# Electronic Supplementary Material for CrystEngComm
# This journal is (c) The Royal Society of Chemistry 2008

data_global
_journal_name_full               CrystEngComm

_journal_coden_Cambridge         1350
_journal_volume                  ?
_journal_page_first              ?
_journal_year                    ?

_publ_contact_author_name        'ProfD En-Qing Gao'
_publ_contact_author_email       EQGAO@CHEM.ECNU.EDU.CN

_publ_section_title              
;
Supramolecular Networks Assembled from Binuclear
Complexes with Pyridazine-3,6-dicarboxylate
;
loop_
_publ_author_name
'En-Qing Gao'
'Ai-Ling Cheng'
'Wei-Wei Sun'
'Qi Yue'

# Attachment '10.cif'

data_10
_database_code_depnum_ccdc_archive 'CCDC 683331'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C18 H10 N6 Na2 O14 Zn2'
_chemical_formula_weight         711.04

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'
Zn Zn 0.2839 1.4301 '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'
Na Na 0.0362 0.0249 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_H-M   Cmcm

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

_cell_length_a                   11.2436(12)
_cell_length_b                   15.2627(16)
_cell_length_c                   13.0841(14)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     2245.3(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    8156
_cell_measurement_theta_min      2.25
_cell_measurement_theta_max      27.21

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.10
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.103
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1416
_exptl_absorpt_coefficient_mu    2.269
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.7724
_exptl_absorpt_correction_T_max  0.8049
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         '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_%        ?
_diffrn_reflns_number            8117
_diffrn_reflns_av_R_equivalents  0.0438
_diffrn_reflns_av_sigmaI/netI    0.0279
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         2.25
_diffrn_reflns_theta_max         26.00
_reflns_number_total             1214
_reflns_number_gt                1115
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_structure_solution    'Bruker SHELXTL'
_computing_structure_refinement  'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0335P)²+28.3718P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     SHELXL
_refine_ls_extinction_coef       0.0103(8)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         1214
_refine_ls_number_parameters     126
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0619
_refine_ls_R_factor_gt           0.0565
_refine_ls_wR_factor_ref         0.1302
_refine_ls_wR_factor_gt          0.1262
_refine_ls_goodness_of_fit_ref   1.110
_refine_ls_restrained_S_all      1.109
_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 0.18202(6) 0.48360(5) 0.7500 0.0354(4) Uani 1 2 d S . .
Na1 Na 0.5000 0.5549(4) 0.9218(5) 0.0501(15) Uani 0.50 2 d SP . .
Na2 Na 0.5000 0.3502(3) 0.7500 0.0668(17) Uani 1 4 d S . .
O1 O 0.2909(4) 0.3789(3) 0.7500 0.0578(19) Uani 1 2 d S . .
O2 O 0.3138(4) 0.2350(3) 0.7500 0.0603(19) Uani 1 2 d S . .
O3 O 0.2911(4) 0.5413(3) 0.8561(5) 0.0730(13) Uani 1 1 d . . .
O4 O 0.3089(6) 0.6468(3) 0.9719(7) 0.0904(14) Uani 1 1 d . . .
N1 N 0.0597(4) 0.3686(3) 0.7500 0.0263(12) Uani 1 2 d S . .
N2 N 0.0594(4) 0.5509(2) 0.8612(3) 0.0340(10) Uani 1 1 d . . .
C1 C 0.1181(6) 0.2933(4) 0.7500 0.0397(19) Uani 1 2 d S . .
C2 C 0.0606(7) 0.2133(5) 0.7500 0.060(2) Uani 1 2 d S . .
H2 H 0.1032 0.1611 0.7500 0.106 Uiso 1 2 calc SR . .
C3 C 0.2531(6) 0.3016(5) 0.7500 0.0415(19) Uani 1 2 d S . .
C4 C 0.1173(6) 0.6077(3) 0.9195(5) 0.0483(16) Uani 1 1 d . . .
C5 C 0.0601(7) 0.6710(4) 0.9776(5) 0.064(2) Uani 1 1 d . . .
H5 H 0.1029 0.7120 1.0152 0.076 Uiso 1 1 calc R . .
C6 C 0.2513(7) 0.5989(4) 0.9154(8) 0.073(2) Uani 1 1 d . . .
O5 O 0.5000 0.5405(9) 1.1020(10) 0.041(3) Uani 0.50 2 d SPD . .
H5W H 0.556(8) 0.508(7) 1.124(10) 0.061 Uiso 0.50 1 d PD . .
O6 O 0.5000 0.3994(9) 0.9017(9) 0.036(2) Uani 0.50 2 d SPD . .
H6W H 0.446(8) 0.386(7) 0.944(7) 0.054 Uiso 0.50 1 d PD . .


