# 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        'Andrew Burrows'
_publ_contact_author_email       A.D.BURROWS@BATH.AC.UK

_publ_section_title              
;
Synthesis and characterisation of metal-organic
frameworks containing bis(diketonate) linkers
;
loop_
_publ_author_name
'Andrew Burrows'
'Kevin Cassar'
'Mary Mahon'
'S P Rigby'
'John E Warren'

# Attachment 'B808350A-rev.cif'

data_compound_1_bath94
_database_code_depnum_ccdc_archive 'CCDC 244503'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C14.70 H22.10 Cl1.95 N1.35 O5.35 Zn'
_chemical_formula_weight         437.83

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Orthorhombic
_symmetry_space_group_name_H-M   Pbca

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

_cell_length_a                   13.2930(4)
_cell_length_b                   16.1758(5)
_cell_length_c                   18.5027(6)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     3978.5(2)
_cell_formula_units_Z            8
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    4794
_cell_measurement_theta_min      2.26
_cell_measurement_theta_max      29.36

_exptl_crystal_description       Tabloid
_exptl_crystal_colour            Colourless
_exptl_crystal_size_max          0.06
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.03
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.462
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1806
_exptl_absorpt_coefficient_mu    1.521
_exptl_absorpt_correction_type   SADABS
_exptl_absorpt_correction_T_min  0.8812
_exptl_absorpt_correction_T_max  0.9021
_exptl_absorpt_process_details   
;
?
;

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.6934
_diffrn_radiation_type           Synchrotron
_diffrn_radiation_source         'Daresbury SRS station 9.8'
_diffrn_radiation_monochromator  'Silicon 111'
_diffrn_measurement_device_type  'Bruker SMART CCD diffractometer'
_diffrn_measurement_method       'ω rotation with narrow frames'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            21702
_diffrn_reflns_av_R_equivalents  0.0353
_diffrn_reflns_av_sigmaI/netI    0.0386
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_theta_min         2.21
_diffrn_reflns_theta_max         29.67
_reflns_number_total             6001
_reflns_number_gt                4444
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'local programs'
_computing_data_reduction        'Bruker SAINT v7.06a'
_computing_structure_solution    'Bruker SHELXTL'
_computing_structure_refinement  'Sir 92'
_computing_molecular_graphics    'ORTEX (P.McArdle, 1995)'
_computing_publication_material  'SHELXL-97/2 (Sheldrick,1997)'

_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.

Disordered DMF was constrained to being flat, and the ADPs
therein were also refined subjects to restraints in the final
least squares cycles.
;

_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)+(0.0566P)²+4.3752P] 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         6001
_refine_ls_number_parameters     268
_refine_ls_number_restraints     19
_refine_ls_R_factor_all          0.0656
_refine_ls_R_factor_gt           0.0471
_refine_ls_wR_factor_ref         0.1321
_refine_ls_wR_factor_gt          0.1240
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_restrained_S_all      1.043
_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
Zn1 Zn 0.77788(2) 0.229866(14) 0.396329(15) 0.02816(10) Uani 1 1 d . . .
Cl1 Cl 0.60697(14) 0.23361(14) 0.57627(10) 0.0592(5) Uani 0.65 1 d P A 1
Cl2 Cl 0.63251(13) 0.24628(15) 0.73007(8) 0.0801(5) Uani 0.65 1 d P A 1
Cl3 Cl 0.5829(2) 0.38972(11) 0.64637(16) 0.1108(8) Uani 0.65 1 d P A 1
O1 O 0.85022(14) 0.31609(9) 0.33714(9) 0.0317(4) Uani 1 1 d . . .
O2 O 0.66041(15) 0.30405(10) 0.39983(10) 0.0345(4) Uani 1 1 d . . .
O3 O 0.78749(15) 0.63863(9) 0.45382(10) 0.0344(4) Uani 1 1 d . . .
O4 O 0.68213(17) 0.64648(9) 0.32408(10) 0.0394(5) Uani 1 1 d . . .
O5 O 0.86527(16) 0.26355(12) 0.48284(11) 0.0401(4) Uani 1 1 d . . .
O6 O 0.6710(14) 0.4413(8) 0.6305(8) 0.138(5) Uani 0.35 1 d P B 2
N1 N 0.9052(2) 0.26096(16) 0.60141(12) 0.0396(5) Uani 1 1 d . . .
N2 N 0.6147(12) 0.3074(9) 0.6424(6) 0.087(3) Uani 0.35 1 d PDU B 2
C1 C 0.9170(3) 0.44751(16) 0.31406(19) 0.0463(7) Uani 1 1 d . . .
H1A H 0.9717 0.4127 0.2958 0.069 Uiso 1 1 calc R . .
H1B H 0.9426 0.4834 0.3526 0.069 Uiso 1 1 calc R . .
H1C H 0.8905 0.4816 0.2746 0.069 Uiso 1 1 calc R . .
C2 C 0.8340(2) 0.39337(12) 0.34364(12) 0.0284(5) Uani 1 1 d . . .
C3 C 0.7485(2) 0.42988(13) 0.37441(13) 0.0278(5) Uani 1 1 d . . .
C4 C 0.6666(2) 0.38334(13) 0.39960(14) 0.0319(5) Uani 1 1 d . . .
C5 C 0.5740(2) 0.42660(17) 0.4281(2) 0.0488(8) Uani 1 1 d . . .
H5A H 0.5315 0.3867 0.4538 0.073 Uiso 1 1 calc R . .
H5B H 0.5362 0.4504 0.3877 0.073 Uiso 1 1 calc R . .
H5C H 0.5942 0.4707 0.4614 0.073 Uiso 1 1 calc R . .
C6 C 0.8331(3) 0.50887(15) 0.49988(16) 0.0430(7) Uani 1 1 d . . .
H6A H 0.8685 0.5447 0.5342 0.064 Uiso 1 1 calc R . .
H6B H 0.8809 0.4703 0.4779 0.064 Uiso 1 1 calc R . .
H6C H 0.7808 0.4777 0.5254 0.064 Uiso 1 1 calc R . .
C7 C 0.7854(2) 0.56095(13) 0.44182(14) 0.0295(5) Uani 1 1 d . . .
C8 C 0.7435(2) 0.52280(12) 0.38009(14) 0.0285(5) Uani 1 1 d . . .
C9 C 0.6969(2) 0.56837(13) 0.32468(14) 0.0344(6) Uani 1 1 d . . .
C10 C 0.6594(3) 0.52500(16) 0.25774(18) 0.0543(9) Uani 1 1 d . . .
H10A H 0.5911 0.5440 0.2466 0.082 Uiso 1 1 calc R . .
H10B H 0.6587 0.4652 0.2661 0.082 Uiso 1 1 calc R . .
H10C H 0.7040 0.5377 0.2171 0.082 Uiso 1 1 calc R . .
C11 C 0.8596(2) 0.23238(17) 0.54384(15) 0.0381(6) Uani 1 1 d . . .
H11 H 0.8193 0.1843 0.5493 0.046 Uiso 1 1 calc R . .
C12 C 0.9700(3) 0.33318(19) 0.59754(17) 0.0449(7) Uani 1 1 d . . .
H12A H 0.9869 0.3445 0.5469 0.067 Uiso 1 1 calc R . .
H12B H 1.0319 0.3227 0.6249 0.067 Uiso 1 1 calc R . .
H12C H 0.9351 0.3810 0.6182 0.067 Uiso 1 1 calc R . .
C13 C 0.8946(3) 0.2224(2) 0.67180(17) 0.0579(9) Uani 1 1 d . . .
H13A H 0.8510 0.1738 0.6677 0.087 Uiso 1 1 calc R . .
H13B H 0.8647 0.2620 0.7057 0.087 Uiso 1 1 calc R . .
H13C H 0.9609 0.2054 0.6895 0.087 Uiso 1 1 calc R . .
C14 C 0.5650(4) 0.2812(3) 0.6556(3) 0.0432(11) Uani 0.65 1 d P A 1
H14 H 0.4919 0.2692 0.6627 0.052 Uiso 0.65 1 calc PR A 1
C15 C 0.6567(14) 0.3713(11) 0.6046(7) 0.088(3) Uani 0.35 1 d PDU B 2
H15 H 0.6761 0.3617 0.5559 0.106 Uiso 0.35 1 calc PR B 2
C16 C 0.6051(11) 0.3157(9) 0.7170(7) 0.078(3) Uani 0.35 1 d PDU B 2
H16A H 0.5792 0.2640 0.7375 0.118 Uiso 0.35 1 calc PR B 2
H16B H 0.5584 0.3609 0.7278 0.118 Uiso 0.35 1 calc PR B 2
H16C H 0.6711 0.3280 0.7381 0.118 Uiso 0.35 1 calc PR B 2
C17 C 0.6055(13) 0.2270(10) 0.6016(8) 0.057(4) Uani 0.35 1 d PDU B 2
H17A H 0.5786 0.1843 0.6338 0.086 Uiso 0.35 1 calc PR B 2
H17B H 0.6720 0.2101 0.5841 0.086 Uiso 0.35 1 calc PR B 2
H17C H 0.5601 0.2344 0.5604 0.086 Uiso 0.35 1 calc PR B 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
Zn1 O2 1.9705(19) . ?
Zn1 O4 1.9721(17) 7_755 ?
Zn1 O3 2.0160(17) 7_755 ?
Zn1 O1 2.0172(16) . ?
Zn1 O5 2.052(2) . ?
Cl1 C14 1.749(5) . ?
Cl2 C14 1.739(6) . ?
Cl3 C14 1.779(6) . ?
O1 C2 1.274(2) . ?
O2 C4 1.285(2) . ?
O3 C7 1.276(2) . ?
O3 Zn1 2.0160(17) 7_765 ?
O4 C9 1.279(3) . ?
O4 Zn1 1.9721(17) 7_765 ?
O5 C11 1.238(3) . ?
O6 C15 1.244(19) . ?
N1 C11 1.310(4) . ?
N1 C13 1.451(4) . ?
N1 C12 1.454(4) . ?
N2 C15 1.37(2) . ?
N2 C16 1.391(17) . ?
N2 C17 1.51(2) . ?
C1 C2 1.511(4) . ?
C2 C3 1.402(4) . ?
C3 C4 1.403(4) . ?
C3 C8 1.508(3) . ?
C4 C5 1.511(4) . ?
C6 C7 1.505(3) . ?
C7 C8 1.413(3) . ?
C8 C9 1.406(3) . ?
C9 C10 1.508(4) . ?

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
O2 Zn1 O4 130.72(9) . 7_755 ?
O2 Zn1 O3 94.98(7) . 7_755 ?
O4 Zn1 O3 88.46(7) 7_755 7_755 ?
O2 Zn1 O1 88.54(7) . . ?
O4 Zn1 O1 88.65(7) 7_755 . ?
O3 Zn1 O1 176.39(7) 7_755 . ?
O2 Zn1 O5 105.15(8) . . ?
O4 Zn1 O5 123.92(9) 7_755 . ?
O3 Zn1 O5 91.54(8) 7_755 . ?
O1 Zn1 O5 88.28(8) . . ?
C2 O1 Zn1 123.13(16) . . ?
C4 O2 Zn1 123.85(18) . . ?
C7 O3 Zn1 128.30(17) . 7_765 ?
C9 O4 Zn1 128.95(17) . 7_765 ?
C11 O5 Zn1 124.63(19) . . ?
C11 N1 C13 122.2(3) . . ?
C11 N1 C12 121.2(2) . . ?
C13 N1 C12 116.6(3) . . ?
C15 N2 C16 118.1(13) . . ?
C15 N2 C17 115.4(12) . . ?
C16 N2 C17 124.9(13) . . ?
O1 C2 C3 126.1(2) . . ?
O1 C2 C1 114.3(2) . . ?
C3 C2 C1 119.7(2) . . ?
C2 C3 C4 122.6(2) . . ?
C2 C3 C8 118.9(2) . . ?
C4 C3 C8 118.5(2) . . ?
O2 C4 C3 125.9(2) . . ?
O2 C4 C5 114.1(2) . . ?
C3 C4 C5 120.0(2) . . ?
O3 C7 C8 125.4(2) . . ?
O3 C7 C6 114.7(2) . . ?
C8 C7 C6 119.9(2) . . ?
C9 C8 C7 122.29(19) . . ?
C9 C8 C3 119.4(2) . . ?
C7 C8 C3 118.3(2) . . ?
O4 C9 C8 126.3(2) . . ?
O4 C9 C10 113.7(2) . . ?
C8 C9 C10 120.0(2) . . ?
O5 C11 N1 124.7(3) . . ?
Cl2 C14 Cl1 110.9(3) . . ?
Cl2 C14 Cl3 109.1(3) . . ?
Cl1 C14 Cl3 108.1(3) . . ?
O6 C15 N2 123.6(14) . . ?

