# 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              
;
Cadmium(II) coordination polymers with flexible
tetradentate ligand 1,2,4,5-tetrakis(imidazol-1-ylmethyl)benzene: anion
effect and reversible anion exchange property
;
loop_
_publ_author_name
'Wei-Yin Sun.'
'Yu-Jie Ding.'
'Qin Hua.'
'Yong-Qing Huang.'
;
Guang-Xiang Liu
;
'Takaaki Okamura'
'Norikazu Ueyama'
'Guan-Cheng Xu.'

# Attachment 'sunwy-cif.cif'

data_L
_database_code_depnum_ccdc_archive 'CCDC 687822'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C22 H22 N8, 4(H2 O)'
_chemical_formula_sum            'C22 H30 N8 O4'
_chemical_formula_weight         470.54

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   '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                   7.3641(18)
_cell_length_b                   18.938(5)
_cell_length_c                   8.707(2)
_cell_angle_alpha                90.00
_cell_angle_beta                 97.859(4)
_cell_angle_gamma                90.00
_cell_volume                     1202.8(5)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    834
_cell_measurement_theta_min      2.99
_cell_measurement_theta_max      27.42

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.20
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.299
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             500
_exptl_absorpt_coefficient_mu    0.093
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.9727
_exptl_absorpt_correction_T_max  0.9817
_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            5831
_diffrn_reflns_av_R_equivalents  0.0218
_diffrn_reflns_av_sigmaI/netI    0.0234
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_theta_min         2.15
_diffrn_reflns_theta_max         25.00
_reflns_number_total             2114
_reflns_number_gt                1984
_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)+(0.0825P)²+0.2777P] 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         2114
_refine_ls_number_parameters     170
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0466
_refine_ls_R_factor_gt           0.0436
_refine_ls_wR_factor_ref         0.1273
_refine_ls_wR_factor_gt          0.1242
_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 0.07390(18) 0.43738(7) 0.55488(17) 0.0325(3) Uani 1 1 d . . .
H1 H 0.1246 0.3947 0.5922 0.039 Uiso 1 1 calc R . .
C2 C 0.10669(18) 0.49719(7) 0.64601(16) 0.0309(3) Uani 1 1 d . . .
C3 C 0.03147(18) 0.56131(7) 0.58970(17) 0.0313(3) Uani 1 1 d . . .
C4 C 0.21150(19) 0.48898(9) 0.80693(17) 0.0385(4) Uani 1 1 d . . .
H4A H 0.2113 0.5338 0.8609 0.046 Uiso 1 1 calc R . .
H4B H 0.1490 0.4547 0.8639 0.046 Uiso 1 1 calc R . .
C5 C 0.4739(2) 0.40456(10) 0.8569(2) 0.0497(4) Uani 1 1 d . . .
H5 H 0.4076 0.3681 0.8944 0.060 Uiso 1 1 calc R . .
C6 C 0.6883(2) 0.46427(11) 0.7875(2) 0.0574(5) Uani 1 1 d . . .
H6 H 0.8040 0.4777 0.7670 0.069 Uiso 1 1 calc R . .
C7 C 0.5386(2) 0.50479(10) 0.7612(2) 0.0539(5) Uani 1 1 d . . .
H7 H 0.5310 0.5502 0.7202 0.065 Uiso 1 1 calc R . .
C8 C 0.0647(2) 0.63024(8) 0.67639(19) 0.0392(4) Uani 1 1 d . . .
H8A H -0.0243 0.6649 0.6320 0.047 Uiso 1 1 calc R . .
H8B H 0.0480 0.6233 0.7839 0.047 Uiso 1 1 calc R . .
C9 C 0.3650(2) 0.68513(9) 0.7854(2) 0.0456(4) Uani 1 1 d . . .
H9 H 0.3384 0.6898 0.8862 0.055 Uiso 1 1 calc R . .
C10 C 0.5007(3) 0.68965(10) 0.5866(2) 0.0531(5) Uani 1 1 d . . .
H10 H 0.5895 0.6981 0.5224 0.064 Uiso 1 1 calc R . .
C11 C 0.3358(2) 0.66022(9) 0.5405(2) 0.0490(4) Uani 1 1 d . . .
H11 H 0.2902 0.6452 0.4409 0.059 Uiso 1 1 calc R . .
H1W H 0.080(4) 0.2366(14) 0.574(3) 0.084(8) Uiso 1 1 d . . .
H2W H 0.245(4) 0.2453(14) 0.676(3) 0.090(8) Uiso 1 1 d . . .
H3W H 0.875(4) 0.3396(15) 0.882(3) 0.093(9) Uiso 1 1 d . . .
H4W H 1.024(4) 0.3047(15) 0.817(4) 0.098(9) Uiso 1 1 d . . .
N1 N 0.40042(16) 0.46627(7) 0.80628(14) 0.0356(3) Uani 1 1 d . . .
N2 N 0.64923(19) 0.40119(9) 0.84770(18) 0.0551(4) Uani 1 1 d . . .
N3 N 0.24932(17) 0.65683(6) 0.66895(14) 0.0362(3) Uani 1 1 d . . .
N4 N 0.5190(2) 0.70536(8) 0.74096(18) 0.0539(4) Uani 1 1 d . . .
O1W O 0.13435(19) 0.26349(7) 0.64908(17) 0.0522(4) Uani 1 1 d . . .
O2W O 0.9859(2) 0.32355(9) 0.90171(19) 0.0665(4) Uani 1 1 d . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 C2 1.385(2) . ?
C1 C3 1.386(2) 3_566 ?
C1 H1 0.9300 . ?
C2 C3 1.395(2) . ?
C2 C4 1.512(2) . ?
C3 C1 1.386(2) 3_566 ?
C3 C8 1.511(2) . ?
C4 N1 1.4569(19) . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
C5 N2 1.306(2) . ?
C5 N1 1.337(2) . ?
C5 H5 0.9300 . ?
C6 C7 1.337(3) . ?
C6 N2 1.351(3) . ?
C6 H6 0.9300 . ?
C7 N1 1.353(2) . ?
C7 H7 0.9300 . ?
C8 N3 1.460(2) . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C9 N4 1.305(2) . ?
C9 N3 1.343(2) . ?
C9 H9 0.9300 . ?
C10 C11 1.347(3) . ?
C10 N4 1.365(2) . ?
C10 H10 0.9300 . ?
C11 N3 1.362(2) . ?
C11 H11 0.9300 . ?
O1W H1W 0.88(3) . ?
O1W H2W 0.88(3) . ?
O2W H3W 0.86(3) . ?
O2W H4W 0.90(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
C2 C1 C3 122.53(13) . 3_566 ?
C2 C1 H1 118.7 . . ?
C3 C1 H1 118.7 3_566 . ?
C1 C2 C3 118.72(13) . . ?
C1 C2 C4 118.27(13) . . ?
C3 C2 C4 122.87(13) . . ?
C1 C3 C2 118.74(13) 3_566 . ?
C1 C3 C8 118.06(13) 3_566 . ?
C2 C3 C8 123.16(13) . . ?
N1 C4 C2 113.16(12) . . ?
N1 C4 H4A 108.9 . . ?
C2 C4 H4A 108.9 . . ?
N1 C4 H4B 108.9 . . ?
C2 C4 H4B 108.9 . . ?
H4A C4 H4B 107.8 . . ?
N2 C5 N1 112.42(16) . . ?
N2 C5 H5 123.8 . . ?
N1 C5 H5 123.8 . . ?
C7 C6 N2 111.07(16) . . ?
C7 C6 H6 124.5 . . ?
N2 C6 H6 124.5 . . ?
C6 C7 N1 106.02(16) . . ?
C6 C7 H7 127.0 . . ?
N1 C7 H7 127.0 . . ?
N3 C8 C3 111.34(12) . . ?
N3 C8 H8A 109.4 . . ?
C3 C8 H8A 109.4 . . ?
N3 C8 H8B 109.4 . . ?
C3 C8 H8B 109.4 . . ?
H8A C8 H8B 108.0 . . ?
N4 C9 N3 112.40(16) . . ?
N4 C9 H9 123.8 . . ?
N3 C9 H9 123.8 . . ?
C11 C10 N4 110.34(16) . . ?
C11 C10 H10 124.8 . . ?
N4 C10 H10 124.8 . . ?
C10 C11 N3 106.16(15) . . ?
C10 C11 H11 126.9 . . ?
N3 C11 H11 126.9 . . ?
C5 N1 C7 106.29(14) . . ?
C5 N1 C4 126.89(14) . . ?
C7 N1 C4 126.75(14) . . ?
C5 N2 C6 104.19(15) . . ?
C9 N3 C11 106.33(14) . . ?
C9 N3 C8 127.07(14) . . ?
C11 N3 C8 126.55(13) . . ?
C9 N4 C10 104.77(14) . . ?
H1W O1W H2W 106(2) . . ?
H3W O2W H4W 112(3) . . ?

_diffrn_measured_fraction_theta_max 0.995
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.995
_refine_diff_density_max         0.149
_refine_diff_density_min         -0.205
_refine_diff_density_rms         0.042

#====END

data_1
_database_code_depnum_ccdc_archive 'CCDC 687823'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C66 H78 Cd2 N28 O18'
_chemical_formula_sum            'C66 H78 Cd2 N28 O18'
_chemical_formula_weight         1776.36

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

_symmetry_cell_setting           trigonal
_symmetry_space_group_name_H-M   '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                   21.5594(12)
_cell_length_b                   21.5594(12)
_cell_length_c                   14.9195(16)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_volume                     6005.6(8)
_cell_formula_units_Z            3
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    3272
_cell_measurement_theta_min      2.57
_cell_measurement_theta_max      25.65

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.07
_exptl_crystal_size_mid          0.06
_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             2730
_exptl_absorpt_coefficient_mu    0.614
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.9582
_exptl_absorpt_correction_T_max  0.9758
_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            12015
_diffrn_reflns_av_R_equivalents  0.0344
_diffrn_reflns_av_sigmaI/netI    0.0356
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         1.75
_diffrn_reflns_theta_max         27.50
_reflns_number_total             3061
_reflns_number_gt                2590
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
;
Refinement of 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)+(0.1367P)²+46.3566P] 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         3061
_refine_ls_number_parameters     160
_refine_ls_number_restraints     7
_refine_ls_R_factor_all          0.0797
_refine_ls_R_factor_gt           0.0691
_refine_ls_wR_factor_ref         0.2287
_refine_ls_wR_factor_gt          0.2181
_refine_ls_goodness_of_fit_ref   1.000
_refine_ls_restrained_S_all      1.005
_refine_ls_shift/su_max          0.005
_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 0.0000 0.0000 -0.5000 0.0447(3) Uani 1 6 d S . .
Cd2 Cd 0.3333 0.6667 -0.3333 0.0277(3) Uani 1 6 d S . .
N1 N 0.2582(3) 0.4586(2) -0.4747(3) 0.0465(11) Uani 1 1 d . . .
N2 N 0.3118(2) 0.5688(2) -0.4230(3) 0.0407(9) Uani 1 1 d . . .
N3 N 0.1749(2) 0.1648(2) -0.6712(3) 0.0416(10) Uani 1 1 d . . .
N4 N 0.1011(3) 0.0719(2) -0.5893(4) 0.0489(11) Uani 1 1 d . . .
C1 C 0.1845(3) 0.3584(2) -0.5794(3) 0.0428(12) Uani 1 1 d . . .
C2 C 0.1990(3) 0.3075(3) -0.6126(4) 0.0474(13) Uani 1 1 d . . .
H2A H 0.2212 0.2900 -0.5751 0.057 Uiso 1 1 calc R . .
C3 C 0.1822(3) 0.2812(2) -0.6984(3) 0.0425(11) Uani 1 1 d . . .
C4 C 0.2041(4) 0.3825(3) -0.4821(4) 0.0557(15) Uani 1 1 d . . .
H4A H 0.1613 0.3738 -0.4500 0.067 Uiso 1 1 calc R . .
H4B H 0.2222 0.3542 -0.4539 0.067 Uiso 1 1 calc R . .
C5 C 0.2552(3) 0.5046(3) -0.4164(3) 0.0451(12) Uani 1 1 d . . .
H5A H 0.2177 0.4925 -0.3764 0.054 Uiso 1 1 calc R . .
C6 C 0.3527(3) 0.5635(3) -0.4895(4) 0.0505(13) Uani 1 1 d . . .
H6A H 0.3964 0.6008 -0.5094 0.061 Uiso 1 1 calc R . .
C7 C 0.3198(4) 0.4959(3) -0.5217(4) 0.0574(15) Uani 1 1 d . . .
H7A H 0.3362 0.4784 -0.5673 0.069 Uiso 1 1 calc R . .
C8 C 0.2033(3) 0.2277(3) -0.7298(4) 0.0485(12) Uani 1 1 d . . .
H8A H 0.1855 0.2124 -0.7902 0.058 Uiso 1 1 calc R . .
H8B H 0.2551 0.2506 -0.7314 0.058 Uiso 1 1 calc R . .
C9 C 0.1077(3) 0.1244(3) -0.6409(4) 0.0506(13) Uani 1 1 d . . .
H9A H 0.0703 0.1325 -0.6547 0.061 Uiso 1 1 calc R . .
C10 C 0.1670(4) 0.0786(4) -0.5890(5) 0.0620(17) Uani 1 1 d . . .
H10A H 0.1788 0.0481 -0.5589 0.074 Uiso 1 1 calc R . .
C11 C 0.2127(3) 0.1349(4) -0.6376(5) 0.0613(16) Uani 1 1 d . . .
H11A H 0.2610 0.1507 -0.6469 0.074 Uiso 1 1 calc R . .
N5 N 0.3022(9) 0.3716(9) -0.2850(7) 0.155(6) Uiso 0.67 1 d PD . .
O1 O 0.3594(8) 0.4087(9) -0.3201(10) 0.173(6) Uiso 0.67 1 d PD . .
O2 O 0.2684(13) 0.4030(13) -0.2636(17) 0.313(13) Uiso 0.67 1 d PD . .
O3 O 0.2759(14) 0.3117(11) -0.2695(17) 0.377(19) Uiso 0.67 1 d PD . .
O1W O 0.4556(13) 0.4816(13) -0.4293(15) 0.362(11) Uiso 1 1 d . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cd1 N4 2.356(5) 12_554 ?
Cd1 N4 2.356(5) 3 ?
Cd1 N4 2.356(5) 10_554 ?
Cd1 N4 2.356(5) . ?
Cd1 N4 2.356(5) 11_554 ?
Cd1 N4 2.356(5) 2 ?
Cd2 N2 2.341(4) . ?
Cd2 N2 2.341(4) 13_564 ?
Cd2 N2 2.341(4) 14_454 ?
Cd2 N2 2.341(4) 2_665 ?
Cd2 N2 2.341(4) 15_554 ?
Cd2 N2 2.341(4) 3_565 ?
N1 C5 1.344(7) . ?
N1 C7 1.354(8) . ?
N1 C4 1.466(7) . ?
N2 C5 1.314(7) . ?
N2 C6 1.369(7) . ?
N3 C9 1.341(8) . ?
N3 C11 1.363(8) . ?
N3 C8 1.465(7) . ?
N4 C9 1.318(8) . ?
N4 C10 1.353(8) . ?
C1 C2 1.375(8) . ?
C1 C3 1.401(8) 16_553 ?
C1 C4 1.529(7) . ?
C2 C3 1.373(7) . ?
C2 H2A 0.9300 . ?
C3 C1 1.401(8) 16_553 ?
C3 C8 1.510(7) . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
C5 H5A 0.9300 . ?
C6 C7 1.351(8) . ?
C6 H6A 0.9300 . ?
C7 H7A 0.9300 . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C9 H9A 0.9300 . ?
C10 C11 1.332(9) . ?
C10 H10A 0.9300 . ?
C11 H11A 0.9300 . ?
N5 O3 1.146(18) . ?
N5 O1 1.204(15) . ?
N5 O2 1.258(17) . ?

