# Supplementary Material (ESI) for Chemical Communications
# This journal is (c) The Royal Society of Chemistry 2009

data_global

_journal_coden_Cambridge         182

loop_
_publ_author_name
'Praveen Thallapally'
'Jerry L Atwood'
'Scott J. Dalgarno'
'Carlos A. Fernandez'
'Motkuri Radha Kishan'
'Jun Liu.'
'Peter B McGrail'
'Jian Tian'
'John E. Warren'

_publ_contact_author_name        'Praveen Thallapally'
_publ_contact_author_email       PRAVEEN.THALLAPALLY@PNL.GOV

_publ_section_title              
;
Flexible Metal-Organic Supramolecular Isomers for Gas Separation
;

# Attachment '2_4.CIF'

data_2
_database_code_depnum_ccdc_archive 'CCDC 740053'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C45 H52 N4 O17 Zn2'
_chemical_formula_weight         1051.65

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'
Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Triclinic
_symmetry_space_group_name_H-M   P-1

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

_cell_length_a                   6.9314(14)
_cell_length_b                   12.382(2)
_cell_length_c                   27.738(5)
_cell_angle_alpha                96.641(3)
_cell_angle_beta                 91.231(2)
_cell_angle_gamma                104.221(2)
_cell_volume                     2289.2(8)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       Prism
_exptl_crystal_colour            Colourless
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.07
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.526
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1092
_exptl_absorpt_coefficient_mu    1.127
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.8956
_exptl_absorpt_correction_T_max  0.9253
_exptl_absorpt_process_details   SADABS-2004/1(Bruker-Nonius-2004)

