# Electronic Supplementary Material for CrystEngComm
# This journal is (c) The Royal Society of Chemistry 2008

data_global
_journal_name_full               CrystEngComm

_journal_coden_Cambridge         1350

_publ_contact_author_name        'Susumu Kitagawa'
_publ_contact_author_email       KITAGAWA@SBCHEM.KYOTO-U.AC.JP

_publ_section_title              
;
Solvent as structure directing agent for the synthesis
of novel coordination frameworks using a tripodal flexible ligand
;
loop_
_publ_author_name
'Susumu Kitagawa'
'Sujit Ghosh'

# Attachment 'Compound_1_2_3_new.cif'

data_{[ME2NH2][(tci)Cd].DMF}n_(1)
_database_code_depnum_ccdc_archive 'CCDC 694561'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C17 H27 Cd N5 O10'
_chemical_formula_weight         573.84

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           monoclinic
_symmetry_space_group_name_H-M   P21/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                   12.375(3)
_cell_length_b                   23.376(5)
_cell_length_c                   8.5893(17)
_cell_angle_alpha                90.00
_cell_angle_beta                 104.46(3)
_cell_angle_gamma                90.00
_cell_volume                     2406.0(9)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.11
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.584
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1168
_exptl_absorpt_coefficient_mu    0.967
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.8607
_exptl_absorpt_correction_T_max  0.9011
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71069
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Rigaku/MSC Mercury CCD'
_diffrn_measurement_method       ω
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            10789
_diffrn_reflns_av_R_equivalents  0.1001
_diffrn_reflns_av_sigmaI/netI    0.1026
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_theta_min         2.43
_diffrn_reflns_theta_max         27.00
_reflns_number_total             5136
_reflns_number_gt                3543
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       crystalclear
_computing_cell_refinement       crystalclear
_computing_data_reduction        crystalclear
_computing_structure_solution    SIR-97
_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)+(0.2000P)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         5136
_refine_ls_number_parameters     253
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1144
_refine_ls_R_factor_gt           0.0999
_refine_ls_wR_factor_ref         0.3084
_refine_ls_wR_factor_gt          0.2861
_refine_ls_goodness_of_fit_ref   1.077
_refine_ls_restrained_S_all      1.077
_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 0.23929(4) 0.21877(2) 0.45246(6) 0.0427(3) Uani 1 1 d . . .
O1 O 0.0941(6) -0.0615(3) 0.3462(11) 0.101(3) Uani 1 1 d . . .
O2 O 0.2484(7) -0.2172(3) 0.6289(12) 0.082(2) Uani 1 1 d . . .
O3 O 0.4432(5) -0.0519(3) 0.6732(10) 0.085(2) Uani 1 1 d . . .
O4 O 0.2164(8) 0.1419(3) 0.6167(10) 0.093(2) Uani 1 1 d . . .
O5 O 0.2556(6) 0.1185(3) 0.3939(9) 0.080(2) Uani 1 1 d . . .
O6 O -0.1043(7) -0.2155(3) 0.1088(12) 0.079(2) Uani 1 1 d . . .
O7 O -0.0486(7) -0.2909(3) 0.2438(13) 0.090(3) Uani 1 1 d . . .
O8 O 0.7069(5) -0.2265(2) 0.7854(8) 0.0566(14) Uani 1 1 d . . .
O9 O 0.5944(6) -0.2376(4) 0.9374(9) 0.080(2) Uani 1 1 d . . .
N1 N 0.1669(5) -0.1399(3) 0.4864(9) 0.0548(15) Uani 1 1 d . . .
N2 N 0.3454(5) -0.1349(2) 0.6548(8) 0.0464(13) Uani 1 1 d . . .
N3 N 0.2704(5) -0.0562(3) 0.5039(9) 0.0591(16) Uani 1 1 d . . .
N4 N 0.1266(8) 0.1189(4) 0.0757(10) 0.080(2) Uani 1 1 d . . .
C1 C 0.1707(7) -0.0836(3) 0.4384(11) 0.061(2) Uani 1 1 d . . .
C2 C 0.2534(6) -0.1675(3) 0.5929(10) 0.0516(16) Uani 1 1 d . . .
C3 C 0.3569(6) -0.0786(3) 0.6114(11) 0.0531(18) Uani 1 1 d . . .
C4 C 0.0627(6) -0.1732(4) 0.4238(11) 0.061(2) Uani 1 1 d . . .
H4A H -0.0001 -0.1473 0.3907 0.073 Uiso 1 1 calc R . .
H4B H 0.0491 -0.1978 0.5078 0.073 Uiso 1 1 calc R . .
C5 C 0.0739(9) -0.2089(5) 0.2827(17) 0.089(4) Uani 1 1 d . . .
H5A H 0.1335 -0.2366 0.3178 0.107 Uiso 1 1 calc R . .
H5B H 0.0931 -0.1845 0.2023 0.107 Uiso 1 1 calc R . .
C6 C -0.0339(7) -0.2399(5) 0.2099(12) 0.063(2) Uani 1 1 d . . .
C7 C 0.4372(6) -0.1629(4) 0.7733(9) 0.0532(18) Uani 1 1 d . . .
H7A H 0.4074 -0.1941 0.8241 0.064 Uiso 1 1 calc R . .
H7B H 0.4709 -0.1355 0.8562 0.064 Uiso 1 1 calc R . .
C8 C 0.5242(6) -0.1854(4) 0.6970(9) 0.0553(18) Uani 1 1 d . . .
H8A H 0.5590 -0.1535 0.6555 0.066 Uiso 1 1 calc R . .
H8B H 0.4890 -0.2096 0.6069 0.066 Uiso 1 1 calc R . .
C9 C 0.6134(7) -0.2194(3) 0.8128(10) 0.0438(17) Uani 1 1 d . . .
C10 C 0.2797(8) 0.0051(4) 0.4650(11) 0.064(2) Uani 1 1 d . . .
H10A H 0.2426 0.0115 0.3528 0.076 Uiso 1 1 calc R . .
H10B H 0.3578 0.0149 0.4805 0.076 Uiso 1 1 calc R . .
C11 C 0.2287(9) 0.0432(4) 0.5679(12) 0.070(2) Uani 1 1 d . . .
H11A H 0.2681 0.0381 0.6798 0.084 Uiso 1 1 calc R . .
H11B H 0.1516 0.0322 0.5563 0.084 Uiso 1 1 calc R . .
C12 C 0.2333(7) 0.1054(3) 0.5234(10) 0.0536(17) Uani 1 1 d . . .
C13 C 0.0322(12) 0.0864(6) 0.082(2) 0.127(5) Uani 1 1 d . . .
H13A H -0.0109 0.1067 0.1426 0.191 Uiso 1 1 calc R . .
H13B H 0.0556 0.0503 0.1326 0.191 Uiso 1 1 calc R . .
H13C H -0.0124 0.0800 -0.0253 0.191 Uiso 1 1 calc R . .
C14 C 0.205(2) 0.0885(12) -0.026(3) 0.204(12) Uani 1 1 d . . .
H14A H 0.2681 0.1127 -0.0257 0.307 Uiso 1 1 calc R . .
H14B H 0.1630 0.0826 -0.1351 0.307 Uiso 1 1 calc R . .
H14C H 0.2311 0.0523 0.0217 0.307 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 O6 2.233(6) 2 ?
Cd1 O9 2.280(6) 2_656 ?
Cd1 O8 2.309(7) 3_656 ?
Cd1 O4 2.345(8) . ?
Cd1 O5 2.417(8) . ?
Cd1 O8 2.530(6) 2_656 ?
Cd1 O7 2.545(9) 2 ?
Cd1 C12 2.724(8) . ?
Cd1 C6 2.752(9) 2 ?
O1 C1 1.191(9) . ?
O2 C2 1.208(9) . ?
O3 C3 1.237(9) . ?
O4 C12 1.223(10) . ?
O5 C12 1.249(12) . ?
O6 C6 1.208(13) . ?
O6 Cd1 2.233(6) 2_545 ?
O7 C6 1.252(12) . ?
O7 Cd1 2.545(9) 2_545 ?
O8 C9 1.247(10) . ?
O8 Cd1 2.309(7) 3_656 ?
O8 Cd1 2.530(6) 2_646 ?
O9 C9 1.229(10) . ?
O9 Cd1 2.280(6) 2_646 ?
N1 C2 1.382(10) . ?
N1 C1 1.383(10) . ?
N1 C4 1.486(9) . ?
N2 C2 1.363(9) . ?
N2 C3 1.384(9) . ?
N2 C7 1.476(9) . ?
N3 C3 1.334(10) . ?
N3 C1 1.379(10) . ?
N3 C10 1.483(11) . ?
N4 C13 1.405(15) . ?
N4 C14 1.63(3) . ?
C4 C5 1.506(15) . ?
C5 C6 1.508(13) . ?
C6 Cd1 2.752(9) 2_545 ?
C7 C8 1.489(10) . ?
C8 C9 1.513(10) . ?
C10 C11 1.501(13) . ?
C11 C12 1.508(11) . ?