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
N4 Cd1 N4 179.999(1) 12_554 3 ?
N4 Cd1 N4 91.18(18) 12_554 10_554 ?
N4 Cd1 N4 88.82(18) 3 10_554 ?
N4 Cd1 N4 88.82(18) 12_554 . ?
N4 Cd1 N4 91.18(18) 3 . ?
N4 Cd1 N4 180.0 10_554 . ?
N4 Cd1 N4 91.18(18) 12_554 11_554 ?
N4 Cd1 N4 88.83(18) 3 11_554 ?
N4 Cd1 N4 91.17(18) 10_554 11_554 ?
N4 Cd1 N4 88.82(18) . 11_554 ?
N4 Cd1 N4 88.83(18) 12_554 2 ?
N4 Cd1 N4 91.17(18) 3 2 ?
N4 Cd1 N4 88.83(18) 10_554 2 ?
N4 Cd1 N4 91.18(18) . 2 ?
N4 Cd1 N4 179.999(1) 11_554 2 ?
N2 Cd2 N2 180.0(2) . 13_564 ?
N2 Cd2 N2 89.41(15) . 14_454 ?
N2 Cd2 N2 90.59(15) 13_564 14_454 ?
N2 Cd2 N2 90.59(15) . 2_665 ?
N2 Cd2 N2 89.41(15) 13_564 2_665 ?
N2 Cd2 N2 179.998(1) 14_454 2_665 ?
N2 Cd2 N2 89.41(15) . 15_554 ?
N2 Cd2 N2 90.59(15) 13_564 15_554 ?
N2 Cd2 N2 90.59(15) 14_454 15_554 ?
N2 Cd2 N2 89.41(15) 2_665 15_554 ?
N2 Cd2 N2 90.59(15) . 3_565 ?
N2 Cd2 N2 89.41(15) 13_564 3_565 ?
N2 Cd2 N2 89.41(15) 14_454 3_565 ?
N2 Cd2 N2 90.59(15) 2_665 3_565 ?
N2 Cd2 N2 180.0 15_554 3_565 ?
C5 N1 C7 107.0(5) . . ?
C5 N1 C4 124.7(5) . . ?
C7 N1 C4 128.3(5) . . ?
C5 N2 C6 105.4(5) . . ?
C5 N2 Cd2 124.6(4) . . ?
C6 N2 Cd2 130.0(4) . . ?
C9 N3 C11 106.0(5) . . ?
C9 N3 C8 128.1(5) . . ?
C11 N3 C8 125.8(5) . . ?
C9 N4 C10 104.7(5) . . ?
C9 N4 Cd1 124.2(4) . . ?
C10 N4 Cd1 130.2(4) . . ?
C2 C1 C3 119.1(4) . 16_553 ?
C2 C1 C4 118.6(5) . . ?
C3 C1 C4 122.2(5) 16_553 . ?
C1 C2 C3 123.2(5) . . ?
C1 C2 H2A 118.4 . . ?
C3 C2 H2A 118.4 . . ?
C2 C3 C1 117.6(5) . 16_553 ?
C2 C3 C8 119.1(5) . . ?
C1 C3 C8 123.2(4) 16_553 . ?
N1 C4 C1 112.5(4) . . ?
N1 C4 H4A 109.1 . . ?
C1 C4 H4A 109.1 . . ?
N1 C4 H4B 109.1 . . ?
C1 C4 H4B 109.1 . . ?
H4A C4 H4B 107.8 . . ?
N2 C5 N1 111.5(5) . . ?
N2 C5 H5A 124.3 . . ?
N1 C5 H5A 124.3 . . ?
C7 C6 N2 109.5(5) . . ?
C7 C6 H6A 125.2 . . ?
N2 C6 H6A 125.2 . . ?
N1 C7 C6 106.6(5) . . ?
N1 C7 H7A 126.7 . . ?
C6 C7 H7A 126.7 . . ?
N3 C8 C3 112.1(4) . . ?
N3 C8 H8A 109.2 . . ?
C3 C8 H8A 109.2 . . ?
N3 C8 H8B 109.2 . . ?
C3 C8 H8B 109.2 . . ?
H8A C8 H8B 107.9 . . ?
N4 C9 N3 111.9(5) . . ?
N4 C9 H9A 124.1 . . ?
N3 C9 H9A 124.1 . . ?
C11 C10 N4 110.8(6) . . ?
C11 C10 H10A 124.6 . . ?
N4 C10 H10A 124.6 . . ?
C10 C11 N3 106.6(5) . . ?
C10 C11 H11A 126.7 . . ?
N3 C11 H11A 126.7 . . ?
O3 N5 O1 127.0(16) . . ?
O3 N5 O2 117.6(15) . . ?
O1 N5 O2 115.4(14) . . ?

_diffrn_measured_fraction_theta_max 0.997
_diffrn_reflns_theta_full        27.50
_diffrn_measured_fraction_theta_full 0.997
_refine_diff_density_max         1.089
_refine_diff_density_min         -0.636
_refine_diff_density_rms         0.131

#====END

data_2
_database_code_depnum_ccdc_archive 'CCDC 687824'
_audit_creation_date             'Sun Jul 1 15:34:41 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        
;
[Cd2(L)3](ClO4)4-2(H2O)
;
_chemical_name_common            (Cd2(L)3)(ClO4)4-2(H2O)
_chemical_melting_point          ?
_chemical_formula_moiety         'C66 H70 Cd2 Cl4 N24 O18 '
_chemical_formula_sum            'C66 H70 Cd2 Cl4 N24 O18'
_chemical_formula_weight         1854.06

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'
Cl Cl 0.1484 0.1585 '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           trigonal
_symmetry_space_group_name_H-M   'R -3'
_symmetry_space_group_name_Hall  '-R 3'
_symmetry_Int_Tables_number      148
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                   21.297(6)
_cell_length_b                   21.297(6)
_cell_length_c                   15.380(4)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_volume                     6041(3)
_cell_formula_units_Z            3
_cell_measurement_temperature    200
_cell_measurement_reflns_used    10219
_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    1.529
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2826
_exptl_absorpt_coefficient_mu    0.741
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.831
_exptl_absorpt_correction_T_max  0.928
_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            19292
_diffrn_reflns_av_R_equivalents  0.0768
_diffrn_reflns_av_sigmaI/netI    0.0445
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         3.21
_diffrn_reflns_theta_max         27.47
_reflns_number_total             3071
_reflns_number_gt                2429
_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)+(0.0377P)²+53.1093P] 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         3071
_refine_ls_number_parameters     203
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0781
_refine_ls_R_factor_gt           0.0589
_refine_ls_wR_factor_ref         0.1249
_refine_ls_wR_factor_gt          0.1175
_refine_ls_goodness_of_fit_ref   1.073
_refine_ls_restrained_S_all      1.073
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Cd1 Cd 0.0000 0.0000 0.0000 0.0311(2) Uani 1 6 d S . .
Cd2 Cd 0.0000 0.0000 0.5000 0.01775(17) Uani 1 6 d S . .
Cl1 Cl 0.03338(10) 0.30176(10) 0.44918(12) 0.0456(4) Uani 0.67 1 d P . .
O1 O 0.1555(10) 0.3115(10) 0.3781(13) 0.045(5) Uani 0.17 1 d P . .
O2 O -0.0783(10) 0.2095(10) 0.5565(11) 0.033(4) Uani 0.17 1 d P . .
O11 O 0.0768(5) 0.2708(5) 0.4281(5) 0.106(3) Uani 0.67 1 d P . .
O12 O -0.0277(4) 0.2485(4) 0.4973(6) 0.093(2) Uani 0.67 1 d P . .
O13 O 0.0102(5) 0.3194(4) 0.3754(4) 0.100(3) Uani 0.67 1 d P . .
O14 O 0.0716(3) 0.3632(3) 0.5017(4) 0.0660(17) Uani 0.67 1 d P . .
N11 N 0.16292(17) -0.01305(17) 0.1713(2) 0.0258(7) Uani 1 1 d . . .
N12 N 0.07117(18) -0.03158(18) 0.0875(2) 0.0330(8) Uani 1 1 d . . .
N21 N 0.20934(17) 0.13412(18) 0.3568(2) 0.0269(7) Uani 1 1 d . . .
N22 N 0.09889(17) 0.07910(17) 0.4118(2) 0.0254(7) Uani 1 1 d . . .
C1 C 0.28033(19) 0.0985(2) 0.1991(2) 0.0251(8) Uani 1 1 d . . .
C2 C 0.30902(19) 0.1594(2) 0.2530(2) 0.0256(8) Uani 1 1 d . . .
C3 C 0.3611(2) 0.2262(2) 0.2193(3) 0.0271(8) Uani 1 1 d . . .
H1 H 0.3802 0.2676 0.2560 0.033 Uiso 1 1 calc R . .
C11 C 0.2257(2) 0.0230(2) 0.2303(3) 0.0307(9) Uani 1 1 d . . .
H2 H 0.2496 -0.0066 0.2345 0.037 Uiso 1 1 calc R . .
H3 H 0.2086 0.0262 0.2891 0.037 Uiso 1 1 calc R . .
C12 C 0.1229(2) 0.0146(2) 0.1388(3) 0.0338(10) Uani 1 1 d . . .
H4 H 0.1312 0.0618 0.1516 0.041 Uiso 1 1 calc R . .
C13 C 0.0778(3) -0.0926(2) 0.0875(3) 0.0412(11) Uani 1 1 d . . .
H5 H 0.0476 -0.1357 0.0560 0.049 Uiso 1 1 calc R . .
C14 C 0.1338(2) -0.0820(2) 0.1393(3) 0.0400(11) Uani 1 1 d . . .
H6 H 0.1497 -0.1156 0.1509 0.048 Uiso 1 1 calc R . .
C21 C 0.2867(2) 0.1567(2) 0.3471(2) 0.0313(9) Uani 1 1 d . . .
H7 H 0.2967 0.1223 0.3793 0.038 Uiso 1 1 calc R . .
H8 H 0.3164 0.2052 0.3735 0.038 Uiso 1 1 calc R . .
C22 C 0.1641(2) 0.0872(2) 0.4175(2) 0.0260(8) Uani 1 1 d . . .
H9 H 0.1778 0.0632 0.4589 0.031 Uiso 1 1 calc R . .
C23 C 0.1025(2) 0.1234(3) 0.3438(3) 0.0350(10) Uani 1 1 d . . .
H10 H 0.0633 0.1292 0.3240 0.042 Uiso 1 1 calc R . .
C24 C 0.1701(2) 0.1574(3) 0.3098(3) 0.0377(10) Uani 1 1 d . . .
H11 H 0.1871 0.1907 0.2626 0.045 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 2.362(4) 3 ?
Cd1 N12 2.362(4) 11 ?
Cd1 N12 2.362(4) 10 ?
Cd1 N12 2.362(4) . ?
Cd1 N12 2.362(4) 2 ?
Cd1 N12 2.362(4) 12 ?
Cd2 N22 2.359(3) 10_556 ?
Cd2 N22 2.359(3) 2 ?
Cd2 N22 2.359(3) . ?
Cd2 N22 2.359(3) 3 ?
Cd2 N22 2.359(3) 12_556 ?
Cd2 N22 2.359(3) 11_556 ?
Cl1 O13 1.362(7) . ?
Cl1 O14 1.400(6) . ?
Cl1 O11 1.415(7) . ?
Cl1 O12 1.432(8) . ?
O1 O1 1.60(4) 16 ?
O1 O11 1.64(2) . ?
O1 O2 1.78(3) 11_556 ?
O2 O12 1.336(19) . ?
O2 O1 1.78(3) 12_556 ?
N11 C12 1.350(5) . ?
N11 C14 1.368(5) . ?
N11 C11 1.475(5) . ?
N12 C12 1.312(5) . ?
N12 C13 1.375(5) . ?
N21 C22 1.354(5) . ?
N21 C24 1.372(5) . ?
N21 C21 1.474(5) . ?
N22 C22 1.314(5) . ?
N22 C23 1.386(5) . ?
C1 C3 1.392(5) 13 ?
C1 C2 1.397(5) . ?
C1 C11 1.515(5) . ?
C2 C3 1.394(5) . ?
C2 C21 1.516(5) . ?
C3 C1 1.392(5) 13 ?
C3 H1 0.9500 . ?
C11 H2 0.9900 . ?
C11 H3 0.9900 . ?
C12 H4 0.9500 . ?
C13 C14 1.356(6) . ?
C13 H5 0.9500 . ?
C14 H6 0.9500 . ?
C21 H7 0.9900 . ?
C21 H8 0.9900 . ?
C22 H9 0.9500 . ?
C23 C24 1.353(6) . ?
C23 H10 0.9500 . ?
C24 H11 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
N12 Cd1 N12 89.23(12) 3 11 ?
N12 Cd1 N12 89.23(12) 3 10 ?
N12 Cd1 N12 90.77(12) 11 10 ?
N12 Cd1 N12 90.77(12) 3 . ?
N12 Cd1 N12 89.23(12) 11 . ?
N12 Cd1 N12 180.0 10 . ?
N12 Cd1 N12 90.77(12) 3 2 ?
N12 Cd1 N12 180.0 11 2 ?
N12 Cd1 N12 89.23(12) 10 2 ?
N12 Cd1 N12 90.77(12) . 2 ?
N12 Cd1 N12 180.0 3 12 ?
N12 Cd1 N12 90.77(12) 11 12 ?
N12 Cd1 N12 90.77(12) 10 12 ?
N12 Cd1 N12 89.23(12) . 12 ?
N12 Cd1 N12 89.23(12) 2 12 ?
N22 Cd2 N22 89.78(11) 10_556 2 ?
N22 Cd2 N22 180.00(15) 10_556 . ?
N22 Cd2 N22 90.22(11) 2 . ?
N22 Cd2 N22 89.78(11) 10_556 3 ?
N22 Cd2 N22 90.23(11) 2 3 ?
N22 Cd2 N22 90.22(11) . 3 ?
N22 Cd2 N22 90.23(11) 10_556 12_556 ?
N22 Cd2 N22 89.77(11) 2 12_556 ?
N22 Cd2 N22 89.77(11) . 12_556 ?
N22 Cd2 N22 180.00(10) 3 12_556 ?
N22 Cd2 N22 90.23(11) 10_556 11_556 ?
N22 Cd2 N22 180.0 2 11_556 ?
N22 Cd2 N22 89.77(11) . 11_556 ?
N22 Cd2 N22 89.77(11) 3 11_556 ?
N22 Cd2 N22 90.22(11) 12_556 11_556 ?
O13 Cl1 O14 110.2(4) . . ?
O13 Cl1 O11 110.4(4) . . ?
O14 Cl1 O11 111.0(5) . . ?
O13 Cl1 O12 109.7(5) . . ?
O14 Cl1 O12 108.3(4) . . ?
O11 Cl1 O12 107.2(5) . . ?
O1 O1 O11 130(2) 16 . ?
O1 O1 O2 127.3(19) 16 11_556 ?
O11 O1 O2 102.7(12) . 11_556 ?
O12 O2 O1 170.7(14) . 12_556 ?
Cl1 O11 O1 126.4(9) . . ?
O2 O12 Cl1 167.3(9) . . ?
C12 N11 C14 106.8(3) . . ?
C12 N11 C11 127.3(3) . . ?
C14 N11 C11 125.9(4) . . ?
C12 N12 C13 105.3(4) . . ?
C12 N12 Cd1 123.2(3) . . ?
C13 N12 Cd1 130.8(3) . . ?
C22 N21 C24 107.0(3) . . ?
C22 N21 C21 125.3(3) . . ?
C24 N21 C21 127.7(3) . . ?
C22 N22 C23 105.4(3) . . ?
C22 N22 Cd2 124.3(3) . . ?
C23 N22 Cd2 130.2(3) . . ?
C3 C1 C2 118.3(3) 13 . ?
C3 C1 C11 118.6(3) 13 . ?
C2 C1 C11 123.0(3) . . ?
C3 C2 C1 118.9(3) . . ?
C3 C2 C21 117.9(4) . . ?
C1 C2 C21 123.2(3) . . ?
C1 C3 C2 122.8(4) 13 . ?
C1 C3 H1 118.6 13 . ?
C2 C3 H1 118.6 . . ?
N11 C11 C1 111.9(3) . . ?
N11 C11 H2 109.2 . . ?
C1 C11 H2 109.2 . . ?
N11 C11 H3 109.2 . . ?
C1 C11 H3 109.2 . . ?
H2 C11 H3 107.9 . . ?
N12 C12 N11 111.9(4) . . ?
N12 C12 H4 124.1 . . ?
N11 C12 H4 124.1 . . ?
C14 C13 N12 109.9(4) . . ?
C14 C13 H5 125.0 . . ?
N12 C13 H5 125.0 . . ?
C13 C14 N11 106.2(4) . . ?
C13 C14 H6 126.9 . . ?
N11 C14 H6 126.9 . . ?
N21 C21 C2 112.8(3) . . ?
N21 C21 H7 109.0 . . ?
C2 C21 H7 109.0 . . ?
N21 C21 H8 109.0 . . ?
C2 C21 H8 109.0 . . ?
H7 C21 H8 107.8 . . ?
N22 C22 N21 111.5(3) . . ?
N22 C22 H9 124.2 . . ?
N21 C22 H9 124.2 . . ?
C24 C23 N22 109.7(4) . . ?
C24 C23 H10 125.2 . . ?
N22 C23 H10 125.2 . . ?
C23 C24 N21 106.3(4) . . ?
C23 C24 H11 126.8 . . ?
N21 C24 H11 126.8 . . ?

