# Supplementary Material (ESI) for Chemical Communications
# This journal is © The Royal Society of Chemistry 2005


data_global
_journal_name_full               Chem.Commun.

_journal_coden_Cambridge         0182

_publ_contact_author_name        'ProfD Hong-Cai Zhou'
_publ_contact_author_address     
;
Department of Chemistry and Biochemistry
Miami University
Oxford
Ohio
45056
UNITED STATES OF AMERICA
;

_publ_contact_author_email       ZHOUH@MUOHIO.EDU

_publ_section_title              
;
Syntheses, characterization, and photoluminescence of
isostructural Mn, Co, and Zn MOFs having a diamondoid structure with
large tetrahedral cages and high thermal stability
;
loop_
_publ_author_name
'Hong-Cai Zhou.'
'Yanxiong Ke.'
'Shengqian Ma.'
'Tracy M. Petersen'
;
Daofeng Sun
;

data_xamd139sad
_database_code_depnum_ccdc_archive 'CCDC 262518'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            none
_chemical_melting_point          'not measured'
_chemical_formula_moiety         
'Co6 O 2(C24 H12 N3 O6) 2(C24 H13 N3 O6) 1.5(H2O)'
_chemical_formula_sum            'C96 H53 Co6 N12 O26.50'
_chemical_formula_weight         2152.08

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'
Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Cubic
_symmetry_space_group_name_H-M   Fd-3

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/4, -y+1/4, z'
'-x+1/4, y, -z+1/4'
'x, -y+1/4, -z+1/4'
'z, x, y'
'z, -x+1/4, -y+1/4'
'-z+1/4, -x+1/4, y'
'-z+1/4, x, -y+1/4'
'y, z, x'
'-y+1/4, z, -x+1/4'
'y, -z+1/4, -x+1/4'
'-y+1/4, -z+1/4, x'
'x, y+1/2, z+1/2'
'-x+1/4, -y+3/4, z+1/2'
'-x+1/4, y+1/2, -z+3/4'
'x, -y+3/4, -z+3/4'
'z, x+1/2, y+1/2'
'z, -x+3/4, -y+3/4'
'-z+1/4, -x+3/4, y+1/2'
'-z+1/4, x+1/2, -y+3/4'
'y, z+1/2, x+1/2'
'-y+1/4, z+1/2, -x+3/4'
'y, -z+3/4, -x+3/4'
'-y+1/4, -z+3/4, x+1/2'
'x+1/2, y, z+1/2'
'-x+3/4, -y+1/4, z+1/2'
'-x+3/4, y, -z+3/4'
'x+1/2, -y+1/4, -z+3/4'
'z+1/2, x, y+1/2'
'z+1/2, -x+1/4, -y+3/4'
'-z+3/4, -x+1/4, y+1/2'
'-z+3/4, x, -y+3/4'
'y+1/2, z, x+1/2'
'-y+3/4, z, -x+3/4'
'y+1/2, -z+1/4, -x+3/4'
'-y+3/4, -z+1/4, x+1/2'
'x+1/2, y+1/2, z'
'-x+3/4, -y+3/4, z'
'-x+3/4, y+1/2, -z+1/4'
'x+1/2, -y+3/4, -z+1/4'
'z+1/2, x+1/2, y'
'z+1/2, -x+3/4, -y+1/4'
'-z+3/4, -x+3/4, y'
'-z+3/4, x+1/2, -y+1/4'
'y+1/2, z+1/2, x'
'-y+3/4, z+1/2, -x+1/4'
'y+1/2, -z+3/4, -x+1/4'
'-y+3/4, -z+3/4, x'
'-x, -y, -z'
'x-1/4, y-1/4, -z'
'x-1/4, -y, z-1/4'
'-x, y-1/4, z-1/4'
'-z, -x, -y'
'-z, x-1/4, y-1/4'
'z-1/4, x-1/4, -y'
'z-1/4, -x, y-1/4'
'-y, -z, -x'
'y-1/4, -z, x-1/4'
'-y, z-1/4, x-1/4'
'y-1/4, z-1/4, -x'
'-x, -y+1/2, -z+1/2'
'x-1/4, y+1/4, -z+1/2'
'x-1/4, -y+1/2, z+1/4'
'-x, y+1/4, z+1/4'
'-z, -x+1/2, -y+1/2'
'-z, x+1/4, y+1/4'
'z-1/4, x+1/4, -y+1/2'
'z-1/4, -x+1/2, y+1/4'
'-y, -z+1/2, -x+1/2'
'y-1/4, -z+1/2, x+1/4'
'-y, z+1/4, x+1/4'
'y-1/4, z+1/4, -x+1/2'
'-x+1/2, -y, -z+1/2'
'x+1/4, y-1/4, -z+1/2'
'x+1/4, -y, z+1/4'
'-x+1/2, y-1/4, z+1/4'
'-z+1/2, -x, -y+1/2'
'-z+1/2, x-1/4, y+1/4'
'z+1/4, x-1/4, -y+1/2'
'z+1/4, -x, y+1/4'
'-y+1/2, -z, -x+1/2'
'y+1/4, -z, x+1/4'
'-y+1/2, z-1/4, x+1/4'
'y+1/4, z-1/4, -x+1/2'
'-x+1/2, -y+1/2, -z'
'x+1/4, y+1/4, -z'
'x+1/4, -y+1/2, z-1/4'
'-x+1/2, y+1/4, z-1/4'
'-z+1/2, -x+1/2, -y'
'-z+1/2, x+1/4, y-1/4'
'z+1/4, x+1/4, -y'
'z+1/4, -x+1/2, y-1/4'
'-y+1/2, -z+1/2, -x'
'y+1/4, -z+1/2, x-1/4'
'-y+1/2, z+1/4, x-1/4'
'y+1/4, z+1/4, -x'