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
O6 Cd1 O9 109.6(3) 2 2_656 ?
O6 Cd1 O8 95.8(3) 2 3_656 ?
O9 Cd1 O8 84.4(2) 2_656 3_656 ?
O6 Cd1 O4 118.3(3) 2 . ?
O9 Cd1 O4 109.0(3) 2_656 . ?
O8 Cd1 O4 134.2(2) 3_656 . ?
O6 Cd1 O5 135.6(3) 2 . ?
O9 Cd1 O5 114.0(3) 2_656 . ?
O8 Cd1 O5 80.5(2) 3_656 . ?
O4 Cd1 O5 53.9(2) . . ?
O6 Cd1 O8 82.9(3) 2 2_656 ?
O9 Cd1 O8 52.8(2) 2_656 2_656 ?
O8 Cd1 O8 132.67(18) 3_656 2_656 ?
O4 Cd1 O8 84.1(2) . 2_656 ?
O5 Cd1 O8 131.2(2) . 2_656 ?
O6 Cd1 O7 52.4(3) 2 2 ?
O9 Cd1 O7 155.0(3) 2_656 2 ?
O8 Cd1 O7 81.1(3) 3_656 2 ?
O4 Cd1 O7 95.7(3) . 2 ?
O5 Cd1 O7 83.6(2) . 2 ?
O8 Cd1 O7 129.0(2) 2_656 2 ?
O6 Cd1 C12 131.4(3) 2 . ?
O9 Cd1 C12 114.5(3) 2_656 . ?
O8 Cd1 C12 107.7(2) 3_656 . ?
O4 Cd1 C12 26.6(2) . . ?
O5 Cd1 C12 27.3(3) . . ?
O8 Cd1 C12 108.0(2) 2_656 . ?
O7 Cd1 C12 89.4(3) 2 . ?
O6 Cd1 C6 25.4(3) 2 2 ?
O9 Cd1 C6 132.6(3) 2_656 2 ?
O8 Cd1 C6 87.6(2) 3_656 2 ?
O4 Cd1 C6 109.8(3) . 2 ?
O5 Cd1 C6 110.5(3) . 2 ?
O8 Cd1 C6 106.1(3) 2_656 2 ?
O7 Cd1 C6 27.0(3) 2 2 ?
C12 Cd1 C6 112.4(3) . 2 ?
C12 O4 Cd1 94.2(6) . . ?
C12 O5 Cd1 90.2(5) . . ?
C6 O6 Cd1 102.0(6) . 2_545 ?
C6 O7 Cd1 85.8(6) . 2_545 ?
C9 O8 Cd1 130.0(5) . 3_656 ?
C9 O8 Cd1 87.2(5) . 2_646 ?
Cd1 O8 Cd1 139.2(2) 3_656 2_646 ?
C9 O9 Cd1 99.6(5) . 2_646 ?
C2 N1 C1 124.3(6) . . ?
C2 N1 C4 116.9(6) . . ?
C1 N1 C4 118.8(6) . . ?
C2 N2 C3 124.0(6) . . ?
C2 N2 C7 116.5(6) . . ?
C3 N2 C7 119.5(6) . . ?
C3 N3 C1 125.6(7) . . ?
C3 N3 C10 116.2(7) . . ?
C1 N3 C10 117.9(7) . . ?
C13 N4 C14 113.6(13) . . ?
O1 C1 N3 123.5(8) . . ?
O1 C1 N1 122.1(8) . . ?
N3 C1 N1 114.4(7) . . ?
O2 C2 N2 121.9(7) . . ?
O2 C2 N1 122.5(7) . . ?
N2 C2 N1 115.5(7) . . ?
O3 C3 N3 123.8(7) . . ?
O3 C3 N2 120.1(7) . . ?
N3 C3 N2 116.1(6) . . ?
N1 C4 C5 109.6(7) . . ?
C4 C5 C6 110.5(9) . . ?
O6 C6 O7 119.7(9) . . ?
O6 C6 C5 118.5(10) . . ?
O7 C6 C5 121.7(10) . . ?
O6 C6 Cd1 52.5(5) . 2_545 ?
O7 C6 Cd1 67.3(6) . 2_545 ?
C5 C6 Cd1 171.0(9) . 2_545 ?
N2 C7 C8 111.7(6) . . ?
C7 C8 C9 112.6(6) . . ?
O9 C9 O8 120.4(7) . . ?
O9 C9 C8 119.2(7) . . ?
O8 C9 C8 120.3(7) . . ?
N3 C10 C11 111.9(8) . . ?
C10 C11 C12 112.0(8) . . ?
O4 C12 O5 121.7(8) . . ?
O4 C12 C11 118.8(8) . . ?
O5 C12 C11 119.5(8) . . ?
O4 C12 Cd1 59.2(5) . . ?
O5 C12 Cd1 62.5(5) . . ?
C11 C12 Cd1 178.0(6) . . ?