_diffrn_measured_fraction_theta_max 0.991
_diffrn_reflns_theta_full        29.67
_diffrn_measured_fraction_theta_full 0.991
_refine_diff_density_max         0.890
_refine_diff_density_min         -0.599
_refine_diff_density_rms         0.074
#===END

data_compound_6_bath93
_database_code_depnum_ccdc_archive 'CCDC 244504'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C20 H33 Cd2 O12.50'
_chemical_formula_weight         698.26

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   P212121

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

_cell_length_a                   11.9762(10)
_cell_length_b                   14.2223(12)
_cell_length_c                   15.5903(14)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     2655.5(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    25
_cell_measurement_theta_min      12
_cell_measurement_theta_max      18

_exptl_crystal_description       Plate
_exptl_crystal_colour            Colourless
_exptl_crystal_size_max          0.015
_exptl_crystal_size_mid          0.015
_exptl_crystal_size_min          0.005
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.747
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1396
_exptl_absorpt_coefficient_mu    1.659
_exptl_absorpt_correction_type   None
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.6934
_diffrn_radiation_type           Synchrotron
_diffrn_radiation_source         'Daresbury SRS station 9.8'
_diffrn_radiation_monochromator  'Silicon 111'
_diffrn_measurement_device_type  'Bruker SMART CCD diffractometer'
_diffrn_measurement_method       'ω rotation with narrow frames'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            10941
_diffrn_reflns_av_R_equivalents  0.0629
_diffrn_reflns_av_sigmaI/netI    0.0894
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         2.09
_diffrn_reflns_theta_max         24.07
_reflns_number_total             4505
_reflns_number_gt                3157
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'local programs'
_computing_data_reduction        'Bruker SAINT v7.06a'
_computing_structure_solution    'Bruker SHELXTL'
_computing_structure_refinement  'Sir 92'
_computing_molecular_graphics    'ORTEX (P.McArdle, 1995)'
_computing_publication_material  'SHELXL-97/2 (Sheldrick,1997)'

_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)+(0.0505P)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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.08(5)
_refine_ls_number_reflns         4505
_refine_ls_number_parameters     325
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0876
_refine_ls_R_factor_gt           0.0495
_refine_ls_wR_factor_ref         0.1120
_refine_ls_wR_factor_gt          0.0973
_refine_ls_goodness_of_fit_ref   1.003
_refine_ls_restrained_S_all      1.003
_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 0.63587(6) 0.18229(4) 0.14079(5) 0.0298(2) Uani 1 1 d . . .
Cd2 Cd 0.85694(6) 0.34447(4) 0.13159(5) 0.0295(2) Uani 1 1 d . . .
O1 O 0.6911(6) 0.0369(4) 0.1127(5) 0.045(2) Uani 1 1 d . . .
O2 O 0.8241(6) 0.1884(4) 0.1606(5) 0.034(2) Uani 1 1 d . . .
O3 O 0.9613(5) -0.1230(5) 0.3756(6) 0.036(2) Uani 1 1 d . . .
O4 O 1.1089(6) -0.1184(5) 0.2325(5) 0.0367(19) Uani 1 1 d . . .
O5 O 0.6691(6) 0.3416(4) 0.1512(5) 0.0351(19) Uani 1 1 d . . .
O6 O 0.8005(6) 0.4862(5) 0.0883(5) 0.038(2) Uani 1 1 d . . .
O7 O 0.5461(5) 0.6525(4) 0.3615(5) 0.0358(18) Uani 1 1 d . . .
O8 O 0.3975(5) 0.6618(5) 0.2211(5) 0.0383(18) Uani 1 1 d . . .
O9 O 0.6291(7) 0.2273(4) -0.0014(5) 0.0401(18) Uani 1 1 d . . .
O10 O 0.8585(7) 0.2761(4) -0.0038(4) 0.0350(17) Uani 1 1 d . . .
O11 O 1.2512(9) -0.2273(8) 0.1242(8) 0.094(4) Uani 1 1 d . . .
O12 O 1.0530(14) -0.2617(10) 0.0278(12) 0.108(6) Uani 0.75 1 d P . .
O13 O 0.9771(16) -0.4337(10) -0.0261(11) 0.122(7) Uani 0.75 1 d P . .
C1 C 0.7528(9) -0.1160(6) 0.1417(10) 0.052(3) Uani 1 1 d . . .
H1A H 0.6824 -0.1294 0.1121 0.078 Uiso 1 1 calc R . .
H1B H 0.7512 -0.1443 0.1990 0.078 Uiso 1 1 calc R . .
H1C H 0.8150 -0.1426 0.1088 0.078 Uiso 1 1 calc R . .
C2 C 0.7679(8) -0.0107(6) 0.1497(8) 0.033(3) Uani 1 1 d . . .
C3 C 0.8594(11) 0.0298(6) 0.1982(7) 0.038(3) Uani 1 1 d . . .
C4 C 0.8843(8) 0.1249(6) 0.1995(7) 0.026(2) Uani 1 1 d . . .
C5 C 0.9827(9) 0.1604(7) 0.2460(8) 0.045(3) Uani 1 1 d . . .
H5A H 1.0500 0.1491 0.2118 0.067 Uiso 1 1 calc R . .
H5B H 0.9893 0.1276 0.3011 0.067 Uiso 1 1 calc R . .
H5C H 0.9742 0.2280 0.2562 0.067 Uiso 1 1 calc R . .
C6 C 0.8011(9) -0.0274(8) 0.3699(10) 0.056(4) Uani 1 1 d . . .
H6A H 0.7408 -0.0732 0.3623 0.084 Uiso 1 1 calc R . .
H6B H 0.7801 0.0322 0.3428 0.084 Uiso 1 1 calc R . .
H6C H 0.8141 -0.0171 0.4313 0.084 Uiso 1 1 calc R . .
C7 C 0.9084(10) -0.0650(7) 0.3281(8) 0.035(3) Uani 1 1 d . . .
C8 C 0.9350(9) -0.0377(6) 0.2446(8) 0.034(3) Uani 1 1 d . . .
C9 C 1.0297(9) -0.0679(6) 0.2002(8) 0.034(3) Uani 1 1 d . . .
C10 C 1.0444(10) -0.0414(8) 0.1093(8) 0.050(4) Uani 1 1 d . . .
H10E H 1.0638 0.0254 0.1055 0.075 Uiso 1 1 calc R . .
H10D H 0.9747 -0.0528 0.0781 0.075 Uiso 1 1 calc R . .
H10C H 1.1043 -0.0792 0.0840 0.075 Uiso 1 1 calc R . .
C11 C 0.5100(9) 0.3775(7) 0.2358(8) 0.042(3) Uani 1 1 d . . .
H11A H 0.4796 0.3204 0.2095 0.063 Uiso 1 1 calc R . .
H11B H 0.4535 0.4273 0.2344 0.063 Uiso 1 1 calc R . .
H11C H 0.5308 0.3644 0.2954 0.063 Uiso 1 1 calc R . .
C12 C 0.6124(9) 0.4090(6) 0.1863(7) 0.036(3) Uani 1 1 d . . .
C13 C 0.6394(10) 0.5023(6) 0.1781(7) 0.037(3) Uani 1 1 d . . .
C14 C 0.7299(9) 0.5364(6) 0.1277(9) 0.037(3) Uani 1 1 d . . .
C15 C 0.7482(9) 0.6412(6) 0.1151(9) 0.048(3) Uani 1 1 d . . .
H15A H 0.8283 0.6538 0.1090 0.072 Uiso 1 1 calc R . .
H15B H 0.7190 0.6754 0.1648 0.072 Uiso 1 1 calc R . .
H15C H 0.7091 0.6620 0.0632 0.072 Uiso 1 1 calc R . .
C16 C 0.7062(10) 0.5577(9) 0.3472(9) 0.055(4) Uani 1 1 d . . .
H16A H 0.7583 0.6098 0.3570 0.082 Uiso 1 1 calc R . .
H16B H 0.7393 0.5130 0.3067 0.082 Uiso 1 1 calc R . .
H16C H 0.6909 0.5258 0.4017 0.082 Uiso 1 1 calc R . .
C17 C 0.5980(9) 0.5957(7) 0.3104(9) 0.039(3) Uani 1 1 d . . .
C18 C 0.5676(9) 0.5725(6) 0.2265(8) 0.033(3) Uani 1 1 d . . .
C19 C 0.4718(10) 0.6105(7) 0.1844(8) 0.038(3) Uani 1 1 d . . .
C20 C 0.4535(10) 0.5882(8) 0.0906(8) 0.044(3) Uani 1 1 d . . .
H20A H 0.3795 0.6104 0.0730 0.065 Uiso 1 1 calc R . .
H20B H 0.4584 0.5201 0.0818 0.065 Uiso 1 1 calc R . .
H20C H 0.5108 0.6197 0.0561 0.065 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 O8 2.209(8) 4_645 ?
Cd1 O1 2.215(6) . ?
Cd1 O7 2.220(6) 4_645 ?
Cd1 O2 2.277(7) . ?
Cd1 O5 2.306(6) . ?
Cd1 O9 2.309(7) . ?
Cd2 O4 2.222(7) 4_755 ?
Cd2 O3 2.228(7) 4_755 ?
Cd2 O6 2.231(7) . ?
Cd2 O5 2.270(7) . ?
Cd2 O2 2.299(6) . ?
Cd2 O10 2.323(6) . ?
O1 C2 1.280(11) . ?
O2 C4 1.305(11) . ?
O3 C7 1.277(12) . ?
O3 Cd2 2.228(7) 4_745 ?
O4 C9 1.292(12) . ?
O4 Cd2 2.222(7) 4_745 ?
O4 O11 2.855(12) . ?
O5 C12 1.297(11) . ?
O6 C14 1.265(12) . ?
O7 C17 1.293(13) . ?
O7 Cd1 2.220(6) 4_655 ?
O8 C19 1.285(13) . ?
O8 Cd1 2.209(8) 4_655 ?
O11 O12 2.85(2) . ?
O12 O13 2.74(2) . ?
O13 O6 2.992(16) 1_545 ?
O13 O1 3.247(19) 3_545 ?
C1 C2 1.514(12) . ?
C2 C3 1.450(15) . ?
C3 C4 1.385(12) . ?
C3 C8 1.506(14) . ?
C4 C5 1.474(14) . ?
C6 C7 1.537(15) . ?
C7 C8 1.394(16) . ?
C8 C9 1.396(15) . ?
C9 C10 1.477(16) . ?
C11 C12 1.517(15) . ?
C12 C13 1.371(13) . ?
C13 C14 1.425(15) . ?
C13 C18 1.518(13) . ?
C14 C15 1.520(13) . ?
C16 C17 1.517(15) . ?
C17 C18 1.397(16) . ?
C18 C19 1.428(15) . ?
C19 C20 1.513(16) . ?