_cell_length_a                   25.7202(5)
_cell_length_b                   25.7202(5)
_cell_length_c                   25.7202(5)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     17014.6(6)
_cell_formula_units_Z            8
_cell_measurement_temperature    213(2)
_cell_measurement_reflns_used    1910
_cell_measurement_theta_min      2.24
_cell_measurement_theta_max      19.51

_exptl_crystal_description       block
_exptl_crystal_colour            blue
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.08
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_density_diffrn    1.680
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             8696
_exptl_absorpt_coefficient_mu    1.236
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.906
_exptl_absorpt_correction_T_max  0.897
_exptl_absorpt_process_details   sadas

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      273(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        none
_diffrn_reflns_number            15971
_diffrn_reflns_av_R_equivalents  0.0702
_diffrn_reflns_av_sigmaI/netI    0.0202
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_theta_min         1.37
_diffrn_reflns_theta_max         20.79
_reflns_number_total             759
_reflns_number_gt                651
_reflns_threshold_expression     >2sigma(I)

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

_refine_special_details          
;
Refinement of 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^)+(0.1592P)^2^+440.6461P] 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    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         759
_refine_ls_number_parameters     110
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0914
_refine_ls_R_factor_gt           0.0753
_refine_ls_wR_factor_ref         0.2564
_refine_ls_wR_factor_gt          0.2336
_refine_ls_goodness_of_fit_ref   1.173
_refine_ls_restrained_S_all      1.173
_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
Co1 Co 0.0000 0.5000 0.0000 0.0214(11) Uani 1 6 d S . .
Co2 Co 0.07845(6) 0.57845(6) 0.07845(6) 0.0417(11) Uani 1 3 d S . .
O1 O 0.1250 0.6250 0.1250 0.017(5) Uani 1 12 d S . .
O2 O 0.0640(3) 0.5192(3) 0.1239(3) 0.052(2) Uani 1 1 d . . .
O3 O -0.0069(3) 0.5026(3) 0.0801(3) 0.039(2) Uani 1 1 d . . .
N1 N 0.0047(4) 0.3183(4) 0.2976(4) 0.061(3) Uani 1 1 d . . .
C1 C 0.0239(5) 0.4932(4) 0.1151(4) 0.039(3) Uani 1 1 d . . .
C2 C 0.0099(4) 0.4494(4) 0.1526(4) 0.033(3) Uani 1 1 d . . .
C3 C -0.0324(5) 0.4196(4) 0.1444(5) 0.047(3) Uani 1 1 d . . .
H3 H -0.0530 0.4258 0.1154 0.056 Uiso 1 1 calc R . .
C4 C -0.0458(5) 0.3800(5) 0.1785(5) 0.051(3) Uani 1 1 d . . .
H4 H -0.0753 0.3601 0.1722 0.061 Uiso 1 1 calc R . .
C5 C -0.0155(4) 0.3700(5) 0.2214(4) 0.047(3) Uani 1 1 d . . .
C6 C 0.0279(5) 0.4006(5) 0.2294(5) 0.056(4) Uani 1 1 d . . .
H6 H 0.0487 0.3949 0.2584 0.068 Uiso 1 1 calc R . .
C7 C 0.0407(5) 0.4393(4) 0.1952(4) 0.050(3) Uani 1 1 d . . .
H7 H 0.0706 0.4590 0.2007 0.060 Uiso 1 1 calc R . .
C8 C -0.0275(5) 0.3266(5) 0.2562(5) 0.059(4) Uani 1 1 d . . .
O1W O -0.059(5) 0.391(6) 0.361(6) 0.17(6) Uiso 0.13 1 d P . .

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
Co1 0.0214(11) 0.0214(11) 0.0214(11) -0.0010(7) -0.0010(7) -0.0010(7)
Co2 0.0417(11) 0.0417(11) 0.0417(11) -0.0007(7) -0.0007(7) -0.0007(7)
O1 0.017(5) 0.017(5) 0.017(5) 0.000 0.000 0.000
O2 0.056(5) 0.048(5) 0.050(5) 0.008(4) -0.009(4) -0.016(5)
O3 0.046(5) 0.052(5) 0.018(4) 0.006(3) 0.002(4) 0.009(4)
N1 0.061(7) 0.066(7) 0.057(7) 0.027(6) -0.024(6) -0.033(6)
C1 0.056(8) 0.038(7) 0.022(6) -0.004(5) 0.006(6) 0.005(6)
C2 0.043(7) 0.030(6) 0.025(6) -0.006(5) -0.006(5) -0.001(5)
C3 0.049(8) 0.042(7) 0.049(7) 0.011(6) -0.020(6) -0.005(6)
C4 0.056(8) 0.047(7) 0.049(8) 0.012(6) -0.022(6) -0.023(6)
C5 0.051(7) 0.048(7) 0.042(7) 0.016(6) -0.020(6) -0.015(6)
C6 0.075(9) 0.050(7) 0.044(7) 0.018(6) -0.030(7) -0.020(7)
C7 0.061(8) 0.046(7) 0.042(7) 0.004(6) -0.017(6) -0.026(6)
C8 0.062(9) 0.054(8) 0.062(9) 0.023(6) -0.027(7) -0.029(7)

