# Electronic Supplementary Material for CrystEngComm
# This journal is (c) The Royal Society of Chemistry 2009

data_global
_journal_name_full               CrystEngComm

_journal_coden_Cambridge         1350

_publ_contact_author_name        'Feng Luo'
_publ_contact_author_email       'LUOFENG 123456@MAIL.NANKAI.EDU.CN'

_publ_section_title              
;
Two new metal-triazole-benzenedicarboxylate frameworks
affording uncommon 3,4-connected net and unique 4,6-connected rod
packing topology: hydrothermal synthesis, structure, thermo-stability,
and luminescence studies
;
loop_
_publ_author_name
'Feng Luo'
'Yun-xia Che'
'Jimin Zheng'

# Attachment '1.cif'

data_shelxl
_database_code_depnum_ccdc_archive 'CCDC 695633'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C10 H7 N3 O4 Zn'
_chemical_formula_weight         298.56

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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   P2(1)/c

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

_cell_length_a                   11.288(2)
_cell_length_b                   9.6710(19)
_cell_length_c                   10.281(2)
_cell_angle_alpha                90.00
_cell_angle_beta                 97.79(3)
_cell_angle_gamma                90.00
_cell_volume                     1112.0(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    9120
_cell_measurement_theta_min      3.28
_cell_measurement_theta_max      30.16

_exptl_crystal_description       Block
_exptl_crystal_colour            Colorless
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.17
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.783
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             600
_exptl_absorpt_coefficient_mu    2.219
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.6530
_exptl_absorpt_correction_T_max  0.7042
_exptl_absorpt_process_details   ?

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      296(2)
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'rotating anode'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'rigaku r-axis rapid IP area detector'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            10753
_diffrn_reflns_av_R_equivalents  0.0284
_diffrn_reflns_av_sigmaI/netI    0.0231
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_theta_min         3.28
_diffrn_reflns_theta_max         27.48
_reflns_number_total             2559
_reflns_number_gt                2312
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'RAXIS-RAPID Auto(Rigaku, 2004)'
_computing_cell_refinement       'RAXIS-RAPID Auto(Rigaku, 2004)'
_computing_data_reduction        'CrystalStructure(Rigaku/MSC, 2004)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'SHELXL-97 (Sheldrick, 2001)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'

_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)+(0.0305P)²+0.4647P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    refu
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         2559
_refine_ls_number_parameters     167
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0271
_refine_ls_R_factor_gt           0.0237
_refine_ls_wR_factor_ref         0.0613
_refine_ls_wR_factor_gt          0.0596
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_restrained_S_all      1.045
_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 -0.21948(17) 0.8921(2) 0.0358(2) 0.0382(4) Uani 1 1 d . . .
C2 C -0.02583(16) 0.7648(2) 0.07347(19) 0.0359(4) Uani 1 1 d . . .
H2 H 0.0100 0.8395 0.0374 0.043 Uiso 1 1 calc R . .
C3 C -0.14806(17) 0.7678(2) 0.08161(19) 0.0352(4) Uani 1 1 d . . .
C4 C 0.04278(16) 0.6516(2) 0.11854(18) 0.0338(4) Uani 1 1 d . . .
C5 C 0.47874(18) 0.33443(18) 0.24332(17) 0.0348(4) Uani 1 1 d . . .
H5 H 0.4358 0.3588 0.3110 0.042 Uiso 1 1 calc R . .
C6 C 0.17390(17) 0.6507(2) 0.10702(18) 0.0353(4) Uani 1 1 d . . .
C7 C -0.1333(2) 0.5419(2) 0.1786(2) 0.0471(5) Uani 1 1 d . . .
H7 H -0.1692 0.4667 0.2138 0.056 Uiso 1 1 calc R . .
C8 C 0.58790(17) 0.22717(18) 0.12907(17) 0.0337(4) Uani 1 1 d . . .
H8 H 0.6372 0.1602 0.0998 0.040 Uiso 1 1 calc R . .
C9 C -0.20126(18) 0.6552(2) 0.1342(2) 0.0416(4) Uani 1 1 d . . .
H9 H -0.2828 0.6561 0.1396 0.050 Uiso 1 1 calc R . .
C10 C -0.01131(18) 0.5395(2) 0.1708(2) 0.0407(4) Uani 1 1 d . . .
H10 H 0.0341 0.4628 0.2007 0.049 Uiso 1 1 calc R . .
H1A H -0.189(3) 1.070(3) -0.019(3) 0.077(9) Uiso 1 1 d . . .
N1 N 0.48276(14) 0.41049(13) 0.13797(15) 0.0293(3) Uani 1 1 d . . .
N2 N 0.55484(13) 0.34051(14) 0.06358(13) 0.0266(3) Uani 1 1 d . . .
N3 N 0.54275(13) 0.21882(14) 0.24272(14) 0.0282(3) Uani 1 1 d . . .
O1 O 0.23414(12) 0.54343(14) 0.14357(14) 0.0388(3) Uani 1 1 d . . .
O2 O 0.22318(13) 0.75288(16) 0.06246(16) 0.0486(4) Uani 1 1 d . . .
O3 O -0.32692(13) 0.90023(16) 0.02748(18) 0.0517(4) Uani 1 1 d . . .
O4 O -0.15147(14) 0.99486(18) 0.0081(2) 0.0627(5) Uani 1 1 d . . .
Zn1 Zn 0.397206(17) 0.593532(18) 0.106514(17) 0.02457(8) Uani 1 1 d . . .