_exptl_special_details           
;
Data were corrected for decay and absorption using the program SADABS
based on the method of R.H. Blessing (Acta Cryst. A51, 33-38, 1995).
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.67100
_diffrn_radiation_type           synchrotron
_diffrn_radiation_source         synchrotron
_diffrn_radiation_monochromator  'silicon 111'
_diffrn_measurement_device_type  'Apex II CCD camera on D8 diffractometer'
_diffrn_measurement_method       'omega rotation'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         .
_diffrn_standards_interval_count .
_diffrn_standards_interval_time  .
_diffrn_standards_decay_%        .
_diffrn_reflns_number            15438
_diffrn_reflns_av_R_equivalents  0.0387
_diffrn_reflns_av_sigmaI/netI    0.0529
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_theta_min         1.68
_diffrn_reflns_theta_max         22.15
_reflns_number_total             6694
_reflns_number_gt                5770
_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 F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ 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/[\s^2^(Fo^2^)+(0.0002P)^2^+66.2228P] where P=(Fo^2^+2Fc^2^)/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         6694
_refine_ls_number_parameters     621
_refine_ls_number_restraints     110
_refine_ls_R_factor_all          0.1198
_refine_ls_R_factor_gt           0.1088
_refine_ls_wR_factor_ref         0.2671
_refine_ls_wR_factor_gt          0.2619
_refine_ls_goodness_of_fit_ref   1.156
_refine_ls_restrained_S_all      1.154
_refine_ls_shift/su_max          0.028
_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 0.70347(17) 0.57231(10) 0.50363(4) 0.0141(3) Uani 1 1 d . . .
Zn2 Zn 0.9889(2) 1.36483(12) 0.00899(5) 0.0310(4) Uani 1 1 d . . .
O1 O 0.9865(11) 0.6560(7) 0.5079(3) 0.0293(19) Uani 1 1 d . . .
O2 O 0.5739(12) 0.6463(9) 0.4556(4) 0.049(3) Uani 1 1 d . . .
O3 O 0.2674(12) 0.5432(8) 0.4519(4) 0.044(3) Uani 1 1 d . . .
O4 O 0.2062(11) 0.8873(6) 0.3028(3) 0.0258(18) Uani 1 1 d . . .
O5 O -0.2043(11) 1.0483(6) 0.2932(3) 0.0233(17) Uani 1 1 d . . .
O6 O -0.2720(14) 1.4540(8) 0.4475(4) 0.050(3) Uani 1 1 d . . .
O7 O -0.5807(12) 1.3500(8) 0.4418(3) 0.041(2) Uani 1 1 d . . .
O8 O -0.1338(10) 0.8192(6) 0.1768(3) 0.0215(17) Uani 1 1 d . . .
O9 O -0.7317(12) 0.4470(7) 0.0326(3) 0.036(2) Uani 1 1 d . . .
O10 O -0.9194(12) 0.5667(7) 0.0493(3) 0.032(2) Uani 1 1 d . . .
O11 O 0.1677(11) 1.0569(6) 0.1846(3) 0.0221(17) Uani 1 1 d . . .
O12 O 0.9543(13) 1.2832(8) 0.0821(3) 0.039(2) Uani 1 1 d . . .
O13 O 0.7217(12) 1.3228(7) 0.0379(3) 0.033(2) Uani 1 1 d . . .
O14 O 1.0335(18) 1.2244(8) -0.0266(3) 0.052(3) Uani 1 1 d U . .
O50 O 1.064(6) 1.305(2) 0.2338(12) 0.258(12) Uani 1 1 d U . .
O51 O -0.374(2) 1.6570(11) 0.2554(6) 0.103(5) Uani 1 1 d DU . .
O52 O 1.1554(19) 0.8630(9) 0.5005(5) 0.071(4) Uani 1 1 d . . .
N1 N 1.217(2) 1.1020(10) -0.0413(5) 0.059(3) Uani 1 1 d U . .
N2 N 1.119(7) 1.489(3) 0.2190(14) 0.244(11) Uani 1 1 d DU . .
N3 N -0.424(4) 1.4747(16) 0.2708(7) 0.107(5) Uani 1 1 d U . .
N4 N 1.1448(18) 0.9940(10) 0.4496(5) 0.049(3) Uani 1 1 d . . .
C1 C 0.3982(16) 0.6216(10) 0.4394(4) 0.022(3) Uani 1 1 d . . .
C2 C 0.3431(16) 0.6901(9) 0.4034(4) 0.023(3) Uani 1 1 d . . .
C3 C 0.1467(16) 0.6725(9) 0.3862(4) 0.023(3) Uani 1 1 d . . .
H3 H 0.0461 0.6157 0.3976 0.027 Uiso 1 1 calc R . .
C4 C 0.0950(16) 0.7365(9) 0.3523(4) 0.022(2) Uani 1 1 d . . .
H4 H -0.0401 0.7243 0.3412 0.027 Uiso 1 1 calc R . .
C5 C 0.2400(17) 0.8171(10) 0.3353(4) 0.026(3) Uani 1 1 d . . .
C6 C 0.4383(17) 0.8349(10) 0.3519(5) 0.032(3) Uani 1 1 d . . .
H6 H 0.5392 0.8905 0.3398 0.038 Uiso 1 1 calc R . .
C7 C 0.4873(17) 0.7728(11) 0.3854(5) 0.034(3) Uani 1 1 d . . .
H7 H 0.6224 0.7861 0.3967 0.041 Uiso 1 1 calc R . .
C8 C 0.0133(16) 0.8623(9) 0.2780(4) 0.020(2) Uani 1 1 d . . .
H8A H -0.0914 0.8601 0.3018 0.024 Uiso 1 1 calc R . .
H8B H -0.0136 0.7880 0.2580 0.024 Uiso 1 1 calc R . .
C9 C 0.0119(15) 0.9527(8) 0.2460(4) 0.015(2) Uani 1 1 d . . .
C10 C -0.0086(15) 1.0623(8) 0.2763(4) 0.016(2) Uani 1 1 d . . .
H10A H 0.0895 1.0819 0.3044 0.019 Uiso 1 1 calc R . .
H10B H 0.0201 1.1246 0.2561 0.019 Uiso 1 1 calc R . .
C11 C -0.2395(16) 1.1364(9) 0.3237(4) 0.020(2) Uani 1 1 d . . .
C12 C -0.4379(17) 1.1238(10) 0.3353(4) 0.025(3) Uani 1 1 d . . .
H12 H -0.5381 1.0617 0.3200 0.030 Uiso 1 1 calc R . .
C13 C -0.4878(17) 1.2017(10) 0.3689(4) 0.028(3) Uani 1 1 d . . .
H13 H -0.6228 1.1917 0.3772 0.033 Uiso 1 1 calc R . .
C14 C -0.3476(16) 1.2933(10) 0.3907(4) 0.022(2) Uani 1 1 d . . .
C15 C -0.1491(18) 1.3070(9) 0.3773(4) 0.027(3) Uani 1 1 d . . .
H15 H -0.0498 1.3709 0.3914 0.032 Uiso 1 1 calc R . .
C16 C -0.0975(17) 1.2291(9) 0.3442(4) 0.025(3) Uani 1 1 d . . .
H16 H 0.0369 1.2393 0.3355 0.030 Uiso 1 1 calc R . .
C17 C -0.4022(17) 1.3741(10) 0.4296(4) 0.023(3) Uani 1 1 d . . .
C18 C -0.1760(15) 0.9084(9) 0.2099(4) 0.015(2) Uani 1 1 d . . .
H18A H -0.2963 0.8797 0.2278 0.018 Uiso 1 1 calc R . .
H18B H -0.1985 0.9692 0.1920 0.018 Uiso 1 1 calc R . .
C19 C -0.2904(17) 0.7535(9) 0.1472(4) 0.025(2) Uani 1 1 d U . .
C20 C -0.2522(17) 0.6602(9) 0.1203(4) 0.024(2) Uani 1 1 d U . .
H20 H -0.1249 0.6448 0.1227 0.029 Uiso 1 1 calc R . .
C21 C -0.4045(17) 0.5898(10) 0.0897(4) 0.023(2) Uani 1 1 d U . .
H21 H -0.3824 0.5234 0.0725 0.028 Uiso 1 1 calc R . .
C22 C -0.5840(17) 0.6134(10) 0.0839(4) 0.028(2) Uani 1 1 d U . .
C23 C -0.6177(19) 0.7110(11) 0.1105(5) 0.039(3) Uani 1 1 d U . .
H23 H -0.7428 0.7286 0.1069 0.046 Uiso 1 1 calc R . .
C24 C -0.4683(18) 0.7814(11) 0.1418(5) 0.034(3) Uani 1 1 d U . .
H24 H -0.4893 0.8479 0.1592 0.041 Uiso 1 1 calc R . .
C25 C -0.7550(18) 0.5373(11) 0.0527(4) 0.031(3) Uani 1 1 d . . .
C26 C 0.1992(15) 0.9820(9) 0.2185(4) 0.016(2) Uani 1 1 d . . .
H26A H 0.3147 1.0192 0.2412 0.020 Uiso 1 1 calc R . .
H26B H 0.2257 0.9133 0.2009 0.020 Uiso 1 1 calc R . .
C27 C 0.3289(16) 1.1156(9) 0.1620(4) 0.020(2) Uani 1 1 d . . .
C28 C 0.5210(17) 1.1085(10) 0.1691(4) 0.024(3) Uani 1 1 d . . .
H28 H 0.5530 1.0645 0.1925 0.028 Uiso 1 1 calc R . .
C29 C 0.6689(16) 1.1661(10) 0.1419(4) 0.025(3) Uani 1 1 d . . .
H29 H 0.8025 1.1615 0.1469 0.030 Uiso 1 1 calc R . .
C30 C 0.6236(16) 1.2300(9) 0.1075(4) 0.021(2) Uani 1 1 d . . .
C31 C 0.4276(16) 1.2404(10) 0.1023(4) 0.025(3) Uani 1 1 d . . .
H31 H 0.3952 1.2858 0.0796 0.030 Uiso 1 1 calc R . .
C32 C 0.2824(17) 1.1853(10) 0.1300(4) 0.025(3) Uani 1 1 d . . .
H32 H 0.1508 1.1946 0.1272 0.031 Uiso 1 1 calc R . .
C33 C 0.7778(17) 1.2815(10) 0.0742(4) 0.026(3) Uani 1 1 d . . .
C34 C 1.191(3) 1.2001(11) -0.0230(5) 0.047(3) Uani 1 1 d U . .
H34 H 1.3013 1.2540 -0.0064 0.057 Uiso 1 1 calc R . .
C35 C 1.051(3) 1.0177(13) -0.0676(6) 0.073(5) Uani 1 1 d U . .
H35A H 1.0450 0.9444 -0.0568 0.110 Uiso 1 1 calc R . .
H35B H 1.0720 1.0134 -0.1026 0.110 Uiso 1 1 calc R . .
H35C H 0.9264 1.0389 -0.0611 0.110 Uiso 1 1 calc R . .
C36 C 1.422(4) 1.0802(18) -0.0388(8) 0.099(6) Uani 1 1 d U . .
H36A H 1.5157 1.1451 -0.0205 0.149 Uiso 1 1 calc R . .
H36B H 1.4672 1.0681 -0.0718 0.149 Uiso 1 1 calc R . .
H36C H 1.4169 1.0134 -0.0227 0.149 Uiso 1 1 calc R . .
C50 C 1.148(8) 1.581(3) 0.1987(17) 0.255(14) Uani 1 1 d U . .
H50A H 1.2752 1.5934 0.1830 0.383 Uiso 1 1 calc R . .
H50B H 1.1495 1.6441 0.2235 0.383 Uiso 1 1 calc R . .
H50C H 1.0395 1.5735 0.1743 0.383 Uiso 1 1 calc R . .
C51 C 1.120(9) 1.495(4) 0.2765(19) 0.268(14) Uani 1 1 d U . .
H51A H 0.9833 1.4839 0.2870 0.402 Uiso 1 1 calc R . .
H51B H 1.2000 1.5687 0.2912 0.402 Uiso 1 1 calc R . .
H51C H 1.1780 1.4362 0.2869 0.402 Uiso 1 1 calc R . .
C52 C 1.088(9) 1.379(3) 0.2040(17) 0.250(11) Uani 1 1 d DU . .
H52 H 1.0842 1.3553 0.1701 0.301 Uiso 1 1 calc R . .
C53 C -0.428(5) 1.357(2) 0.2526(10) 0.125(8) Uani 1 1 d U . .
H53A H -0.5599 1.3090 0.2566 0.187 Uiso 1 1 calc R . .
H53B H -0.3271 1.3334 0.2711 0.187 Uiso 1 1 calc R . .
H53C H -0.3990 1.3521 0.2181 0.187 Uiso 1 1 calc R . .
C54 C -0.420(4) 1.503(2) 0.3223(8) 0.108(7) Uani 1 1 d U . .
H54A H -0.3984 1.5844 0.3301 0.162 Uiso 1 1 calc R . .
H54B H -0.3110 1.4789 0.3374 0.162 Uiso 1 1 calc R . .
H54C H -0.5468 1.4649 0.3346 0.162 Uiso 1 1 calc R . .
C55 C -0.393(4) 1.5564(16) 0.2391(9) 0.107(6) Uani 1 1 d DU . .
H55 H -0.3857 1.5356 0.2052 0.128 Uiso 1 1 calc R . .
C56 C 1.037(3) 1.0210(17) 0.4095(7) 0.074(5) Uani 1 1 d . . .
H56A H 0.9240 0.9574 0.3984 0.111 Uiso 1 1 calc R . .
H56B H 1.1261 1.0367 0.3828 0.111 Uiso 1 1 calc R . .
H56C H 0.9882 1.0874 0.4201 0.111 Uiso 1 1 calc R . .
C57 C 1.334(3) 1.0702(16) 0.4718(8) 0.089(7) Uani 1 1 d . . .
H57A H 1.3598 1.0510 0.5042 0.133 Uiso 1 1 calc R . .
H57B H 1.3237 1.1481 0.4744 0.133 Uiso 1 1 calc R . .
H57C H 1.4443 1.0616 0.4513 0.133 Uiso 1 1 calc R . .
C58 C 1.079(3) 0.8948(14) 0.4675(6) 0.058(4) Uani 1 1 d . . .
H58 H 0.9604 0.8456 0.4524 0.070 Uiso 1 1 calc R . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Zn1 0.0116(6) 0.0113(6) 0.0196(7) 0.0034(5) 0.0011(5) 0.0025(5)
Zn2 0.0219(8) 0.0366(9) 0.0225(8) -0.0044(6) 0.0039(6) -0.0121(6)
O1 0.017(4) 0.026(4) 0.044(5) -0.001(4) -0.001(4) 0.005(3)
O2 0.020(5) 0.064(7) 0.068(7) 0.050(6) -0.010(4) 0.002(4)
O3 0.019(4) 0.044(6) 0.072(7) 0.044(5) -0.007(4) -0.006(4)
O4 0.020(4) 0.025(4) 0.030(5) 0.016(4) -0.008(3) -0.003(3)
O5 0.022(4) 0.022(4) 0.023(4) -0.006(3) -0.001(3) 0.005(3)
O6 0.035(5) 0.039(6) 0.059(7) -0.034(5) 0.013(5) -0.009(5)
O7 0.024(5) 0.043(6) 0.042(5) -0.029(4) 0.010(4) -0.001(4)
O8 0.014(4) 0.019(4) 0.027(4) -0.009(3) -0.008(3) 0.001(3)
O9 0.029(5) 0.039(5) 0.025(5) -0.008(4) 0.002(4) -0.015(4)
O10 0.017(4) 0.048(6) 0.020(4) -0.004(4) 0.002(3) -0.011(4)
O11 0.018(4) 0.032(4) 0.019(4) 0.016(3) 0.004(3) 0.006(3)
O12 0.026(5) 0.055(6) 0.040(5) 0.023(5) 0.012(4) 0.008(4)
O13 0.027(5) 0.047(5) 0.025(5) 0.013(4) -0.001(4) 0.006(4)
O14 0.079(7) 0.028(5) 0.031(5) -0.009(4) 0.014(5) -0.014(5)
O50 0.40(3) 0.163(18) 0.24(2) 0.129(17) 0.02(2) 0.08(2)
O51 0.124(11) 0.054(8) 0.111(11) 0.015(8) 0.038(9) -0.020(8)
O52 0.084(9) 0.045(7) 0.082(9) 0.028(6) -0.013(7) 0.002(6)
N1 0.101(8) 0.034(5) 0.040(6) 0.001(5) -0.018(6) 0.014(6)
N2 0.37(3) 0.156(17) 0.24(2) 0.128(17) -0.01(2) 0.09(2)
N3 0.155(12) 0.076(9) 0.079(9) 0.003(7) 0.015(9) 0.009(9)
N4 0.044(7) 0.045(8) 0.049(8) -0.001(6) 0.000(6) -0.005(6)
C1 0.013(6) 0.033(7) 0.025(6) 0.005(5) 0.005(5) 0.015(5)
C2 0.020(6) 0.023(6) 0.027(6) 0.011(5) 0.005(5) 0.002(5)
C3 0.011(5) 0.026(6) 0.031(7) 0.012(5) 0.007(5) 0.002(5)
C4 0.016(6) 0.025(6) 0.027(6) 0.011(5) 0.000(5) 0.003(5)
C5 0.024(6) 0.038(7) 0.020(6) 0.010(5) 0.000(5) 0.010(5)
C6 0.015(6) 0.037(7) 0.040(7) 0.028(6) -0.007(5) -0.009(5)
C7 0.013(6) 0.046(8) 0.044(8) 0.019(6) -0.005(5) 0.002(5)
C8 0.017(6) 0.020(6) 0.023(6) 0.003(5) -0.009(5) 0.002(4)
C9 0.012(5) 0.016(5) 0.014(5) 0.002(4) -0.006(4) -0.004(4)
C10 0.014(5) 0.015(5) 0.015(5) 0.001(4) 0.005(4) -0.004(4)
C11 0.021(6) 0.021(6) 0.019(6) -0.005(5) -0.005(5) 0.010(5)
C12 0.018(6) 0.027(6) 0.023(6) -0.004(5) 0.003(5) -0.005(5)
C13 0.018(6) 0.035(7) 0.031(7) -0.005(6) 0.005(5) 0.012(5)
C14 0.015(6) 0.028(6) 0.020(6) -0.003(5) -0.002(5) 0.005(5)
C15 0.028(6) 0.015(6) 0.033(7) -0.007(5) -0.001(5) 0.002(5)
C16 0.020(6) 0.026(6) 0.027(6) -0.004(5) 0.008(5) 0.005(5)
C17 0.026(7) 0.030(7) 0.017(6) 0.002(5) -0.006(5) 0.014(5)
C18 0.011(5) 0.018(5) 0.014(5) -0.004(4) -0.004(4) 0.004(4)
C19 0.023(5) 0.022(5) 0.023(5) -0.011(4) -0.005(4) 0.001(4)
C20 0.027(5) 0.021(5) 0.023(5) -0.002(4) 0.000(4) 0.006(4)
C21 0.026(5) 0.024(5) 0.018(5) -0.002(4) 0.004(4) 0.004(4)
C22 0.024(5) 0.030(5) 0.023(5) -0.009(4) 0.000(4) -0.002(4)
C23 0.026(5) 0.039(6) 0.043(6) -0.020(5) -0.008(5) 0.006(5)
C24 0.029(5) 0.030(5) 0.036(5) -0.025(5) -0.008(5) 0.007(4)
C25 0.026(7) 0.035(8) 0.017(6) -0.011(5) 0.003(5) -0.013(6)
C26 0.014(5) 0.017(5) 0.016(5) 0.000(4) -0.003(4) 0.002(4)
C27 0.020(6) 0.020(6) 0.019(6) 0.003(5) 0.004(5) 0.004(5)
C28 0.028(6) 0.030(6) 0.018(6) 0.010(5) 0.004(5) 0.014(5)
C29 0.012(5) 0.029(7) 0.034(7) 0.007(5) 0.009(5) 0.004(5)
C30 0.021(6) 0.021(6) 0.022(6) 0.008(5) 0.003(5) 0.003(5)
C31 0.020(6) 0.032(7) 0.027(6) 0.014(5) 0.002(5) 0.010(5)
C32 0.021(6) 0.029(7) 0.025(6) 0.003(5) -0.002(5) 0.003(5)
C33 0.023(7) 0.024(6) 0.027(7) 0.004(5) 0.006(5) -0.005(5)
C34 0.088(8) 0.020(5) 0.026(5) 0.005(4) -0.009(6) -0.002(6)
C35 0.121(13) 0.034(8) 0.054(9) 0.001(7) -0.008(10) 0.002(9)
C36 0.144(15) 0.074(11) 0.085(12) -0.010(10) -0.055(12) 0.053(11)
C50 0.38(3) 0.17(2) 0.25(3) 0.14(2) 0.00(3) 0.08(2)
C51 0.38(3) 0.20(2) 0.25(3) 0.11(2) -0.01(3) 0.07(3)
C52 0.38(3) 0.160(17) 0.24(2) 0.122(17) 0.00(2) 0.09(2)
C53 0.176(18) 0.082(13) 0.106(15) -0.003(12) -0.018(15) 0.023(14)
C54 0.165(17) 0.085(13) 0.070(12) 0.015(11) 0.007(13) 0.022(13)
C55 0.147(12) 0.076(10) 0.085(10) 0.011(8) 0.023(10) 0.003(10)
C56 0.079(13) 0.089(14) 0.055(11) 0.025(10) -0.001(10) 0.016(11)
C57 0.091(15) 0.061(12) 0.100(16) 0.037(11) -0.018(13) -0.018(11)
C58 0.062(11) 0.044(10) 0.062(11) 0.005(8) -0.003(9) 0.002(8)

