# 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
_journal_volume                  ?
_journal_page_first              ?
_journal_year                    ?

_publ_contact_author_name        'Yuan-Gen Yao'
_publ_contact_author_email       YYG@FJIRSM.AC.CN

_publ_section_title              
;
Novel (3,6)-connected network and (4,6)-connected framework
in two Copper(II) and Cadmium(II) complexes of flexible
(2S,3S,4R,5R)-tetrahydrofurantetracarboxylic acid:
synthesis, structure, thermostability, and luminescence studies
;
loop_
_publ_author_name
'Lei Zhang.'
'Jian Zhang.'
'Zhao-Ji Li.'
'Ye-Yan Qin.'
'Qi-Pu Lin.'
'Yuan-Gen Yao.'

# Attachment '1.CIF'

data_a
_database_code_depnum_ccdc_archive 'CCDC 691748'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C20 H14 Cu2 N2 O10'
_chemical_formula_weight         569.41

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'
Cu Cu 0.3201 1.2651 '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                   7.2243(8)
_cell_length_b                   12.1310(12)
_cell_length_c                   22.654(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 96.066(6)
_cell_angle_gamma                90.00
_cell_volume                     1974.2(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    4193
_cell_measurement_theta_min      2.4686
_cell_measurement_theta_max      27.4835

_exptl_crystal_description       Prism
_exptl_crystal_colour            Green
_exptl_crystal_size_max          0.2000
_exptl_crystal_size_mid          0.1500
_exptl_crystal_size_min          0.1000
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.916
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1144
_exptl_absorpt_coefficient_mu    2.221
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_max  0.801
_exptl_absorpt_correction_T_min  0.677
_exptl_absorpt_process_details   crystalclear

_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  'Bruker P4'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean none
_diffrn_standards_number         none
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  none
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            15100
_diffrn_reflns_av_R_equivalents  0.0461
_diffrn_reflns_av_sigmaI/netI    0.0464
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_theta_min         2.47
_diffrn_reflns_theta_max         27.48
_reflns_number_total             4541
_reflns_number_gt                3870
_reflns_threshold_expression     >2sigma(I)