_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
Co1 O3 2.068(7) 65 ?
Co1 O3 2.068(7) 93 ?
Co1 O3 2.068(7) . ?
Co1 O3 2.068(7) 49_565 ?
Co1 O3 2.068(7) 45_455 ?
Co1 O3 2.068(7) 17_554 ?
Co2 O2 1.956(8) 45_455 ?
Co2 O2 1.956(8) . ?
Co2 O2 1.956(8) 17_554 ?
Co2 O1 2.074(3) . ?
O1 Co2 2.074(3) 4_565 ?
O1 Co2 2.074(3) 3 ?
O1 Co2 2.074(3) 2_565 ?
O2 C1 1.249(14) . ?
O3 C1 1.225(13) . ?
N1 C8 1.317(15) 7 ?
N1 C8 1.366(15) . ?
C1 C2 1.527(15) . ?
C2 C3 1.347(14) . ?
C2 C7 1.375(15) . ?
C3 C4 1.388(16) . ?
C3 H3 0.9300 . ?
C4 C5 1.376(15) . ?
C4 H4 0.9300 . ?
C5 C6 1.382(17) . ?
C5 C8 1.462(17) . ?
C6 C7 1.369(16) . ?
C6 H6 0.9300 . ?
C7 H7 0.9300 . ?
C8 N1 1.317(15) 10 ?
O1W O1W 1.1(2) 16 ?
O1W O1W 1.8(2) 47_455 ?
O1W O1W 1.8(2) 20 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O3 Co1 O3 93.2(3) 65 93 ?
O3 Co1 O3 86.8(3) 65 . ?
O3 Co1 O3 86.8(3) 93 . ?
O3 Co1 O3 93.2(3) 65 49_565 ?
O3 Co1 O3 93.2(3) 93 49_565 ?
O3 Co1 O3 180.0 . 49_565 ?
O3 Co1 O3 86.8(3) 65 45_455 ?
O3 Co1 O3 180.0(4) 93 45_455 ?
O3 Co1 O3 93.2(3) . 45_455 ?
O3 Co1 O3 86.8(3) 49_565 45_455 ?
O3 Co1 O3 180.0(6) 65 17_554 ?
O3 Co1 O3 86.8(3) 93 17_554 ?
O3 Co1 O3 93.2(3) . 17_554 ?
O3 Co1 O3 86.8(3) 49_565 17_554 ?
O3 Co1 O3 93.2(3) 45_455 17_554 ?
O2 Co2 O2 115.51(17) 45_455 . ?
O2 Co2 O2 115.51(17) 45_455 17_554 ?
O2 Co2 O2 115.51(17) . 17_554 ?
O2 Co2 O1 102.4(2) 45_455 . ?
O2 Co2 O1 102.4(2) . . ?
O2 Co2 O1 102.4(2) 17_554 . ?
Co2 O1 Co2 109.5 . 4_565 ?
Co2 O1 Co2 109.5 . 3 ?
Co2 O1 Co2 109.5 4_565 3 ?
Co2 O1 Co2 109.5 . 2_565 ?
Co2 O1 Co2 109.5 4_565 2_565 ?
Co2 O1 Co2 109.471(1) 3 2_565 ?
C1 O2 Co2 117.8(7) . . ?
C1 O3 Co1 132.2(7) . . ?
C8 N1 C8 116.0(11) 7 . ?
O3 C1 O2 124.1(10) . . ?
O3 C1 C2 117.3(10) . . ?
O2 C1 C2 118.5(10) . . ?
C3 C2 C7 118.9(10) . . ?
C3 C2 C1 120.7(10) . . ?
C7 C2 C1 120.4(10) . . ?
C2 C3 C4 121.2(11) . . ?
C2 C3 H3 119.4 . . ?
C4 C3 H3 119.4 . . ?
C5 C4 C3 120.3(11) . . ?
C5 C4 H4 119.9 . . ?
C3 C4 H4 119.9 . . ?
C4 C5 C6 118.0(10) . . ?
C4 C5 C8 121.0(10) . . ?
C6 C5 C8 120.9(10) . . ?
C7 C6 C5 121.0(11) . . ?
C7 C6 H6 119.5 . . ?
C5 C6 H6 119.5 . . ?
C6 C7 C2 120.6(11) . . ?
C6 C7 H7 119.7 . . ?
C2 C7 H7 119.7 . . ?
N1 C8 N1 124.0(11) 10 . ?
N1 C8 C5 118.0(10) 10 . ?
N1 C8 C5 118.0(10) . . ?
O1W O1W O1W 117(10) 16 47_455 ?
O1W O1W O1W 123(10) 16 20 ?
O1W O1W O1W 60.000(19) 47_455 20 ?

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        20.79
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         0.866
_refine_diff_density_min         -1.510
_refine_diff_density_rms         0.206

data_xamd130sad
_database_code_depnum_ccdc_archive 'CCDC 262519'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            none
_chemical_melting_point          'not measured'
_chemical_formula_moiety         
'Mn6 O 2(C24 H12 N3 O6) 2(C24 H13 N3 O6) 2.5(H2 O)'
_chemical_formula_sum            'C96 H55 Mn6 N12 O27.50'
_chemical_formula_weight         2146.16

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'
Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Cubic
_symmetry_space_group_name_H-M   Fd-3

