# 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
_journal_volume                  ?
_journal_page_first              ?
_journal_year                    ?

_publ_contact_author_name        'Wei-Yin Sun'
_publ_contact_author_email       SUNWY@NJU.EDU.CN

_publ_section_title              
;
Structure diversity and reversible anion exchange
properties of cadmium(II) complexes with flexible tripodal ligand
1,3,5-tris(imidazol-1-ylmethyl)benzene
;
loop_
_publ_author_name
'Wei-Yin Sun.'
'Yu-Jie Ding.'
'Yong-Qing Huang.'
'Guang-Xiang Liu.'
;
T.Okamura
;
'Norikazu Ueyama'
'Guan-Cheng Xu.'

# Attachment 'B803236J-cif.cif'

data_l
_database_code_depnum_ccdc_archive 'CCDC 679257'
_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C36 H36 Cd N12, 2(B F4)'
_chemical_formula_sum            'C36 H36 B2 Cd F8 N12'
_chemical_formula_weight         922.79

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'
B B 0.0013 0.0007 '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'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Rhombohedral
_symmetry_space_group_name_H-M   'R -3'
_symmetry_space_group_name_Hall  '-R 3'

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

_cell_length_a                   9.8988(5)
_cell_length_b                   9.8988(5)
_cell_length_c                   36.629(4)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_volume                     3108.3(4)
_cell_formula_units_Z            3
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    1772
_cell_measurement_theta_min      2.44
_cell_measurement_theta_max      20.55

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.19
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.479
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1398
_exptl_absorpt_coefficient_mu    0.606
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.8682
_exptl_absorpt_correction_T_max  0.8936
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            5589
_diffrn_reflns_av_R_equivalents  0.0291
_diffrn_reflns_av_sigmaI/netI    0.0320
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_limit_l_max       45
_diffrn_reflns_theta_min         2.44
_diffrn_reflns_theta_max         25.98
_reflns_number_total             1363
_reflns_number_gt                1221
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'Bruker SHELXTL'
_computing_structure_refinement  'Bruker SHELXTL'
_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)+(0.0621P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         1363
_refine_ls_number_parameters     90
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0488
_refine_ls_R_factor_gt           0.0441
_refine_ls_wR_factor_ref         0.1039
_refine_ls_wR_factor_gt          0.1013
_refine_ls_goodness_of_fit_ref   1.000
_refine_ls_restrained_S_all      1.000
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 1.0011(4) 0.2146(4) 0.06952(9) 0.0681(8) Uani 1 1 d . . .
H1 H 1.0431 0.1688 0.0844 0.082 Uiso 1 1 calc R . .
C2 C 0.9054(5) 0.2695(5) 0.02427(11) 0.0861(10) Uani 1 1 d . . .
H2 H 0.8663 0.2683 0.0011 0.103 Uiso 1 1 calc R . .
C3 C 0.9155(4) 0.3636(4) 0.05126(12) 0.0882(12) Uani 1 1 d . . .
H3 H 0.8868 0.4398 0.0503 0.106 Uiso 1 1 calc R . .
C4 C 1.0181(4) 0.4059(4) 0.11639(9) 0.0759(10) Uani 1 1 d . . .
H4A H 1.0088 0.3319 0.1350 0.091 Uiso 1 1 calc R . .
H4B H 0.9463 0.4423 0.1225 0.091 Uiso 1 1 calc R . .
C5 C 1.1819(3) 0.5417(3) 0.11618(8) 0.0595(8) Uani 1 1 d . . .
C6 C 1.2090(4) 0.6920(4) 0.11617(8) 0.0626(8) Uani 1 1 d . . .
H6 H 1.1250 0.7095 0.1162 0.075 Uiso 1 1 calc R . .
N1 N 0.9611(3) 0.1741(3) 0.03564(7) 0.0648(7) Uani 1 1 d . . .
N2 N 0.9758(3) 0.3274(3) 0.08059(8) 0.0652(7) Uani 1 1 d . . .
Cd1 Cd 1.0000 0.0000 0.0000 0.0574(2) Uani 1 6 d S . .
B1 B 0.0000 0.0000 0.15817(18) 0.0633(15) Uani 1 3 d S . .
F1 F 0.1321(2) 0.1286(2) 0.14488(6) 0.0958(7) Uani 1 1 d . . .
F2 F 0.0000 0.0000 0.19574(9) 0.0838(9) Uani 1 3 d S . .


_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 N1 1.303(4) . ?
C1 N2 1.325(4) . ?
C1 H1 0.9300 . ?
C2 C3 1.327(5) . ?
C2 N1 1.375(4) . ?
C2 H2 0.9300 . ?
C3 N2 1.361(5) . ?
C3 H3 0.9300 . ?
C4 N2 1.474(4) . ?
C4 C5 1.502(4) . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
C5 C6 1.374(4) . ?
C5 C6 1.387(4) 2_755 ?
C6 C5 1.387(4) 3_775 ?
C6 H6 0.9300 . ?
N1 Cd1 2.343(3) . ?
Cd1 N1 2.343(3) 3_765 ?
Cd1 N1 2.343(3) 12_545 ?
Cd1 N1 2.343(3) 10_755 ?
Cd1 N1 2.343(3) 2_645 ?
Cd1 N1 2.343(3) 11_665 ?
B1 F2 1.376(7) . ?
B1 F1 1.379(3) 3 ?
B1 F1 1.379(3) . ?
B1 F1 1.379(3) 2 ?

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 C1 N2 113.2(3) . . ?
N1 C1 H1 123.4 . . ?
N2 C1 H1 123.4 . . ?
C3 C2 N1 109.9(3) . . ?
C3 C2 H2 125.0 . . ?
N1 C2 H2 125.0 . . ?
C2 C3 N2 107.0(3) . . ?
C2 C3 H3 126.5 . . ?
N2 C3 H3 126.5 . . ?
N2 C4 C5 111.2(3) . . ?
N2 C4 H4A 109.4 . . ?
C5 C4 H4A 109.4 . . ?
N2 C4 H4B 109.4 . . ?
C5 C4 H4B 109.4 . . ?
H4A C4 H4B 108.0 . . ?
C6 C5 C6 119.0(3) . 2_755 ?
C6 C5 C4 120.6(3) . . ?
C6 C5 C4 120.4(3) 2_755 . ?
C5 C6 C5 121.0(3) . 3_775 ?
C5 C6 H6 119.5 . . ?
C5 C6 H6 119.5 3_775 . ?
C1 N1 C2 104.0(3) . . ?
C1 N1 Cd1 128.3(2) . . ?
C2 N1 Cd1 127.3(2) . . ?
C1 N2 C3 105.8(3) . . ?
C1 N2 C4 126.4(3) . . ?
C3 N2 C4 127.6(3) . . ?
N1 Cd1 N1 180.00(16) 3_765 12_545 ?
N1 Cd1 N1 88.05(9) 3_765 10_755 ?
N1 Cd1 N1 91.95(9) 12_545 10_755 ?
N1 Cd1 N1 91.95(9) 3_765 . ?
N1 Cd1 N1 88.05(9) 12_545 . ?
N1 Cd1 N1 180.00(15) 10_755 . ?
N1 Cd1 N1 91.95(9) 3_765 2_645 ?
N1 Cd1 N1 88.05(9) 12_545 2_645 ?
N1 Cd1 N1 88.05(9) 10_755 2_645 ?
N1 Cd1 N1 91.95(9) . 2_645 ?
N1 Cd1 N1 88.05(9) 3_765 11_665 ?
N1 Cd1 N1 91.95(9) 12_545 11_665 ?
N1 Cd1 N1 91.95(9) 10_755 11_665 ?
N1 Cd1 N1 88.05(9) . 11_665 ?
N1 Cd1 N1 180.00(16) 2_645 11_665 ?
F2 B1 F1 110.7(3) . 3 ?
F2 B1 F1 110.7(3) . . ?
F1 B1 F1 108.2(3) 3 . ?
F2 B1 F1 110.7(3) . 2 ?
F1 B1 F1 108.2(3) 3 2 ?
F1 B1 F1 108.2(3) . 2 ?

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        25.98
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         0.677
_refine_diff_density_min         -0.300
_refine_diff_density_rms         0.064

#====END

data_2
_database_code_depnum_ccdc_archive 'CCDC 679258'
_audit_creation_date             'Wed Apr 23 21:26:00 2008'
_audit_creation_method           SHELXL-97
_publ_section_references         
;
Molecular Structure Corporation, Rigaku Corporation. (2004). teXsan.
Single Crystal Structure Analysis Software. Version 2.0.
MSC, 9009 New Trails Drive, The Woodlands, TX 77381-5209, USA.
Rigaku, 3-9-12 Akishima, Tokyo, Japan.
;
_chemical_name_systematic        
;
[Cd(tib)2](NO3)2-2(EtOH)
;
_chemical_name_common            (Cd(tib)2)(NO3)2-2(EtOH)
_chemical_melting_point          ?
_chemical_formula_moiety         'C40 H48 Cd N14 O8 '
_chemical_formula_sum            'C40 H48 Cd N14 O8'
_chemical_formula_weight         965.32

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Cd Cd -0.8075 1.2024 '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'
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'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'C 2/c'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_Int_Tables_number      15

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                   22.183(7)
_cell_length_b                   14.357(4)
_cell_length_c                   17.947(4)
_cell_angle_alpha                90.00
_cell_angle_beta                 128.555(9)
_cell_angle_gamma                90.00
_cell_volume                     4470(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    200
_cell_measurement_reflns_used    12213
_cell_measurement_theta_min      3.2
_cell_measurement_theta_max      27.5

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.100
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.434
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1992
_exptl_absorpt_coefficient_mu    0.555
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.839
_exptl_absorpt_correction_T_max  0.946
_exptl_absorpt_process_details   '(Higashi, 1995)'