_geom_special_details            
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 O3 1.207(2) . ?
C1 O4 1.311(2) . ?
C1 C3 1.487(3) . ?
C2 C4 1.384(3) . ?
C2 C3 1.394(3) . ?
C2 H2 0.9300 . ?
C3 C9 1.389(3) . ?
C4 C10 1.388(3) . ?
C4 C6 1.501(3) . ?
C5 N1 1.315(2) . ?
C5 N3 1.332(2) . ?
C5 H5 0.9300 . ?
C6 O2 1.251(2) . ?
C6 O1 1.269(2) . ?
C6 Zn1 2.5813(19) . ?
C7 C9 1.379(3) . ?
C7 C10 1.390(3) . ?
C7 H7 0.9300 . ?
C8 N2 1.314(2) . ?
C8 N3 1.339(2) . ?
C8 H8 0.9300 . ?
C9 H9 0.9300 . ?
C10 H10 0.9300 . ?
N1 N2 1.3689(18) . ?
N1 Zn1 2.0214(14) . ?
N2 Zn1 2.0036(14) 3_665 ?
N3 Zn1 2.0112(14) 2_645 ?
O1 Zn1 1.9895(14) . ?
O2 Zn1 2.4894(14) . ?
O4 H1A 0.87(3) . ?
Zn1 N2 2.0036(14) 3_665 ?
Zn1 N3 2.0112(14) 2_655 ?

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 C1 O4 123.21(19) . . ?
O3 C1 C3 124.86(19) . . ?
O4 C1 C3 111.91(17) . . ?
C4 C2 C3 120.70(18) . . ?
C4 C2 H2 119.7 . . ?
C3 C2 H2 119.7 . . ?
C9 C3 C2 119.37(18) . . ?
C9 C3 C1 120.84(17) . . ?
C2 C3 C1 119.79(17) . . ?
C2 C4 C10 119.45(18) . . ?
C2 C4 C6 119.44(17) . . ?
C10 C4 C6 121.09(18) . . ?
N1 C5 N3 112.74(14) . . ?
N1 C5 H5 123.6 . . ?
N3 C5 H5 123.6 . . ?
O2 C6 O1 120.47(17) . . ?
O2 C6 C4 121.10(17) . . ?
O1 C6 C4 118.43(18) . . ?
O2 C6 Zn1 71.67(10) . . ?
O1 C6 Zn1 48.80(9) . . ?
C4 C6 Zn1 167.22(14) . . ?
C9 C7 C10 120.4(2) . . ?
C9 C7 H7 119.8 . . ?
C10 C7 H7 119.8 . . ?
N2 C8 N3 112.48(15) . . ?
N2 C8 H8 123.8 . . ?
N3 C8 H8 123.8 . . ?
C7 C9 C3 120.09(19) . . ?
C7 C9 H9 120.0 . . ?
C3 C9 H9 120.0 . . ?
C4 C10 C7 120.03(19) . . ?
C4 C10 H10 120.0 . . ?
C7 C10 H10 120.0 . . ?
C5 N1 N2 105.85(13) . . ?
C5 N1 Zn1 123.54(12) . . ?
N2 N1 Zn1 130.60(11) . . ?
C8 N2 N1 105.97(13) . . ?
C8 N2 Zn1 128.42(11) . 3_665 ?
N1 N2 Zn1 125.57(10) . 3_665 ?
C5 N3 C8 102.96(14) . . ?
C5 N3 Zn1 128.95(11) . 2_645 ?
C8 N3 Zn1 125.49(12) . 2_645 ?
C6 O1 Zn1 102.52(12) . . ?
C6 O2 Zn1 79.83(11) . . ?
C1 O4 H1A 116(2) . . ?
O1 Zn1 N2 127.67(6) . 3_665 ?
O1 Zn1 N3 102.89(6) . 2_655 ?
N2 Zn1 N3 112.22(6) 3_665 2_655 ?
O1 Zn1 N1 100.97(6) . . ?
N2 Zn1 N1 103.81(6) 3_665 . ?
N3 Zn1 N1 107.49(6) 2_655 . ?
O1 Zn1 O2 57.17(5) . . ?
N2 Zn1 O2 86.79(6) 3_665 . ?
N3 Zn1 O2 86.70(6) 2_655 . ?
N1 Zn1 O2 156.82(6) . . ?
O1 Zn1 C6 28.68(6) . . ?
N2 Zn1 C6 108.24(6) 3_665 . ?
N3 Zn1 C6 95.54(6) 2_655 . ?
N1 Zn1 C6 129.25(6) . . ?
O2 Zn1 C6 28.49(5) . . ?

