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

data_global
_journal_name_full               CrystEngComm

_journal_coden_Cambridge         1350

_publ_contact_author_name        'Junfeng Bai'
_publ_contact_author_email       BJUNFENG@NJU.EDU.CN

_publ_section_title              
;
pH-Controlled Change of the Coordination Modes
of the Highly Symmetrical Multitopic Ligand and Metal-Oxygen Arrays
to Construct Coordination Assemblies
;
loop_
_publ_author_name
'Junfeng Bai'
'Zhuxiu Zhang'
'Bo Zheng'

# Attachment '732255.cif'

data_260304g
_database_code_depnum_ccdc_archive 'CCDC 732255'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C8 H2 Cd3 O10'
_chemical_formula_sum            'C8 H2 Cd3 O10'
_chemical_formula_weight         595.33

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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   'C 2/m'
_symmetry_space_group_name_Hall  '-C 2y'

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

_cell_length_a                   13.2366(13)
_cell_length_b                   7.1753(6)
_cell_length_c                   12.7690(12)
_cell_angle_alpha                90.00
_cell_angle_beta                 117.344(2)
_cell_angle_gamma                90.00
_cell_volume                     1077.25(17)
_cell_formula_units_Z            4
_cell_measurement_temperature    291(2)
_cell_measurement_reflns_used    2364
_cell_measurement_theta_min      3.084
_cell_measurement_theta_max      28.258

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.19
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    3.671
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1096
_exptl_absorpt_coefficient_mu    5.925
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.216
_exptl_absorpt_correction_T_max  0.315
_exptl_absorpt_process_details   'SADABS(Brucker, 2000)'

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      291(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker Smart Aepex 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            2915
_diffrn_reflns_av_R_equivalents  0.0319
_diffrn_reflns_av_sigmaI/netI    0.0335
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_theta_min         1.80
_diffrn_reflns_theta_max         26.00
_reflns_number_total             1139
_reflns_number_gt                1094
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'SMART (Bruker, 2000)'
_computing_cell_refinement       SMART
_computing_data_reduction        'SAINT (Bruker, 2000)'
_computing_structure_solution    'SHELXTL (Bruker, 2000)'
_computing_structure_refinement  SHELXTL
_computing_molecular_graphics    SHELXTL
_computing_publication_material  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)+(0.0335P)²+2.3520P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     SHELXL
_refine_ls_extinction_coef       0.0046(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         1139
_refine_ls_number_parameters     110
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0233
_refine_ls_R_factor_gt           0.0221
_refine_ls_wR_factor_ref         0.0593
_refine_ls_wR_factor_gt          0.0586
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_restrained_S_all      1.063
_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 0.5262(4) 0.5000 0.3865(4) 0.0134(10) Uani 1 2 d S . .
C2 C 0.4446(3) 0.3559(5) 0.3155(3) 0.0128(7) Uani 1 1 d . . .
C3 C 0.3693(4) 0.5000 0.2334(4) 0.0132(10) Uani 1 2 d S . .
C4 C 0.8764(3) 0.6010(5) 0.7644(3) 0.0135(7) Uani 1 1 d . . .
C5 C 0.9916(3) 0.6032(5) 0.8635(3) 0.0153(8) Uani 1 1 d . . .
Cd1 Cd 0.7500 0.7500 0.5000 0.01431(15) Uani 1 2 d S . .
Cd2 Cd 0.70920(3) 1.0000 0.71437(3) 0.01312(15) Uani 1 2 d S . .
Cd3 Cd 0.7500 1.2500 1.0000 0.01409(15) Uani 1 2 d S . .
O1 O 0.6230(3) 0.5000 0.4699(3) 0.0156(7) Uani 1 2 d S . .
O2 O 0.4437(2) 0.1841(4) 0.3255(3) 0.0206(6) Uani 1 1 d . . .
O3 O 0.2831(3) 0.5000 0.1370(3) 0.0151(7) Uani 1 2 d S . .
O4 O 0.8095(2) 0.7275(4) 0.7012(2) 0.0180(6) Uani 1 1 d . . .
O5 O 1.0594(2) 0.7282(4) 0.9191(3) 0.0220(6) Uani 1 1 d . . .
O6 O 0.6629(3) 1.0000 0.5205(3) 0.0129(7) Uani 1 2 d S . .
H6 H 0.5916 1.0000 0.4756 0.016 Uiso 1 2 d SR . .
O7 O 0.7810(3) 1.0000 0.9067(3) 0.0151(7) Uani 1 2 d S . .
H7 H 0.8518 1.0000 0.9390 0.018 Uiso 1 2 d SR . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
C1 0.013(2) 0.014(2) 0.015(3) 0.000 0.008(2) 0.000
C2 0.0130(15) 0.0143(17) 0.0103(17) -0.0016(14) 0.0048(13) 0.0005(13)
C3 0.015(2) 0.013(2) 0.011(2) 0.000 0.006(2) 0.000
C4 0.0145(16) 0.0166(19) 0.0120(17) -0.0008(15) 0.0082(14) 0.0015(14)
C5 0.0117(16) 0.024(2) 0.0119(17) 0.0019(15) 0.0069(14) 0.0019(14)
Cd1 0.0210(2) 0.0096(2) 0.0124(2) -0.00195(13) 0.00773(18) -0.00055(12)
Cd2 0.0171(2) 0.0120(2) 0.0111(2) 0.000 0.00728(17) 0.000
Cd3 0.0152(2) 0.0105(2) 0.0138(2) -0.00086(13) 0.00429(17) -0.00055(12)
O1 0.0128(16) 0.0128(18) 0.0176(19) 0.000 0.0038(15) 0.000
O2 0.0196(12) 0.0084(13) 0.0324(16) 0.0011(12) 0.0108(12) -0.0008(10)
O3 0.0163(17) 0.0154(18) 0.0113(18) 0.000 0.0043(14) 0.000
O4 0.0199(13) 0.0181(14) 0.0140(14) 0.0012(11) 0.0060(11) 0.0062(10)
O5 0.0178(13) 0.0215(15) 0.0218(15) -0.0074(11) 0.0048(12) -0.0072(10)
O6 0.0106(16) 0.0176(18) 0.0086(17) 0.000 0.0027(13) 0.000
O7 0.0179(17) 0.0136(18) 0.0123(18) 0.000 0.0058(14) 0.000