_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 O1 1.974(8) . ?
Zn1 O2 2.013(8) . ?
Zn1 O7 2.016(8) 2_576 ?
Zn1 O3 2.037(8) 2_666 ?
Zn1 O6 2.051(8) 1_645 ?
Zn1 Zn1 2.935(2) 2_666 ?
Zn2 O14 1.993(10) . ?
Zn2 O13 2.008(8) . ?
Zn2 O9 2.010(8) 1_765 ?
Zn2 O10 2.013(9) 2_575 ?
Zn2 O12 2.359(9) . ?
Zn2 C33 2.507(11) . ?
Zn2 C25 2.574(11) 1_765 ?
O2 C1 1.241(14) . ?
O3 C1 1.242(14) . ?
O3 Zn1 2.037(8) 2_666 ?
O4 C5 1.376(14) . ?
O4 C8 1.437(12) . ?
O5 C11 1.376(13) . ?
O5 C10 1.421(12) . ?
O6 C17 1.211(14) . ?
O6 Zn1 2.051(8) 1_465 ?
O7 C17 1.263(14) . ?
O7 Zn1 2.016(8) 2_576 ?
O8 C19 1.374(13) . ?
O8 C18 1.443(12) . ?
O9 C25 1.239(15) . ?
O9 Zn2 2.010(8) 1_345 ?
O10 C25 1.284(16) . ?
O10 Zn2 2.013(9) 2_575 ?
O11 C27 1.381(13) . ?
O11 C26 1.443(12) . ?
O12 C33 1.232(15) . ?
O13 C33 1.276(14) . ?
O14 C34 1.209(19) . ?
O50 C52 1.29(4) . ?
O51 C55 1.249(16) . ?
O52 C58 1.201(19) . ?
N1 C34 1.317(19) . ?
N1 C35 1.46(2) . ?
N1 C36 1.51(3) . ?
N2 C50 1.30(4) . ?
N2 C52 1.34(2) . ?
N2 C51 1.59(5) . ?
N3 C55 1.40(3) . ?
N3 C54 1.43(3) . ?
N3 C53 1.47(3) . ?
N4 C58 1.36(2) . ?
N4 C56 1.44(2) . ?
N4 C57 1.49(2) . ?
C1 C2 1.484(16) . ?
C2 C3 1.390(16) . ?
C2 C7 1.390(16) . ?
C3 C4 1.391(16) . ?
C4 C5 1.366(16) . ?
C5 C6 1.397(16) . ?
C6 C7 1.360(17) . ?
C8 C9 1.509(14) . ?
C9 C26 1.507(14) . ?
C9 C10 1.551(14) . ?
C9 C18 1.570(13) . ?
C11 C16 1.370(16) . ?
C11 C12 1.394(16) . ?
C12 C13 1.375(16) . ?
C13 C14 1.368(16) . ?
C14 C15 1.408(16) . ?
C14 C17 1.503(16) . ?
C15 C16 1.372(16) . ?
C19 C24 1.370(17) . ?
C19 C20 1.385(16) . ?
C20 C21 1.390(16) . ?
C21 C22 1.357(17) . ?
C22 C23 1.413(17) . ?
C22 C25 1.504(16) . ?
C23 C24 1.389(17) . ?
C25 Zn2 2.574(11) 1_345 ?
C27 C28 1.367(16) . ?
C27 C32 1.393(16) . ?
C28 C29 1.388(16) . ?
C29 C30 1.385(16) . ?
C30 C31 1.402(16) . ?
C30 C33 1.499(15) . ?
C31 C32 1.372(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
O1 Zn1 O2 104.2(4) . . ?
O1 Zn1 O7 104.5(3) . 2_576 ?
O2 Zn1 O7 89.6(4) . 2_576 ?
O1 Zn1 O3 96.9(3) . 2_666 ?
O2 Zn1 O3 158.6(4) . 2_666 ?
O7 Zn1 O3 88.6(4) 2_576 2_666 ?
O1 Zn1 O6 96.1(3) . 1_645 ?
O2 Zn1 O6 88.2(5) . 1_645 ?
O7 Zn1 O6 159.1(4) 2_576 1_645 ?
O3 Zn1 O6 86.0(5) 2_666 1_645 ?
O1 Zn1 Zn1 174.4(2) . 2_666 ?
O2 Zn1 Zn1 79.6(3) . 2_666 ?
O7 Zn1 Zn1 79.4(2) 2_576 2_666 ?
O3 Zn1 Zn1 79.0(2) 2_666 2_666 ?
O6 Zn1 Zn1 79.8(3) 1_645 2_666 ?
O14 Zn2 O13 106.7(4) . . ?
O14 Zn2 O9 101.3(4) . 1_765 ?
O13 Zn2 O9 136.8(3) . 1_765 ?
O14 Zn2 O10 97.5(4) . 2_575 ?
O13 Zn2 O10 100.8(3) . 2_575 ?
O9 Zn2 O10 107.4(3) 1_765 2_575 ?
O14 Zn2 O12 90.9(4) . . ?
O13 Zn2 O12 59.4(3) . . ?
O9 Zn2 O12 88.4(3) 1_765 . ?
O10 Zn2 O12 160.1(3) 2_575 . ?
O14 Zn2 C33 99.1(4) . . ?
O13 Zn2 C33 30.3(4) . . ?
O9 Zn2 C33 113.8(4) 1_765 . ?
O10 Zn2 C33 131.1(4) 2_575 . ?
O12 Zn2 C33 29.1(3) . . ?
O14 Zn2 C25 129.2(5) . 1_765 ?
O13 Zn2 C25 116.9(4) . 1_765 ?
O9 Zn2 C25 28.1(4) 1_765 1_765 ?
O10 Zn2 C25 98.5(4) 2_575 1_765 ?
O12 Zn2 C25 89.9(4) . 1_765 ?
C33 Zn2 C25 105.5(4) . 1_765 ?
C1 O2 Zn1 129.1(8) . . ?
C1 O3 Zn1 128.6(7) . 2_666 ?
C5 O4 C8 118.4(8) . . ?
C11 O5 C10 116.7(8) . . ?
C17 O6 Zn1 127.0(8) . 1_465 ?
C17 O7 Zn1 128.0(7) . 2_576 ?
C19 O8 C18 116.7(8) . . ?
C25 O9 Zn2 102.2(8) . 1_345 ?
C25 O10 Zn2 120.8(7) . 2_575 ?
C27 O11 C26 119.1(8) . . ?
C33 O12 Zn2 82.1(7) . . ?
C33 O13 Zn2 97.0(7) . . ?
C34 O14 Zn2 121.6(10) . . ?
C34 N1 C35 119.9(16) . . ?
C34 N1 C36 119.9(15) . . ?
C35 N1 C36 120.0(15) . . ?
C50 N2 C52 137(4) . . ?
C50 N2 C51 120(4) . . ?
C52 N2 C51 104(3) . . ?
C55 N3 C54 122.1(19) . . ?
C55 N3 C53 120(2) . . ?
C54 N3 C53 117(2) . . ?
C58 N4 C56 120.4(14) . . ?
C58 N4 C57 117.3(14) . . ?
C56 N4 C57 122.2(14) . . ?
O2 C1 O3 123.4(11) . . ?
O2 C1 C2 117.8(10) . . ?
O3 C1 C2 118.8(10) . . ?
C3 C2 C7 118.1(10) . . ?
C3 C2 C1 121.1(10) . . ?
C7 C2 C1 120.8(10) . . ?
C2 C3 C4 121.1(10) . . ?
C5 C4 C3 119.5(10) . . ?
C4 C5 O4 124.6(10) . . ?
C4 C5 C6 120.0(10) . . ?
O4 C5 C6 115.3(10) . . ?
C7 C6 C5 120.1(11) . . ?
C6 C7 C2 121.2(11) . . ?
O4 C8 C9 108.2(8) . . ?
C26 C9 C8 112.6(9) . . ?
C26 C9 C10 107.3(8) . . ?
C8 C9 C10 111.1(9) . . ?
C26 C9 C18 110.7(8) . . ?
C8 C9 C18 107.0(8) . . ?
C10 C9 C18 108.1(8) . . ?
O5 C10 C9 110.4(8) . . ?
C16 C11 O5 125.6(10) . . ?
C16 C11 C12 119.7(10) . . ?
O5 C11 C12 114.6(10) . . ?
C13 C12 C11 119.6(10) . . ?
C14 C13 C12 121.6(11) . . ?
C13 C14 C15 118.1(10) . . ?
C13 C14 C17 121.0(10) . . ?
C15 C14 C17 120.9(10) . . ?
C16 C15 C14 120.7(11) . . ?
C11 C16 C15 120.2(11) . . ?
O6 C17 O7 125.7(11) . . ?
O6 C17 C14 118.0(11) . . ?
O7 C17 C14 116.2(10) . . ?
O8 C18 C9 106.0(8) . . ?
C24 C19 O8 122.8(10) . . ?
C24 C19 C20 121.6(10) . . ?
O8 C19 C20 115.4(10) . . ?
C19 C20 C21 118.5(11) . . ?
C22 C21 C20 121.6(11) . . ?
C21 C22 C23 119.0(11) . . ?
C21 C22 C25 123.3(11) . . ?
C23 C22 C25 117.7(11) . . ?
C24 C23 C22 120.2(12) . . ?
C19 C24 C23 119.0(11) . . ?
O9 C25 O10 123.2(11) . . ?
O9 C25 C22 118.0(12) . . ?
O10 C25 C22 118.8(11) . . ?
O9 C25 Zn2 49.7(6) . 1_345 ?
O10 C25 Zn2 74.0(6) . 1_345 ?
C22 C25 Zn2 164.1(10) . 1_345 ?
O11 C26 C9 107.0(8) . . ?
C28 C27 O11 124.8(10) . . ?
C28 C27 C32 120.6(10) . . ?
O11 C27 C32 114.6(10) . . ?
C27 C28 C29 119.6(10) . . ?
C30 C29 C28 120.7(10) . . ?
C29 C30 C31 118.9(10) . . ?
C29 C30 C33 120.8(10) . . ?
C31 C30 C33 120.2(10) . . ?
C32 C31 C30 120.3(10) . . ?
C31 C32 C27 119.7(11) . . ?
O12 C33 O13 121.4(11) . . ?
O12 C33 C30 120.2(11) . . ?
O13 C33 C30 118.5(10) . . ?
O12 C33 Zn2 68.8(6) . . ?
O13 C33 Zn2 52.7(6) . . ?
C30 C33 Zn2 170.7(9) . . ?
O14 C34 N1 122.7(15) . . ?
O50 C52 N2 123(4) . . ?
O51 C55 N3 120(2) . . ?
O52 C58 N4 126.5(16) . . ?