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      200
_diffrn_radiation_wavelength     0.71075
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Rigaku RAXIS-RAPID Imaging Plate'
_diffrn_measurement_method       ω
_diffrn_detector_area_resol_mean 10.00
_diffrn_reflns_number            16531
_diffrn_reflns_av_R_equivalents  0.0530
_diffrn_reflns_av_sigmaI/netI    0.0381
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         3.18
_diffrn_reflns_theta_max         25.00
_reflns_number_total             3928
_reflns_number_gt                3412
_reflns_threshold_expression     I>2σ(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SIR92 (Alatomare et al., 1994)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
;
Refinement of F² against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F², conventional R-factors R are based
on F, with F set to zero for negative F². The threshold expression of
F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F² are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0692P)²+13.2897P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         3928
_refine_ls_number_parameters     350
_refine_ls_number_restraints     136
_refine_ls_R_factor_all          0.0599
_refine_ls_R_factor_gt           0.0498
_refine_ls_wR_factor_ref         0.1285
_refine_ls_wR_factor_gt          0.1232
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_restrained_S_all      1.101
_refine_ls_shift/su_max          0.003
_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 0.5000 0.57728(3) 0.7500 0.03160(17) Uani 1 2 d S . .
O11 O 0.8791(6) 0.6442(7) 0.8050(6) 0.070(2) Uani 0.597(11) 1 d PDU . .
O11B O 0.8527(11) 0.6392(12) 0.7553(15) 0.109(5) Uani 0.403(11) 1 d PDU . .
O12 O 0.9023(7) 0.7873(5) 0.7982(9) 0.108(4) Uani 0.597(11) 1 d PDU . .
O12B O 0.8765(12) 0.7623(13) 0.8148(13) 0.123(6) Uani 0.403(11) 1 d PDU . .
O13 O 0.8558(9) 0.7102(11) 0.6843(8) 0.173(5) Uani 0.597(11) 1 d PDU . .
O13B O 0.9353(10) 0.7090(15) 0.7557(12) 0.154(6) Uani 0.403(11) 1 d PDU . .
O21 O 0.8599(11) 0.3972(11) 0.6499(14) 0.104(7) Uani 0.250(10) 1 d PDU . .
O21B O 0.8168(15) 0.483(2) 0.5626(13) 0.137(6) Uani 0.250(10) 1 d PDU . .
O22 O 0.7738(10) 0.5633(9) 0.5643(13) 0.185(6) Uani 0.50 1 d PDU . .
N1 N 0.8853(3) 0.7100(3) 0.7692(3) 0.0641(13) Uani 1 1 d D . .
N11 N 0.44984(19) 0.8117(2) 0.5578(2) 0.0371(8) Uani 1 1 d . . .
N12 N 0.4463(2) 0.6956(2) 0.6351(3) 0.0410(9) Uani 1 1 d . . .
N31 N 0.6105(2) 0.6575(3) 0.4600(3) 0.0439(9) Uani 1 1 d . . .
N32 N 0.5481(2) 0.5358(2) 0.3695(2) 0.0400(8) Uani 1 1 d . . .
N51 N 0.8027(2) 1.0193(3) 0.7541(2) 0.0383(8) Uani 1 1 d . . .
N52 N 0.8881(2) 1.0740(2) 0.7404(3) 0.0410(8) Uani 1 1 d . . .
C1 C 0.5570(3) 0.8813(3) 0.5704(3) 0.0381(10) Uani 1 1 d . . .
C2 C 0.5683(3) 0.8222(3) 0.5187(3) 0.0432(10) Uani 1 1 d . . .
H1 H 0.5253 0.7931 0.4625 0.052 Uiso 1 1 calc R . .
C3 C 0.6421(3) 0.8056(3) 0.5489(3) 0.0462(11) Uani 1 1 d . . .
C4 C 0.7043(3) 0.8480(3) 0.6307(3) 0.0440(11) Uani 1 1 d . . .
H2 H 0.7549 0.8357 0.6523 0.053 Uiso 1 1 calc R . .
C5 C 0.6934(3) 0.9090(3) 0.6823(3) 0.0403(10) Uani 1 1 d . . .
C6 C 0.6196(3) 0.9247(3) 0.6515(3) 0.0393(10) Uani 1 1 d . . .
H3 H 0.6117 0.9657 0.6863 0.047 Uiso 1 1 calc R . .
C11 C 0.4778(3) 0.8954(3) 0.5405(4) 0.0481(12) Uani 1 1 d . . .
H4 H 0.4785 0.9485 0.5762 0.058 Uiso 1 1 calc R . .
H5 H 0.4419 0.9110 0.4718 0.058 Uiso 1 1 calc R . .
C12 C 0.4838(3) 0.7704(3) 0.6412(3) 0.0486(12) Uani 1 1 d . . .
H6 H 0.5301 0.7922 0.6991 0.058 Uiso 1 1 calc R . .
C13 C 0.3859(3) 0.6902(4) 0.5423(4) 0.0688(17) Uani 1 1 d . . .
H7 H 0.3474 0.6432 0.5145 0.083 Uiso 1 1 calc R . .
C14 C 0.3874(3) 0.7611(4) 0.4939(4) 0.0732(18) Uani 1 1 d . . .
H8 H 0.3512 0.7726 0.4274 0.088 Uiso 1 1 calc R . .
C31 C 0.6566(3) 0.7433(4) 0.4940(4) 0.0664(16) Uani 1 1 d . . .
H9 H 0.6447 0.7781 0.4386 0.080 Uiso 1 1 calc R . .
H10 H 0.7120 0.7266 0.5354 0.080 Uiso 1 1 calc R . .
C32 C 0.5808(3) 0.6162(3) 0.3772(3) 0.0412(10) Uani 1 1 d . . .
H11 H 0.5827 0.6412 0.3298 0.049 Uiso 1 1 calc R . .
C33 C 0.5583(3) 0.5263(3) 0.4528(3) 0.0482(11) Uani 1 1 d . . .
H12 H 0.5409 0.4752 0.4684 0.058 Uiso 1 1 calc R . .
C34 C 0.5972(3) 0.6011(3) 0.5096(3) 0.0498(12) Uani 1 1 d . . .
H13 H 0.6121 0.6120 0.5713 0.060 Uiso 1 1 calc R . .
C51 C 0.7620(3) 0.9544(4) 0.7715(3) 0.0498(12) Uani 1 1 d . . .
H14 H 0.7445 0.9882 0.8030 0.060 Uiso 1 1 calc R . .
H15 H 0.7984 0.9053 0.8158 0.060 Uiso 1 1 calc R . .
C52 C 0.8662(3) 1.0009(3) 0.7628(3) 0.0395(10) Uani 1 1 d . . .
H16 H 0.8921 0.9426 0.7826 0.047 Uiso 1 1 calc R . .
C53 C 0.8356(3) 1.1423(3) 0.7157(4) 0.0496(12) Uani 1 1 d . . .
H17 H 0.8359 1.2033 0.6953 0.060 Uiso 1 1 calc R . .
C54 C 0.7829(3) 1.1096(4) 0.7247(4) 0.0502(12) Uani 1 1 d . . .
H18 H 0.7407 1.1429 0.7130 0.060 Uiso 1 1 calc R . .
C101 C 0.8751(8) 0.4955(10) 0.6644(11) 0.108(4) Uani 0.250(10) 1 d PDU . .
H19 H 0.8502 0.5236 0.6894 0.130 Uiso 0.250(10) 1 calc PR . .
H20 H 0.8548 0.5265 0.6035 0.130 Uiso 0.250(10) 1 calc PR . .
C102 C 0.9646(8) 0.5070(12) 0.7379(13) 0.121(6) Uani 0.250(10) 1 d PDU . .
H21 H 0.9776 0.5734 0.7501 0.145 Uiso 0.250(10) 1 calc PR . .
H22 H 0.9884 0.4792 0.7120 0.145 Uiso 0.250(10) 1 calc PR . .
H23 H 0.9839 0.4757 0.7975 0.145 Uiso 0.250(10) 1 calc PR . .
C103 C 0.7725(11) 0.4923(11) 0.5130(11) 0.114(5) Uani 0.50 1 d PDU . .
H24 H 0.7983 0.5120 0.4863 0.137 Uiso 0.50 1 calc PR . .
H25 H 0.7184 0.4759 0.4594 0.137 Uiso 0.50 1 calc PR . .
C104 C 0.8142(9) 0.4067(10) 0.5779(13) 0.101(4) Uani 0.50 1 d PDU . .
H26 H 0.8101 0.3544 0.5400 0.121 Uiso 0.50 1 calc PR . .
H27 H 0.7903 0.3897 0.6071 0.121 Uiso 0.50 1 calc PR . .
H28 H 0.8686 0.4218 0.6280 0.121 Uiso 0.50 1 calc PR . .
C105 C 0.8751(8) 0.4955(10) 0.6644(11) 0.108(4) Uani 0.250(10) 1 d P . .
H19B H 0.8655 0.4424 0.6908 0.130 Uiso 0.250(10) 1 calc PR . .
H20B H 0.8562 0.5509 0.6771 0.130 Uiso 0.250(10) 1 calc PR . .
C106 C 0.9646(8) 0.5070(12) 0.7379(13) 0.121(6) Uani 0.250(10) 1 d P . .
H21B H 0.9804 0.5105 0.8024 0.145 Uiso 0.250(10) 1 calc PR . .
H22B H 0.9799 0.5643 0.7239 0.145 Uiso 0.250(10) 1 calc PR . .
H23B H 0.9896 0.4535 0.7334 0.145 Uiso 0.250(10) 1 calc PR . .


_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 N12 2.344(3) . ?
Cd1 N12 2.344(3) 2_656 ?
Cd1 N32 2.349(3) 5_666 ?
Cd1 N32 2.349(3) 6_566 ?
Cd1 N52 2.379(4) 4_646 ?
Cd1 N52 2.379(4) 3_445 ?
O11 O11B 0.701(19) . ?
O11 N1 1.197(8) . ?
O11 O12B 1.71(2) . ?
O11B N1 1.181(13) . ?
O11B O13 1.67(2) . ?
O12 O12B 0.87(2) . ?
O12 N1 1.182(9) . ?
O12 O13B 1.75(2) . ?
O12B N1 1.212(13) . ?
O13 N1 1.227(10) . ?
O13 O13B 1.391(19) . ?
O13B N1 1.274(12) . ?
O21 C101 1.436(10) . ?
O21B O22 1.51(4) . ?
O22 C103 1.362(10) . ?
N11 C12 1.324(5) . ?
N11 C14 1.335(6) . ?
N11 C11 1.472(5) . ?
N12 C12 1.320(6) . ?
N12 C13 1.339(6) . ?
N31 C32 1.333(5) . ?
N31 C34 1.365(6) . ?
N31 C31 1.469(6) . ?
N32 C32 1.324(6) . ?
N32 C33 1.371(5) . ?
N32 Cd1 2.349(3) 5_666 ?
N51 C52 1.341(6) . ?
N51 C54 1.364(6) . ?
N51 C51 1.461(5) . ?
N52 C52 1.320(5) . ?
N52 C53 1.368(6) . ?
N52 Cd1 2.379(4) 3 ?
C1 C6 1.384(6) . ?
C1 C2 1.391(6) . ?
C1 C11 1.497(6) . ?
C2 C3 1.386(7) . ?
C2 H1 0.9500 . ?
C3 C4 1.380(6) . ?
C3 C31 1.507(6) . ?
C4 C5 1.400(6) . ?
C4 H2 0.9500 . ?
C5 C6 1.381(7) . ?
C5 C51 1.506(6) . ?
C6 H3 0.9500 . ?
C11 H4 0.9900 . ?
C11 H5 0.9900 . ?
C12 H6 0.9500 . ?
C13 C14 1.353(8) . ?
C13 H7 0.9500 . ?
C14 H8 0.9500 . ?
C31 H9 0.9900 . ?
C31 H10 0.9900 . ?
C32 H11 0.9500 . ?
C33 C34 1.357(7) . ?
C33 H12 0.9500 . ?
C34 H13 0.9500 . ?
C51 H14 0.9900 . ?
C51 H15 0.9900 . ?
C52 H16 0.9500 . ?
C53 C54 1.360(7) . ?
C53 H17 0.9500 . ?
C54 H18 0.9500 . ?
C101 C102 1.563(10) . ?
C101 H19 0.9900 . ?
C101 H20 0.9900 . ?
C102 H21 0.9800 . ?
C102 H22 0.9800 . ?
C102 H23 0.9800 . ?
C103 C104 1.542(10) . ?
C103 H24 0.9900 . ?
C103 H25 0.9900 . ?
C104 H26 0.9800 . ?
C104 H27 0.9800 . ?
C104 H28 0.9800 . ?

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
N12 Cd1 N12 87.09(19) . 2_656 ?
N12 Cd1 N32 90.30(13) . 5_666 ?
N12 Cd1 N32 175.04(12) 2_656 5_666 ?
N12 Cd1 N32 175.03(12) . 6_566 ?
N12 Cd1 N32 90.30(13) 2_656 6_566 ?
N32 Cd1 N32 92.61(18) 5_666 6_566 ?
N12 Cd1 N52 90.77(12) . 4_646 ?
N12 Cd1 N52 90.88(13) 2_656 4_646 ?
N32 Cd1 N52 84.94(13) 5_666 4_646 ?
N32 Cd1 N52 93.50(13) 6_566 4_646 ?
N12 Cd1 N52 90.88(12) . 3_445 ?
N12 Cd1 N52 90.76(12) 2_656 3_445 ?
N32 Cd1 N52 93.49(13) 5_666 3_445 ?
N32 Cd1 N52 84.93(13) 6_566 3_445 ?
N52 Cd1 N52 177.74(17) 4_646 3_445 ?
O12 N1 O11 128.0(9) . . ?
O11B N1 O12B 109.9(16) . . ?
O12 N1 O13 108.7(11) . . ?
O11 N1 O13 121.2(10) . . ?
O11B N1 O13B 116.2(17) . . ?
O12B N1 O13B 131.3(15) . . ?
C12 N11 C14 106.3(4) . . ?
C12 N11 C11 126.0(4) . . ?
C14 N11 C11 127.7(4) . . ?
C12 N12 C13 103.9(4) . . ?
C12 N12 Cd1 124.6(3) . . ?
C13 N12 Cd1 128.1(3) . . ?
C32 N31 C34 107.8(4) . . ?
C32 N31 C31 124.7(4) . . ?
C34 N31 C31 127.2(4) . . ?
C32 N32 C33 105.3(4) . . ?
C32 N32 Cd1 127.2(3) . 5_666 ?
C33 N32 Cd1 126.8(3) . 5_666 ?
C52 N51 C54 107.1(4) . . ?
C52 N51 C51 126.3(4) . . ?
C54 N51 C51 126.5(4) . . ?
C52 N52 C53 105.5(4) . . ?
C52 N52 Cd1 124.0(3) . 3 ?
C53 N52 Cd1 130.4(3) . 3 ?
C6 C1 C2 119.7(4) . . ?
C6 C1 C11 120.0(4) . . ?
C2 C1 C11 120.2(4) . . ?
C3 C2 C1 120.2(4) . . ?
C3 C2 H1 119.9 . . ?
C1 C2 H1 119.9 . . ?
C4 C3 C2 119.6(4) . . ?
C4 C3 C31 118.5(4) . . ?
C2 C3 C31 121.8(4) . . ?
C3 C4 C5 120.6(4) . . ?
C3 C4 H2 119.7 . . ?
C5 C4 H2 119.7 . . ?
C6 C5 C4 119.2(4) . . ?
C6 C5 C51 121.1(4) . . ?
C4 C5 C51 119.8(4) . . ?
C5 C6 C1 120.6(4) . . ?
C5 C6 H3 119.7 . . ?
C1 C6 H3 119.7 . . ?
N11 C11 C1 111.6(4) . . ?
N11 C11 H4 109.3 . . ?
C1 C11 H4 109.3 . . ?
N11 C11 H5 109.3 . . ?
C1 C11 H5 109.3 . . ?
H4 C11 H5 108.0 . . ?
N12 C12 N11 112.7(4) . . ?
N12 C12 H6 123.6 . . ?
N11 C12 H6 123.6 . . ?
N12 C13 C14 110.4(5) . . ?
N12 C13 H7 124.8 . . ?
C14 C13 H7 124.8 . . ?
N11 C14 C13 106.6(4) . . ?
N11 C14 H8 126.7 . . ?
C13 C14 H8 126.7 . . ?
N31 C31 C3 113.0(4) . . ?
N31 C31 H9 109.0 . . ?
C3 C31 H9 109.0 . . ?
N31 C31 H10 109.0 . . ?
C3 C31 H10 109.0 . . ?
H9 C31 H10 107.8 . . ?
N32 C32 N31 111.3(4) . . ?
N32 C32 H11 124.4 . . ?
N31 C32 H11 124.4 . . ?
C34 C33 N32 109.7(4) . . ?
C34 C33 H12 125.1 . . ?
N32 C33 H12 125.1 . . ?
C33 C34 N31 105.9(4) . . ?
C33 C34 H13 127.1 . . ?
N31 C34 H13 127.1 . . ?
N51 C51 C5 113.6(4) . . ?
N51 C51 H14 108.9 . . ?
C5 C51 H14 108.9 . . ?
N51 C51 H15 108.9 . . ?
C5 C51 H15 108.9 . . ?
H14 C51 H15 107.7 . . ?
N52 C52 N51 111.5(4) . . ?
N52 C52 H16 124.2 . . ?
N51 C52 H16 124.2 . . ?
C54 C53 N52 109.5(4) . . ?
C54 C53 H17 125.2 . . ?
N52 C53 H17 125.2 . . ?
C53 C54 N51 106.3(4) . . ?
C53 C54 H18 126.9 . . ?
N51 C54 H18 126.9 . . ?
O21 C101 C102 106.7(9) . . ?
O21 C101 H19 110.4 . . ?
C102 C101 H19 110.4 . . ?
O21 C101 H20 110.4 . . ?
C102 C101 H20 110.4 . . ?
H19 C101 H20 108.6 . . ?
C101 C102 H21 109.5 . . ?
C101 C102 H22 109.5 . . ?
H21 C102 H22 109.5 . . ?
C101 C102 H23 109.5 . . ?
H21 C102 H23 109.5 . . ?
H22 C102 H23 109.5 . . ?
O22 C103 C104 109.6(9) . . ?
O22 C103 H24 109.8 . . ?
C104 C103 H24 109.8 . . ?
O22 C103 H25 109.8 . . ?
C104 C103 H25 109.8 . . ?
H24 C103 H25 108.2 . . ?
C103 C104 H26 109.5 . . ?
C103 C104 H27 109.5 . . ?
H26 C104 H27 109.5 . . ?
C103 C104 H28 109.5 . . ?
H26 C104 H28 109.5 . . ?
H27 C104 H28 109.5 . . ?

