# Supplementary Material (ESI) for Chemical Communications
# This journal is (c) The Royal Society of Chemistry 2010


data_global
_journal_name_full               Chem.Commun.

_journal_coden_Cambridge         0182
_journal_volume                  ?
_journal_page_first              ?
_journal_year                    ?

_publ_contact_author_name        'Thallapally, Praveen'
_publ_contact_author_email       praveen.thallapally@pnl.gov

_publ_section_title              
;
Conversion of Nanoporous Helical
Cadmium Organic Framework to Porous Form
;
loop_
_publ_author_name
P.Thallapally
Yu.Cai
J.Liu
J.Tian
Z.-G.Gu
H.-C.Fang
Z.-Y.Zhou

# Attachment '- Revised_773501(2).cif'

data_g2
_database_code_depnum_ccdc_archive 'CCDC 773501'
#TrackingRef '- Revised_773501(2).cif'

_audit_creation_method           SHELXL-97

_chemical_name_systematic        
;

?

;

_chemical_name_common            ?

_chemical_melting_point          ?

_chemical_formula_moiety         'C10 H7 Cd N3 O4'

_chemical_formula_sum            'C10 H7 Cd N3 O4'

_chemical_formula_weight         345.59

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           Trigonal

_symmetry_space_group_name_H-M   R3c

loop_

_symmetry_equiv_pos_as_xyz

'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'-y, -x, z+1/2'
'-x+y, y, z+1/2'
'x, x-y, z+1/2'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'-y+2/3, -x+1/3, z+5/6'
'-x+y+2/3, y+1/3, z+5/6'
'x+2/3, x-y+1/3, z+5/6'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'-y+1/3, -x+2/3, z+7/6'
'-x+y+1/3, y+2/3, z+7/6'
'x+1/3, x-y+2/3, z+7/6'

_cell_length_a                   21.1266(16)

_cell_length_b                   21.1266(16)

_cell_length_c                   13.967(2)

_cell_angle_alpha                90.00

_cell_angle_beta                 90.00

_cell_angle_gamma                120.00

_cell_volume                     5398.9(10)

_cell_formula_units_Z            18

_cell_measurement_temperature    298(2)

_cell_measurement_reflns_used    6620

_cell_measurement_theta_min      3.12

_cell_measurement_theta_max      27.97

_exptl_crystal_description       block

_exptl_crystal_colour            'pale yellow'

_exptl_crystal_size_max          0.22

_exptl_crystal_size_mid          0.16

_exptl_crystal_size_min          0.11

_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.913

_exptl_crystal_density_method    'not measured'

_exptl_crystal_F_000             3024

_exptl_absorpt_coefficient_mu    1.830

_exptl_absorpt_correction_type   multi-scan

_exptl_absorpt_correction_T_min  0.6890

_exptl_absorpt_correction_T_max  0.8241

_exptl_absorpt_process_details   'SADABS (Sheldrick, 1996)'

_exptl_special_details           
;

?

;

_diffrn_ambient_temperature      298(2)

_diffrn_radiation_wavelength     0.71073

_diffrn_radiation_type           MoK\a

_diffrn_radiation_source         'fine-focus sealed tube'

_diffrn_radiation_monochromator  graphite

_diffrn_measurement_device_type  'CCD area detector'

_diffrn_measurement_method       'phi and omega scans'

_diffrn_detector_area_resol_mean ?

_diffrn_standards_number         ?

_diffrn_standards_interval_count ?

_diffrn_standards_interval_time  ?

_diffrn_standards_decay_%        ?

_diffrn_reflns_number            8802

_diffrn_reflns_av_R_equivalents  0.0235

_diffrn_reflns_av_sigmaI/netI    0.0205

_diffrn_reflns_limit_h_min       -25

_diffrn_reflns_limit_h_max       14

_diffrn_reflns_limit_k_min       -24

_diffrn_reflns_limit_k_max       25

_diffrn_reflns_limit_l_min       -16

_diffrn_reflns_limit_l_max       16

_diffrn_reflns_theta_min         1.93

_diffrn_reflns_theta_max         25.16

_reflns_number_total             2151

_reflns_number_gt                2085

_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    'Bruker SHELXTL'

_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
;