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
O8 Cd1 O1 97.1(3) 4_645 . ?
O8 Cd1 O7 79.2(3) 4_645 4_645 ?
O1 Cd1 O7 96.4(3) . 4_645 ?
O8 Cd1 O2 93.0(3) 4_645 . ?
O1 Cd1 O2 76.5(3) . . ?
O7 Cd1 O2 168.9(2) 4_645 . ?
O8 Cd1 O5 95.3(3) 4_645 . ?
O1 Cd1 O5 151.6(3) . . ?
O7 Cd1 O5 111.0(2) 4_645 . ?
O2 Cd1 O5 77.4(2) . . ?
O8 Cd1 O9 165.0(3) 4_645 . ?
O1 Cd1 O9 94.6(3) . . ?
O7 Cd1 O9 90.2(3) 4_645 . ?
O2 Cd1 O9 98.9(3) . . ?
O5 Cd1 O9 78.6(3) . . ?
O4 Cd2 O3 79.6(3) 4_755 4_755 ?
O4 Cd2 O6 97.4(3) 4_755 . ?
O3 Cd2 O6 95.3(3) 4_755 . ?
O4 Cd2 O5 93.3(3) 4_755 . ?
O3 Cd2 O5 168.1(2) 4_755 . ?
O6 Cd2 O5 75.9(2) . . ?
O4 Cd2 O2 94.2(3) 4_755 . ?
O3 Cd2 O2 112.2(2) 4_755 . ?
O6 Cd2 O2 151.7(3) . . ?
O5 Cd2 O2 77.7(2) . . ?
O4 Cd2 O10 164.6(2) 4_755 . ?
O3 Cd2 O10 91.9(3) 4_755 . ?
O6 Cd2 O10 96.1(3) . . ?
O5 Cd2 O10 97.1(3) . . ?
O2 Cd2 O10 77.1(2) . . ?
C2 O1 Cd1 128.3(7) . . ?
C4 O2 Cd1 125.7(6) . . ?
C4 O2 Cd2 131.7(6) . . ?
Cd1 O2 Cd2 100.4(3) . . ?
C7 O3 Cd2 126.1(7) . 4_745 ?
C9 O4 Cd2 129.7(7) . 4_745 ?
C9 O4 O11 120.7(7) . . ?
Cd2 O4 O11 109.0(3) 4_745 . ?
C12 O5 Cd2 124.3(6) . . ?
C12 O5 Cd1 131.8(6) . . ?
Cd2 O5 Cd1 100.3(2) . . ?
C14 O6 Cd2 124.4(7) . . ?
C17 O7 Cd1 125.5(7) . 4_655 ?
C19 O8 Cd1 129.4(7) . 4_655 ?
O12 O11 O4 84.7(5) . . ?
O13 O12 O11 126.2(7) . . ?
O12 O13 O6 113.0(7) . 1_545 ?
O12 O13 O1 105.6(6) . 3_545 ?
O6 O13 O1 129.3(6) 1_545 3_545 ?
O1 C2 C3 124.6(8) . . ?
O1 C2 C1 113.6(8) . . ?
C3 C2 C1 121.8(9) . . ?
C4 C3 C2 123.9(9) . . ?
C4 C3 C8 119.1(10) . . ?
C2 C3 C8 116.8(8) . . ?
O2 C4 C3 123.4(9) . . ?
O2 C4 C5 115.7(8) . . ?
C3 C4 C5 120.9(9) . . ?
O3 C7 C8 127.4(10) . . ?
O3 C7 C6 113.1(11) . . ?
C8 C7 C6 119.4(10) . . ?
C7 C8 C9 124.3(10) . . ?
C7 C8 C3 119.2(10) . . ?
C9 C8 C3 116.5(11) . . ?
O4 C9 C8 125.1(11) . . ?
O4 C9 C10 115.3(10) . . ?
C8 C9 C10 119.6(10) . . ?
O5 C12 C13 123.6(10) . . ?
O5 C12 C11 114.8(8) . . ?
C13 C12 C11 121.6(9) . . ?
C12 C13 C14 124.1(9) . . ?
C12 C13 C18 117.2(10) . . ?
C14 C13 C18 118.8(8) . . ?
O6 C14 C13 125.8(8) . . ?
O6 C14 C15 113.2(10) . . ?
C13 C14 C15 121.0(9) . . ?
O7 C17 C18 126.8(10) . . ?
O7 C17 C16 113.6(11) . . ?
C18 C17 C16 119.5(10) . . ?
C17 C18 C19 123.3(10) . . ?
C17 C18 C13 118.3(9) . . ?
C19 C18 C13 118.4(11) . . ?
O8 C19 C18 124.5(11) . . ?
O8 C19 C20 116.7(11) . . ?
C18 C19 C20 118.8(11) . . ?

_diffrn_measured_fraction_theta_max 0.993
_diffrn_reflns_theta_full        24.07
_diffrn_measured_fraction_theta_full 0.993
_refine_diff_density_max         1.175
_refine_diff_density_min         -0.815
_refine_diff_density_rms         0.124
#===END

#===END

data_compound_2_bath135
_database_code_depnum_ccdc_archive 'CCDC 688575'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C41 H70 O18 S5 Zn3'
_chemical_formula_weight         1207.38

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'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Orthorhombic
_symmetry_space_group_name_H-M   Pbca

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

_cell_length_a                   16.3499(13)
_cell_length_b                   15.4909(13)
_cell_length_c                   42.062(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     10653.3(15)
_cell_formula_units_Z            8
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    2759
_cell_measurement_theta_min      3.651
_cell_measurement_theta_max      28.628

_exptl_crystal_description       Block
_exptl_crystal_colour            Colourless
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.02
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.506
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             5040
_exptl_absorpt_coefficient_mu    1.602
_exptl_absorpt_correction_type   Multi-Scan
_exptl_absorpt_correction_T_min  0.94
_exptl_absorpt_correction_T_max  0.96
_exptl_absorpt_process_details   
;
?
;

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.84590
_diffrn_radiation_type           ?
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  ?
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            52160
_diffrn_reflns_av_R_equivalents  0.0937
_diffrn_reflns_av_sigmaI/netI    0.0808
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -51
_diffrn_reflns_limit_l_max       51
_diffrn_reflns_theta_min         4.26
_diffrn_reflns_theta_max         31.95
_reflns_number_total             10795
_reflns_number_gt                6391
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_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. Similarity restraints
applied to distances and ADPs in the disordered fractions of the DMSO
moieties. We were fully aware of the clash between the 20% DMSO fraction
and the full-occupancy methanol, and spent much time scrutinising this region
of the electron density map. Given the ADPs associated with the methanol
in question, we concluded that it is very likely that disorder exists
in this region also. However, 20% of a methanol is not a lot of electron
density, and attempts to locate and refined such a fraction of solvent met
with failure. It is likely that the 20% DMSO would not have been
modelled had it not been for the presence of a second period element
in the solvent which could not be ignored. Thus, on balance,
the methanol ligand has been included at full occupancy.
;