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/4, -y+1/4, z'
'-x+1/4, y, -z+1/4'
'x, -y+1/4, -z+1/4'
'z, x, y'
'z, -x+1/4, -y+1/4'
'-z+1/4, -x+1/4, y'
'-z+1/4, x, -y+1/4'
'y, z, x'
'-y+1/4, z, -x+1/4'
'y, -z+1/4, -x+1/4'
'-y+1/4, -z+1/4, x'
'x, y+1/2, z+1/2'
'-x+1/4, -y+3/4, z+1/2'
'-x+1/4, y+1/2, -z+3/4'
'x, -y+3/4, -z+3/4'
'z, x+1/2, y+1/2'
'z, -x+3/4, -y+3/4'
'-z+1/4, -x+3/4, y+1/2'
'-z+1/4, x+1/2, -y+3/4'
'y, z+1/2, x+1/2'
'-y+1/4, z+1/2, -x+3/4'
'y, -z+3/4, -x+3/4'
'-y+1/4, -z+3/4, x+1/2'
'x+1/2, y, z+1/2'
'-x+3/4, -y+1/4, z+1/2'
'-x+3/4, y, -z+3/4'
'x+1/2, -y+1/4, -z+3/4'
'z+1/2, x, y+1/2'
'z+1/2, -x+1/4, -y+3/4'
'-z+3/4, -x+1/4, y+1/2'
'-z+3/4, x, -y+3/4'
'y+1/2, z, x+1/2'
'-y+3/4, z, -x+3/4'
'y+1/2, -z+1/4, -x+3/4'
'-y+3/4, -z+1/4, x+1/2'
'x+1/2, y+1/2, z'
'-x+3/4, -y+3/4, z'
'-x+3/4, y+1/2, -z+1/4'
'x+1/2, -y+3/4, -z+1/4'
'z+1/2, x+1/2, y'
'z+1/2, -x+3/4, -y+1/4'
'-z+3/4, -x+3/4, y'
'-z+3/4, x+1/2, -y+1/4'
'y+1/2, z+1/2, x'
'-y+3/4, z+1/2, -x+1/4'
'y+1/2, -z+3/4, -x+1/4'
'-y+3/4, -z+3/4, x'
'-x, -y, -z'
'x-1/4, y-1/4, -z'
'x-1/4, -y, z-1/4'
'-x, y-1/4, z-1/4'
'-z, -x, -y'
'-z, x-1/4, y-1/4'
'z-1/4, x-1/4, -y'
'z-1/4, -x, y-1/4'
'-y, -z, -x'
'y-1/4, -z, x-1/4'
'-y, z-1/4, x-1/4'
'y-1/4, z-1/4, -x'
'-x, -y+1/2, -z+1/2'
'x-1/4, y+1/4, -z+1/2'
'x-1/4, -y+1/2, z+1/4'
'-x, y+1/4, z+1/4'
'-z, -x+1/2, -y+1/2'
'-z, x+1/4, y+1/4'
'z-1/4, x+1/4, -y+1/2'
'z-1/4, -x+1/2, y+1/4'
'-y, -z+1/2, -x+1/2'
'y-1/4, -z+1/2, x+1/4'
'-y, z+1/4, x+1/4'
'y-1/4, z+1/4, -x+1/2'
'-x+1/2, -y, -z+1/2'
'x+1/4, y-1/4, -z+1/2'
'x+1/4, -y, z+1/4'
'-x+1/2, y-1/4, z+1/4'
'-z+1/2, -x, -y+1/2'
'-z+1/2, x-1/4, y+1/4'
'z+1/4, x-1/4, -y+1/2'
'z+1/4, -x, y+1/4'
'-y+1/2, -z, -x+1/2'
'y+1/4, -z, x+1/4'
'-y+1/2, z-1/4, x+1/4'
'y+1/4, z-1/4, -x+1/2'
'-x+1/2, -y+1/2, -z'
'x+1/4, y+1/4, -z'
'x+1/4, -y+1/2, z-1/4'
'-x+1/2, y+1/4, z-1/4'
'-z+1/2, -x+1/2, -y'
'-z+1/2, x+1/4, y-1/4'
'z+1/4, x+1/4, -y'
'z+1/4, -x+1/2, y-1/4'
'-y+1/2, -z+1/2, -x'
'y+1/4, -z+1/2, x-1/4'
'-y+1/2, z+1/4, x-1/4'
'y+1/4, z+1/4, -x'

_cell_length_a                   25.764(6)
_cell_length_b                   25.764(6)
_cell_length_c                   25.764(6)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     17102(7)
_cell_formula_units_Z            8
_cell_measurement_temperature    213(2)
_cell_measurement_reflns_used    1269
_cell_measurement_theta_min      2.24
_cell_measurement_theta_max      16.66

_exptl_crystal_description       block
_exptl_crystal_colour            'light yellow'
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.16
_exptl_crystal_density_meas      none
_exptl_crystal_density_diffrn    1.667
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             8680
_exptl_absorpt_coefficient_mu    0.954
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.65
_exptl_absorpt_correction_T_max  0.86
_exptl_absorpt_process_details   sadas

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        none
_diffrn_reflns_number            6561
_diffrn_reflns_av_R_equivalents  0.0936
_diffrn_reflns_av_sigmaI/netI    0.0334
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         2.24
_diffrn_reflns_theta_max         17.21
_reflns_number_total             443
_reflns_number_gt                350
_reflns_threshold_expression     >2sigma(I)

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

_refine_special_details          
;
Refinement of 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^)+(0.0850P)^2^+1486.9053P] 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    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         443
_refine_ls_number_parameters     109
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1129
_refine_ls_R_factor_gt           0.0937
_refine_ls_wR_factor_ref         0.2589
_refine_ls_wR_factor_gt          0.2425
_refine_ls_goodness_of_fit_ref   1.188
_refine_ls_restrained_S_all      1.188
_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
Mn1 Mn 0.0000 0.5000 0.0000 0.056(3) Uani 1 6 d S . .
Mn2 Mn 0.07741(13) 0.57741(13) 0.07741(13) 0.081(3) Uani 1 3 d S . .
O1 O 0.1250 0.6250 0.1250 0.030(10) Uani 1 12 d S . .
O2 O 0.0677(12) 0.5175(9) 0.1279(8) 0.146(9) Uani 1 1 d . . .
O3 O -0.0012(10) 0.5007(12) 0.0797(8) 0.144(12) Uani 1 1 d . . .
N1 N 0.0069(9) 0.3162(11) 0.2970(13) 0.101(9) Uani 1 1 d . . .
C1 C 0.0259(16) 0.4918(15) 0.1149(17) 0.122(15) Uani 1 1 d . . .
C2 C 0.0131(19) 0.4480(12) 0.1535(13) 0.079(9) Uani 1 1 d . . .
C3 C -0.0290(16) 0.4206(17) 0.1467(13) 0.098(9) Uani 1 1 d . . .
H3 H -0.0505 0.4279 0.1187 0.117 Uiso 1 1 calc R . .
C4 C -0.0421(12) 0.3807(15) 0.1808(16) 0.101(9) Uani 1 1 d . . .
H4 H -0.0717 0.3609 0.1751 0.122 Uiso 1 1 calc R . .
C5 C -0.0114(16) 0.3713(13) 0.2220(14) 0.096(9) Uani 1 1 d . . .
C6 C 0.0290(15) 0.3986(15) 0.2305(12) 0.124(13) Uani 1 1 d . . .
H6 H 0.0479 0.3931 0.2608 0.149 Uiso 1 1 calc R . .
C7 C 0.0457(12) 0.4364(13) 0.1955(19) 0.118(11) Uani 1 1 d . . .
H7 H 0.0773 0.4533 0.1999 0.142 Uiso 1 1 calc R . .
C8 C -0.025(2) 0.3251(11) 0.2582(18) 0.106(10) Uani 1 1 d . . .
O1W O -0.1250 0.3750 0.3750 0.19(7) Uiso 0.50 12 d SP . .
O2W O -0.093(2) 0.343(2) 0.407(2) 0.25(5) Uiso 0.50 3 d SP . .