Refinement of F^2^ against ALL reflections. The weighted R-factor wR and

goodness of fit S are based on F^2^, conventional R-factors R are based

on F, with F set to zero for negative F^2^. The threshold expression of

F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is

not relevant to the choice of reflections for refinement. R-factors based

on F^2^ 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/[\s^2^(Fo^2^)+(0.0213P)^2^+3.8889P] where P=(Fo^2^+2Fc^2^)/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   -0.04(2)

_refine_ls_number_reflns         2151

_refine_ls_number_parameters     164

_refine_ls_number_restraints     1

_refine_ls_R_factor_all          0.0177

_refine_ls_R_factor_gt           0.0168

_refine_ls_wR_factor_ref         0.0413

_refine_ls_wR_factor_gt          0.0407

_refine_ls_goodness_of_fit_ref   1.043

_refine_ls_restrained_S_all      1.042

_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 0.412945(10) 0.077262(9) 0.84122(3) 0.03214(7) Uani 1 1 d . . .
O1 O 0.51557(16) 0.12825(14) 0.9622(2) 0.0538(7) Uani 1 1 d . . .
O2 O 0.59624(15) 0.10336(18) 1.02565(18) 0.0646(7) Uani 1 1 d . . .
H2 H 0.6226 0.0878 1.0068 0.097 Uiso 1 1 calc R . .
O3 O 0.65710(13) 0.03246(14) 0.97289(18) 0.0531(6) Uani 1 1 d . . .
O4 O 0.66340(17) -0.02739(14) 0.8490(2) 0.0503(5) Uani 1 1 d . . .
N1 N 0.49385(13) 0.04298(13) 0.80537(17) 0.0352(5) Uani 1 1 d . . .
N2 N 0.55199(13) -0.01487(14) 0.75580(18) 0.0356(5) Uani 1 1 d . . .
N3 N 0.46988(14) 0.19127(16) 0.7617(2) 0.0397(7) Uani 1 1 d . . .
C1 C 0.5008(2) 0.0025(2) 0.7372(2) 0.0380(8) Uani 1 1 d . . .
H1 H 0.4724 -0.0123 0.6820 0.046 Uiso 1 1 calc R . .
C2 C 0.57983(14) 0.01571(14) 0.84329(19) 0.0309(6) Uani 1 1 d . . .
C3 C 0.63727(15) 0.00563(16) 0.8898(2) 0.0379(7) Uani 1 1 d . . .
C4 C 0.54408(14) 0.05160(15) 0.8741(2) 0.0315(6) Uani 1 1 d . . .
C5 C 0.55106(16) 0.09692(17) 0.9576(2) 0.0398(7) Uani 1 1 d . . .
C6 C 0.5147(2) 0.25125(19) 0.8115(3) 0.0514(8) Uani 1 1 d . . .
H6 H 0.5250 0.2460 0.8747 0.062 Uiso 1 1 calc R . .
C7 C 0.5464(2) 0.3207(2) 0.7730(3) 0.0687(11) Uani 1 1 d . . .
H7 H 0.5770 0.3615 0.8096 0.082 Uiso 1 1 calc R . .
C8 C 0.5315(2) 0.3280(2) 0.6791(4) 0.0785(13) Uani 1 1 d . . .
H8 H 0.5529 0.3739 0.6508 0.094 Uiso 1 1 calc R . .
C9 C 0.4855(3) 0.2679(2) 0.6285(3) 0.0751(13) Uani 1 1 d . . .
H9 H 0.4740 0.2721 0.5655 0.090 Uiso 1 1 calc R . .
C10 C 0.4557(2) 0.2000(2) 0.6716(3) 0.0541(9) Uani 1 1 d . . .
H10 H 0.4246 0.1588 0.6360 0.065 Uiso 1 1 calc R . .