_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)+(0.0985P)²+25.2401P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         10795
_refine_ls_number_parameters     685
_refine_ls_number_restraints     38
_refine_ls_R_factor_all          0.1216
_refine_ls_R_factor_gt           0.0707
_refine_ls_wR_factor_ref         0.2197
_refine_ls_wR_factor_gt          0.1879
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_restrained_S_all      5.210
_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
Zn1 Zn 0.74756(18) 0.3948(2) 0.08447(7) 0.0224(9) Uani 1 1 d . A .
Zn2 Zn 1.2465(2) 0.3801(2) 0.07888(10) 0.0355(11) Uani 1 1 d . . .
Zn3 Zn 0.74512(19) 0.1670(3) 0.24185(9) 0.0362(11) Uani 1 1 d . . .
S1 S 0.7139(8) 0.5409(9) 0.0293(3) 0.020(3) Uani 0.50 1 d P A 1
S2 S 0.7593(13) 0.2029(11) 0.1112(5) 0.050(5) Uani 0.50 1 d P A 1
S3 S 1.2587(10) 0.2004(12) 0.0463(5) 0.048(5) Uani 0.50 1 d PD B 1
S4 S 0.7580(18) -0.0191(14) 0.2160(5) 0.066(7) Uani 0.50 1 d PD C 1
S5 S 0.7868(8) 0.3005(9) 0.3071(3) 0.044(3) Uani 0.70 1 d P D 1
S2A S 0.7810(10) 0.2447(11) 0.1376(4) 0.036(4) Uani 0.50 1 d P A 2
O1 O 0.6669(12) 0.3209(14) 0.0598(5) 0.036(5) Uani 1 1 d . . .
O2 O 0.6559(11) 0.4153(13) 0.1165(4) 0.026(4) Uani 1 1 d . . .
O3 O 0.8357(11) 0.3746(13) 0.0510(4) 0.028(5) Uani 1 1 d . . .
O4 O 0.8307(11) 0.4656(13) 0.1088(5) 0.031(5) Uani 1 1 d . . .
O5 O 1.1690(11) 0.4737(13) 0.0661(5) 0.035(5) Uani 1 1 d . . .
O6 O 1.1557(11) 0.3317(14) 0.1064(5) 0.035(5) Uani 1 1 d . . .
O7 O 0.3388(11) 0.4434(14) 0.0571(5) 0.034(5) Uani 1 1 d . . .
O8 O 0.3285(12) 0.3007(16) 0.0981(6) 0.047(6) Uani 1 1 d . . .
O9 O 0.6585(13) 0.2465(16) 0.2269(6) 0.050(7) Uani 1 1 d . E .
O10 O 0.6656(12) 0.1240(15) 0.2743(5) 0.037(5) Uani 1 1 d . E .
O11 O 0.3328(14) 0.110(2) 0.2319(7) 0.071(10) Uani 1 1 d . . .
O12 O 0.3315(12) 0.2370(15) 0.2792(5) 0.042(6) Uani 1 1 d . . .
O13 O 0.7021(14) 0.5110(17) 0.0603(7) 0.058(8) Uani 1 1 d . . .
O14 O 0.7938(14) 0.2809(17) 0.1092(7) 0.066(9) Uani 1 1 d . . .
O15 O 1.2189(18) 0.2921(15) 0.0418(6) 0.057(7) Uani 1 1 d . . .
O16 O 1.284(2) 0.457(3) 0.1250(9) 0.097(11) Uani 1 1 d . . .
O17 O 0.729(3) 0.0745(18) 0.2077(7) 0.094(13) Uani 1 1 d . C .
C39 C 0.681(4) 0.337(7) 0.311(2) 0.10(3) Uani 0.70 1 d P D 1
H39A H 0.6725 0.3883 0.2981 0.147 Uiso 0.70 1 calc PR D 1
H39B H 0.6696 0.3499 0.3334 0.147 Uiso 0.70 1 calc PR D 1
H39C H 0.6441 0.2907 0.3039 0.147 Uiso 0.70 1 calc PR D 1
C1 C 0.5452(19) 0.279(2) 0.0343(9) 0.044(9) Uani 1 1 d . . .
H1A H 0.5126 0.3209 0.0222 0.066 Uiso 1 1 calc R . .
H1B H 0.5090 0.2351 0.0433 0.066 Uiso 1 1 calc R . .
H1C H 0.5849 0.2515 0.0201 0.066 Uiso 1 1 calc R . .
C2 C 0.5902(16) 0.3254(19) 0.0609(7) 0.027(7) Uani 1 1 d . . .
C3 C 0.5436(16) 0.3682(18) 0.0846(7) 0.025(6) Uani 1 1 d . . .
C4 C 0.5799(16) 0.4116(18) 0.1105(7) 0.024(6) Uani 1 1 d . . .
C5 C 0.5255(18) 0.456(2) 0.1344(8) 0.037(8) Uani 1 1 d . . .
H5A H 0.5590 0.4798 0.1516 0.056 Uiso 1 1 calc R . .
H5B H 0.4863 0.4147 0.1431 0.056 Uiso 1 1 calc R . .
H5C H 0.4958 0.5032 0.1239 0.056 Uiso 1 1 calc R . .
C6 C 0.9567(18) 0.499(2) 0.1338(8) 0.038(8) Uani 1 1 d . . .
H6A H 0.9190 0.5262 0.1488 0.057 Uiso 1 1 calc R . .
H6B H 0.9940 0.5423 0.1251 0.057 Uiso 1 1 calc R . .
H6C H 0.9883 0.4541 0.1448 0.057 Uiso 1 1 calc R . .
C7 C 0.9081(16) 0.4577(19) 0.1068(7) 0.027(6) Uani 1 1 d . . .
C8 C 0.9519(15) 0.4159(19) 0.0821(7) 0.024(6) Uani 1 1 d . . .
C9 C 0.9120(16) 0.3759(19) 0.0562(7) 0.025(6) Uani 1 1 d . . .
C10 C 0.9639(17) 0.333(2) 0.0310(7) 0.034(7) Uani 1 1 d . . .
H10A H 0.9881 0.2800 0.0397 0.051 Uiso 1 1 calc R . .
H10B H 1.0074 0.3721 0.0243 0.051 Uiso 1 1 calc R . .
H10C H 0.9296 0.3180 0.0126 0.051 Uiso 1 1 calc R . .
C11 C 1.0493(18) 0.546(2) 0.0509(9) 0.047(9) Uani 1 1 d . . .
H11A H 1.0025 0.5660 0.0634 0.070 Uiso 1 1 calc R . .
H11B H 1.0302 0.5251 0.0302 0.070 Uiso 1 1 calc R . .
H11C H 1.0879 0.5935 0.0478 0.070 Uiso 1 1 calc R . .
C12 C 1.0915(16) 0.4731(19) 0.0684(8) 0.029(7) Uani 1 1 d . . .
C13 C 1.0433(16) 0.4104(19) 0.0839(7) 0.027(6) Uani 1 1 d . . .
C14 C 1.0798(17) 0.342(2) 0.1017(7) 0.030(7) Uani 1 1 d . . .
C15 C 1.0243(19) 0.274(2) 0.1163(9) 0.048(10) Uani 1 1 d . . .
H15A H 1.0569 0.2350 0.1295 0.073 Uiso 1 1 calc R . .
H15B H 0.9974 0.2412 0.0994 0.073 Uiso 1 1 calc R . .
H15C H 0.9827 0.3023 0.1295 0.073 Uiso 1 1 calc R . .
C16 C 0.4687(18) 0.500(2) 0.0461(8) 0.041(8) Uani 1 1 d . . .
H16A H 0.4385 0.5272 0.0286 0.061 Uiso 1 1 calc R . .
H16B H 0.5176 0.4716 0.0377 0.061 Uiso 1 1 calc R . .
H16C H 0.4851 0.5447 0.0614 0.061 Uiso 1 1 calc R . .
C17 C 0.4147(17) 0.434(2) 0.0624(7) 0.029(7) Uani 1 1 d . . .
C18 C 0.4524(16) 0.3695(18) 0.0814(7) 0.026(6) Uani 1 1 d . . .
C19 C 0.4059(17) 0.306(2) 0.0968(8) 0.035(8) Uani 1 1 d . . .
C20 C 0.450(2) 0.234(2) 0.1143(9) 0.049(10) Uani 1 1 d . . .
H20A H 0.4625 0.2528 0.1360 0.074 Uiso 1 1 calc R . .
H20B H 0.5007 0.2197 0.1032 0.074 Uiso 1 1 calc R . .
H20C H 0.4147 0.1827 0.1151 0.074 Uiso 1 1 calc R . .
C21 C 0.530(2) 0.300(3) 0.2107(11) 0.087(18) Uani 1 1 d . E .
H21A H 0.5658 0.3334 0.1967 0.130 Uiso 1 1 calc R . .
H21B H 0.4986 0.3386 0.2243 0.130 Uiso 1 1 calc R . .
H21C H 0.4926 0.2649 0.1977 0.130 Uiso 1 1 calc R . .
C22 C 0.582(2) 0.241(3) 0.2311(8) 0.046(9) Uani 1 1 d . . .
C23 C 0.5427(17) 0.183(2) 0.2526(8) 0.036(8) Uani 1 1 d . E .
C24 C 0.5882(17) 0.128(2) 0.2729(8) 0.037(8) Uani 1 1 d . . .
C25 C 0.543(2) 0.072(3) 0.2967(9) 0.061(12) Uani 1 1 d . E .
H25A H 0.5827 0.0486 0.3119 0.091 Uiso 1 1 calc R . .
H25B H 0.5160 0.0251 0.2855 0.091 Uiso 1 1 calc R . .
H25C H 0.5027 0.1072 0.3080 0.091 Uiso 1 1 calc R . .
C26 C 0.458(2) 0.294(3) 0.2962(10) 0.063(12) Uani 1 1 d . . .
H26A H 0.4209 0.3209 0.3117 0.095 Uiso 1 1 calc R . .
H26B H 0.4834 0.3387 0.2832 0.095 Uiso 1 1 calc R . .
H26C H 0.5000 0.2612 0.3075 0.095 Uiso 1 1 calc R . .
C27 C 0.4094(18) 0.234(2) 0.2752(8) 0.039(8) Uani 1 1 d . E .
C28 C 0.4508(17) 0.180(2) 0.2536(8) 0.039(8) Uani 1 1 d . . .
C29 C 0.4090(19) 0.121(3) 0.2334(9) 0.058(12) Uani 1 1 d . E .
C30 C 0.459(2) 0.067(4) 0.2105(12) 0.10(2) Uani 1 1 d . . .
H30A H 0.4232 0.0410 0.1945 0.144 Uiso 1 1 calc R E .
H30B H 0.4871 0.0206 0.2223 0.144 Uiso 1 1 calc R . .
H30C H 0.5000 0.1032 0.2000 0.144 Uiso 1 1 calc R . .
C31 C 0.658(8) 0.636(7) 0.022(2) 0.049(18) Uani 0.50 1 d P A 1
H31A H 0.5998 0.6242 0.0247 0.073 Uiso 0.50 1 calc PR A 1
H31B H 0.6688 0.6557 0.0004 0.073 Uiso 0.50 1 calc PR A 1
H31C H 0.6753 0.6805 0.0373 0.073 Uiso 0.50 1 calc PR A 1
C33 C 0.680(14) 0.209(13) 0.146(4) 0.06(4) Uani 0.50 1 d PU A 1
H33A H 0.6322 0.2419 0.1395 0.097 Uiso 0.50 1 calc PR A 1
H33B H 0.7056 0.2368 0.1646 0.097 Uiso 0.50 1 calc PR A 1
H33C H 0.6633 0.1501 0.1521 0.097 Uiso 0.50 1 calc PR A 1
C34 C 0.832(3) 0.138(3) 0.1371(13) 0.084(17) Uani 0.50 1 d P A 1
H34A H 0.8842 0.1318 0.1263 0.127 Uiso 0.50 1 calc PR A 1
H34B H 0.8080 0.0813 0.1413 0.127 Uiso 0.50 1 calc PR A 1
H34C H 0.8398 0.1687 0.1573 0.127 Uiso 0.50 1 calc PR A 1
C35 C 1.223(4) 0.135(4) 0.0145(13) 0.103(18) Uani 0.50 1 d PDU B 1
H35A H 1.2467 0.1551 -0.0055 0.155 Uiso 0.50 1 calc PR B 1
H35B H 1.1631 0.1386 0.0133 0.155 Uiso 0.50 1 calc PR B 1
H35C H 1.2390 0.0748 0.0183 0.155 Uiso 0.50 1 calc PR B 1
C36 C 1.205(3) 0.150(2) 0.0771(9) 0.059(11) Uani 0.50 1 d P B 1
H36A H 1.2208 0.1760 0.0974 0.089 Uiso 0.50 1 calc PR B 1
H36B H 1.2191 0.0882 0.0774 0.089 Uiso 0.50 1 calc PR B 1
H36C H 1.1465 0.1567 0.0737 0.089 Uiso 0.50 1 calc PR B 1
C37 C 0.688(5) -0.060(4) 0.2441(16) 0.050(19) Uani 0.50 1 d PDU C 1
H37A H 0.6907 -0.0256 0.2637 0.075 Uiso 0.50 1 calc PR C 1
H37B H 0.7008 -0.1202 0.2489 0.075 Uiso 0.50 1 calc PR C 1
H37C H 0.6320 -0.0564 0.2354 0.075 Uiso 0.50 1 calc PR C 1
C38 C 0.752(4) -0.076(4) 0.1841(15) 0.14(3) Uani 0.50 1 d P C 1
H38A H 0.7916 -0.0540 0.1684 0.209 Uiso 0.50 1 calc PR C 1
H38B H 0.6970 -0.0722 0.1754 0.209 Uiso 0.50 1 calc PR C 1
H38C H 0.7653 -0.1363 0.1890 0.209 Uiso 0.50 1 calc PR C 1
O18 O 0.840(2) 0.365(3) 0.3241(9) 0.060(10) Uani 0.70 1 d P D 1
C40 C 0.781(5) 0.207(5) 0.3330(14) 0.08(2) Uani 0.70 1 d P D 1
H40A H 0.8359 0.1824 0.3360 0.116 Uiso 0.70 1 calc PR D 1
H40B H 0.7454 0.1629 0.3234 0.116 Uiso 0.70 1 calc PR D 1
H40C H 0.7586 0.2237 0.3537 0.116 Uiso 0.70 1 calc PR D 1
C41 C 1.223(5) 0.514(5) 0.1404(19) 0.15(3) Uani 1 1 d . B .
H41A H 1.2194 0.5685 0.1287 0.228 Uiso 1 1 calc R . .
H41B H 1.2398 0.5252 0.1623 0.228 Uiso 1 1 calc R . .
H41C H 1.1694 0.4854 0.1403 0.228 Uiso 1 1 calc R . .
S1A S 0.7473(17) 0.5821(16) 0.0526(7) 0.082(8) Uani 0.50 1 d P A 2
S3A S 1.1815(10) 0.2016(11) 0.0415(4) 0.039(4) Uani 0.50 1 d P B 2
S4A S 0.6977(14) -0.0166(13) 0.2069(6) 0.055(5) Uani 0.50 1 d PD C 2
C31A C 0.672(7) 0.658(7) 0.035(2) 0.049(18) Uani 0.50 1 d P A 2
H31D H 0.6269 0.6666 0.0499 0.073 Uiso 0.50 1 calc PR A 2
H31E H 0.6508 0.6333 0.0151 0.073 Uiso 0.50 1 calc PR A 2
H31F H 0.6988 0.7130 0.0305 0.073 Uiso 0.50 1 calc PR A 2
C33A C 0.680(14) 0.189(13) 0.134(4) 0.06(4) Uani 0.50 1 d PU A 2
H33D H 0.6357 0.2320 0.1350 0.097 Uiso 0.50 1 calc PR A 2
H33E H 0.6732 0.1486 0.1521 0.097 Uiso 0.50 1 calc PR A 2
H33F H 0.6770 0.1572 0.1142 0.097 Uiso 0.50 1 calc PR A 2
C34A C 0.832(3) 0.138(3) 0.1371(13) 0.084(17) Uani 0.50 1 d P A 2
H34D H 0.8908 0.1463 0.1351 0.127 Uiso 0.50 1 calc PR A 2
H34E H 0.8112 0.1046 0.1191 0.127 Uiso 0.50 1 calc PR A 2
H34F H 0.8196 0.1079 0.1570 0.127 Uiso 0.50 1 calc PR A 2
C35A C 1.223(4) 0.135(4) 0.0145(13) 0.103(18) Uani 0.50 1 d PDU B 2
H35D H 1.2469 0.1688 -0.0028 0.155 Uiso 0.50 1 calc PR B 2
H35E H 1.1804 0.0968 0.0060 0.155 Uiso 0.50 1 calc PR B 2
H35F H 1.2655 0.1000 0.0247 0.155 Uiso 0.50 1 calc PR B 2
C36A C 1.205(3) 0.150(2) 0.0771(9) 0.059(11) Uani 0.50 1 d P B 2
H36D H 1.1746 0.1763 0.0945 0.089 Uiso 0.50 1 calc PR B 2
H36E H 1.2642 0.1553 0.0812 0.089 Uiso 0.50 1 calc PR B 2
H36F H 1.1910 0.0885 0.0755 0.089 Uiso 0.50 1 calc PR B 2
C37A C 0.752(9) -0.053(10) 0.243(3) 0.16(7) Uani 0.50 1 d PDU C 2
H37D H 0.7277 -0.0252 0.2618 0.245 Uiso 0.50 1 calc PR C 2
H37E H 0.8098 -0.0373 0.2416 0.245 Uiso 0.50 1 calc PR C 2
H37F H 0.7469 -0.1158 0.2451 0.245 Uiso 0.50 1 calc PR C 2
C38A C 0.752(4) -0.076(4) 0.1841(15) 0.14(3) Uani 0.50 1 d P C 2
H38D H 0.7426 -0.0599 0.1619 0.209 Uiso 0.50 1 calc PR C 2
H38E H 0.7378 -0.1367 0.1873 0.209 Uiso 0.50 1 calc PR C 2
H38F H 0.8104 -0.0676 0.1892 0.209 Uiso 0.50 1 calc PR C 2
C32 C 0.812(2) 0.580(3) 0.0227(15) 0.10(2) Uani 0.50 1 d P A 1
H32A H 0.8517 0.5338 0.0260 0.155 Uiso 0.50 1 calc PR A 1
H32B H 0.8232 0.6275 0.0375 0.155 Uiso 0.50 1 calc PR A 1
H32C H 0.8161 0.6015 0.0008 0.155 Uiso 0.50 1 calc PR A 1
C32A C 0.812(2) 0.580(3) 0.0227(15) 0.10(2) Uani 0.50 1 d P A 2
H32D H 0.8576 0.5417 0.0278 0.155 Uiso 0.50 1 calc PR A 2
H32E H 0.8327 0.6386 0.0189 0.155 Uiso 0.50 1 calc PR A 2
H32F H 0.7839 0.5592 0.0036 0.155 Uiso 0.50 1 calc PR A 2
O18A O 0.747(7) 0.294(8) 0.276(3) 0.09(4) Uiso 0.30 1 d P E 2
S5A S 0.717(5) 0.311(4) 0.3080(16) 0.096(19) Uiso 0.30 1 d P E 2
C40A C 0.724(10) 0.225(12) 0.333(5) 0.07(5) Uiso 0.30 1 d P E 2
H40D H 0.7044 0.1724 0.3222 0.112 Uiso 0.30 1 calc PR E 2
H40E H 0.6896 0.2351 0.3519 0.112 Uiso 0.30 1 calc PR E 2
H40F H 0.7806 0.2166 0.3397 0.112 Uiso 0.30 1 calc PR E 2
C39A C 0.748(14) 0.399(17) 0.325(6) 0.14(9) Uiso 0.30 1 d P E 2
H39D H 0.7426 0.4474 0.3102 0.210 Uiso 0.30 1 calc PR E 2
H39E H 0.8056 0.3927 0.3312 0.210 Uiso 0.30 1 calc PR E 2
H39F H 0.7149 0.4101 0.3440 0.210 Uiso 0.30 1 calc PR E 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
Zn1 O4 2.025(19) . ?
Zn1 O1 2.03(2) . ?
Zn1 O2 2.039(18) . ?
Zn1 O3 2.039(18) . ?
Zn1 O14 2.18(2) . ?
Zn1 O13 2.20(2) . ?
Zn2 O8 1.99(2) 1_655 ?
Zn2 O5 1.999(19) . ?
Zn2 O7 2.020(19) 1_655 ?
Zn2 O6 2.03(2) . ?
Zn2 O15 2.12(3) . ?
Zn2 O16 2.36(4) . ?
Zn3 O9 1.98(2) . ?
Zn3 O12 1.99(2) 6_656 ?
Zn3 O10 2.00(2) . ?
Zn3 O11 2.01(2) 6_656 ?
Zn3 O17 2.05(3) . ?
Zn3 O18A 2.43(13) . ?
S1 O13 1.40(3) . ?
S1 C32 1.74(4) . ?
S1 C31 1.75(12) . ?
S2 O14 1.34(3) . ?
S2 C34 1.89(4) . ?
S2 C33 1.96(19) . ?
S3 O15 1.57(3) . ?
S3 C36 1.75(4) . ?
S3 C35 1.78(6) . ?
S4 O17 1.57(4) . ?
S4 C38 1.61(7) . ?
S4 C37 1.77(6) . ?
S5 O18 1.51(4) . ?
S5 C40 1.82(7) . ?
S5 C39 1.82(7) . ?
S2A O14 1.34(3) . ?
S2A C33A 1.9(2) . ?
O1 C2 1.26(3) . ?
O2 C4 1.27(3) . ?
O3 C9 1.27(3) . ?
O4 C7 1.27(3) . ?
O5 C12 1.27(3) . ?
O6 C14 1.27(3) . ?
O7 C17 1.27(3) . ?
O7 Zn2 2.020(19) 1_455 ?
O8 C19 1.27(3) . ?
O8 Zn2 1.99(2) 1_455 ?
O9 C22 1.27(4) . ?
O10 C24 1.27(3) . ?
O11 C29 1.26(4) . ?
O11 Zn3 2.01(2) 6_556 ?
O12 C27 1.29(3) . ?
O12 Zn3 1.99(2) 6_556 ?
O13 S1A 1.37(3) . ?
O15 S3A 1.53(3) . ?
O16 C41 1.47(7) . ?
O17 S4A 1.50(4) . ?
C1 C2 1.52(4) . ?
C2 C3 1.42(4) . ?
C3 C4 1.41(4) . ?
C3 C18 1.50(4) . ?
C4 C5 1.51(4) . ?
C6 C7 1.52(4) . ?
C7 C8 1.42(4) . ?
C8 C9 1.41(4) . ?
C8 C13 1.50(4) . ?
C9 C10 1.51(4) . ?
C11 C12 1.51(4) . ?
C12 C13 1.41(4) . ?
C13 C14 1.42(4) . ?
C14 C15 1.52(4) . ?
C16 C17 1.51(4) . ?
C17 C18 1.42(4) . ?
C18 C19 1.40(4) . ?
C19 C20 1.52(4) . ?
C21 C22 1.51(5) . ?
C22 C23 1.42(5) . ?
C23 C24 1.41(4) . ?
C23 C28 1.51(4) . ?
C24 C25 1.51(4) . ?
C26 C27 1.51(4) . ?
C27 C28 1.41(4) . ?
C28 C29 1.42(5) . ?
C29 C30 1.52(5) . ?
S1A C31A 1.85(11) . ?
S4A C37A 1.85(9) . ?
O18A S5A 1.46(13) . ?
S5A C39A 1.6(3) . ?
S5A C40A 1.70(18) . ?

