# 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        'Jhy-Der Chen'
_publ_contact_author_email       JDCHEN@CYCU.EDU.TW

_publ_section_title              
;
Ligand isomerism-controlled structural diversity of
cadmium(II) perchlorate coordination polymers containing
dipyridyladipoamide ligands
;
loop_
_publ_author_name
'Jhy-Der Chen.'
'Yi-Fen Hsu.'
'Hui-Ling Hu.'
'Davide Proserpio'
'Chia-Jun Wu.'
;
Chun-Wei Yeh
;

# Attachment 'Cd26_36_46-cif.txt'

data_L2
_database_code_depnum_ccdc_archive 'CCDC 695629'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C16 H18 N4 O2'
_chemical_formula_weight         298.34

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'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   P2(1)/n

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

_cell_length_a                   9.4559(12)
_cell_length_b                   7.8465(10)
_cell_length_c                   10.6879(17)
_cell_angle_alpha                90.00
_cell_angle_beta                 108.137(11)
_cell_angle_gamma                90.00
_cell_volume                     753.60(18)
_cell_formula_units_Z            2
_cell_measurement_temperature    295(2)
_cell_measurement_reflns_used    27
_cell_measurement_theta_min      5.07
_cell_measurement_theta_max      12.47

_exptl_crystal_description       plate
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.6
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.1
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.315
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             316
_exptl_absorpt_coefficient_mu    0.090
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.9200
_exptl_absorpt_correction_T_max  0.9719
_exptl_absorpt_process_details   ?

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      295(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         3
_diffrn_standards_interval_count 97
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            1801
_diffrn_reflns_av_R_equivalents  0.0338
_diffrn_reflns_av_sigmaI/netI    0.0488
_diffrn_reflns_limit_h_min       -1
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -1
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_theta_min         2.52
_diffrn_reflns_theta_max         24.99
_reflns_number_total             1305
_reflns_number_gt                764
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker XSCANS'
_computing_cell_refinement       'Bruker XSCANS'
_computing_data_reduction        'Bruker SHELXTL'
_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 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)+(0.0549P)²+0.0939P] 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         1305
_refine_ls_number_parameters     136
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1010
_refine_ls_R_factor_gt           0.0500
_refine_ls_wR_factor_ref         0.1272
_refine_ls_wR_factor_gt          0.1048
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_restrained_S_all      1.032
_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
O O 0.6307(2) 0.1498(3) -0.16323(17) 0.0834(7) Uani 1 1 d . . .
N1 N 0.5891(2) 0.1936(3) 0.0327(2) 0.0563(6) Uani 1 1 d . . .
N2 N 0.2233(2) 0.3438(3) -0.17779(19) 0.0689(7) Uani 1 1 d . . .
C1 C 0.9236(3) 0.0287(5) -0.0433(3) 0.0650(8) Uani 1 1 d . . .
C2 C 0.8285(3) 0.0912(5) 0.0358(3) 0.0668(9) Uani 1 1 d . . .
C3 C 0.6737(3) 0.1464(4) -0.0434(2) 0.0577(7) Uani 1 1 d . . .
C4 C 0.4466(2) 0.2660(3) -0.0088(2) 0.0505(7) Uani 1 1 d . . .
C5 C 0.3885(3) 0.3330(4) 0.0838(3) 0.0667(8) Uani 1 1 d . . .
C6 C 0.2492(3) 0.4054(4) 0.0448(3) 0.0738(9) Uani 1 1 d . . .
C7 C 0.1709(3) 0.4094(4) -0.0859(3) 0.0668(8) Uani 1 1 d . . .
C8 C 0.3590(3) 0.2723(4) -0.1384(2) 0.0652(8) Uani 1 1 d . . .
H1N H 0.630(3) 0.189(3) 0.123(3) 0.066(8) Uiso 1 1 d . . .
H1A H 0.869(3) -0.066(4) -0.105(3) 0.082(9) Uiso 1 1 d . . .
H1B H 0.930(3) 0.133(4) -0.107(3) 0.098(10) Uiso 1 1 d . . .
H2A H 0.879(4) 0.188(4) 0.088(3) 0.105(12) Uiso 1 1 d . . .
H2B H 0.822(3) 0.011(4) 0.101(3) 0.083(10) Uiso 1 1 d . . .
H5 H 0.444(3) 0.327(3) 0.169(3) 0.071(8) Uiso 1 1 d . . .
H6 H 0.205(3) 0.451(4) 0.110(3) 0.082(9) Uiso 1 1 d . . .
H7 H 0.070(3) 0.460(3) -0.122(2) 0.063(7) Uiso 1 1 d . . .
H8 H 0.394(3) 0.226(3) -0.206(3) 0.081(9) 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
O C3 1.217(3) . ?
N1 C3 1.358(3) . ?
N1 C4 1.401(3) . ?
N2 C7 1.333(3) . ?
N2 C8 1.343(3) . ?
C1 C2 1.496(4) . ?
C1 C1 1.522(5) 3_755 ?
C2 C3 1.508(4) . ?
C4 C8 1.375(3) . ?
C4 C5 1.377(4) . ?
C5 C6 1.374(4) . ?
C6 C7 1.363(4) . ?

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
C3 N1 C4 127.5(2) . . ?
C7 N2 C8 117.9(2) . . ?
C2 C1 C1 112.2(3) . 3_755 ?
C1 C2 C3 115.2(2) . . ?
O C3 N1 123.9(2) . . ?
O C3 C2 123.0(2) . . ?
N1 C3 C2 113.1(2) . . ?
C8 C4 C5 117.4(2) . . ?
C8 C4 N1 123.5(2) . . ?
C5 C4 N1 119.1(2) . . ?
C6 C5 C4 119.9(2) . . ?
C7 C6 C5 119.0(3) . . ?
N2 C7 C6 122.5(3) . . ?
N2 C8 C4 123.2(3) . . ?