_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 O1 1.233(6) . ?
C1 C2 1.469(5) . ?
C1 C2 1.469(5) 6_565 ?
C2 O2 1.241(5) . ?
C2 C3 1.483(5) . ?
C3 O3 1.236(6) . ?
C3 C2 1.483(5) 6_565 ?
C4 O4 1.266(4) . ?
C4 C4 1.449(7) 6_565 ?
C4 C5 1.468(5) . ?
C5 O5 1.236(5) . ?
C5 C5 1.481(8) 6_565 ?
Cd1 O6 2.2116(19) 7_666 ?
Cd1 O6 2.2116(19) . ?
Cd1 O4 2.321(3) 7_666 ?
Cd1 O4 2.321(3) . ?
Cd1 O1 2.366(2) . ?
Cd1 O1 2.366(2) 7_666 ?
Cd2 O7 2.189(3) . ?
Cd2 O6 2.261(3) . ?
Cd2 O2 2.270(3) 5_666 ?
Cd2 O2 2.270(3) 2_666 ?
Cd2 O4 2.412(3) 6_575 ?
Cd2 O4 2.412(2) . ?
Cd3 O5 2.250(3) 3_455 ?
Cd3 O5 2.250(3) 5_777 ?
Cd3 O7 2.292(2) . ?
Cd3 O7 2.292(2) 7_677 ?
Cd3 O3 2.401(2) 3_556 ?
Cd3 O3 2.401(2) 5_676 ?
O1 Cd1 2.366(2) 4_646 ?
O2 Cd2 2.270(3) 5_666 ?
O3 Cd3 2.401(2) 2_646 ?
O3 Cd3 2.401(2) 3_444 ?
O5 Cd3 2.250(3) 3_545 ?
O6 Cd1 2.2116(19) 4_656 ?
O6 H6 0.8500 . ?
O7 Cd3 2.292(2) 4_647 ?
O7 H7 0.8330 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 C1 C2 135.3(2) . . ?
O1 C1 C2 135.3(2) . 6_565 ?
C2 C1 C2 89.5(4) . 6_565 ?
O2 C2 C1 132.5(3) . . ?
O2 C2 C3 136.9(3) . . ?
C1 C2 C3 90.6(3) . . ?
O3 C3 C2 135.82(19) . 6_565 ?
O3 C3 C2 135.82(19) . . ?
C2 C3 C2 88.3(4) 6_565 . ?
O4 C4 C4 135.8(2) . 6_565 ?
O4 C4 C5 133.4(3) . . ?
C4 C4 C5 90.6(2) 6_565 . ?
O5 C5 C4 134.1(4) . . ?
O5 C5 C5 136.5(2) . 6_565 ?
C4 C5 C5 89.4(2) . 6_565 ?
O6 Cd1 O6 180.000(1) 7_666 . ?
O6 Cd1 O4 81.72(10) 7_666 7_666 ?
O6 Cd1 O4 98.28(10) . 7_666 ?
O6 Cd1 O4 98.28(10) 7_666 . ?
O6 Cd1 O4 81.72(10) . . ?
O4 Cd1 O4 180.000(1) 7_666 . ?
O6 Cd1 O1 74.69(10) 7_666 . ?
O6 Cd1 O1 105.31(10) . . ?
O4 Cd1 O1 91.04(11) 7_666 . ?
O4 Cd1 O1 88.96(11) . . ?
O6 Cd1 O1 105.31(10) 7_666 7_666 ?
O6 Cd1 O1 74.69(10) . 7_666 ?