_diffrn_measured_fraction_theta_max 0.986
_diffrn_reflns_theta_full        22.15
_diffrn_measured_fraction_theta_full 0.986
_refine_diff_density_max         1.775
_refine_diff_density_min         -1.130
_refine_diff_density_rms         0.176

##############END##################

data_3
_database_code_depnum_ccdc_archive 'CCDC 740054'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            3
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C36 H32 N O13 Zn2'
_chemical_formula_weight         817.37

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'
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   C2/c

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

_cell_length_a                   32.084(6)
_cell_length_b                   12.458(2)
_cell_length_c                   30.972(6)
_cell_angle_alpha                90.00
_cell_angle_beta                 116.899(5)
_cell_angle_gamma                90.00
_cell_volume                     11040(4)
_cell_formula_units_Z            8
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       Prism
_exptl_crystal_colour            Colourless
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.18
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    0.984
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             3352
_exptl_absorpt_coefficient_mu    0.913
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.8352
_exptl_absorpt_correction_T_max  0.9476
_exptl_absorpt_process_details   Bruker-SADABS

_exptl_special_details           
;
Data were corrected for decay and absorption using the program SADABS
based on the method of R.H. Blessing (Acta Cryst. A51, 33-38, 1995).
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.77490
_diffrn_radiation_type           synchrotron
_diffrn_radiation_source         'Advanced Light Source station 11.3.1'
_diffrn_radiation_monochromator  'silicon 111'
_diffrn_measurement_device_type  'Bruker Apex II CCD Diffractometer'
_diffrn_measurement_method       '\w 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            38062
_diffrn_reflns_av_R_equivalents  0.0481
_diffrn_reflns_av_sigmaI/netI    0.0714
_diffrn_reflns_limit_h_min       -41
_diffrn_reflns_limit_h_max       40
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -39
_diffrn_reflns_limit_l_max       39
_diffrn_reflns_theta_min         1.42
_diffrn_reflns_theta_max         27.17
_reflns_number_total             12122
_reflns_number_gt                7106
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Apex II'
_computing_cell_refinement       'SAINT (Bruker, 1998)'
_computing_data_reduction        'SAINT (Bruker, 1998)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'XSeed (Barbour, 2001)'
_computing_publication_material  'local program'

_refine_special_details          
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger. Restraints have been
applied to a dimethylformamide ligand on one Zn centre due to disorder.
These atoms have also been refined isotropically. The routine SQUEEZE was
applied to the data to remove diffuse electron density associated with
DMF molecules of crystallisation that were badly disordered and that
could not be modelled. This dramatically improved the agreement indices.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[\s^2^(Fo^2^)+(0.0921P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/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         12122
_refine_ls_number_parameters     479
_refine_ls_number_restraints     32
_refine_ls_R_factor_all          0.0844
_refine_ls_R_factor_gt           0.0515
_refine_ls_wR_factor_ref         0.1491
_refine_ls_wR_factor_gt          0.1377
_refine_ls_goodness_of_fit_ref   0.897
_refine_ls_restrained_S_all      0.915
_refine_ls_shift/su_max          0.003
_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 0.154048(13) 0.56650(3) 0.171792(13) 0.03026(12) Uani 1 1 d . . .
Zn2 Zn 0.156473(14) 0.36019(3) 0.243779(13) 0.03378(12) Uani 1 1 d . . .
O2 O 0.15261(10) 0.2592(2) 0.29011(10) 0.0552(7) Uani 1 1 d D . .
O3 O -0.28032(8) 1.03940(19) 0.21960(9) 0.0452(6) Uani 1 1 d . . .
O4 O 0.12645(9) 0.62596(19) 0.21147(9) 0.0469(6) Uani 1 1 d . . .
O5 O -0.06275(8) 0.97009(17) 0.32835(8) 0.0362(5) Uani 1 1 d . . .
O6 O 0.13860(10) 0.57987(19) 0.64505(9) 0.0540(7) Uani 1 1 d . . .
O7 O 0.12360(9) 0.71569(18) 0.68237(8) 0.0412(6) Uani 1 1 d . . .
O8 O 0.07158(8) 1.0718(2) 0.42738(8) 0.0448(6) Uani 1 1 d . . .
O9 O 0.09186(12) 1.3727(3) 0.60242(11) 0.0773(10) Uani 1 1 d . . .
O10 O 0.03990(8) 0.89722(19) 0.46878(7) 0.0384(6) Uani 1 1 d . . .
O11 O 0.11810(10) 0.4758(2) 0.24682(10) 0.0564(7) Uani 1 1 d . . .
O12 O 0.16517(11) 1.3328(2) 0.62662(9) 0.0561(7) Uani 1 1 d . . .
O13 O -0.27910(8) 0.8914(2) 0.26193(9) 0.0477(6) Uani 1 1 d . . .
O19 O 0.03000(9) 0.79437(18) 0.33858(8) 0.0424(6) Uani 1 1 d . . .
N305 N 0.1383(5) 0.2358(11) 0.3559(5) 0.141(4) Uiso 0.50 1 d PDU A 1
C1 C 0.11332(13) 0.5756(3) 0.23868(13) 0.0408(8) Uani 1 1 d . . .
C2 C 0.08979(13) 0.6369(3) 0.26308(12) 0.0373(8) Uani 1 1 d . . .
C3 C 0.08510(13) 0.7477(3) 0.25899(12) 0.0380(8) Uani 1 1 d . . .
H3 H 0.0961 0.7853 0.2395 0.046 Uiso 1 1 calc R . .
C4 C 0.06455(12) 0.8046(3) 0.28298(12) 0.0371(8) Uani 1 1 d . . .
H4 H 0.0608 0.8802 0.2795 0.044 Uiso 1 1 calc R A .
C5 C 0.04960(12) 0.7484(3) 0.31214(11) 0.0350(8) Uani 1 1 d . . .
C6 C 0.05331(16) 0.6372(3) 0.31626(15) 0.0543(11) Uani 1 1 d . . .
H6 H 0.0419 0.5993 0.3354 0.065 Uiso 1 1 calc R A .
C7 C 0.07409(15) 0.5826(3) 0.29181(14) 0.0526(11) Uani 1 1 d . . .
H7 H 0.0775 0.5069 0.2949 0.063 Uiso 1 1 calc R . .
C8 C 0.03271(13) 0.9081(3) 0.34539(12) 0.0359(8) Uani 1 1 d . . .
H8A H 0.0120 0.9452 0.3149 0.043 Uiso 1 1 calc R . .
H8B H 0.0651 0.9336 0.3561 0.043 Uiso 1 1 calc R . .
C9 C 0.01686(11) 0.9295(2) 0.38446(11) 0.0311(7) Uani 1 1 d . . .
C10 C -0.25942(12) 0.9646(3) 0.24839(12) 0.0387(8) Uani 1 1 d . . .
C11 C -0.20770(12) 0.9620(3) 0.26947(12) 0.0362(8) Uani 1 1 d . . .
C12 C -0.18104(12) 0.8847(3) 0.30346(12) 0.0399(8) Uani 1 1 d . . .
H12 H -0.1965 0.8312 0.3128 0.048 Uiso 1 1 calc R . .
C13 C -0.13316(12) 0.8843(3) 0.32368(12) 0.0357(8) Uani 1 1 d . . .
H13 H -0.1158 0.8314 0.3470 0.043 Uiso 1 1 calc R . .
C14 C -0.11032(11) 0.9606(3) 0.31013(11) 0.0322(7) Uani 1 1 d . . .
C15 C -0.13612(12) 1.0393(3) 0.27547(13) 0.0411(8) Uani 1 1 d . . .
H15 H -0.1206 1.0923 0.2660 0.049 Uiso 1 1 calc R . .
C16 C -0.18444(12) 1.0382(3) 0.25547(13) 0.0418(9) Uani 1 1 d . . .
H16 H -0.2020 1.0902 0.2318 0.050 Uiso 1 1 calc R . .
C17 C 0.12331(16) 1.3261(3) 0.59703(15) 0.0479(9) Uani 1 1 d . . .
C18 C 0.10959(15) 1.2570(3) 0.55145(14) 0.0479(10) Uani 1 1 d . . .
C19 C 0.14127(15) 1.1928(4) 0.54559(16) 0.0629(12) Uani 1 1 d . . .
H19 H 0.1727 1.1907 0.5702 0.075 Uiso 1 1 calc R . .
C20 C 0.12797(15) 1.1295(4) 0.50358(16) 0.0644(12) Uani 1 1 d . . .
H20 H 0.1499 1.0839 0.4999 0.077 Uiso 1 1 calc R . .
C21 C 0.08255(13) 1.1357(3) 0.46816(12) 0.0406(8) Uani 1 1 d . . .
C22 C 0.05138(15) 1.2020(3) 0.47423(15) 0.0589(11) Uani 1 1 d . . .
H22 H 0.0201 1.2067 0.4494 0.071 Uiso 1 1 calc R . .
C23 C 0.06479(17) 1.2611(4) 0.51545(16) 0.0652(12) Uani 1 1 d . . .
H23 H 0.0426 1.3058 0.5191 0.078 Uiso 1 1 calc R . .
C24 C 0.12200(12) 0.6713(3) 0.64521(12) 0.0341(8) Uani 1 1 d . . .
C26 C 0.09760(15) 0.6824(3) 0.55666(13) 0.0527(11) Uani 1 1 d . . .
H26 H 0.1087 0.6112 0.5581 0.063 Uiso 1 1 calc R . .
C27 C 0.07893(15) 0.7367(3) 0.51327(13) 0.0528(11) Uani 1 1 d . . .
H27 H 0.0779 0.7036 0.4852 0.063 Uiso 1 1 calc R . .
C28 C 0.06165(12) 0.8398(3) 0.51062(12) 0.0346(8) Uani 1 1 d . . .
C29 C 0.06487(13) 0.8887(3) 0.55211(12) 0.0403(9) Uani 1 1 d . . .
H29 H 0.0538 0.9600 0.5506 0.048 Uiso 1 1 calc R . .
C30 C 0.08402(13) 0.8343(3) 0.59567(12) 0.0404(9) Uani 1 1 d . . .
H30 H 0.0859 0.8684 0.6239 0.048 Uiso 1 1 calc R . .
C31 C 0.04583(12) 0.8592(3) 0.42768(11) 0.0362(8) Uani 1 1 d . . .
H31A H 0.0354 0.7836 0.4205 0.043 Uiso 1 1 calc R . .
H31B H 0.0792 0.8628 0.4350 0.043 Uiso 1 1 calc R . .
C32 C 0.02274(12) 1.0493(3) 0.39775(12) 0.0372(8) Uani 1 1 d . . .
H32A H 0.0107 1.0934 0.3680 0.045 Uiso 1 1 calc R . .
H32B H 0.0048 1.0675 0.4157 0.045 Uiso 1 1 calc R . .
C33 C -0.03446(11) 0.8987(3) 0.36663(11) 0.0331(7) Uani 1 1 d . . .
H33A H -0.0396 0.8237 0.3547 0.040 Uiso 1 1 calc R . .
H33B H -0.0430 0.9041 0.3935 0.040 Uiso 1 1 calc R . .
C304 C 0.1616(4) 0.2896(9) 0.3322(3) 0.064(3) Uiso 0.50 1 d PDU A 1
H30A H 0.1540 0.3670 0.3307 0.077 Uiso 0.50 1 calc PR A 1
H30B H 0.1957 0.2823 0.3528 0.077 Uiso 0.50 1 calc PR A 1
C306 C 0.1407(8) 0.1296(14) 0.3402(8) 0.195(8) Uiso 0.50 1 d PDU A 1
H30C H 0.1436 0.1325 0.3101 0.292 Uiso 0.50 1 calc PR A 1
H30D H 0.1123 0.0903 0.3347 0.292 Uiso 0.50 1 calc PR A 1
H30E H 0.1680 0.0928 0.3652 0.292 Uiso 0.50 1 calc PR A 1
C100 C 0.10046(12) 0.7309(3) 0.59860(12) 0.0339(8) Uani 1 1 d . . .
C300 C 0.1707(4) 0.2503(11) 0.3332(3) 0.085(3) Uiso 0.50 1 d PDU A 2
H30F H 0.1971 0.3013 0.3429 0.102 Uiso 0.50 1 calc PR A 2
H30G H 0.1853 0.1785 0.3376 0.102 Uiso 0.50 1 calc PR A 2
C308 C 0.1473(6) 0.2731(14) 0.4046(5) 0.140(5) Uiso 0.50 1 d PDU A 1
H30H H 0.1622 0.2155 0.4281 0.210 Uiso 0.50 1 calc PR A 1
H30I H 0.1177 0.2930 0.4044 0.210 Uiso 0.50 1 calc PR A 1
H30J H 0.1680 0.3357 0.4135 0.210 Uiso 0.50 1 calc PR A 1
C302 C 0.1965(6) 0.2466(15) 0.4240(5) 0.061(4) Uiso 0.25 1 d PDU A 2
H30K H 0.2274 0.2365 0.4254 0.092 Uiso 0.25 1 calc PR A 2
H30L H 0.1892 0.1849 0.4389 0.092 Uiso 0.25 1 calc PR A 2
H30M H 0.1965 0.3122 0.4414 0.092 Uiso 0.25 1 calc PR A 2
N301 N 0.1610(5) 0.2558(12) 0.3729(4) 0.151(4) Uiso 0.50 1 d PDU A 2
C303 C 0.1750(7) 0.3222(13) 0.4140(6) 0.056(4) Uiso 0.25 1 d PDU A 2
H30N H 0.1820 0.3943 0.4063 0.083 Uiso 0.25 1 calc PR A 2
H30O H 0.2030 0.2920 0.4407 0.083 Uiso 0.25 1 calc PR A 2
H30P H 0.1497 0.3265 0.4234 0.083 Uiso 0.25 1 calc PR A 2
C309 C 0.1679(12) 0.170(2) 0.4065(10) 0.132(7) Uiso 0.25 1 d PDU A 2
H30Q H 0.1659 0.1013 0.3906 0.198 Uiso 0.25 1 calc PR A 2
H30R H 0.1436 0.1739 0.4174 0.198 Uiso 0.25 1 calc PR A 2
H30S H 0.1987 0.1777 0.4344 0.198 Uiso 0.25 1 calc PR A 2
C310 C 0.1258(8) 0.174(2) 0.3536(10) 0.103(6) Uiso 0.25 1 d PDU A 2
H31C H 0.1061 0.1867 0.3191 0.155 Uiso 0.25 1 calc PR A 2
H31D H 0.1064 0.1754 0.3707 0.155 Uiso 0.25 1 calc PR A 2
H31E H 0.1408 0.1033 0.3581 0.155 Uiso 0.25 1 calc PR A 2