_diffrn_measured_fraction_theta_max 0.985
_diffrn_reflns_theta_full        24.99
_diffrn_measured_fraction_theta_full 0.985
_refine_diff_density_max         0.142
_refine_diff_density_min         -0.143
_refine_diff_density_rms         0.037

#===END

data_1
_database_code_depnum_ccdc_archive 'CCDC 695630'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C16 H18 Cd Cl2 N4 O10'
_chemical_formula_weight         609.64

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'
Cl Cl 0.1484 0.1585 '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   P2(1)/n

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

_cell_length_a                   9.1730(11)
_cell_length_b                   11.3098(13)
_cell_length_c                   11.0517(10)
_cell_angle_alpha                90.00
_cell_angle_beta                 107.793(8)
_cell_angle_gamma                90.00
_cell_volume                     1091.7(2)
_cell_formula_units_Z            2
_cell_measurement_temperature    295(2)
_cell_measurement_reflns_used    27
_cell_measurement_theta_min      4.85
_cell_measurement_theta_max      12.48

_exptl_crystal_description       plate
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.2
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.855
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             608
_exptl_absorpt_coefficient_mu    1.307
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.3425
_exptl_absorpt_correction_T_max  0.3683
_exptl_absorpt_process_details   ?

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      295(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         3
_diffrn_standards_interval_count 97
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            2543
_diffrn_reflns_av_R_equivalents  0.0271
_diffrn_reflns_av_sigmaI/netI    0.0392
_diffrn_reflns_limit_h_min       -1
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -1
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_theta_min         2.53
_diffrn_reflns_theta_max         24.99
_reflns_number_total             1917
_reflns_number_gt                1500
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker XSCANS'
_computing_cell_refinement       'Bruker XSCANS'
_computing_data_reduction        'Bruker SHELXTL'
_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 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)+(0.0344P)²+1.1440P] 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         1917
_refine_ls_number_parameters     187
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0511
_refine_ls_R_factor_gt           0.0329
_refine_ls_wR_factor_ref         0.0793
_refine_ls_wR_factor_gt          0.0713
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_restrained_S_all      1.031
_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
Cd Cd 0.0000 0.0000 0.5000 0.03539(15) Uani 1 2 d S . .
O1 O 0.0695(3) 0.0653(3) 0.6984(2) 0.0453(7) Uani 1 1 d . . .
N1 N 0.2440(4) -0.0684(3) 0.5604(3) 0.0333(7) Uani 1 1 d . . .
N2 N 0.2854(4) -0.0454(3) 0.7828(3) 0.0330(8) Uani 1 1 d . . .
C1 C 0.3355(4) -0.0788(3) 0.6799(3) 0.0304(8) Uani 1 1 d . . .
C2 C 0.4820(5) -0.1260(4) 0.7084(4) 0.0429(10) Uani 1 1 d . . .
C3 C 0.5361(5) -0.1594(4) 0.6121(5) 0.0492(12) Uani 1 1 d . . .
C4 C 0.4435(5) -0.1481(4) 0.4870(4) 0.0461(11) Uani 1 1 d . . .
C5 C 0.3011(5) -0.1030(4) 0.4671(4) 0.0430(11) Uani 1 1 d . . .
C6 C 0.1663(4) 0.0215(4) 0.7906(3) 0.0333(9) Uani 1 1 d . . .
C7 C 0.1559(5) 0.0409(5) 0.9223(4) 0.0386(10) Uani 1 1 d . . .
C8 C 0.0066(5) -0.0086(5) 0.9341(4) 0.0403(9) Uani 1 1 d . . .
Cl Cl 0.04009(12) 0.28397(10) 0.37950(9) 0.0408(3) Uani 1 1 d . . .
O2 O 0.1017(4) 0.1698(3) 0.4216(5) 0.0858(14) Uani 1 1 d . . .
O3 O 0.0054(4) 0.3444(4) 0.4796(3) 0.0759(12) Uani 1 1 d . . .
O4 O 0.1511(4) 0.3479(3) 0.3401(3) 0.0649(10) Uani 1 1 d . . .
O5 O -0.0965(4) 0.2715(4) 0.2762(3) 0.0707(11) Uani 1 1 d . . .
H2N H 0.335(5) -0.066(4) 0.856(4) 0.050(14) Uiso 1 1 d . . .
H2 H 0.536(5) -0.137(4) 0.793(4) 0.053(13) Uiso 1 1 d . . .
H3 H 0.630(5) -0.196(4) 0.629(4) 0.040(11) Uiso 1 1 d . . .
H4 H 0.483(5) -0.177(4) 0.419(4) 0.059(14) Uiso 1 1 d . . .
H5 H 0.240(5) -0.100(4) 0.387(4) 0.038(11) Uiso 1 1 d . . .
H7A H 0.164(5) 0.123(4) 0.934(4) 0.046(13) Uiso 1 1 d . . .
H7B H 0.239(6) 0.001(4) 0.983(5) 0.053(13) Uiso 1 1 d . . .
H8A H -0.077(6) 0.021(4) 0.872(5) 0.060(15) Uiso 1 1 d . . .
H8B H 0.002(6) -0.091(5) 0.911(4) 0.059(15) 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
Cd O1 2.215(3) 3_556 ?
Cd O1 2.215(3) . ?
Cd N1 2.267(3) . ?
Cd N1 2.267(3) 3_556 ?
Cd O2 2.409(4) . ?
Cd O2 2.409(4) 3_556 ?
O1 C6 1.233(4) . ?
N1 C1 1.336(5) . ?
N1 C5 1.350(5) . ?
N2 C6 1.353(5) . ?
N2 C1 1.403(5) . ?
C1 C2 1.390(5) . ?
C2 C3 1.359(6) . ?
C3 C4 1.390(6) . ?
C4 C5 1.356(6) . ?
C6 C7 1.503(5) . ?
C7 C8 1.522(6) . ?
C8 C8 1.511(8) 3_557 ?
Cl O3 1.417(3) . ?
Cl O5 1.421(3) . ?
Cl O4 1.421(3) . ?
Cl O2 1.430(4) . ?