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
O13 Cl1 O11 O1 64.4(12) . . . . ?
O14 Cl1 O11 O1 -58.1(12) . . . . ?
O12 Cl1 O11 O1 -176.2(11) . . . . ?
O1 O1 O11 Cl1 -52(3) 16 . . . ?
O2 O1 O11 Cl1 133.1(10) 11_556 . . . ?
O13 Cl1 O12 O2 -125(4) . . . . ?
O14 Cl1 O12 O2 -4(5) . . . . ?
O11 Cl1 O12 O2 115(4) . . . . ?
N12 Cd1 N12 C12 -110.4(3) 3 . . . ?
N12 Cd1 N12 C12 160.3(4) 11 . . . ?
N12 Cd1 N12 C12 -19.7(4) 2 . . . ?
N12 Cd1 N12 C12 69.6(3) 12 . . . ?
N12 Cd1 N12 C13 81.2(5) 3 . . . ?
N12 Cd1 N12 C13 -8.0(4) 11 . . . ?
N12 Cd1 N12 C13 172.0(4) 2 . . . ?
N12 Cd1 N12 C13 -98.8(5) 12 . . . ?
N22 Cd2 N22 C22 -170.4(3) 2 . . . ?
N22 Cd2 N22 C22 -80.1(4) 3 . . . ?
N22 Cd2 N22 C22 99.8(4) 12_556 . . . ?
N22 Cd2 N22 C22 9.6(3) 11_556 . . . ?
N22 Cd2 N22 C23 7.0(4) 2 . . . ?
N22 Cd2 N22 C23 97.2(3) 3 . . . ?
N22 Cd2 N22 C23 -82.8(3) 12_556 . . . ?
N22 Cd2 N22 C23 -173.0(4) 11_556 . . . ?
C3 C1 C2 C3 0.5(6) 13 . . . ?
C11 C1 C2 C3 177.6(4) . . . . ?
C3 C1 C2 C21 -179.1(4) 13 . . . ?
C11 C1 C2 C21 -2.1(6) . . . . ?
C1 C2 C3 C1 -0.5(6) . . . 13 ?
C21 C2 C3 C1 179.1(4) . . . 13 ?
C12 N11 C11 C1 -48.6(5) . . . . ?
C14 N11 C11 C1 131.9(4) . . . . ?
C3 C1 C11 N11 -52.3(5) 13 . . . ?
C2 C1 C11 N11 130.7(4) . . . . ?
C13 N12 C12 N11 0.6(5) . . . . ?
Cd1 N12 C12 N11 -170.3(3) . . . . ?
C14 N11 C12 N12 -0.9(5) . . . . ?
C11 N11 C12 N12 179.4(4) . . . . ?
C12 N12 C13 C14 0.0(6) . . . . ?
Cd1 N12 C13 C14 169.9(3) . . . . ?
N12 C13 C14 N11 -0.5(6) . . . . ?
C12 N11 C14 C13 0.9(5) . . . . ?
C11 N11 C14 C13 -179.5(4) . . . . ?
C22 N21 C21 C2 137.6(4) . . . . ?
C24 N21 C21 C2 -44.7(6) . . . . ?
C3 C2 C21 N21 117.6(4) . . . . ?
C1 C2 C21 N21 -62.7(5) . . . . ?
C23 N22 C22 N21 -0.1(5) . . . . ?
Cd2 N22 C22 N21 177.8(2) . . . . ?
C24 N21 C22 N22 0.1(5) . . . . ?
C21 N21 C22 N22 178.2(3) . . . . ?
C22 N22 C23 C24 0.1(5) . . . . ?
Cd2 N22 C23 C24 -177.7(3) . . . . ?
N22 C23 C24 N21 0.0(5) . . . . ?
C22 N21 C24 C23 -0.1(5) . . . . ?
C21 N21 C24 C23 -178.1(4) . . . . ?

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        27.47
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         0.735
_refine_diff_density_min         -0.736
_refine_diff_density_rms         0.097

#====END

data_3
_database_code_depnum_ccdc_archive 'CCDC 687825'
_audit_creation_date             'Sun Jul 1 14:18:33 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        
;
[Cd2(L)3](BF4)4-2(H2O)
;
_chemical_name_common            (Cd2(L)3)(BF4)4-2(H2O)
_chemical_melting_point          ?
_chemical_formula_moiety         'C66 H70 B4 Cd2 F16 N24 O2 '
_chemical_formula_sum            'C66 H70 B4 Cd2 F16 N24 O2'
_chemical_formula_weight         1803.50

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'
F F 0.0171 0.0103 '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'
B B 0.0013 0.0007 '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           trigonal
_symmetry_space_group_name_H-M   'R -3'
_symmetry_space_group_name_Hall  '-R 3'
_symmetry_Int_Tables_number      148
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                   21.218(5)
_cell_length_b                   21.218(5)
_cell_length_c                   15.259(4)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_volume                     5949(2)
_cell_formula_units_Z            3
_cell_measurement_temperature    200
_cell_measurement_reflns_used    10850
_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    1.510
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2730
_exptl_absorpt_coefficient_mu    0.633
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.812
_exptl_absorpt_correction_T_max  0.939
_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            18998
_diffrn_reflns_av_R_equivalents  0.0467
_diffrn_reflns_av_sigmaI/netI    0.0277
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         3.22
_diffrn_reflns_theta_max         27.45
_reflns_number_total             3031
_reflns_number_gt                2411
_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)+(0.0420P)²+26.3075P] 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         3031
_refine_ls_number_parameters     203
_refine_ls_number_restraints     18
_refine_ls_R_factor_all          0.0554
_refine_ls_R_factor_gt           0.0410
_refine_ls_wR_factor_ref         0.1069
_refine_ls_wR_factor_gt          0.1002
_refine_ls_goodness_of_fit_ref   1.089
_refine_ls_restrained_S_all      1.089
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Cd1 Cd 0.0000 0.0000 0.0000 0.01954(14) Uani 1 6 d S . .
Cd2 Cd 0.0000 0.0000 0.5000 0.03089(16) Uani 1 6 d S . .
F1 F 0.3912(3) 0.3081(3) 0.3389(5) 0.124(2) Uani 0.67 1 d P . .
F2 F 0.4702(2) 0.4076(4) 0.4055(3) 0.121(2) Uani 0.67 1 d P . .
F3 F 0.3583(2) 0.3440(4) 0.4556(3) 0.135(3) Uani 0.67 1 d PU . .
F4 F 0.3772(2) 0.4040(2) 0.3335(3) 0.0735(11) Uani 0.67 1 d P . .
O1 O 0.3788(7) 0.2530(8) 0.2750(9) 0.038(3) Uani 0.17 1 d PU . .
O2 O 0.5137(8) 0.4919(9) 0.4553(10) 0.050(4) Uani 0.17 1 d PU . .
N11 N 0.07582(14) 0.20983(13) 0.14198(15) 0.0273(5) Uani 1 1 d . . .
N12 N 0.02033(13) 0.09891(13) 0.08844(15) 0.0260(5) Uani 1 1 d . . .
N21 N 0.17681(13) 0.16347(13) 0.32731(16) 0.0272(5) Uani 1 1 d . . .
N22 N 0.10297(14) 0.07179(13) 0.41154(18) 0.0330(6) Uani 1 1 d . . .
C1 C 0.14991(16) 0.30920(15) 0.24603(18) 0.0277(6) Uani 1 1 d . . .
C2 C 0.18282(16) 0.28130(15) 0.29985(18) 0.0270(6) Uani 1 1 d . . .
C3 C 0.19942(16) 0.30602(15) 0.38670(19) 0.0289(6) Uani 1 1 d . . .
H1 H 0.2222 0.2872 0.4234 0.035 Uiso 1 1 calc R . .
C11 C 0.13088(19) 0.28742(16) 0.15133(19) 0.0332(7) Uani 1 1 d . . .
H2 H 0.1121 0.3174 0.1247 0.040 Uiso 1 1 calc R . .
H3 H 0.1754 0.2973 0.1192 0.040 Uiso 1 1 calc R . .
C12 C 0.07749(16) 0.16410(15) 0.08234(18) 0.0277(6) Uani 1 1 d . . .
H4 H 0.1155 0.1774 0.0408 0.033 Uiso 1 1 calc R . .
C13 C -0.02024(17) 0.10329(18) 0.1558(2) 0.0355(7) Uani 1 1 d . . .
H5 H -0.0652 0.0641 0.1759 0.043 Uiso 1 1 calc R . .
C14 C 0.01308(18) 0.17151(18) 0.1894(2) 0.0379(8) Uani 1 1 d . . .
H6 H -0.0036 0.1891 0.2361 0.045 Uiso 1 1 calc R . .
C21 C 0.20445(18) 0.22710(16) 0.26873(19) 0.0321(7) Uani 1 1 d . . .
H7 H 0.1851 0.2106 0.2089 0.039 Uiso 1 1 calc R . .
H8 H 0.2582 0.2513 0.2658 0.039 Uiso 1 1 calc R . .
C22 C 0.10896(17) 0.12415(16) 0.3600(2) 0.0321(7) Uani 1 1 d . . .
H9 H 0.0703 0.1331 0.3473 0.039 Uiso 1 1 calc R . .
C23 C 0.16980(18) 0.07724(19) 0.4106(2) 0.0403(8) Uani 1 1 d . . .
H10 H 0.1822 0.0462 0.4418 0.048 Uiso 1 1 calc R . .
C24 C 0.21581(18) 0.13326(18) 0.3591(2) 0.0383(7) Uani 1 1 d . . .
H11 H 0.2654 0.1485 0.3473 0.046 Uiso 1 1 calc R . .
B1 B 0.3970(3) 0.3664(4) 0.3861(5) 0.0466(15) Uani 0.67 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
Cd1 N12 2.346(2) 3 ?
Cd1 N12 2.346(2) 11 ?
Cd1 N12 2.347(2) 10 ?
Cd1 N12 2.347(2) 2 ?
Cd1 N12 2.347(2) 12 ?
Cd1 N12 2.347(2) . ?
Cd2 N22 2.364(3) 11_556 ?
Cd2 N22 2.364(3) 3 ?
Cd2 N22 2.364(3) 12_556 ?
Cd2 N22 2.364(3) 10_556 ?
Cd2 N22 2.364(3) 2 ?
Cd2 N22 2.364(3) . ?
F1 B1 1.382(9) . ?
F1 O1 1.443(16) . ?
F2 B1 1.381(7) . ?
F2 O2 1.725(17) . ?
F3 B1 1.278(8) . ?
F4 B1 1.340(8) . ?
O1 O2 1.67(2) 18_545 ?
O2 O2 1.59(3) 10_666 ?
O2 O1 1.67(2) 17 ?
N11 C12 1.344(4) . ?
N11 C14 1.370(4) . ?
N11 C11 1.474(4) . ?
N12 C12 1.310(4) . ?
N12 C13 1.373(4) . ?
N21 C22 1.347(4) . ?
N21 C24 1.365(4) . ?
N21 C21 1.474(4) . ?
N22 C22 1.315(4) . ?
N22 C23 1.364(4) . ?
C1 C2 1.388(4) . ?
C1 C3 1.395(4) 16 ?
C1 C11 1.509(4) . ?
C2 C3 1.404(4) . ?
C2 C21 1.512(4) . ?
C3 C1 1.395(4) 16 ?
C3 H1 0.9500 . ?
C11 H2 0.9900 . ?
C11 H3 0.9900 . ?
C12 H4 0.9500 . ?
C13 C14 1.355(4) . ?
C13 H5 0.9500 . ?
C14 H6 0.9500 . ?
C21 H7 0.9900 . ?
C21 H8 0.9900 . ?
C22 H9 0.9500 . ?
C23 C24 1.351(5) . ?
C23 H10 0.9500 . ?
C24 H11 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
N12 Cd1 N12 89.78(8) 3 11 ?
N12 Cd1 N12 89.78(8) 3 10 ?
N12 Cd1 N12 90.22(8) 11 10 ?
N12 Cd1 N12 90.22(8) 3 2 ?
N12 Cd1 N12 180.0 11 2 ?
N12 Cd1 N12 89.78(8) 10 2 ?
N12 Cd1 N12 180.0 3 12 ?
N12 Cd1 N12 90.22(8) 11 12 ?
N12 Cd1 N12 90.22(8) 10 12 ?
N12 Cd1 N12 89.77(8) 2 12 ?
N12 Cd1 N12 90.22(8) 3 . ?
N12 Cd1 N12 89.78(8) 11 . ?
N12 Cd1 N12 180.0 10 . ?
N12 Cd1 N12 90.22(8) 2 . ?
N12 Cd1 N12 89.78(8) 12 . ?
N22 Cd2 N22 89.38(9) 11_556 3 ?
N22 Cd2 N22 90.62(9) 11_556 12_556 ?
N22 Cd2 N22 179.998(1) 3 12_556 ?
N22 Cd2 N22 90.62(9) 11_556 10_556 ?
N22 Cd2 N22 89.38(9) 3 10_556 ?
N22 Cd2 N22 90.62(9) 12_556 10_556 ?
N22 Cd2 N22 180.0 11_556 2 ?
N22 Cd2 N22 90.62(9) 3 2 ?
N22 Cd2 N22 89.38(9) 12_556 2 ?
N22 Cd2 N22 89.37(9) 10_556 2 ?
N22 Cd2 N22 89.38(9) 11_556 . ?
N22 Cd2 N22 90.62(9) 3 . ?
N22 Cd2 N22 89.38(9) 12_556 . ?
N22 Cd2 N22 179.999(1) 10_556 . ?
N22 Cd2 N22 90.63(9) 2 . ?
C12 N11 C14 107.3(2) . . ?
C12 N11 C11 125.5(3) . . ?
C14 N11 C11 127.2(3) . . ?
C12 N12 C13 105.2(2) . . ?
C12 N12 Cd1 124.24(19) . . ?
C13 N12 Cd1 130.5(2) . . ?
C22 N21 C24 106.8(3) . . ?
C22 N21 C21 127.1(3) . . ?
C24 N21 C21 126.1(3) . . ?
C22 N22 C23 105.4(3) . . ?
C22 N22 Cd2 123.6(2) . . ?
C23 N22 Cd2 130.3(2) . . ?
C2 C1 C3 119.0(3) . 16 ?
C2 C1 C11 123.4(3) . . ?
C3 C1 C11 117.5(3) 16 . ?
C1 C2 C3 119.0(3) . . ?
C1 C2 C21 123.2(3) . . ?
C3 C2 C21 117.8(3) . . ?
C1 C3 C2 121.9(3) 16 . ?
C1 C3 H1 119.0 16 . ?
C2 C3 H1 119.0 . . ?
N11 C11 C1 112.1(2) . . ?
N11 C11 H2 109.2 . . ?
C1 C11 H2 109.2 . . ?
N11 C11 H3 109.2 . . ?
C1 C11 H3 109.2 . . ?
H2 C11 H3 107.9 . . ?
N12 C12 N11 111.7(3) . . ?
N12 C12 H4 124.2 . . ?
N11 C12 H4 124.2 . . ?
C14 C13 N12 110.2(3) . . ?
C14 C13 H5 124.9 . . ?
N12 C13 H5 124.9 . . ?
C13 C14 N11 105.5(3) . . ?
C13 C14 H6 127.3 . . ?
N11 C14 H6 127.3 . . ?
N21 C21 C2 111.9(2) . . ?
N21 C21 H7 109.2 . . ?
C2 C21 H7 109.2 . . ?
N21 C21 H8 109.2 . . ?
C2 C21 H8 109.2 . . ?
H7 C21 H8 107.9 . . ?
N22 C22 N21 111.5(3) . . ?
N22 C22 H9 124.3 . . ?
N21 C22 H9 124.3 . . ?
C24 C23 N22 110.1(3) . . ?
C24 C23 H10 124.9 . . ?
N22 C23 H10 124.9 . . ?
C23 C24 N21 106.2(3) . . ?
C23 C24 H11 126.9 . . ?
N21 C24 H11 126.9 . . ?
F3 B1 F4 112.5(6) . . ?
F3 B1 F2 111.6(6) . . ?
F4 B1 F2 109.8(6) . . ?
F3 B1 F1 110.3(7) . . ?
F4 B1 F1 107.9(6) . . ?
F2 B1 F1 104.4(6) . . ?