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
C4 C2 C3 C9 -0.7(3) . . . . ?
C4 C2 C3 C1 178.36(18) . . . . ?
O3 C1 C3 C9 -8.0(3) . . . . ?
O4 C1 C3 C9 170.4(2) . . . . ?
O3 C1 C3 C2 172.9(2) . . . . ?
O4 C1 C3 C2 -8.7(3) . . . . ?
C3 C2 C4 C10 0.8(3) . . . . ?
C3 C2 C4 C6 179.31(17) . . . . ?
C2 C4 C6 O2 3.0(3) . . . . ?
C10 C4 C6 O2 -178.48(19) . . . . ?
C2 C4 C6 O1 -176.92(18) . . . . ?
C10 C4 C6 O1 1.6(3) . . . . ?
C2 C4 C6 Zn1 -174.4(5) . . . . ?
C10 C4 C6 Zn1 4.0(7) . . . . ?
C10 C7 C9 C3 -0.1(3) . . . . ?
C2 C3 C9 C7 0.4(3) . . . . ?
C1 C3 C9 C7 -178.7(2) . . . . ?
C2 C4 C10 C7 -0.5(3) . . . . ?
C6 C4 C10 C7 -179.0(2) . . . . ?
C9 C7 C10 C4 0.1(3) . . . . ?
N3 C5 N1 N2 -0.4(2) . . . . ?
N3 C5 N1 Zn1 -179.52(12) . . . . ?
N3 C8 N2 N1 -0.5(2) . . . . ?
N3 C8 N2 Zn1 177.08(12) . . . 3_665 ?
C5 N1 N2 C8 0.5(2) . . . . ?
Zn1 N1 N2 C8 179.60(14) . . . . ?
C5 N1 N2 Zn1 -177.16(13) . . . 3_665 ?
Zn1 N1 N2 Zn1 1.9(2) . . . 3_665 ?
N1 C5 N3 C8 0.1(2) . . . . ?
N1 C5 N3 Zn1 162.23(13) . . . 2_645 ?
N2 C8 N3 C5 0.3(2) . . . . ?
N2 C8 N3 Zn1 -162.68(13) . . . 2_645 ?
O2 C6 O1 Zn1 -0.7(2) . . . . ?
C4 C6 O1 Zn1 179.27(14) . . . . ?
O1 C6 O2 Zn1 0.55(17) . . . . ?
C4 C6 O2 Zn1 -179.41(17) . . . . ?
C6 O1 Zn1 N2 -54.03(14) . . . 3_665 ?
C6 O1 Zn1 N3 77.78(13) . . . 2_655 ?
C6 O1 Zn1 N1 -171.22(12) . . . . ?
C6 O1 Zn1 O2 0.36(11) . . . . ?
C5 N1 Zn1 O1 -49.15(17) . . . . ?
N2 N1 Zn1 O1 131.94(16) . . . . ?
C5 N1 Zn1 N2 177.33(16) . . . 3_665 ?
N2 N1 Zn1 N2 -1.59(19) . . . 3_665 ?
C5 N1 Zn1 N3 58.27(17) . . . 2_655 ?
N2 N1 Zn1 N3 -120.65(16) . . . 2_655 ?
C5 N1 Zn1 O2 -67.4(2) . . . . ?
N2 N1 Zn1 O2 113.73(18) . . . . ?
C5 N1 Zn1 C6 -54.57(19) . . . . ?
N2 N1 Zn1 C6 126.51(15) . . . . ?
C6 O2 Zn1 O1 -0.36(11) . . . . ?
C6 O2 Zn1 N2 139.51(12) . . . 3_665 ?
C6 O2 Zn1 N3 -108.00(12) . . . 2_655 ?
C6 O2 Zn1 N1 21.1(2) . . . . ?
O2 C6 Zn1 O1 179.4(2) . . . . ?
C4 C6 Zn1 O1 -2.9(5) . . . . ?
O2 C6 Zn1 N2 -43.05(13) . . . 3_665 ?
O1 C6 Zn1 N2 137.58(12) . . . 3_665 ?
C4 C6 Zn1 N2 134.7(6) . . . 3_665 ?
O2 C6 Zn1 N3 72.54(12) . . . 2_655 ?
O1 C6 Zn1 N3 -106.82(12) . . . 2_655 ?
C4 C6 Zn1 N3 -109.7(6) . . . 2_655 ?
O2 C6 Zn1 N1 -169.48(11) . . . . ?
O1 C6 Zn1 N1 11.15(15) . . . . ?
C4 C6 Zn1 N1 8.2(6) . . . . ?
O1 C6 Zn1 O2 -179.4(2) . . . . ?
C4 C6 Zn1 O2 177.7(7) . . . . ?