_diffrn_measured_fraction_theta_max 0.981
_diffrn_reflns_theta_full        27.00
_diffrn_measured_fraction_theta_full 0.981
_refine_diff_density_max         3.698
_refine_diff_density_min         -2.272
_refine_diff_density_rms         0.253

#= = =END

data_{[Cd3.(tci)2.2DEF].DEF}n_(2)
_database_code_depnum_ccdc_archive 'CCDC 694562'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C39 H57 Cd3 N9 O21'
_chemical_formula_weight         1325.14

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'
Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_H-M   Pna21

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

_cell_length_a                   17.640(2)
_cell_length_b                   13.380(3)
_cell_length_c                   21.460(4)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     5065.1(16)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       rectangular-parallelopipeds
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.10
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.738
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2664
_exptl_absorpt_coefficient_mu    1.333
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.8150
_exptl_absorpt_correction_T_max  0.8782
_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  'Rigaku/MSC Mercury CCD'
_diffrn_measurement_method       ω
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            30623
_diffrn_reflns_av_R_equivalents  0.0739
_diffrn_reflns_av_sigmaI/netI    0.0567
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_theta_min         3.23
_diffrn_reflns_theta_max         27.00
_reflns_number_total             7316
_reflns_number_gt                6736
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       crystalclear
_computing_cell_refinement       crystalclear
_computing_data_reduction        crystalclear
_computing_structure_solution    SIR-97
_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)+(0.1115P)²+21.3849P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.06(5)
_refine_ls_number_reflns         7316
_refine_ls_number_parameters     586
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0666
_refine_ls_R_factor_gt           0.0606
_refine_ls_wR_factor_ref         0.1758
_refine_ls_wR_factor_gt          0.1703
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_restrained_S_all      1.062
_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 0.12778(4) 0.29706(6) 0.85687(4) 0.01992(18) Uani 1 1 d . . .
Cd2 Cd 0.44341(4) 1.17052(6) 0.76575(4) 0.02176(19) Uani 1 1 d . . .
Cd3 Cd 0.30072(4) 0.35288(6) 0.78012(4) 0.02143(19) Uani 1 1 d . . .
O1 O 0.0258(7) -0.1746(7) 0.8164(4) 0.044(3) Uani 1 1 d . . .
O2 O 0.0161(5) -0.3530(7) 0.9940(4) 0.034(2) Uani 1 1 d . . .
O3 O 0.0886(6) -0.0289(7) 0.9998(5) 0.042(2) Uani 1 1 d . . .
O4 O 0.0549(4) 0.1734(6) 0.8149(4) 0.0252(18) Uani 1 1 d . . .
O5 O -0.0669(4) 0.1695(6) 0.7944(5) 0.030(2) Uani 1 1 d . . .
O6 O -0.0426(4) -0.5020(5) 0.7849(5) 0.0302(18) Uani 1 1 d . . .
O7 O 0.0181(4) -0.6057(6) 0.8462(4) 0.0257(17) Uani 1 1 d . . .
O8 O 0.1105(5) -0.3441(7) 1.1747(4) 0.038(2) Uani 1 1 d . . .
O9 O 0.1646(5) -0.1961(7) 1.1839(4) 0.0312(19) Uani 1 1 d . . .
O10 O 0.3910(5) 0.6702(6) 1.0214(5) 0.037(2) Uani 1 1 d . . .
O11 O 0.3181(6) 0.9938(7) 1.0358(4) 0.038(2) Uani 1 1 d . . .
O12 O 0.2417(7) 0.8068(7) 0.8713(4) 0.047(3) Uani 1 1 d . . .
O13 O 0.2978(4) 0.4473(6) 0.8647(4) 0.0309(19) Uani 1 1 d . . .
O14 O 0.1802(4) 0.4315(6) 0.9006(4) 0.0304(19) Uani 1 1 d . . .
O15 O 0.4401(4) 0.8348(6) 1.2129(4) 0.0270(18) Uani 1 1 d . . .
O16 O 0.3282(4) 0.8292(6) 1.2602(4) 0.0212(15) Uani 1 1 d . . .
O17 O 0.3198(4) 1.1950(6) 0.8155(4) 0.0266(18) Uani 1 1 d . . .
O18 O 0.2170(4) 1.1797(6) 0.8749(4) 0.0285(19) Uani 1 1 d . . .
O1S O 0.0734(5) 0.2566(7) 0.9480(4) 0.038(2) Uani 1 1 d . . .