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 Cd O1 180.0 3_556 . ?
O1 Cd N1 97.89(10) 3_556 . ?
O1 Cd N1 82.11(10) . . ?
O1 Cd N1 82.11(10) 3_556 3_556 ?
O1 Cd N1 97.89(10) . 3_556 ?
N1 Cd N1 180.0 . 3_556 ?
O1 Cd O2 86.30(15) 3_556 . ?
O1 Cd O2 93.70(15) . . ?
N1 Cd O2 85.53(12) . . ?
N1 Cd O2 94.47(12) 3_556 . ?
O1 Cd O2 93.70(15) 3_556 3_556 ?
O1 Cd O2 86.30(15) . 3_556 ?
N1 Cd O2 94.47(12) . 3_556 ?
N1 Cd O2 85.53(12) 3_556 3_556 ?
O2 Cd O2 180.00(11) . 3_556 ?
C6 O1 Cd 127.0(3) . . ?
C1 N1 C5 117.1(3) . . ?
C1 N1 Cd 125.9(2) . . ?
C5 N1 Cd 116.9(3) . . ?
C6 N2 C1 132.4(3) . . ?
N1 C1 C2 122.0(3) . . ?
N1 C1 N2 121.0(3) . . ?
C2 C1 N2 117.0(3) . . ?
C3 C2 C1 119.3(4) . . ?
C2 C3 C4 119.7(4) . . ?
C5 C4 C3 117.5(4) . . ?
N1 C5 C4 124.4(4) . . ?
O1 C6 N2 124.3(3) . . ?
O1 C6 C7 119.9(4) . . ?
N2 C6 C7 115.8(3) . . ?
C6 C7 C8 110.7(3) . . ?
C8 C8 C7 112.0(5) 3_557 . ?
O3 Cl O5 108.8(2) . . ?
O3 Cl O4 110.3(2) . . ?
O5 Cl O4 110.0(2) . . ?
O3 Cl O2 110.0(3) . . ?
O5 Cl O2 109.6(3) . . ?
O4 Cl O2 108.1(2) . . ?
Cl O2 Cd 132.8(2) . . ?

_diffrn_measured_fraction_theta_max 0.997
_diffrn_reflns_theta_full        24.99
_diffrn_measured_fraction_theta_full 0.997
_refine_diff_density_max         0.509
_refine_diff_density_min         -0.503
_refine_diff_density_rms         0.080

#===END

data_2
_database_code_depnum_ccdc_archive 'CCDC 695631'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C36 H52 Cd Cl2 N8 O16'
_chemical_formula_weight         1036.16

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'
Cl Cl 0.1484 0.1585 '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           Triclinic
_symmetry_space_group_name_H-M   P-1

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

_cell_length_a                   9.6762(11)
_cell_length_b                   9.9743(11)
_cell_length_c                   12.4337(14)
_cell_angle_alpha                76.553(9)
_cell_angle_beta                 78.663(9)
_cell_angle_gamma                79.367(9)
_cell_volume                     1132.2(2)
_cell_formula_units_Z            1
_cell_measurement_temperature    295(2)
_cell_measurement_reflns_used    26
_cell_measurement_theta_min      5.12
_cell_measurement_theta_max      12.47

_exptl_crystal_description       plate
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.2
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.520
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             534
_exptl_absorpt_coefficient_mu    0.677
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.8203
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_process_details   ?