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 80.6(3) 3 . . . ?
N12 Cd1 N12 C12 -9.2(2) 11 . . . ?
N12 Cd1 N12 C12 170.8(2) 2 . . . ?
N12 Cd1 N12 C12 -99.4(3) 12 . . . ?
N12 Cd1 N12 C13 -98.1(2) 3 . . . ?
N12 Cd1 N12 C13 172.2(3) 11 . . . ?
N12 Cd1 N12 C13 -7.8(3) 2 . . . ?
N12 Cd1 N12 C13 81.9(2) 12 . . . ?
N22 Cd2 N22 C22 -159.7(3) 11_556 . . . ?
N22 Cd2 N22 C22 110.9(2) 3 . . . ?
N22 Cd2 N22 C22 -69.1(2) 12_556 . . . ?
N22 Cd2 N22 C22 20.3(3) 2 . . . ?
N22 Cd2 N22 C23 9.6(3) 11_556 . . . ?
N22 Cd2 N22 C23 -79.7(3) 3 . . . ?
N22 Cd2 N22 C23 100.3(3) 12_556 . . . ?
N22 Cd2 N22 C23 -170.4(3) 2 . . . ?
C3 C1 C2 C3 -0.4(5) 16 . . . ?
C11 C1 C2 C3 178.9(3) . . . . ?
C3 C1 C2 C21 -178.1(3) 16 . . . ?
C11 C1 C2 C21 1.2(4) . . . . ?
C1 C2 C3 C1 0.4(5) . . . 16 ?
C21 C2 C3 C1 178.2(3) . . . 16 ?
C12 N11 C11 C1 -137.0(3) . . . . ?
C14 N11 C11 C1 45.3(4) . . . . ?
C2 C1 C11 N11 64.0(4) . . . . ?
C3 C1 C11 N11 -116.7(3) 16 . . . ?
C13 N12 C12 N11 0.1(3) . . . . ?
Cd1 N12 C12 N11 -178.86(18) . . . . ?
C14 N11 C12 N12 -0.3(4) . . . . ?
C11 N11 C12 N12 -178.5(3) . . . . ?
C12 N12 C13 C14 0.2(4) . . . . ?
Cd1 N12 C13 C14 179.0(2) . . . . ?
N12 C13 C14 N11 -0.4(4) . . . . ?
C12 N11 C14 C13 0.4(4) . . . . ?
C11 N11 C14 C13 178.5(3) . . . . ?
C22 N21 C21 C2 46.7(4) . . . . ?
C24 N21 C21 C2 -133.1(3) . . . . ?
C1 C2 C21 N21 -129.2(3) . . . . ?
C3 C2 C21 N21 53.1(4) . . . . ?
C23 N22 C22 N21 -1.0(4) . . . . ?
Cd2 N22 C22 N21 170.60(19) . . . . ?
C24 N21 C22 N22 1.1(4) . . . . ?
C21 N21 C22 N22 -178.7(3) . . . . ?
C22 N22 C23 C24 0.5(4) . . . . ?
Cd2 N22 C23 C24 -170.3(2) . . . . ?
N22 C23 C24 N21 0.1(4) . . . . ?
C22 N21 C24 C23 -0.7(4) . . . . ?
C21 N21 C24 C23 179.1(3) . . . . ?

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        27.45
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         0.470
_refine_diff_density_min         -0.475
_refine_diff_density_rms         0.080

#====END

data_4
_database_code_depnum_ccdc_archive 'CCDC 687826'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C22 H26 Cd Cl2 N8 O2'
_chemical_formula_weight         617.81

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)/c

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

_cell_length_a                   11.0403(16)
_cell_length_b                   8.9060(13)
_cell_length_c                   13.640(2)
_cell_angle_alpha                90.00
_cell_angle_beta                 109.155(3)
_cell_angle_gamma                90.00
_cell_volume                     1266.9(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    1933
_cell_measurement_theta_min      2.78
_cell_measurement_theta_max      24.69

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.620
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             624
_exptl_absorpt_coefficient_mu    1.109
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.8972
_exptl_absorpt_correction_T_max  0.8972
_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            6604
_diffrn_reflns_av_R_equivalents  0.0339
_diffrn_reflns_av_sigmaI/netI    0.0499
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_theta_min         1.95
_diffrn_reflns_theta_max         26.00
_reflns_number_total             2486
_reflns_number_gt                2147
_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)+(0.0560P)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         2486
_refine_ls_number_parameters     160
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0560
_refine_ls_R_factor_gt           0.0462
_refine_ls_wR_factor_ref         0.1141
_refine_ls_wR_factor_gt          0.1086
_refine_ls_goodness_of_fit_ref   1.071
_refine_ls_restrained_S_all      1.071
_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 0.8682(4) 0.5290(4) 0.9749(3) 0.0331(10) Uani 1 1 d . . .
C2 C 0.9437(4) 0.6187(4) 0.9347(3) 0.0315(9) Uani 1 1 d . . .
C3 C 1.0719(4) 0.5899(4) 0.9606(3) 0.0352(10) Uani 1 1 d . . .
H3 H 1.1214 0.6520 0.9341 0.042 Uiso 1 1 calc R . .
C4 C 0.7251(4) 0.5589(5) 0.9479(4) 0.0460(12) Uani 1 1 d . . .
H4A H 0.7125 0.6596 0.9700 0.055 Uiso 1 1 calc R . .
H4B H 0.6846 0.5537 0.8732 0.055 Uiso 1 1 calc R . .
C5 C 0.6159(3) 0.3178(5) 0.9574(3) 0.0369(10) Uani 1 1 d . . .
H5 H 0.6084 0.2859 0.8907 0.044 Uiso 1 1 calc R . .
C6 C 0.6076(4) 0.3255(5) 1.1111(3) 0.0436(11) Uani 1 1 d . . .
H6 H 0.5920 0.2985 1.1717 0.052 Uiso 1 1 calc R . .
C7 C 0.6598(4) 0.4559(5) 1.0954(4) 0.0451(11) Uani 1 1 d . . .
H7 H 0.6876 0.5341 1.1427 0.054 Uiso 1 1 calc R . .
C8 C 0.8856(4) 0.7448(5) 0.8593(3) 0.0395(10) Uani 1 1 d . . .
H8A H 0.8171 0.7920 0.8780 0.047 Uiso 1 1 calc R . .
H8B H 0.9505 0.8201 0.8632 0.047 Uiso 1 1 calc R . .
C9 C 0.9032(4) 0.6301(6) 0.6942(4) 0.0584(14) Uani 1 1 d . . .
H9 H 0.9920 0.6305 0.7110 0.070 Uiso 1 1 calc R . .
C10 C 0.8179(5) 0.5740(7) 0.6074(4) 0.0583(14) Uani 1 1 d . . .
H10 H 0.8382 0.5287 0.5534 0.070 Uiso 1 1 calc R . .
C11 C 0.7108(4) 0.6616(5) 0.6996(3) 0.0360(10) Uani 1 1 d . . .
H11 H 0.6434 0.6890 0.7225 0.043 Uiso 1 1 calc R . .
Cd1 Cd 0.5000 0.5000 0.5000 0.03426(17) Uani 1 2 d S . .
Cl1 Cl 0.42093(12) 0.46386(13) 0.66499(9) 0.0469(3) Uani 1 1 d . . .
N1 N 0.6641(3) 0.4511(4) 0.9973(3) 0.0357(8) Uani 1 1 d . . .
N2 N 0.5810(3) 0.2387(4) 1.0238(3) 0.0376(8) Uani 1 1 d . . .
N3 N 0.8346(3) 0.6861(4) 0.7526(3) 0.0373(8) Uani 1 1 d . . .
N4 N 0.6967(3) 0.5939(4) 0.6109(3) 0.0412(9) Uani 1 1 d . . .
O1W O 0.1558(8) 0.8804(11) 0.1284(9) 0.259(5) Uani 1 1 d . . .
H1WB H 0.2158 0.9412 0.1302 0.388 Uiso 1 1 d R . .
H1WA H 0.0943 0.8917 0.0718 0.388 Uiso 1 1 d 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
C1 C2 1.390(5) . ?
C1 C3 1.397(5) 3_767 ?
C1 C4 1.524(5) . ?
C2 C3 1.366(5) . ?
C2 C8 1.515(5) . ?
C3 C1 1.397(5) 3_767 ?
C3 H3 0.9300 . ?
C4 N1 1.459(5) . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
C5 N2 1.301(5) . ?
C5 N1 1.341(5) . ?
C5 H5 0.9300 . ?
C6 C7 1.344(6) . ?
C6 N2 1.368(5) . ?
C6 H6 0.9300 . ?
C7 N1 1.355(6) . ?
C7 H7 0.9300 . ?
C8 N3 1.473(5) . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C9 C10 1.343(7) . ?
C9 N3 1.362(6) . ?
C9 H9 0.9300 . ?
C10 N4 1.366(5) . ?
C10 H10 0.9300 . ?
C11 N4 1.314(5) . ?
C11 N3 1.338(5) . ?
C11 H11 0.9300 . ?
Cd1 N2 2.288(3) 4_565 ?
Cd1 N2 2.288(3) 2_656 ?
Cd1 N4 2.356(3) 3_666 ?
Cd1 N4 2.356(3) . ?
Cd1 Cl1 2.6869(12) 3_666 ?
Cd1 Cl1 2.6869(12) . ?
N2 Cd1 2.288(3) 2_646 ?
O1W H1WB 0.8500 . ?
O1W H1WA 0.8500 . ?

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
C2 C1 C3 117.6(4) . 3_767 ?
C2 C1 C4 120.8(4) . . ?
C3 C1 C4 121.6(4) 3_767 . ?
C3 C2 C1 119.6(4) . . ?
C3 C2 C8 119.1(3) . . ?
C1 C2 C8 121.3(3) . . ?
C2 C3 C1 122.8(4) . 3_767 ?
C2 C3 H3 118.6 . . ?
C1 C3 H3 118.6 3_767 . ?
N1 C4 C1 111.9(3) . . ?
N1 C4 H4A 109.2 . . ?
C1 C4 H4A 109.2 . . ?
N1 C4 H4B 109.2 . . ?
C1 C4 H4B 109.2 . . ?
H4A C4 H4B 107.9 . . ?
N2 C5 N1 111.4(4) . . ?
N2 C5 H5 124.3 . . ?
N1 C5 H5 124.3 . . ?
C7 C6 N2 109.3(4) . . ?
C7 C6 H6 125.3 . . ?
N2 C6 H6 125.3 . . ?
C6 C7 N1 106.6(4) . . ?
C6 C7 H7 126.7 . . ?
N1 C7 H7 126.7 . . ?
N3 C8 C2 110.3(3) . . ?
N3 C8 H8A 109.6 . . ?
C2 C8 H8A 109.6 . . ?
N3 C8 H8B 109.6 . . ?
C2 C8 H8B 109.6 . . ?
H8A C8 H8B 108.1 . . ?
C10 C9 N3 106.7(4) . . ?
C10 C9 H9 126.6 . . ?
N3 C9 H9 126.6 . . ?
C9 C10 N4 109.4(4) . . ?
C9 C10 H10 125.3 . . ?
N4 C10 H10 125.3 . . ?
N4 C11 N3 111.4(4) . . ?
N4 C11 H11 124.3 . . ?
N3 C11 H11 124.3 . . ?
N2 Cd1 N2 180.000(1) 4_565 2_656 ?
N2 Cd1 N4 89.79(12) 4_565 3_666 ?
N2 Cd1 N4 90.21(12) 2_656 3_666 ?
N2 Cd1 N4 90.21(12) 4_565 . ?
N2 Cd1 N4 89.79(12) 2_656 . ?
N4 Cd1 N4 180.0 3_666 . ?
N2 Cd1 Cl1 90.62(9) 4_565 3_666 ?
N2 Cd1 Cl1 89.38(9) 2_656 3_666 ?
N4 Cd1 Cl1 89.37(9) 3_666 3_666 ?
N4 Cd1 Cl1 90.63(9) . 3_666 ?
N2 Cd1 Cl1 89.38(9) 4_565 . ?
N2 Cd1 Cl1 90.62(9) 2_656 . ?
N4 Cd1 Cl1 90.63(9) 3_666 . ?
N4 Cd1 Cl1 89.37(9) . . ?
Cl1 Cd1 Cl1 180.0 3_666 . ?
C5 N1 C7 106.9(4) . . ?
C5 N1 C4 125.2(4) . . ?
C7 N1 C4 127.4(4) . . ?
C5 N2 C6 105.8(4) . . ?
C5 N2 Cd1 126.5(3) . 2_646 ?
C6 N2 Cd1 127.6(3) . 2_646 ?
C11 N3 C9 106.8(4) . . ?
C11 N3 C8 125.7(4) . . ?
C9 N3 C8 127.1(4) . . ?
C11 N4 C10 105.7(4) . . ?
C11 N4 Cd1 124.1(3) . . ?
C10 N4 Cd1 129.7(3) . . ?
H1WB O1W H1WA 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
C3 C1 C2 C3 -1.1(7) 3_767 . . . ?
C4 C1 C2 C3 179.6(4) . . . . ?
C3 C1 C2 C8 176.6(4) 3_767 . . . ?
C4 C1 C2 C8 -2.7(6) . . . . ?
C1 C2 C3 C1 1.2(7) . . . 3_767 ?
C8 C2 C3 C1 -176.6(4) . . . 3_767 ?
C2 C1 C4 N1 179.4(4) . . . . ?
C3 C1 C4 N1 0.2(6) 3_767 . . . ?
N2 C6 C7 N1 0.8(5) . . . . ?
C3 C2 C8 N3 93.3(4) . . . . ?
C1 C2 C8 N3 -84.4(5) . . . . ?
N3 C9 C10 N4 -0.1(6) . . . . ?
N2 C5 N1 C7 0.3(5) . . . . ?
N2 C5 N1 C4 172.7(4) . . . . ?
C6 C7 N1 C5 -0.7(5) . . . . ?
C6 C7 N1 C4 -172.8(4) . . . . ?
C1 C4 N1 C5 -87.7(5) . . . . ?
C1 C4 N1 C7 83.0(6) . . . . ?
N1 C5 N2 C6 0.2(5) . . . . ?
N1 C5 N2 Cd1 -177.5(2) . . . 2_646 ?
C7 C6 N2 C5 -0.6(5) . . . . ?
C7 C6 N2 Cd1 177.0(3) . . . 2_646 ?
N4 C11 N3 C9 -0.2(5) . . . . ?
N4 C11 N3 C8 -173.1(4) . . . . ?
C10 C9 N3 C11 0.2(6) . . . . ?
C10 C9 N3 C8 173.0(4) . . . . ?
C2 C8 N3 C11 103.2(4) . . . . ?
C2 C8 N3 C9 -68.4(5) . . . . ?
N3 C11 N4 C10 0.1(5) . . . . ?
N3 C11 N4 Cd1 172.1(2) . . . . ?
C9 C10 N4 C11 0.0(6) . . . . ?
C9 C10 N4 Cd1 -171.3(3) . . . . ?
N2 Cd1 N4 C11 -116.6(3) 4_565 . . . ?
N2 Cd1 N4 C11 63.4(3) 2_656 . . . ?
N4 Cd1 N4 C11 -44(100) 3_666 . . . ?
Cl1 Cd1 N4 C11 152.8(3) 3_666 . . . ?
Cl1 Cd1 N4 C11 -27.2(3) . . . . ?
N2 Cd1 N4 C10 53.3(4) 4_565 . . . ?
N2 Cd1 N4 C10 -126.7(4) 2_656 . . . ?
N4 Cd1 N4 C10 125(100) 3_666 . . . ?
Cl1 Cd1 N4 C10 -37.3(4) 3_666 . . . ?
Cl1 Cd1 N4 C10 142.7(4) . . . . ?