O2S O 0.2960(6) 0.5054(7) 0.7341(5) 0.049(3) Uani 1 1 d . . .
N1 N 0.0558(5) -0.0952(8) 0.9076(5) 0.027(2) Uani 1 1 d . . .
N2 N 0.0167(6) -0.2650(7) 0.9046(5) 0.030(2) Uani 1 1 d . . .
N3 N 0.0628(5) -0.1962(8) 0.9970(5) 0.026(2) Uani 1 1 d . . .
N4 N 0.3136(5) 0.7358(7) 0.9469(5) 0.025(2) Uani 1 1 d . . .
N5 N 0.2831(5) 0.9070(7) 0.9511(4) 0.0217(19) Uani 1 1 d . . .
N6 N 0.3469(5) 0.8291(7) 1.0349(4) 0.0202(18) Uani 1 1 d . . .
N1S N 0.0030(8) 0.3173(10) 1.0285(6) 0.051(3) Uani 1 1 d . . .
N2S N 0.3146(8) 0.6258(9) 0.6624(6) 0.044(3) Uani 1 1 d . . .
C1 C 0.0339(7) -0.1789(9) 0.8714(7) 0.032(3) Uani 1 1 d . . .
C2 C 0.0328(6) -0.2755(10) 0.9672(6) 0.029(3) Uani 1 1 d . . .
C3 C 0.0698(7) -0.1008(10) 0.9702(6) 0.031(3) Uani 1 1 d . . .
C4 C 0.0612(6) 0.0010(9) 0.8750(6) 0.026(2) Uani 1 1 d . . .
H4A H 0.0921 -0.0066 0.8379 0.032 Uiso 1 1 calc R . .
H4B H 0.0854 0.0498 0.9018 0.032 Uiso 1 1 calc R . .
C5 C -0.0169(6) 0.0377(8) 0.8569(7) 0.030(2) Uani 1 1 d . . .
H5A H -0.0428 -0.0124 0.8322 0.036 Uiso 1 1 calc R . .
H5B H -0.0469 0.0507 0.8940 0.036 Uiso 1 1 calc R . .
C6 C -0.0073(7) 0.1328(8) 0.8197(6) 0.025(2) Uani 1 1 d . . .
C7 C -0.0144(7) -0.3494(9) 0.8706(7) 0.034(3) Uani 1 1 d . . .
H7A H -0.0350 -0.3261 0.8313 0.041 Uiso 1 1 calc R . .
H7B H -0.0556 -0.3784 0.8945 0.041 Uiso 1 1 calc R . .
C8 C 0.0437(6) -0.4274(9) 0.8582(7) 0.033(3) Uani 1 1 d . . .
H8A H 0.0669 -0.4485 0.8970 0.039 Uiso 1 1 calc R . .
H8B H 0.0830 -0.4009 0.8313 0.039 Uiso 1 1 calc R . .
C9 C 0.0041(6) -0.5179(8) 0.8262(6) 0.025(2) Uani 1 1 d . . .
C10 C 0.0732(7) -0.2058(11) 1.0645(6) 0.033(3) Uani 1 1 d . . .
H10A H 0.0296 -0.2400 1.0820 0.039 Uiso 1 1 calc R . .
H10B H 0.0753 -0.1396 1.0828 0.039 Uiso 1 1 calc R . .
C11 C 0.1457(7) -0.2637(10) 1.0824(6) 0.032(3) Uani 1 1 d . . .
H11A H 0.1461 -0.3295 1.0634 0.038 Uiso 1 1 calc R . .
H11B H 0.1907 -0.2276 1.0693 0.038 Uiso 1 1 calc R . .
C12 C 0.1418(6) -0.2712(9) 1.1528(6) 0.026(2) Uani 1 1 d . . .
C13 C 0.3522(6) 0.7396(9) 1.0027(6) 0.027(2) Uani 1 1 d . . .
C14 C 0.3159(6) 0.9174(9) 1.0081(6) 0.028(2) Uani 1 1 d . . .
C15 C 0.2773(6) 0.8139(9) 0.9202(6) 0.026(2) Uani 1 1 d . . .
C16 C 0.3156(8) 0.6379(9) 0.9116(6) 0.031(3) Uani 1 1 d . . .
H16A H 0.3630 0.6037 0.9200 0.038 Uiso 1 1 calc R . .
H16B H 0.3127 0.6508 0.8672 0.038 Uiso 1 1 calc R . .
C17 C 0.2493(7) 0.5719(9) 0.9314(6) 0.029(2) Uani 1 1 d . . .
H17A H 0.2548 0.5563 0.9753 0.034 Uiso 1 1 calc R . .
H17B H 0.2027 0.6096 0.9264 0.034 Uiso 1 1 calc R . .
C18 C 0.2422(7) 0.4753(8) 0.8955(5) 0.026(2) Uani 1 1 d . . .
C19 C 0.2530(6) 0.9959(8) 0.9225(5) 0.023(2) Uani 1 1 d . . .
H19A H 0.2330 1.0394 0.9547 0.028 Uiso 1 1 calc R . .
H19B H 0.2114 0.9775 0.8953 0.028 Uiso 1 1 calc R . .
C20 C 0.3118(6) 1.0525(9) 0.8851(5) 0.025(2) Uani 1 1 d . . .
H20A H 0.3297 1.0104 0.8514 0.030 Uiso 1 1 calc R . .
H20B H 0.3547 1.0678 0.9117 0.030 Uiso 1 1 calc R . .
C21 C 0.2800(6) 1.1501(8) 0.8579(5) 0.020(2) Uani 1 1 d . . .
C22 C 0.3853(7) 0.8391(11) 1.0945(6) 0.031(3) Uani 1 1 d . . .
H22A H 0.4114 0.9030 1.0957 0.037 Uiso 1 1 calc R . .
H22B H 0.4232 0.7869 1.0981 0.037 Uiso 1 1 calc R . .
C23 C 0.3318(7) 0.8326(13) 1.1494(7) 0.042(4) Uani 1 1 d . . .
H23A H 0.2980 0.8897 1.1485 0.050 Uiso 1 1 calc R . .
H23B H 0.3012 0.7728 1.1452 0.050 Uiso 1 1 calc R . .
C24 C 0.3717(6) 0.8299(9) 1.2112(6) 0.026(3) Uani 1 1 d . . .
C1S C 0.0587(8) 0.3233(13) 0.9850(8) 0.045(4) Uani 1 1 d . . .
C2S C -0.0427(9) 0.2236(15) 1.0306(8) 0.059(5) Uani 1 1 d . . .
H2S1 H -0.0102 0.1665 1.0230 0.071 Uiso 1 1 calc R . .
H2S2 H -0.0652 0.2160 1.0716 0.071 Uiso 1 1 calc R . .
C3S C -0.1029(11) 0.2277(17) 0.9830(10) 0.069(5) Uani 1 1 d . . .
H3S1 H -0.1326 0.1676 0.9849 0.103 Uiso 1 1 calc R . .
H3S2 H -0.0804 0.2336 0.9425 0.103 Uiso 1 1 calc R . .
H3S3 H -0.1349 0.2844 0.9907 0.103 Uiso 1 1 calc R . .