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
N12 Cd1 N12 C12 44.9(4) 2_656 . . . ?
N32 Cd1 N12 C12 -130.9(4) 5_666 . . . ?
N52 Cd1 N12 C12 -45.9(4) 4_646 . . . ?
N52 Cd1 N12 C12 135.6(4) 3_445 . . . ?
N12 Cd1 N12 C13 -159.0(5) 2_656 . . . ?
N32 Cd1 N12 C13 25.2(5) 5_666 . . . ?
N52 Cd1 N12 C13 110.2(5) 4_646 . . . ?
N52 Cd1 N12 C13 -68.3(5) 3_445 . . . ?
C6 C1 C2 C3 1.0(6) . . . . ?
C11 C1 C2 C3 -176.9(4) . . . . ?
C1 C2 C3 C4 0.1(7) . . . . ?
C1 C2 C3 C31 -178.9(5) . . . . ?
C2 C3 C4 C5 -1.3(7) . . . . ?
C31 C3 C4 C5 177.7(5) . . . . ?
C3 C4 C5 C6 1.4(7) . . . . ?
C3 C4 C5 C51 179.9(4) . . . . ?
C4 C5 C6 C1 -0.4(6) . . . . ?
C51 C5 C6 C1 -178.8(4) . . . . ?
C2 C1 C6 C5 -0.8(6) . . . . ?
C11 C1 C6 C5 177.0(4) . . . . ?
C12 N11 C11 C1 58.2(6) . . . . ?
C14 N11 C11 C1 -119.9(6) . . . . ?
C6 C1 C11 N11 -107.3(5) . . . . ?
C2 C1 C11 N11 70.6(5) . . . . ?
C13 N12 C12 N11 0.4(6) . . . . ?
Cd1 N12 C12 N11 161.2(3) . . . . ?
C14 N11 C12 N12 -0.5(6) . . . . ?
C11 N11 C12 N12 -178.9(4) . . . . ?
C12 N12 C13 C14 -0.1(7) . . . . ?
Cd1 N12 C13 C14 -160.0(4) . . . . ?
C12 N11 C14 C13 0.4(7) . . . . ?
C11 N11 C14 C13 178.8(5) . . . . ?
N12 C13 C14 N11 -0.2(8) . . . . ?
C32 N31 C31 C3 144.0(5) . . . . ?
C34 N31 C31 C3 -43.4(8) . . . . ?
C4 C3 C31 N31 137.9(5) . . . . ?
C2 C3 C31 N31 -43.0(8) . . . . ?
C33 N32 C32 N31 -0.2(5) . . . . ?
Cd1 N32 C32 N31 -171.7(3) 5_666 . . . ?
C34 N31 C32 N32 0.5(6) . . . . ?
C31 N31 C32 N32 174.3(5) . . . . ?
C32 N32 C33 C34 -0.1(6) . . . . ?
Cd1 N32 C33 C34 171.4(3) 5_666 . . . ?
N32 C33 C34 N31 0.4(6) . . . . ?
C32 N31 C34 C33 -0.5(6) . . . . ?
C31 N31 C34 C33 -174.1(5) . . . . ?
C52 N51 C51 C5 -97.4(5) . . . . ?
C54 N51 C51 C5 81.7(6) . . . . ?
C6 C5 C51 N51 -115.7(5) . . . . ?
C4 C5 C51 N51 65.9(6) . . . . ?
C53 N52 C52 N51 -0.3(5) . . . . ?
Cd1 N52 C52 N51 177.8(3) 3 . . . ?
C54 N51 C52 N52 -0.3(5) . . . . ?
C51 N51 C52 N52 179.0(4) . . . . ?
C52 N52 C53 C54 0.7(6) . . . . ?
Cd1 N52 C53 C54 -177.1(3) 3 . . . ?
N52 C53 C54 N51 -0.9(6) . . . . ?
C52 N51 C54 C53 0.7(5) . . . . ?
C51 N51 C54 C53 -178.5(4) . . . . ?
O21B O22 C103 C104 39(2) . . . . ?

_diffrn_measured_fraction_theta_max 0.997
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.997
_refine_diff_density_max         1.070
_refine_diff_density_min         -0.885
_refine_diff_density_rms         0.089

#====END

data_3
_database_code_depnum_ccdc_archive 'CCDC 679259'
_audit_creation_date             'Tue Apr 24 11:02:33 2007'
_audit_creation_method           SHELXL-97
_publ_section_references         
;
Molecular Structure Corporation, Rigaku Corporation. (2004). teXsan.
Single Crystal Structure Analysis Software. Version 2.0.
MSC, 9009 New Trails Drive, The Woodlands, TX 77381-5209, USA.
Rigaku, 3-9-12 Akishima, Tokyo, Japan.
;
_chemical_name_systematic        
;
[Cd(tib)(OAc)2]-4.5(H2O)
;
_chemical_name_common            (Cd(tib)(OAc)2)-4.5(H2O)
_chemical_melting_point          ?
_chemical_formula_moiety         'C22 H33 Cd N6 O8.50 '
_chemical_formula_sum            'C22 H33 Cd N6 O8.50'
_chemical_formula_weight         629.94

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Cd Cd -0.8075 1.2024 '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'
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'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'C 2/c'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_Int_Tables_number      15
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                   14.294(2)
_cell_length_b                   17.334(3)
_cell_length_c                   22.245(2)
_cell_angle_alpha                90.00
_cell_angle_beta                 99.827(8)
_cell_angle_gamma                90.00
_cell_volume                     5430.8(13)
_cell_formula_units_Z            8
_cell_measurement_temperature    200
_cell_measurement_reflns_used    16129
_cell_measurement_theta_min      3.1
_cell_measurement_theta_max      27.5

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.250
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.040
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.541
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2584
_exptl_absorpt_coefficient_mu    0.861
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.796
_exptl_absorpt_correction_T_max  0.966
_exptl_absorpt_process_details   '(Higashi, 1995)'