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      295(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         3
_diffrn_standards_interval_count 97
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            4673
_diffrn_reflns_av_R_equivalents  0.0346
_diffrn_reflns_av_sigmaI/netI    0.0550
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       1
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         2.12
_diffrn_reflns_theta_max         24.99
_reflns_number_total             3919
_reflns_number_gt                3162
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker XSCANS'
_computing_cell_refinement       'Bruker XSCANS'
_computing_data_reduction        'Bruker SHELXTL'
_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 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)+(0.0842P)²+1.8685P] 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         3919
_refine_ls_number_parameters     305
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0808
_refine_ls_R_factor_gt           0.0617
_refine_ls_wR_factor_ref         0.1605
_refine_ls_wR_factor_gt          0.1467
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_restrained_S_all      1.026
_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
Cd Cd -0.5000 0.5000 0.5000 0.0455(2) Uani 1 2 d S . .
O1 O -0.7042(5) 0.6278(6) -0.0706(4) 0.0770(14) Uani 1 1 d . . .
O2 O -0.9069(5) 1.0818(5) 0.7206(4) 0.0701(12) Uani 1 1 d . . .
N1 N -0.5348(5) 0.5847(5) 0.3106(4) 0.0473(11) Uani 1 1 d . . .
N2 N -0.6842(5) 0.4883(5) 0.0969(4) 0.0499(11) Uani 1 1 d . . .
H2A H -0.6992 0.4078 0.1367 0.060 Uiso 1 1 calc R . .
N3 N -0.6967(5) 0.6607(5) 0.5550(4) 0.0484(11) Uani 1 1 d . . .
N4 N -0.8159(5) 0.8591(5) 0.7770(4) 0.0552(12) Uani 1 1 d . . .
H4A H -0.7865 0.7987 0.8325 0.066 Uiso 1 1 calc R . .
C1 C -0.5964(6) 0.5184(6) 0.2561(4) 0.0435(12) Uani 1 1 d . . .
H1A H -0.6261 0.4339 0.2937 0.052 Uiso 1 1 calc R . .
C2 C -0.6190(5) 0.5684(6) 0.1462(4) 0.0439(12) Uani 1 1 d . . .
C3 C -0.5742(6) 0.6947(6) 0.0906(5) 0.0508(14) Uani 1 1 d . . .
H3A H -0.5853 0.7315 0.0164 0.061 Uiso 1 1 calc R . .
C4 C -0.5132(7) 0.7636(7) 0.1487(5) 0.0590(15) Uani 1 1 d . . .
H4B H -0.4842 0.8494 0.1140 0.071 Uiso 1 1 calc R . .
C5 C -0.4947(7) 0.7065(6) 0.2577(5) 0.0566(15) Uani 1 1 d . . .
H5A H -0.4528 0.7546 0.2954 0.068 Uiso 1 1 calc R . .
C6 C -0.7265(6) 0.5204(7) -0.0042(5) 0.0523(14) Uani 1 1 d . . .
C7 C -0.8018(7) 0.4160(7) -0.0300(6) 0.0637(17) Uani 1 1 d . . .
H7A H -0.7600 0.3230 0.0028 0.076 Uiso 1 1 calc R . .
H7B H -0.7872 0.4237 -0.1106 0.076 Uiso 1 1 calc R . .
C8 C -0.9590(8) 0.4349(9) 0.0131(11) 0.111(4) Uani 1 1 d . . .
H8A H -1.0000 0.3690 -0.0131 0.167 Uiso 1 1 calc R . .
H8B H -0.9710 0.4076 0.0942 0.167 Uiso 1 1 calc R . .
C9 C -0.7072(6) 0.7122(6) 0.6478(4) 0.0491(13) Uani 1 1 d . . .
H9A H -0.6360 0.6811 0.6921 0.059 Uiso 1 1 calc R . .
C10 C -0.8207(6) 0.8104(6) 0.6796(4) 0.0453(13) Uani 1 1 d . . .
C11 C -0.9275(6) 0.8548(6) 0.6162(5) 0.0545(15) Uani 1 1 d . . .
H11A H -1.0058 0.9183 0.6373 0.065 Uiso 1 1 calc R . .
C12 C -0.9167(7) 0.8038(7) 0.5207(6) 0.0606(16) Uani 1 1 d . . .
H12A H -0.9872 0.8330 0.4757 0.073 Uiso 1 1 calc R . .
C13 C -0.7990(7) 0.7079(6) 0.4922(5) 0.0572(15) Uani 1 1 d . . .
H13A H -0.7915 0.6755 0.4267 0.069 Uiso 1 1 calc R . .
C14 C -0.8534(6) 0.9915(7) 0.7900(5) 0.0550(15) Uani 1 1 d . . .
C15 C -0.8204(7) 1.0210(8) 0.8956(5) 0.0678(18) Uani 1 1 d . . .
C16 C -0.9260(19) 0.967(3) 1.0049(15) 0.061(4) Uani 0.42 1 d P . .
C16' C -0.9583(19) 1.0626(16) 0.9753(10) 0.061(3) Uani 0.58 1 d P . .
C17 C -0.6269(9) 0.1936(9) 0.5082(7) 0.087(2) Uani 1 1 d . . .
H17A H -0.7157 0.1586 0.5197 0.130 Uiso 1 1 calc R . .
H17B H -0.5710 0.1406 0.5638 0.130 Uiso 1 1 calc R . .
H17C H -0.5758 0.1857 0.4350 0.130 Uiso 1 1 calc R . .
O3 O -0.6541(5) 0.3387(4) 0.5173(4) 0.0617(11) Uani 1 1 d . . .
H3C H -0.7502 0.3738 0.5329 0.074 Uiso 1 1 calc R . .
Cl Cl 0.3397(2) 0.10517(19) 0.22526(15) 0.0736(5) Uani 1 1 d . . .
O4 O 0.2535(7) 0.2310(6) 0.2493(5) 0.1019(19) Uani 1 1 d . . .
O5 O 0.2999(11) -0.0024(7) 0.3083(8) 0.175(4) Uani 1 1 d . . .
O6 O 0.3333(14) 0.0896(9) 0.1187(7) 0.192(5) Uani 1 1 d . . .
O7 O 0.4781(9) 0.1170(15) 0.2232(10) 0.207(5) Uani 1 1 d . . .
C18 C 0.0024(9) 0.5547(10) 0.3123(9) 0.101(3) Uani 1 1 d . . .
O8 O -0.1271(11) 0.6476(11) 0.3129(9) 0.073(3) Uani 0.60 1 d P . .
O8' O -0.0841(18) 0.6488(18) 0.3650(15) 0.078(4) Uani 0.40 1 d P . .