C4S C -0.0104(17) 0.4016(18) 1.0684(9) 0.104(10) Uani 1 1 d . . .
H4S1 H -0.0647 0.4125 1.0698 0.124 Uiso 1 1 calc R . .
H4S2 H 0.0118 0.4596 1.0484 0.124 Uiso 1 1 calc R . .
C5S C 0.017(2) 0.400(2) 1.1327(14) 0.133(12) Uani 1 1 d . . .
H5S1 H 0.0018 0.4599 1.1536 0.199 Uiso 1 1 calc R . .
H5S2 H 0.0713 0.3947 1.1329 0.199 Uiso 1 1 calc R . .
H5S3 H -0.0042 0.3430 1.1539 0.199 Uiso 1 1 calc R . .
C6S C 0.3153(8) 0.5320(9) 0.6809(7) 0.040(3) Uani 1 1 d . . .
C7S C 0.3409(10) 0.6553(11) 0.6008(8) 0.050(4) Uani 1 1 d . . .
H7S1 H 0.3581 0.5961 0.5789 0.060 Uiso 1 1 calc R . .
H7S2 H 0.3841 0.6994 0.6056 0.060 Uiso 1 1 calc R . .
C8S C 0.2824(11) 0.7072(13) 0.5612(10) 0.064(5) Uani 1 1 d . . .
H8S1 H 0.3037 0.7223 0.5212 0.095 Uiso 1 1 calc R . .
H8S2 H 0.2669 0.7681 0.5812 0.095 Uiso 1 1 calc R . .
H8S3 H 0.2392 0.6643 0.5560 0.095 Uiso 1 1 calc R . .
C9S C 0.2975(12) 0.7037(11) 0.7085(9) 0.065(6) Uani 1 1 d . . .
H9S1 H 0.2668 0.7554 0.6893 0.078 Uiso 1 1 calc R . .
H9S2 H 0.2687 0.6750 0.7426 0.078 Uiso 1 1 calc R . .
C10S C 0.3662(17) 0.747(2) 0.732(2) 0.18(2) Uani 1 1 d . . .
H10C H 0.3541 0.7980 0.7620 0.268 Uiso 1 1 calc R . .
H10D H 0.3945 0.7757 0.6984 0.268 Uiso 1 1 calc R . .
H10E H 0.3961 0.6960 0.7520 0.268 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 O14 2.229(8) . ?
Cd1 O1S 2.244(9) . ?
Cd1 O18 2.257(7) 1_545 ?
Cd1 O16 2.257(8) 3_544 ?
Cd1 O4 2.281(7) . ?
Cd1 O7 2.343(7) 1_565 ?
Cd2 O8 2.182(9) 3_564 ?
Cd2 O5 2.235(8) 4_565 ?
Cd2 O6 2.305(8) 4 ?
Cd2 O7 2.338(8) 4 ?
Cd2 O15 2.349(8) 2_674 ?
Cd2 O17 2.450(8) . ?
Cd2 C9 2.645(11) 4 ?
Cd3 O13 2.212(8) . ?
Cd3 O9 2.252(9) 3_554 ?
Cd3 O2S 2.269(10) . ?
Cd3 O17 2.270(8) 1_545 ?
Cd3 O16 2.336(7) 3_544 ?
Cd3 O5 2.374(8) 4 ?
O1 C1 1.190(17) . ?
O2 C2 1.222(15) . ?
O3 C3 1.201(15) . ?
O4 C6 1.229(14) . ?
O5 C6 1.281(15) . ?
O5 Cd2 2.235(8) 4_465 ?
O5 Cd3 2.374(8) 4_455 ?
O6 C9 1.228(14) . ?
O6 Cd2 2.305(7) 4_455 ?
O7 C9 1.274(14) . ?
O7 Cd2 2.338(8) 4_455 ?
O7 Cd1 2.343(7) 1_545 ?
O8 C12 1.215(15) . ?
O8 Cd2 2.182(9) 3_535 ?
O9 C12 1.270(15) . ?
O9 Cd3 2.252(9) 3_545 ?
O10 C13 1.221(15) . ?
O11 C14 1.184(15) . ?
O12 C15 1.225(15) . ?
O13 C18 1.241(14) . ?
O14 C18 1.245(15) . ?
O15 C24 1.208(13) . ?
O15 Cd2 2.349(8) 2_675 ?
O16 C24 1.301(14) . ?
O16 Cd1 2.257(8) 3 ?
O16 Cd3 2.336(7) 3 ?
O17 C21 1.296(14) . ?
O17 Cd3 2.270(8) 1_565 ?
O18 C21 1.236(13) . ?
O18 Cd1 2.257(7) 1_565 ?
O1S C1S 1.222(18) . ?
O2S C6S 1.243(18) . ?
N1 C3 1.367(16) . ?
N1 C1 1.417(15) . ?
N1 C4 1.468(15) . ?
N2 C2 1.381(16) . ?
N2 C1 1.388(16) . ?
N2 C7 1.451(15) . ?
N3 C2 1.348(16) . ?
N3 C3 1.405(16) . ?
N3 C10 1.465(15) . ?
N4 C15 1.353(15) . ?
N4 C13 1.380(15) . ?
N4 C16 1.513(15) . ?
N5 C14 1.360(15) . ?
N5 C15 1.415(15) . ?
N5 C19 1.440(14) . ?
N6 C13 1.386(16) . ?
N6 C14 1.422(15) . ?
N6 C22 1.453(15) . ?
N1S C1S 1.36(2) . ?
N1S C4S 1.44(2) . ?
N1S C2S 1.49(2) . ?
N2S C6S 1.316(16) . ?
N2S C7S 1.455(19) . ?
N2S C9S 1.47(2) . ?
C4 C5 1.513(15) . ?
C5 C6 1.511(16) . ?
C7 C8 1.487(16) . ?
C8 C9 1.558(17) . ?
C9 Cd2 2.645(11) 4_455 ?
C10 C11 1.543(17) . ?
C11 C12 1.517(17) . ?
C16 C17 1.525(17) . ?
C17 C18 1.510(14) . ?
C19 C20 1.514(15) . ?
C20 C21 1.536(15) . ?
C22 C23 1.512(18) . ?
C23 C24 1.503(18) . ?
C2S C3S 1.47(3) . ?
C4S C5S 1.46(3) . ?
C7S C8S 1.51(2) . ?
C9S C10S 1.44(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
O14 Cd1 O1S 90.3(4) . . ?
O14 Cd1 O18 101.6(3) . 1_545 ?
O1S Cd1 O18 88.9(3) . 1_545 ?
O14 Cd1 O16 95.2(3) . 3_544 ?
O1S Cd1 O16 173.7(3) . 3_544 ?
O18 Cd1 O16 92.9(3) 1_545 3_544 ?
O14 Cd1 O4 170.1(3) . . ?
O1S Cd1 O4 85.9(4) . . ?
O18 Cd1 O4 87.5(3) 1_545 . ?
O16 Cd1 O4 88.2(3) 3_544 . ?
O14 Cd1 O7 86.3(3) . 1_565 ?
O1S Cd1 O7 82.3(3) . 1_565 ?
O18 Cd1 O7 168.3(3) 1_545 1_565 ?
O16 Cd1 O7 95.0(3) 3_544 1_565 ?
O4 Cd1 O7 84.2(3) . 1_565 ?
O8 Cd2 O5 107.3(3) 3_564 4_565 ?