loop_

_atom_site_aniso_label

_atom_site_aniso_U_11

_atom_site_aniso_U_22

_atom_site_aniso_U_33

_atom_site_aniso_U_23

_atom_site_aniso_U_13

_atom_site_aniso_U_12

Cd1 0.03011(13) 0.02973(13) 0.04226(11) -0.00816(12) -0.00110(12) 0.01923(8)
O1 0.0618(18) 0.0640(16) 0.0528(16) -0.0228(13) -0.0105(14) 0.0443(14)
O2 0.0686(17) 0.096(2) 0.0495(15) -0.0307(14) -0.0245(13) 0.0560(16)
O3 0.0466(13) 0.0668(16) 0.0538(15) -0.0007(12) -0.0146(11) 0.0344(13)
O4 0.0456(12) 0.0564(16) 0.0660(15) 0.0112(14) 0.0086(10) 0.0384(15)
N1 0.0345(13) 0.0430(14) 0.0370(13) -0.0091(11) -0.0061(11) 0.0260(11)
N2 0.0382(13) 0.0420(14) 0.0371(13) -0.0064(11) -0.0018(11) 0.0281(12)
N3 0.0376(14) 0.0374(15) 0.0447(17) 0.0005(12) 0.0054(12) 0.0192(12)
C1 0.0426(15) 0.0497(16) 0.036(2) -0.0119(18) -0.0079(15) 0.0335(14)
C2 0.0283(13) 0.0308(14) 0.0352(16) 0.0018(11) 0.0004(11) 0.0158(12)
C3 0.0288(14) 0.0368(16) 0.049(2) 0.0114(13) 0.0023(13) 0.0169(13)
C4 0.0264(13) 0.0337(14) 0.0365(15) -0.0028(11) -0.0009(11) 0.0166(12)
C5 0.0367(16) 0.0423(17) 0.0404(16) -0.0075(13) -0.0032(13) 0.0196(14)
C6 0.053(2) 0.0445(19) 0.050(2) -0.0042(15) -0.0008(16) 0.0194(16)
C7 0.066(3) 0.0333(19) 0.091(3) -0.0037(19) 0.002(2) 0.0132(17)
C8 0.076(3) 0.052(2) 0.096(4) 0.030(2) 0.006(2) 0.024(2)
C9 0.084(3) 0.068(3) 0.063(3) 0.023(2) -0.002(2) 0.030(3)
C10 0.055(2) 0.053(2) 0.052(2) 0.0017(17) 0.0001(18) 0.0261(19)

_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 2.205(2) 16_554 ?
Cd1 N1 2.221(2) . ?
Cd1 O3 2.322(2) 12_444 ?
Cd1 N3 2.363(3) . ?
Cd1 O1 2.526(3) . ?
O1 C5 1.225(4) . ?
O2 C5 1.305(4) . ?
O2 H2 0.8200 . ?
O3 C3 1.268(4) . ?
O3 Cd1 2.322(2) 18_544 ?
O4 C3 1.225(4) . ?
N1 C1 1.336(4) . ?
N1 C4 1.374(3) . ?
N2 C1 1.330(4) . ?
N2 C2 1.370(4) . ?
N2 Cd1 2.205(2) 10_554 ?
N3 C10 1.328(5) . ?
N3 C6 1.336(4) . ?
C1 H1 0.9300 . ?
C2 C4 1.379(4) . ?
C2 C3 1.482(4) . ?
C4 C5 1.470(4) . ?
C6 C7 1.381(5) . ?
C6 H6 0.9300 . ?
C7 C8 1.375(6) . ?
C7 H7 0.9300 . ?
C8 C9 1.349(6) . ?
C8 H8 0.9300 . ?
C9 C10 1.384(5) . ?
C9 H9 0.9300 . ?
C10 H10 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