_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
Cd O3 2.336(4) 2_466 ?
Cd O3 2.336(4) . ?
Cd N3 2.352(4) . ?
Cd N3 2.352(4) 2_466 ?
Cd N1 2.377(4) . ?
Cd N1 2.377(4) 2_466 ?
O1 C6 1.216(8) . ?
O2 C14 1.211(7) . ?
N1 C5 1.328(8) . ?
N1 C1 1.328(7) . ?
N2 C6 1.348(7) . ?
N2 C2 1.406(7) . ?
N2 H2A 0.8600 . ?
N3 C13 1.331(7) . ?
N3 C9 1.348(7) . ?
N4 C14 1.342(8) . ?
N4 C10 1.417(7) . ?
N4 H4A 0.8600 . ?
C1 C2 1.387(7) . ?
C1 H1A 0.9300 . ?
C2 C3 1.390(8) . ?
C3 C4 1.375(9) . ?
C3 H3A 0.9300 . ?
C4 C5 1.375(9) . ?
C4 H4B 0.9300 . ?
C5 H5A 0.9300 . ?
C6 C7 1.498(9) . ?
C7 C8 1.503(11) . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C8 C8 1.396(17) 2_365 ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C9 C10 1.391(8) . ?
C9 H9A 0.9300 . ?
C10 C11 1.369(8) . ?
C11 C12 1.376(9) . ?
C11 H11A 0.9300 . ?
C12 C13 1.390(8) . ?
C12 H12A 0.9300 . ?
C13 H13A 0.9300 . ?
C14 C15 1.514(9) . ?
C15 C16' 1.549(16) . ?
C15 C16 1.58(2) . ?
C16 C16' 0.96(2) . ?
C16 C16' 1.175(17) 2_377 ?
C16 C16 1.48(4) 2_377 ?
C16' C16 1.175(17) 2_377 ?
C16' C16' 1.55(3) 2_377 ?
C17 O3 1.449(9) . ?
C17 H17A 0.9600 . ?
C17 H17B 0.9600 . ?
C17 H17C 0.9600 . ?
O3 H3C 0.9300 . ?
Cl O5 1.359(7) . ?
Cl O7 1.360(8) . ?
Cl O6 1.383(7) . ?
Cl O4 1.432(6) . ?
C18 O8' 1.338(18) . ?
C18 O8 1.414(14) . ?
O8 O8' 0.839(15) . ?

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 Cd O3 180.0 2_466 . ?
O3 Cd N3 90.78(16) 2_466 . ?
O3 Cd N3 89.22(16) . . ?
O3 Cd N3 89.22(16) 2_466 2_466 ?
O3 Cd N3 90.78(16) . 2_466 ?
N3 Cd N3 180.000(1) . 2_466 ?
O3 Cd N1 91.06(16) 2_466 . ?
O3 Cd N1 88.94(16) . . ?
N3 Cd N1 89.18(15) . . ?
N3 Cd N1 90.82(15) 2_466 . ?
O3 Cd N1 88.94(16) 2_466 2_466 ?
O3 Cd N1 91.06(16) . 2_466 ?
N3 Cd N1 90.82(15) . 2_466 ?
N3 Cd N1 89.18(15) 2_466 2_466 ?
N1 Cd N1 180.000(1) . 2_466 ?
C5 N1 C1 118.2(5) . . ?
C5 N1 Cd 118.4(4) . . ?
C1 N1 Cd 123.4(4) . . ?
C6 N2 C2 128.8(5) . . ?
C6 N2 H2A 115.6 . . ?
C2 N2 H2A 115.6 . . ?
C13 N3 C9 117.8(5) . . ?
C13 N3 Cd 120.5(4) . . ?
C9 N3 Cd 121.6(4) . . ?
C14 N4 C10 125.5(5) . . ?
C14 N4 H4A 117.3 . . ?
C10 N4 H4A 117.3 . . ?
N1 C1 C2 123.6(5) . . ?
N1 C1 H1A 118.2 . . ?
C2 C1 H1A 118.2 . . ?
C1 C2 C3 117.8(5) . . ?
C1 C2 N2 118.5(5) . . ?
C3 C2 N2 123.7(5) . . ?
C4 C3 C2 118.0(5) . . ?
C4 C3 H3A 121.0 . . ?
C2 C3 H3A 121.0 . . ?
C5 C4 C3 120.4(6) . . ?
C5 C4 H4B 119.8 . . ?
C3 C4 H4B 119.8 . . ?
N1 C5 C4 121.9(6) . . ?
N1 C5 H5A 119.0 . . ?
C4 C5 H5A 119.0 . . ?
O1 C6 N2 121.7(6) . . ?
O1 C6 C7 122.1(5) . . ?
N2 C6 C7 116.1(6) . . ?
C6 C7 C8 113.0(5) . . ?
C6 C7 H7A 109.0 . . ?
C8 C7 H7A 109.0 . . ?
C6 C7 H7B 109.0 . . ?
C8 C7 H7B 109.0 . . ?
H7A C7 H7B 107.8 . . ?
C8 C8 C7 119.9(12) 2_365 . ?
C8 C8 H8A 107.3 2_365 . ?
C7 C8 H8A 107.3 . . ?
C8 C8 H8B 107.3 2_365 . ?
C7 C8 H8B 107.3 . . ?
H8A C8 H8B 106.9 . . ?
N3 C9 C10 122.3(5) . . ?
N3 C9 H9A 118.8 . . ?
C10 C9 H9A 118.8 . . ?
C11 C10 C9 119.3(5) . . ?
C11 C10 N4 124.3(5) . . ?
C9 C10 N4 116.4(5) . . ?
C10 C11 C12 118.7(5) . . ?
C10 C11 H11A 120.7 . . ?
C12 C11 H11A 120.7 . . ?
C11 C12 C13 119.2(5) . . ?
C11 C12 H12A 120.4 . . ?
C13 C12 H12A 120.4 . . ?
N3 C13 C12 122.7(5) . . ?
N3 C13 H13A 118.7 . . ?
C12 C13 H13A 118.7 . . ?
O2 C14 N4 122.1(6) . . ?
O2 C14 C15 122.3(6) . . ?
N4 C14 C15 115.5(6) . . ?
C14 C15 C16' 111.5(7) . . ?
C14 C15 C16 113.6(8) . . ?
C16' C15 C16 35.6(7) . . ?
C16' C16 C16' 93(2) . 2_377 ?
C16' C16 C16 52.5(17) . 2_377 ?
C16' C16 C16 40.3(11) 2_377 2_377 ?
C16' C16 C15 70(2) . . ?
C16' C16 C15 135.9(15) 2_377 . ?
C16 C16 C15 111(2) 2_377 . ?
C16 C16' C16 87(2) . 2_377 ?
C16 C16' C15 74.0(18) . . ?
C16 C16' C15 134.6(13) 2_377 . ?
C16 C16' C16' 49.1(14) . 2_377 ?
C16 C16' C16' 38.1(13) 2_377 2_377 ?
C15 C16' C16' 111.2(14) . 2_377 ?
O3 C17 H17A 109.5 . . ?
O3 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
O3 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C17 O3 Cd 131.5(4) . . ?
C17 O3 H3C 114.2 . . ?
Cd O3 H3C 114.2 . . ?
O5 Cl O7 110.0(8) . . ?
O5 Cl O6 114.3(7) . . ?
O7 Cl O6 105.1(7) . . ?
O5 Cl O4 108.1(4) . . ?
O7 Cl O4 108.0(6) . . ?
O6 Cl O4 111.1(4) . . ?
O8' C18 O8 35.4(7) . . ?
O8' O8 C18 67.4(16) . . ?
O8 O8' C18 77.3(16) . . ?