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
Mn1 0.056(3) 0.056(3) 0.056(3) -0.001(2) -0.001(2) -0.001(2)
Mn2 0.081(3) 0.081(3) 0.081(3) -0.013(2) -0.013(2) -0.013(2)
O1 0.030(10) 0.030(10) 0.030(10) 0.000 0.000 0.000
O2 0.26(3) 0.093(17) 0.086(16) 0.014(13) 0.015(19) 0.019(19)
O3 0.17(2) 0.20(3) 0.066(14) 0.000(16) -0.025(14) 0.054(19)
N1 0.11(2) 0.12(3) 0.071(17) 0.04(2) -0.05(2) -0.051(18)
C1 0.14(4) 0.10(4) 0.12(4) -0.04(4) 0.08(3) -0.02(3)
C2 0.11(3) 0.06(2) 0.07(3) -0.01(2) 0.01(2) 0.00(2)
C3 0.10(3) 0.08(2) 0.12(3) 0.00(3) -0.02(2) 0.02(2)
C4 0.12(3) 0.10(3) 0.09(2) 0.04(2) -0.03(3) -0.01(2)
C5 0.11(3) 0.09(2) 0.09(3) 0.02(2) -0.02(2) -0.02(2)
C6 0.14(3) 0.11(3) 0.12(3) 0.02(2) -0.02(2) -0.09(2)
C7 0.13(3) 0.09(3) 0.13(3) -0.02(2) -0.06(3) -0.06(2)
C8 0.11(3) 0.10(3) 0.11(3) 0.01(3) -0.01(2) -0.06(3)

_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
Mn1 O3 2.05(2) 93 ?
Mn1 O3 2.05(2) 45_455 ?
Mn1 O3 2.05(2) . ?
Mn1 O3 2.05(2) 49_565 ?
Mn1 O3 2.05(2) 17_554 ?
Mn1 O3 2.05(2) 65 ?
Mn2 O2 2.03(2) 17_554 ?
Mn2 O2 2.03(2) . ?
Mn2 O2 2.03(2) 45_455 ?
Mn2 O1 2.124(6) . ?
O1 Mn2 2.124(6) 2_565 ?
O1 Mn2 2.124(6) 4_565 ?
O1 Mn2 2.124(6) 3 ?
O2 C1 1.31(4) . ?
O3 C1 1.17(5) . ?
N1 C8 1.32(4) . ?
N1 C8 1.34(3) 7 ?
C1 C2 1.54(5) . ?
C2 C3 1.30(3) . ?
C2 C7 1.40(3) . ?
C3 C4 1.39(4) . ?
C3 H3 0.9300 . ?
C4 C5 1.35(3) . ?
C4 H4 0.9300 . ?
C5 C6 1.28(3) . ?
C5 C8 1.55(4) . ?
C6 C7 1.39(4) . ?
C6 H6 0.9300 . ?
C7 H7 0.9300 . ?
C8 N1 1.34(3) 10 ?
O1W O2W 1.42(10) 27_455 ?
O1W O2W 1.42(10) . ?
O1W O2W 1.42(10) 16 ?
O1W O2W 1.42(10) 38_455 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O3 Mn1 O3 180.0(14) 93 45_455 ?
O3 Mn1 O3 89.6(12) 93 . ?
O3 Mn1 O3 90.4(12) 45_455 . ?
O3 Mn1 O3 90.4(12) 93 49_565 ?
O3 Mn1 O3 89.6(12) 45_455 49_565 ?
O3 Mn1 O3 180.0(17) . 49_565 ?
O3 Mn1 O3 89.6(12) 93 17_554 ?
O3 Mn1 O3 90.4(12) 45_455 17_554 ?
O3 Mn1 O3 90.4(12) . 17_554 ?
O3 Mn1 O3 89.6(12) 49_565 17_554 ?
O3 Mn1 O3 90.4(12) 93 65 ?
O3 Mn1 O3 89.6(12) 45_455 65 ?
O3 Mn1 O3 89.6(12) . 65 ?
O3 Mn1 O3 90.4(12) 49_565 65 ?
O3 Mn1 O3 180.0(17) 17_554 65 ?
O2 Mn2 O2 118.1(4) 17_554 . ?
O2 Mn2 O2 118.1(4) 17_554 45_455 ?
O2 Mn2 O2 118.1(4) . 45_455 ?
O2 Mn2 O1 98.1(8) 17_554 . ?
O2 Mn2 O1 98.1(8) . . ?
O2 Mn2 O1 98.1(8) 45_455 . ?
Mn2 O1 Mn2 109.5 . 2_565 ?
Mn2 O1 Mn2 109.5 . 4_565 ?
Mn2 O1 Mn2 109.5 2_565 4_565 ?
Mn2 O1 Mn2 109.5 . 3 ?
Mn2 O1 Mn2 109.471(1) 2_565 3 ?
Mn2 O1 Mn2 109.5 4_565 3 ?
C1 O2 Mn2 109(3) . . ?
C1 O3 Mn1 140(3) . . ?
C8 N1 C8 111(3) . 7 ?
O3 C1 O2 126(4) . . ?
O3 C1 C2 121(4) . . ?
O2 C1 C2 112(4) . . ?
C3 C2 C7 119(3) . . ?
C3 C2 C1 119(4) . . ?
C7 C2 C1 122(5) . . ?
C2 C3 C4 121(3) . . ?
C2 C3 H3 119.5 . . ?
C4 C3 H3 119.5 . . ?
C5 C4 C3 119(3) . . ?
C5 C4 H4 120.4 . . ?
C3 C4 H4 120.4 . . ?
C6 C5 C4 121(3) . . ?
C6 C5 C8 120(4) . . ?
C4 C5 C8 119(4) . . ?
C5 C6 C7 122(3) . . ?
C5 C6 H6 119.2 . . ?
C7 C6 H6 119.2 . . ?
C6 C7 C2 118(3) . . ?
C6 C7 H7 121.2 . . ?
C2 C7 H7 121.2 . . ?
N1 C8 N1 128(3) . 10 ?
N1 C8 C5 117(5) . . ?
N1 C8 C5 115(5) 10 . ?
O2W O1W O2W 109.471(4) 27_455 . ?
O2W O1W O2W 109.471(14) 27_455 16 ?
O2W O1W O2W 109.47(4) . 16 ?
O2W O1W O2W 109.471(10) 27_455 38_455 ?
O2W O1W O2W 109.5 . 38_455 ?
O2W O1W O2W 109.471(15) 16 38_455 ?