N2 Cd1 N1 161.61(9) 16_554 . ?
N2 Cd1 O3 100.67(9) 16_554 12_444 ?
N1 Cd1 O3 86.43(9) . 12_444 ?
N2 Cd1 N3 88.13(9) 16_554 . ?
N1 Cd1 N3 98.28(9) . . ?
O3 Cd1 N3 136.94(10) 12_444 . ?
N2 Cd1 O1 93.26(9) 16_554 . ?
N1 Cd1 O1 69.73(8) . . ?
O3 Cd1 O1 131.40(9) 12_444 . ?
N3 Cd1 O1 89.35(10) . . ?
C5 O1 Cd1 111.2(2) . . ?
C5 O2 H2 109.5 . . ?
C3 O3 Cd1 101.67(19) . 18_544 ?
C1 N1 C4 104.9(2) . . ?
C1 N1 Cd1 135.9(2) . . ?
C4 N1 Cd1 117.95(17) . . ?
C1 N2 C2 105.1(2) . . ?
C1 N2 Cd1 131.6(2) . 10_554 ?
C2 N2 Cd1 123.30(18) . 10_554 ?
C10 N3 C6 117.6(3) . . ?
C10 N3 Cd1 123.5(2) . . ?
C6 N3 Cd1 118.7(2) . . ?
N2 C1 N1 113.7(3) . . ?
N2 C1 H1 123.1 . . ?
N1 C1 H1 123.1 . . ?
N2 C2 C4 108.3(2) . . ?
N2 C2 C3 120.8(2) . . ?
C4 C2 C3 130.9(3) . . ?
O4 C3 O3 122.5(3) . . ?
O4 C3 C2 120.8(3) . . ?
O3 C3 C2 116.6(3) . . ?
N1 C4 C2 108.0(2) . . ?
N1 C4 C5 117.4(2) . . ?
C2 C4 C5 134.5(3) . . ?
O1 C5 O2 121.3(3) . . ?
O1 C5 C4 120.3(3) . . ?
O2 C5 C4 118.4(3) . . ?
N3 C6 C7 122.9(4) . . ?
N3 C6 H6 118.6 . . ?
C7 C6 H6 118.6 . . ?
C8 C7 C6 118.2(4) . . ?
C8 C7 H7 120.9 . . ?
C6 C7 H7 120.9 . . ?
C9 C8 C7 119.5(4) . . ?
C9 C8 H8 120.3 . . ?
C7 C8 H8 120.3 . . ?
C8 C9 C10 119.2(4) . . ?
C8 C9 H9 120.4 . . ?
C10 C9 H9 120.4 . . ?
N3 C10 C9 122.6(4) . . ?
N3 C10 H10 118.7 . . ?
C9 C10 H10 118.7 . . ?

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

N2 Cd1 O1 C5 156.9(2) 16_554 . . . ?
N1 Cd1 O1 C5 -15.9(2) . . . . ?
O3 Cd1 O1 C5 49.6(3) 12_444 . . . ?
N3 Cd1 O1 C5 -115.0(3) . . . . ?
N2 Cd1 N1 C1 156.2(3) 16_554 . . . ?
O3 Cd1 N1 C1 42.6(3) 12_444 . . . ?
N3 Cd1 N1 C1 -94.3(3) . . . . ?
O1 Cd1 N1 C1 179.5(3) . . . . ?
N2 Cd1 N1 C4 -8.9(4) 16_554 . . . ?
O3 Cd1 N1 C4 -122.5(2) 12_444 . . . ?
N3 Cd1 N1 C4 100.5(2) . . . . ?
O1 Cd1 N1 C4 14.32(19) . . . . ?
N2 Cd1 N3 C10 -106.3(3) 16_554 . . . ?
N1 Cd1 N3 C10 91.1(3) . . . . ?
O3 Cd1 N3 C10 -2.6(3) 12_444 . . . ?
O1 Cd1 N3 C10 160.5(3) . . . . ?
N2 Cd1 N3 C6 68.7(2) 16_554 . . . ?
N1 Cd1 N3 C6 -94.0(2) . . . . ?
O3 Cd1 N3 C6 172.3(2) 12_444 . . . ?
O1 Cd1 N3 C6 -24.6(2) . . . . ?
C2 N2 C1 N1 0.9(4) . . . . ?
Cd1 N2 C1 N1 179.6(2) 10_554 . . . ?
C4 N1 C1 N2 -0.9(4) . . . . ?
Cd1 N1 C1 N2 -167.3(2) . . . . ?
C1 N2 C2 C4 -0.6(3) . . . . ?
Cd1 N2 C2 C4 -179.47(19) 10_554 . . . ?
C1 N2 C2 C3 177.9(3) . . . . ?
Cd1 N2 C2 C3 -1.0(4) 10_554 . . . ?
Cd1 O3 C3 O4 1.0(4) 18_544 . . . ?
Cd1 O3 C3 C2 -179.3(2) 18_544 . . . ?
N2 C2 C3 O4 3.4(4) . . . . ?
C4 C2 C3 O4 -178.5(3) . . . . ?
N2 C2 C3 O3 -176.3(3) . . . . ?
C4 C2 C3 O3 1.8(5) . . . . ?
C1 N1 C4 C2 0.4(3) . . . . ?
Cd1 N1 C4 C2 169.76(19) . . . . ?
C1 N1 C4 C5 177.7(3) . . . . ?
Cd1 N1 C4 C5 -12.9(3) . . . . ?
N2 C2 C4 N1 0.1(3) . . . . ?
C3 C2 C4 N1 -178.2(3) . . . . ?
N2 C2 C4 C5 -176.5(3) . . . . ?
C3 C2 C4 C5 5.2(6) . . . . ?
Cd1 O1 C5 O2 -165.4(3) . . . . ?
Cd1 O1 C5 C4 15.4(4) . . . . ?
N1 C4 C5 O1 -3.5(4) . . . . ?
C2 C4 C5 O1 172.9(3) . . . . ?
N1 C4 C5 O2 177.2(3) . . . . ?
C2 C4 C5 O2 -6.4(5) . . . . ?
C10 N3 C6 C7 -0.2(5) . . . . ?
Cd1 N3 C6 C7 -175.4(3) . . . . ?
N3 C6 C7 C8 -0.6(6) . . . . ?
C6 C7 C8 C9 1.5(7) . . . . ?
C7 C8 C9 C10 -1.6(8) . . . . ?
C6 N3 C10 C9 0.1(6) . . . . ?
Cd1 N3 C10 C9 175.0(3) . . . . ?
C8 C9 C10 N3 0.8(7) . . . . ?