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Zn1 0.0376(2) 0.0247(2) 0.0277(2) 0.00332(15) 0.01415(17) 0.00433(16)
Zn2 0.0435(2) 0.0286(2) 0.0297(2) 0.00086(16) 0.01698(19) 0.00192(17)
O2 0.078(2) 0.0510(16) 0.0415(16) 0.0149(13) 0.0314(15) 0.0028(14)
O3 0.0377(14) 0.0379(14) 0.0465(15) 0.0135(12) 0.0071(12) 0.0056(11)
O4 0.0675(18) 0.0383(14) 0.0461(15) 0.0024(12) 0.0356(14) 0.0119(12)
O5 0.0349(13) 0.0306(12) 0.0352(13) 0.0074(10) 0.0089(11) 0.0074(10)
O6 0.086(2) 0.0340(14) 0.0419(16) 0.0095(12) 0.0291(15) 0.0136(14)
O7 0.0567(16) 0.0379(13) 0.0287(13) 0.0032(11) 0.0190(12) 0.0027(12)
O8 0.0416(14) 0.0528(16) 0.0360(14) -0.0191(12) 0.0141(12) -0.0050(12)
O9 0.082(2) 0.082(2) 0.061(2) -0.0351(17) 0.0265(18) 0.0019(19)
O10 0.0465(14) 0.0451(13) 0.0210(12) 0.0037(10) 0.0130(11) 0.0205(12)
O11 0.082(2) 0.0306(14) 0.077(2) -0.0038(13) 0.0541(18) 0.0094(14)
O12 0.078(2) 0.0409(15) 0.0375(16) -0.0041(12) 0.0160(15) -0.0090(14)
O13 0.0392(14) 0.0454(15) 0.0497(16) 0.0119(13) 0.0122(13) 0.0015(12)
O19 0.0652(17) 0.0321(13) 0.0407(14) -0.0031(11) 0.0333(13) 0.0071(12)
C1 0.050(2) 0.034(2) 0.040(2) -0.0051(16) 0.0211(18) 0.0014(17)
C2 0.050(2) 0.0327(18) 0.0314(18) -0.0045(15) 0.0197(17) 0.0053(16)
C3 0.051(2) 0.0367(19) 0.0298(18) 0.0037(15) 0.0215(17) 0.0093(16)
C4 0.047(2) 0.0306(18) 0.0338(19) 0.0009(15) 0.0191(17) 0.0112(16)
C5 0.044(2) 0.0343(18) 0.0274(18) -0.0072(14) 0.0173(16) 0.0049(15)
C6 0.086(3) 0.039(2) 0.057(3) 0.0050(19) 0.049(3) 0.008(2)
C7 0.083(3) 0.031(2) 0.060(3) 0.0019(18) 0.046(2) 0.009(2)
C8 0.047(2) 0.0329(18) 0.0301(18) -0.0027(14) 0.0192(17) 0.0037(16)
C9 0.0374(19) 0.0321(17) 0.0198(16) -0.0023(13) 0.0093(14) 0.0072(15)
C10 0.041(2) 0.0338(19) 0.0345(19) 0.0026(16) 0.0114(17) 0.0045(16)
C11 0.0349(19) 0.0254(16) 0.039(2) 0.0035(15) 0.0088(16) 0.0004(14)
C12 0.043(2) 0.0280(18) 0.038(2) 0.0078(15) 0.0092(17) 0.0014(15)
C13 0.039(2) 0.0254(17) 0.0342(19) 0.0069(14) 0.0086(16) 0.0069(15)
C14 0.0318(18) 0.0299(17) 0.0276(17) -0.0016(14) 0.0069(15) 0.0045(14)
C15 0.037(2) 0.0344(19) 0.047(2) 0.0076(16) 0.0146(17) 0.0036(16)
C16 0.036(2) 0.0337(19) 0.042(2) 0.0068(16) 0.0058(17) 0.0028(16)
C17 0.055(3) 0.034(2) 0.054(3) -0.0014(18) 0.024(2) -0.0004(19)
C18 0.065(3) 0.042(2) 0.037(2) -0.0020(17) 0.022(2) 0.0032(19)
C19 0.044(2) 0.078(3) 0.051(3) -0.016(2) 0.007(2) -0.005(2)
C20 0.048(3) 0.077(3) 0.062(3) -0.027(2) 0.020(2) -0.004(2)
C21 0.047(2) 0.038(2) 0.0320(19) -0.0074(16) 0.0142(17) -0.0078(17)
C22 0.060(3) 0.061(3) 0.047(3) -0.022(2) 0.017(2) 0.000(2)
C23 0.067(3) 0.065(3) 0.055(3) -0.026(2) 0.019(2) 0.003(2)
C24 0.0355(19) 0.0307(18) 0.0350(19) 0.0001(15) 0.0151(16) -0.0033(15)
C26 0.084(3) 0.0311(19) 0.033(2) -0.0004(16) 0.017(2) 0.015(2)
C27 0.082(3) 0.044(2) 0.029(2) -0.0031(17) 0.023(2) 0.016(2)
C28 0.0340(19) 0.0393(19) 0.0283(18) 0.0035(15) 0.0121(15) 0.0093(15)
C29 0.055(2) 0.0384(19) 0.0321(19) 0.0017(15) 0.0239(18) 0.0165(17)
C30 0.053(2) 0.045(2) 0.0255(18) 0.0004(15) 0.0189(17) 0.0142(17)
C31 0.042(2) 0.0404(19) 0.0269(17) -0.0043(15) 0.0164(16) 0.0141(16)
C32 0.038(2) 0.0378(19) 0.0288(18) -0.0094(15) 0.0093(16) 0.0031(15)
C33 0.0391(19) 0.0306(16) 0.0248(17) 0.0021(14) 0.0102(15) 0.0056(15)
C100 0.0378(19) 0.0337(18) 0.0274(18) -0.0020(14) 0.0122(15) 0.0015(15)

