C6 H6B 107.4 . . ?
C6 C7 H7A 109.5 . . ?
C6 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
C6 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?

_diffrn_measured_fraction_theta_max 1.000
_diffrn_reflns_theta_full        28.31
_diffrn_measured_fraction_theta_full 1.000
_refine_diff_density_max         0.948
_refine_diff_density_min         -0.767
_refine_diff_density_rms         0.143