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        27.48
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         0.278
_refine_diff_density_min         -0.443
_refine_diff_density_rms         0.063

# Attachment '2R.cif'

data_shelxl
_database_code_depnum_ccdc_archive 'CCDC 695634'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C28 H16 Cd4 N6 O15'
_chemical_formula_weight         1126.07

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

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   C2/c

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

_cell_length_a                   18.981(7)
_cell_length_b                   6.9876(14)
_cell_length_c                   25.368(5)
_cell_angle_alpha                90.00
_cell_angle_beta                 100.63(3)
_cell_angle_gamma                90.00
_cell_volume                     3306.9(15)
_cell_formula_units_Z            4
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    13372
_cell_measurement_theta_min      3.11
_cell_measurement_theta_max      25.00

_exptl_crystal_description       Block
_exptl_crystal_colour            Colorless
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.10
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.262
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2152
_exptl_absorpt_coefficient_mu    2.620
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.4878
_exptl_absorpt_correction_T_max  0.7796
_exptl_absorpt_process_details   ?

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      296(2)
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'rotating anode'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'rigaku r-axis rapid IP area detector'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            11870
_diffrn_reflns_av_R_equivalents  0.1296
_diffrn_reflns_av_sigmaI/netI    0.1314
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_theta_min         3.11
_diffrn_reflns_theta_max         25.00
_reflns_number_total             2746
_reflns_number_gt                2180
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'RAXIS-RAPID Auto(Rigaku, 2004)'
_computing_cell_refinement       'RAXIS-RAPID Auto(Rigaku, 2004)'
_computing_data_reduction        'CrystalStructure(Rigaku/MSC, 2004)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'SHELXL-97 (Sheldrick, 2001)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'

_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)+(0.0000P)²+13.1368P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     SHELXL
_refine_ls_extinction_coef       0.000610(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         2746
_refine_ls_number_parameters     241
_refine_ls_number_restraints     6
_refine_ls_R_factor_all          0.0925
_refine_ls_R_factor_gt           0.0779
_refine_ls_wR_factor_ref         0.1440
_refine_ls_wR_factor_gt          0.1348
_refine_ls_goodness_of_fit_ref   1.156
_refine_ls_restrained_S_all      1.155
_refine_ls_shift/su_max          0.120
_refine_ls_shift/su_mean         0.006