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

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0825P)²+3.9910P] 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         4541
_refine_ls_number_parameters     317
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0680
_refine_ls_R_factor_gt           0.0549
_refine_ls_wR_factor_ref         0.1490
_refine_ls_wR_factor_gt          0.1385
_refine_ls_goodness_of_fit_ref   1.016
_refine_ls_restrained_S_all      1.016
_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
Cu1 Cu -0.68309(7) -0.33722(4) 0.27928(2) 0.02064(16) Uani 1 1 d . . .
Cu2 Cu -0.23772(7) -0.35202(4) 0.35969(2) 0.01961(16) Uani 1 1 d . . .
C1 C -0.9158(6) -0.1286(3) 0.27755(18) 0.0190(8) Uani 1 1 d . . .
H1A H -0.9958 -0.1162 0.2404 0.023 Uiso 1 1 calc R . .
C2 C -0.9015(5) -0.0211(3) 0.31359(18) 0.0197(8) Uani 1 1 d . . .
H2A H -0.9268 -0.0397 0.3541 0.024 Uiso 1 1 calc R . .
C3 C -0.6942(6) 0.0122(3) 0.31667(19) 0.0203(8) Uani 1 1 d . . .
H3A H -0.6493 0.0439 0.3554 0.024 Uiso 1 1 calc R . .
C4 C -0.5991(6) -0.0987(3) 0.30609(18) 0.0198(8) Uani 1 1 d . . .
H4A H -0.4866 -0.0833 0.2868 0.024 Uiso 1 1 calc R . .
C5 C -0.9946(5) -0.2227(3) 0.31108(18) 0.0192(8) Uani 1 1 d . . .
C6 C -1.0373(6) 0.0696(4) 0.2918(2) 0.0252(9) Uani 1 1 d . . .
C7 C -0.6500(5) 0.0862(3) 0.26577(18) 0.0183(8) Uani 1 1 d . . .
C8 C -0.5432(6) -0.1714(3) 0.36065(19) 0.0218(8) Uani 1 1 d . . .
C9 C -0.1222(8) -0.2100(5) 0.4665(3) 0.0438(13) Uani 1 1 d . . .
H9A H -0.1038 -0.1523 0.4407 0.053 Uiso 1 1 calc R . .
C10 C -0.0923(10) -0.1923(6) 0.5282(3) 0.0604(18) Uani 1 1 d . . .
H10A H -0.0546 -0.1233 0.5427 0.072 Uiso 1 1 calc R . .
C11 C -0.1184(9) -0.2756(6) 0.5666(3) 0.0565(18) Uani 1 1 d . . .
H11A H -0.0988 -0.2635 0.6073 0.068 Uiso 1 1 calc R . .
C12 C -0.1740(7) -0.3782(5) 0.5451(2) 0.0408(13) Uani 1 1 d . . .
C13 C -0.2054(8) -0.4729(6) 0.5811(2) 0.0527(17) Uani 1 1 d . . .
H13A H -0.1838 -0.4672 0.6221 0.063 Uiso 1 1 calc R . .
C14 C -0.2649(7) -0.5691(6) 0.5568(3) 0.0486(16) Uani 1 1 d . . .
H14A H -0.2866 -0.6279 0.5815 0.058 Uiso 1 1 calc R . .
C15 C -0.2959(7) -0.5835(5) 0.4939(2) 0.0376(12) Uani 1 1 d . . .
C16 C -0.3548(8) -0.6817(5) 0.4657(3) 0.0468(15) Uani 1 1 d . . .
H16A H -0.3789 -0.7433 0.4881 0.056 Uiso 1 1 calc R . .
C17 C -0.3768(9) -0.6867(5) 0.4049(3) 0.0493(15) Uani 1 1 d . . .
H17A H -0.4158 -0.7517 0.3857 0.059 Uiso 1 1 calc R . .
C18 C -0.3401(7) -0.5933(4) 0.3723(2) 0.0353(11) Uani 1 1 d . . .
H18A H -0.3531 -0.5978 0.3311 0.042 Uiso 1 1 calc R . .
C19 C -0.2638(6) -0.4933(4) 0.4576(2) 0.0288(10) Uani 1 1 d . . .
C20 C -0.2017(6) -0.3900(4) 0.4833(2) 0.0298(10) Uani 1 1 d . . .
O1 O -0.8977(4) -0.3082(2) 0.32393(13) 0.0219(6) Uani 1 1 d . . .
O2 O -1.1540(4) -0.2116(2) 0.32691(15) 0.0254(7) Uani 1 1 d . . .
O3 O -1.1795(4) 0.0394(3) 0.25724(17) 0.0329(8) Uani 1 1 d . . .
O4 O -1.0026(5) 0.1651(3) 0.30805(16) 0.0365(8) Uani 1 1 d . . .
O5 O -0.7495(4) 0.0737(3) 0.21707(13) 0.0249(6) Uani 1 1 d . . .
O6 O -0.5073(4) 0.1466(3) 0.27463(14) 0.0255(7) Uani 1 1 d . . .
O7 O -0.5117(6) -0.1302(3) 0.40984(17) 0.0478(11) Uani 1 1 d . . .
O8 O -0.5248(4) -0.2742(2) 0.34873(13) 0.0221(6) Uani 1 1 d . . .
O9 O -0.7292(4) -0.1545(2) 0.26378(13) 0.0193(6) Uani 1 1 d . . .
N1 N -0.1760(5) -0.3069(3) 0.44458(17) 0.0279(8) Uani 1 1 d . . .
N2 N -0.2875(5) -0.4983(3) 0.39761(17) 0.0258(8) Uani 1 1 d . . .
O1W O -0.342(3) 0.0428(11) 0.4849(9) 0.211(10) Uani 0.657(17) 1 d P A 1
O1W' O -0.247(3) 0.0480(16) 0.4066(11) 0.109(9) Uani 0.343(17) 1 d P A 2