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

O2 H2 O3 0.82 1.72 2.523(3) 164.4 .

_diffrn_measured_fraction_theta_max 1.000

_diffrn_reflns_theta_full        25.16

_diffrn_measured_fraction_theta_full 1.000

_refine_diff_density_max         0.256

_refine_diff_density_min         -0.481

_refine_diff_density_rms         0.069


# Attachment '- Revised_717400(1).cif'

data_g
_database_code_depnum_ccdc_archive 'CCDC 773950'
#TrackingRef '- Revised_717400(1).cif'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C8 H6 Cd N4 O4'
_chemical_formula_sum            'C8 H6 Cd N4 O4'
_chemical_formula_weight         334.57

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'

_space_group_crystal_system      trigonal
_space_group_name_H-M_alt        'R 3 c'
_space_group_name_Hall           'R 3 -2"c'

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'-y, -x, z+1/2'
'-x+y, y, z+1/2'
'x, x-y, z+1/2'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'-y+2/3, -x+1/3, z+5/6'
'-x+y+2/3, y+1/3, z+5/6'
'x+2/3, x-y+1/3, z+5/6'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'-y+1/3, -x+2/3, z+7/6'
'-x+y+1/3, y+2/3, z+7/6'
'x+1/3, x-y+2/3, z+7/6'

_cell_length_a                   20.6556(6)
_cell_length_b                   20.6556(6)
_cell_length_c                   13.3915(7)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_volume                     4948.1(3)
_cell_formula_units_Z            18
_cell_measurement_temperature    298(2)
_cell_measurement_reflns_used    3854
_cell_measurement_theta_min      3.25
_cell_measurement_theta_max      26.73

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.15
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.021
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2916
_exptl_absorpt_coefficient_mu    1.995
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6250
_exptl_absorpt_correction_T_max  0.7540
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1996)'