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        17.21
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         0.514
_refine_diff_density_min         -0.424
_refine_diff_density_rms         0.102

data_xamd199
_database_code_depnum_ccdc_archive 'CCDC 262520'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            none
_chemical_melting_point          'not measured'
_chemical_formula_moiety         
'Zn6 O 2(C24 H12 N3 O6) 2(C24 H13 N3 O6) 2(H2O)'
_chemical_formula_sum            'C96 H54 N12 O27 Zn6'
_chemical_formula_weight         2199.73

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           Cubic
_symmetry_space_group_name_H-M   Fd-3

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/4, -y+1/4, z'
'-x+1/4, y, -z+1/4'
'x, -y+1/4, -z+1/4'
'z, x, y'
'z, -x+1/4, -y+1/4'
'-z+1/4, -x+1/4, y'
'-z+1/4, x, -y+1/4'
'y, z, x'
'-y+1/4, z, -x+1/4'
'y, -z+1/4, -x+1/4'
'-y+1/4, -z+1/4, x'
'x, y+1/2, z+1/2'
'-x+1/4, -y+3/4, z+1/2'
'-x+1/4, y+1/2, -z+3/4'
'x, -y+3/4, -z+3/4'
'z, x+1/2, y+1/2'
'z, -x+3/4, -y+3/4'
'-z+1/4, -x+3/4, y+1/2'
'-z+1/4, x+1/2, -y+3/4'
'y, z+1/2, x+1/2'
'-y+1/4, z+1/2, -x+3/4'
'y, -z+3/4, -x+3/4'
'-y+1/4, -z+3/4, x+1/2'
'x+1/2, y, z+1/2'
'-x+3/4, -y+1/4, z+1/2'
'-x+3/4, y, -z+3/4'
'x+1/2, -y+1/4, -z+3/4'
'z+1/2, x, y+1/2'
'z+1/2, -x+1/4, -y+3/4'
'-z+3/4, -x+1/4, y+1/2'
'-z+3/4, x, -y+3/4'
'y+1/2, z, x+1/2'
'-y+3/4, z, -x+3/4'
'y+1/2, -z+1/4, -x+3/4'
'-y+3/4, -z+1/4, x+1/2'
'x+1/2, y+1/2, z'
'-x+3/4, -y+3/4, z'
'-x+3/4, y+1/2, -z+1/4'
'x+1/2, -y+3/4, -z+1/4'
'z+1/2, x+1/2, y'
'z+1/2, -x+3/4, -y+1/4'
'-z+3/4, -x+3/4, y'
'-z+3/4, x+1/2, -y+1/4'
'y+1/2, z+1/2, x'
'-y+3/4, z+1/2, -x+1/4'
'y+1/2, -z+3/4, -x+1/4'
'-y+3/4, -z+3/4, x'
'-x, -y, -z'
'x-1/4, y-1/4, -z'
'x-1/4, -y, z-1/4'
'-x, y-1/4, z-1/4'
'-z, -x, -y'
'-z, x-1/4, y-1/4'
'z-1/4, x-1/4, -y'
'z-1/4, -x, y-1/4'
'-y, -z, -x'
'y-1/4, -z, x-1/4'
'-y, z-1/4, x-1/4'
'y-1/4, z-1/4, -x'
'-x, -y+1/2, -z+1/2'
'x-1/4, y+1/4, -z+1/2'
'x-1/4, -y+1/2, z+1/4'
'-x, y+1/4, z+1/4'
'-z, -x+1/2, -y+1/2'
'-z, x+1/4, y+1/4'
'z-1/4, x+1/4, -y+1/2'
'z-1/4, -x+1/2, y+1/4'
'-y, -z+1/2, -x+1/2'
'y-1/4, -z+1/2, x+1/4'
'-y, z+1/4, x+1/4'
'y-1/4, z+1/4, -x+1/2'
'-x+1/2, -y, -z+1/2'
'x+1/4, y-1/4, -z+1/2'
'x+1/4, -y, z+1/4'
'-x+1/2, y-1/4, z+1/4'
'-z+1/2, -x, -y+1/2'
'-z+1/2, x-1/4, y+1/4'
'z+1/4, x-1/4, -y+1/2'
'z+1/4, -x, y+1/4'
'-y+1/2, -z, -x+1/2'
'y+1/4, -z, x+1/4'
'-y+1/2, z-1/4, x+1/4'
'y+1/4, z-1/4, -x+1/2'
'-x+1/2, -y+1/2, -z'
'x+1/4, y+1/4, -z'
'x+1/4, -y+1/2, z-1/4'
'-x+1/2, y+1/4, z-1/4'
'-z+1/2, -x+1/2, -y'
'-z+1/2, x+1/4, y-1/4'
'z+1/4, x+1/4, -y'
'z+1/4, -x+1/2, y-1/4'
'-y+1/2, -z+1/2, -x'
'y+1/4, -z+1/2, x-1/4'
'-y+1/2, z+1/4, x-1/4'
'y+1/4, z+1/4, -x'