_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
Cu1 O3 1.933(3) 2_345 ?
Cu1 O6 1.943(3) 2_445 ?
Cu1 O1 1.970(3) . ?
Cu1 O8 1.997(3) . ?
Cu1 O9 2.263(3) . ?
Cu2 O5 1.952(3) 2_445 ?
Cu2 O2 1.978(3) 1_655 ?
Cu2 N1 2.004(4) . ?
Cu2 N2 2.021(4) . ?
Cu2 O8 2.269(3) . ?
C1 O9 1.450(5) . ?
C1 C5 1.515(5) . ?
C1 C2 1.536(6) . ?
C1 H1A 0.9800 . ?
C2 C6 1.521(6) . ?
C2 C3 1.546(6) . ?
C2 H2A 0.9800 . ?
C3 C7 1.522(6) . ?
C3 C4 1.540(6) . ?
C3 H3A 0.9800 . ?
C4 O9 1.439(5) . ?
C4 C8 1.538(6) . ?
C4 H4A 0.9800 . ?
C5 O2 1.249(5) . ?
C5 O1 1.268(5) . ?
C6 O4 1.233(6) . ?
C6 O3 1.278(6) . ?
C7 O5 1.261(5) . ?
C7 O6 1.263(5) . ?
C8 O7 1.221(6) . ?
C8 O8 1.285(5) . ?
C9 N1 1.318(7) . ?
C9 C10 1.408(8) . ?
C9 H9A 0.9300 . ?
C10 C11 1.359(10) . ?
C10 H10A 0.9300 . ?
C11 C12 1.381(9) . ?
C11 H11A 0.9300 . ?
C12 C20 1.399(7) . ?
C12 C13 1.441(9) . ?
C13 C14 1.341(10) . ?
C13 H13A 0.9300 . ?
C14 C15 1.428(8) . ?
C14 H14A 0.9300 . ?
C15 C16 1.396(9) . ?
C15 C19 1.403(7) . ?
C16 C17 1.371(9) . ?
C16 H16A 0.9300 . ?
C17 C18 1.393(7) . ?
C17 H17A 0.9300 . ?
C18 N2 1.324(6) . ?
C18 H18A 0.9300 . ?
C19 N2 1.353(6) . ?
C19 C20 1.435(7) . ?
C20 N1 1.362(6) . ?
O2 Cu2 1.978(3) 1_455 ?
O3 Cu1 1.933(3) 2_355 ?
O5 Cu2 1.952(3) 2_455 ?
O6 Cu1 1.943(3) 2_455 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O3 Cu1 O6 91.04(14) 2_345 2_445 ?
O3 Cu1 O1 87.81(13) 2_345 . ?
O6 Cu1 O1 171.18(13) 2_445 . ?
O3 Cu1 O8 149.24(14) 2_345 . ?
O6 Cu1 O8 98.61(13) 2_445 . ?
O1 Cu1 O8 86.74(12) . . ?
O3 Cu1 O9 129.15(13) 2_345 . ?
O6 Cu1 O9 95.95(12) 2_445 . ?
O1 Cu1 O9 78.10(11) . . ?
O8 Cu1 O9 79.03(11) . . ?
O5 Cu2 O2 92.90(13) 2_445 1_655 ?
O5 Cu2 N1 164.97(15) 2_445 . ?
O2 Cu2 N1 94.54(15) 1_655 . ?
O5 Cu2 N2 88.83(14) 2_445 . ?
O2 Cu2 N2 172.36(14) 1_655 . ?
N1 Cu2 N2 82.16(16) . . ?
O5 Cu2 O8 97.94(12) 2_445 . ?
O2 Cu2 O8 85.00(11) 1_655 . ?
N1 Cu2 O8 95.71(13) . . ?
N2 Cu2 O8 102.14(13) . . ?
O9 C1 C5 110.6(3) . . ?
O9 C1 C2 106.7(3) . . ?
C5 C1 C2 112.4(3) . . ?
O9 C1 H1A 109.1 . . ?
C5 C1 H1A 109.1 . . ?
C2 C1 H1A 109.1 . . ?
C6 C2 C1 115.9(4) . . ?