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 1.117120(15) -0.08376(4) 0.704976(12) 0.01909(9) Uani 1 1 d . . .
C2 C 1.253388(15) -0.18009(4) 0.880336(12) 0.02152(9) Uani 1 1 d . . .
H2 H 1.2405 -0.2947 0.8946 0.026 Uiso 1 1 calc R . .
C3 C 0.945706(17) 0.26196(4) 0.624670(13) 0.02541(10) Uani 1 1 d . . .
C4 C 1.056941(16) 0.03750(4) 0.676527(12) 0.02248(9) Uani 1 1 d . . .
C5 C 0.884937(16) 0.37873(4) 0.594847(13) 0.02402(9) Uani 1 1 d . . .
C6 C 1.071226(17) 0.19470(5) 0.647980(14) 0.03191(11) Uani 1 1 d . . .
H6 H 1.1183 0.2270 0.6463 0.038 Uiso 1 1 calc R . .
C7 C 0.986444(15) -0.00972(4) 0.679124(13) 0.02523(10) Uani 1 1 d . . .
H7 H 0.9770 -0.1179 0.6980 0.030 Uiso 1 1 calc R . .
C8 C 1.014870(17) 0.30509(5) 0.621694(14) 0.03475(11) Uani 1 1 d . . .
H8 H 1.0244 0.4103 0.6017 0.042 Uiso 1 1 calc R . .
C9 C 0.540123(15) 0.35517(4) 0.525938(13) 0.02471(10) Uani 1 1 d . . .
H9 H 0.5680 0.2582 0.5443 0.030 Uiso 1 1 calc R . .
C10 C 0.532366(15) 0.65198(4) 0.477676(13) 0.02530(10) Uani 1 1 d . . .
H10 H 0.5537 0.7548 0.4634 0.030 Uiso 1 1 calc R . .
C11 C 1.289741(16) 0.10231(4) 0.873006(11) 0.01894(9) Uani 1 1 d . . .
H11 H 1.3078 0.2247 0.8811 0.023 Uiso 1 1 calc R . .
C13 C 0.574051(14) 0.50292(4) 0.503075(12) 0.01868(9) Uani 1 1 d . . .
C14 C 0.930942(16) 0.10179(4) 0.654102(13) 0.02247(9) Uani 1 1 d . . .
H14 H 0.8839 0.0716 0.6566 0.027 Uiso 1 1 calc R . .
Cd2 Cd 0.795075(1) 0.500435(3) 0.498809(1) 0.01479(1) Uani 1 1 d . . .
Cd1 Cd 1.276376(1) 0.171277(3) 0.744664(1) 0.01841(1) Uani 1 1 d . . .
N1 N 1.247568(12) -0.14848(3) 0.828439(9) 0.01639(7) Uani 1 1 d . . .
N2 N 1.280136(13) -0.02792(3) 0.910595(9) 0.01665(7) Uani 1 1 d . . .
N3 N 1.270787(13) 0.03661(3) 0.823923(10) 0.01941(7) Uani 1 1 d . . .
O1 O 0.688476(10) 0.35268(3) 0.516749(8) 0.02194(6) Uani 1 1 d . . .
O2 O 0.683293(10) 0.65519(3) 0.496819(9) 0.02770(7) Uani 1 1 d . . .
O3 O 1.180776(11) -0.03345(3) 0.705798(9) 0.02512(7) Uani 1 1 d . . .
O4 O 1.101438(12) -0.23706(3) 0.727340(10) 0.03596(8) Uani 1 1 d . . .
O5 O 0.895248(11) 0.45505(3) 0.552051(9) 0.03140(7) Uani 1 1 d . . .
O6 O 0.827180(12) 0.39195(3) 0.612649(11) 0.03822(8) Uani 1 1 d . . .
O7 O 1.333930(12) -0.10359(3) 0.720047(10) 0.03764(8) Uani 1 1 d . . .
O8 O 0.0000 0.53300(6) 0.2500 0.07406(18) Uani 1 2 d S . .
C12 C 0.653065(13) 0.50062(4) 0.505888(11) 0.00948(7) Uani 1 1 d U . .


_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 O3 1.2548(6) . ?
C1 O4 1.2729(4) . ?
C1 C4 1.4965(6) . ?
C2 N1 1.3193(4) . ?
C2 N2 1.3542(4) . ?
C3 C8 1.3625(7) . ?
C3 C14 1.4021(5) . ?
C3 C5 1.4989(6) . ?
C4 C6 1.3700(5) . ?
C4 C7 1.3915(6) . ?
C5 O5 1.2569(5) . ?
C5 O6 1.2637(6) . ?
C6 C8 1.3859(6) . ?
C7 C14 1.3686(5) . ?
C9 C10 1.3629(7) 5_666 ?
C9 C13 1.3981(5) . ?
C10 C9 1.3629(7) 5_666 ?
C10 C13 1.3921(5) . ?
C11 N3 1.3135(5) . ?
C11 N2 1.3545(4) . ?
C13 C12 1.4883(7) . ?
Cd2 O5 2.1430(9) . ?
Cd2 N2 2.2116(5) 8_455 ?
Cd2 O2 2.3736(7) . ?
Cd2 O1 2.3889(7) . ?
Cd2 O2 2.4402(5) 7_666 ?
Cd2 O1 2.5272(5) 7_656 ?
Cd2 C12 2.7343(10) . ?
Cd1 N1 2.2183(4) 4_756 ?
Cd1 N3 2.2401(4) . ?
Cd1 O7 2.3503(5) . ?
Cd1 O3 2.3772(6) . ?
Cd1 O4 2.3845(9) 4_756 ?
Cd1 O3 2.4740(5) 4_756 ?
N1 N3 1.3779(4) . ?
N1 Cd1 2.2183(4) 4_746 ?
N2 Cd2 2.2116(5) 8_556 ?
O1 C12 1.2361(4) . ?
O1 Cd2 2.5272(5) 7_656 ?
O2 C12 1.2639(4) . ?
O2 Cd2 2.4402(5) 7_666 ?
O3 Cd1 2.4740(5) 4_746 ?
O4 Cd1 2.3845(9) 4_746 ?