O4 Cd1 O1 88.96(11) 7_666 7_666 ?
O4 Cd1 O1 91.04(11) . 7_666 ?
O1 Cd1 O1 180.000(1) . 7_666 ?
O7 Cd2 O6 171.24(12) . . ?
O7 Cd2 O2 97.72(10) . 5_666 ?
O6 Cd2 O2 89.39(10) . 5_666 ?
O7 Cd2 O2 97.72(10) . 2_666 ?
O6 Cd2 O2 89.39(10) . 2_666 ?
O2 Cd2 O2 71.16(13) 5_666 2_666 ?
O7 Cd2 O4 96.26(9) . 6_575 ?
O6 Cd2 O4 78.73(8) . 6_575 ?
O2 Cd2 O4 156.72(10) 5_666 6_575 ?
O2 Cd2 O4 88.59(9) 2_666 6_575 ?
O7 Cd2 O4 96.26(8) . . ?
O6 Cd2 O4 78.73(8) . . ?
O2 Cd2 O4 88.59(9) 5_666 . ?
O2 Cd2 O4 156.72(10) 2_666 . ?
O4 Cd2 O4 108.30(13) 6_575 . ?
O5 Cd3 O5 180.00(6) 3_455 5_777 ?
O5 Cd3 O7 97.91(11) 3_455 . ?
O5 Cd3 O7 82.09(11) 5_777 . ?
O5 Cd3 O7 82.09(11) 3_455 7_677 ?
O5 Cd3 O7 97.91(11) 5_777 7_677 ?
O7 Cd3 O7 180.000(1) . 7_677 ?
O5 Cd3 O3 94.22(11) 3_455 3_556 ?
O5 Cd3 O3 85.78(11) 5_777 3_556 ?
O7 Cd3 O3 77.15(10) . 3_556 ?
O7 Cd3 O3 102.85(10) 7_677 3_556 ?
O5 Cd3 O3 85.78(11) 3_455 5_676 ?
O5 Cd3 O3 94.22(11) 5_777 5_676 ?
O7 Cd3 O3 102.85(10) . 5_676 ?
O7 Cd3 O3 77.15(10) 7_677 5_676 ?
O3 Cd3 O3 180.000(1) 3_556 5_676 ?
C1 O1 Cd1 121.28(17) . . ?
C1 O1 Cd1 121.28(17) . 4_646 ?
Cd1 O1 Cd1 98.59(12) . 4_646 ?
C2 O2 Cd2 127.3(2) . 5_666 ?
C3 O3 Cd3 120.11(16) . 2_646 ?
C3 O3 Cd3 120.11(16) . 3_444 ?
Cd3 O3 Cd3 96.66(12) 2_646 3_444 ?
C4 O4 Cd1 122.5(2) . . ?
C4 O4 Cd2 141.6(2) . . ?
Cd1 O4 Cd2 95.91(9) . . ?
C5 O5 Cd3 132.7(3) . 3_545 ?
Cd1 O6 Cd1 108.41(14) . 4_656 ?
Cd1 O6 Cd2 103.63(10) . . ?
Cd1 O6 Cd2 103.63(10) 4_656 . ?
Cd1 O6 H6 113.5 . . ?
Cd1 O6 H6 113.5 4_656 . ?
Cd2 O6 H6 113.3 . . ?
Cd2 O7 Cd3 119.61(10) . 4_647 ?
Cd2 O7 Cd3 119.61(10) . . ?
Cd3 O7 Cd3 103.00(13) 4_647 . ?
Cd2 O7 H7 111.4 . . ?
Cd3 O7 H7 99.9 4_647 . ?
Cd3 O7 H7 99.9 . . ?