C6 C2 C3 114.5(3) . . ?
C1 C2 C3 104.8(3) . . ?
C6 C2 H2A 107.1 . . ?
C1 C2 H2A 107.1 . . ?
C3 C2 H2A 107.1 . . ?
C7 C3 C4 105.3(3) . . ?
C7 C3 C2 113.6(3) . . ?
C4 C3 C2 102.2(3) . . ?
C7 C3 H3A 111.7 . . ?
C4 C3 H3A 111.7 . . ?
C2 C3 H3A 111.7 . . ?
O9 C4 C8 111.3(3) . . ?
O9 C4 C3 104.1(3) . . ?
C8 C4 C3 117.4(3) . . ?
O9 C4 H4A 107.9 . . ?
C8 C4 H4A 107.9 . . ?
C3 C4 H4A 107.9 . . ?
O2 C5 O1 121.7(4) . . ?
O2 C5 C1 118.0(4) . . ?
O1 C5 C1 120.3(3) . . ?
O4 C6 O3 125.2(4) . . ?
O4 C6 C2 118.6(4) . . ?
O3 C6 C2 116.2(4) . . ?
O5 C7 O6 126.1(4) . . ?
O5 C7 C3 116.5(4) . . ?
O6 C7 C3 117.0(4) . . ?
O7 C8 O8 125.2(4) . . ?
O7 C8 C4 120.4(4) . . ?
O8 C8 C4 114.3(4) . . ?
N1 C9 C10 121.2(6) . . ?
N1 C9 H9A 119.4 . . ?
C10 C9 H9A 119.4 . . ?
C11 C10 C9 120.3(6) . . ?
C11 C10 H10A 119.9 . . ?
C9 C10 H10A 119.9 . . ?
C10 C11 C12 120.0(5) . . ?
C10 C11 H11A 120.0 . . ?
C12 C11 H11A 120.0 . . ?
C11 C12 C20 116.8(6) . . ?
C11 C12 C13 125.2(5) . . ?
C20 C12 C13 118.0(6) . . ?
C14 C13 C12 121.6(5) . . ?
C14 C13 H13A 119.2 . . ?
C12 C13 H13A 119.2 . . ?
C13 C14 C15 121.7(5) . . ?
C13 C14 H14A 119.2 . . ?
C15 C14 H14A 119.2 . . ?
C16 C15 C19 117.2(5) . . ?
C16 C15 C14 124.7(5) . . ?
C19 C15 C14 118.1(6) . . ?
C17 C16 C15 119.7(5) . . ?
C17 C16 H16A 120.2 . . ?
C15 C16 H16A 120.2 . . ?
C16 C17 C18 119.2(6) . . ?
C16 C17 H17A 120.4 . . ?
C18 C17 H17A 120.4 . . ?
N2 C18 C17 122.7(5) . . ?
N2 C18 H18A 118.7 . . ?
C17 C18 H18A 118.7 . . ?
N2 C19 C15 122.9(5) . . ?
N2 C19 C20 116.6(4) . . ?
C15 C19 C20 120.5(5) . . ?
N1 C20 C12 123.6(5) . . ?
N1 C20 C19 116.3(4) . . ?
C12 C20 C19 120.1(5) . . ?
C5 O1 Cu1 118.3(3) . . ?
C5 O2 Cu2 110.1(3) . 1_455 ?
C6 O3 Cu1 112.6(3) . 2_355 ?
C7 O5 Cu2 133.9(3) . 2_455 ?
C7 O6 Cu1 125.3(3) . 2_455 ?
C8 O8 Cu1 118.3(3) . . ?
C8 O8 Cu2 119.6(3) . . ?
Cu1 O8 Cu2 111.56(13) . . ?
C4 O9 C1 108.1(3) . . ?
C4 O9 Cu1 106.4(2) . . ?
C1 O9 Cu1 107.7(2) . . ?
C9 N1 C20 118.1(5) . . ?
C9 N1 Cu2 129.2(4) . . ?
C20 N1 Cu2 112.6(3) . . ?
C18 N2 C19 118.3(4) . . ?
C18 N2 Cu2 129.5(3) . . ?
C19 N2 Cu2 112.2(3) . . ?