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      200
_diffrn_radiation_wavelength     0.71075
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Rigaku RAXIS-RAPID Imaging Plate'
_diffrn_measurement_method       ω
_diffrn_detector_area_resol_mean 10.00
_diffrn_reflns_number            25609
_diffrn_reflns_av_R_equivalents  0.0399
_diffrn_reflns_av_sigmaI/netI    0.0309
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_theta_min         3.00
_diffrn_reflns_theta_max         27.46
_reflns_number_total             6201
_reflns_number_gt                5177
_reflns_threshold_expression     I>2σ(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
;
Refinement of F² against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F², conventional R-factors R are based
on F, with F set to zero for negative F². The threshold expression of
F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F² are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0224P)²+10.4211P] 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         6201
_refine_ls_number_parameters     368
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0436
_refine_ls_R_factor_gt           0.0316
_refine_ls_wR_factor_ref         0.0692
_refine_ls_wR_factor_gt          0.0647
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_restrained_S_all      1.034
_refine_ls_shift/su_max          0.003
_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 0.726030(12) 0.427675(10) 0.632563(7) 0.02971(6) Uani 1 1 d . . .
O1 O 0.86359(12) 0.36667(10) 0.67540(8) 0.0370(4) Uani 1 1 d . . .
O2 O 0.81044(15) 0.30986(11) 0.58793(8) 0.0467(5) Uani 1 1 d . . .
O3 O 0.73482(13) 0.52652(11) 0.69980(8) 0.0420(4) Uani 1 1 d . . .
O4 O 0.58423(15) 0.52891(12) 0.65883(9) 0.0537(5) Uani 1 1 d . . .
O5 O 1.0000 0.44377(16) 0.7500 0.0421(6) Uani 1 2 d S . .
H25 H 0.958(2) 0.4112(17) 0.7269(13) 0.050 Uiso 1 1 d . . .
O6 O 0.83638(16) 0.30101(13) 0.46292(10) 0.0479(5) Uani 1 1 d . . .
H26 H 0.832(2) 0.3025(19) 0.5012(16) 0.057 Uiso 1 1 d . . .
H27 H 0.798(2) 0.269(2) 0.4477(15) 0.057 Uiso 1 1 d . . .
O7 O 0.77917(16) 0.56401(14) 0.89233(10) 0.0514(5) Uani 1 1 d . . .
H28 H 0.812(3) 0.5558(19) 0.8630(16) 0.062 Uiso 1 1 d . . .
H29 H 0.796(3) 0.603(2) 0.9083(16) 0.062 Uiso 1 1 d . . .
O8 O 0.39078(17) 0.47969(13) 0.64871(11) 0.0518(5) Uani 1 1 d . . .
H30 H 0.445(3) 0.504(2) 0.6578(15) 0.062 Uiso 1 1 d . . .
H31 H 0.346(3) 0.514(2) 0.6385(15) 0.062 Uiso 1 1 d . . .
O9 O 0.87399(17) 0.54367(16) 0.79707(11) 0.0617(7) Uani 1 1 d . . .
H32 H 0.904(3) 0.508(2) 0.7926(17) 0.074 Uiso 1 1 d . . .
H33 H 0.823(3) 0.538(2) 0.7649(17) 0.074 Uiso 1 1 d . . .
N11 N 0.47307(14) 0.39500(11) 0.49537(9) 0.0270(4) Uani 1 1 d . . .
N12 N 0.61480(14) 0.41002(12) 0.55030(9) 0.0313(4) Uani 1 1 d . . .
N31 N 0.41298(14) 0.06474(11) 0.52163(9) 0.0299(4) Uani 1 1 d . . .
N32 N 0.33304(14) 0.00360(11) 0.58386(9) 0.0325(5) Uani 1 1 d . . .
N51 N 0.13950(14) 0.20887(11) 0.28224(9) 0.0307(4) Uani 1 1 d . . .
N52 N 0.15699(16) 0.15749(13) 0.19417(9) 0.0375(5) Uani 1 1 d . . .
C1 C 0.34379(16) 0.30490(13) 0.45328(10) 0.0254(5) Uani 1 1 d . . .
C2 C 0.39990(16) 0.24057(13) 0.46974(10) 0.0266(5) Uani 1 1 d . . .
H1 H 0.4576 0.2457 0.4978 0.032 Uiso 1 1 calc R . .
C3 C 0.37227(16) 0.16829(13) 0.44534(10) 0.0278(5) Uani 1 1 d . . .
C4 C 0.28743(17) 0.16081(13) 0.40505(11) 0.0301(5) Uani 1 1 d . . .
H2 H 0.2689 0.1116 0.3883 0.036 Uiso 1 1 calc R . .
C5 C 0.22899(16) 0.22430(13) 0.38870(10) 0.0277(5) Uani 1 1 d . . .
C6 C 0.25843(16) 0.29614(13) 0.41269(10) 0.0274(5) Uani 1 1 d . . .
H3 H 0.2197 0.3401 0.4012 0.033 Uiso 1 1 calc R . .
C11 C 0.37078(17) 0.38434(14) 0.47897(12) 0.0324(5) Uani 1 1 d . . .
H4 H 0.3449 0.4237 0.4483 0.039 Uiso 1 1 calc R . .
H5 H 0.3413 0.3926 0.5156 0.039 Uiso 1 1 calc R . .
C12 C 0.52317(17) 0.40615(14) 0.55110(11) 0.0318(5) Uani 1 1 d . . .
H6 H 0.4959 0.4107 0.5870 0.038 Uiso 1 1 calc R . .
C13 C 0.62370(18) 0.40115(15) 0.49003(11) 0.0341(5) Uani 1 1 d . . .
H7 H 0.6820 0.4011 0.4749 0.041 Uiso 1 1 calc R . .
C14 C 0.53684(18) 0.39255(15) 0.45577(11) 0.0337(5) Uani 1 1 d . . .
H8 H 0.5227 0.3861 0.4128 0.040 Uiso 1 1 calc R . .
C31 C 0.43347(18) 0.09841(14) 0.46462(12) 0.0336(5) Uani 1 1 d . . .
H9 H 0.4223 0.0591 0.4319 0.040 Uiso 1 1 calc R . .
H10 H 0.5012 0.1135 0.4703 0.040 Uiso 1 1 calc R . .
C32 C 0.33889(17) 0.01830(13) 0.52626(11) 0.0302(5) Uani 1 1 d . . .
H11 H 0.2961 -0.0014 0.4923 0.036 Uiso 1 1 calc R . .
C33 C 0.40775(18) 0.04295(14) 0.61735(12) 0.0353(6) Uani 1 1 d . . .
H12 H 0.4226 0.0432 0.6606 0.042 Uiso 1 1 calc R . .
C34 C 0.45723(18) 0.08139(14) 0.57995(12) 0.0351(6) Uani 1 1 d . . .
H13 H 0.5113 0.1133 0.5917 0.042 Uiso 1 1 calc R . .
C51 C 0.13379(18) 0.21479(15) 0.34727(11) 0.0342(5) Uani 1 1 d . . .
H14 H 0.1026 0.1678 0.3597 0.041 Uiso 1 1 calc R . .
H15 H 0.0931 0.2594 0.3533 0.041 Uiso 1 1 calc R . .
C52 C 0.1535(2) 0.14414(15) 0.25206(11) 0.0377(6) Uani 1 1 d . . .
H16 H 0.1601 0.0944 0.2703 0.045 Uiso 1 1 calc R . .
C53 C 0.1431(2) 0.23528(16) 0.18699(12) 0.0439(7) Uani 1 1 d . . .
H17 H 0.1412 0.2625 0.1497 0.053 Uiso 1 1 calc R . .
C54 C 0.1323(2) 0.26773(16) 0.24042(13) 0.0428(6) Uani 1 1 d . . .
H18 H 0.1219 0.3208 0.2477 0.051 Uiso 1 1 calc R . .
C71 C 0.87010(19) 0.31537(15) 0.63611(12) 0.0362(6) Uani 1 1 d . . .
C72 C 0.9515(3) 0.2602(2) 0.65013(16) 0.0659(10) Uani 1 1 d . . .
H19 H 0.9296 0.2121 0.6662 0.079 Uiso 1 1 calc R . .
H20 H 1.0014 0.2831 0.6806 0.079 Uiso 1 1 calc R . .
H21 H 0.9769 0.2493 0.6128 0.079 Uiso 1 1 calc R . .
C81 C 0.65199(19) 0.55455(14) 0.69513(11) 0.0340(6) Uani 1 1 d . . .
C82 C 0.6390(2) 0.62241(18) 0.73485(14) 0.0492(7) Uani 1 1 d . . .
H22 H 0.6474 0.6703 0.7130 0.059 Uiso 1 1 calc R . .
H23 H 0.6862 0.6201 0.7724 0.059 Uiso 1 1 calc R . .
H24 H 0.5751 0.6211 0.7451 0.059 Uiso 1 1 calc R . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cd1 N12 2.231(2) . ?
Cd1 O3 2.2637(18) . ?
Cd1 O1 2.2919(17) . ?
Cd1 N52 2.344(2) 8_556 ?
Cd1 N32 2.411(2) 3 ?
Cd1 O2 2.650(2) . ?
O1 C71 1.261(3) . ?
O2 C71 1.254(3) . ?
O3 C81 1.268(3) . ?
O4 C81 1.233(3) . ?
O5 H25 0.91(3) . ?
O6 H26 0.86(3) . ?
O6 H27 0.80(3) . ?
O7 H28 0.88(4) . ?
O7 H29 0.78(4) . ?
O8 H30 0.87(4) . ?
O8 H31 0.87(4) . ?
O9 H32 0.78(4) . ?
O9 H33 0.94(4) . ?
N11 C12 1.336(3) . ?
N11 C14 1.372(3) . ?
N11 C11 1.457(3) . ?
N12 C12 1.315(3) . ?
N12 C13 1.377(3) . ?
N31 C32 1.348(3) . ?
N31 C34 1.373(3) . ?
N31 C31 1.470(3) . ?
N32 C32 1.323(3) . ?
N32 C33 1.374(3) . ?
N32 Cd1 2.411(2) 3_445 ?
N51 C52 1.340(3) . ?
N51 C54 1.373(3) . ?
N51 C51 1.466(3) . ?
N52 C52 1.318(3) . ?
N52 C53 1.368(3) . ?
N52 Cd1 2.344(2) 8_455 ?
C1 C2 1.386(3) . ?
C1 C6 1.397(3) . ?
C1 C11 1.515(3) . ?
C2 C3 1.395(3) . ?
C2 H1 0.9500 . ?
C3 C4 1.386(3) . ?
C3 C31 1.513(3) . ?
C4 C5 1.392(3) . ?
C4 H2 0.9500 . ?
C5 C6 1.391(3) . ?
C5 C51 1.517(3) . ?
C6 H3 0.9500 . ?
C11 H4 0.9900 . ?
C11 H5 0.9900 . ?
C12 H6 0.9500 . ?
C13 C14 1.350(3) . ?
C13 H7 0.9500 . ?
C14 H8 0.9500 . ?
C31 H9 0.9900 . ?
C31 H10 0.9900 . ?
C32 H11 0.9500 . ?
C33 C34 1.355(4) . ?
C33 H12 0.9500 . ?
C34 H13 0.9500 . ?
C51 H14 0.9900 . ?
C51 H15 0.9900 . ?
C52 H16 0.9500 . ?
C53 C54 1.347(4) . ?
C53 H17 0.9500 . ?
C54 H18 0.9500 . ?
C71 C72 1.498(4) . ?
C72 H19 0.9800 . ?
C72 H20 0.9800 . ?
C72 H21 0.9800 . ?
C81 C82 1.502(4) . ?
C82 H22 0.9800 . ?
C82 H23 0.9800 . ?
C82 H24 0.9800 . ?

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
N12 Cd1 O3 126.67(7) . . ?
N12 Cd1 O1 135.93(7) . . ?
O3 Cd1 O1 97.33(6) . . ?
N12 Cd1 N52 94.65(7) . 8_556 ?
O3 Cd1 N52 94.11(7) . 8_556 ?
O1 Cd1 N52 83.29(7) . 8_556 ?
N12 Cd1 N32 97.14(7) . 3 ?
O3 Cd1 N32 85.17(7) . 3 ?
O1 Cd1 N32 82.74(7) . 3 ?
N52 Cd1 N32 165.81(7) 8_556 3 ?
N12 Cd1 O2 83.87(7) . . ?
O3 Cd1 O2 148.59(6) . . ?
O1 Cd1 O2 52.19(6) . . ?
N52 Cd1 O2 89.87(7) 8_556 . ?
N32 Cd1 O2 83.57(7) 3 . ?
C71 O1 Cd1 101.34(15) . . ?
C71 O2 Cd1 84.71(15) . . ?
C81 O3 Cd1 106.88(16) . . ?
H26 O6 H27 106(3) . . ?
H28 O7 H29 109(3) . . ?
H30 O8 H31 107(3) . . ?
H32 O9 H33 101(3) . . ?
C12 N11 C14 106.9(2) . . ?
C12 N11 C11 127.4(2) . . ?
C14 N11 C11 125.7(2) . . ?
C12 N12 C13 105.4(2) . . ?
C12 N12 Cd1 124.61(16) . . ?
C13 N12 Cd1 130.00(16) . . ?
C32 N31 C34 107.1(2) . . ?
C32 N31 C31 125.3(2) . . ?
C34 N31 C31 127.2(2) . . ?
C32 N32 C33 104.9(2) . . ?
C32 N32 Cd1 133.65(16) . 3_445 ?
C33 N32 Cd1 121.41(16) . 3_445 ?
C52 N51 C54 106.4(2) . . ?
C52 N51 C51 126.2(2) . . ?
C54 N51 C51 127.3(2) . . ?
C52 N52 C53 105.0(2) . . ?
C52 N52 Cd1 123.43(18) . 8_455 ?
C53 N52 Cd1 128.30(17) . 8_455 ?
C2 C1 C6 119.0(2) . . ?
C2 C1 C11 122.2(2) . . ?
C6 C1 C11 118.7(2) . . ?
C1 C2 C3 120.5(2) . . ?
C1 C2 H1 119.8 . . ?
C3 C2 H1 119.8 . . ?
C4 C3 C2 119.6(2) . . ?
C4 C3 C31 120.6(2) . . ?
C2 C3 C31 119.8(2) . . ?
C3 C4 C5 121.0(2) . . ?
C3 C4 H2 119.5 . . ?
C5 C4 H2 119.5 . . ?
C6 C5 C4 118.6(2) . . ?
C6 C5 C51 120.8(2) . . ?
C4 C5 C51 120.6(2) . . ?
C5 C6 C1 121.3(2) . . ?
C5 C6 H3 119.4 . . ?
C1 C6 H3 119.4 . . ?
N11 C11 C1 112.93(19) . . ?
N11 C11 H4 109.0 . . ?
C1 C11 H4 109.0 . . ?
N11 C11 H5 109.0 . . ?
C1 C11 H5 109.0 . . ?
H4 C11 H5 107.8 . . ?
N12 C12 N11 111.8(2) . . ?
N12 C12 H6 124.1 . . ?
N11 C12 H6 124.1 . . ?
C14 C13 N12 109.5(2) . . ?
C14 C13 H7 125.3 . . ?
N12 C13 H7 125.3 . . ?
C13 C14 N11 106.4(2) . . ?
C13 C14 H8 126.8 . . ?
N11 C14 H8 126.8 . . ?
N31 C31 C3 111.82(19) . . ?
N31 C31 H9 109.3 . . ?
C3 C31 H9 109.3 . . ?
N31 C31 H10 109.3 . . ?
C3 C31 H10 109.3 . . ?
H9 C31 H10 107.9 . . ?
N32 C32 N31 111.7(2) . . ?
N32 C32 H11 124.2 . . ?
N31 C32 H11 124.2 . . ?
C34 C33 N32 110.5(2) . . ?
C34 C33 H12 124.8 . . ?
N32 C33 H12 124.8 . . ?
C33 C34 N31 105.8(2) . . ?
C33 C34 H13 127.1 . . ?
N31 C34 H13 127.1 . . ?
N51 C51 C5 114.3(2) . . ?
N51 C51 H14 108.7 . . ?
C5 C51 H14 108.7 . . ?
N51 C51 H15 108.7 . . ?
C5 C51 H15 108.7 . . ?
H14 C51 H15 107.6 . . ?
N52 C52 N51 112.1(2) . . ?
N52 C52 H16 123.9 . . ?
N51 C52 H16 123.9 . . ?
C54 C53 N52 110.2(2) . . ?
C54 C53 H17 124.9 . . ?
N52 C53 H17 124.9 . . ?
C53 C54 N51 106.3(2) . . ?
C53 C54 H18 126.8 . . ?
N51 C54 H18 126.8 . . ?
O2 C71 O1 121.7(2) . . ?
O2 C71 C72 121.4(3) . . ?
O1 C71 C72 116.9(3) . . ?
C71 C72 H19 109.5 . . ?
C71 C72 H20 109.5 . . ?
H19 C72 H20 109.5 . . ?
C71 C72 H21 109.5 . . ?
H19 C72 H21 109.5 . . ?
H20 C72 H21 109.5 . . ?
O4 C81 O3 122.3(2) . . ?
O4 C81 C82 120.4(2) . . ?
O3 C81 C82 117.4(2) . . ?
C81 C82 H22 109.5 . . ?
C81 C82 H23 109.5 . . ?
H22 C82 H23 109.5 . . ?
C81 C82 H24 109.5 . . ?
H22 C82 H24 109.5 . . ?
H23 C82 H24 109.5 . . ?