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 C1 O4 122.14(3) . . ?
O3 C1 C4 119.76(3) . . ?
O4 C1 C4 118.10(3) . . ?
N1 C2 N2 112.82(3) . . ?
C8 C3 C14 119.69(3) . . ?
C8 C3 C5 120.75(4) . . ?
C14 C3 C5 119.51(3) . . ?
C6 C4 C7 120.06(3) . . ?
C6 C4 C1 120.07(3) . . ?
C7 C4 C1 119.87(3) . . ?
O5 C5 O6 124.14(3) . . ?
O5 C5 C3 116.04(4) . . ?
O6 C5 C3 119.80(3) . . ?
C4 C6 C8 119.35(4) . . ?
C14 C7 C4 120.51(4) . . ?
C3 C8 C6 121.08(4) . . ?
C10 C9 C13 122.39(3) 5_666 . ?
C9 C10 C13 118.96(3) 5_666 . ?
N3 C11 N2 112.56(3) . . ?
C10 C13 C9 118.59(3) . . ?
C10 C13 C12 120.79(3) . . ?
C9 C13 C12 120.62(3) . . ?
C7 C14 C3 119.28(3) . . ?
O5 Cd2 N2 125.72(3) . 8_455 ?
O5 Cd2 O2 140.040(17) . . ?
N2 Cd2 O2 89.52(3) 8_455 . ?
O5 Cd2 O1 120.01(2) . . ?
N2 Cd2 O1 105.98(3) 8_455 . ?
O2 Cd2 O1 54.25(2) . . ?
O5 Cd2 O2 89.712(11) . 7_666 ?
N2 Cd2 O2 87.102(10) 8_455 7_666 ?
O2 Cd2 O2 72.180(16) . 7_666 ?
O1 Cd2 O2 123.978(9) . 7_666 ?
O5 Cd2 O1 80.396(9) . 7_656 ?
N2 Cd2 O1 85.598(9) 8_455 7_656 ?
O2 Cd2 O1 125.252(11) . 7_656 ?
O1 Cd2 O1 74.999(15) . 7_656 ?
O2 Cd2 O1 160.959(10) 7_666 7_656 ?
O5 Cd2 C12 136.841(19) . . ?
N2 Cd2 C12 97.03(3) 8_455 . ?
O2 Cd2 C12 27.506(12) . . ?
O1 Cd2 C12 26.853(12) . . ?
O2 Cd2 C12 98.986(8) 7_666 . ?
O1 Cd2 C12 99.346(9) 7_656 . ?
N1 Cd1 N3 162.274(11) 4_756 . ?
N1 Cd1 O7 105.988(19) 4_756 . ?
N3 Cd1 O7 89.799(19) . . ?
N1 Cd1 O3 88.39(2) 4_756 . ?
N3 Cd1 O3 87.74(2) . . ?
O7 Cd1 O3 75.80(2) . . ?
N1 Cd1 O4 97.73(3) 4_756 4_756 ?
N3 Cd1 O4 92.87(3) . 4_756 ?
O7 Cd1 O4 79.888(19) . 4_756 ?
O3 Cd1 O4 155.678(10) . 4_756 ?
N1 Cd1 O3 87.05(2) 4_756 4_756 ?
N3 Cd1 O3 87.706(17) . 4_756 ?
O7 Cd1 O3 133.719(19) . 4_756 ?
O3 Cd1 O3 150.088(9) . 4_756 ?
O4 Cd1 O3 54.137(14) 4_756 4_756 ?
C2 N1 N3 105.72(2) . . ?
C2 N1 Cd1 134.89(2) . 4_746 ?
N3 N1 Cd1 118.86(2) . 4_746 ?
C2 N2 C11 102.33(3) . . ?
C2 N2 Cd2 127.33(2) . 8_556 ?
C11 N2 Cd2 130.18(2) . 8_556 ?
C11 N3 N1 106.57(3) . . ?
C11 N3 Cd1 130.84(2) . . ?
N1 N3 Cd1 122.53(2) . . ?
C12 O1 Cd2 92.35(3) . . ?
C12 O1 Cd2 149.25(2) . 7_656 ?
Cd2 O1 Cd2 105.001(15) . 7_656 ?
C12 O2 Cd2 92.34(3) . . ?
C12 O2 Cd2 155.88(2) . 7_666 ?
Cd2 O2 Cd2 107.820(16) . 7_666 ?
C1 O3 Cd1 146.56(2) . . ?
C1 O3 Cd1 90.01(3) . 4_746 ?
Cd1 O3 Cd1 97.87(2) . 4_746 ?
C1 O4 Cd1 93.68(2) . 4_746 ?
C5 O5 Cd2 110.23(3) . . ?
O1 C12 O2 120.58(3) . . ?
O1 C12 C13 121.43(3) . . ?
O2 C12 C13 117.99(3) . . ?