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        27.48
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         0.589
_refine_diff_density_min         -0.563
_refine_diff_density_rms         0.103

# Attachment '2.CIF'

data_a2
_database_code_depnum_ccdc_archive 'CCDC 723112'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C8 H10 Cd2 O12'
_chemical_formula_weight         522.98

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'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   'P 21/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                   6.4810(6)
_cell_length_b                   26.9381(16)
_cell_length_c                   8.3967(6)
_cell_angle_alpha                90.00
_cell_angle_beta                 120.004(5)
_cell_angle_gamma                90.00
_cell_volume                     1269.49(17)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    3430
_cell_measurement_theta_min      2.2680
_cell_measurement_theta_max      27.4797

_exptl_crystal_description       Prism
_exptl_crystal_colour            Colorless
_exptl_crystal_size_max          0.2000
_exptl_crystal_size_mid          0.2000
_exptl_crystal_size_min          0.2000
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.736
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1000
_exptl_absorpt_coefficient_mu    3.418
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_max  0.510
_exptl_absorpt_correction_T_min  0.505
_exptl_absorpt_process_details   crystalclear

_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  'Bruker P4'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean none
_diffrn_standards_number         none
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  none
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            8890
_diffrn_reflns_av_R_equivalents  0.0216
_diffrn_reflns_av_sigmaI/netI    0.0213
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_theta_min         2.90
_diffrn_reflns_theta_max         27.48
_reflns_number_total             2909
_reflns_number_gt                2684
_reflns_threshold_expression     >2sigma(I)