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      298(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            8201
_diffrn_reflns_av_R_equivalents  0.0281
_diffrn_reflns_av_sigmaI/netI    0.0248
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_theta_min         1.97
_diffrn_reflns_theta_max         25.24
_reflns_number_total             1870
_reflns_number_gt                1794
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ 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/[\s^2^(Fo^2^)+(0.0153P)^2^+2.5507P] where P=(Fo^2^+2Fc^2^)/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   0.00(2)
_refine_ls_number_reflns         1870
_refine_ls_number_parameters     155
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0196
_refine_ls_R_factor_gt           0.0180
_refine_ls_wR_factor_ref         0.0380
_refine_ls_wR_factor_gt          0.0373
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_restrained_S_all      1.048
_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 0.657046(13) 0.576693(13) 0.88949(2) 0.03266(7) Uani 1 1 d . . .
O1 O 0.70741(15) 0.52274(16) 0.7574(2) 0.0483(8) Uani 1 1 d . . .
O2 O 0.81509(17) 0.5488(2) 0.6874(2) 0.0599(9) Uani 1 1 d . . .
H2 H 0.8594 0.5798 0.6947 0.090 Uiso 1 1 calc R . .
O3 O 0.94912(16) 0.62655(18) 0.7313(2) 0.0535(7) Uani 1 1 d . . .
O4 O 1.02127(15) 0.69550(17) 0.85318(19) 0.0470(7) Uani 1 1 d . . .
N1 N 0.77541(15) 0.61473(16) 0.9147(2) 0.0333(7) Uani 1 1 d . . .
N2 N 0.89544(15) 0.68037(17) 0.9583(2) 0.0353(7) Uani 1 1 d . . .
N3 N 0.59875(19) 0.46423(19) 0.9715(2) 0.0393(8) Uani 1 1 d . . .
N4 N 0.5445(2) 0.3764(2) 1.0822(3) 0.0610(10) Uani 1 1 d . . .
H4 H 0.5254 0.3546 1.1380 0.073 Uiso 1 1 calc R . .
C1 C 0.8248(2) 0.6600(3) 0.9796(4) 0.0402(8) Uani 1 1 d . . .
H1 H 0.8115 0.6766 1.0364 0.048 Uiso 1 1 calc R . .
C2 C 0.89132(19) 0.64622(19) 0.8690(2) 0.0308(7) Uani 1 1 d . . .
C3 C 0.9585(2) 0.6573(2) 0.8161(3) 0.0393(9) Uani 1 1 d . . .
C4 C 0.81666(18) 0.60529(18) 0.8423(2) 0.0313(8) Uani 1 1 d . . .
C5 C 0.7764(2) 0.5562(2) 0.7584(3) 0.0388(9) Uani 1 1 d . . .
C6 C 0.5829(3) 0.3982(2) 0.9311(3) 0.0667(14) Uani 1 1 d . . .
H6 H 0.5936 0.3915 0.8657 0.080 Uiso 1 1 calc R . .
C7 C 0.5498(3) 0.3435(3) 0.9987(4) 0.0718(15) Uani 1 1 d . . .
H7 H 0.5338 0.2930 0.9896 0.086 Uiso 1 1 calc R . .
C8 C 0.5744(2) 0.4495(3) 1.0628(3) 0.0480(10) Uani 1 1 d . . .
H8 H 0.5773 0.4848 1.1085 0.058 Uiso 1 1 calc R . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Cd1 0.02348(12) 0.03246(14) 0.03847(13) -0.00613(11) -0.00621(10) 0.01131(11)
O1 0.0381(17) 0.0576(18) 0.0447(16) -0.0193(13) -0.0157(13) 0.0205(15)
O2 0.0544(19) 0.083(3) 0.0433(16) -0.0271(17) -0.0048(15) 0.0352(19)
O3 0.0475(17) 0.075(2) 0.0447(17) -0.0031(15) 0.0099(14) 0.0352(16)
O4 0.0324(15) 0.0546(19) 0.0533(18) 0.0056(14) 0.0046(12) 0.0212(15)
N1 0.0251(15) 0.0394(17) 0.0339(16) -0.0077(14) -0.0021(13) 0.0151(14)
N2 0.0239(16) 0.0429(18) 0.0353(17) -0.0049(14) -0.0004(13) 0.0138(14)
N3 0.0400(18) 0.0396(19) 0.0367(19) 0.0018(14) 0.0022(14) 0.0187(16)
N4 0.055(2) 0.060(3) 0.051(2) 0.023(2) 0.0080(19) 0.016(2)
C1 0.0331(19) 0.051(2) 0.036(2) -0.0163(16) -0.0022(16) 0.021(2)
C2 0.0307(18) 0.0348(19) 0.0300(18) -0.0017(15) -0.0025(14) 0.0187(16)
C3 0.040(2) 0.041(2) 0.042(2) 0.0099(18) 0.0070(18) 0.0239(19)
C4 0.033(2) 0.0354(19) 0.0283(17) 0.0015(15) 0.0007(14) 0.0190(16)
C5 0.048(3) 0.039(2) 0.036(2) -0.0064(16) -0.0080(18) 0.027(2)
C6 0.098(4) 0.038(3) 0.047(2) 0.002(2) 0.009(3) 0.021(3)
C7 0.089(4) 0.040(3) 0.067(3) 0.006(2) 0.007(3) 0.018(3)
C8 0.044(3) 0.054(3) 0.042(3) -0.001(2) -0.0009(19) 0.021(2)