_diffrn_measured_fraction_theta_max 0.984
_diffrn_reflns_theta_full        24.99
_diffrn_measured_fraction_theta_full 0.984
_refine_diff_density_max         0.852
_refine_diff_density_min         -1.061
_refine_diff_density_rms         0.095

#===END

data_3
_database_code_depnum_ccdc_archive 'CCDC 695632'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C36 H48 Cd Cl2 N8 O14'
_chemical_formula_weight         1000.12

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'
Cl Cl 0.1484 0.1585 '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   Pcca

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

_cell_length_a                   16.779(2)
_cell_length_b                   12.1263(13)
_cell_length_c                   21.766(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     4428.6(9)
_cell_formula_units_Z            4
_cell_measurement_temperature    295(2)
_cell_measurement_reflns_used    28
_cell_measurement_theta_min      5.10
_cell_measurement_theta_max      12.53

_exptl_crystal_description       plate
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.6
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.2
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.500
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2056
_exptl_absorpt_coefficient_mu    0.686
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.9107
_exptl_absorpt_correction_T_max  0.9836
_exptl_absorpt_process_details   ?

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      295(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         3
_diffrn_standards_interval_count 97
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            4495
_diffrn_reflns_av_R_equivalents  0.0262
_diffrn_reflns_av_sigmaI/netI    0.0315
_diffrn_reflns_limit_h_min       -1
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_k_min       -1
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_limit_l_max       1
_diffrn_reflns_theta_min         2.23
_diffrn_reflns_theta_max         25.01
_reflns_number_total             3864
_reflns_number_gt                2735
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker XSCANS'
_computing_cell_refinement       'Bruker XSCANS'
_computing_data_reduction        'Bruker SHELXTL'
_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 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)+(0.0826P)²+7.9674P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     SHELXL
_refine_ls_extinction_coef       0.0009(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         3864
_refine_ls_number_parameters     300
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0763
_refine_ls_R_factor_gt           0.0523
_refine_ls_wR_factor_ref         0.1554
_refine_ls_wR_factor_gt          0.1381
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_restrained_S_all      1.035
_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
Cd Cd 0.2500 0.5000 0.34279(2) 0.03853(14) Uani 1 2 d S . .
O1 O -0.1566(2) 0.7274(3) 0.3096(2) 0.0855(14) Uani 1 1 d . . .
O2 O 0.0211(3) 0.0792(3) 0.16110(17) 0.0729(11) Uani 1 1 d . . .
N1 N 0.1428(2) 0.6229(3) 0.34306(18) 0.0445(9) Uani 1 1 d . . .
N2 N -0.0496(2) 0.8409(3) 0.3247(2) 0.0553(11) Uani 1 1 d . . .
H2A H -0.0367 0.9093 0.3275 0.066 Uiso 1 1 calc R . .
N3 N 0.1754(2) 0.4010(3) 0.26900(18) 0.0453(9) Uani 1 1 d . . .
N4 N 0.0460(3) 0.2504(3) 0.1265(2) 0.0624(12) Uani 1 1 d . . .
H4A H 0.0370 0.2943 0.0963 0.075 Uiso 1 1 calc R . .
C1 C 0.1503(3) 0.7325(4) 0.3469(3) 0.0555(13) Uani 1 1 d . . .
H1A H 0.2010 0.7611 0.3534 0.067 Uiso 1 1 calc R . .