_diffrn_measured_fraction_theta_max 1.000
_diffrn_reflns_theta_full        26.00
_diffrn_measured_fraction_theta_full 1.000
_refine_diff_density_max         0.731
_refine_diff_density_min         -0.722
_refine_diff_density_rms         0.092

#====END

data_5
_database_code_depnum_ccdc_archive 'CCDC 687827'
_audit_creation_date             'Sun Jul 1 13:46:32 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        
;
[Cd2(H2O)(SO4)2(L)2]-2(H2O)
;
_chemical_name_common            (Cd2(H2O)(SO4)2(L)2)-2(H2O)
_chemical_melting_point          ?
_chemical_formula_moiety         'C44 H50 Cd2 N16 O11 S2 '
_chemical_formula_sum            'C44 H50 Cd2 N16 O11 S2'
_chemical_formula_weight         1267.92

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'
S S 0.1246 0.1234 '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           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                   12.839(3)
_cell_length_b                   14.410(4)
_cell_length_c                   15.128(4)
_cell_angle_alpha                80.422(11)
_cell_angle_beta                 69.344(10)
_cell_angle_gamma                65.301(11)
_cell_volume                     2378.8(10)
_cell_formula_units_Z            2
_cell_measurement_temperature    200
_cell_measurement_reflns_used    17693
_cell_measurement_theta_min      3.1
_cell_measurement_theta_max      27.6