O8 Cd2 O6 96.8(3) 3_564 4 ?
O5 Cd2 O6 153.7(4) 4_565 4 ?
O8 Cd2 O7 150.9(3) 3_564 4 ?
O5 Cd2 O7 101.4(3) 4_565 4 ?
O6 Cd2 O7 56.3(3) 4 4 ?
O8 Cd2 O15 86.9(3) 3_564 2_674 ?
O5 Cd2 O15 103.5(3) 4_565 2_674 ?
O6 Cd2 O15 87.9(3) 4 2_674 ?
O7 Cd2 O15 81.5(3) 4 2_674 ?
O8 Cd2 O17 90.8(3) 3_564 . ?
O5 Cd2 O17 71.3(3) 4_565 . ?
O6 Cd2 O17 98.5(3) 4 . ?
O7 Cd2 O17 103.2(3) 4 . ?
O15 Cd2 O17 173.4(3) 2_674 . ?
O8 Cd2 C9 123.1(4) 3_564 4 ?
O5 Cd2 C9 129.6(4) 4_565 4 ?
O6 Cd2 C9 27.7(3) 4 4 ?
O7 Cd2 C9 28.8(3) 4 4 ?
O15 Cd2 C9 81.9(3) 2_674 4 ?
O17 Cd2 C9 104.5(3) . 4 ?
O13 Cd3 O9 157.7(3) . 3_554 ?
O13 Cd3 O2S 80.9(4) . . ?
O9 Cd3 O2S 82.7(4) 3_554 . ?
O13 Cd3 O17 105.1(3) . 1_545 ?
O9 Cd3 O17 89.8(3) 3_554 1_545 ?
O2S Cd3 O17 171.2(4) . 1_545 ?
O13 Cd3 O16 101.8(3) . 3_544 ?
O9 Cd3 O16 93.3(3) 3_554 3_544 ?
O2S Cd3 O16 90.4(3) . 3_544 ?
O17 Cd3 O16 94.6(3) 1_545 3_544 ?
O13 Cd3 O5 89.4(3) . 4 ?
O9 Cd3 O5 79.3(3) 3_554 4 ?
O2S Cd3 O5 101.9(4) . 4 ?
O17 Cd3 O5 72.2(3) 1_545 4 ?
O16 Cd3 O5 164.6(3) 3_544 4 ?
C6 O4 Cd1 142.3(8) . . ?
C6 O5 Cd2 114.6(7) . 4_465 ?
C6 O5 Cd3 144.5(7) . 4_455 ?
Cd2 O5 Cd3 99.5(3) 4_465 4_455 ?
C9 O6 Cd2 91.8(7) . 4_455 ?
C9 O7 Cd2 89.1(7) . 4_455 ?
C9 O7 Cd1 134.8(7) . 1_545 ?
Cd2 O7 Cd1 109.4(3) 4_455 1_545 ?
C12 O8 Cd2 118.1(9) . 3_535 ?
C12 O9 Cd3 142.8(8) . 3_545 ?
C18 O13 Cd3 128.9(7) . . ?
C18 O14 Cd1 135.0(7) . . ?
C24 O15 Cd2 152.4(9) . 2_675 ?
C24 O16 Cd1 122.8(7) . 3 ?
C24 O16 Cd3 136.2(7) . 3 ?
Cd1 O16 Cd3 101.1(3) 3 3 ?
C21 O17 Cd3 125.9(7) . 1_565 ?
C21 O17 Cd2 136.5(7) . . ?
Cd3 O17 Cd2 96.3(3) 1_565 . ?
C21 O18 Cd1 143.1(8) . 1_565 ?
C1S O1S Cd1 118.7(10) . . ?
C6S O2S Cd3 130.3(9) . . ?
C3 N1 C1 122.9(11) . . ?
C3 N1 C4 120.3(11) . . ?
C1 N1 C4 116.7(10) . . ?
C2 N2 C1 122.6(11) . . ?
C2 N2 C7 119.1(11) . . ?
C1 N2 C7 118.1(11) . . ?
C2 N3 C3 123.7(10) . . ?
C2 N3 C10 116.7(11) . . ?
C3 N3 C10 118.4(11) . . ?
C15 N4 C13 125.0(10) . . ?
C15 N4 C16 117.9(10) . . ?
C13 N4 C16 117.0(10) . . ?
C14 N5 C15 122.9(10) . . ?
C14 N5 C19 117.1(10) . . ?
C15 N5 C19 120.0(9) . . ?
C13 N6 C14 122.8(10) . . ?
C13 N6 C22 119.1(10) . . ?
C14 N6 C22 117.3(10) . . ?
C1S N1S C4S 118.9(18) . . ?
C1S N1S C2S 117.5(14) . . ?
C4S N1S C2S 123.6(17) . . ?
C6S N2S C7S 122.0(14) . . ?
C6S N2S C9S 118.3(14) . . ?
C7S N2S C9S 119.0(13) . . ?
O1 C1 N2 121.5(12) . . ?
O1 C1 N1 122.6(13) . . ?
N2 C1 N1 115.8(12) . . ?
O2 C2 N3 122.6(12) . . ?
O2 C2 N2 119.7(12) . . ?
N3 C2 N2 117.5(11) . . ?
O3 C3 N1 121.7(12) . . ?
O3 C3 N3 122.3(12) . . ?
N1 C3 N3 116.0(11) . . ?
N1 C4 C5 110.4(9) . . ?
C6 C5 C4 107.8(9) . . ?
O4 C6 O5 121.8(11) . . ?
O4 C6 C5 121.1(11) . . ?
O5 C6 C5 117.0(10) . . ?
N2 C7 C8 112.0(10) . . ?
C7 C8 C9 108.4(9) . . ?
O6 C9 O7 122.2(10) . . ?
O6 C9 C8 119.0(10) . . ?
O7 C9 C8 118.7(10) . . ?
O6 C9 Cd2 60.6(6) . 4_455 ?
O7 C9 Cd2 62.1(6) . 4_455 ?
C8 C9 Cd2 176.3(9) . 4_455 ?
N3 C10 C11 113.2(10) . . ?
C12 C11 C10 104.1(10) . . ?
O8 C12 O9 125.2(12) . . ?
O8 C12 C11 117.3(12) . . ?
O9 C12 C11 117.1(11) . . ?
O10 C13 N4 122.3(12) . . ?
O10 C13 N6 122.1(11) . . ?
N4 C13 N6 115.6(10) . . ?
O11 C14 N5 123.7(12) . . ?
O11 C14 N6 120.1(12) . . ?
N5 C14 N6 116.3(10) . . ?
O12 C15 N4 123.0(11) . . ?
O12 C15 N5 120.5(11) . . ?
N4 C15 N5 116.6(10) . . ?
N4 C16 C17 110.2(9) . . ?
C18 C17 C16 114.8(10) . . ?
O13 C18 O14 126.8(10) . . ?
O13 C18 C17 117.6(10) . . ?
O14 C18 C17 115.6(10) . . ?
N5 C19 C20 112.8(9) . . ?
C19 C20 C21 112.2(9) . . ?
O18 C21 O17 123.0(10) . . ?
O18 C21 C20 119.2(10) . . ?
O17 C21 C20 117.7(9) . . ?
N6 C22 C23 112.9(10) . . ?
C24 C23 C22 113.4(10) . . ?
O15 C24 O16 124.5(11) . . ?
O15 C24 C23 119.5(11) . . ?
O16 C24 C23 115.9(9) . . ?
O1S C1S N1S 123.9(16) . . ?
C3S C2S N1S 109.7(16) . . ?
N1S C4S C5S 119.6(19) . . ?
O2S C6S N2S 123.2(14) . . ?
N2S C7S C8S 114.8(16) . . ?
C10S C9S N2S 111(2) . . ?