_diffrn_measured_fraction_theta_max 0.992
_diffrn_reflns_theta_full        26.00
_diffrn_measured_fraction_theta_full 0.992
_refine_diff_density_max         1.330
_refine_diff_density_min         -0.882
_refine_diff_density_rms         0.172

# Attachment '732256.cif'

data_1
_database_code_depnum_ccdc_archive 'CCDC 732256'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C2 H Cd O3'
_chemical_formula_sum            'C2 H Cd O3'
_chemical_formula_weight         185.43

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

_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_H-M   'P b c a'
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, z-1/2'
'-x-1/2, y-1/2, z'

_cell_length_a                   6.8958(3)
_cell_length_b                   5.8147(3)
_cell_length_c                   15.8331(8)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     634.86(5)
_cell_formula_units_Z            8
_cell_measurement_temperature    291(2)
_cell_measurement_reflns_used    2350
_cell_measurement_theta_min      2.573
_cell_measurement_theta_max      28.288

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.21
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    3.880
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             680
_exptl_absorpt_coefficient_mu    6.680
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.159
_exptl_absorpt_correction_T_max  0.251
_exptl_absorpt_process_details   'SADABS(Brucker, 2000)'

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      291(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker Smart Aepex 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            3062
_diffrn_reflns_av_R_equivalents  0.0607
_diffrn_reflns_av_sigmaI/netI    0.0343
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         2.57
_diffrn_reflns_theta_max         25.99
_reflns_number_total             625
_reflns_number_gt                597
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'SMART (Bruker, 2000)'
_computing_cell_refinement       SMART
_computing_data_reduction        'SAINT (Bruker, 2000)'
_computing_structure_solution    'SHELXTL (Bruker, 2000)'
_computing_structure_refinement  SHELXTL
_computing_molecular_graphics    SHELXTL
_computing_publication_material  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)+(0.0219P)²+0.5382P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     SHELXL
_refine_ls_extinction_coef       0.0160(7)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         625
_refine_ls_number_parameters     56
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0251
_refine_ls_R_factor_gt           0.0200
_refine_ls_wR_factor_ref         0.0447
_refine_ls_wR_factor_gt          0.0441
_refine_ls_goodness_of_fit_ref   1.075
_refine_ls_restrained_S_all      1.075
_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
O2 O 0.3502(3) 0.3085(4) 0.39203(14) 0.0173(5) Uani 1 1 d . . .
C2 C 0.4331(4) 0.4142(6) 0.4516(2) 0.0132(6) Uani 1 1 d . . .
Cd1 Cd 0.39710(3) 0.96733(4) 0.309487(13) 0.01213(15) Uani 1 1 d . . .
O1 O 0.5895(3) 0.7881(5) 0.40924(15) 0.0203(6) Uani 1 1 d . . .
O3 O 0.3368(3) 0.6480(4) 0.23362(13) 0.0129(4) Uani 1 1 d . . .
H3A H 0.2726 0.7014 0.1820 0.016 Uiso 1 1 calc R . .
C1 C 0.5391(4) 0.6303(5) 0.45871(18) 0.0138(6) Uani 1 1 d . . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
O2 0.0195(11) 0.0151(13) 0.0174(11) -0.0051(9) -0.0076(9) 0.0028(10)
C2 0.0123(14) 0.0126(15) 0.0146(14) -0.0007(12) -0.0003(11) 0.0031(12)
Cd1 0.01101(19) 0.0107(2) 0.01472(18) 0.00048(8) 0.00029(7) -0.00050(8)
O1 0.0187(12) 0.0211(14) 0.0211(12) 0.0101(10) -0.0041(9) -0.0047(9)
O3 0.0131(10) 0.0108(11) 0.0150(10) -0.0010(8) 0.0017(8) 0.0001(8)
C1 0.0096(14) 0.0174(17) 0.0144(14) 0.0001(11) -0.0008(12) 0.0028(12)