O1 C12 Cd2 60.801(19) . . ?
O2 C12 Cd2 60.154(17) . . ?
C13 C12 Cd2 173.57(2) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O3 C1 C4 C6 5.08(5) . . . . ?
O4 C1 C4 C6 -174.33(3) . . . . ?
O3 C1 C4 C7 -174.92(3) . . . . ?
O4 C1 C4 C7 5.67(4) . . . . ?
C8 C3 C5 O5 29.62(4) . . . . ?
C14 C3 C5 O5 -147.67(3) . . . . ?
C8 C3 C5 O6 -151.88(3) . . . . ?
C14 C3 C5 O6 30.83(4) . . . . ?
C7 C4 C6 C8 -0.24(5) . . . . ?
C1 C4 C6 C8 179.76(3) . . . . ?
C6 C4 C7 C14 -1.17(5) . . . . ?
C1 C4 C7 C14 178.83(3) . . . . ?
C14 C3 C8 C6 -0.96(5) . . . . ?
C5 C3 C8 C6 -178.24(3) . . . . ?
C4 C6 C8 C3 1.31(5) . . . . ?
C9 C10 C13 C9 -2.66(5) 5_666 . . . ?
C9 C10 C13 C12 177.36(3) 5_666 . . . ?
C10 C9 C13 C10 2.75(5) 5_666 . . . ?
C10 C9 C13 C12 -177.26(3) 5_666 . . . ?
C4 C7 C14 C3 1.52(5) . . . . ?
C8 C3 C14 C7 -0.46(5) . . . . ?
C5 C3 C14 C7 176.86(3) . . . . ?
N2 C2 N1 N3 -0.95(3) . . . . ?
N2 C2 N1 Cd1 170.22(2) . . . 4_746 ?
N1 C2 N2 C11 0.67(3) . . . . ?
N1 C2 N2 Cd2 176.480(19) . . . 8_556 ?
N3 C11 N2 C2 -0.11(3) . . . . ?
N3 C11 N2 Cd2 -175.749(19) . . . 8_556 ?
N2 C11 N3 N1 -0.44(3) . . . . ?
N2 C11 N3 Cd1 -177.569(19) . . . . ?
C2 N1 N3 C11 0.82(3) . . . . ?
Cd1 N1 N3 C11 -172.039(19) 4_746 . . . ?
C2 N1 N3 Cd1 178.244(19) . . . . ?
Cd1 N1 N3 Cd1 5.38(3) 4_746 . . . ?
N1 Cd1 N3 C11 -77.25(4) 4_756 . . . ?
O7 Cd1 N3 C11 129.42(3) . . . . ?
O3 Cd1 N3 C11 -154.79(3) . . . . ?
O4 Cd1 N3 C11 49.55(3) 4_756 . . . ?
O3 Cd1 N3 C11 -4.36(3) 4_756 . . . ?
N1 Cd1 N3 N1 106.02(3) 4_756 . . . ?
O7 Cd1 N3 N1 -47.32(3) . . . . ?
O3 Cd1 N3 N1 28.48(2) . . . . ?
O4 Cd1 N3 N1 -127.18(2) 4_756 . . . ?
O3 Cd1 N3 N1 178.91(2) 4_756 . . . ?
O5 Cd2 O1 C12 136.393(18) . . . . ?
N2 Cd2 O1 C12 -73.53(2) 8_455 . . . ?
O2 Cd2 O1 C12 3.950(15) . . . . ?
O2 Cd2 O1 C12 23.92(2) 7_666 . . . ?
O1 Cd2 O1 C12 -154.35(2) 7_656 . . . ?
O5 Cd2 O1 Cd2 -69.252(15) . . . 7_656 ?
N2 Cd2 O1 Cd2 80.828(15) 8_455 . . 7_656 ?
O2 Cd2 O1 Cd2 158.305(13) . . . 7_656 ?
O2 Cd2 O1 Cd2 178.273(7) 7_666 . . 7_656 ?
O1 Cd2 O1 Cd2 0.0 7_656 . . 7_656 ?
C12 Cd2 O1 Cd2 154.35(2) . . . 7_656 ?
O5 Cd2 O2 C12 -99.63(2) . . . . ?
N2 Cd2 O2 C12 106.33(2) 8_455 . . . ?
O1 Cd2 O2 C12 -3.863(15) . . . . ?
O2 Cd2 O2 C12 -166.56(2) 7_666 . . . ?
O1 Cd2 O2 C12 22.07(2) 7_656 . . . ?
O5 Cd2 O2 Cd2 66.931(19) . . . 7_666 ?
N2 Cd2 O2 Cd2 -87.109(17) 8_455 . . 7_666 ?
O1 Cd2 O2 Cd2 162.695(14) . . . 7_666 ?