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

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0344P)²+2.7839P] 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         2909
_refine_ls_number_parameters     199
_refine_ls_number_restraints     9
_refine_ls_R_factor_all          0.0269
_refine_ls_R_factor_gt           0.0248
_refine_ls_wR_factor_ref         0.0652
_refine_ls_wR_factor_gt          0.0640
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_restrained_S_all      1.031
_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 0.1632(5) -0.13903(12) 0.8390(4) 0.0149(6) Uani 1 1 d . . .
H1A H 0.2784 -0.1191 0.8233 0.018 Uiso 1 1 calc R . .
C2 C -0.0832(5) -0.11516(11) 0.7298(4) 0.0154(6) Uani 1 1 d . . .
H2A H -0.2034 -0.1397 0.7149 0.018 Uiso 1 1 calc R . .
C3 C -0.0680(5) -0.07474(12) 0.8670(4) 0.0158(6) Uani 1 1 d . . .
H3A H -0.2275 -0.0640 0.8382 0.019 Uiso 1 1 calc R . .
C4 C 0.0513(5) -0.10526(11) 1.0444(4) 0.0149(6) Uani 1 1 d . . .
H4A H 0.1343 -0.0832 1.1507 0.018 Uiso 1 1 calc R . .
C5 C 0.1698(6) -0.19198(12) 0.7813(4) 0.0186(6) Uani 1 1 d . . .
C6 C -0.1489(6) -0.09487(12) 0.5408(4) 0.0195(6) Uani 1 1 d . . .
C7 C 0.0812(6) -0.03064(12) 0.8692(4) 0.0168(6) Uani 1 1 d . . .
C8 C -0.1339(6) -0.13659(12) 1.0634(4) 0.0176(6) Uani 1 1 d . . .
O1W O 0.6470(6) -0.22770(18) 1.2746(5) 0.0612(11) Uani 1 1 d D . .
H1WB H 0.7532 -0.2426 1.3647 0.073 Uiso 1 1 d RD . .
H1WA H 0.6990 -0.1999 1.2688 0.073 Uiso 1 1 d RD . .
O1 O 0.2213(4) -0.13649(9) 1.0290(3) 0.0156(4) Uani 1 1 d . . .
O2W O 0.3637(6) -0.16528(12) 1.4335(4) 0.0425(8) Uani 1 1 d D . .
H2WB H 0.2793 -0.1634 1.4818 0.064 Uiso 1 1 d RD . .
H2WA H 0.4109 -0.1369 1.4298 0.064 Uiso 1 1 d RD . .
O2 O 0.2069(5) -0.22740(10) 0.8883(4) 0.0281(6) Uani 1 1 d . . .
O3 O 0.1409(6) -0.19839(10) 0.6245(4) 0.0357(7) Uani 1 1 d . . .
O3W O -0.3736(5) 0.01773(10) 1.3722(4) 0.0295(6) Uani 1 1 d D . .
H3WB H -0.3184 0.0039 1.4739 0.044 Uiso 1 1 d RD . .
H3WA H -0.2939 0.0433 1.3857 0.044 Uiso 1 1 d RD . .
O4 O 0.0073(5) -0.08242(11) 0.5047(4) 0.0305(6) Uani 1 1 d . . .
O5 O -0.3685(5) -0.08998(10) 0.4269(3) 0.0272(6) Uani 1 1 d . . .
O6 O 0.3003(5) -0.02923(11) 0.9767(4) 0.0298(6) Uani 1 1 d . . .
O7 O -0.0234(5) 0.00310(9) 0.7532(4) 0.0258(5) Uani 1 1 d . . .
O8 O -0.2975(4) -0.11346(10) 1.0683(4) 0.0250(5) Uani 1 1 d . . .
O9 O -0.1163(5) -0.18318(10) 1.0683(4) 0.0280(6) Uani 1 1 d . . .
Cd1 Cd 0.25853(4) -0.215758(9) 1.18152(3) 0.01905(8) Uani 1 1 d . . .
Cd2 Cd -0.31702(4) -0.045269(9) 1.20955(3) 0.01838(8) 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 O1 1.446(3) . ?
C1 C5 1.514(4) . ?
C1 C2 1.529(4) . ?
C1 H1A 0.9800 . ?
C2 C6 1.524(4) . ?
C2 C3 1.553(4) . ?
C2 H2A 0.9800 . ?
C3 C7 1.526(4) . ?
C3 C4 1.530(4) . ?
C3 H3A 0.9800 . ?
C4 O1 1.443(3) . ?
C4 C8 1.539(4) . ?
C4 H4A 0.9800 . ?
C5 O3 1.246(4) . ?
C5 O2 1.249(4) . ?
C6 O4 1.240(4) . ?
C6 O5 1.263(4) . ?
C7 O6 1.246(4) . ?
C7 O7 1.254(4) . ?
C8 O8 1.249(4) . ?
C8 O9 1.259(4) . ?
O1W Cd1 2.255(4) . ?
O1W H1WB 0.8287 . ?
O1W H1WA 0.8317 . ?
O1 Cd1 2.439(2) . ?
O2W Cd1 2.313(3) . ?
O2W H2WB 0.8293 . ?
O2W H2WA 0.8290 . ?
O2 Cd1 2.334(3) . ?
O2 Cd1 2.460(3) 4 ?
O3 Cd1 2.407(3) 4 ?
O3W Cd2 2.320(3) . ?
O3W H3WB 0.8310 . ?
O3W H3WA 0.8352 . ?
O4 Cd2 2.520(3) 1_554 ?
O5 Cd2 2.345(3) 1_554 ?
O6 Cd2 2.304(3) 1_655 ?
O6 Cd2 2.580(3) 3_557 ?
O7 Cd2 2.359(3) 3_557 ?
O8 Cd2 2.224(3) . ?
O9 Cd1 2.295(3) . ?
Cd1 O3 2.407(3) 4_556 ?
Cd1 O2 2.460(3) 4_556 ?
Cd2 O6 2.304(3) 1_455 ?
Cd2 O5 2.345(3) 1_556 ?
Cd2 O7 2.359(3) 3_557 ?
Cd2 O4 2.520(3) 1_556 ?
Cd2 O6 2.580(3) 3_557 ?