_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
O2 C2 1.263(4) . ?
O2 Cd1 2.339(2) 8_655 ?
O2 Cd1 2.397(2) 1_545 ?
C2 C1 1.456(4) 5_666 ?
C2 C1 1.458(5) . ?
Cd1 O3 2.222(2) 3_655 ?
Cd1 O3 2.250(2) . ?
Cd1 O3 2.269(2) 8_665 ?
Cd1 O1 2.311(2) . ?
Cd1 O2 2.339(2) 8_665 ?
Cd1 O2 2.397(2) 1_565 ?
O1 C1 1.255(4) . ?
O3 Cd1 2.222(2) 3_645 ?
O3 Cd1 2.269(2) 8_655 ?
O3 H3A 0.9800 . ?
C1 C2 1.456(4) 5_666 ?

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 O2 Cd1 123.7(2) . 8_655 ?
C2 O2 Cd1 138.5(2) . 1_545 ?
Cd1 O2 Cd1 96.92(8) 8_655 1_545 ?
O2 C2 C1 134.6(3) . 5_666 ?
O2 C2 C1 134.7(3) . . ?
C1 C2 C1 90.7(3) 5_666 . ?
O3 Cd1 O3 112.26(5) 3_655 . ?
O3 Cd1 O3 101.87(7) 3_655 8_665 ?
O3 Cd1 O3 88.17(7) . 8_665 ?
O3 Cd1 O1 87.07(8) 3_655 . ?
O3 Cd1 O1 95.66(9) . . ?
O3 Cd1 O1 168.16(8) 8_665 . ?
O3 Cd1 O2 163.87(8) 3_655 8_665 ?
O3 Cd1 O2 80.66(7) . 8_665 ?
O3 Cd1 O2 87.72(8) 8_665 8_665 ?
O1 Cd1 O2 81.88(8) . 8_665 ?
O3 Cd1 O2 83.55(8) 3_655 1_565 ?
O3 Cd1 O2 161.59(8) . 1_565 ?
O3 Cd1 O2 79.03(8) 8_665 1_565 ?
O1 Cd1 O2 94.48(9) . 1_565 ?
O2 Cd1 O2 85.63(7) 8_665 1_565 ?
C1 O1 Cd1 126.65(19) . . ?
Cd1 O3 Cd1 113.67(9) 3_645 . ?
Cd1 O3 Cd1 122.07(10) 3_645 8_655 ?
Cd1 O3 Cd1 103.34(8) . 8_655 ?
Cd1 O3 H3A 105.5 3_645 . ?
Cd1 O3 H3A 105.5 . . ?
Cd1 O3 H3A 105.5 8_655 . ?
O1 C1 C2 134.6(3) . 5_666 ?
O1 C1 C2 136.1(3) . . ?
C2 C1 C2 89.3(3) 5_666 . ?