_diffrn_measured_fraction_theta_max 0.952
_diffrn_reflns_theta_full        27.00
_diffrn_measured_fraction_theta_full 0.952
_refine_diff_density_max         2.261
_refine_diff_density_min         -0.835
_refine_diff_density_rms         0.183

#= = =END

data_{[Cd1.(tci).ProH].2PrOH}n_(3)
_database_code_depnum_ccdc_archive 'CCDC 695570'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C21 H36 Cd1.50 N3 O12'
_chemical_formula_weight         691.13

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           triclinic
_symmetry_space_group_name_H-M   P-1

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

_cell_length_a                   9.550(2)
_cell_length_b                   13.300(5)
_cell_length_c                   13.377(4)
_cell_angle_alpha                61.820(5)
_cell_angle_beta                 69.880(7)
_cell_angle_gamma                76.100(5)
_cell_volume                     1400.1(7)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.11
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.639
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             702
_exptl_absorpt_coefficient_mu    1.212
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.8297
_exptl_absorpt_correction_T_max  0.8782
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71069
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Rigaku/MSC Mercury CCD'
_diffrn_measurement_method       ω
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            10292
_diffrn_reflns_av_R_equivalents  0.0308
_diffrn_reflns_av_sigmaI/netI    0.0378
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         3.17
_diffrn_reflns_theta_max         27.00
_reflns_number_total             5839
_reflns_number_gt                5240
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       crystalclear
_computing_cell_refinement       crystalclear
_computing_data_reduction        crystalclear
_computing_structure_solution    SIR-97
_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)+(0.1175P)²+16.2314P] 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         5839
_refine_ls_number_parameters     268
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0866
_refine_ls_R_factor_gt           0.0814
_refine_ls_wR_factor_ref         0.2588
_refine_ls_wR_factor_gt          0.2548
_refine_ls_goodness_of_fit_ref   1.163
_refine_ls_restrained_S_all      1.163
_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 1.0000 -1.0000 0.0322(3) Uani 1 2 d S . .
Cd2 Cd -0.37310(7) 0.10733(5) -0.09513(6) 0.0344(2) Uani 1 1 d . . .
O1 O -0.2092(12) 0.5178(7) -0.9928(7) 0.062(2) Uani 1 1 d . . .
O2 O -0.3836(13) 0.2206(7) -0.6450(8) 0.072(3) Uani 1 1 d . . .
O3 O -0.2411(13) 0.5209(8) -0.6487(8) 0.071(3) Uani 1 1 d . . .
O4 O -0.4084(9) 0.2254(9) -1.0019(9) 0.067(3) Uani 1 1 d . . .
O6 O -0.4066(11) 0.2104(11) -0.2767(7) 0.090(4) Uani 1 1 d . . .
O7 O -0.1849(11) 0.1293(11) -0.2732(8) 0.083(3) Uani 1 1 d . . .
O8 O -0.3760(7) 0.9211(5) -0.9804(6) 0.0404(15) Uani 1 1 d . . .
O9 O -0.1376(7) 0.8687(5) -0.9847(7) 0.0415(15) Uani 1 1 d . . .
O1S O 0.0757(8) 1.0527(8) -1.1997(6) 0.056(2) Uani 1 1 d . . .
N1 N -0.2153(9) 0.5205(6) -0.8235(7) 0.0331(15) Uani 1 1 d . . .
N2 N -0.3001(10) 0.3691(7) -0.8212(7) 0.0383(17) Uani 1 1 d . . .
N3 N -0.3079(10) 0.3666(7) -0.6440(7) 0.0438(19) Uani 1 1 d . . .
C1 C -0.2386(11) 0.4727(8) -0.8884(8) 0.0374(19) Uani 1 1 d . . .
C2 C -0.3325(12) 0.3121(8) -0.7010(9) 0.043(2) Uani 1 1 d . . .
C3 C -0.2541(12) 0.4737(8) -0.7022(9) 0.043(2) Uani 1 1 d . . .
C4 C -0.3485(11) 0.3233(9) -0.8844(10) 0.043(2) Uani 1 1 d . . .
H4A H -0.3787 0.3867 -0.9511 0.052 Uiso 1 1 calc R . .
H4B H -0.4350 0.2811 -0.8321 0.052 Uiso 1 1 calc R . .
C5 C -0.2275(11) 0.2460(10) -0.9271(10) 0.047(2) Uani 1 1 d . . .
H5A H -0.1949 0.1838 -0.8608 0.056 Uiso 1 1 calc R . .
H5B H -0.1422 0.2888 -0.9816 0.056 Uiso 1 1 calc R . .
C6 C -0.2809(10) 0.1971(8) -0.9876(8) 0.0359(18) Uani 1 1 d . . .
C7 C -0.3547(13) 0.3147(10) -0.5140(9) 0.049(2) Uani 1 1 d . . .
H7A H -0.4365 0.2685 -0.4862 0.059 Uiso 1 1 calc R . .
H7B H -0.3917 0.3752 -0.4878 0.059 Uiso 1 1 calc R . .
C8 C -0.2318(15) 0.2419(13) -0.4607(10) 0.068(4) Uani 1 1 d . . .
H8A H -0.1954 0.1814 -0.4868 0.082 Uiso 1 1 calc R . .
H8B H -0.1498 0.2882 -0.4893 0.082 Uiso 1 1 calc R . .
C9 C -0.2759(13) 0.1897(11) -0.3306(9) 0.054(3) Uani 1 1 d . . .
C10 C -0.1646(10) 0.6376(7) -0.8883(10) 0.040(2) Uani 1 1 d . . .
H10A H -0.0997 0.6483 -0.9659 0.048 Uiso 1 1 calc R . .
H10B H -0.1083 0.6477 -0.8461 0.048 Uiso 1 1 calc R . .
C11 C -0.2981(10) 0.7234(7) -0.8995(9) 0.038(2) Uani 1 1 d . . .
H11A H -0.3645 0.7084 -0.8215 0.046 Uiso 1 1 calc R . .
H11B H -0.3516 0.7131 -0.9435 0.046 Uiso 1 1 calc R . .
C12 C -0.2618(10) 0.8475(7) -0.9602(8) 0.0328(18) Uani 1 1 d . . .
C1C C 0.2080(19) 1.1042(14) -1.2857(14) 0.080(4) Uani 1 1 d . . .
H1C H 0.2814 1.0805 -1.2406 0.095 Uiso 1 1 calc R . .
C2C C 0.192(4) 1.226(2) -1.333(3) 0.180(14) Uani 1 1 d . . .
H2C1 H 0.1427 1.2493 -1.2701 0.270 Uiso 1 1 calc R . .
H2C2 H 0.1323 1.2568 -1.3879 0.270 Uiso 1 1 calc R . .
H2C3 H 0.2885 1.2545 -1.3722 0.270 Uiso 1 1 calc R . .
C3C C 0.276(5) 1.073(3) -1.372(3) 0.27(3) Uani 1 1 d . . .
H3C1 H 0.2910 0.9904 -1.3398 0.412 Uiso 1 1 calc R . .
H3C2 H 0.3714 1.1035 -1.4126 0.412 Uiso 1 1 calc R . .
H3C3 H 0.2156 1.1006 -1.4257 0.412 Uiso 1 1 calc R . .
O5 O -0.1958(8) 0.1290(6) -1.0253(7) 0.0465(17) 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
Cd1 O5 2.214(6) 2_563 ?
Cd1 O5 2.214(6) 1_565 ?
Cd1 O1S 2.301(7) . ?
Cd1 O1S 2.301(7) 2_573 ?
Cd1 O9 2.323(6) . ?
Cd1 O9 2.323(6) 2_573 ?
Cd2 O8 2.215(6) 1_546 ?
Cd2 O6 2.249(8) . ?
Cd2 O8 2.305(6) 2_464 ?
Cd2 O5 2.324(6) 1_556 ?
Cd2 O4 2.332(8) 1_556 ?
Cd2 O7 2.375(9) . ?
Cd2 C9 2.684(10) . ?
Cd2 C6 2.695(9) 1_556 ?
O1 C1 1.188(12) . ?
O2 C2 1.206(13) . ?
O3 C3 1.203(12) . ?
O4 C6 1.238(11) . ?
O4 Cd2 2.332(8) 1_554 ?
O6 C9 1.248(14) . ?
O7 C9 1.237(14) . ?
O8 C12 1.289(10) . ?
O8 Cd2 2.215(6) 1_564 ?
O8 Cd2 2.305(6) 2_464 ?
O9 C12 1.183(11) . ?
O1S C1C 1.436(16) . ?
N1 C3 1.378(12) . ?
N1 C1 1.389(11) . ?
N1 C10 1.487(11) . ?
N2 C2 1.369(12) . ?
N2 C1 1.381(13) . ?
N2 C4 1.479(12) . ?
N3 C2 1.375(13) . ?
N3 C3 1.388(13) . ?
N3 C7 1.476(12) . ?
C4 C5 1.500(13) . ?
C5 C6 1.511(13) . ?
C6 O5 1.237(11) . ?
C6 Cd2 2.695(9) 1_554 ?
C7 C8 1.484(16) . ?
C8 C9 1.477(14) . ?
C10 C11 1.491(12) . ?
C11 C12 1.523(12) . ?
C1C C3C 1.32(3) . ?
C1C C2C 1.43(3) . ?
O5 Cd1 2.214(6) 1_545 ?
O5 Cd2 2.324(6) 1_554 ?