O2 Cd2 O2 Cd2 0.0 7_666 . . 7_666 ?
O1 Cd2 O2 Cd2 -171.376(7) 7_656 . . 7_666 ?
C12 Cd2 O2 Cd2 166.56(2) . . . 7_666 ?
O4 C1 O3 Cd1 -102.50(4) . . . . ?
C4 C1 O3 Cd1 78.11(5) . . . . ?
O4 C1 O3 Cd1 1.89(3) . . . 4_746 ?
C4 C1 O3 Cd1 -177.49(3) . . . 4_746 ?
N1 Cd1 O3 C1 -102.63(4) 4_756 . . . ?
N3 Cd1 O3 C1 60.07(4) . . . . ?
O7 Cd1 O3 C1 150.43(4) . . . . ?
O4 Cd1 O3 C1 152.03(3) 4_756 . . . ?
O3 Cd1 O3 C1 -21.37(4) 4_756 . . . ?
N1 Cd1 O3 Cd1 155.278(12) 4_756 . . 4_746 ?
N3 Cd1 O3 Cd1 -42.024(15) . . . 4_746 ?
O7 Cd1 O3 Cd1 48.341(16) . . . 4_746 ?
O4 Cd1 O3 Cd1 49.94(3) 4_756 . . 4_746 ?
O3 Cd1 O3 Cd1 -123.459(17) 4_756 . . 4_746 ?
O3 C1 O4 Cd1 -1.97(3) . . . 4_746 ?
C4 C1 O4 Cd1 177.43(2) . . . 4_746 ?
O6 C5 O5 Cd2 -24.45(4) . . . . ?
C3 C5 O5 Cd2 153.97(2) . . . . ?
N2 Cd2 O5 C5 -156.323(19) 8_455 . . . ?
O2 Cd2 O5 C5 56.30(3) . . . . ?
O1 Cd2 O5 C5 -12.52(2) . . . . ?
O2 Cd2 O5 C5 117.45(2) 7_666 . . . ?
O1 Cd2 O5 C5 -78.89(2) 7_656 . . . ?
C12 Cd2 O5 C5 14.57(2) . . . . ?
Cd2 O1 C12 O2 -7.01(3) . . . . ?
Cd2 O1 C12 O2 -132.15(3) 7_656 . . . ?
Cd2 O1 C12 C13 173.01(2) . . . . ?
Cd2 O1 C12 C13 47.87(5) 7_656 . . . ?
Cd2 O1 C12 Cd2 -125.14(4) 7_656 . . . ?
Cd2 O2 C12 O1 7.05(3) . . . . ?
Cd2 O2 C12 O1 -140.16(4) 7_666 . . . ?
Cd2 O2 C12 C13 -172.97(2) . . . . ?
Cd2 O2 C12 C13 39.82(6) 7_666 . . . ?
Cd2 O2 C12 Cd2 -147.22(5) 7_666 . . . ?
C10 C13 C12 O1 -163.06(3) . . . . ?
C9 C13 C12 O1 16.96(4) . . . . ?
C10 C13 C12 O2 16.96(4) . . . . ?
C9 C13 C12 O2 -163.03(3) . . . . ?
C10 C13 C12 Cd2 -54.59(18) . . . . ?
C9 C13 C12 Cd2 125.43(16) . . . . ?
O5 Cd2 C12 O1 -60.82(2) . . . . ?
N2 Cd2 C12 O1 111.738(17) 8_455 . . . ?
O2 Cd2 C12 O1 -173.05(3) . . . . ?
O2 Cd2 C12 O1 -160.100(17) 7_666 . . . ?
O1 Cd2 C12 O1 25.07(2) 7_656 . . . ?
O5 Cd2 C12 O2 112.224(17) . . . . ?
N2 Cd2 C12 O2 -75.215(17) 8_455 . . . ?
O1 Cd2 C12 O2 173.05(3) . . . . ?
O2 Cd2 C12 O2 12.95(2) 7_666 . . . ?
O1 Cd2 C12 O2 -161.886(17) 7_656 . . . ?
O5 Cd2 C12 C13 -172.82(16) . . . . ?
N2 Cd2 C12 C13 -0.26(17) 8_455 . . . ?
O2 Cd2 C12 C13 74.95(17) . . . . ?
O1 Cd2 C12 C13 -112.00(17) . . . . ?
O2 Cd2 C12 C13 87.90(17) 7_666 . . . ?
O1 Cd2 C12 C13 -86.93(17) 7_656 . . . ?

_diffrn_measured_fraction_theta_max 0.943
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.943
_refine_diff_density_max         1.511
_refine_diff_density_min         -1.564
_refine_diff_density_rms         0.233