_cell_length_a                   25.6887(3)
_cell_length_b                   25.6887(3)
_cell_length_c                   25.6887(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     16952.2(3)
_cell_formula_units_Z            8
_cell_measurement_temperature    213(2)
_cell_measurement_reflns_used    3844
_cell_measurement_theta_min      2.24
_cell_measurement_theta_max      22.23

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.13
_exptl_crystal_density_meas      none
_exptl_crystal_density_diffrn    1.724
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             8880
_exptl_absorpt_coefficient_mu    1.765
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.768
_exptl_absorpt_correction_T_max  0.769
_exptl_absorpt_process_details   sadas

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        none
_diffrn_reflns_number            18078
_diffrn_reflns_av_R_equivalents  0.0508
_diffrn_reflns_av_sigmaI/netI    0.0222
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_theta_min         2.24
_diffrn_reflns_theta_max         22.71
_reflns_number_total             964
_reflns_number_gt                797
_reflns_threshold_expression     >2sigma(I)

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

_refine_special_details          
;
Refinement of 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^)+(0.0712P)^2^+119.5708P] 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    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         964
_refine_ls_number_parameters     109
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0479
_refine_ls_R_factor_gt           0.0399
_refine_ls_wR_factor_ref         0.1256
_refine_ls_wR_factor_gt          0.1224
_refine_ls_goodness_of_fit_ref   1.106
_refine_ls_restrained_S_all      1.106
_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 0.0000 0.5000 0.0000 0.0241(4) Uani 1 6 d S . .
Zn2 Zn 0.07855(2) 0.57855(2) 0.07855(2) 0.0319(4) Uani 1 3 d S . .
O1 O 0.1250 0.6250 0.1250 0.016(2) Uani 1 12 d S . .
O2 O 0.06349(15) 0.52018(14) 0.12489(15) 0.0448(10) Uani 1 1 d . . .
O3 O -0.00826(14) 0.50335(15) 0.07996(14) 0.0414(10) Uani 1 1 d . . .
N1 N 0.00454(19) 0.31874(19) 0.29718(19) 0.0519(14) Uani 1 1 d . . .
C1 C 0.0226(2) 0.4941(2) 0.1155(2) 0.0413(14) Uani 1 1 d . . .
C2 C 0.0095(2) 0.4501(2) 0.1527(2) 0.0384(13) Uani 1 1 d . . .
C3 C -0.0343(2) 0.4205(2) 0.1445(2) 0.0510(16) Uani 1 1 d . . .
H3 H -0.0557 0.4272 0.1161 0.061 Uiso 1 1 calc R . .
C4 C -0.0465(3) 0.3808(3) 0.1784(2) 0.0557(17) Uani 1 1 d . . .
H4 H -0.0758 0.3605 0.1723 0.067 Uiso 1 1 calc R . .
C5 C -0.0155(2) 0.3708(2) 0.2215(2) 0.0460(15) Uani 1 1 d . . .
C6 C 0.0274(3) 0.4013(3) 0.2292(3) 0.066(2) Uani 1 1 d . . .
H6 H 0.0483 0.3956 0.2583 0.079 Uiso 1 1 calc R . .
C7 C 0.0402(3) 0.4402(3) 0.1947(3) 0.0608(19) Uani 1 1 d . . .
H7 H 0.0701 0.4599 0.2001 0.073 Uiso 1 1 calc R . .
C8 C -0.0275(2) 0.3270(2) 0.2566(2) 0.0486(16) Uani 1 1 d . . .
O1W O -0.1077(9) 0.3577(9) 0.3923(9) 0.25(3) Uiso 0.50 3 d SP . .

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 0.0241(4) 0.0241(4) 0.0241(4) -0.0037(3) -0.0037(3) -0.0037(3)
Zn2 0.0319(4) 0.0319(4) 0.0319(4) -0.0017(2) -0.0017(2) -0.0017(2)
O1 0.016(2) 0.016(2) 0.016(2) 0.000 0.000 0.000
O2 0.044(2) 0.045(2) 0.045(2) 0.0046(18) -0.0008(19) -0.0122(19)
O3 0.043(2) 0.054(2) 0.026(2) 0.0085(16) -0.0012(17) 0.0051(18)
N1 0.052(3) 0.053(3) 0.050(3) 0.017(3) -0.018(3) -0.020(2)
C1 0.048(4) 0.041(3) 0.035(3) 0.000(3) 0.008(3) 0.009(3)
C2 0.047(3) 0.032(3) 0.037(3) 0.005(2) 0.000(3) -0.001(3)
C3 0.053(4) 0.054(4) 0.045(4) 0.017(3) -0.011(3) -0.008(3)
C4 0.056(4) 0.055(4) 0.056(4) 0.015(3) -0.018(3) -0.019(3)
C5 0.049(3) 0.046(3) 0.043(3) 0.014(3) -0.015(3) -0.009(3)
C6 0.077(5) 0.064(4) 0.056(4) 0.027(3) -0.035(4) -0.035(4)
C7 0.067(4) 0.057(4) 0.059(4) 0.015(3) -0.027(4) -0.032(3)
C8 0.048(4) 0.048(4) 0.049(4) 0.012(3) -0.016(3) -0.016(3)