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
N12 Cd1 O1 C71 4.5(2) . . . . ?
O3 Cd1 O1 C71 -172.42(16) . . . . ?
N52 Cd1 O1 C71 94.27(16) 8_556 . . . ?
N32 Cd1 O1 C71 -88.28(16) 3 . . . ?
O2 Cd1 O1 C71 -0.80(15) . . . . ?
N12 Cd1 O2 C71 -175.49(16) . . . . ?
O3 Cd1 O2 C71 16.9(2) . . . . ?
O1 Cd1 O2 C71 0.80(14) . . . . ?
N52 Cd1 O2 C71 -80.80(16) 8_556 . . . ?
N32 Cd1 O2 C71 86.58(16) 3 . . . ?
N12 Cd1 O3 C81 21.7(2) . . . . ?
O1 Cd1 O3 C81 -160.92(16) . . . . ?
N52 Cd1 O3 C81 -77.16(17) 8_556 . . . ?
N32 Cd1 O3 C81 117.06(17) 3 . . . ?
O2 Cd1 O3 C81 -173.69(14) . . . . ?
O3 Cd1 N12 C12 -56.3(2) . . . . ?
O1 Cd1 N12 C12 127.53(19) . . . . ?
N52 Cd1 N12 C12 42.4(2) 8_556 . . . ?
N32 Cd1 N12 C12 -145.5(2) 3 . . . ?
O2 Cd1 N12 C12 131.8(2) . . . . ?
O3 Cd1 N12 C13 123.6(2) . . . . ?
O1 Cd1 N12 C13 -52.6(2) . . . . ?
N52 Cd1 N12 C13 -137.7(2) 8_556 . . . ?
N32 Cd1 N12 C13 34.3(2) 3 . . . ?
O2 Cd1 N12 C13 -48.4(2) . . . . ?
C6 C1 C2 C3 1.0(3) . . . . ?
C11 C1 C2 C3 179.6(2) . . . . ?
C1 C2 C3 C4 -0.9(3) . . . . ?
C1 C2 C3 C31 -178.9(2) . . . . ?
C2 C3 C4 C5 -0.3(3) . . . . ?
C31 C3 C4 C5 177.7(2) . . . . ?
C3 C4 C5 C6 1.3(3) . . . . ?
C3 C4 C5 C51 -176.7(2) . . . . ?
C4 C5 C6 C1 -1.2(3) . . . . ?
C51 C5 C6 C1 176.8(2) . . . . ?
C2 C1 C6 C5 0.0(3) . . . . ?
C11 C1 C6 C5 -178.6(2) . . . . ?
C12 N11 C11 C1 -114.8(3) . . . . ?
C14 N11 C11 C1 62.7(3) . . . . ?
C2 C1 C11 N11 28.8(3) . . . . ?
C6 C1 C11 N11 -152.6(2) . . . . ?
C13 N12 C12 N11 0.3(3) . . . . ?
Cd1 N12 C12 N11 -179.77(15) . . . . ?
C14 N11 C12 N12 -0.9(3) . . . . ?
C11 N11 C12 N12 177.0(2) . . . . ?
C12 N12 C13 C14 0.3(3) . . . . ?
Cd1 N12 C13 C14 -179.55(17) . . . . ?
N12 C13 C14 N11 -0.8(3) . . . . ?
C12 N11 C14 C13 1.0(3) . . . . ?
C11 N11 C14 C13 -176.9(2) . . . . ?
C32 N31 C31 C3 79.5(3) . . . . ?
C34 N31 C31 C3 -92.0(3) . . . . ?
C4 C3 C31 N31 -93.6(3) . . . . ?
C2 C3 C31 N31 84.4(3) . . . . ?
C33 N32 C32 N31 -0.1(3) . . . . ?
Cd1 N32 C32 N31 -179.66(15) 3_445 . . . ?
C34 N31 C32 N32 -0.4(3) . . . . ?
C31 N31 C32 N32 -173.3(2) . . . . ?
C32 N32 C33 C34 0.6(3) . . . . ?
Cd1 N32 C33 C34 -179.80(16) 3_445 . . . ?
N32 C33 C34 N31 -0.8(3) . . . . ?
C32 N31 C34 C33 0.7(3) . . . . ?
C31 N31 C34 C33 173.4(2) . . . . ?
C52 N51 C51 C5 86.6(3) . . . . ?
C54 N51 C51 C5 -92.9(3) . . . . ?
C6 C5 C51 N51 102.3(3) . . . . ?
C4 C5 C51 N51 -79.8(3) . . . . ?
C53 N52 C52 N51 -0.8(3) . . . . ?
Cd1 N52 C52 N51 160.05(17) 8_455 . . . ?
C54 N51 C52 N52 0.8(3) . . . . ?
C51 N51 C52 N52 -178.8(2) . . . . ?
C52 N52 C53 C54 0.6(3) . . . . ?
Cd1 N52 C53 C54 -159.0(2) 8_455 . . . ?
N52 C53 C54 N51 -0.1(3) . . . . ?
C52 N51 C54 C53 -0.4(3) . . . . ?
C51 N51 C54 C53 179.2(2) . . . . ?
Cd1 O2 C71 O1 -1.3(2) . . . . ?
Cd1 O2 C71 C72 177.5(3) . . . . ?
Cd1 O1 C71 O2 1.6(3) . . . . ?
Cd1 O1 C71 C72 -177.3(2) . . . . ?
Cd1 O3 C81 O4 -0.6(3) . . . . ?
Cd1 O3 C81 C82 -179.2(2) . . . . ?

_diffrn_measured_fraction_theta_max 0.997
_diffrn_reflns_theta_full        27.46
_diffrn_measured_fraction_theta_full 0.997
_refine_diff_density_max         0.509
_refine_diff_density_min         -0.470
_refine_diff_density_rms         0.065

#====END

data_4
_database_code_depnum_ccdc_archive 'CCDC 679260'
_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C18 H18 Cd Cl2 N6, C H3 O'
_chemical_formula_sum            'C19 H21 Cd Cl2 N6 O'
_chemical_formula_weight         532.72

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
_symmetry_space_group_name_Hall  '-P 1'

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

_cell_length_a                   9.780(2)
_cell_length_b                   10.532(2)
_cell_length_c                   11.572(2)
_cell_angle_alpha                63.37(3)
_cell_angle_beta                 77.83(3)
_cell_angle_gamma                82.84(3)
_cell_volume                     1041.0(4)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    1129
_cell_measurement_theta_min      2.656
_cell_measurement_theta_max      20.924

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.06
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.699
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             534
_exptl_absorpt_coefficient_mu    1.329
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.8568
_exptl_absorpt_correction_T_max  0.9245
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            5212
_diffrn_reflns_av_R_equivalents  0.0336
_diffrn_reflns_av_sigmaI/netI    0.1044
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -7
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_theta_min         2.00
_diffrn_reflns_theta_max         25.00
_reflns_number_total             3599
_reflns_number_gt                2681
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'Bruker SHELXTL'
_computing_structure_refinement  'Bruker SHELXTL'
_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)+(0.0000P)²+-0.2300P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         3599
_refine_ls_number_parameters     263
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0742
_refine_ls_R_factor_gt           0.0536
_refine_ls_wR_factor_ref         0.0705
_refine_ls_wR_factor_gt          0.0666
_refine_ls_goodness_of_fit_ref   1.001
_refine_ls_restrained_S_all      1.001
_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 0.00352(5) 0.41516(5) 0.69231(4) 0.03295(14) Uani 1 1 d . . .
Cl1 Cl -0.18793(15) 0.48108(16) 0.54090(14) 0.0406(4) Uani 1 1 d . . .
Cl2 Cl 0.04104(17) 0.15385(16) 0.73807(16) 0.0519(5) Uani 1 1 d . . .
O1 O 0.5471(5) 0.6196(5) 0.6605(5) 0.0885(18) Uani 1 1 d . . .
N1 N 0.3920(5) 0.2910(5) 0.8580(5) 0.0365(13) Uani 1 1 d . . .
N2 N 0.1843(5) 0.3820(5) 0.8057(5) 0.0386(14) Uani 1 1 d . . .
N3 N 0.2741(5) -0.2404(5) 0.9105(5) 0.0331(12) Uani 1 1 d . . .
N4 N 0.1655(5) -0.3551(5) 1.1139(4) 0.0377(14) Uani 1 1 d . . .
N5 N 0.8922(5) -0.1372(5) 0.6362(5) 0.0350(13) Uani 1 1 d . . .
N6 N 0.9762(5) -0.3562(5) 0.6775(5) 0.0337(13) Uani 1 1 d . . .
C1 C 0.5457(6) 0.1219(6) 0.7941(6) 0.0367(16) Uani 1 1 d . . .
C2 C 0.4342(6) 0.0446(6) 0.8129(5) 0.0361(16) Uani 1 1 d . . .
H2A H 0.3498 0.0584 0.8613 0.043 Uiso 1 1 calc R . .
C3 C 0.4415(6) -0.0531(6) 0.7630(5) 0.0318(15) Uani 1 1 d . . .
C4 C 0.5683(6) -0.0707(6) 0.6898(5) 0.0365(16) Uani 1 1 d . . .
H4A H 0.5767 -0.1361 0.6550 0.044 Uiso 1 1 calc R . .
C5 C 0.6813(6) 0.0070(6) 0.6681(5) 0.0321(15) Uani 1 1 d . . .
C6 C 0.6705(6) 0.1040(6) 0.7201(6) 0.0383(17) Uani 1 1 d . . .
H6A H 0.7470 0.1569 0.7053 0.046 Uiso 1 1 calc R . .
C7 C 0.5350(6) 0.2347(6) 0.8424(6) 0.0434(18) Uani 1 1 d . . .
H7A H 0.5670 0.1946 0.9261 0.052 Uiso 1 1 calc R . .
H7B H 0.5956 0.3116 0.7805 0.052 Uiso 1 1 calc R . .
C8 C 0.3159(7) 0.3601(6) 0.7639(6) 0.0455(18) Uani 1 1 d . . .
H8A H 0.3533 0.3904 0.6753 0.055 Uiso 1 1 calc R . .
C9 C 0.1766(7) 0.3219(7) 0.9366(7) 0.055(2) Uani 1 1 d . . .
H9A H 0.0953 0.3197 0.9959 0.066 Uiso 1 1 calc R . .
C10 C 0.3023(7) 0.2646(7) 0.9718(6) 0.056(2) Uani 1 1 d . . .
H10A H 0.3223 0.2171 1.0564 0.067 Uiso 1 1 calc R . .
C11 C 0.3129(6) -0.1282(6) 0.7784(5) 0.0367(16) Uani 1 1 d . . .
H11A H 0.2355 -0.0594 0.7575 0.044 Uiso 1 1 calc R . .
H11B H 0.3297 -0.1691 0.7162 0.044 Uiso 1 1 calc R . .
C12 C 0.1759(6) -0.2360(6) 1.0088(6) 0.0351(16) Uani 1 1 d . . .
H12A H 0.1206 -0.1553 1.0022 0.042 Uiso 1 1 calc R . .
C13 C 0.2628(6) -0.4452(6) 1.0810(6) 0.0448(18) Uani 1 1 d . . .
H13A H 0.2787 -0.5402 1.1363 0.054 Uiso 1 1 calc R . .
C14 C 0.3315(6) -0.3762(6) 0.9578(6) 0.0455(18) Uani 1 1 d . . .
H14A H 0.4034 -0.4129 0.9135 0.055 Uiso 1 1 calc R . .
C15 C 0.8156(5) -0.0030(6) 0.5782(6) 0.0441(18) Uani 1 1 d . . .
H15A H 0.7931 0.0080 0.4964 0.053 Uiso 1 1 calc R . .
H15B H 0.8747 0.0742 0.5581 0.053 Uiso 1 1 calc R . .
C16 C 0.8980(6) -0.2519(6) 0.6081(5) 0.0366(16) Uani 1 1 d . . .
H16A H 0.8517 -0.2545 0.5469 0.044 Uiso 1 1 calc R . .
C17 C 1.0245(6) -0.3084(6) 0.7531(6) 0.0398(17) Uani 1 1 d . . .
H17A H 1.0844 -0.3601 0.8125 0.048 Uiso 1 1 calc R . .
C18 C 0.9726(6) -0.1742(6) 0.7294(6) 0.0386(16) Uani 1 1 d . . .
H18A H 0.9890 -0.1193 0.7691 0.046 Uiso 1 1 calc R . .
C19 C 0.4761(9) 0.6847(7) 0.5521(7) 0.101(3) Uani 1 1 d . . .
H19A H 0.3807 0.7064 0.5814 0.152 Uiso 1 1 calc R . .
H19B H 0.4784 0.6210 0.5129 0.152 Uiso 1 1 calc R . .
H19C H 0.5211 0.7707 0.4886 0.152 Uiso 1 1 calc R . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cd1 N6 2.321(5) 1_465 ?
Cd1 N2 2.320(5) . ?
Cd1 N4 2.364(4) 2_557 ?
Cd1 Cl2 2.5522(17) . ?
Cd1 Cl1 2.6506(18) . ?
Cd1 Cl1 2.7435(19) 2_566 ?
Cl1 Cd1 2.7435(19) 2_566 ?
O1 C19 1.416(7) . ?
N1 C8 1.329(7) . ?
N1 C10 1.351(6) . ?
N1 C7 1.457(6) . ?
N2 C8 1.306(7) . ?
N2 C9 1.344(7) . ?
N3 C12 1.340(6) . ?
N3 C14 1.374(6) . ?
N3 C11 1.458(6) . ?
N4 C12 1.295(6) . ?
N4 C13 1.377(6) . ?
N4 Cd1 2.364(4) 2_557 ?
N5 C18 1.355(7) . ?
N5 C16 1.377(7) . ?
N5 C15 1.451(6) . ?
N6 C16 1.302(6) . ?
N6 C17 1.368(7) . ?
N6 Cd1 2.321(5) 1_645 ?
C1 C2 1.365(7) . ?
C1 C6 1.381(7) . ?
C1 C7 1.508(7) . ?
C2 C3 1.375(7) . ?
C2 H2A 0.9300 . ?
C3 C4 1.390(7) . ?
C3 C11 1.506(7) . ?
C4 C5 1.370(8) . ?
C4 H4A 0.9300 . ?
C5 C6 1.383(7) . ?
C5 C15 1.519(7) . ?
C6 H6A 0.9300 . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C8 H8A 0.9300 . ?
C9 C10 1.358(8) . ?
C9 H9A 0.9300 . ?
C10 H10A 0.9300 . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
C12 H12A 0.9300 . ?
C13 C14 1.342(7) . ?
C13 H13A 0.9300 . ?
C14 H14A 0.9300 . ?
C15 H15A 0.9700 . ?
C15 H15B 0.9700 . ?
C16 H16A 0.9300 . ?
C17 C18 1.365(7) . ?
C17 H17A 0.9300 . ?
C18 H18A 0.9300 . ?
C19 H19A 0.9600 . ?
C19 H19B 0.9600 . ?
C19 H19C 0.9600 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N6 Cd1 N2 86.70(17) 1_465 . ?
N6 Cd1 N4 85.19(16) 1_465 2_557 ?
N2 Cd1 N4 91.81(17) . 2_557 ?
N6 Cd1 Cl2 172.58(13) 1_465 . ?
N2 Cd1 Cl2 87.30(12) . . ?
N4 Cd1 Cl2 90.64(13) 2_557 . ?
N6 Cd1 Cl1 88.98(13) 1_465 . ?
N2 Cd1 Cl1 173.11(13) . . ?
N4 Cd1 Cl1 93.18(13) 2_557 . ?
Cl2 Cd1 Cl1 97.39(6) . . ?
N6 Cd1 Cl1 88.13(12) 1_465 2_566 ?
N2 Cd1 Cl1 90.11(13) . 2_566 ?
N4 Cd1 Cl1 172.93(12) 2_557 2_566 ?
Cl2 Cd1 Cl1 96.26(6) . 2_566 ?
Cl1 Cd1 Cl1 84.38(5) . 2_566 ?
Cd1 Cl1 Cd1 95.62(5) . 2_566 ?
C8 N1 C10 105.4(5) . . ?
C8 N1 C7 126.7(5) . . ?
C10 N1 C7 127.1(5) . . ?
C8 N2 C9 102.6(5) . . ?
C8 N2 Cd1 124.8(4) . . ?
C9 N2 Cd1 126.9(4) . . ?
C12 N3 C14 105.9(5) . . ?
C12 N3 C11 128.5(5) . . ?
C14 N3 C11 125.6(5) . . ?
C12 N4 C13 104.4(5) . . ?
C12 N4 Cd1 127.9(4) . 2_557 ?
C13 N4 Cd1 127.2(4) . 2_557 ?
C18 N5 C16 106.3(5) . . ?
C18 N5 C15 126.5(5) . . ?
C16 N5 C15 127.2(5) . . ?
C16 N6 C17 105.1(5) . . ?
C16 N6 Cd1 127.6(4) . 1_645 ?
C17 N6 Cd1 126.8(4) . 1_645 ?
C2 C1 C6 119.0(6) . . ?
C2 C1 C7 122.5(5) . . ?
C6 C1 C7 118.3(6) . . ?
C3 C2 C1 122.7(5) . . ?
C3 C2 H2A 118.7 . . ?
C1 C2 H2A 118.7 . . ?
C2 C3 C4 117.5(6) . . ?
C2 C3 C11 120.6(5) . . ?
C4 C3 C11 121.7(6) . . ?
C5 C4 C3 120.9(6) . . ?
C5 C4 H4A 119.5 . . ?
C3 C4 H4A 119.5 . . ?
C4 C5 C6 120.1(5) . . ?
C4 C5 C15 120.7(6) . . ?
C6 C5 C15 119.0(6) . . ?
C5 C6 C1 119.8(6) . . ?
C5 C6 H6A 120.1 . . ?
C1 C6 H6A 120.1 . . ?
N1 C7 C1 111.7(5) . . ?
N1 C7 H7A 109.3 . . ?
C1 C7 H7A 109.3 . . ?
N1 C7 H7B 109.3 . . ?
C1 C7 H7B 109.3 . . ?
H7A C7 H7B 107.9 . . ?
N2 C8 N1 114.7(6) . . ?
N2 C8 H8A 122.6 . . ?
N1 C8 H8A 122.6 . . ?
N2 C9 C10 111.7(6) . . ?
N2 C9 H9A 124.1 . . ?
C10 C9 H9A 124.1 . . ?
N1 C10 C9 105.5(6) . . ?
N1 C10 H10A 127.2 . . ?
C9 C10 H10A 127.2 . . ?
N3 C11 C3 112.8(5) . . ?
N3 C11 H11A 109.0 . . ?
C3 C11 H11A 109.0 . . ?
N3 C11 H11B 109.0 . . ?
C3 C11 H11B 109.0 . . ?
H11A C11 H11B 107.8 . . ?
N4 C12 N3 113.3(5) . . ?
N4 C12 H12A 123.3 . . ?
N3 C12 H12A 123.3 . . ?
C14 C13 N4 110.3(5) . . ?
C14 C13 H13A 124.8 . . ?
N4 C13 H13A 124.8 . . ?
C13 C14 N3 106.1(5) . . ?
C13 C14 H14A 127.0 . . ?
N3 C14 H14A 127.0 . . ?
N5 C15 C5 112.5(4) . . ?
N5 C15 H15A 109.1 . . ?
C5 C15 H15A 109.1 . . ?
N5 C15 H15B 109.1 . . ?
C5 C15 H15B 109.1 . . ?
H15A C15 H15B 107.8 . . ?
N6 C16 N5 112.0(5) . . ?
N6 C16 H16A 124.0 . . ?
N5 C16 H16A 124.0 . . ?
C18 C17 N6 110.5(6) . . ?
C18 C17 H17A 124.8 . . ?
N6 C17 H17A 124.8 . . ?
N5 C18 C17 106.2(6) . . ?
N5 C18 H18A 126.9 . . ?
C17 C18 H18A 126.9 . . ?
O1 C19 H19A 109.5 . . ?
O1 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
O1 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?