_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 2.013(5) . ?
Zn1 O3 2.051(5) . ?
Zn1 O3 2.051(5) 10_557 ?
Zn1 N1 2.229(5) . ?
Zn1 N2 2.252(4) . ?
Zn1 N2 2.252(4) 10_557 ?
Na1 O5 1.489(14) 9_667 ?
Na1 O5 2.368(14) . ?
Na1 O6 2.388(14) . ?
Na1 O6 2.413(13) 9_667 ?
Na1 O3 2.509(5) . ?
Na1 O3 2.509(5) 12_655 ?
Na1 O4 2.648(8) 12_655 ?
Na1 O4 2.648(8) . ?
Na1 Na1 2.645(12) 9_667 ?
Na1 C6 2.877(8) 12_655 ?
Na1 C6 2.877(8) . ?
Na1 Na2 3.848(7) . ?
Na2 O6 2.122(12) . ?
Na2 O6 2.122(12) 10_557 ?
Na2 O1 2.391(5) . ?
Na2 O1 2.391(5) 3_656 ?
Na2 O5 2.556(13) 9_667 ?
Na2 O5 2.556(13) 2_664 ?
Na2 O2 2.734(6) . ?
Na2 O2 2.734(6) 3_656 ?
Na2 C3 2.874(7) 3_656 ?
Na2 C3 2.874(7) . ?
Na2 Na1 3.848(7) 10_557 ?
Na2 H6W 2.67(8) . ?
O1 C3 1.253(8) . ?
O2 C3 1.225(9) . ?
O3 C6 1.255(10) . ?
O4 C6 1.226(8) . ?
N1 C1 1.325(8) . ?
N1 N1 1.342(10) 3_556 ?
N2 C4 1.325(6) . ?
N2 N2 1.337(8) 12 ?
C1 C2 1.382(10) . ?
C1 C3 1.523(9) . ?
C2 C2 1.362(15) 3_556 ?
C2 H2 0.9300 . ?
C4 C5 1.388(8) . ?
C4 C6 1.514(11) . ?
C5 C5 1.351(15) 12 ?
C5 H5 0.9300 . ?
O5 O6 0.919(14) 9_667 ?
O5 Na1 1.489(14) 9_667 ?
O5 Na2 2.556(13) 9_667 ?
O5 H5W 0.85(2) . ?
O6 O5 0.919(14) 9_667 ?
O6 Na1 2.413(13) 9_667 ?
O6 H6W 0.85(2) . ?