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
O4 Zn1 O1 178.2(8) . . ?
O4 Zn1 O2 94.3(8) . . ?
O1 Zn1 O2 87.0(8) . . ?
O4 Zn1 O3 87.6(8) . . ?
O1 Zn1 O3 91.1(8) . . ?
O2 Zn1 O3 177.6(7) . . ?
O4 Zn1 O14 88.0(10) . . ?
O1 Zn1 O14 90.7(10) . . ?
O2 Zn1 O14 93.8(9) . . ?
O3 Zn1 O14 87.7(9) . . ?
O4 Zn1 O13 90.9(10) . . ?
O1 Zn1 O13 90.3(10) . . ?
O2 Zn1 O13 85.9(9) . . ?
O3 Zn1 O13 92.6(9) . . ?
O14 Zn1 O13 178.9(12) . . ?
O8 Zn2 O5 169.8(10) 1_655 . ?
O8 Zn2 O7 88.9(8) 1_655 1_655 ?
O5 Zn2 O7 90.0(8) . 1_655 ?
O8 Zn2 O6 91.9(9) 1_655 . ?
O5 Zn2 O6 87.6(8) . . ?
O7 Zn2 O6 170.6(9) 1_655 . ?
O8 Zn2 O15 92.5(11) 1_655 . ?
O5 Zn2 O15 97.7(10) . . ?
O7 Zn2 O15 97.9(10) 1_655 . ?
O6 Zn2 O15 91.5(10) . . ?
O8 Zn2 O16 78.8(12) 1_655 . ?
O5 Zn2 O16 91.0(12) . . ?
O7 Zn2 O16 86.3(11) 1_655 . ?
O6 Zn2 O16 84.7(11) . . ?
O15 Zn2 O16 170.4(12) . . ?
O9 Zn3 O12 91.6(9) . 6_656 ?
O9 Zn3 O10 87.7(9) . . ?
O12 Zn3 O10 161.4(10) 6_656 . ?
O9 Zn3 O11 163.2(13) . 6_656 ?
O12 Zn3 O11 88.7(9) 6_656 6_656 ?
O10 Zn3 O11 86.7(9) . 6_656 ?
O9 Zn3 O17 96.7(14) . . ?
O12 Zn3 O17 99.3(12) 6_656 . ?
O10 Zn3 O17 99.2(11) . . ?
O11 Zn3 O17 99.8(15) 6_656 . ?
O9 Zn3 O18A 72(3) . . ?
O12 Zn3 O18A 79(3) 6_656 . ?
O10 Zn3 O18A 83(3) . . ?
O11 Zn3 O18A 92(3) 6_656 . ?
O17 Zn3 O18A 169(3) . . ?
O13 S1 C32 113(2) . . ?
O13 S1 C31 112(4) . . ?
C32 S1 C31 99(4) . . ?
O14 S2 C34 104(2) . . ?
O14 S2 C33 107(6) . . ?
C34 S2 C33 90(7) . . ?
O15 S3 C36 106.7(19) . . ?
O15 S3 C35 107(2) . . ?
C36 S3 C35 98(2) . . ?
O17 S4 C38 108(3) . . ?
O17 S4 C37 106(3) . . ?
C38 S4 C37 109(4) . . ?
O18 S5 C40 106(3) . . ?
O18 S5 C39 107(3) . . ?
C40 S5 C39 98(4) . . ?
O14 S2A C33A 105(6) . . ?
C2 O1 Zn1 126.7(19) . . ?
C4 O2 Zn1 125.7(18) . . ?
C9 O3 Zn1 125.1(18) . . ?
C7 O4 Zn1 125.5(18) . . ?
C12 O5 Zn2 127.3(19) . . ?
C14 O6 Zn2 125.5(19) . . ?
C17 O7 Zn2 126.8(19) . 1_455 ?
C19 O8 Zn2 128(2) . 1_455 ?
C22 O9 Zn3 128(2) . . ?
C24 O10 Zn3 127(2) . . ?
C29 O11 Zn3 128(2) . 6_556 ?
C27 O12 Zn3 129(2) . 6_556 ?
S1A O13 S1 55.6(15) . . ?
S1A O13 Zn1 126.0(17) . . ?
S1 O13 Zn1 131.0(18) . . ?
S2 O14 S2A 59.9(15) . . ?
S2 O14 Zn1 128.0(18) . . ?
S2A O14 Zn1 135(2) . . ?
S3A O15 S3 48.6(11) . . ?
S3A O15 Zn2 133.0(16) . . ?
S3 O15 Zn2 113.9(16) . . ?
C41 O16 Zn2 119(4) . . ?
S4A O17 S4 40.3(13) . . ?
S4A O17 Zn3 135.9(19) . . ?
S4 O17 Zn3 117(2) . . ?
O1 C2 C3 126(3) . . ?
O1 C2 C1 115(3) . . ?
C3 C2 C1 119(2) . . ?
C4 C3 C2 123(2) . . ?
C4 C3 C18 119(3) . . ?
C2 C3 C18 119(2) . . ?
O2 C4 C3 126(3) . . ?
O2 C4 C5 115(2) . . ?
C3 C4 C5 119(2) . . ?
O4 C7 C8 127(3) . . ?
O4 C7 C6 115(2) . . ?
C8 C7 C6 118(2) . . ?
C9 C8 C7 122(2) . . ?
C9 C8 C13 118(2) . . ?
C7 C8 C13 119(2) . . ?
O3 C9 C8 126(3) . . ?
O3 C9 C10 115(2) . . ?
C8 C9 C10 118(2) . . ?
O5 C12 C13 127(3) . . ?
O5 C12 C11 114(3) . . ?
C13 C12 C11 119(2) . . ?
C12 C13 C14 121(2) . . ?
C12 C13 C8 119(3) . . ?
C14 C13 C8 119(2) . . ?
O6 C14 C13 126(3) . . ?
O6 C14 C15 116(3) . . ?
C13 C14 C15 118(3) . . ?
O7 C17 C18 127(3) . . ?
O7 C17 C16 115(3) . . ?
C18 C17 C16 119(2) . . ?
C19 C18 C17 121(3) . . ?
C19 C18 C3 119(2) . . ?
C17 C18 C3 119(2) . . ?
O8 C19 C18 127(3) . . ?
O8 C19 C20 114(3) . . ?
C18 C19 C20 119(2) . . ?
O9 C22 C23 125(3) . . ?
O9 C22 C21 115(3) . . ?
C23 C22 C21 120(3) . . ?
C24 C23 C22 122(3) . . ?
C24 C23 C28 119(3) . . ?
C22 C23 C28 119(3) . . ?
O10 C24 C23 126(3) . . ?
O10 C24 C25 115(3) . . ?
C23 C24 C25 119(3) . . ?
O12 C27 C28 126(3) . . ?
O12 C27 C26 115(3) . . ?
C28 C27 C26 120(3) . . ?
C27 C28 C29 122(3) . . ?
C27 C28 C23 118(3) . . ?
C29 C28 C23 119(3) . . ?
O11 C29 C28 126(3) . . ?
O11 C29 C30 116(3) . . ?
C28 C29 C30 118(3) . . ?
O13 S1A C31A 104(4) . . ?
O17 S4A C37A 96(6) . . ?
S5A O18A Zn3 133(8) . . ?
O18A S5A C39A 117(10) . . ?
O18A S5A C40A 115(9) . . ?
C39A S5A C40A 111(10) . . ?