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 C5 111.4(2) . . ?
O1 C1 C2 105.1(2) . . ?
C5 C1 C2 113.1(3) . . ?
O1 C1 H1A 109.1 . . ?
C5 C1 H1A 109.1 . . ?
C2 C1 H1A 109.1 . . ?
C6 C2 C1 116.1(3) . . ?
C6 C2 C3 113.7(3) . . ?
C1 C2 C3 101.0(2) . . ?
C6 C2 H2A 108.6 . . ?
C1 C2 H2A 108.6 . . ?
C3 C2 H2A 108.6 . . ?
C7 C3 C4 113.5(3) . . ?
C7 C3 C2 111.1(2) . . ?
C4 C3 C2 99.2(2) . . ?
C7 C3 H3A 110.9 . . ?
C4 C3 H3A 110.9 . . ?
C2 C3 H3A 110.9 . . ?
O1 C4 C3 105.2(2) . . ?
O1 C4 C8 111.1(2) . . ?
C3 C4 C8 110.8(3) . . ?
O1 C4 H4A 109.9 . . ?
C3 C4 H4A 109.9 . . ?
C8 C4 H4A 109.9 . . ?
O3 C5 O2 121.9(3) . . ?
O3 C5 C1 117.1(3) . . ?
O2 C5 C1 121.0(3) . . ?
O4 C6 O5 122.4(3) . . ?
O4 C6 C2 121.0(3) . . ?
O5 C6 C2 116.6(3) . . ?
O6 C7 O7 121.2(3) . . ?
O6 C7 C3 121.2(3) . . ?
O7 C7 C3 117.5(3) . . ?
O8 C8 O9 124.1(3) . . ?
O8 C8 C4 116.7(3) . . ?
O9 C8 C4 119.2(3) . . ?
Cd1 O1W H1WB 131.2 . . ?
Cd1 O1W H1WA 105.5 . . ?
H1WB O1W H1WA 108.3 . . ?
C4 O1 C1 109.7(2) . . ?
C4 O1 Cd1 110.03(17) . . ?
C1 O1 Cd1 116.16(17) . . ?
Cd1 O2W H2WB 121.3 . . ?
Cd1 O2W H2WA 116.9 . . ?
H2WB O2W H2WA 108.0 . . ?
C5 O2 Cd1 122.1(2) . . ?
C5 O2 Cd1 90.7(2) . 4 ?
Cd1 O2 Cd1 146.07(12) . 4 ?
C5 O3 Cd1 93.3(2) . 4 ?
Cd2 O3W H3WB 99.3 . . ?
Cd2 O3W H3WA 114.5 . . ?
H3WB O3W H3WA 108.2 . . ?
C6 O4 Cd2 88.1(2) . 1_554 ?
C6 O5 Cd2 95.6(2) . 1_554 ?
C7 O6 Cd2 164.3(2) . 1_655 ?
C7 O6 Cd2 87.8(2) . 3_557 ?
Cd2 O6 Cd2 107.86(10) 1_655 3_557 ?
C7 O7 Cd2 98.0(2) . 3_557 ?
C8 O8 Cd2 134.9(2) . . ?
C8 O9 Cd1 117.0(2) . . ?
O1W Cd1 O9 164.87(13) . . ?
O1W Cd1 O2W 89.98(14) . . ?
O9 Cd1 O2W 85.46(12) . . ?
O1W Cd1 O2 83.84(12) . . ?
O9 Cd1 O2 92.89(10) . . ?
O2W Cd1 O2 149.92(10) . . ?
O1W Cd1 O3 96.85(15) . 4_556 ?
O9 Cd1 O3 96.94(11) . 4_556 ?
O2W Cd1 O3 131.77(10) . 4_556 ?
O2 Cd1 O3 78.27(9) . 4_556 ?
O1W Cd1 O1 96.14(12) . . ?
O9 Cd1 O1 68.98(8) . . ?
O2W Cd1 O1 82.66(10) . . ?
O2 Cd1 O1 68.86(8) . . ?
O3 Cd1 O1 142.96(8) 4_556 . ?
O1W Cd1 O2 100.89(13) . 4_556 ?
O9 Cd1 O2 92.35(10) . 4_556 ?
O2W Cd1 O2 78.59(10) . 4_556 ?
O2 Cd1 O2 131.49(5) . 4_556 ?
O3 Cd1 O2 53.22(8) 4_556 4_556 ?
O1 Cd1 O2 154.54(8) . 4_556 ?
O8 Cd2 O6 91.51(10) . 1_455 ?
O8 Cd2 O3W 170.42(10) . . ?
O6 Cd2 O3W 86.71(10) 1_455 . ?
O8 Cd2 O5 93.37(10) . 1_556 ?
O6 Cd2 O5 104.19(9) 1_455 1_556 ?
O3W Cd2 O5 77.97(10) . 1_556 ?
O8 Cd2 O7 99.78(9) . 3_557 ?
O6 Cd2 O7 124.09(9) 1_455 3_557 ?
O3W Cd2 O7 88.98(10) . 3_557 ?
O5 Cd2 O7 129.16(9) 1_556 3_557 ?
O8 Cd2 O4 87.39(10) . 1_556 ?
O6 Cd2 O4 157.42(9) 1_455 1_556 ?
O3W Cd2 O4 90.64(10) . 1_556 ?
O5 Cd2 O4 53.43(9) 1_556 1_556 ?
O7 Cd2 O4 78.22(9) 3_557 1_556 ?
O8 Cd2 O6 106.77(10) . 3_557 ?
O6 Cd2 O6 72.14(10) 1_455 3_557 ?
O3W Cd2 O6 81.65(10) . 3_557 ?
O5 Cd2 O6 159.49(10) 1_556 3_557 ?
O7 Cd2 O6 52.11(8) 3_557 3_557 ?
O4 Cd2 O6 129.63(9) 1_556 3_557 ?