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.250
_exptl_crystal_size_mid          0.250
_exptl_crystal_size_min          0.100
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.770
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1284
_exptl_absorpt_coefficient_mu    1.062
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.690
_exptl_absorpt_correction_T_max  0.899
_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            22949
_diffrn_reflns_av_R_equivalents  0.0271
_diffrn_reflns_av_sigmaI/netI    0.0348
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         3.11
_diffrn_reflns_theta_max         27.49
_reflns_number_total             10864
_reflns_number_gt                9573
_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)+(0.0236P)²+1.9438P] 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         10864
_refine_ls_number_parameters     694
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0338
_refine_ls_R_factor_gt           0.0276
_refine_ls_wR_factor_ref         0.0637
_refine_ls_wR_factor_gt          0.0613
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_restrained_S_all      1.043
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Cd1 Cd 0.732703(13) 0.253375(11) 0.260525(11) 0.01570(4) Uani 1 1 d . . .
Cd2 Cd 0.213514(13) 0.236220(12) 0.275568(12) 0.01820(5) Uani 1 1 d . . .
S1 S 0.41033(5) 0.30071(4) 0.35253(4) 0.01810(11) Uani 1 1 d . . .
S2 S 0.06033(4) 0.18677(4) 0.18996(4) 0.01751(11) Uani 1 1 d . . .
O1 O 0.19214(15) 0.19490(14) 0.43217(12) 0.0247(4) Uani 1 1 d . . .
H1 H 0.221(2) 0.131(2) 0.437(2) 0.030 Uiso 1 1 d . . .
H2 H 0.245(2) 0.214(2) 0.4430(19) 0.030 Uiso 1 1 d . . .
O2 O 0.38890(16) 0.37713(16) 0.10459(14) 0.0319(4) Uani 1 1 d . . .
H3 H 0.333(3) 0.432(2) 0.104(2) 0.038 Uiso 1 1 d . . .
H4 H 0.374(3) 0.361(2) 0.157(2) 0.038 Uiso 1 1 d . . .
O3 O 0.3547(2) 0.25002(17) 0.00084(15) 0.0418(5) Uani 1 1 d . . .
H5 H 0.293(3) 0.244(3) 0.031(2) 0.050 Uiso 1 1 d . . .
H6 H 0.364(3) 0.288(3) 0.032(2) 0.050 Uiso 1 1 d . . .
O11 O 0.54071(15) 0.24542(14) 0.31210(16) 0.0407(5) Uani 1 1 d . . .
O12 O 0.38188(17) 0.40485(14) 0.37343(14) 0.0370(4) Uani 1 1 d . . .
O13 O 0.3625(2) 0.24781(17) 0.43818(13) 0.0443(5) Uani 1 1 d . . .
O14 O 0.35215(14) 0.30128(13) 0.28314(11) 0.0238(3) Uani 1 1 d . . .
O21 O 0.07974(14) 0.15979(13) 0.28425(11) 0.0236(3) Uani 1 1 d . . .
O22 O 0.13521(14) 0.24568(13) 0.13827(12) 0.0273(4) Uani 1 1 d . . .
O23 O -0.06802(13) 0.25123(13) 0.20361(12) 0.0247(4) Uani 1 1 d . . .
O24 O 0.09749(15) 0.09368(13) 0.14058(13) 0.0282(4) Uani 1 1 d . . .
N11 N 0.53530(16) 0.55394(14) 0.15017(13) 0.0191(4) Uani 1 1 d . . .
N12 N 0.65362(17) 0.41892(14) 0.20933(14) 0.0222(4) Uani 1 1 d . . .
N21 N 0.26059(15) 0.84410(13) 0.00781(12) 0.0150(3) Uani 1 1 d . . .
N22 N 0.24217(16) 0.80500(14) -0.11841(13) 0.0202(4) Uani 1 1 d . . .
N41 N -0.08293(16) 0.94142(14) 0.36240(13) 0.0180(4) Uani 1 1 d . . .
N42 N -0.19712(16) 1.08575(14) 0.31083(13) 0.0207(4) Uani 1 1 d . . .
N51 N 0.22320(15) 0.65027(13) 0.49481(12) 0.0155(4) Uani 1 1 d . . .
N52 N 0.27224(16) 0.69035(15) 0.60394(13) 0.0201(4) Uani 1 1 d . . .
N111 N -0.10012(16) 0.52068(14) 0.35550(14) 0.0208(4) Uani 1 1 d . . .
N112 N 0.07756(17) 0.39559(15) 0.30664(15) 0.0246(4) Uani 1 1 d . . .
N121 N -0.57973(16) 0.82955(15) 0.41031(13) 0.0216(4) Uani 1 1 d . . .
N122 N -0.71504(18) 0.98716(17) 0.43571(16) 0.0310(5) Uani 1 1 d . . .
N141 N -0.43660(15) 1.00123(14) 0.13465(13) 0.0183(4) Uani 1 1 d . . .
N142 N -0.62194(16) 1.11030(14) 0.19651(14) 0.0200(4) Uani 1 1 d . . .
N151 N 0.03731(17) 0.68178(17) 0.05997(15) 0.0309(5) Uani 1 1 d . . .
N152 N 0.1982(2) 0.5519(2) 0.07724(19) 0.0472(7) Uani 1 1 d . . .
C1 C 0.32836(18) 0.68582(16) 0.18529(15) 0.0164(4) Uani 1 1 d . . .
C2 C 0.26829(18) 0.79000(16) 0.16976(15) 0.0153(4) Uani 1 1 d . . .
C3 C 0.16437(18) 0.84590(17) 0.23941(15) 0.0171(4) Uani 1 1 d . . .
H7 H 0.1220 0.9162 0.2274 0.020 Uiso 1 1 calc R . .
C4 C 0.12041(18) 0.80229(17) 0.32605(15) 0.0163(4) Uani 1 1 d . . .
C5 C 0.18295(18) 0.69916(16) 0.34342(15) 0.0152(4) Uani 1 1 d . . .
C6 C 0.28411(19) 0.64226(16) 0.27180(15) 0.0178(4) Uani 1 1 d . . .
H8 H 0.3242 0.5712 0.2826 0.021 Uiso 1 1 calc R . .
C11 C 0.43795(19) 0.61756(18) 0.11166(16) 0.0225(5) Uani 1 1 d . . .
H9 H 0.4143 0.5732 0.0860 0.027 Uiso 1 1 calc R . .
H10 H 0.4674 0.6605 0.0589 0.027 Uiso 1 1 calc R . .
C12 C 0.5640(2) 0.45464(17) 0.17374(17) 0.0218(5) Uani 1 1 d . . .
H11 H 0.5246 0.4150 0.1658 0.026 Uiso 1 1 calc R . .
C13 C 0.6828(2) 0.5001(2) 0.2080(2) 0.0314(6) Uani 1 1 d . . .
H12 H 0.7455 0.4976 0.2291 0.038 Uiso 1 1 calc R . .
C14 C 0.6104(2) 0.58402(19) 0.17273(19) 0.0293(5) Uani 1 1 d . . .
H13 H 0.6113 0.6505 0.1651 0.035 Uiso 1 1 calc R . .
C21 C 0.31128(19) 0.84600(16) 0.07989(14) 0.0167(4) Uani 1 1 d . . .
H14 H 0.2880 0.9178 0.0944 0.020 Uiso 1 1 calc R . .
H15 H 0.4006 0.8142 0.0547 0.020 Uiso 1 1 calc R . .
C22 C 0.31591(19) 0.78836(17) -0.07023(15) 0.0191(4) Uani 1 1 d . . .
H16 H 0.3983 0.7425 -0.0885 0.023 Uiso 1 1 calc R . .
C23 C 0.13322(19) 0.87510(18) -0.06793(16) 0.0216(5) Uani 1 1 d . . .
H17 H 0.0616 0.9018 -0.0852 0.026 Uiso 1 1 calc R . .
C24 C 0.14305(19) 0.90043(18) 0.00992(16) 0.0213(5) Uani 1 1 d . . .
H18 H 0.0814 0.9475 0.0566 0.026 Uiso 1 1 calc R . .
C41 C 0.01096(19) 0.86950(18) 0.40089(16) 0.0216(5) Uani 1 1 d . . .
H19 H -0.0227 0.8257 0.4498 0.026 Uiso 1 1 calc R . .
H20 H 0.0366 0.9079 0.4318 0.026 Uiso 1 1 calc R . .
C42 C -0.10399(19) 1.03995(17) 0.34269(16) 0.0198(4) Uani 1 1 d . . .
H21 H -0.0577 1.0731 0.3506 0.024 Uiso 1 1 calc R . .
C43 C -0.2377(2) 1.01092(19) 0.31154(17) 0.0252(5) Uani 1 1 d . . .
H22 H -0.3050 1.0208 0.2929 0.030 Uiso 1 1 calc R . .
C44 C -0.1681(2) 0.92206(18) 0.34236(17) 0.0251(5) Uani 1 1 d . . .
H23 H -0.1761 0.8584 0.3490 0.030 Uiso 1 1 calc R . .
C51 C 0.15243(19) 0.64686(16) 0.43842(15) 0.0165(4) Uani 1 1 d . . .
H24 H 0.0652 0.6810 0.4727 0.020 Uiso 1 1 calc R . .
H25 H 0.1696 0.5748 0.4293 0.020 Uiso 1 1 calc R . .
C52 C 0.18354(19) 0.70738(17) 0.57045(15) 0.0183(4) Uani 1 1 d . . .
H26 H 0.1025 0.7539 0.5965 0.022 Uiso 1 1 calc R . .
C53 C 0.37262(19) 0.61878(17) 0.54665(16) 0.0202(4) Uani 1 1 d . . .
H27 H 0.4508 0.5912 0.5535 0.024 Uiso 1 1 calc R . .
C54 C 0.34402(19) 0.59316(17) 0.47873(16) 0.0207(5) Uani 1 1 d . . .
H28 H 0.3968 0.5454 0.4300 0.025 Uiso 1 1 calc R . .
C101 C -0.24654(19) 0.67682(17) 0.30378(16) 0.0184(4) Uani 1 1 d . . .
C102 C -0.36217(18) 0.75446(17) 0.32075(15) 0.0180(4) Uani 1 1 d . . .
C103 C -0.37935(19) 0.83824(17) 0.26043(16) 0.0196(4) Uani 1 1 d . . .
H29 H -0.4575 0.8915 0.2726 0.024 Uiso 1 1 calc R . .
C104 C -0.28601(19) 0.84748(17) 0.18227(16) 0.0181(4) Uani 1 1 d . . .
C105 C -0.17127(19) 0.76874(17) 0.16423(16) 0.0195(4) Uani 1 1 d . . .
C106 C -0.15380(19) 0.68531(17) 0.22567(16) 0.0208(5) Uani 1 1 d . . .
H30 H -0.0756 0.6322 0.2139 0.025 Uiso 1 1 calc R . .
C111 C -0.22769(19) 0.58641(17) 0.37176(17) 0.0222(5) Uani 1 1 d . . .
H31 H -0.2637 0.6115 0.4372 0.027 Uiso 1 1 calc R . .
H32 H -0.2704 0.5456 0.3655 0.027 Uiso 1 1 calc R . .
C112 C -0.0356(2) 0.43373(17) 0.30690(17) 0.0214(5) Uani 1 1 d . . .
H33 H -0.0672 0.4037 0.2768 0.026 Uiso 1 1 calc R . .
C113 C 0.0853(2) 0.4628(2) 0.3562(2) 0.0352(6) Uani 1 1 d . . .
H34 H 0.1565 0.4560 0.3674 0.042 Uiso 1 1 calc R . .
C114 C -0.0236(2) 0.53990(19) 0.3867(2) 0.0339(6) Uani 1 1 d . . .
H35 H -0.0432 0.5964 0.4227 0.041 Uiso 1 1 calc R . .
C121 C -0.46562(19) 0.74329(19) 0.40295(17) 0.0238(5) Uani 1 1 d . . .
H36 H -0.4742 0.6801 0.3957 0.029 Uiso 1 1 calc R . .
H37 H -0.4464 0.7361 0.4622 0.029 Uiso 1 1 calc R . .
C122 C -0.6194(2) 0.9165(2) 0.45496(17) 0.0281(5) Uani 1 1 d . . .
H38 H -0.5830 0.9261 0.4957 0.034 Uiso 1 1 calc R . .
C123 C -0.7361(2) 0.94193(19) 0.37425(18) 0.0284(5) Uani 1 1 d . . .
H39 H -0.7992 0.9741 0.3469 0.034 Uiso 1 1 calc R . .
C124 C -0.6535(2) 0.84454(19) 0.35835(18) 0.0256(5) Uani 1 1 d . . .
H40 H -0.6481 0.7966 0.3191 0.031 Uiso 1 1 calc R . .
C141 C -0.30793(18) 0.94094(17) 0.11821(17) 0.0210(5) Uani 1 1 d . . .
H41 H -0.2703 0.9838 0.1290 0.025 Uiso 1 1 calc R . .
H42 H -0.2691 0.9196 0.0516 0.025 Uiso 1 1 calc R . .
C142 C -0.50743(19) 1.08498(17) 0.18745(16) 0.0199(4) Uani 1 1 d . . .
H43 H -0.4789 1.1209 0.2144 0.024 Uiso 1 1 calc R . .
C143 C -0.6242(2) 1.03895(18) 0.14813(17) 0.0241(5) Uani 1 1 d . . .
H44 H -0.6951 1.0379 0.1424 0.029 Uiso 1 1 calc R . .
C144 C -0.5103(2) 0.97015(18) 0.10978(17) 0.0232(5) Uani 1 1 d . . .
H45 H -0.4864 0.9127 0.0734 0.028 Uiso 1 1 calc R . .
C151 C -0.0678(2) 0.7776(2) 0.08023(19) 0.0319(6) Uani 1 1 d . . .
H46 H -0.0954 0.8004 0.0240 0.038 Uiso 1 1 calc R . .
H47 H -0.0444 0.8302 0.0928 0.038 Uiso 1 1 calc R . .
C152 C 0.1271(2) 0.6467(2) 0.0981(2) 0.0385(7) Uani 1 1 d . . .
H48 H 0.1375 0.6865 0.1359 0.046 Uiso 1 1 calc R . .
C153 C 0.1496(3) 0.5241(3) 0.0239(2) 0.0597(10) Uani 1 1 d . . .
H49 H 0.1809 0.4583 -0.0016 0.072 Uiso 1 1 calc R . .
C154 C 0.0510(3) 0.6035(3) 0.0126(2) 0.0524(9) Uani 1 1 d . . .
H50 H 0.0012 0.6043 -0.0217 0.063 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 2.288(2) . ?
Cd1 N42 2.298(2) 1_645 ?
Cd1 N52 2.2989(19) 2_666 ?
Cd1 N22 2.3065(19) 2_665 ?
Cd1 O11 2.3554(17) . ?
Cd1 O23 2.3826(15) 1_655 ?
Cd2 N142 2.2187(19) 1_645 ?
Cd2 N112 2.230(2) . ?
Cd2 O1 2.2915(18) . ?
Cd2 O21 2.3566(16) . ?
Cd2 O14 2.3738(15) . ?
Cd2 O22 2.5707(18) . ?
S1 O12 1.4504(18) . ?
S1 O11 1.4616(18) . ?
S1 O13 1.4623(19) . ?
S1 O14 1.4851(16) . ?
S2 O24 1.4602(17) . ?
S2 O23 1.4717(16) . ?
S2 O22 1.4789(17) . ?
S2 O21 1.4944(17) . ?
O1 H1 0.84(3) . ?
O1 H2 0.90(3) . ?
O2 H3 0.82(3) . ?
O2 H4 0.76(3) . ?
O3 H5 0.79(3) . ?
O3 H6 0.85(3) . ?
O23 Cd1 2.3826(15) 1_455 ?
N11 C12 1.339(3) . ?
N11 C14 1.365(3) . ?
N11 C11 1.456(3) . ?
N12 C12 1.315(3) . ?
N12 C13 1.365(3) . ?
N21 C22 1.338(3) . ?
N21 C24 1.374(3) . ?
N21 C21 1.462(3) . ?
N22 C22 1.313(3) . ?
N22 C23 1.372(3) . ?
N22 Cd1 2.3065(19) 2_665 ?
N41 C42 1.332(3) . ?
N41 C44 1.372(3) . ?
N41 C41 1.455(3) . ?
N42 C42 1.319(3) . ?
N42 C43 1.377(3) . ?
N42 Cd1 2.298(2) 1_465 ?
N51 C52 1.341(3) . ?
N51 C54 1.370(3) . ?
N51 C51 1.468(3) . ?
N52 C52 1.321(3) . ?
N52 C53 1.369(3) . ?
N52 Cd1 2.2987(19) 2_666 ?
N111 C112 1.344(3) . ?
N111 C114 1.365(3) . ?
N111 C111 1.462(3) . ?
N112 C112 1.320(3) . ?
N112 C113 1.373(3) . ?
N121 C122 1.338(3) . ?
N121 C124 1.363(3) . ?
N121 C121 1.454(3) . ?
N122 C122 1.319(3) . ?
N122 C123 1.374(3) . ?
N141 C142 1.346(3) . ?
N141 C144 1.378(3) . ?
N141 C141 1.459(3) . ?
N142 C142 1.319(3) . ?
N142 C143 1.373(3) . ?
N142 Cd2 2.2186(19) 1_465 ?
N151 C152 1.342(3) . ?
N151 C154 1.354(4) . ?
N151 C151 1.454(3) . ?
N152 C152 1.303(4) . ?
N152 C153 1.368(5) . ?
C1 C6 1.389(3) . ?
C1 C2 1.395(3) . ?
C1 C11 1.513(3) . ?
C2 C3 1.390(3) . ?
C2 C21 1.511(3) . ?
C3 C4 1.390(3) . ?
C3 H7 0.9500 . ?
C4 C5 1.394(3) . ?
C4 C41 1.516(3) . ?
C5 C6 1.395(3) . ?
C5 C51 1.509(3) . ?
C6 H8 0.9500 . ?
C11 H9 0.9900 . ?
C11 H10 0.9900 . ?
C12 H11 0.9500 . ?
C13 C14 1.345(4) . ?
C13 H12 0.9500 . ?
C14 H13 0.9500 . ?
C21 H14 0.9900 . ?
C21 H15 0.9900 . ?
C22 H16 0.9500 . ?
C23 C24 1.350(3) . ?
C23 H17 0.9500 . ?
C24 H18 0.9500 . ?
C41 H19 0.9900 . ?
C41 H20 0.9900 . ?
C42 H21 0.9500 . ?
C43 C44 1.340(3) . ?
C43 H22 0.9500 . ?
C44 H23 0.9500 . ?
C51 H24 0.9900 . ?
C51 H25 0.9900 . ?
C52 H26 0.9500 . ?
C53 C54 1.354(3) . ?
C53 H27 0.9500 . ?
C54 H28 0.9500 . ?
C101 C106 1.382(3) . ?
C101 C102 1.400(3) . ?
C101 C111 1.510(3) . ?
C102 C103 1.375(3) . ?
C102 C121 1.511(3) . ?
C103 C104 1.390(3) . ?
C103 H29 0.9500 . ?
C104 C105 1.398(3) . ?
C104 C141 1.508(3) . ?
C105 C106 1.382(3) . ?
C105 C151 1.514(3) . ?
C106 H30 0.9500 . ?
C111 H31 0.9900 . ?
C111 H32 0.9900 . ?
C112 H33 0.9500 . ?
C113 C114 1.349(3) . ?
C113 H34 0.9500 . ?
C114 H35 0.9500 . ?
C121 H36 0.9900 . ?
C121 H37 0.9900 . ?
C122 H38 0.9500 . ?
C123 C124 1.357(3) . ?
C123 H39 0.9500 . ?
C124 H40 0.9500 . ?
C141 H41 0.9900 . ?
C141 H42 0.9900 . ?
C142 H43 0.9500 . ?
C143 C144 1.356(3) . ?
C143 H44 0.9500 . ?
C144 H45 0.9500 . ?
C151 H46 0.9900 . ?
C151 H47 0.9900 . ?
C152 H48 0.9500 . ?
C153 C154 1.349(4) . ?
C153 H49 0.9500 . ?
C154 H50 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
N12 Cd1 N42 176.63(6) . 1_645 ?
N12 Cd1 N52 90.04(7) . 2_666 ?
N42 Cd1 N52 91.87(7) 1_645 2_666 ?
N12 Cd1 N22 90.58(7) . 2_665 ?
N42 Cd1 N22 87.79(7) 1_645 2_665 ?
N52 Cd1 N22 174.20(6) 2_666 2_665 ?
N12 Cd1 O11 90.69(7) . . ?
N42 Cd1 O11 86.26(7) 1_645 . ?
N52 Cd1 O11 99.60(7) 2_666 . ?
N22 Cd1 O11 86.15(7) 2_665 . ?
N12 Cd1 O23 91.78(6) . 1_655 ?
N42 Cd1 O23 91.19(6) 1_645 1_655 ?
N52 Cd1 O23 83.10(6) 2_666 1_655 ?
N22 Cd1 O23 91.12(6) 2_665 1_655 ?
O11 Cd1 O23 176.34(6) . 1_655 ?
N142 Cd2 N112 157.74(7) 1_645 . ?
N142 Cd2 O1 105.59(7) 1_645 . ?
N112 Cd2 O1 92.80(7) . . ?
N142 Cd2 O21 94.99(6) 1_645 . ?
N112 Cd2 O21 97.83(7) . . ?
O1 Cd2 O21 88.98(6) . . ?
N142 Cd2 O14 84.40(6) 1_645 . ?
N112 Cd2 O14 84.95(7) . . ?
O1 Cd2 O14 84.63(6) . . ?
O21 Cd2 O14 173.15(6) . . ?
N142 Cd2 O22 85.25(6) 1_645 . ?
N112 Cd2 O22 86.43(7) . . ?
O1 Cd2 O22 145.79(6) . . ?
O21 Cd2 O22 57.40(5) . . ?
O14 Cd2 O22 129.22(5) . . ?
O12 S1 O11 110.96(11) . . ?
O12 S1 O13 110.16(13) . . ?
O11 S1 O13 110.22(13) . . ?
O12 S1 O14 109.70(11) . . ?
O11 S1 O14 108.28(11) . . ?
O13 S1 O14 107.44(10) . . ?
O24 S2 O23 111.00(10) . . ?
O24 S2 O22 111.21(10) . . ?
O23 S2 O22 109.76(10) . . ?
O24 S2 O21 109.77(10) . . ?
O23 S2 O21 109.03(10) . . ?
O22 S2 O21 105.93(9) . . ?
Cd2 O1 H1 106.8(19) . . ?
Cd2 O1 H2 103.5(18) . . ?
H1 O1 H2 105(2) . . ?
H3 O2 H4 103(3) . . ?
H5 O3 H6 106(3) . . ?
S1 O11 Cd1 146.50(12) . . ?
S1 O14 Cd2 137.08(10) . . ?
S2 O21 Cd2 102.64(8) . . ?
S2 O22 Cd2 94.02(8) . . ?
S2 O23 Cd1 144.53(10) . 1_455 ?
C12 N11 C14 107.29(19) . . ?
C12 N11 C11 125.46(19) . . ?
C14 N11 C11 127.2(2) . . ?
C12 N12 C13 105.2(2) . . ?
C12 N12 Cd1 123.82(15) . . ?
C13 N12 Cd1 130.97(16) . . ?
C22 N21 C24 107.12(17) . . ?
C22 N21 C21 128.06(18) . . ?
C24 N21 C21 124.82(18) . . ?
C22 N22 C23 105.54(18) . . ?
C22 N22 Cd1 133.28(15) . 2_665 ?
C23 N22 Cd1 121.12(14) . 2_665 ?
C42 N41 C44 107.22(19) . . ?
C42 N41 C41 125.77(19) . . ?
C44 N41 C41 126.98(19) . . ?
C42 N42 C43 105.10(19) . . ?
C42 N42 Cd1 125.98(15) . 1_465 ?
C43 N42 Cd1 128.88(15) . 1_465 ?
C52 N51 C54 107.66(18) . . ?
C52 N51 C51 127.42(18) . . ?
C54 N51 C51 124.92(18) . . ?
C52 N52 C53 105.70(18) . . ?
C52 N52 Cd1 130.11(15) . 2_666 ?
C53 N52 Cd1 123.75(14) . 2_666 ?
C112 N111 C114 107.39(19) . . ?
C112 N111 C111 127.99(19) . . ?
C114 N111 C111 124.6(2) . . ?
C112 N112 C113 105.7(2) . . ?
C112 N112 Cd2 127.85(15) . . ?
C113 N112 Cd2 123.91(15) . . ?
C122 N121 C124 107.3(2) . . ?
C122 N121 C121 125.9(2) . . ?
C124 N121 C121 125.6(2) . . ?
C122 N122 C123 104.8(2) . . ?
C142 N141 C144 107.84(18) . . ?
C142 N141 C141 127.89(19) . . ?
C144 N141 C141 123.50(19) . . ?
C142 N142 C143 106.21(18) . . ?
C142 N142 Cd2 130.14(15) . 1_465 ?
C143 N142 Cd2 123.61(14) . 1_465 ?
C152 N151 C154 106.8(2) . . ?
C152 N151 C151 126.9(3) . . ?
C154 N151 C151 125.3(2) . . ?
C152 N152 C153 104.6(3) . . ?
C6 C1 C2 118.45(19) . . ?
C6 C1 C11 118.4(2) . . ?
C2 C1 C11 123.1(2) . . ?
C3 C2 C1 119.3(2) . . ?
C3 C2 C21 117.79(19) . . ?
C1 C2 C21 122.88(19) . . ?
C2 C3 C4 122.1(2) . . ?
C2 C3 H7 118.9 . . ?
C4 C3 H7 118.9 . . ?
C3 C4 C5 118.75(19) . . ?
C3 C4 C41 119.2(2) . . ?
C5 C4 C41 121.98(19) . . ?
C4 C5 C6 118.9(2) . . ?
C4 C5 C51 123.33(19) . . ?
C6 C5 C51 117.60(19) . . ?
C1 C6 C5 122.3(2) . . ?
C1 C6 H8 118.8 . . ?
C5 C6 H8 118.8 . . ?
N11 C11 C1 112.17(18) . . ?
N11 C11 H9 109.2 . . ?
C1 C11 H9 109.2 . . ?
N11 C11 H10 109.2 . . ?
C1 C11 H10 109.2 . . ?
H9 C11 H10 107.9 . . ?
N12 C12 N11 111.3(2) . . ?
N12 C12 H11 124.3 . . ?
N11 C12 H11 124.3 . . ?
C14 C13 N12 110.4(2) . . ?
C14 C13 H12 124.8 . . ?
N12 C13 H12 124.8 . . ?
C13 C14 N11 105.8(2) . . ?
C13 C14 H13 127.1 . . ?
N11 C14 H13 127.1 . . ?
N21 C21 C2 112.21(17) . . ?
N21 C21 H14 109.2 . . ?
C2 C21 H14 109.2 . . ?
N21 C21 H15 109.2 . . ?
C2 C21 H15 109.2 . . ?
H14 C21 H15 107.9 . . ?
N22 C22 N21 111.59(19) . . ?
N22 C22 H16 124.2 . . ?
N21 C22 H16 124.2 . . ?
C24 C23 N22 109.84(19) . . ?
C24 C23 H17 125.1 . . ?
N22 C23 H17 125.1 . . ?
C23 C24 N21 105.91(19) . . ?
C23 C24 H18 127.0 . . ?
N21 C24 H18 127.0 . . ?
N41 C41 C4 112.68(18) . . ?
N41 C41 H19 109.1 . . ?
C4 C41 H19 109.1 . . ?
N41 C41 H20 109.1 . . ?
C4 C41 H20 109.1 . . ?
H19 C41 H20 107.8 . . ?
N42 C42 N41 111.6(2) . . ?
N42 C42 H21 124.2 . . ?
N41 C42 H21 124.2 . . ?
C44 C43 N42 109.9(2) . . ?
C44 C43 H22 125.1 . . ?
N42 C43 H22 125.1 . . ?
C43 C44 N41 106.2(2) . . ?
C43 C44 H23 126.9 . . ?
N41 C44 H23 126.9 . . ?
N51 C51 C5 110.80(17) . . ?
N51 C51 H24 109.5 . . ?
C5 C51 H24 109.5 . . ?
N51 C51 H25 109.5 . . ?
C5 C51 H25 109.5 . . ?
H24 C51 H25 108.1 . . ?
N52 C52 N51 110.94(19) . . ?
N52 C52 H26 124.5 . . ?
N51 C52 H26 124.5 . . ?
C54 C53 N52 109.94(19) . . ?
C54 C53 H27 125.0 . . ?
N52 C53 H27 125.0 . . ?
C53 C54 N51 105.77(19) . . ?
C53 C54 H28 127.1 . . ?
N51 C54 H28 127.1 . . ?
C106 C101 C102 119.1(2) . . ?
C106 C101 C111 122.27(19) . . ?
C102 C101 C111 118.61(19) . . ?
C103 C102 C101 118.9(2) . . ?
C103 C102 C121 121.51(19) . . ?
C101 C102 C121 119.5(2) . . ?
C102 C103 C104 122.1(2) . . ?
C102 C103 H29 119.0 . . ?
C104 C103 H29 119.0 . . ?
C103 C104 C105 118.9(2) . . ?
C103 C104 C141 120.62(19) . . ?
C105 C104 C141 120.51(19) . . ?
C106 C105 C104 118.9(2) . . ?
C106 C105 C151 121.2(2) . . ?
C104 C105 C151 119.9(2) . . ?
C105 C106 C101 122.0(2) . . ?
C105 C106 H30 119.0 . . ?
C101 C106 H30 119.0 . . ?
N111 C111 C101 112.77(18) . . ?
N111 C111 H31 109.0 . . ?
C101 C111 H31 109.0 . . ?
N111 C111 H32 109.0 . . ?
C101 C111 H32 109.0 . . ?
H31 C111 H32 107.8 . . ?
N112 C112 N111 110.9(2) . . ?
N112 C112 H33 124.5 . . ?
N111 C112 H33 124.5 . . ?
C114 C113 N112 109.6(2) . . ?
C114 C113 H34 125.2 . . ?
N112 C113 H34 125.2 . . ?
C113 C114 N111 106.4(2) . . ?
C113 C114 H35 126.8 . . ?
N111 C114 H35 126.8 . . ?
N121 C121 C102 112.84(19) . . ?
N121 C121 H36 109.0 . . ?
C102 C121 H36 109.0 . . ?
N121 C121 H37 109.0 . . ?
C102 C121 H37 109.0 . . ?
H36 C121 H37 107.8 . . ?
N122 C122 N121 111.9(2) . . ?
N122 C122 H38 124.0 . . ?
N121 C122 H38 124.0 . . ?
C124 C123 N122 110.1(2) . . ?
C124 C123 H39 125.0 . . ?
N122 C123 H39 125.0 . . ?
C123 C124 N121 105.9(2) . . ?
C123 C124 H40 127.1 . . ?
N121 C124 H40 127.1 . . ?
N141 C141 C104 111.83(17) . . ?
N141 C141 H41 109.3 . . ?
C104 C141 H41 109.3 . . ?
N141 C141 H42 109.3 . . ?
C104 C141 H42 109.3 . . ?
H41 C141 H42 107.9 . . ?
N142 C142 N141 110.59(19) . . ?
N142 C142 H43 124.7 . . ?
N141 C142 H43 124.7 . . ?
C144 C143 N142 109.9(2) . . ?
C144 C143 H44 125.1 . . ?
N142 C143 H44 125.1 . . ?
C143 C144 N141 105.5(2) . . ?
C143 C144 H45 127.3 . . ?
N141 C144 H45 127.3 . . ?
N151 C151 C105 112.7(2) . . ?
N151 C151 H46 109.1 . . ?
C105 C151 H46 109.1 . . ?
N151 C151 H47 109.1 . . ?
C105 C151 H47 109.1 . . ?
H46 C151 H47 107.8 . . ?
N152 C152 N151 112.3(3) . . ?
N152 C152 H48 123.8 . . ?
N151 C152 H48 123.8 . . ?
C154 C153 N152 110.3(3) . . ?
C154 C153 H49 124.8 . . ?
N152 C153 H49 124.8 . . ?
C153 C154 N151 106.0(3) . . ?
C153 C154 H50 127.0 . . ?
N151 C154 H50 127.0 . . ?