_diffrn_measured_fraction_theta_max 0.988
_diffrn_reflns_theta_full        31.95
_diffrn_measured_fraction_theta_full 0.988
_refine_diff_density_max         1.135
_refine_diff_density_min         -1.129
_refine_diff_density_rms         0.120
#===END

data_compound_3_bath233
_database_code_depnum_ccdc_archive 'CCDC 688576'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C24 H40 O12 Zn2'
_chemical_formula_weight         649.28

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'
Zn Zn 0.2839 1.4301 '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

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

_cell_length_a                   10.470(3)
_cell_length_b                   13.926(3)
_cell_length_c                   10.476(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 109.048(4)
_cell_angle_gamma                90.00
_cell_volume                     1443.9(6)
_cell_formula_units_Z            2
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    3550
_cell_measurement_theta_min      2.451
_cell_measurement_theta_max      26.49

_exptl_crystal_description       Tabloid
_exptl_crystal_colour            Colourless
_exptl_crystal_size_max          0.03
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.02
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.494
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             680
_exptl_absorpt_coefficient_mu    1.72
_exptl_absorpt_correction_type   Multi-Scan
_exptl_absorpt_correction_T_min  0.97
_exptl_absorpt_correction_T_max  0.98
_exptl_absorpt_process_details   
;
?
;

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.69040
_diffrn_radiation_type           Synchrotron
_diffrn_radiation_source         'Daresbury SRS station 9.8 SMX'
_diffrn_radiation_monochromator  'Silicon 111'
_diffrn_measurement_device_type  'Bruker APEXII diffractometer'
_diffrn_measurement_method       'ω rotation with narrow frames'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            9446
_diffrn_reflns_av_R_equivalents  0.0468
_diffrn_reflns_av_sigmaI/netI    0.0823
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_theta_min         3.47
_diffrn_reflns_theta_max         26.50
_reflns_number_total             6168
_reflns_number_gt                4992
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'local programs'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'Bruker SHELXTL'
_computing_structure_refinement  'Bruker SHELXTL'
_computing_molecular_graphics    'ORTEX (P.McArdle, 1995)'
_computing_publication_material  'SHELXL-97/2 (Sheldrick,1997)'

_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.

Distance similarity restraints applied to disordered lattice methanol. ADPS
in dosordered fractions also refined subject to similarity restraints
;