_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 1.956(2) . ?
Zn1 O6 1.971(2) 6_565 ?
Zn1 O3 1.980(2) 3_545 ?
Zn1 O12 2.027(3) 6_575 ?
Zn1 O9 2.300(3) 6_575 ?
Zn1 C17 2.461(4) 6_575 ?
Zn2 O13 1.921(3) 3_545 ?
Zn2 O11 1.924(2) . ?
Zn2 O7 1.951(2) 6_565 ?
Zn2 O2 1.954(2) . ?
O2 C300 1.194(8) . ?
O2 C304 1.259(7) . ?
O3 C10 1.254(4) . ?
O3 Zn1 1.980(2) 3_455 ?
O4 C1 1.266(4) . ?
O5 C14 1.372(4) . ?
O5 C33 1.431(4) . ?
O6 C24 1.258(4) . ?
O6 Zn1 1.971(2) 6_566 ?
O7 C24 1.257(4) . ?
O7 Zn2 1.951(2) 6_566 ?
O8 C21 1.396(4) . ?
O8 C32 1.441(4) . ?
O9 C17 1.239(5) . ?
O9 Zn1 2.300(3) 6_576 ?
O10 C28 1.364(4) . ?
O10 C31 1.449(3) . ?
O11 C1 1.264(4) . ?
O12 C17 1.240(5) . ?
O12 Zn1 2.027(3) 6_576 ?
O13 C10 1.282(4) . ?
O13 Zn2 1.921(3) 3_455 ?
O19 C5 1.364(4) . ?
O19 C8 1.430(4) . ?
N305 C306 1.423(9) . ?
N305 C304 1.429(9) . ?
N305 C308 1.476(9) . ?
C1 C2 1.497(5) . ?
C2 C7 1.381(5) . ?
C2 C3 1.388(4) . ?
C3 C4 1.390(4) . ?
C4 C5 1.389(5) . ?
C5 C6 1.391(5) . ?
C6 C7 1.392(5) . ?
C8 C9 1.533(4) . ?
C9 C31 1.516(4) . ?
C9 C33 1.530(5) . ?
C9 C32 1.537(4) . ?
C10 C11 1.483(5) . ?
C11 C16 1.392(5) . ?
C11 C12 1.397(5) . ?
C12 C13 1.372(5) . ?
C13 C14 1.377(5) . ?
C14 C15 1.413(4) . ?
C15 C16 1.385(5) . ?
C17 C18 1.538(5) . ?
C17 Zn1 2.461(4) 6_576 ?
C18 C23 1.364(6) . ?
C18 C19 1.369(5) . ?
C19 C20 1.412(6) . ?
C20 C21 1.373(5) . ?
C21 C22 1.374(5) . ?
C22 C23 1.364(5) . ?
C24 C100 1.487(5) . ?
C26 C27 1.376(5) . ?
C26 C100 1.397(5) . ?
C27 C28 1.386(5) . ?
C28 C29 1.383(4) . ?
C29 C30 1.381(5) . ?
C30 C100 1.379(5) . ?
C300 N301 1.401(9) . ?
C302 N301 1.477(9) . ?
N301 C303 1.410(9) . ?
N301 C309 1.433(10) . ?
N301 C310 1.439(10) . ?

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 O6 121.00(11) . 6_565 ?
O4 Zn1 O3 103.02(11) . 3_545 ?
O6 Zn1 O3 97.85(11) 6_565 3_545 ?
O4 Zn1 O12 118.06(10) . 6_575 ?
O6 Zn1 O12 111.81(10) 6_565 6_575 ?
O3 Zn1 O12 99.31(11) 3_545 6_575 ?
O4 Zn1 O9 90.82(12) . 6_575 ?
O6 Zn1 O9 88.00(12) 6_565 6_575 ?
O3 Zn1 O9 159.11(11) 3_545 6_575 ?
O12 Zn1 O9 60.05(12) 6_575 6_575 ?
O4 Zn1 C17 106.41(12) . 6_575 ?
O6 Zn1 C17 100.95(12) 6_565 6_575 ?
O3 Zn1 C17 129.36(13) 3_545 6_575 ?
O12 Zn1 C17 30.14(12) 6_575 6_575 ?
O9 Zn1 C17 29.92(12) 6_575 6_575 ?
O13 Zn2 O11 117.49(12) 3_545 . ?
O13 Zn2 O7 114.77(11) 3_545 6_565 ?
O11 Zn2 O7 109.55(11) . 6_565 ?
O13 Zn2 O2 109.45(11) 3_545 . ?
O11 Zn2 O2 101.03(11) . . ?
O7 Zn2 O2 102.59(11) 6_565 . ?
C300 O2 C304 26.4(8) . . ?
C300 O2 Zn2 136.0(7) . . ?
C304 O2 Zn2 120.4(5) . . ?
C10 O3 Zn1 134.8(2) . 3_455 ?
C1 O4 Zn1 127.7(2) . . ?
C14 O5 C33 117.2(2) . . ?
C24 O6 Zn1 149.6(2) . 6_566 ?
C24 O7 Zn2 117.4(2) . 6_566 ?
C21 O8 C32 116.3(3) . . ?
C17 O9 Zn1 82.3(3) . 6_576 ?
C28 O10 C31 116.7(2) . . ?
C1 O11 Zn2 138.5(3) . . ?
C17 O12 Zn1 94.7(3) . 6_576 ?
C10 O13 Zn2 132.3(2) . 3_455 ?
C5 O19 C8 119.4(3) . . ?
C306 N305 C304 98.0(13) . . ?
C306 N305 C308 128.7(15) . . ?
C304 N305 C308 118.0(12) . . ?
O11 C1 O4 125.0(3) . . ?
O11 C1 C2 116.4(3) . . ?
O4 C1 C2 118.6(3) . . ?
C7 C2 C3 119.3(3) . . ?
C7 C2 C1 119.3(3) . . ?
C3 C2 C1 121.3(3) . . ?
C2 C3 C4 121.1(3) . . ?
C5 C4 C3 118.5(3) . . ?
O19 C5 C4 124.5(3) . . ?
O19 C5 C6 114.0(3) . . ?
C4 C5 C6 121.4(3) . . ?
C5 C6 C7 118.6(3) . . ?
C2 C7 C6 121.0(3) . . ?
O19 C8 C9 105.6(3) . . ?
C31 C9 C33 107.6(3) . . ?
C31 C9 C8 107.9(3) . . ?
C33 C9 C8 111.0(3) . . ?
C31 C9 C32 111.9(3) . . ?
C33 C9 C32 108.8(3) . . ?
C8 C9 C32 109.6(3) . . ?
O3 C10 O13 125.2(3) . . ?
O3 C10 C11 117.4(3) . . ?
O13 C10 C11 117.4(3) . . ?
C16 C11 C12 118.2(3) . . ?
C16 C11 C10 119.9(3) . . ?
C12 C11 C10 121.8(3) . . ?
C13 C12 C11 121.6(3) . . ?
C12 C13 C14 119.9(3) . . ?
O5 C14 C13 125.5(3) . . ?
O5 C14 C15 114.4(3) . . ?
C13 C14 C15 120.1(3) . . ?
C16 C15 C14 119.0(3) . . ?
C15 C16 C11 121.1(3) . . ?
O9 C17 O12 123.0(4) . . ?
O9 C17 C18 118.3(4) . . ?
O12 C17 C18 118.7(4) . . ?
O9 C17 Zn1 67.8(2) . 6_576 ?
O12 C17 Zn1 55.2(2) . 6_576 ?
C18 C17 Zn1 173.8(3) . 6_576 ?
C23 C18 C19 119.0(4) . . ?
C23 C18 C17 119.2(4) . . ?
C19 C18 C17 121.8(4) . . ?
C18 C19 C20 121.0(4) . . ?
C21 C20 C19 118.3(4) . . ?
C20 C21 C22 119.9(4) . . ?
C20 C21 O8 115.7(3) . . ?
C22 C21 O8 124.4(3) . . ?
C23 C22 C21 120.8(4) . . ?
C22 C23 C18 121.0(4) . . ?
O7 C24 O6 124.0(3) . . ?
O7 C24 C100 118.5(3) . . ?
O6 C24 C100 117.4(3) . . ?
C27 C26 C100 120.8(3) . . ?
C26 C27 C28 119.9(3) . . ?
O10 C28 C29 116.3(3) . . ?
O10 C28 C27 124.1(3) . . ?
C29 C28 C27 119.6(3) . . ?
C30 C29 C28 120.3(3) . . ?
C100 C30 C29 120.7(3) . . ?
O10 C31 C9 108.3(2) . . ?
O8 C32 C9 109.0(3) . . ?
O5 C33 C9 108.6(3) . . ?
O2 C304 N305 117.6(9) . . ?
C30 C100 C26 118.7(3) . . ?
C30 C100 C24 121.8(3) . . ?
C26 C100 C24 119.5(3) . . ?
O2 C300 N301 141.9(12) . . ?
C300 N301 C303 135.6(14) . . ?
C300 N301 C309 125.4(18) . . ?
C303 N301 C309 84.2(17) . . ?
C300 N301 C310 92.7(14) . . ?
C303 N301 C310 131.3(16) . . ?
C309 N301 C310 66.9(18) . . ?
C300 N301 C302 124.6(13) . . ?
C303 N301 C302 45.8(10) . . ?
C309 N301 C302 51.3(15) . . ?
C310 N301 C302 118.0(16) . . ?

_diffrn_measured_fraction_theta_max 0.990
_diffrn_reflns_theta_full        27.17
_diffrn_measured_fraction_theta_full 0.990
_refine_diff_density_max         1.057
_refine_diff_density_min         -0.918
_refine_diff_density_rms         0.084

##############END###################

data_4
_database_code_depnum_ccdc_archive 'CCDC 740055'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            4
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C33 H24 O12 Zn'
_chemical_formula_weight         677.89

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           orthorhombic
_symmetry_space_group_name_H-M   Pbcn

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

_cell_length_a                   24.4646(19)
_cell_length_b                   15.2591(11)
_cell_length_c                   33.563(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     12529.3(16)
_cell_formula_units_Z            8
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    .
_cell_measurement_theta_min      .
_cell_measurement_theta_max      .