C2 C 0.0887(3) 0.8049(4) 0.3420(2) 0.0530(13) Uani 1 1 d . . .
H2B H 0.0979 0.8802 0.3456 0.064 Uiso 1 1 calc R . .
C3 C 0.0121(3) 0.7659(3) 0.3316(2) 0.0448(11) Uani 1 1 d . . .
C4 C 0.0033(3) 0.6526(3) 0.3279(2) 0.0492(12) Uani 1 1 d . . .
H4B H -0.0468 0.6217 0.3216 0.059 Uiso 1 1 calc R . .
C5 C 0.0687(3) 0.5865(4) 0.3335(2) 0.0465(11) Uani 1 1 d . . .
H5A H 0.0612 0.5107 0.3305 0.056 Uiso 1 1 calc R . .
C6 C -0.1292(3) 0.8196(4) 0.3140(3) 0.0699(16) Uani 1 1 d . . .
C7 C -0.1790(4) 0.9248(5) 0.3045(4) 0.097(2) Uani 1 1 d . . .
H7A H -0.1439 0.9876 0.2991 0.117 Uiso 1 1 calc R . .
H7B H -0.2114 0.9174 0.2678 0.117 Uiso 1 1 calc R . .
C8 C -0.2293(6) 0.9424(7) 0.3568(5) 0.130(3) Uani 1 1 d . . .
H8A H -0.1976 0.9353 0.3939 0.157 Uiso 1 1 calc R . .
H8B H -0.2699 0.8855 0.3577 0.196 Uiso 1 1 calc R . .
C9 C 0.1473(3) 0.2979(3) 0.2754(2) 0.0478(11) Uani 1 1 d . . .
H9A H 0.1584 0.2609 0.3119 0.057 Uiso 1 1 calc R . .
C10 C 0.1034(3) 0.2436(4) 0.2318(2) 0.0528(12) Uani 1 1 d . . .
H10A H 0.0844 0.1728 0.2392 0.063 Uiso 1 1 calc R . .
C11 C 0.0878(3) 0.2958(4) 0.1763(2) 0.0501(12) Uani 1 1 d . . .
C12 C 0.1158(3) 0.4035(4) 0.1691(2) 0.0552(13) Uani 1 1 d . . .
H12A H 0.1057 0.4423 0.1331 0.066 Uiso 1 1 calc R . .
C13 C 0.1580(3) 0.4508(4) 0.2155(2) 0.0524(12) Uani 1 1 d . . .
H13A H 0.1760 0.5226 0.2098 0.063 Uiso 1 1 calc R . .
C14 C 0.0180(3) 0.1453(4) 0.1200(3) 0.0573(13) Uani 1 1 d . . .
C15 C -0.0162(4) 0.1200(5) 0.0573(3) 0.0749(17) Uani 1 1 d . . .
H15A H -0.0033 0.1798 0.0294 0.090 Uiso 1 1 calc R . .
H15B H -0.0737 0.1151 0.0603 0.090 Uiso 1 1 calc R . .
C16 C 0.0164(3) 0.0126(4) 0.0316(2) 0.0602(13) Uani 1 1 d . . .
H16A H 0.0740 0.0171 0.0294 0.072 Uiso 1 1 calc R . .
H16B H 0.0028 -0.0472 0.0592 0.072 Uiso 1 1 calc R . .
O7 O 0.1881(3) 0.3969(3) 0.4221(2) 0.0835(13) Uani 1 1 d . . .
C17 C 0.2375(12) 0.326(2) 0.4773(7) 0.264(10) Uani 1 1 d . . .
C18 C 0.201(2) 0.292(3) 0.5257(13) 0.203(13) Uani 0.50 1 d P . .
C18' C 0.250(2) 0.321(5) 0.5430(18) 0.30(3) Uani 0.50 1 d P . .
Cl1 Cl 0.2500 0.0000 0.40928(15) 0.0981(9) Uani 1 2 d S . .
O3 O 0.2056(4) 0.0743(5) 0.3723(4) 0.149(3) Uani 1 1 d . . .
O4 O 0.1961(3) -0.0613(4) 0.4464(3) 0.129(2) Uani 1 1 d . . .
Cl2 Cl 0.0064(4) 0.5164(10) 0.0067(3) 0.103(2) Uani 0.50 1 d P . .
O5 O -0.0250(5) 0.4481(9) 0.0484(4) 0.193(4) Uani 1 1 d . . .
O6 O 0.0616(10) 0.5723(18) 0.0409(6) 0.196(8) Uani 0.50 1 d P . .
O6' O 0.0612(9) 0.4209(16) -0.0074(8) 0.197(7) Uani 0.50 1 d P . .


_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
Cd N1 2.336(3) 2_565 ?
Cd N1 2.336(3) . ?
Cd N3 2.364(4) . ?
Cd N3 2.364(4) 2_565 ?
Cd O7 2.372(4) 2_565 ?
Cd O7 2.372(4) . ?
O1 C6 1.213(6) . ?
O2 C14 1.202(6) . ?
N1 C5 1.335(6) . ?
N1 C1 1.338(6) . ?
N2 C6 1.380(6) . ?
N2 C3 1.386(5) . ?
N3 C9 1.343(5) . ?
N3 C13 1.345(6) . ?
N4 C14 1.366(6) . ?
N4 C11 1.403(6) . ?
C1 C2 1.359(6) . ?
C2 C3 1.387(6) . ?
C3 C4 1.385(6) . ?
C4 C5 1.364(6) . ?
C6 C7 1.539(7) . ?
C7 C8 1.433(12) . ?
C8 C8 1.559(15) 2_475 ?
C9 C10 1.370(6) . ?
C10 C11 1.388(7) . ?
C11 C12 1.397(7) . ?
C12 C13 1.359(7) . ?
C14 C15 1.511(7) . ?
C15 C16 1.519(7) . ?
C16 C16 1.512(10) 5 ?
O7 C17 1.69(2) . ?
C17 C18 1.29(3) . ?
C17 C18' 1.45(4) . ?
C18 C18' 0.97(4) . ?
Cl1 O3 1.420(6) . ?
Cl1 O3 1.420(6) 2 ?
Cl1 O4 1.422(6) 2 ?
Cl1 O4 1.422(6) . ?
Cl2 Cl2 0.537(18) 5_565 ?
Cl2 O5 1.311(12) 5_565 ?
Cl2 O5 1.337(13) . ?
Cl2 O6' 1.366(16) 5_565 ?
Cl2 O6 1.368(17) . ?
Cl2 O6' 1.510(18) . ?
Cl2 O6 1.879(17) 5_565 ?
O5 Cl2 1.311(12) 5_565 ?
O6 Cl2 1.879(17) 5_565 ?
O6' Cl2 1.366(16) 5_565 ?