_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)+(0.1209P)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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.02(2)
_refine_ls_number_reflns         6168
_refine_ls_number_parameters     370
_refine_ls_number_restraints     5
_refine_ls_R_factor_all          0.0853
_refine_ls_R_factor_gt           0.0711
_refine_ls_wR_factor_ref         0.1813
_refine_ls_wR_factor_gt          0.1736
_refine_ls_goodness_of_fit_ref   0.985
_refine_ls_restrained_S_all      0.985
_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
Zn1 Zn 0.91784(8) 0.29937(5) 0.27852(8) 0.0250(2) Uani 1 1 d . . .
Zn2 Zn 0.72148(8) 0.14006(5) 0.08223(8) 0.0251(2) Uani 1 1 d . . .
O1 O 0.9208(5) 0.4312(4) 0.1932(6) 0.0349(13) Uani 1 1 d . . .
O2 O 0.7322(5) 0.2868(4) 0.1220(5) 0.0280(11) Uani 1 1 d . . .
O3 O 0.8777(6) 0.1524(4) 0.2675(5) 0.0283(11) Uani 1 1 d . . .
O4 O 0.8067(6) 0.0083(4) 0.0789(5) 0.0336(12) Uani 1 1 d . . .
O5 O 0.4231(5) 0.6303(4) 0.0970(5) 0.0328(12) Uani 1 1 d . . .
O6 O 0.4161(6) 0.5937(4) -0.1678(5) 0.0326(12) Uani 1 1 d . . .
O7 O 1.1689(5) -0.1547(4) 0.5846(6) 0.0331(12) Uani 1 1 d . . .
O8 O 0.9033(5) -0.1915(4) 0.5767(5) 0.0340(12) Uani 1 1 d . . .
O9 O 1.0496(6) 0.2595(5) 0.1517(6) 0.0411(14) Uani 1 1 d . . .
O10 O 0.8486(6) 0.1799(5) -0.0483(6) 0.0408(14) Uani 1 1 d . . .
O11 O 1.4436(14) -0.1852(12) 0.6215(18) 0.073(5) Uani 0.50 1 d PD A 1
H11 H 1.3635 -0.1689 0.6104 0.088 Uiso 0.50 1 calc PR A 1
O12 O 1.2204(12) 0.4178(8) 0.1615(12) 0.036(3) Uani 0.50 1 d PD B 1
H12 H 1.1556 0.3820 0.1608 0.044 Uiso 0.50 1 calc PR B 1
O11A O 1.3786(17) -0.3723(13) 0.5558(14) 0.073(5) Uani 0.50 1 d PD C 2
H11D H 1.3918 -0.3906 0.6354 0.088 Uiso 0.50 1 calc PR C 2
O12A O 1.1628(12) 0.5207(8) 0.2193(14) 0.041(3) Uani 0.50 1 d PD D 2
H12A H 1.0959 0.4936 0.2311 0.050 Uiso 0.50 1 calc PR D 2
C1 C 0.8534(9) 0.5879(6) 0.1220(9) 0.041(2) Uani 1 1 d . . .
H1A H 0.9513 0.5968 0.1607 0.062 Uiso 1 1 calc R . .
H1B H 0.8078 0.6280 0.1707 0.062 Uiso 1 1 calc R . .
H1C H 0.8233 0.6063 0.0265 0.062 Uiso 1 1 calc R . .
C2 C 0.8191(7) 0.4837(5) 0.1344(7) 0.0255(14) Uani 1 1 d . . .
C3 C 0.6820(7) 0.4525(5) 0.0851(7) 0.0244(14) Uani 1 1 d . . .
C4 C 0.6452(7) 0.3571(5) 0.0847(7) 0.0243(14) Uani 1 1 d . . .
C5 C 0.4997(7) 0.3259(5) 0.0344(8) 0.0313(17) Uani 1 1 d . . .
H5A H 0.4948 0.2560 0.0420 0.047 Uiso 1 1 calc R . .
H5B H 0.4589 0.3449 -0.0603 0.047 Uiso 1 1 calc R . .
H5C H 0.4507 0.3565 0.0888 0.047 Uiso 1 1 calc R . .
C6 C 0.5873(8) 0.4958(6) -0.1973(8) 0.0326(17) Uani 1 1 d . . .
H6A H 0.5386 0.5132 -0.2912 0.049 Uiso 1 1 calc R . .
H6B H 0.5869 0.4258 -0.1874 0.049 Uiso 1 1 calc R . .
H6C H 0.6808 0.5186 -0.1725 0.049 Uiso 1 1 calc R . .
C7 C 0.5189(8) 0.5416(5) -0.1056(7) 0.0273(15) Uani 1 1 d . . .
C8 C 0.5725(7) 0.5256(5) 0.0329(7) 0.0248(14) Uani 1 1 d . . .
C9 C 0.5237(8) 0.5738(5) 0.1277(7) 0.0280(16) Uani 1 1 d . . .
C10 C 0.5949(9) 0.5600(7) 0.2769(8) 0.040(2) Uani 1 1 d . . .
H10A H 0.5491 0.5976 0.3280 0.060 Uiso 1 1 calc R . .
H10B H 0.6889 0.5815 0.2999 0.060 Uiso 1 1 calc R . .
H10C H 0.5931 0.4918 0.2996 0.060 Uiso 1 1 calc R . .
C11 C 0.8783(8) -0.1477(6) 0.1471(9) 0.040(2) Uani 1 1 d . . .
H11A H 0.8388 -0.1569 0.0493 0.061 Uiso 1 1 calc R . .
H11B H 0.8311 -0.1885 0.1935 0.061 Uiso 1 1 calc R . .
H11C H 0.9742 -0.1651 0.1762 0.061 Uiso 1 1 calc R . .
C12 C 0.8643(7) -0.0452(5) 0.1809(7) 0.0270(15) Uani 1 1 d . . .
C13 C 0.9145(7) -0.0132(5) 0.3186(7) 0.0247(14) Uani 1 1 d . . .
C14 C 0.9148(7) 0.0835(5) 0.3541(7) 0.0234(14) Uani 1 1 d . . .
C15 C 0.9652(8) 0.1136(5) 0.4999(8) 0.0331(17) Uani 1 1 d . . .
H15A H 0.9584 0.1835 0.5059 0.050 Uiso 1 1 calc R . .
H15B H 1.0598 0.0940 0.5404 0.050 Uiso 1 1 calc R . .
H15C H 0.9105 0.0828 0.5483 0.050 Uiso 1 1 calc R . .
C16 C 0.7222(8) -0.1195(7) 0.4049(9) 0.041(2) Uani 1 1 d . . .
H16A H 0.6709 -0.1570 0.4507 0.061 Uiso 1 1 calc R . .
H16B H 0.6995 -0.1413 0.3112 0.061 Uiso 1 1 calc R . .
H16C H 0.6994 -0.0514 0.4063 0.061 Uiso 1 1 calc R . .
C17 C 0.8718(7) -0.1332(5) 0.4767(7) 0.0267(16) Uani 1 1 d . . .
C18 C 0.9666(7) -0.0858(5) 0.4284(7) 0.0249(14) Uani 1 1 d . . .
C19 C 1.1059(8) -0.1018(5) 0.4807(8) 0.0284(16) Uani 1 1 d . . .
C20 C 1.1973(8) -0.0560(6) 0.4117(8) 0.0358(18) Uani 1 1 d . . .
H20A H 1.2913 -0.0737 0.4598 0.054 Uiso 1 1 calc R . .
H20B H 1.1878 0.0140 0.4126 0.054 Uiso 1 1 calc R . .
H20C H 1.1718 -0.0786 0.3182 0.054 Uiso 1 1 calc R . .
C21 C 0.7949(10) 0.2486(7) -0.1551(10) 0.047(2) Uani 1 1 d . . .
H21A H 0.6998 0.2339 -0.2032 0.070 Uiso 1 1 calc R . .
H21B H 0.8463 0.2454 -0.2183 0.070 Uiso 1 1 calc R . .
H21C H 0.8022 0.3133 -0.1166 0.070 Uiso 1 1 calc R . .
C22 C 1.1545(10) 0.1900(7) 0.2052(10) 0.048(2) Uani 1 1 d . . .
H22A H 1.1971 0.2009 0.3023 0.072 Uiso 1 1 calc R . .
H22B H 1.2224 0.1964 0.1598 0.072 Uiso 1 1 calc R . .
H22C H 1.1157 0.1253 0.1902 0.072 Uiso 1 1 calc R . .
C23 C 1.4445(18) -0.2788(11) 0.5574(18) 0.104(6) Uani 0.50 1 d PD A 1
H23A H 1.3520 -0.2964 0.5034 0.155 Uiso 0.50 1 calc PR A 1
H23B H 1.4816 -0.3275 0.6272 0.155 Uiso 0.50 1 calc PR A 1
H23C H 1.5005 -0.2750 0.4987 0.155 Uiso 0.50 1 calc PR A 1
C24 C 1.250(3) 0.483(2) 0.275(3) 0.039(5) Uani 0.50 1 d PD B 1
H24A H 1.2478 0.5491 0.2427 0.059 Uiso 0.50 1 calc PR B 1
H24B H 1.3393 0.4685 0.3389 0.059 Uiso 0.50 1 calc PR B 1
H24C H 1.1816 0.4751 0.3198 0.059 Uiso 0.50 1 calc PR B 1
C23A C 1.4445(18) -0.2788(11) 0.5574(18) 0.104(6) Uani 0.50 1 d PD C 2
H23D H 1.5319 -0.2885 0.5438 0.155 Uiso 0.50 1 calc PR C 2
H23E H 1.4586 -0.2474 0.6446 0.155 Uiso 0.50 1 calc PR C 2
H23F H 1.3870 -0.2383 0.4848 0.155 Uiso 0.50 1 calc PR C 2
C24A C 1.274(3) 0.454(2) 0.249(3) 0.039(5) Uani 0.50 1 d PD D 2
H24D H 1.3533 0.4821 0.3166 0.059 Uiso 0.50 1 calc PR D 2
H24E H 1.2954 0.4409 0.1660 0.059 Uiso 0.50 1 calc PR D 2
H24F H 1.2491 0.3942 0.2834 0.059 Uiso 0.50 1 calc PR D 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
Zn1 O8 1.992(5) 2_756 ?
Zn1 O7 2.035(6) 2_756 ?
Zn1 O1 2.046(6) . ?
Zn1 O3 2.085(5) . ?
Zn1 O2 2.102(5) . ?
Zn1 O9 2.275(6) . ?
Zn2 O5 1.995(5) 2_645 ?
Zn2 O6 2.034(6) 2_645 ?
Zn2 O4 2.046(5) . ?
Zn2 O2 2.081(5) . ?
Zn2 O3 2.098(5) . ?
Zn2 O10 2.267(6) . ?
O1 C2 1.273(9) . ?
O2 C4 1.307(8) . ?
O3 C14 1.290(9) . ?
O4 C12 1.281(9) . ?
O5 C9 1.269(9) . ?
O5 Zn2 1.995(5) 2_655 ?
O6 C7 1.285(9) . ?
O6 Zn2 2.034(6) 2_655 ?
O7 C19 1.302(9) . ?
O7 Zn1 2.035(6) 2_746 ?
O8 C17 1.280(9) . ?
O8 Zn1 1.992(5) 2_746 ?
O9 C22 1.434(10) . ?
O10 C21 1.440(10) . ?
O11 C23 1.468(16) . ?
O12 C24 1.445(16) . ?
O12A C24A 1.441(16) . ?
C1 C2 1.510(11) . ?
C2 C3 1.426(10) . ?
C3 C4 1.382(10) . ?
C3 C8 1.497(9) . ?
C4 C5 1.504(10) . ?
C6 C7 1.513(11) . ?
C7 C8 1.393(10) . ?
C8 C9 1.424(10) . ?
C9 C10 1.508(10) . ?
C11 C12 1.488(10) . ?
C12 C13 1.435(10) . ?
C13 C14 1.397(10) . ?
C13 C18 1.495(10) . ?
C14 C15 1.503(10) . ?
C16 C17 1.512(10) . ?
C17 C18 1.416(10) . ?
C18 C19 1.398(10) . ?
C19 C20 1.515(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
O8 Zn1 O7 88.2(2) 2_756 2_756 ?
O8 Zn1 O1 97.5(2) 2_756 . ?
O7 Zn1 O1 95.7(2) 2_756 . ?
O8 Zn1 O3 103.1(2) 2_756 . ?
O7 Zn1 O3 102.7(2) 2_756 . ?
O1 Zn1 O3 152.6(2) . . ?
O8 Zn1 O2 178.1(2) 2_756 . ?
O7 Zn1 O2 93.7(2) 2_756 . ?
O1 Zn1 O2 82.9(2) . . ?
O3 Zn1 O2 75.9(2) . . ?
O8 Zn1 O9 82.1(2) 2_756 . ?
O7 Zn1 O9 169.6(2) 2_756 . ?
O1 Zn1 O9 82.2(2) . . ?
O3 Zn1 O9 83.0(2) . . ?
O2 Zn1 O9 96.1(2) . . ?
O5 Zn2 O6 87.9(2) 2_645 2_645 ?
O5 Zn2 O4 97.1(2) 2_645 . ?
O6 Zn2 O4 95.6(2) 2_645 . ?
O5 Zn2 O2 103.3(2) 2_645 . ?
O6 Zn2 O2 102.9(2) 2_645 . ?
O4 Zn2 O2 152.7(2) . . ?
O5 Zn2 O3 178.1(2) 2_645 . ?
O6 Zn2 O3 93.9(2) 2_645 . ?
O4 Zn2 O3 82.9(2) . . ?
O2 Zn2 O3 76.1(2) . . ?
O5 Zn2 O10 82.1(2) 2_645 . ?
O6 Zn2 O10 169.5(2) 2_645 . ?
O4 Zn2 O10 82.2(2) . . ?
O2 Zn2 O10 82.9(2) . . ?
O3 Zn2 O10 96.0(2) . . ?
C2 O1 Zn1 126.7(5) . . ?
C4 O2 Zn2 133.6(4) . . ?
C4 O2 Zn1 123.2(5) . . ?
Zn2 O2 Zn1 102.3(2) . . ?
C14 O3 Zn1 133.0(5) . . ?
C14 O3 Zn2 123.7(5) . . ?
Zn1 O3 Zn2 102.3(2) . . ?
C12 O4 Zn2 126.7(5) . . ?
C9 O5 Zn2 126.4(5) . 2_655 ?
C7 O6 Zn2 123.5(5) . 2_655 ?
C19 O7 Zn1 123.1(5) . 2_746 ?
C17 O8 Zn1 126.2(5) . 2_746 ?
C22 O9 Zn1 118.0(5) . . ?
C21 O10 Zn2 118.3(5) . . ?
O1 C2 C3 125.8(7) . . ?
O1 C2 C1 114.1(6) . . ?
C3 C2 C1 120.1(7) . . ?
C4 C3 C2 122.8(7) . . ?
C4 C3 C8 118.2(6) . . ?
C2 C3 C8 119.0(6) . . ?
O2 C4 C3 123.5(6) . . ?
O2 C4 C5 114.5(6) . . ?
C3 C4 C5 121.9(6) . . ?
O6 C7 C8 127.2(7) . . ?
O6 C7 C6 114.1(6) . . ?
C8 C7 C6 118.7(6) . . ?
C7 C8 C9 122.5(6) . . ?
C7 C8 C3 119.3(6) . . ?
C9 C8 C3 118.2(6) . . ?
O5 C9 C8 124.9(6) . . ?
O5 C9 C10 115.5(6) . . ?
C8 C9 C10 119.6(6) . . ?
O4 C12 C13 125.1(7) . . ?
O4 C12 C11 114.5(7) . . ?
C13 C12 C11 120.3(7) . . ?
C14 C13 C12 122.4(7) . . ?
C14 C13 C18 118.6(6) . . ?
C12 C13 C18 119.0(6) . . ?
O3 C14 C13 123.8(6) . . ?
O3 C14 C15 115.6(6) . . ?
C13 C14 C15 120.6(6) . . ?
O8 C17 C18 124.4(6) . . ?
O8 C17 C16 115.8(7) . . ?
C18 C17 C16 119.7(6) . . ?
C19 C18 C17 123.3(6) . . ?
C19 C18 C13 118.8(6) . . ?
C17 C18 C13 117.9(6) . . ?
O7 C19 C18 126.7(7) . . ?
O7 C19 C20 114.2(6) . . ?
C18 C19 C20 119.1(7) . . ?

_diffrn_measured_fraction_theta_max 0.995
_diffrn_reflns_theta_full        26.50
_diffrn_measured_fraction_theta_full 0.995
_refine_diff_density_max         2.533
_refine_diff_density_min         -1.113
_refine_diff_density_rms         0.162
#===END

data_compound_4_bath162
_database_code_depnum_ccdc_archive 'CCDC 688577'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C21 H32 O11 Zn2'
_chemical_formula_weight         591.21

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'
Zn Zn 0.2839 1.4301 '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

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

_cell_length_a                   7.539(4)
_cell_length_b                   13.843(8)
_cell_length_c                   12.155(7)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.190(9)
_cell_angle_gamma                90.00
_cell_volume                     1268.5(12)
_cell_formula_units_Z            2
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    306
_cell_measurement_theta_min      3.633
_cell_measurement_theta_max      18.605

_exptl_crystal_description       Block
_exptl_crystal_colour            Colourless
_exptl_crystal_size_max          0.03
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.01
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.548
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             612
_exptl_absorpt_coefficient_mu    1.945
_exptl_absorpt_correction_type   Multi-Scan
_exptl_absorpt_correction_T_min  0.93
_exptl_absorpt_correction_T_max  0.99
_exptl_absorpt_process_details   
;
?
;

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.8460
_diffrn_radiation_type           Synchrotron
_diffrn_radiation_source         'Daresbury SRS station 16.2 SMX'
_diffrn_radiation_monochromator  'Silicon 111'
_diffrn_measurement_device_type  'Bruker APEXII diffractometer'
_diffrn_measurement_method       'ω rotation with narrow frames'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            3924
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.2212
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       0
_diffrn_reflns_theta_min         4.36
_diffrn_reflns_theta_max         31.18
_reflns_number_total             3924
_reflns_number_gt                2142
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'local programs'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'Bruker SHELXTL'
_computing_structure_refinement  'Bruker SHELXTL'
_computing_molecular_graphics    'ORTEX (P.McArdle, 1995)'
_computing_publication_material  'SHELXL-97/2 (Sheldrick,1997)'

_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.