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
O12 S1 O11 Cd1 -2.4(3) . . . . ?
O13 S1 O11 Cd1 -124.7(2) . . . . ?
O14 S1 O11 Cd1 118.1(2) . . . . ?
N12 Cd1 O11 S1 -33.9(3) . . . . ?
N42 Cd1 O11 S1 147.5(3) 1_645 . . . ?
N52 Cd1 O11 S1 56.3(3) 2_666 . . . ?
N22 Cd1 O11 S1 -124.4(3) 2_665 . . . ?
O12 S1 O14 Cd2 -122.25(15) . . . . ?
O11 S1 O14 Cd2 116.53(15) . . . . ?
O13 S1 O14 Cd2 -2.50(19) . . . . ?
N142 Cd2 O14 S1 -98.24(15) 1_645 . . . ?
N112 Cd2 O14 S1 101.34(16) . . . . ?
O1 Cd2 O14 S1 8.05(15) . . . . ?
O22 Cd2 O14 S1 -177.44(12) . . . . ?
O24 S2 O21 Cd2 121.06(9) . . . . ?
O23 S2 O21 Cd2 -117.16(9) . . . . ?
O22 S2 O21 Cd2 0.90(10) . . . . ?
N142 Cd2 O21 S2 -81.70(9) 1_645 . . . ?
N112 Cd2 O21 S2 80.06(10) . . . . ?
O1 Cd2 O21 S2 172.74(9) . . . . ?
O22 Cd2 O21 S2 -0.59(7) . . . . ?
O24 S2 O22 Cd2 -120.03(9) . . . . ?
O23 S2 O22 Cd2 116.76(9) . . . . ?
O21 S2 O22 Cd2 -0.81(9) . . . . ?
N142 Cd2 O22 S2 99.61(9) 1_645 . . . ?
N112 Cd2 O22 S2 -101.06(9) . . . . ?
O1 Cd2 O22 S2 -11.33(15) . . . . ?
O21 Cd2 O22 S2 0.59(7) . . . . ?
O14 Cd2 O22 S2 178.42(7) . . . . ?
O24 S2 O23 Cd1 51.5(2) . . . 1_455 ?
O22 S2 O23 Cd1 174.84(16) . . . 1_455 ?
O21 S2 O23 Cd1 -69.54(19) . . . 1_455 ?
N52 Cd1 N12 C12 -133.65(19) 2_666 . . . ?
N22 Cd1 N12 C12 52.11(19) 2_665 . . . ?
O11 Cd1 N12 C12 -34.04(19) . . . . ?
O23 Cd1 N12 C12 143.25(19) 1_655 . . . ?
N52 Cd1 N12 C13 45.8(2) 2_666 . . . ?
N22 Cd1 N12 C13 -128.4(2) 2_665 . . . ?
O11 Cd1 N12 C13 145.4(2) . . . . ?
O23 Cd1 N12 C13 -37.3(2) 1_655 . . . ?
N142 Cd2 N112 C112 111.2(2) 1_645 . . . ?
O1 Cd2 N112 C112 -102.8(2) . . . . ?
O21 Cd2 N112 C112 -13.4(2) . . . . ?
O14 Cd2 N112 C112 172.8(2) . . . . ?
O22 Cd2 N112 C112 42.9(2) . . . . ?
N142 Cd2 N112 C113 -89.6(3) 1_645 . . . ?
O1 Cd2 N112 C113 56.4(2) . . . . ?
O21 Cd2 N112 C113 145.8(2) . . . . ?
O14 Cd2 N112 C113 -27.9(2) . . . . ?
O22 Cd2 N112 C113 -157.8(2) . . . . ?
C6 C1 C2 C3 -2.3(3) . . . . ?
C11 C1 C2 C3 176.49(19) . . . . ?
C6 C1 C2 C21 177.57(18) . . . . ?
C11 C1 C2 C21 -3.7(3) . . . . ?
C1 C2 C3 C4 2.5(3) . . . . ?
C21 C2 C3 C4 -177.29(18) . . . . ?
C2 C3 C4 C5 0.1(3) . . . . ?
C2 C3 C4 C41 176.24(19) . . . . ?
C3 C4 C5 C6 -2.9(3) . . . . ?
C41 C4 C5 C6 -178.95(19) . . . . ?
C3 C4 C5 C51 172.54(19) . . . . ?
C41 C4 C5 C51 -3.5(3) . . . . ?
C2 C1 C6 C5 -0.6(3) . . . . ?
C11 C1 C6 C5 -179.41(19) . . . . ?
C4 C5 C6 C1 3.2(3) . . . . ?
C51 C5 C6 C1 -172.49(19) . . . . ?
C12 N11 C11 C1 102.5(3) . . . . ?
C14 N11 C11 C1 -74.5(3) . . . . ?
C6 C1 C11 N11 -49.0(3) . . . . ?
C2 C1 C11 N11 132.2(2) . . . . ?
C13 N12 C12 N11 0.0(3) . . . . ?
Cd1 N12 C12 N11 179.58(14) . . . . ?
C14 N11 C12 N12 -0.5(3) . . . . ?
C11 N11 C12 N12 -178.02(19) . . . . ?
C12 N12 C13 C14 0.6(3) . . . . ?
Cd1 N12 C13 C14 -178.98(17) . . . . ?
N12 C13 C14 N11 -0.9(3) . . . . ?
C12 N11 C14 C13 0.9(3) . . . . ?
C11 N11 C14 C13 178.3(2) . . . . ?
C22 N21 C21 C2 -105.1(2) . . . . ?
C24 N21 C21 C2 73.8(3) . . . . ?
C3 C2 C21 N21 -91.0(2) . . . . ?
C1 C2 C21 N21 89.2(2) . . . . ?
C23 N22 C22 N21 -0.3(3) . . . . ?
Cd1 N22 C22 N21 176.92(15) 2_665 . . . ?
C24 N21 C22 N22 0.0(3) . . . . ?
C21 N21 C22 N22 179.1(2) . . . . ?
C22 N22 C23 C24 0.4(3) . . . . ?
Cd1 N22 C23 C24 -177.19(16) 2_665 . . . ?
N22 C23 C24 N21 -0.4(3) . . . . ?
C22 N21 C24 C23 0.2(3) . . . . ?
C21 N21 C24 C23 -178.9(2) . . . . ?
C42 N41 C41 C4 -100.6(3) . . . . ?
C44 N41 C41 C4 81.5(3) . . . . ?
C3 C4 C41 N41 42.7(3) . . . . ?
C5 C4 C41 N41 -141.2(2) . . . . ?
C43 N42 C42 N41 0.6(3) . . . . ?
Cd1 N42 C42 N41 -177.26(14) 1_465 . . . ?
C44 N41 C42 N42 -0.2(3) . . . . ?
C41 N41 C42 N42 -178.42(19) . . . . ?
C42 N42 C43 C44 -0.8(3) . . . . ?
Cd1 N42 C43 C44 177.00(16) 1_465 . . . ?
N42 C43 C44 N41 0.6(3) . . . . ?
C42 N41 C44 C43 -0.3(3) . . . . ?
C41 N41 C44 C43 177.9(2) . . . . ?
C52 N51 C51 C5 107.4(2) . . . . ?
C54 N51 C51 C5 -73.2(3) . . . . ?
C4 C5 C51 N51 -91.8(2) . . . . ?
C6 C5 C51 N51 83.7(2) . . . . ?
C53 N52 C52 N51 -0.2(3) . . . . ?
Cd1 N52 C52 N51 -172.56(14) 2_666 . . . ?
C54 N51 C52 N52 0.1(3) . . . . ?
C51 N51 C52 N52 179.55(19) . . . . ?
C52 N52 C53 C54 0.1(3) . . . . ?
Cd1 N52 C53 C54 173.16(15) 2_666 . . . ?
N52 C53 C54 N51 -0.1(3) . . . . ?
C52 N51 C54 C53 0.0(2) . . . . ?
C51 N51 C54 C53 -179.47(19) . . . . ?
C106 C101 C102 C103 -1.7(3) . . . . ?
C111 C101 C102 C103 178.4(2) . . . . ?
C106 C101 C102 C121 176.8(2) . . . . ?
C111 C101 C102 C121 -3.2(3) . . . . ?
C101 C102 C103 C104 1.1(3) . . . . ?
C121 C102 C103 C104 -177.3(2) . . . . ?
C102 C103 C104 C105 0.4(3) . . . . ?
C102 C103 C104 C141 -179.4(2) . . . . ?
C103 C104 C105 C106 -1.3(3) . . . . ?
C141 C104 C105 C106 178.5(2) . . . . ?
C103 C104 C105 C151 -179.3(2) . . . . ?
C141 C104 C105 C151 0.5(3) . . . . ?
C104 C105 C106 C101 0.7(3) . . . . ?
C151 C105 C106 C101 178.7(2) . . . . ?
C102 C101 C106 C105 0.8(3) . . . . ?
C111 C101 C106 C105 -179.3(2) . . . . ?
C112 N111 C111 C101 -97.7(3) . . . . ?
C114 N111 C111 C101 80.6(3) . . . . ?
C106 C101 C111 N111 10.2(3) . . . . ?
C102 C101 C111 N111 -169.9(2) . . . . ?
C113 N112 C112 N111 -1.0(3) . . . . ?
Cd2 N112 C112 N111 161.18(16) . . . . ?
C114 N111 C112 N112 1.0(3) . . . . ?
C111 N111 C112 N112 179.5(2) . . . . ?
C112 N112 C113 C114 0.7(3) . . . . ?
Cd2 N112 C113 C114 -162.4(2) . . . . ?
N112 C113 C114 N111 -0.1(3) . . . . ?
C112 N111 C114 C113 -0.5(3) . . . . ?
C111 N111 C114 C113 -179.1(2) . . . . ?
C122 N121 C121 C102 -86.0(3) . . . . ?
C124 N121 C121 C102 80.4(3) . . . . ?
C103 C102 C121 N121 -0.9(3) . . . . ?
C101 C102 C121 N121 -179.3(2) . . . . ?
C123 N122 C122 N121 -0.6(3) . . . . ?
C124 N121 C122 N122 0.4(3) . . . . ?
C121 N121 C122 N122 168.8(2) . . . . ?
C122 N122 C123 C124 0.6(3) . . . . ?
N122 C123 C124 N121 -0.4(3) . . . . ?
C122 N121 C124 C123 0.0(3) . . . . ?
C121 N121 C124 C123 -168.4(2) . . . . ?
C142 N141 C141 C104 98.0(3) . . . . ?
C144 N141 C141 C104 -70.8(3) . . . . ?
C103 C104 C141 N141 -14.3(3) . . . . ?
C105 C104 C141 N141 165.9(2) . . . . ?
C143 N142 C142 N141 0.6(3) . . . . ?
Cd2 N142 C142 N141 178.50(15) 1_465 . . . ?
C144 N141 C142 N142 -1.0(3) . . . . ?
C141 N141 C142 N142 -171.2(2) . . . . ?
C142 N142 C143 C144 0.1(3) . . . . ?
Cd2 N142 C143 C144 -178.00(16) 1_465 . . . ?
N142 C143 C144 N141 -0.7(3) . . . . ?
C142 N141 C144 C143 1.0(3) . . . . ?
C141 N141 C144 C143 171.7(2) . . . . ?
C152 N151 C151 C105 -86.8(3) . . . . ?
C154 N151 C151 C105 80.1(3) . . . . ?
C106 C105 C151 N151 14.2(4) . . . . ?
C104 C105 C151 N151 -167.8(2) . . . . ?
C153 N152 C152 N151 -1.1(3) . . . . ?
C154 N151 C152 N152 0.9(3) . . . . ?
C151 N151 C152 N152 169.8(2) . . . . ?
C152 N152 C153 C154 0.9(4) . . . . ?
N152 C153 C154 N151 -0.4(4) . . . . ?
C152 N151 C154 C153 -0.3(4) . . . . ?
C151 N151 C154 C153 -169.4(3) . . . . ?