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
O1 C1 C2 C6 157.4(3) . . . . ?
C5 C1 C2 C6 -80.9(3) . . . . ?
O1 C1 C2 C3 33.9(3) . . . . ?
C5 C1 C2 C3 155.6(2) . . . . ?
C6 C2 C3 C7 -48.5(4) . . . . ?
C1 C2 C3 C7 76.5(3) . . . . ?
C6 C2 C3 C4 -168.1(3) . . . . ?
C1 C2 C3 C4 -43.1(3) . . . . ?
C7 C3 C4 O1 -79.8(3) . . . . ?
C2 C3 C4 O1 38.1(3) . . . . ?
C7 C3 C4 C8 160.1(3) . . . . ?
C2 C3 C4 C8 -82.0(3) . . . . ?
O1 C1 C5 O3 -174.5(3) . . . . ?
C2 C1 C5 O3 67.4(4) . . . . ?
O1 C1 C5 O2 4.3(4) . . . . ?
C2 C1 C5 O2 -113.8(3) . . . . ?
C1 C2 C6 O4 -24.4(5) . . . . ?
C3 C2 C6 O4 92.1(4) . . . . ?
C1 C2 C6 O5 157.9(3) . . . . ?
C3 C2 C6 O5 -85.6(4) . . . . ?
C4 C3 C7 O6 20.8(4) . . . . ?
C2 C3 C7 O6 -90.0(4) . . . . ?
C4 C3 C7 O7 -162.3(3) . . . . ?
C2 C3 C7 O7 87.0(3) . . . . ?
O1 C4 C8 O8 -176.4(3) . . . . ?
C3 C4 C8 O8 -59.9(4) . . . . ?
O1 C4 C8 O9 1.8(4) . . . . ?
C3 C4 C8 O9 118.4(3) . . . . ?
C3 C4 O1 C1 -18.1(3) . . . . ?
C8 C4 O1 C1 101.8(3) . . . . ?
C3 C4 O1 Cd1 -147.08(18) . . . . ?
C8 C4 O1 Cd1 -27.1(3) . . . . ?
C5 C1 O1 C4 -133.2(3) . . . . ?
C2 C1 O1 C4 -10.4(3) . . . . ?
C5 C1 O1 Cd1 -7.7(3) . . . . ?
C2 C1 O1 Cd1 115.1(2) . . . . ?
O3 C5 O2 Cd1 -179.6(3) . . . . ?
C1 C5 O2 Cd1 1.7(4) . . . . ?
O3 C5 O2 Cd1 9.6(4) . . . 4 ?
C1 C5 O2 Cd1 -169.1(3) . . . 4 ?
O2 C5 O3 Cd1 -9.9(4) . . . 4 ?
C1 C5 O3 Cd1 168.9(2) . . . 4 ?
O5 C6 O4 Cd2 7.1(3) . . . 1_554 ?
C2 C6 O4 Cd2 -170.4(3) . . . 1_554 ?
O4 C6 O5 Cd2 -7.7(4) . . . 1_554 ?
C2 C6 O5 Cd2 170.0(2) . . . 1_554 ?
O7 C7 O6 Cd2 173.2(8) . . . 1_655 ?
C3 C7 O6 Cd2 -10.0(11) . . . 1_655 ?
O7 C7 O6 Cd2 -8.7(3) . . . 3_557 ?
C3 C7 O6 Cd2 168.1(3) . . . 3_557 ?
O6 C7 O7 Cd2 9.6(4) . . . 3_557 ?
C3 C7 O7 Cd2 -167.3(2) . . . 3_557 ?
O9 C8 O8 Cd2 138.4(3) . . . . ?
C4 C8 O8 Cd2 -43.5(4) . . . . ?
O8 C8 O9 Cd1 -154.0(3) . . . . ?
C4 C8 O9 Cd1 27.9(4) . . . . ?
C8 O9 Cd1 O1W -20.3(6) . . . . ?
C8 O9 Cd1 O2W 52.5(3) . . . . ?
C8 O9 Cd1 O2 -97.4(3) . . . . ?
C8 O9 Cd1 O3 -175.9(2) . . . 4_556 ?
C8 O9 Cd1 O1 -31.3(2) . . . . ?
C8 O9 Cd1 O2 130.9(3) . . . 4_556 ?
C5 O2 Cd1 O1W -103.4(3) . . . . ?
Cd1 O2 Cd1 O1W 60.0(3) 4 . . . ?
C5 O2 Cd1 O9 61.8(3) . . . . ?
Cd1 O2 Cd1 O9 -134.8(2) 4 . . . ?
C5 O2 Cd1 O2W -24.1(4) . . . . ?
Cd1 O2 Cd1 O2W 139.2(2) 4 . . . ?
C5 O2 Cd1 O3 158.3(3) . . . 4_556 ?
Cd1 O2 Cd1 O3 -38.4(2) 4 . . 4_556 ?
C5 O2 Cd1 O1 -4.3(3) . . . . ?
Cd1 O2 Cd1 O1 159.0(3) 4 . . . ?
C5 O2 Cd1 O2 157.52(19) . . . 4_556 ?
Cd1 O2 Cd1 O2 -39.1(4) 4 . . 4_556 ?
C4 O1 Cd1 O1W -147.3(2) . . . . ?
C1 O1 Cd1 O1W 87.3(2) . . . . ?
C4 O1 Cd1 O9 29.85(18) . . . . ?
C1 O1 Cd1 O9 -95.5(2) . . . . ?
C4 O1 Cd1 O2W -58.08(19) . . . . ?
C1 O1 Cd1 O2W 176.5(2) . . . . ?
C4 O1 Cd1 O2 131.8(2) . . . . ?
C1 O1 Cd1 O2 6.37(19) . . . . ?
C4 O1 Cd1 O3 102.7(2) . . . 4_556 ?
C1 O1 Cd1 O3 -22.7(3) . . . 4_556 ?
C4 O1 Cd1 O2 -15.4(3) . . . 4_556 ?
C1 O1 Cd1 O2 -140.8(2) . . . 4_556 ?
C8 O8 Cd2 O6 150.8(3) . . . 1_455 ?
C8 O8 Cd2 O3W -130.1(5) . . . . ?
C8 O8 Cd2 O5 -104.9(3) . . . 1_556 ?
C8 O8 Cd2 O7 25.8(3) . . . 3_557 ?
C8 O8 Cd2 O4 -51.7(3) . . . 1_556 ?
C8 O8 Cd2 O6 79.0(3) . . . 3_557 ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O1W H1WB O9 0.83 2.49 3.227(5) 149.2 4_656
O1W H1WB O3 0.83 2.65 3.177(5) 123.1 1_656
O1W H1WA O9 0.83 2.55 3.074(5) 122.5 1_655
O2W H2WB O3 0.83 2.05 2.786(4) 147.7 1_556
O2W H2WA O5 0.83 1.92 2.689(4) 154.1 1_656
O3W H3WB O7 0.83 2.16 2.877(4) 144.3 1_556
O3W H3WA O4 0.84 1.92 2.699(4) 154.4 3_557

_diffrn_measured_fraction_theta_max 0.965
_diffrn_reflns_theta_full        27.48
_diffrn_measured_fraction_theta_full 0.965
_refine_diff_density_max         0.572
_refine_diff_density_min         -0.612
_refine_diff_density_rms         0.107