_diffrn_measured_fraction_theta_max 0.983
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.983
_refine_diff_density_max         0.813
_refine_diff_density_min         -0.822
_refine_diff_density_rms         0.103

#====END

data_5
_database_code_depnum_ccdc_archive 'CCDC 679261'
_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C36 H40 Cd N12 O2, 4(H2 O), 2(Cl)'
_chemical_formula_sum            'C36 H48 Cd Cl2 N12 O6'
_chemical_formula_weight         928.16

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           Monoclinic
_symmetry_space_group_name_H-M   'P 21/c'
_symmetry_space_group_name_Hall  '-P 2ybc'

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                   10.7409(16)
_cell_length_b                   10.2112(15)
_cell_length_c                   19.623(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 103.429(3)
_cell_angle_gamma                90.00
_cell_volume                     2093.3(5)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    2670
_cell_measurement_theta_min      2.26
_cell_measurement_theta_max      24.76

_exptl_crystal_description       platelet
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.04
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.473
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             956
_exptl_absorpt_coefficient_mu    0.708
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.9013
_exptl_absorpt_correction_T_max  0.9722
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            10912
_diffrn_reflns_av_R_equivalents  0.0710
_diffrn_reflns_av_sigmaI/netI    0.0733
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_theta_min         1.95
_diffrn_reflns_theta_max         26.00
_reflns_number_total             4111
_reflns_number_gt                3396
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'Bruker SHELXTL'
_computing_structure_refinement  'Bruker SHELXTL'
_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)+(0.0706P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         4111
_refine_ls_number_parameters     283
_refine_ls_number_restraints     6
_refine_ls_R_factor_all          0.0697
_refine_ls_R_factor_gt           0.0545
_refine_ls_wR_factor_ref         0.1371
_refine_ls_wR_factor_gt          0.1274
_refine_ls_goodness_of_fit_ref   1.000
_refine_ls_restrained_S_all      0.999
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.2469(4) 0.2101(4) 0.30148(19) 0.0319(9) Uani 1 1 d . . .
C2 C 0.3242(4) 0.2692(4) 0.35972(19) 0.0325(9) Uani 1 1 d . . .
H2 H 0.2917 0.3365 0.3824 0.039 Uiso 1 1 calc R . .
C3 C 0.4507(4) 0.2285(4) 0.38472(19) 0.0298(9) Uani 1 1 d . . .
C4 C 0.4968(4) 0.1271(4) 0.3506(2) 0.0359(10) Uani 1 1 d . . .
H4 H 0.5810 0.0993 0.3668 0.043 Uiso 1 1 calc R . .
C5 C 0.4200(4) 0.0665(4) 0.29308(19) 0.0348(10) Uani 1 1 d . . .
C6 C 0.2963(4) 0.1088(4) 0.2692(2) 0.0355(10) Uani 1 1 d . . .
H6 H 0.2445 0.0684 0.2304 0.043 Uiso 1 1 calc R . .
C7 C 0.1109(4) 0.2559(4) 0.2730(2) 0.0376(10) Uani 1 1 d . . .
H7A H 0.0582 0.1821 0.2528 0.045 Uiso 1 1 calc R . .
H7B H 0.0769 0.2905 0.3110 0.045 Uiso 1 1 calc R . .
C8 C 0.0624(4) 0.3459(4) 0.1504(2) 0.0382(10) Uani 1 1 d . . .
H8 H 0.0258 0.2702 0.1279 0.046 Uiso 1 1 calc R . .
C9 C 0.1344(4) 0.5401(4) 0.1694(2) 0.0391(10) Uani 1 1 d . . .
H9 H 0.1577 0.6259 0.1623 0.047 Uiso 1 1 calc R . .
C10 C 0.1509(5) 0.4806(4) 0.2325(2) 0.0416(11) Uani 1 1 d . . .
H10 H 0.1865 0.5171 0.2761 0.050 Uiso 1 1 calc R . .
C11 C 0.5337(4) 0.2951(4) 0.4479(2) 0.0409(10) Uani 1 1 d . . .
H11A H 0.5733 0.3717 0.4327 0.049 Uiso 1 1 calc R . .
H11B H 0.4805 0.3243 0.4787 0.049 Uiso 1 1 calc R . .
C12 C 0.7506(4) 0.1939(4) 0.4759(2) 0.0352(9) Uani 1 1 d . . .
H12 H 0.7861 0.2495 0.4479 0.042 Uiso 1 1 calc R . .
C13 C 0.7255(5) 0.0399(5) 0.5443(2) 0.0442(11) Uani 1 1 d . . .
H13 H 0.7414 -0.0329 0.5736 0.053 Uiso 1 1 calc R . .
C14 C 0.6170(4) 0.1090(5) 0.5305(2) 0.0413(11) Uani 1 1 d . . .
H14 H 0.5444 0.0926 0.5473 0.050 Uiso 1 1 calc R . .
C15 C 0.4691(5) -0.0491(5) 0.2592(2) 0.0453(11) Uani 1 1 d . . .
H15A H 0.4130 -0.0647 0.2135 0.054 Uiso 1 1 calc R . .
H15B H 0.5536 -0.0290 0.2523 0.054 Uiso 1 1 calc R . .
C16 C 0.5784(4) -0.2138(5) 0.3471(2) 0.0468(11) Uani 1 1 d . . .
H16 H 0.6594 -0.1765 0.3544 0.056 Uiso 1 1 calc R . .
C17 C 0.4233(5) -0.3371(5) 0.3552(3) 0.0525(12) Uani 1 1 d . . .
H17 H 0.3755 -0.4034 0.3694 0.063 Uiso 1 1 calc R . .
C18 C 0.3768(4) -0.2448(5) 0.3065(2) 0.0492(12) Uani 1 1 d . . .
H18 H 0.2924 -0.2365 0.2812 0.059 Uiso 1 1 calc R . .
Cd1 Cd 0.0000 0.5000 0.0000 0.03113(16) Uani 1 2 d S . .
Cl1 Cl 0.12006(12) 0.89763(13) 0.13645(6) 0.0554(3) Uani 1 1 d . . .
H1WA H -0.028(4) 0.745(4) 0.059(2) 0.019(12) Uiso 1 1 d . . .
H2WA H 0.707(4) 0.624(5) 0.443(2) 0.065(17) Uiso 1 1 d D . .
H3WA H 0.936(3) 0.025(7) 0.112(3) 0.11(3) Uiso 1 1 d D . .
H1WB H -0.108(6) 0.749(6) 0.010(3) 0.06(2) Uiso 1 1 d . . .
H2WB H 0.806(6) 0.530(6) 0.440(3) 0.12(3) Uiso 1 1 d D . .
H3WB H 0.817(5) 0.041(7) 0.0579(19) 0.09(3) Uiso 1 1 d D . .
N1 N 0.1050(3) 0.3572(3) 0.21947(15) 0.0314(8) Uani 1 1 d . . .
N2 N 0.0785(3) 0.4548(4) 0.11776(17) 0.0369(8) Uani 1 1 d . . .
N3 N 0.6333(3) 0.2087(3) 0.48665(15) 0.0319(8) Uani 1 1 d . . .
N4 N 0.8102(3) 0.0925(4) 0.50896(16) 0.0361(8) Uani 1 1 d . . .
N5 N 0.4758(3) -0.1670(3) 0.30151(18) 0.0389(8) Uani 1 1 d . . .
N6 N 0.5529(4) -0.3175(4) 0.3805(2) 0.0511(10) Uani 1 1 d . . .
O1W O -0.0694(4) 0.7106(4) 0.0331(2) 0.0504(10) Uani 1 1 d . . .
O2W O 0.7748(4) 0.5838(4) 0.4663(2) 0.0674(11) Uani 1 1 d D . .
O3W O 0.8568(6) 0.0561(5) 0.1011(3) 0.0857(13) Uani 1 1 d 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 C6 1.381(5) . ?
C1 C2 1.385(5) . ?
C1 C7 1.512(5) . ?
C2 C3 1.396(5) . ?
C2 H2 0.9300 . ?
C3 C4 1.385(5) . ?
C3 C11 1.510(5) . ?
C4 C5 1.380(6) . ?
C4 H4 0.9300 . ?
C5 C6 1.372(6) . ?
C5 C15 1.509(6) . ?
C6 H6 0.9300 . ?
C7 N1 1.465(5) . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C8 N2 1.315(5) . ?
C8 N1 1.332(5) . ?
C8 H8 0.9300 . ?
C9 C10 1.354(6) . ?
C9 N2 1.364(6) . ?
C9 H9 0.9300 . ?
C10 N1 1.355(5) . ?
C10 H10 0.9300 . ?
C11 N3 1.457(5) . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
C12 N4 1.308(5) . ?
C12 N3 1.334(5) . ?
C12 H12 0.9300 . ?
C13 C14 1.335(6) . ?
C13 N4 1.375(5) . ?
C13 H13 0.9300 . ?
C14 N3 1.370(5) . ?
C14 H14 0.9300 . ?
C15 N5 1.455(6) . ?
C15 H15A 0.9700 . ?
C15 H15B 0.9700 . ?
C16 N6 1.307(6) . ?
C16 N5 1.336(6) . ?
C16 H16 0.9300 . ?
C17 C18 1.353(7) . ?
C17 N6 1.379(6) . ?
C17 H17 0.9300 . ?
C18 N5 1.350(6) . ?
C18 H18 0.9300 . ?
Cd1 N4 2.290(3) 2_655 ?
Cd1 N4 2.290(3) 4_465 ?
Cd1 N2 2.315(3) . ?
Cd1 N2 2.315(3) 3_565 ?
Cd1 O1W 2.413(4) 3_565 ?
Cd1 O1W 2.413(4) . ?
N4 Cd1 2.290(3) 2_645 ?
O1W H1WA 0.69(4) . ?
O1W H1WB 0.67(6) . ?
O2W H2WA 0.87(3) . ?
O2W H2WB 0.87(3) . ?
O3W H3WA 0.88(3) . ?
O3W H3WB 0.87(3) . ?