_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 O3 2.067(4) 65 ?
Zn1 O3 2.067(4) 45_455 ?
Zn1 O3 2.067(4) . ?
Zn1 O3 2.067(4) 49_565 ?
Zn1 O3 2.067(4) 93 ?
Zn1 O3 2.067(4) 17_554 ?
Zn2 O2 1.953(4) 45_455 ?
Zn2 O2 1.953(4) . ?
Zn2 O2 1.953(4) 17_554 ?
Zn2 O1 2.0668(10) . ?
O1 Zn2 2.0668(10) 4_565 ?
O1 Zn2 2.0668(10) 2_565 ?
O1 Zn2 2.0668(10) 3 ?
O2 C1 1.269(7) . ?
O3 C1 1.231(7) . ?
N1 C8 1.338(7) 7 ?
N1 C8 1.345(7) . ?
C1 C2 1.519(7) . ?
C2 C7 1.361(8) . ?
C2 C3 1.373(8) . ?
C3 C4 1.376(8) . ?
C3 H3 0.9300 . ?
C4 C5 1.387(8) . ?
C4 H4 0.9300 . ?
C5 C6 1.367(8) . ?
C5 C8 1.474(8) . ?
C6 C7 1.377(8) . ?
C6 H6 0.9300 . ?
C7 H7 0.9300 . ?
C8 N1 1.338(7) 10 ?
O1W O1W 1.26(6) 38_455 ?
O1W O1W 1.26(6) 27_455 ?
O1W O1W 1.26(6) 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
O3 Zn1 O3 86.28(14) 65 45_455 ?
O3 Zn1 O3 86.28(14) 65 . ?
O3 Zn1 O3 93.72(14) 45_455 . ?
O3 Zn1 O3 93.72(14) 65 49_565 ?
O3 Zn1 O3 86.28(14) 45_455 49_565 ?
O3 Zn1 O3 180.0 . 49_565 ?
O3 Zn1 O3 93.72(14) 65 93 ?
O3 Zn1 O3 180.0(2) 45_455 93 ?
O3 Zn1 O3 86.28(14) . 93 ?
O3 Zn1 O3 93.72(14) 49_565 93 ?
O3 Zn1 O3 180.0(3) 65 17_554 ?
O3 Zn1 O3 93.72(14) 45_455 17_554 ?
O3 Zn1 O3 93.72(14) . 17_554 ?
O3 Zn1 O3 86.28(14) 49_565 17_554 ?
O3 Zn1 O3 86.28(14) 93 17_554 ?
O2 Zn2 O2 115.88(7) 45_455 . ?
O2 Zn2 O2 115.88(7) 45_455 17_554 ?
O2 Zn2 O2 115.88(7) . 17_554 ?
O2 Zn2 O1 101.87(11) 45_455 . ?
O2 Zn2 O1 101.87(11) . . ?
O2 Zn2 O1 101.87(11) 17_554 . ?
Zn2 O1 Zn2 109.5 4_565 . ?
Zn2 O1 Zn2 109.5 4_565 2_565 ?
Zn2 O1 Zn2 109.5 . 2_565 ?
Zn2 O1 Zn2 109.5 4_565 3 ?
Zn2 O1 Zn2 109.471(1) . 3 ?
Zn2 O1 Zn2 109.5 2_565 3 ?
C1 O2 Zn2 116.9(4) . . ?
C1 O3 Zn1 131.4(4) . . ?
C8 N1 C8 115.9(5) 7 . ?
O3 C1 O2 124.9(5) . . ?
O3 C1 C2 117.8(5) . . ?
O2 C1 C2 117.1(5) . . ?
C7 C2 C3 119.6(5) . . ?
C7 C2 C1 120.6(5) . . ?
C3 C2 C1 119.8(5) . . ?
C2 C3 C4 120.0(5) . . ?
C2 C3 H3 120.0 . . ?
C4 C3 H3 120.0 . . ?
C3 C4 C5 120.8(6) . . ?
C3 C4 H4 119.6 . . ?
C5 C4 H4 119.6 . . ?
C6 C5 C4 118.1(5) . . ?
C6 C5 C8 121.1(5) . . ?
C4 C5 C8 120.7(5) . . ?
C5 C6 C7 121.0(6) . . ?
C5 C6 H6 119.5 . . ?
C7 C6 H6 119.5 . . ?
C2 C7 C6 120.5(6) . . ?
C2 C7 H7 119.8 . . ?
C6 C7 H7 119.8 . . ?
N1 C8 N1 124.1(5) 10 . ?
N1 C8 C5 118.1(5) 10 . ?
N1 C8 C5 117.8(5) . . ?
O1W O1W O1W 60.000(8) 38_455 27_455 ?
O1W O1W O1W 60.000(4) 38_455 16 ?
O1W O1W O1W 60.000(3) 27_455 16 ?

_diffrn_measured_fraction_theta_max 0.997
_diffrn_reflns_theta_full        22.71
_diffrn_measured_fraction_theta_full 0.997
_refine_diff_density_max         0.874
_refine_diff_density_min         -0.735
_refine_diff_density_rms         0.094