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
N1 Cd N1 179.71(19) 2_565 . ?
N1 Cd N3 94.90(12) 2_565 . ?
N1 Cd N3 85.29(12) . . ?
N1 Cd N3 85.29(12) 2_565 2_565 ?
N1 Cd N3 94.90(12) . 2_565 ?
N3 Cd N3 94.41(18) . 2_565 ?
N1 Cd O7 89.85(14) 2_565 2_565 ?
N1 Cd O7 89.94(14) . 2_565 ?
N3 Cd O7 173.94(15) . 2_565 ?
N3 Cd O7 89.72(15) 2_565 2_565 ?
N1 Cd O7 89.94(14) 2_565 . ?
N1 Cd O7 89.85(14) . . ?
N3 Cd O7 89.72(15) . . ?
N3 Cd O7 173.94(15) 2_565 . ?
O7 Cd O7 86.5(2) 2_565 . ?
C5 N1 C1 115.2(4) . . ?
C5 N1 Cd 120.3(3) . . ?
C1 N1 Cd 124.2(3) . . ?
C6 N2 C3 128.3(4) . . ?
C9 N3 C13 115.6(4) . . ?
C9 N3 Cd 126.0(3) . . ?
C13 N3 Cd 118.4(3) . . ?
C14 N4 C11 128.3(4) . . ?
N1 C1 C2 124.4(4) . . ?
C1 C2 C3 119.8(4) . . ?
C4 C3 N2 124.4(4) . . ?
C4 C3 C2 116.5(4) . . ?
N2 C3 C2 119.1(4) . . ?
C5 C4 C3 119.5(4) . . ?
N1 C5 C4 124.6(4) . . ?
O1 C6 N2 123.5(4) . . ?
O1 C6 C7 123.2(5) . . ?
N2 C6 C7 113.2(5) . . ?
C8 C7 C6 109.7(7) . . ?
C7 C8 C8 113.3(6) . 2_475 ?
N3 C9 C10 124.3(4) . . ?
C9 C10 C11 119.0(4) . . ?
C10 C11 C12 117.5(4) . . ?
C10 C11 N4 125.9(4) . . ?
C12 C11 N4 116.6(4) . . ?
C13 C12 C11 119.1(5) . . ?
N3 C13 C12 124.5(4) . . ?
O2 C14 N4 121.9(5) . . ?
O2 C14 C15 123.6(5) . . ?
N4 C14 C15 114.5(5) . . ?
C14 C15 C16 111.8(5) . . ?
C16 C16 C15 112.2(6) 5 . ?
C17 O7 Cd 124.7(7) . . ?
C18 C17 C18' 41.0(18) . . ?
C18 C17 O7 121(2) . . ?
C18' C17 O7 143(3) . . ?
C18' C18 C17 78(4) . . ?
C18 C18' C17 61(3) . . ?
O3 Cl1 O3 110.9(7) . 2 ?
O3 Cl1 O4 108.9(4) . 2 ?
O3 Cl1 O4 108.6(4) 2 2 ?
O3 Cl1 O4 108.6(4) . . ?
O3 Cl1 O4 108.9(4) 2 . ?
O4 Cl1 O4 110.8(6) 2 . ?
Cl2 Cl2 O5 80.9(17) 5_565 5_565 ?
Cl2 Cl2 O5 76(2) 5_565 . ?
O5 Cl2 O5 156.6(8) 5_565 . ?
Cl2 Cl2 O6' 95(2) 5_565 5_565 ?
O5 Cl2 O6' 91.5(10) 5_565 5_565 ?
O5 Cl2 O6' 90.5(9) . 5_565 ?
Cl2 Cl2 O6 159(3) 5_565 . ?
O5 Cl2 O6 100.0(9) 5_565 . ?
O5 Cl2 O6 101.8(9) . . ?
O6' Cl2 O6 106.2(14) 5_565 . ?
Cl2 Cl2 O6' 64(2) 5_565 . ?
O5 Cl2 O6' 85.5(9) 5_565 . ?
O5 Cl2 O6' 84.4(10) . . ?
O6' Cl2 O6' 159.2(7) 5_565 . ?
O6 Cl2 O6' 94.5(12) . . ?
Cl2 Cl2 O6 15.3(19) 5_565 5_565 ?
O5 Cl2 O6 80.1(7) 5_565 5_565 ?
O5 Cl2 O6 77.3(7) . 5_565 ?
O6' Cl2 O6 79.7(10) 5_565 5_565 ?
O6 Cl2 O6 174.1(8) . 5_565 ?
O6' Cl2 O6 79.6(10) . 5_565 ?
Cl2 O5 Cl2 23.4(8) 5_565 . ?
Cl2 O6 Cl2 5.9(8) . 5_565 ?
Cl2 O6' Cl2 20.8(7) 5_565 . ?

_diffrn_measured_fraction_theta_max 0.986
_diffrn_reflns_theta_full        25.01
_diffrn_measured_fraction_theta_full 0.986
_refine_diff_density_max         0.874
_refine_diff_density_min         -0.883
_refine_diff_density_rms         0.092

#===END