The refinement only convered satisfactorily once 23% twinning
about the reciprocal 0 0 1 direction was accounted for in the model.
Oxygen bond hydrogens in the solvent could no be reliably located
and hence were omitted from the final least squares. The disordered
water fragments were treated isotropically, and some ligand atoms
were refined subject to restraints on their ADPs.
;

_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)+(0.0851P)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       0.021(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.12(5)
_refine_ls_number_reflns         3924
_refine_ls_number_parameters     317
_refine_ls_number_restraints     79
_refine_ls_R_factor_all          0.1663
_refine_ls_R_factor_gt           0.0872
_refine_ls_wR_factor_ref         0.2006
_refine_ls_wR_factor_gt          0.1646
_refine_ls_goodness_of_fit_ref   0.973
_refine_ls_restrained_S_all      0.965
_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
Zn1 Zn 0.6907(3) 0.50776(13) 0.83977(18) 0.0343(7) Uani 1 1 d . . .
Zn2 Zn 0.6223(4) 0.67013(13) 0.65958(19) 0.0354(7) Uani 1 1 d . . .
O1 O 0.5935(18) 0.6510(8) 0.8257(10) 0.032(3) Uani 1 1 d . . .
O2 O 0.730(2) 0.7987(9) 0.7032(10) 0.041(4) Uani 1 1 d . . .
O3 O 0.563(2) 0.9633(9) 1.1344(10) 0.039(4) Uani 1 1 d . . .
O4 O 0.2657(17) 0.9948(10) 0.9991(10) 0.036(4) Uani 1 1 d . . .
O5 O 0.787(2) 0.3774(9) 0.7976(11) 0.044(4) Uani 1 1 d . . .
O6 O 0.6516(16) 0.5224(10) 0.6704(10) 0.032(3) Uani 1 1 d U . .
O7 O 0.3121(18) 0.1892(9) 0.4975(9) 0.036(3) Uani 1 1 d . . .
O8 O 0.6297(18) 0.1984(8) 0.3769(10) 0.037(4) Uani 1 1 d . . .
O9 O 0.9318(18) 0.5798(8) 0.8167(11) 0.040(4) Uani 1 1 d . . .
O10 O 1.212(2) 0.5283(9) 0.7072(10) 0.054(4) Uani 1 1 d . . .
O11A O 1.025(5) 0.535(2) 0.488(3) 0.070(10) Uiso 0.50 1 d P A 2
O11B O 0.911(4) 0.5479(19) 0.407(2) 0.045(7) Uiso 0.50 1 d P B 1
C1 C 0.473(3) 0.6849(12) 0.9988(15) 0.046(6) Uani 1 1 d . . .
H1A H 0.4588 0.6146 0.9966 0.069 Uiso 1 1 calc R . .
H1B H 0.3576 0.7154 1.0111 0.069 Uiso 1 1 calc R . .
H1C H 0.5543 0.7024 1.0587 0.069 Uiso 1 1 calc R . .
C2 C 0.545(3) 0.7179(14) 0.8957(16) 0.033(5) Uani 1 1 d U . .
C3 C 0.574(3) 0.8189(13) 0.8731(15) 0.029(5) Uani 1 1 d U . .
C4 C 0.680(3) 0.8500(14) 0.7830(16) 0.034(5) Uani 1 1 d U . .
C5 C 0.730(3) 0.9596(13) 0.7732(16) 0.047(7) Uani 1 1 d . . .
H5A H 0.8149 0.9683 0.7134 0.071 Uiso 1 1 calc R . .
H5B H 0.7825 0.9817 0.8425 0.071 Uiso 1 1 calc R . .
H5C H 0.6224 0.9974 0.7576 0.071 Uiso 1 1 calc R . .
C6 C 0.803(3) 0.8724(17) 1.0595(19) 0.051(7) Uani 1 1 d . . .
H6A H 0.8640 0.9060 1.1194 0.076 Uiso 1 1 calc R . .
H6B H 0.8641 0.8848 0.9900 0.076 Uiso 1 1 calc R . .
H6C H 0.8019 0.8028 1.0742 0.076 Uiso 1 1 calc R . .
C7 C 0.610(3) 0.9094(15) 1.0512(17) 0.034(6) Uani 1 1 d U . .
C8 C 0.514(2) 0.8917(13) 0.9545(14) 0.024(4) Uani 1 1 d U . .
C9 C 0.345(3) 0.9355(13) 0.9377(15) 0.023(5) Uani 1 1 d U . .
C10 C 0.248(4) 0.9152(15) 0.8306(18) 0.057(7) Uani 1 1 d . . .
H10A H 0.1263 0.8954 0.8465 0.085 Uiso 1 1 calc R . .
H10B H 0.3092 0.8633 0.7909 0.085 Uiso 1 1 calc R . .
H10C H 0.2469 0.9737 0.7853 0.085 Uiso 1 1 calc R . .
C11 C 0.776(3) 0.2150(13) 0.7308(16) 0.043(6) Uani 1 1 d . . .
H11A H 0.8801 0.2063 0.7779 0.064 Uiso 1 1 calc R . .
H11B H 0.7986 0.1871 0.6581 0.064 Uiso 1 1 calc R . .
H11C H 0.6735 0.1826 0.7641 0.064 Uiso 1 1 calc R . .
C12 C 0.737(3) 0.3208(13) 0.7189(15) 0.030(5) Uani 1 1 d U . .
C13 C 0.643(3) 0.3547(15) 0.6216(17) 0.039(6) Uani 1 1 d U . .
C14 C 0.604(3) 0.4519(13) 0.6019(14) 0.027(4) Uani 1 1 d U . .
C15 C 0.518(3) 0.4776(13) 0.4954(16) 0.041(6) Uani 1 1 d . . .
H15A H 0.3961 0.4532 0.4942 0.062 Uiso 1 1 calc R . .
H15B H 0.5850 0.4486 0.4348 0.062 Uiso 1 1 calc R . .
H15C H 0.5169 0.5480 0.4869 0.062 Uiso 1 1 calc R . .
C16 C 0.303(3) 0.2719(15) 0.6661(19) 0.047(6) Uani 1 1 d . . .
H16A H 0.2752 0.3410 0.6671 0.071 Uiso 1 1 calc R . .
H16B H 0.3779 0.2560 0.7296 0.071 Uiso 1 1 calc R . .
H16C H 0.1928 0.2345 0.6697 0.071 Uiso 1 1 calc R . .
C17 C 0.399(3) 0.2477(14) 0.5627(16) 0.027(5) Uani 1 1 d U . .
C18 C 0.570(3) 0.2818(13) 0.5443(15) 0.031(5) Uani 1 1 d U . .
C19 C 0.669(3) 0.2542(14) 0.4547(16) 0.027(5) Uani 1 1 d U . .
C20 C 0.863(3) 0.2907(18) 0.4483(17) 0.056(8) Uani 1 1 d . . .
H20A H 0.9411 0.2370 0.4279 0.084 Uiso 1 1 calc R . .
H20B H 0.8994 0.3162 0.5202 0.084 Uiso 1 1 calc R . .
H20C H 0.8717 0.3418 0.3929 0.084 Uiso 1 1 calc R . .
C21 C 1.009(3) 0.6466(15) 0.8918(18) 0.057(7) Uani 1 1 d . . .
H21A H 0.9274 0.7010 0.9026 0.086 Uiso 1 1 calc R . .
H21B H 1.1211 0.6703 0.8621 0.086 Uiso 1 1 calc R . .
H21C H 1.0301 0.6144 0.9624 0.086 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
Zn1 O4 1.993(13) 2_647 ?
Zn1 O5 2.012(14) . ?
Zn1 O3 2.031(16) 2_647 ?
Zn1 O6 2.088(13) . ?
Zn1 O9 2.093(13) . ?
Zn1 O1 2.121(12) . ?
Zn2 O8 1.988(14) 2_656 ?
Zn2 O7 1.991(11) 2_656 ?
Zn2 O2 2.025(13) . ?
Zn2 O1 2.048(12) . ?
Zn2 O6 2.061(14) . ?
O1 C2 1.31(2) . ?
O2 C4 1.26(2) . ?
O3 C7 1.31(2) . ?
O3 Zn1 2.031(16) 2_657 ?
O4 C9 1.26(2) . ?
O4 Zn1 1.993(13) 2_657 ?
O5 C12 1.29(2) . ?
O6 C14 1.33(2) . ?
O7 C17 1.31(2) . ?
O7 Zn2 1.991(11) 2_646 ?
O8 C19 1.26(2) . ?
O8 Zn2 1.988(14) 2_646 ?
O9 C21 1.42(2) . ?
C1 C2 1.44(3) . ?
C2 C3 1.44(2) . ?
C3 C4 1.42(3) . ?
C3 C8 1.48(2) . ?
C4 C5 1.57(3) . ?
C6 C7 1.54(3) . ?
C7 C8 1.40(3) . ?
C8 C9 1.42(3) . ?
C9 C10 1.52(3) . ?
C11 C12 1.50(2) . ?
C12 C13 1.45(3) . ?
C13 C14 1.40(3) . ?
C13 C18 1.48(3) . ?
C14 C15 1.49(3) . ?
C16 C17 1.49(3) . ?
C17 C18 1.39(3) . ?
C18 C19 1.37(3) . ?
C19 C20 1.55(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
O4 Zn1 O5 96.4(6) 2_647 . ?
O4 Zn1 O3 88.5(5) 2_647 2_647 ?
O5 Zn1 O3 96.2(6) . 2_647 ?
O4 Zn1 O6 178.5(6) 2_647 . ?
O5 Zn1 O6 83.4(5) . . ?
O3 Zn1 O6 93.0(5) 2_647 . ?
O4 Zn1 O9 91.9(5) 2_647 . ?
O5 Zn1 O9 94.6(5) . . ?
O3 Zn1 O9 169.2(5) 2_647 . ?
O6 Zn1 O9 86.6(5) . . ?
O4 Zn1 O1 102.7(5) 2_647 . ?
O5 Zn1 O1 160.5(5) . . ?
O3 Zn1 O1 88.3(5) 2_647 . ?
O6 Zn1 O1 77.4(5) . . ?
O9 Zn1 O1 81.0(5) . . ?
O8 Zn2 O7 90.0(6) 2_656 2_656 ?
O8 Zn2 O2 105.5(6) 2_656 . ?
O7 Zn2 O2 92.0(5) 2_656 . ?
O8 Zn2 O1 98.1(5) 2_656 . ?
O7 Zn2 O1 171.7(6) 2_656 . ?
O2 Zn2 O1 84.2(5) . . ?
O8 Zn2 O6 108.1(5) 2_656 . ?
O7 Zn2 O6 99.5(5) 2_656 . ?
O2 Zn2 O6 144.3(6) . . ?
O1 Zn2 O6 79.7(5) . . ?
C2 O1 Zn2 125.4(11) . . ?
C2 O1 Zn1 134.9(12) . . ?
Zn2 O1 Zn1 99.4(5) . . ?
C4 O2 Zn2 125.1(13) . . ?
C7 O3 Zn1 123.5(13) . 2_657 ?
C9 O4 Zn1 124.2(13) . 2_657 ?
C12 O5 Zn1 128.9(13) . . ?
C14 O6 Zn2 131.1(11) . . ?
C14 O6 Zn1 125.7(11) . . ?
Zn2 O6 Zn1 100.0(6) . . ?
C17 O7 Zn2 122.5(13) . 2_646 ?
C19 O8 Zn2 120.6(12) . 2_646 ?
C21 O9 Zn1 125.2(12) . . ?
O1 C2 C1 116.6(17) . . ?
O1 C2 C3 121.2(16) . . ?
C1 C2 C3 122.0(17) . . ?
C4 C3 C2 121.7(17) . . ?
C4 C3 C8 118.7(16) . . ?
C2 C3 C8 119.0(16) . . ?
O2 C4 C3 126.3(18) . . ?
O2 C4 C5 114.5(17) . . ?
C3 C4 C5 119.1(17) . . ?
O3 C7 C8 128(2) . . ?
O3 C7 C6 113.5(18) . . ?
C8 C7 C6 118.6(18) . . ?
C7 C8 C9 120.2(17) . . ?
C7 C8 C3 121.5(18) . . ?
C9 C8 C3 117.9(16) . . ?
O4 C9 C8 128.2(17) . . ?
O4 C9 C10 113.5(18) . . ?
C8 C9 C10 118.2(17) . . ?
O5 C12 C13 123.2(17) . . ?
O5 C12 C11 117.6(18) . . ?
C13 C12 C11 119.2(18) . . ?
C14 C13 C12 123.5(19) . . ?
C14 C13 C18 117.9(19) . . ?
C12 C13 C18 118.3(18) . . ?
O6 C14 C13 122.7(17) . . ?
O6 C14 C15 119.0(15) . . ?
C13 C14 C15 118.1(17) . . ?
O7 C17 C18 125.2(18) . . ?
O7 C17 C16 113.9(18) . . ?
C18 C17 C16 120.8(18) . . ?
C19 C18 C17 122.4(18) . . ?
C19 C18 C13 119.5(19) . . ?
C17 C18 C13 118.1(18) . . ?
O8 C19 C18 130.0(19) . . ?
O8 C19 C20 112.4(16) . . ?
C18 C19 C20 117.4(18) . . ?

_diffrn_measured_fraction_theta_max 0.974
_diffrn_reflns_theta_full        31.18
_diffrn_measured_fraction_theta_full 0.974
_refine_diff_density_max         0.913
_refine_diff_density_min         -0.905
_refine_diff_density_rms         0.139