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
C6 C1 C2 118.9(4) . . ?
C6 C1 C7 120.2(4) . . ?
C2 C1 C7 120.9(4) . . ?
C1 C2 C3 120.6(4) . . ?
C1 C2 H2 119.7 . . ?
C3 C2 H2 119.7 . . ?
C4 C3 C2 118.7(4) . . ?
C4 C3 C11 121.6(3) . . ?
C2 C3 C11 119.7(4) . . ?
C5 C4 C3 121.2(4) . . ?
C5 C4 H4 119.4 . . ?
C3 C4 H4 119.4 . . ?
C6 C5 C4 119.0(4) . . ?
C6 C5 C15 120.4(4) . . ?
C4 C5 C15 120.5(4) . . ?
C5 C6 C1 121.6(4) . . ?
C5 C6 H6 119.2 . . ?
C1 C6 H6 119.2 . . ?
N1 C7 C1 111.2(3) . . ?
N1 C7 H7A 109.4 . . ?
C1 C7 H7A 109.4 . . ?
N1 C7 H7B 109.4 . . ?
C1 C7 H7B 109.4 . . ?
H7A C7 H7B 108.0 . . ?
N2 C8 N1 111.6(4) . . ?
N2 C8 H8 124.2 . . ?
N1 C8 H8 124.2 . . ?
C10 C9 N2 109.5(4) . . ?
C10 C9 H9 125.2 . . ?
N2 C9 H9 125.2 . . ?
C9 C10 N1 106.3(4) . . ?
C9 C10 H10 126.9 . . ?
N1 C10 H10 126.9 . . ?
N3 C11 C3 112.2(3) . . ?
N3 C11 H11A 109.2 . . ?
C3 C11 H11A 109.2 . . ?
N3 C11 H11B 109.2 . . ?
C3 C11 H11B 109.2 . . ?
H11A C11 H11B 107.9 . . ?
N4 C12 N3 112.5(4) . . ?
N4 C12 H12 123.8 . . ?
N3 C12 H12 123.8 . . ?
C14 C13 N4 109.9(4) . . ?
C14 C13 H13 125.1 . . ?
N4 C13 H13 125.1 . . ?
C13 C14 N3 106.7(4) . . ?
C13 C14 H14 126.6 . . ?
N3 C14 H14 126.6 . . ?
N5 C15 C5 111.8(3) . . ?
N5 C15 H15A 109.3 . . ?
C5 C15 H15A 109.3 . . ?
N5 C15 H15B 109.3 . . ?
C5 C15 H15B 109.3 . . ?
H15A C15 H15B 107.9 . . ?
N6 C16 N5 112.9(4) . . ?
N6 C16 H16 123.5 . . ?
N5 C16 H16 123.5 . . ?
C18 C17 N6 109.2(4) . . ?
C18 C17 H17 125.4 . . ?
N6 C17 H17 125.4 . . ?
N5 C18 C17 107.0(4) . . ?
N5 C18 H18 126.5 . . ?
C17 C18 H18 126.5 . . ?
N4 Cd1 N4 180.0(2) 2_655 4_465 ?
N4 Cd1 N2 91.96(12) 2_655 . ?
N4 Cd1 N2 88.04(12) 4_465 . ?
N4 Cd1 N2 88.04(12) 2_655 3_565 ?
N4 Cd1 N2 91.96(12) 4_465 3_565 ?
N2 Cd1 N2 180.0 . 3_565 ?
N4 Cd1 O1W 90.60(13) 2_655 3_565 ?
N4 Cd1 O1W 89.40(13) 4_465 3_565 ?
N2 Cd1 O1W 91.56(15) . 3_565 ?
N2 Cd1 O1W 88.44(15) 3_565 3_565 ?
N4 Cd1 O1W 89.40(13) 2_655 . ?
N4 Cd1 O1W 90.60(13) 4_465 . ?
N2 Cd1 O1W 88.44(15) . . ?
N2 Cd1 O1W 91.56(15) 3_565 . ?
O1W Cd1 O1W 180.0(2) 3_565 . ?
C8 N1 C10 107.3(3) . . ?
C8 N1 C7 128.0(4) . . ?
C10 N1 C7 124.6(3) . . ?
C8 N2 C9 105.3(3) . . ?
C8 N2 Cd1 126.6(3) . . ?
C9 N2 Cd1 127.5(3) . . ?
C12 N3 C14 106.2(3) . . ?
C12 N3 C11 126.3(4) . . ?
C14 N3 C11 126.3(4) . . ?
C12 N4 C13 104.8(4) . . ?
C12 N4 Cd1 129.0(3) . 2_645 ?
C13 N4 Cd1 125.7(3) . 2_645 ?
C16 N5 C18 106.4(4) . . ?
C16 N5 C15 127.1(4) . . ?
C18 N5 C15 126.4(4) . . ?
C16 N6 C17 104.4(4) . . ?
Cd1 O1W H1WA 118(4) . . ?
Cd1 O1W H1WB 121(5) . . ?
H1WA O1W H1WB 113(7) . . ?
H2WA O2W H2WB 113(4) . . ?
H3WA O3W H3WB 113(4) . . ?

_diffrn_measured_fraction_theta_max 0.997
_diffrn_reflns_theta_full        26.00
_diffrn_measured_fraction_theta_full 0.997
_refine_diff_density_max         1.332
_refine_diff_density_min         -0.605
_refine_diff_density_rms         0.083

#====END

data_6
_database_code_depnum_ccdc_archive 'CCDC 679262'
_audit_creation_date             'Sun Aug 19 14:41:50 2007'
_audit_creation_method           SHELXL-97
_publ_section_references         
;
Molecular Structure Corporation, Rigaku Corporation. (2004). teXsan.
Single Crystal Structure Analysis Software. Version 2.0.
MSC, 9009 New Trails Drive, The Woodlands, TX 77381-5209, USA.
Rigaku, 3-9-12 Akishima, Tokyo, Japan.
;
_chemical_name_systematic        
;
[Cd(XG4)2][Cd2I6]?
;
_chemical_name_common            (Cd(XG4)2)(Cd2I6)?
_chemical_melting_point          ?
_chemical_formula_moiety         'C36 H36 Cd3 I6 N12 '
_chemical_formula_sum            'C36 H36 Cd3 I6 N12'
_chemical_formula_weight         1735.37

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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'

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_Int_Tables_number      2
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   9.795(5)
_cell_length_b                   11.219(6)
_cell_length_c                   13.129(6)
_cell_angle_alpha                64.551(16)
_cell_angle_beta                 67.682(16)
_cell_angle_gamma                74.765(19)
_cell_volume                     1196.5(10)
_cell_formula_units_Z            1
_cell_measurement_temperature    200
_cell_measurement_reflns_used    7980
_cell_measurement_theta_min      3.2
_cell_measurement_theta_max      27.5

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.250
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.200
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.408
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             798
_exptl_absorpt_coefficient_mu    5.231
_exptl_absorpt_correction_type   none

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      200
_diffrn_radiation_wavelength     0.71075
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Rigaku RAXIS-RAPID Imaging Plate'
_diffrn_measurement_method       ω
_diffrn_detector_area_resol_mean 10.00
_diffrn_reflns_number            11326
_diffrn_reflns_av_R_equivalents  0.0712
_diffrn_reflns_av_sigmaI/netI    0.0753
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         3.17
_diffrn_reflns_theta_max         27.48
_reflns_number_total             5423
_reflns_number_gt                4645
_reflns_threshold_expression     I>2σ(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1985)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
;
Refinement of F² against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F², conventional R-factors R are based
on F, with F set to zero for negative F². The threshold expression of
F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F² are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0313P)²+0.7585P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         5423
_refine_ls_number_parameters     259
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0477
_refine_ls_R_factor_gt           0.0397
_refine_ls_wR_factor_ref         0.0938
_refine_ls_wR_factor_gt          0.0899
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_restrained_S_all      1.040
_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
I1 I 0.82603(3) -0.12519(3) 0.58171(3) 0.03222(10) Uani 1 1 d . . .
I2 I 0.75285(4) 0.24333(3) 0.66839(3) 0.03908(11) Uani 1 1 d . . .
I3 I 1.06704(4) -0.14216(4) 0.82048(3) 0.04388(12) Uani 1 1 d . . .
Cd1 Cd 0.5000 0.5000 0.0000 0.01759(11) Uani 1 2 d S . .
Cd2 Cd 0.95552(4) 0.02991(4) 0.64238(3) 0.03146(11) Uani 1 1 d . . .
N11 N 0.5428(4) 0.3205(4) 0.3652(3) 0.0226(9) Uani 1 1 d . . .
N12 N 0.5431(4) 0.4439(4) 0.1815(3) 0.0227(8) Uani 1 1 d . . .
N31 N 0.3808(4) -0.0656(4) 0.9256(3) 0.0229(8) Uani 1 1 d . . .
N32 N 0.4854(4) -0.2736(4) 0.9616(3) 0.0228(8) Uani 1 1 d . . .
N51 N -0.0428(4) 0.4889(4) 0.7516(3) 0.0243(9) Uani 1 1 d . . .
N52 N -0.2444(4) 0.4950(4) 0.8994(3) 0.0261(9) Uani 1 1 d . . .
C1 C 0.3965(5) 0.2270(5) 0.5786(4) 0.0233(10) Uani 1 1 d . . .
C2 C 0.3903(5) 0.1307(5) 0.6921(4) 0.0238(10) Uani 1 1 d . . .
H1 H 0.4637 0.0555 0.7015 0.029 Uiso 1 1 calc R . .
C3 C 0.2774(5) 0.1453(4) 0.7903(3) 0.0198(9) Uani 1 1 d . . .
C4 C 0.1694(5) 0.2545(5) 0.7755(4) 0.0234(10) Uani 1 1 d . . .
H2 H 0.0920 0.2648 0.8429 0.028 Uiso 1 1 calc R . .
C5 C 0.1731(5) 0.3487(4) 0.6637(4) 0.0234(10) Uani 1 1 d . . .
C6 C 0.2876(5) 0.3339(4) 0.5656(3) 0.0219(10) Uani 1 1 d . . .
H3 H 0.2908 0.3983 0.4887 0.026 Uiso 1 1 calc R . .
C11 C 0.5259(5) 0.2053(5) 0.4757(4) 0.0328(12) Uani 1 1 d . . .
H4 H 0.6188 0.1817 0.4971 0.039 Uiso 1 1 calc R . .
H5 H 0.5118 0.1290 0.4631 0.039 Uiso 1 1 calc R . .
C12 C 0.5199(5) 0.3272(5) 0.2675(4) 0.0221(9) Uani 1 1 d . . .
H6 H 0.4907 0.2566 0.2616 0.027 Uiso 1 1 calc R . .
C13 C 0.5833(5) 0.5155(5) 0.2265(4) 0.0273(10) Uani 1 1 d . . .
H7 H 0.6066 0.6044 0.1849 0.033 Uiso 1 1 calc R . .
C14 C 0.5847(5) 0.4394(5) 0.3397(4) 0.0307(11) Uani 1 1 d . . .
H8 H 0.6096 0.4642 0.3906 0.037 Uiso 1 1 calc R . .
C31 C 0.2648(5) 0.0479(5) 0.9161(4) 0.0275(11) Uani 1 1 d . . .
H9 H 0.2682 0.0960 0.9629 0.033 Uiso 1 1 calc R . .
H10 H 0.1668 0.0143 0.9518 0.033 Uiso 1 1 calc R . .
C32 C 0.3605(5) -0.1930(5) 0.9628(4) 0.0242(10) Uani 1 1 d . . .
H11 H 0.2662 -0.2220 0.9874 0.029 Uiso 1 1 calc R . .
C33 C 0.5927(5) -0.1907(5) 0.9198(4) 0.0244(10) Uani 1 1 d . . .
H12 H 0.6960 -0.2195 0.9074 0.029 Uiso 1 1 calc R . .
C34 C 0.5311(5) -0.0641(5) 0.8992(4) 0.0269(10) Uani 1 1 d . . .
H13 H 0.5807 0.0113 0.8721 0.032 Uiso 1 1 calc R . .
C51 C 0.0544(5) 0.4685(5) 0.6434(4) 0.0314(12) Uani 1 1 d . . .
H14 H 0.1040 0.5493 0.5889 0.038 Uiso 1 1 calc R . .
H15 H -0.0069 0.4564 0.6042 0.038 Uiso 1 1 calc R . .
C52 C -0.1871(5) 0.4696(5) 0.8010(4) 0.0242(10) Uani 1 1 d . . .
H16 H -0.2404 0.4417 0.7694 0.029 Uiso 1 1 calc R . .
C53 C -0.1324(5) 0.5306(5) 0.9134(4) 0.0297(11) Uani 1 1 d . . .
H17 H -0.1411 0.5536 0.9774 0.036 Uiso 1 1 calc R . .
C54 C -0.0066(5) 0.5285(5) 0.8226(4) 0.0303(11) Uani 1 1 d . . .
H18 H 0.0873 0.5501 0.8106 0.036 Uiso 1 1 calc R . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
I1 Cd2 2.8451(12) 2_756 ?
I1 Cd2 2.8964(11) . ?
I2 Cd2 2.7350(12) . ?
I3 Cd2 2.7091(11) . ?
Cd1 N32 2.343(4) 1_564 ?
Cd1 N32 2.343(4) 2_656 ?
Cd1 N52 2.344(4) 1_654 ?
Cd1 N52 2.344(4) 2_566 ?
Cd1 N12 2.364(4) . ?
Cd1 N12 2.364(4) 2_665 ?
Cd2 I1 2.8451(12) 2_756 ?
N11 C12 1.352(5) . ?
N11 C14 1.364(7) . ?
N11 C11 1.457(6) . ?
N12 C12 1.316(6) . ?
N12 C13 1.378(6) . ?
N31 C32 1.341(6) . ?
N31 C34 1.382(6) . ?
N31 C31 1.462(6) . ?
N32 C32 1.316(6) . ?
N32 C33 1.381(6) . ?
N32 Cd1 2.343(4) 1_546 ?
N51 C52 1.346(6) . ?
N51 C54 1.371(6) . ?
N51 C51 1.454(6) . ?
N52 C52 1.322(6) . ?
N52 C53 1.358(6) . ?
N52 Cd1 2.344(4) 1_456 ?
C1 C6 1.377(6) . ?
C1 C2 1.405(6) . ?
C1 C11 1.519(6) . ?
C2 C3 1.384(6) . ?
C2 H1 0.9500 . ?
C3 C4 1.389(6) . ?
C3 C31 1.517(5) . ?
C4 C5 1.385(6) . ?
C4 H2 0.9500 . ?
C5 C6 1.391(6) . ?
C5 C51 1.529(6) . ?
C6 H3 0.9500 . ?
C11 H4 0.9900 . ?
C11 H5 0.9900 . ?
C12 H6 0.9500 . ?
C13 C14 1.362(7) . ?
C13 H7 0.9500 . ?
C14 H8 0.9500 . ?
C31 H9 0.9900 . ?
C31 H10 0.9900 . ?
C32 H11 0.9500 . ?
C33 C34 1.342(7) . ?
C33 H12 0.9500 . ?
C34 H13 0.9500 . ?
C51 H14 0.9900 . ?
C51 H15 0.9900 . ?
C52 H16 0.9500 . ?
C53 C54 1.354(7) . ?
C53 H17 0.9500 . ?
C54 H18 0.9500 . ?