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
O5 Cd1 O5 180.000(1) 2_563 1_565 ?
O5 Cd1 O1S 91.1(3) 2_563 . ?
O5 Cd1 O1S 88.9(3) 1_565 . ?
O5 Cd1 O1S 88.9(3) 2_563 2_573 ?
O5 Cd1 O1S 91.1(3) 1_565 2_573 ?
O1S Cd1 O1S 180.000(1) . 2_573 ?
O5 Cd1 O9 91.1(2) 2_563 . ?
O5 Cd1 O9 88.9(2) 1_565 . ?
O1S Cd1 O9 87.0(3) . . ?
O1S Cd1 O9 93.0(3) 2_573 . ?
O5 Cd1 O9 88.9(2) 2_563 2_573 ?
O5 Cd1 O9 91.1(2) 1_565 2_573 ?
O1S Cd1 O9 93.0(3) . 2_573 ?
O1S Cd1 O9 87.0(3) 2_573 2_573 ?
O9 Cd1 O9 180.000(1) . 2_573 ?
O8 Cd2 O6 130.6(4) 1_546 . ?
O8 Cd2 O8 75.8(2) 1_546 2_464 ?
O6 Cd2 O8 89.9(3) . 2_464 ?
O8 Cd2 O5 93.8(3) 1_546 1_556 ?
O6 Cd2 O5 126.7(4) . 1_556 ?
O8 Cd2 O5 134.5(3) 2_464 1_556 ?
O8 Cd2 O4 116.3(3) 1_546 1_556 ?
O6 Cd2 O4 110.6(4) . 1_556 ?
O8 Cd2 O4 90.2(3) 2_464 1_556 ?
O5 Cd2 O4 54.6(2) 1_556 1_556 ?
O8 Cd2 O7 106.9(3) 1_546 . ?
O6 Cd2 O7 55.0(3) . . ?
O8 Cd2 O7 137.0(3) 2_464 . ?
O5 Cd2 O7 88.5(3) 1_556 . ?
O4 Cd2 O7 122.9(4) 1_556 . ?
O8 Cd2 C9 121.8(3) 1_546 . ?
O6 Cd2 C9 27.5(3) . . ?
O8 Cd2 C9 114.2(3) 2_464 . ?
O5 Cd2 C9 109.0(3) 1_556 . ?
O4 Cd2 C9 120.6(4) 1_556 . ?
O7 Cd2 C9 27.5(3) . . ?
O8 Cd2 C6 106.3(3) 1_546 1_556 ?
O6 Cd2 C6 122.6(4) . 1_556 ?
O8 Cd2 C6 113.1(3) 2_464 1_556 ?
O5 Cd2 C6 27.3(2) 1_556 1_556 ?
O4 Cd2 C6 27.3(3) 1_556 1_556 ?
O7 Cd2 C6 107.2(4) . 1_556 ?
C9 Cd2 C6 118.3(4) . 1_556 ?
C6 O4 Cd2 92.9(6) . 1_554 ?
C9 O6 Cd2 96.0(7) . . ?
C9 O7 Cd2 90.3(7) . . ?
C12 O8 Cd2 126.9(6) . 1_564 ?
C12 O8 Cd2 128.9(6) . 2_464 ?
Cd2 O8 Cd2 104.2(2) 1_564 2_464 ?
C12 O9 Cd1 142.3(6) . . ?
C1C O1S Cd1 129.6(9) . . ?
C3 N1 C1 124.5(8) . . ?
C3 N1 C10 117.3(8) . . ?
C1 N1 C10 117.6(8) . . ?
C2 N2 C1 125.2(8) . . ?
C2 N2 C4 117.9(9) . . ?
C1 N2 C4 116.5(8) . . ?
C2 N3 C3 123.2(8) . . ?
C2 N3 C7 118.7(9) . . ?
C3 N3 C7 117.8(9) . . ?
O1 C1 N2 122.9(9) . . ?
O1 C1 N1 122.7(9) . . ?
N2 C1 N1 114.4(8) . . ?
O2 C2 N2 123.7(10) . . ?
O2 C2 N3 120.0(10) . . ?
N2 C2 N3 116.3(9) . . ?
O3 C3 N1 122.8(10) . . ?
O3 C3 N3 121.1(10) . . ?
N1 C3 N3 116.0(8) . . ?
N2 C4 C5 112.5(8) . . ?
C4 C5 C6 111.6(8) . . ?
O5 C6 O4 119.2(9) . . ?
O5 C6 C5 119.8(8) . . ?
O4 C6 C5 121.0(8) . . ?
O5 C6 Cd2 59.4(5) . 1_554 ?
O4 C6 Cd2 59.8(5) . 1_554 ?
C5 C6 Cd2 179.2(7) . 1_554 ?
N3 C7 C8 113.1(9) . . ?
C9 C8 C7 114.0(10) . . ?
O7 C9 O6 118.7(10) . . ?
O7 C9 C8 121.8(11) . . ?
O6 C9 C8 119.5(11) . . ?
O7 C9 Cd2 62.2(6) . . ?
O6 C9 Cd2 56.5(5) . . ?
C8 C9 Cd2 175.7(9) . . ?
N1 C10 C11 109.0(7) . . ?
C10 C11 C12 114.3(8) . . ?
O9 C12 O8 126.1(8) . . ?
O9 C12 C11 120.1(8) . . ?
O8 C12 C11 113.8(8) . . ?
C3C C1C C2C 109(3) . . ?
C3C C1C O1S 119.6(19) . . ?
C2C C1C O1S 113.2(17) . . ?
C6 O5 Cd1 143.3(6) . 1_545 ?
C6 O5 Cd2 93.3(5) . 1_554 ?
Cd1 O5 Cd2 119.1(3) 1_545 1_554 ?

_diffrn_measured_fraction_theta_max 0.955
_diffrn_reflns_theta_full        27.00
_diffrn_measured_fraction_theta_full 0.955
_refine_diff_density_max         2.390
_refine_diff_density_min         -1.433
_refine_diff_density_rms         0.243

#= = =END