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        25.99
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         0.951
_refine_diff_density_min         -0.983
_refine_diff_density_rms         0.267

# Attachment '732257.cif'

data_2
_database_code_depnum_ccdc_archive 'CCDC 732257'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C4 H2 Cd2 O6'
_chemical_formula_sum            'C4 H2 Cd2 O6'
_chemical_formula_weight         370.86

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

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

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

_cell_length_a                   3.5793(3)
_cell_length_b                   10.4878(9)
_cell_length_c                   8.5834(7)
_cell_angle_alpha                90.00
_cell_angle_beta                 99.5510(10)
_cell_angle_gamma                90.00
_cell_volume                     317.75(5)
_cell_formula_units_Z            2
_cell_measurement_temperature    291(2)
_cell_measurement_reflns_used    1275
_cell_measurement_theta_min      3.093
_cell_measurement_theta_max      28.220

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.19
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    3.876
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             340
_exptl_absorpt_coefficient_mu    6.673
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.175
_exptl_absorpt_correction_T_max  0.272
_exptl_absorpt_process_details   'SADABS(Brucker, 2000)'

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      291(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker Smart Aepex 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            1675
_diffrn_reflns_av_R_equivalents  0.0813
_diffrn_reflns_av_sigmaI/netI    0.0608
_diffrn_reflns_limit_h_min       -4
_diffrn_reflns_limit_h_max       4
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -5
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_theta_min         3.09
_diffrn_reflns_theta_max         26.00
_reflns_number_total             619
_reflns_number_gt                559
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'SMART (Bruker, 2000)'
_computing_cell_refinement       SMART
_computing_data_reduction        'SAINT (Bruker, 2000)'
_computing_structure_solution    'SHELXTL (Bruker, 2000)'
_computing_structure_refinement  SHELXTL
_computing_molecular_graphics    SHELXTL
_computing_publication_material  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)+(0.0250P)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     SHELXL
_refine_ls_extinction_coef       0.022(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         619
_refine_ls_number_parameters     56
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0299
_refine_ls_R_factor_gt           0.0275
_refine_ls_wR_factor_ref         0.0561
_refine_ls_wR_factor_gt          0.0546
_refine_ls_goodness_of_fit_ref   0.975
_refine_ls_restrained_S_all      0.975
_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
C1 C 0.5743(9) 0.5552(3) 0.6000(4) 0.0149(8) Uani 1 1 d . . .
C2 C 0.3533(10) 0.5762(4) 0.4425(5) 0.0149(8) Uani 1 1 d . . .
Cd1 Cd 1.21353(7) 0.62225(2) 0.92213(3) 0.01602(19) Uani 1 1 d . . .
O1 O 0.6586(8) 0.6226(2) 0.7216(4) 0.0190(7) Uani 1 1 d . . .
O2 O 0.1729(7) 0.6681(3) 0.3738(4) 0.0209(6) Uani 1 1 d . . .
O3 O 1.7695(7) 0.5947(3) 1.0733(3) 0.0161(6) Uani 1 1 d . . .
H3 H 1.8072 0.6393 1.1746 0.019 Uiso 1 1 d . . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
C1 0.0122(17) 0.019(2) 0.0134(17) -0.0004(15) 0.0008(15) -0.0018(14)
C2 0.0129(17) 0.0154(19) 0.0170(18) -0.0002(15) 0.0045(15) -0.0041(15)
Cd1 0.0122(2) 0.0149(3) 0.0204(2) 0.00309(10) 0.00085(14) 0.00015(9)
O1 0.0176(14) 0.0210(17) 0.0174(14) -0.0043(11) -0.0006(12) 0.0005(9)
O2 0.0232(14) 0.0135(15) 0.0226(14) 0.0027(14) -0.0065(12) 0.0019(11)
O3 0.0152(13) 0.0195(15) 0.0124(14) -0.0026(11) -0.0007(12) 0.0007(9)