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
Cd2 I1 Cd2 83.30(4) 2_756 . ?
N32 Cd1 N32 180.0 1_564 2_656 ?
N32 Cd1 N52 89.99(14) 1_564 1_654 ?
N32 Cd1 N52 90.01(14) 2_656 1_654 ?
N32 Cd1 N52 90.01(14) 1_564 2_566 ?
N32 Cd1 N52 89.99(14) 2_656 2_566 ?
N52 Cd1 N52 180.000(1) 1_654 2_566 ?
N32 Cd1 N12 90.30(13) 1_564 . ?
N32 Cd1 N12 89.70(13) 2_656 . ?
N52 Cd1 N12 91.28(13) 1_654 . ?
N52 Cd1 N12 88.72(13) 2_566 . ?
N32 Cd1 N12 89.70(13) 1_564 2_665 ?
N32 Cd1 N12 90.30(13) 2_656 2_665 ?
N52 Cd1 N12 88.72(13) 1_654 2_665 ?
N52 Cd1 N12 91.27(13) 2_566 2_665 ?
N12 Cd1 N12 180.0 . 2_665 ?
I3 Cd2 I2 120.82(3) . . ?
I3 Cd2 I1 114.45(4) . 2_756 ?
I2 Cd2 I1 107.03(3) . 2_756 ?
I3 Cd2 I1 106.96(4) . . ?
I2 Cd2 I1 108.01(4) . . ?
I1 Cd2 I1 96.70(4) 2_756 . ?
C12 N11 C14 107.4(4) . . ?
C12 N11 C11 125.1(4) . . ?
C14 N11 C11 127.5(4) . . ?
C12 N12 C13 105.5(4) . . ?
C12 N12 Cd1 121.8(3) . . ?
C13 N12 Cd1 132.6(3) . . ?
C32 N31 C34 106.5(4) . . ?
C32 N31 C31 126.0(4) . . ?
C34 N31 C31 127.5(4) . . ?
C32 N32 C33 104.3(4) . . ?
C32 N32 Cd1 122.7(3) . 1_546 ?
C33 N32 Cd1 132.4(3) . 1_546 ?
C52 N51 C54 107.5(4) . . ?
C52 N51 C51 124.9(4) . . ?
C54 N51 C51 127.6(4) . . ?
C52 N52 C53 106.2(4) . . ?
C52 N52 Cd1 121.4(3) . 1_456 ?
C53 N52 Cd1 131.8(3) . 1_456 ?
C6 C1 C2 119.5(4) . . ?
C6 C1 C11 123.6(4) . . ?
C2 C1 C11 116.8(4) . . ?
C3 C2 C1 120.1(4) . . ?
C3 C2 H1 120.0 . . ?
C1 C2 H1 120.0 . . ?
C2 C3 C4 119.5(4) . . ?
C2 C3 C31 123.4(4) . . ?
C4 C3 C31 117.1(4) . . ?
C5 C4 C3 120.8(4) . . ?
C5 C4 H2 119.6 . . ?
C3 C4 H2 119.6 . . ?
C4 C5 C6 119.3(4) . . ?
C4 C5 C51 122.4(4) . . ?
C6 C5 C51 118.3(4) . . ?
C1 C6 C5 120.7(4) . . ?
C1 C6 H3 119.6 . . ?
C5 C6 H3 119.6 . . ?
N11 C11 C1 113.8(4) . . ?
N11 C11 H4 108.8 . . ?
C1 C11 H4 108.8 . . ?
N11 C11 H5 108.8 . . ?
C1 C11 H5 108.8 . . ?
H4 C11 H5 107.7 . . ?
N12 C12 N11 111.4(4) . . ?
N12 C12 H6 124.3 . . ?
N11 C12 H6 124.3 . . ?
C14 C13 N12 109.7(4) . . ?
C14 C13 H7 125.1 . . ?
N12 C13 H7 125.1 . . ?
C13 C14 N11 106.0(4) . . ?
C13 C14 H8 127.0 . . ?
N11 C14 H8 127.0 . . ?
N31 C31 C3 114.4(4) . . ?
N31 C31 H9 108.7 . . ?
C3 C31 H9 108.7 . . ?
N31 C31 H10 108.7 . . ?
C3 C31 H10 108.7 . . ?
H9 C31 H10 107.6 . . ?
N32 C32 N31 112.5(4) . . ?
N32 C32 H11 123.7 . . ?
N31 C32 H11 123.7 . . ?
C34 C33 N32 110.7(4) . . ?
C34 C33 H12 124.7 . . ?
N32 C33 H12 124.7 . . ?
C33 C34 N31 105.9(4) . . ?
C33 C34 H13 127.0 . . ?
N31 C34 H13 127.0 . . ?
N51 C51 C5 113.7(4) . . ?
N51 C51 H14 108.8 . . ?
C5 C51 H14 108.8 . . ?
N51 C51 H15 108.8 . . ?
C5 C51 H15 108.8 . . ?
H14 C51 H15 107.7 . . ?
N52 C52 N51 110.5(4) . . ?
N52 C52 H16 124.8 . . ?
N51 C52 H16 124.8 . . ?
C54 C53 N52 110.1(4) . . ?
C54 C53 H17 125.0 . . ?
N52 C53 H17 125.0 . . ?
C53 C54 N51 105.7(4) . . ?
C53 C54 H18 127.1 . . ?
N51 C54 H18 127.1 . . ?

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
Cd2 I1 Cd2 I3 -118.13(4) 2_756 . . . ?
Cd2 I1 Cd2 I2 110.38(3) 2_756 . . . ?
Cd2 I1 Cd2 I1 0.0 2_756 . . 2_756 ?
N32 Cd1 N12 C12 159.8(3) 1_564 . . . ?
N32 Cd1 N12 C12 -20.2(3) 2_656 . . . ?
N52 Cd1 N12 C12 -110.2(3) 1_654 . . . ?
N52 Cd1 N12 C12 69.8(3) 2_566 . . . ?
N32 Cd1 N12 C13 -15.2(4) 1_564 . . . ?
N32 Cd1 N12 C13 164.8(4) 2_656 . . . ?
N52 Cd1 N12 C13 74.7(4) 1_654 . . . ?
N52 Cd1 N12 C13 -105.3(4) 2_566 . . . ?
C6 C1 C2 C3 -1.6(7) . . . . ?
C11 C1 C2 C3 178.6(5) . . . . ?
C1 C2 C3 C4 1.0(7) . . . . ?
C1 C2 C3 C31 -178.4(5) . . . . ?
C2 C3 C4 C5 0.2(7) . . . . ?
C31 C3 C4 C5 179.6(5) . . . . ?
C3 C4 C5 C6 -0.7(7) . . . . ?
C3 C4 C5 C51 178.5(5) . . . . ?
C2 C1 C6 C5 1.0(7) . . . . ?
C11 C1 C6 C5 -179.2(5) . . . . ?
C4 C5 C6 C1 0.1(7) . . . . ?
C51 C5 C6 C1 -179.2(5) . . . . ?
C12 N11 C11 C1 -112.1(5) . . . . ?
C14 N11 C11 C1 68.3(6) . . . . ?
C6 C1 C11 N11 12.1(7) . . . . ?
C2 C1 C11 N11 -168.2(4) . . . . ?
C13 N12 C12 N11 0.1(5) . . . . ?
Cd1 N12 C12 N11 -176.1(3) . . . . ?
C14 N11 C12 N12 -0.6(5) . . . . ?
C11 N11 C12 N12 179.7(4) . . . . ?
C12 N12 C13 C14 0.4(5) . . . . ?
Cd1 N12 C13 C14 176.1(3) . . . . ?
N12 C13 C14 N11 -0.8(5) . . . . ?
C12 N11 C14 C13 0.9(5) . . . . ?
C11 N11 C14 C13 -179.5(4) . . . . ?
C32 N31 C31 C3 -114.1(5) . . . . ?
C34 N31 C31 C3 66.3(6) . . . . ?
C2 C3 C31 N31 -1.3(7) . . . . ?
C4 C3 C31 N31 179.3(4) . . . . ?
C33 N32 C32 N31 -0.3(5) . . . . ?
Cd1 N32 C32 N31 -173.0(3) 1_546 . . . ?
C34 N31 C32 N32 -0.6(5) . . . . ?
C31 N31 C32 N32 179.7(4) . . . . ?
C32 N32 C33 C34 1.2(5) . . . . ?
Cd1 N32 C33 C34 172.9(3) 1_546 . . . ?
N32 C33 C34 N31 -1.6(5) . . . . ?
C32 N31 C34 C33 1.3(5) . . . . ?
C31 N31 C34 C33 -179.0(4) . . . . ?
C52 N51 C51 C5 -110.1(5) . . . . ?
C54 N51 C51 C5 68.9(6) . . . . ?
C4 C5 C51 N51 12.1(7) . . . . ?
C6 C5 C51 N51 -168.7(4) . . . . ?
C53 N52 C52 N51 -0.5(5) . . . . ?
Cd1 N52 C52 N51 172.1(3) 1_456 . . . ?
C54 N51 C52 N52 0.1(5) . . . . ?
C51 N51 C52 N52 179.2(4) . . . . ?
C52 N52 C53 C54 0.7(5) . . . . ?
Cd1 N52 C53 C54 -170.8(3) 1_456 . . . ?
N52 C53 C54 N51 -0.7(5) . . . . ?
C52 N51 C54 C53 0.4(5) . . . . ?
C51 N51 C54 C53 -178.8(4) . . . . ?

_diffrn_measured_fraction_theta_max 0.988
_diffrn_reflns_theta_full        27.48
_diffrn_measured_fraction_theta_full 0.988
_refine_diff_density_max         1.019
_refine_diff_density_min         -1.348
_refine_diff_density_rms         0.201

#====END