_diffrn_measured_fraction_theta_max 0.994
_diffrn_reflns_theta_full        27.49
_diffrn_measured_fraction_theta_full 0.994
_refine_diff_density_max         0.857
_refine_diff_density_min         -0.675
_refine_diff_density_rms         0.080

#====END

data_6
_database_code_depnum_ccdc_archive 'CCDC 687828'
_audit_creation_date             'Sun Aug 19 15:11:51 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        
;
[Cd2(OH2)3(OSO3)2(L)]-4(H2O)
;
_chemical_name_common            (Cd2(OH2)3(OSO3)2(L))-4(H2O)
_chemical_melting_point          ?
_chemical_formula_moiety         'C22 H36 Cd2 N8 O15 S2 '
_chemical_formula_sum            'C22 H36 Cd2 N8 O15 S2'
_chemical_formula_weight         941.51

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'
S S 0.1246 0.1234 '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           tetragonal
_symmetry_space_group_name_H-M   'P 43 21 2'
_symmetry_space_group_name_Hall  'P 4nw 2abw'
_symmetry_Int_Tables_number      96

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z+1/2'
'-y+1/2, x+1/2, z+3/4'
'y+1/2, -x+1/2, z+1/4'
'y, x, -z'
'-y, -x, -z+1/2'
'-x+1/2, y+1/2, -z+3/4'
'x+1/2, -y+1/2, -z+1/4'

_cell_length_a                   10.116(2)
_cell_length_b                   10.116(2)
_cell_length_c                   31.186(5)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     3191.6(11)
_cell_formula_units_Z            4
_cell_measurement_temperature    200
_cell_measurement_reflns_used    23852
_cell_measurement_theta_min      3.1
_cell_measurement_theta_max      27.5

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.120
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.959
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1888
_exptl_absorpt_coefficient_mu    1.547
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.713
_exptl_absorpt_correction_T_max  0.830
_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            29993
_diffrn_reflns_av_R_equivalents  0.0441
_diffrn_reflns_av_sigmaI/netI    0.0237
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -40
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_theta_min         3.13
_diffrn_reflns_theta_max         27.48
_reflns_number_total             3655
_reflns_number_gt                3552
_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)+(0.0156P)²+2.6824P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.032(19)
_refine_ls_number_reflns         3655
_refine_ls_number_parameters     244
_refine_ls_number_restraints     4
_refine_ls_R_factor_all          0.0220
_refine_ls_R_factor_gt           0.0209
_refine_ls_wR_factor_ref         0.0440
_refine_ls_wR_factor_gt          0.0437
_refine_ls_goodness_of_fit_ref   1.075
_refine_ls_restrained_S_all      1.080
_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 0.149888(18) 0.310551(18) 0.068252(6) 0.01376(5) Uani 1 1 d . . .
S1 S 0.45874(6) 0.15155(7) 0.081786(18) 0.01441(13) Uani 1 1 d . . .
O1 O 0.2759(2) 0.2759(2) 0.0000 0.0183(6) Uani 1 2 d S . .
H1 H 0.348(3) 0.270(3) 0.0090(10) 0.022 Uiso 1 1 d . . .
O2 O -0.0140(2) 0.4122(3) 0.02625(7) 0.0308(5) Uani 1 1 d . . .
H2 H -0.005(4) 0.425(3) 0.0010(11) 0.037 Uiso 1 1 d . . .
H3 H -0.086(4) 0.404(4) 0.0317(11) 0.037 Uiso 1 1 d . . .
O3 O 0.7418(2) 0.3820(2) 0.06667(7) 0.0308(5) Uani 1 1 d D . .
H4 H 0.671(2) 0.342(3) 0.0593(10) 0.037 Uiso 1 1 d D . .
H5 H 0.759(3) 0.357(3) 0.0922(7) 0.037 Uiso 1 1 d D . .
O4 O 0.8837(3) 0.6240(3) 0.10412(10) 0.0648(9) Uani 1 1 d D . .
H6 H 0.909(4) 0.582(4) 0.1292(9) 0.078 Uiso 1 1 d D . .
H7 H 0.852(5) 0.569(4) 0.0837(11) 0.078 Uiso 1 1 d D . .
O11 O 0.33370(18) 0.20358(18) 0.10099(5) 0.0190(4) Uani 1 1 d . . .
O12 O 0.5610(2) 0.1428(2) 0.11501(6) 0.0298(5) Uani 1 1 d . . .
O13 O 0.50271(19) 0.2419(2) 0.04751(6) 0.0229(4) Uani 1 1 d . . .
O14 O 0.43531(19) 0.01970(19) 0.06374(6) 0.0236(4) Uani 1 1 d . . .
N11 N 0.4278(2) 0.6417(2) 0.06686(7) 0.0173(4) Uani 1 1 d . . .
N12 N 0.2629(2) 0.5001(2) 0.06593(7) 0.0170(4) Uani 1 1 d . . .
N21 N 0.8923(2) 0.9651(2) 0.07283(7) 0.0152(4) Uani 1 1 d . . .
N22 N 1.0447(2) 1.1181(2) 0.06626(7) 0.0196(5) Uani 1 1 d . . .
C1 C 0.6438(3) 0.7144(2) 0.03546(7) 0.0154(5) Uani 1 1 d . . .
C2 C 0.7427(2) 0.8104(3) 0.03567(7) 0.0148(5) Uani 1 1 d . . .
C3 C 0.8237(2) 0.8237(2) 0.0000 0.0165(7) Uani 1 2 d S . .
H8 H 0.8901 0.8901 0.0000 0.020 Uiso 1 2 calc SR . .
C4 C 0.6313(2) 0.6313(2) 0.0000 0.0184(8) Uani 1 2 d S . .
H9 H 0.5649 0.5649 0.0000 0.022 Uiso 1 2 calc SR . .
C11 C 0.5595(3) 0.6970(3) 0.07511(8) 0.0233(6) Uani 1 1 d . . .
H10 H 0.6066 0.6383 0.0954 0.028 Uiso 1 1 calc R . .
H11 H 0.5490 0.7841 0.0892 0.028 Uiso 1 1 calc R . .
C12 C 0.3887(3) 0.5178(3) 0.07565(8) 0.0183(6) Uani 1 1 d . . .
H12 H 0.4444 0.4514 0.0874 0.022 Uiso 1 1 calc R . .
C13 C 0.2204(3) 0.6188(3) 0.04951(8) 0.0217(6) Uani 1 1 d . . .
H13 H 0.1338 0.6362 0.0392 0.026 Uiso 1 1 calc R . .
C14 C 0.3207(3) 0.7070(3) 0.05020(9) 0.0251(6) Uani 1 1 d . . .
H14 H 0.3176 0.7964 0.0410 0.030 Uiso 1 1 calc R . .
C21 C 0.7630(3) 0.8994(3) 0.07425(8) 0.0186(6) Uani 1 1 d . . .
H15 H 0.6924 0.9671 0.0750 0.022 Uiso 1 1 calc R . .
H16 H 0.7565 0.8462 0.1008 0.022 Uiso 1 1 calc R . .
C22 C 0.9167(3) 1.0941(3) 0.06719(8) 0.0181(5) Uani 1 1 d . . .
H17 H 0.8502 1.1598 0.0642 0.022 Uiso 1 1 calc R . .
C23 C 1.1050(3) 0.9971(3) 0.07126(9) 0.0208(6) Uani 1 1 d . . .
H18 H 1.1978 0.9829 0.0719 0.025 Uiso 1 1 calc R . .
C24 C 1.0124(3) 0.9016(3) 0.07512(8) 0.0190(6) Uani 1 1 d . . .
H19 H 1.0271 0.8095 0.0787 0.023 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 N22 2.219(2) 1_445 ?
Cd1 N12 2.233(2) . ?
Cd1 O12 2.3160(18) 8_455 ?
Cd1 O2 2.350(2) . ?
Cd1 O11 2.3814(18) . ?
Cd1 O1 2.5056(9) . ?
S1 O12 1.4669(18) . ?
S1 O14 1.467(2) . ?
S1 O13 1.4751(19) . ?
S1 O11 1.4952(18) . ?
O1 Cd1 2.5056(9) 5 ?
O1 H1 0.79(3) . ?
O2 H2 0.80(3) . ?
O2 H3 0.75(4) . ?
O3 H4 0.854(18) . ?
O3 H5 0.852(18) . ?
O4 H6 0.926(19) . ?
O4 H7 0.90(4) . ?
O12 Cd1 2.3159(18) 8 ?
N11 C12 1.343(3) . ?
N11 C14 1.371(4) . ?
N11 C11 1.467(3) . ?
N12 C12 1.321(3) . ?
N12 C13 1.374(3) . ?
N21 C22 1.340(3) . ?
N21 C24 1.375(3) . ?
N21 C21 1.468(3) . ?
N22 C22 1.318(3) . ?
N22 C23 1.377(3) . ?
N22 Cd1 2.219(2) 1_665 ?
C1 C4 1.394(3) . ?
C1 C2 1.394(3) . ?
C1 C11 1.512(3) . ?
C2 C3 1.388(3) . ?
C2 C21 1.517(3) . ?
C3 C2 1.388(3) 5 ?
C3 H8 0.9500 . ?
C4 C1 1.394(3) 5 ?
C4 H9 0.9500 . ?
C11 H10 0.9900 . ?
C11 H11 0.9900 . ?
C12 H12 0.9500 . ?
C13 C14 1.351(4) . ?
C13 H13 0.9500 . ?
C14 H14 0.9500 . ?
C21 H15 0.9900 . ?
C21 H16 0.9900 . ?
C22 H17 0.9500 . ?
C23 C24 1.351(4) . ?
C23 H18 0.9500 . ?
C24 H19 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
N22 Cd1 N12 175.93(8) 1_445 . ?
N22 Cd1 O12 91.03(8) 1_445 8_455 ?
N12 Cd1 O12 93.02(8) . 8_455 ?
N22 Cd1 O2 91.72(8) 1_445 . ?
N12 Cd1 O2 88.11(8) . . ?
O12 Cd1 O2 97.92(8) 8_455 . ?
N22 Cd1 O11 89.31(8) 1_445 . ?
N12 Cd1 O11 90.26(7) . . ?
O12 Cd1 O11 90.61(7) 8_455 . ?
O2 Cd1 O11 171.39(7) . . ?
N22 Cd1 O1 95.59(9) 1_445 . ?
N12 Cd1 O1 80.34(8) . . ?
O12 Cd1 O1 171.68(8) 8_455 . ?
O2 Cd1 O1 86.94(6) . . ?
O11 Cd1 O1 84.45(4) . . ?
O12 S1 O14 109.25(12) . . ?
O12 S1 O13 109.68(13) . . ?
O14 S1 O13 109.53(12) . . ?
O12 S1 O11 109.58(11) . . ?
O14 S1 O11 109.69(11) . . ?
O13 S1 O11 109.10(11) . . ?
Cd1 O1 Cd1 149.77(13) 5 . ?
Cd1 O1 H1 98(2) 5 . ?
Cd1 O1 H1 100(2) . . ?
Cd1 O2 H2 122(3) . . ?
Cd1 O2 H3 121(3) . . ?
H2 O2 H3 110(4) . . ?
H4 O3 H5 106(3) . . ?
H6 O4 H7 114(4) . . ?
S1 O11 Cd1 130.46(9) . . ?
S1 O12 Cd1 153.67(13) . 8 ?
C12 N11 C14 107.1(2) . . ?
C12 N11 C11 126.0(2) . . ?
C14 N11 C11 126.9(2) . . ?
C12 N12 C13 105.5(2) . . ?
C12 N12 Cd1 127.04(19) . . ?
C13 N12 Cd1 127.05(18) . . ?
C22 N21 C24 107.4(2) . . ?
C22 N21 C21 127.5(2) . . ?
C24 N21 C21 125.0(2) . . ?
C22 N22 C23 105.6(2) . . ?
C22 N22 Cd1 129.23(18) . 1_665 ?
C23 N22 Cd1 124.35(18) . 1_665 ?
C4 C1 C2 119.2(2) . . ?
C4 C1 C11 121.9(2) . . ?
C2 C1 C11 118.8(2) . . ?
C3 C2 C1 119.2(2) . . ?
C3 C2 C21 119.9(2) . . ?
C1 C2 C21 121.0(2) . . ?
C2 C3 C2 121.9(3) . 5 ?
C2 C3 H8 119.1 . . ?
C2 C3 H8 119.1 5 . ?
C1 C4 C1 121.4(3) 5 . ?
C1 C4 H9 119.3 5 . ?
C1 C4 H9 119.3 . . ?
N11 C11 C1 114.4(2) . . ?
N11 C11 H10 108.7 . . ?
C1 C11 H10 108.7 . . ?
N11 C11 H11 108.7 . . ?
C1 C11 H11 108.7 . . ?
H10 C11 H11 107.6 . . ?
N12 C12 N11 111.4(2) . . ?
N12 C12 H12 124.3 . . ?
N11 C12 H12 124.3 . . ?
C14 C13 N12 109.7(2) . . ?
C14 C13 H13 125.2 . . ?
N12 C13 H13 125.2 . . ?
C13 C14 N11 106.4(2) . . ?
C13 C14 H14 126.8 . . ?
N11 C14 H14 126.8 . . ?
N21 C21 C2 111.4(2) . . ?
N21 C21 H15 109.3 . . ?
C2 C21 H15 109.3 . . ?
N21 C21 H16 109.3 . . ?
C2 C21 H16 109.3 . . ?
H15 C21 H16 108.0 . . ?
N22 C22 N21 111.3(2) . . ?
N22 C22 H17 124.4 . . ?
N21 C22 H17 124.4 . . ?
C24 C23 N22 109.8(2) . . ?
C24 C23 H18 125.1 . . ?
N22 C23 H18 125.1 . . ?
C23 C24 N21 105.9(2) . . ?
C23 C24 H19 127.0 . . ?
N21 C24 H19 127.0 . . ?

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
N22 Cd1 O1 Cd1 13.60(6) 1_445 . . 5 ?
N12 Cd1 O1 Cd1 -166.44(6) . . . 5 ?
O2 Cd1 O1 Cd1 -77.83(6) . . . 5 ?
O11 Cd1 O1 Cd1 102.36(5) . . . 5 ?
O12 S1 O11 Cd1 157.77(14) . . . . ?
O14 S1 O11 Cd1 -82.29(16) . . . . ?
O13 S1 O11 Cd1 37.68(18) . . . . ?
N22 Cd1 O11 S1 97.06(15) 1_445 . . . ?
N12 Cd1 O11 S1 -78.89(15) . . . . ?
O12 Cd1 O11 S1 -171.92(15) 8_455 . . . ?
O1 Cd1 O11 S1 1.38(15) . . . . ?
O14 S1 O12 Cd1 -135.2(3) . . . 8 ?
O13 S1 O12 Cd1 104.7(3) . . . 8 ?
O11 S1 O12 Cd1 -15.0(4) . . . 8 ?
O12 Cd1 N12 C12 97.8(2) 8_455 . . . ?
O2 Cd1 N12 C12 -164.3(2) . . . . ?
O11 Cd1 N12 C12 7.2(2) . . . . ?
O1 Cd1 N12 C12 -77.1(2) . . . . ?
O12 Cd1 N12 C13 -90.3(2) 8_455 . . . ?
O2 Cd1 N12 C13 7.6(2) . . . . ?
O11 Cd1 N12 C13 179.1(2) . . . . ?
O1 Cd1 N12 C13 94.8(2) . . . . ?
C4 C1 C2 C3 2.0(4) . . . . ?
C11 C1 C2 C3 177.7(2) . . . . ?
C4 C1 C2 C21 -177.7(2) . . . . ?
C11 C1 C2 C21 -2.1(4) . . . . ?
C1 C2 C3 C2 -1.01(18) . . . 5 ?
C21 C2 C3 C2 178.7(3) . . . 5 ?
C2 C1 C4 C1 -1.01(18) . . . 5 ?
C11 C1 C4 C1 -176.5(3) . . . 5 ?
C12 N11 C11 C1 105.6(3) . . . . ?
C14 N11 C11 C1 -76.7(3) . . . . ?
C4 C1 C11 N11 -30.2(4) . . . . ?
C2 C1 C11 N11 154.2(3) . . . . ?
C13 N12 C12 N11 0.9(3) . . . . ?
Cd1 N12 C12 N11 174.18(16) . . . . ?
C14 N11 C12 N12 -0.5(3) . . . . ?
C11 N11 C12 N12 177.6(2) . . . . ?
C12 N12 C13 C14 -1.0(3) . . . . ?
Cd1 N12 C13 C14 -174.28(18) . . . . ?
N12 C13 C14 N11 0.7(3) . . . . ?
C12 N11 C14 C13 -0.2(3) . . . . ?
C11 N11 C14 C13 -178.2(2) . . . . ?
C22 N21 C21 C2 112.0(3) . . . . ?
C24 N21 C21 C2 -64.7(3) . . . . ?
C3 C2 C21 N21 -15.9(3) . . . . ?
C1 C2 C21 N21 163.8(2) . . . . ?
C23 N22 C22 N21 0.5(3) . . . . ?
Cd1 N22 C22 N21 -169.27(17) 1_665 . . . ?
C24 N21 C22 N22 -0.8(3) . . . . ?
C21 N21 C22 N22 -178.0(2) . . . . ?
C22 N22 C23 C24 0.0(3) . . . . ?
Cd1 N22 C23 C24 170.45(18) 1_665 . . . ?
N22 C23 C24 N21 -0.5(3) . . . . ?
C22 N21 C24 C23 0.8(3) . . . . ?
C21 N21 C24 C23 178.0(2) . . . . ?

_diffrn_measured_fraction_theta_max 0.997
_diffrn_reflns_theta_full        27.48
_diffrn_measured_fraction_theta_full 0.997
_refine_diff_density_max         0.282
_refine_diff_density_min         -0.346
_refine_diff_density_rms         0.074

#====END