_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 O1 1.255(5) . ?
C1 C2 1.460(5) 3_666 ?
C1 C2 1.465(5) . ?
C2 O2 1.252(5) . ?
C2 C1 1.460(5) 3_666 ?
Cd1 O3 2.207(2) . ?
Cd1 O3 2.231(3) 1_455 ?
Cd1 O2 2.238(3) 4_676 ?
Cd1 O3 2.277(4) 3_867 ?
Cd1 O1 2.403(3) . ?
Cd1 O1 2.532(3) 1_655 ?
Cd1 Cd1 3.3730(5) 3_767 ?
Cd1 Cd1 3.4144(5) 3_867 ?
O1 Cd1 2.532(3) 1_455 ?
O2 Cd1 2.238(3) 4_475 ?
O3 Cd1 2.231(3) 1_655 ?
O3 Cd1 2.277(4) 3_867 ?
O3 H3 0.9766 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 C1 C2 135.3(3) . 3_666 ?
O1 C1 C2 134.5(4) . . ?
C2 C1 C2 90.1(3) 3_666 . ?
O2 C2 C1 135.1(4) . 3_666 ?
O2 C2 C1 135.0(4) . . ?
C1 C2 C1 89.9(3) 3_666 . ?
O3 Cd1 O3 107.52(11) . 1_455 ?
O3 Cd1 O2 105.18(12) . 4_676 ?
O3 Cd1 O2 101.78(12) 1_455 4_676 ?
O3 Cd1 O3 80.81(12) . 3_867 ?
O3 Cd1 O3 83.12(11) 1_455 3_867 ?
O2 Cd1 O3 170.43(11) 4_676 3_867 ?
O3 Cd1 O1 168.24(10) . . ?
O3 Cd1 O1 80.37(10) 1_455 . ?
O2 Cd1 O1 81.09(9) 4_676 . ?
O3 Cd1 O1 91.75(8) 3_867 . ?
O3 Cd1 O1 78.00(9) . 1_655 ?
O3 Cd1 O1 170.04(10) 1_455 1_655 ?
O2 Cd1 O1 84.34(9) 4_676 1_655 ?
O3 Cd1 O1 89.73(8) 3_867 1_655 ?
O1 Cd1 O1 92.97(11) . 1_655 ?
O3 Cd1 Cd1 95.24(9) . 3_767 ?
O3 Cd1 Cd1 42.08(9) 1_455 3_767 ?
O2 Cd1 Cd1 143.19(8) 4_676 3_767 ?
O3 Cd1 Cd1 41.04(6) 3_867 3_767 ?
O1 Cd1 Cd1 84.83(7) . 3_767 ?
O1 Cd1 Cd1 130.41(5) 1_655 3_767 ?
O3 Cd1 Cd1 41.17(9) . 3_867 ?
O3 Cd1 Cd1 96.59(8) 1_455 3_867 ?
O2 Cd1 Cd1 145.77(7) 4_676 3_867 ?
O3 Cd1 Cd1 39.65(6) 3_867 3_867 ?
O1 Cd1 Cd1 130.78(6) . 3_867 ?
O1 Cd1 Cd1 82.10(6) 1_655 3_867 ?
Cd1 Cd1 Cd1 63.649(11) 3_767 3_867 ?
C1 O1 Cd1 130.6(2) . . ?
C1 O1 Cd1 118.2(2) . 1_455 ?
Cd1 O1 Cd1 92.97(11) . 1_455 ?
C2 O2 Cd1 131.1(3) . 4_475 ?
Cd1 O3 Cd1 107.52(11) . 1_655 ?
Cd1 O3 Cd1 99.19(12) . 3_867 ?
Cd1 O3 Cd1 96.88(11) 1_655 3_867 ?
Cd1 O3 H3 116.0 . . ?
Cd1 O3 H3 116.7 1_655 . ?
Cd1 O3 H3 117.6 3_867 . ?

_diffrn_measured_fraction_theta_max 0.983
_diffrn_reflns_theta_full        26.00
_diffrn_measured_fraction_theta_full 0.983
_refine_diff_density_max         1.038
_refine_diff_density_min         -1.237
_refine_diff_density_rms         0.237