_exptl_crystal_description       Prism
_exptl_crystal_colour            Colourless
_exptl_crystal_size_max          0.07
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.02
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    0.719
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2784
_exptl_absorpt_coefficient_mu    0.424
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.8428
_exptl_absorpt_correction_T_max  0.9916
_exptl_absorpt_process_details   Bruker-SADABS

_exptl_special_details           
;
Data were corrected for decay and absorption using the program SADABS
based on the method of R.H. Blessing (Acta Cryst. A51, 33-38, 1995).
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.77490
_diffrn_radiation_type           synchrotron
_diffrn_radiation_source         'Advanced Light Source station 11.3.1'
_diffrn_radiation_monochromator  'silicon 111'
_diffrn_measurement_device_type  'Bruker Apex II CCD Diffractometer'
_diffrn_measurement_method       '\w 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            72926
_diffrn_reflns_av_R_equivalents  0.0575
_diffrn_reflns_av_sigmaI/netI    0.0265
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_theta_min         2.62
_diffrn_reflns_theta_max         22.81
_reflns_number_total             6506
_reflns_number_gt                5187
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Apex II'
_computing_cell_refinement       'SAINT (Bruker, 1998)'
_computing_data_reduction        'SAINT (Bruker, 1998)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'XSeed (Barbour, 2001)'
_computing_publication_material  'local program'