_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 2.182(3) 12_454 ?
Cd1 N1 2.188(3) . ?
Cd1 N3 2.293(3) . ?
Cd1 O4 2.404(3) 16_664 ?
Cd1 O3 2.558(3) 16_664 ?
Cd1 O1 2.572(3) . ?
O1 C5 1.235(4) . ?
O2 C5 1.299(5) . ?
O2 H2 0.8200 . ?
O3 C3 1.268(5) . ?
O3 Cd1 2.558(3) 10_664 ?
O4 C3 1.235(4) . ?
O4 Cd1 2.405(3) 10_664 ?
N1 C1 1.310(6) . ?
N1 C4 1.367(4) . ?
N2 C1 1.331(5) . ?
N2 C2 1.369(4) . ?
N2 Cd1 2.181(3) 18_554 ?
N3 C8 1.299(5) . ?
N3 C6 1.348(5) . ?
N4 C8 1.340(5) . ?
N4 C7 1.342(6) . ?
N4 H4 0.8600 . ?
C1 H1 0.9300 . ?
C2 C4 1.384(5) . ?
C2 C3 1.471(5) . ?
C4 C5 1.463(5) . ?
C6 C7 1.338(6) . ?
C6 H6 0.9300 . ?
C7 H7 0.9300 . ?
C8 H8 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
N2 Cd1 N1 151.91(10) 12_454 . ?
N2 Cd1 N3 94.03(12) 12_454 . ?
N1 Cd1 N3 102.50(12) . . ?
N2 Cd1 O4 101.70(10) 12_454 16_664 ?
N1 Cd1 O4 99.25(10) . 16_664 ?
N3 Cd1 O4 95.28(11) . 16_664 ?
N2 Cd1 O3 97.30(10) 12_454 16_664 ?
N1 Cd1 O3 81.00(10) . 16_664 ?
N3 Cd1 O3 147.14(10) . 16_664 ?
O4 Cd1 O3 52.24(9) 16_664 16_664 ?
N2 Cd1 O1 88.56(10) 12_454 . ?
N1 Cd1 O1 68.91(9) . . ?
N3 Cd1 O1 90.69(11) . . ?
O4 Cd1 O1 167.71(9) 16_664 . ?
O3 Cd1 O1 120.25(9) 16_664 . ?
C5 O1 Cd1 110.7(2) . . ?
C5 O2 H2 109.5 . . ?
C3 O3 Cd1 88.8(2) . 10_664 ?
C3 O4 Cd1 96.9(2) . 10_664 ?
C1 N1 C4 104.7(3) . . ?
C1 N1 Cd1 133.7(2) . . ?
C4 N1 Cd1 120.3(2) . . ?
C1 N2 C2 104.4(3) . . ?
C1 N2 Cd1 124.6(3) . 18_554 ?
C2 N2 Cd1 130.9(2) . 18_554 ?
C8 N3 C6 105.8(4) . . ?
C8 N3 Cd1 129.4(3) . . ?
C6 N3 Cd1 124.9(3) . . ?
C8 N4 C7 107.5(4) . . ?
C8 N4 H4 126.2 . . ?
C7 N4 H4 126.2 . . ?
N1 C1 N2 115.0(4) . . ?
N1 C1 H1 122.5 . . ?
N2 C1 H1 122.5 . . ?
N2 C2 C4 107.6(3) . . ?
N2 C2 C3 122.0(3) . . ?
C4 C2 C3 130.4(3) . . ?
O4 C3 O3 122.0(3) . . ?
O4 C3 C2 120.9(4) . . ?
O3 C3 C2 117.2(3) . . ?
N1 C4 C2 108.3(3) . . ?
N1 C4 C5 117.7(3) . . ?
C2 C4 C5 134.0(3) . . ?
O1 C5 O2 122.1(4) . . ?
O1 C5 C4 119.6(4) . . ?
O2 C5 C4 118.3(4) . . ?
C7 C6 N3 110.2(4) . . ?
C7 C6 H6 124.9 . . ?
N3 C6 H6 124.9 . . ?
C6 C7 N4 105.8(4) . . ?
C6 C7 H7 127.1 . . ?
N4 C7 H7 127.1 . . ?
N3 C8 N4 110.6(4) . . ?
N3 C8 H8 124.7 . . ?
N4 C8 H8 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
N2 Cd1 O1 C5 148.4(3) 12_454 . . . ?
N1 Cd1 O1 C5 -14.4(3) . . . . ?
N3 Cd1 O1 C5 -117.6(3) . . . . ?
O4 Cd1 O1 C5 1.6(6) 16_664 . . . ?
O3 Cd1 O1 C5 50.8(3) 16_664 . . . ?
N2 Cd1 N1 C1 138.7(4) 12_454 . . . ?
N3 Cd1 N1 C1 -96.7(4) . . . . ?
O4 Cd1 N1 C1 0.9(4) 16_664 . . . ?
O3 Cd1 N1 C1 50.1(4) 16_664 . . . ?
O1 Cd1 N1 C1 177.5(4) . . . . ?
N2 Cd1 N1 C4 -25.4(4) 12_454 . . . ?
N3 Cd1 N1 C4 99.2(3) . . . . ?
O4 Cd1 N1 C4 -163.2(2) 16_664 . . . ?
O3 Cd1 N1 C4 -114.1(3) 16_664 . . . ?
O1 Cd1 N1 C4 13.4(2) . . . . ?
N2 Cd1 N3 C8 -110.3(4) 12_454 . . . ?
N1 Cd1 N3 C8 92.6(4) . . . . ?
O4 Cd1 N3 C8 -8.1(4) 16_664 . . . ?
O3 Cd1 N3 C8 -0.2(5) 16_664 . . . ?
O1 Cd1 N3 C8 161.1(4) . . . . ?
N2 Cd1 N3 C6 69.8(4) 12_454 . . . ?
N1 Cd1 N3 C6 -87.4(4) . . . . ?
O4 Cd1 N3 C6 171.9(4) 16_664 . . . ?
O3 Cd1 N3 C6 179.9(3) 16_664 . . . ?
O1 Cd1 N3 C6 -18.8(4) . . . . ?
C4 N1 C1 N2 -1.4(5) . . . . ?
Cd1 N1 C1 N2 -167.3(3) . . . . ?
C2 N2 C1 N1 1.6(5) . . . . ?
Cd1 N2 C1 N1 -174.5(3) 18_554 . . . ?
C1 N2 C2 C4 -1.1(4) . . . . ?
Cd1 N2 C2 C4 174.6(2) 18_554 . . . ?
C1 N2 C2 C3 177.2(3) . . . . ?
Cd1 N2 C2 C3 -7.1(5) 18_554 . . . ?
Cd1 O4 C3 O3 -3.2(4) 10_664 . . . ?
Cd1 O4 C3 C2 177.4(3) 10_664 . . . ?
Cd1 O3 C3 O4 3.0(4) 10_664 . . . ?
Cd1 O3 C3 C2 -177.6(3) 10_664 . . . ?
N2 C2 C3 O4 3.2(5) . . . . ?
C4 C2 C3 O4 -178.9(4) . . . . ?
N2 C2 C3 O3 -176.1(3) . . . . ?
C4 C2 C3 O3 1.7(6) . . . . ?
C1 N1 C4 C2 0.6(4) . . . . ?
Cd1 N1 C4 C2 168.8(2) . . . . ?
C1 N1 C4 C5 179.5(3) . . . . ?
Cd1 N1 C4 C5 -12.3(4) . . . . ?
N2 C2 C4 N1 0.4(4) . . . . ?
C3 C2 C4 N1 -177.7(3) . . . . ?
N2 C2 C4 C5 -178.3(4) . . . . ?
C3 C2 C4 C5 3.6(7) . . . . ?
Cd1 O1 C5 O2 -167.2(3) . . . . ?
Cd1 O1 C5 C4 13.7(4) . . . . ?
N1 C4 C5 O1 -3.2(5) . . . . ?
C2 C4 C5 O1 175.4(4) . . . . ?
N1 C4 C5 O2 177.7(3) . . . . ?
C2 C4 C5 O2 -3.7(6) . . . . ?
C8 N3 C6 C7 -0.8(6) . . . . ?
Cd1 N3 C6 C7 179.1(4) . . . . ?
N3 C6 C7 N4 0.5(6) . . . . ?
C8 N4 C7 C6 0.0(6) . . . . ?
C6 N3 C8 N4 0.8(5) . . . . ?
Cd1 N3 C8 N4 -179.2(3) . . . . ?
C7 N4 C8 N3 -0.5(6) . . . . ?

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
N4 H4 O1 0.86 1.98 2.833(4) 172.9 4_665
O2 H2 O3 0.82 1.68 2.478(4) 164.8 .

_diffrn_measured_fraction_theta_max 1.000
_diffrn_reflns_theta_full        25.24
_diffrn_measured_fraction_theta_full 1.000
_refine_diff_density_max         0.326
_refine_diff_density_min         -0.209
_refine_diff_density_rms         0.048