_refine_special_details          
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger. Due to disorder in the
dimethylformamide molecules of crystallisation, the routine SQUEEZE was
applied to the data. This dramatically improved the agreement indices.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[\s^2^(Fo^2^)+(0.1304P)^2^+4.7906P] where P=(Fo^2^+2Fc^2^)/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         6506
_refine_ls_number_parameters     415
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0690
_refine_ls_R_factor_gt           0.0563
_refine_ls_wR_factor_ref         0.1816
_refine_ls_wR_factor_gt          0.1725
_refine_ls_goodness_of_fit_ref   1.001
_refine_ls_restrained_S_all      1.001
_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 0.697592(19) 0.24503(3) 0.097955(13) 0.0478(3) Uani 1 1 d . . .
O1 O 0.57569(10) -0.37961(17) 0.25296(7) 0.0517(7) Uani 1 1 d . . .
C1 C 0.6370(2) 0.0980(3) 0.12793(14) 0.0678(13) Uani 1 1 d . . .
O2 O 0.63234(11) -0.1550(2) 0.25114(8) 0.0615(8) Uani 1 1 d . . .
C2 C 0.63582(19) 0.0295(3) 0.16093(12) 0.0566(11) Uani 1 1 d . . .
O3 O 0.67117(12) -0.26694(18) 0.54394(8) 0.0556(8) Uani 1 1 d . . .
C3 C 0.68230(19) -0.0094(3) 0.17477(14) 0.0665(13) Uani 1 1 d . . .
H3 H 0.7164 0.0063 0.1633 0.080 Uiso 1 1 calc R . .
O4 O 0.63608(12) -0.29660(19) 0.35841(8) 0.0643(8) Uani 1 1 d . . .
C4 C 0.68117(19) -0.0703(3) 0.20463(14) 0.0758(14) Uani 1 1 d . . .
H4 H 0.7140 -0.0970 0.2136 0.091 Uiso 1 1 calc R . .
O5 O 0.67355(14) -0.6642(2) 0.13523(8) 0.0674(8) Uani 1 1 d . . .
C5 C 0.63054(18) -0.0929(3) 0.22180(12) 0.0548(11) Uani 1 1 d . . .
O6 O 0.52443(12) -0.21509(19) 0.34236(8) 0.0619(8) Uani 1 1 d . . .
C6 C 0.58399(18) -0.0547(3) 0.20869(12) 0.0569(11) Uani 1 1 d . . .
H6 H 0.5498 -0.0687 0.2205 0.068 Uiso 1 1 calc R . .
O7 O 0.72457(16) -0.1575(2) 0.52439(8) 0.0859(11) Uani 1 1 d . . .
C7 C 0.5871(2) 0.0060(3) 0.17738(14) 0.0698(13) Uani 1 1 d . . .
H7 H 0.5544 0.0313 0.1674 0.084 Uiso 1 1 calc R . .
C8 C 0.58373(16) -0.1845(3) 0.26745(11) 0.0488(10) Uani 1 1 d . . .
H8A H 0.5593 -0.2051 0.2459 0.059 Uiso 1 1 calc R . .
H8B H 0.5653 -0.1354 0.2813 0.059 Uiso 1 1 calc R . .
C9 C 0.59369(17) -0.2587(3) 0.29675(12) 0.0510(11) Uani 1 1 d . . .
O10 O 0.68441(15) 0.12787(19) 0.12027(9) 0.0716(9) Uani 1 1 d . . .
C10 C 0.61828(17) -0.3384(3) 0.27537(11) 0.0541(11) Uani 1 1 d . . .
H10A H 0.6481 -0.3195 0.2574 0.065 Uiso 1 1 calc R . .
H10B H 0.6336 -0.3800 0.2951 0.065 Uiso 1 1 calc R . .
C11 C 0.59029(18) -0.4462(3) 0.22766(11) 0.0509(11) Uani 1 1 d . . .
O12 O 0.29570(13) -0.1287(2) 0.42261(9) 0.0735(9) Uani 1 1 d . . .
C12 C 0.54830(17) -0.4844(3) 0.20735(12) 0.0516(10) Uani 1 1 d . . .
H12 H 0.5117 -0.4663 0.2120 0.062 Uiso 1 1 calc R . .
C13 C 0.55940(18) -0.5501(3) 0.17964(13) 0.0606(11) Uani 1 1 d . . .
H13 H 0.5299 -0.5767 0.1657 0.073 Uiso 1 1 calc R . .
O14 O 0.27603(13) -0.25465(19) 0.39177(10) 0.0626(8) Uani 1 1 d . . .
C14 C 0.61239(17) -0.5779(3) 0.17187(11) 0.0493(10) Uani 1 1 d . . .
C15 C 0.65392(18) -0.5388(3) 0.19340(12) 0.0602(12) Uani 1 1 d . . .
H15 H 0.6905 -0.5568 0.1887 0.072 Uiso 1 1 calc R . .
C16 C 0.64401(16) -0.4735(3) 0.22195(11) 0.0508(10) Uani 1 1 d . . .
H16 H 0.6731 -0.4486 0.2369 0.061 Uiso 1 1 calc R . .
C17 C 0.6235(2) -0.6448(3) 0.14057(13) 0.0600(12) Uani 1 1 d . . .
C18 C 0.63508(18) -0.2286(3) 0.32838(12) 0.0578(11) Uani 1 1 d . . .
H18A H 0.6718 -0.2211 0.3164 0.069 Uiso 1 1 calc R . .
H18B H 0.6236 -0.1721 0.3402 0.069 Uiso 1 1 calc R . .
C19 C 0.65177(19) -0.2738(3) 0.39629(12) 0.0546(11) Uani 1 1 d . . .
C20 C 0.63329(17) -0.3278(3) 0.42575(11) 0.0556(11) Uani 1 1 d . . .
H20 H 0.6114 -0.3772 0.4194 0.067 Uiso 1 1 calc R . .
O21 O 0.59591(18) 0.1180(3) 0.10968(13) 0.1059(13) Uani 1 1 d . . .
C21 C 0.64685(18) -0.3099(3) 0.46542(11) 0.0544(11) Uani 1 1 d . . .
H21 H 0.6343 -0.3477 0.4860 0.065 Uiso 1 1 calc R . .
C22 C 0.6779(2) -0.2388(3) 0.47490(13) 0.0588(12) Uani 1 1 d . . .
C23 C 0.6969(2) -0.1844(3) 0.44400(13) 0.0740(14) Uani 1 1 d . . .
H23 H 0.7199 -0.1360 0.4501 0.089 Uiso 1 1 calc R . .
C24 C 0.6826(2) -0.2005(4) 0.40521(12) 0.0734(15) Uani 1 1 d . . .
H24 H 0.6937 -0.1617 0.3846 0.088 Uiso 1 1 calc R . .
C25 C 0.6934(2) -0.2175(3) 0.51728(13) 0.0600(12) Uani 1 1 d . . .
C26 C 0.53916(17) -0.2842(3) 0.31568(11) 0.0535(11) Uani 1 1 d . . .
H26A H 0.5108 -0.2915 0.2949 0.064 Uiso 1 1 calc R . .
H26B H 0.5429 -0.3402 0.3304 0.064 Uiso 1 1 calc R . .
C27 C 0.47082(18) -0.2174(3) 0.35692(12) 0.0515(11) Uani 1 1 d . . .
C28 C 0.4584(2) -0.1504(3) 0.38358(12) 0.0679(13) Uani 1 1 d . . .
H28 H 0.4857 -0.1098 0.3916 0.081 Uiso 1 1 calc R . .
C29 C 0.40619(19) -0.1440(3) 0.39816(12) 0.0579(12) Uani 1 1 d . . .
H29 H 0.3974 -0.0976 0.4159 0.070 Uiso 1 1 calc R . .
C30 C 0.36636(17) -0.2029(3) 0.38771(11) 0.0488(11) Uani 1 1 d . . .
C31 C 0.38046(17) -0.2693(3) 0.36084(12) 0.0519(11) Uani 1 1 d . . .
H31 H 0.3533 -0.3098 0.3524 0.062 Uiso 1 1 calc R . .
C32 C 0.43263(17) -0.2770(3) 0.34648(11) 0.0488(10) Uani 1 1 d . . .
H32 H 0.4419 -0.3241 0.3293 0.059 Uiso 1 1 calc R . .
C33 C 0.3090(2) -0.1934(4) 0.40230(12) 0.0613(13) Uani 1 1 d . . .
O47 O 0.58649(16) -0.6753(3) 0.12202(12) 0.1053(14) Uani 1 1 d . . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Zn1 0.0609(4) 0.0450(4) 0.0376(4) 0.00646(19) 0.0010(2) 0.0067(2)
O1 0.0548(17) 0.0597(17) 0.0406(15) -0.0058(14) 0.0061(13) 0.0035(14)
C1 0.076(4) 0.060(3) 0.068(3) 0.019(3) -0.003(3) -0.006(3)
O2 0.0578(18) 0.078(2) 0.0489(16) 0.0204(16) 0.0060(14) -0.0008(16)
C2 0.069(3) 0.049(3) 0.051(3) 0.002(2) 0.006(2) -0.009(2)
O3 0.076(2) 0.0519(17) 0.0391(16) -0.0041(14) -0.0004(15) -0.0055(15)
C3 0.067(3) 0.063(3) 0.069(3) 0.025(3) 0.007(3) -0.010(2)
O4 0.096(2) 0.0567(18) 0.0402(17) 0.0022(14) -0.0126(15) -0.0138(16)
C4 0.058(3) 0.090(4) 0.079(3) 0.034(3) 0.004(3) 0.002(3)
O5 0.087(2) 0.064(2) 0.0512(17) -0.0071(15) 0.0032(16) 0.0177(18)
C5 0.070(3) 0.050(3) 0.044(2) 0.005(2) 0.006(2) 0.000(2)
O6 0.071(2) 0.0648(19) 0.0498(17) -0.0072(15) 0.0239(15) -0.0107(16)
C6 0.059(3) 0.056(3) 0.056(3) 0.009(2) 0.009(2) 0.003(2)
O7 0.125(3) 0.083(2) 0.0493(18) -0.0086(17) -0.0150(18) -0.054(2)
C7 0.073(3) 0.063(3) 0.074(3) 0.007(3) -0.001(3) 0.012(3)
C8 0.048(2) 0.055(3) 0.044(2) 0.007(2) 0.0051(19) 0.004(2)
C9 0.056(3) 0.058(3) 0.039(2) 0.0034(19) 0.009(2) -0.008(2)
O10 0.098(3) 0.0472(19) 0.069(2) 0.0180(15) 0.0125(18) 0.0017(18)
C10 0.057(3) 0.065(3) 0.040(2) 0.003(2) -0.004(2) 0.002(2)
C11 0.068(3) 0.048(2) 0.037(2) 0.008(2) 0.010(2) 0.010(2)
O12 0.089(2) 0.059(2) 0.072(2) -0.0196(18) 0.0168(17) 0.0155(17)
C12 0.045(2) 0.054(3) 0.056(3) -0.002(2) 0.001(2) 0.002(2)
C13 0.062(3) 0.054(3) 0.066(3) -0.002(2) -0.001(2) -0.003(2)
O14 0.058(2) 0.064(2) 0.0654(19) -0.0077(15) 0.0063(16) 0.0033(16)
C14 0.057(3) 0.048(2) 0.043(2) 0.004(2) -0.004(2) 0.005(2)
C15 0.059(3) 0.069(3) 0.053(3) 0.016(2) 0.011(2) 0.015(2)
C16 0.051(3) 0.061(3) 0.040(2) -0.003(2) 0.0026(19) 0.008(2)
C17 0.070(3) 0.059(3) 0.051(3) 0.004(2) 0.006(3) 0.016(3)
C18 0.077(3) 0.063(3) 0.033(2) 0.008(2) -0.002(2) -0.009(2)
C19 0.070(3) 0.057(3) 0.036(3) -0.002(2) -0.002(2) -0.014(2)
C20 0.077(3) 0.051(3) 0.038(2) 0.000(2) -0.012(2) -0.010(2)
O21 0.095(3) 0.103(3) 0.119(3) 0.060(3) -0.008(3) -0.002(2)
C21 0.077(3) 0.045(3) 0.041(2) -0.0015(19) -0.002(2) -0.011(2)
C22 0.075(3) 0.056(3) 0.046(3) 0.002(2) -0.006(2) -0.011(2)
C23 0.098(4) 0.073(3) 0.052(3) 0.005(3) 0.007(2) -0.035(3)
C24 0.096(4) 0.084(4) 0.040(3) 0.005(2) -0.003(2) -0.033(3)
C25 0.080(3) 0.055(3) 0.045(3) -0.004(2) -0.006(2) -0.007(3)
C26 0.066(3) 0.056(3) 0.039(2) -0.006(2) 0.015(2) -0.001(2)
C27 0.067(3) 0.045(2) 0.043(2) -0.001(2) 0.011(2) -0.001(2)
C28 0.084(4) 0.074(3) 0.045(2) -0.013(2) 0.017(2) -0.022(3)
C29 0.079(3) 0.052(3) 0.043(2) -0.015(2) 0.015(2) -0.005(3)
C30 0.064(3) 0.048(3) 0.034(2) -0.002(2) 0.005(2) 0.012(2)
C31 0.054(3) 0.058(3) 0.043(2) -0.001(2) 0.007(2) -0.001(2)
C32 0.064(3) 0.039(2) 0.043(2) -0.0073(19) 0.008(2) -0.007(2)
C33 0.077(3) 0.064(3) 0.043(3) 0.014(2) 0.004(2) 0.008(3)
O47 0.081(3) 0.118(3) 0.117(3) -0.066(3) -0.011(2) 0.012(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 O14 1.950(3) 6_666 ?
Zn1 O3 1.953(3) 8 ?
Zn1 O5 1.957(3) 1_565 ?
Zn1 O10 1.965(3) . ?
O1 C11 1.372(5) . ?
O1 C10 1.431(5) . ?
C1 O21 1.216(6) . ?
C1 O10 1.273(5) . ?
C1 C2 1.523(6) . ?
O2 C5 1.367(5) . ?
O2 C8 1.384(4) . ?
C2 C7 1.361(6) . ?
C2 C3 1.364(6) . ?
O3 C25 1.291(5) . ?
O3 Zn1 1.953(3) 8_556 ?
C3 C4 1.368(6) . ?
O4 C19 1.373(5) . ?
O4 C18 1.447(5) . ?
C4 C5 1.409(6) . ?
O5 C17 1.271(5) . ?
O5 Zn1 1.957(3) 1_545 ?
C5 C6 1.353(6) . ?
O6 C27 1.400(5) . ?
O6 C26 1.430(5) . ?
C6 C7 1.402(6) . ?
O7 C25 1.214(5) . ?
C8 C9 1.520(5) . ?
C9 C26 1.528(6) . ?
C9 C10 1.535(6) . ?
C9 C18 1.537(6) . ?
C11 C12 1.364(6) . ?
C11 C16 1.392(6) . ?
O12 C33 1.243(5) . ?
C12 C13 1.394(6) . ?
C13 C14 1.388(6) . ?
O14 C33 1.284(6) . ?
O14 Zn1 1.950(3) 6_556 ?
C14 C15 1.382(6) . ?
C14 C17 1.490(6) . ?
C15 C16 1.404(6) . ?
C17 O47 1.194(5) . ?
C19 C20 1.364(6) . ?
C19 C24 1.381(7) . ?
C20 C21 1.399(5) . ?
C21 C22 1.362(6) . ?
C22 C23 1.408(6) . ?
C22 C25 1.508(6) . ?
C23 C24 1.371(6) . ?
C27 C32 1.350(6) . ?
C27 C28 1.392(6) . ?
C28 C29 1.371(6) . ?
C29 C30 1.372(6) . ?
C30 C31 1.400(6) . ?
C30 C33 1.493(6) . ?
C31 C32 1.369(6) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O14 Zn1 O3 119.30(13) 6_666 8 ?
O14 Zn1 O5 100.42(14) 6_666 1_565 ?
O3 Zn1 O5 111.88(12) 8 1_565 ?
O14 Zn1 O10 95.53(14) 6_666 . ?
O3 Zn1 O10 117.07(13) 8 . ?
O5 Zn1 O10 110.55(13) 1_565 . ?
C11 O1 C10 117.5(3) . . ?
O21 C1 O10 124.2(4) . . ?
O21 C1 C2 121.5(5) . . ?
O10 C1 C2 114.2(4) . . ?
C5 O2 C8 118.8(3) . . ?
C7 C2 C3 118.4(4) . . ?
C7 C2 C1 119.5(4) . . ?
C3 C2 C1 122.0(4) . . ?
C25 O3 Zn1 113.8(3) . 8_556 ?
C4 C3 C2 121.9(4) . . ?
C19 O4 C18 117.9(3) . . ?
C3 C4 C5 118.9(4) . . ?
C17 O5 Zn1 123.0(3) . 1_545 ?
C6 C5 O2 124.1(4) . . ?
C6 C5 C4 120.1(4) . . ?
O2 C5 C4 115.8(4) . . ?
C27 O6 C26 115.9(3) . . ?
C5 C6 C7 118.8(4) . . ?
C2 C7 C6 121.8(4) . . ?
O2 C8 C9 111.1(3) . . ?
C8 C9 C26 108.6(3) . . ?
C8 C9 C10 110.5(3) . . ?
C26 C9 C10 109.6(3) . . ?
C8 C9 C18 109.3(3) . . ?
C26 C9 C18 111.3(3) . . ?
C10 C9 C18 107.5(3) . . ?
C1 O10 Zn1 123.5(3) . . ?
O1 C10 C9 108.0(3) . . ?
C12 C11 O1 115.5(4) . . ?
C12 C11 C16 121.0(4) . . ?
O1 C11 C16 123.5(4) . . ?
C11 C12 C13 119.6(4) . . ?
C14 C13 C12 121.8(4) . . ?
C33 O14 Zn1 124.8(3) . 6_556 ?
C15 C14 C13 117.2(4) . . ?
C15 C14 C17 122.0(4) . . ?
C13 C14 C17 120.8(4) . . ?
C14 C15 C16 122.4(4) . . ?
C11 C16 C15 118.0(4) . . ?
O47 C17 O5 124.5(4) . . ?
O47 C17 C14 119.7(4) . . ?
O5 C17 C14 115.8(4) . . ?
O4 C18 C9 106.1(3) . . ?
C20 C19 O4 115.2(4) . . ?
C20 C19 C24 120.8(4) . . ?
O4 C19 C24 123.9(4) . . ?
C19 C20 C21 119.6(4) . . ?
C22 C21 C20 120.6(4) . . ?
C21 C22 C23 118.8(4) . . ?
C21 C22 C25 122.2(4) . . ?
C23 C22 C25 119.0(4) . . ?
C24 C23 C22 120.6(4) . . ?
C23 C24 C19 119.4(4) . . ?
O7 C25 O3 124.6(4) . . ?
O7 C25 C22 120.4(4) . . ?
O3 C25 C22 114.9(4) . . ?
O6 C26 C9 107.0(3) . . ?
C32 C27 C28 120.7(4) . . ?
C32 C27 O6 125.0(4) . . ?
C28 C27 O6 114.3(4) . . ?
C29 C28 C27 119.1(4) . . ?
C28 C29 C30 121.6(4) . . ?
C29 C30 C31 117.7(4) . . ?
C29 C30 C33 121.3(4) . . ?
C31 C30 C33 120.9(4) . . ?
C32 C31 C30 121.2(4) . . ?
C27 C32 C31 119.7(4) . . ?
O12 C33 O14 124.4(4) . . ?
O12 C33 C30 120.2(5) . . ?
O14 C33 C30 115.4(4) . . ?

_diffrn_measured_fraction_theta_max 0.990
_diffrn_reflns_theta_full        22.81
_diffrn_measured_fraction_theta_full 0.990
_refine_diff_density_max         0.316
_refine_diff_density_min         -0.317
_refine_diff_density_rms         0.061