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 O3 88.71(16) . . ?
O1 Zn1 O3 88.71(16) . 10_557 ?
O3 Zn1 O3 85.2(4) . 10_557 ?
O1 Zn1 N1 75.5(2) . . ?
O3 Zn1 N1 134.99(18) . . ?
O3 Zn1 N1 134.99(18) 10_557 . ?
O1 Zn1 N2 137.22(11) . . ?
O3 Zn1 N2 74.51(19) . . ?
O3 Zn1 N2 127.41(16) 10_557 . ?
N1 Zn1 N2 88.92(14) . . ?
O1 Zn1 N2 137.22(11) . 10_557 ?
O3 Zn1 N2 127.41(16) . 10_557 ?
O3 Zn1 N2 74.51(19) 10_557 10_557 ?
N1 Zn1 N2 88.92(15) . 10_557 ?
N2 Zn1 N2 80.5(2) . 10_557 ?
O5 Na1 O5 96.7(6) 9_667 . ?
O5 Na1 O6 5.7(6) 9_667 . ?
O5 Na1 O6 91.0(5) . . ?
O5 Na1 O6 118.9(6) 9_667 9_667 ?
O5 Na1 O6 22.1(3) . 9_667 ?
O6 Na1 O6 113.1(4) . 9_667 ?
O5 Na1 O3 81.3(2) 9_667 . ?
O5 Na1 O3 109.5(2) . . ?
O6 Na1 O3 83.14(19) . . ?
O6 Na1 O3 110.6(2) 9_667 . ?
O5 Na1 O3 81.3(2) 9_667 12_655 ?
O5 Na1 O3 109.5(2) . 12_655 ?
O6 Na1 O3 83.14(19) . 12_655 ?
O6 Na1 O3 110.6(2) 9_667 12_655 ?
O3 Na1 O3 138.8(4) . 12_655 ?
O5 Na1 O4 124.73(19) 9_667 12_655 ?
O5 Na1 O4 78.6(3) . 12_655 ?
O6 Na1 O4 123.62(19) . 12_655 ?
O6 Na1 O4 67.0(3) 9_667 12_655 ?
O3 Na1 O4 152.6(3) . 12_655 ?
O3 Na1 O4 50.90(17) 12_655 12_655 ?
O5 Na1 O4 124.73(19) 9_667 . ?
O5 Na1 O4 78.6(3) . . ?
O6 Na1 O4 123.6(2) . . ?
O6 Na1 O4 67.0(3) 9_667 . ?
O3 Na1 O4 50.90(17) . . ?
O3 Na1 O4 152.6(3) 12_655 . ?
O4 Na1 O4 108.4(3) 12_655 . ?
O5 Na1 Na1 62.8(5) 9_667 9_667 ?
O5 Na1 Na1 34.0(4) . 9_667 ?
O6 Na1 Na1 57.0(3) . 9_667 ?
O6 Na1 Na1 56.1(4) 9_667 9_667 ?
O3 Na1 Na1 102.3(2) . 9_667 ?
O3 Na1 Na1 102.3(2) 12_655 9_667 ?
O4 Na1 Na1 98.2(3) 12_655 9_667 ?
O4 Na1 Na1 98.2(3) . 9_667 ?
O5 Na1 C6 102.84(17) 9_667 12_655 ?
O5 Na1 C6 92.9(3) . 12_655 ?
O6 Na1 C6 103.23(16) . 12_655 ?
O6 Na1 C6 87.7(2) 9_667 12_655 ?
O3 Na1 C6 156.8(4) . 12_655 ?
O3 Na1 C6 25.80(19) 12_655 12_655 ?
O4 Na1 C6 25.20(17) 12_655 12_655 ?
O4 Na1 C6 132.2(3) . 12_655 ?
Na1 Na1 C6 99.8(2) 9_667 12_655 ?
O5 Na1 C6 102.84(17) 9_667 . ?
O5 Na1 C6 92.9(3) . . ?
O6 Na1 C6 103.23(16) . . ?
O6 Na1 C6 87.7(2) 9_667 . ?
O3 Na1 C6 25.80(19) . . ?
O3 Na1 C6 156.8(4) 12_655 . ?
O4 Na1 C6 132.2(3) 12_655 . ?
O4 Na1 C6 25.20(17) . . ?
Na1 Na1 C6 99.8(2) 9_667 . ?
C6 Na1 C6 152.8(3) 12_655 . ?
O5 Na1 Na2 23.7(5) 9_667 . ?
O5 Na1 Na2 120.4(4) . . ?
O6 Na1 Na2 29.4(3) . . ?
O6 Na1 Na2 142.6(4) 9_667 . ?
O3 Na1 Na2 74.52(18) . . ?
O3 Na1 Na2 74.52(18) 12_655 . ?
O4 Na1 Na2 125.08(15) 12_655 . ?
O4 Na1 Na2 125.08(15) . . ?
Na1 Na1 Na2 86.4(3) 9_667 . ?
C6 Na1 Na2 99.94(18) 12_655 . ?
C6 Na1 Na2 99.94(18) . . ?
O6 Na2 O6 138.6(7) . 10_557 ?
O6 Na2 O1 86.30(10) . . ?
O6 Na2 O1 86.30(10) 10_557 . ?
O6 Na2 O1 86.30(10) . 3_656 ?
O6 Na2 O1 86.30(10) 10_557 3_656 ?
O1 Na2 O1 158.9(3) . 3_656 ?
O6 Na2 O5 20.0(4) . 9_667 ?
O6 Na2 O5 118.6(6) 10_557 9_667 ?
O1 Na2 O5 83.15(12) . 9_667 ?
O1 Na2 O5 83.15(12) 3_656 9_667 ?
O6 Na2 O5 118.6(6) . 2_664 ?
O6 Na2 O5 20.0(4) 10_557 2_664 ?
O1 Na2 O5 83.15(12) . 2_664 ?
O1 Na2 O5 83.15(12) 3_656 2_664 ?
O5 Na2 O5 98.5(6) 9_667 2_664 ?
O6 Na2 O2 103.1(2) . . ?
O6 Na2 O2 103.1(2) 10_557 . ?
O1 Na2 O2 50.55(16) . . ?
O1 Na2 O2 150.5(3) 3_656 . ?
O5 Na2 O2 114.81(17) 9_667 . ?
O5 Na2 O2 114.81(17) 2_664 . ?
O6 Na2 O2 103.1(2) . 3_656 ?
O6 Na2 O2 103.1(2) 10_557 3_656 ?
O1 Na2 O2 150.5(3) . 3_656 ?
O1 Na2 O2 50.55(16) 3_656 3_656 ?
O5 Na2 O2 114.81(17) 9_667 3_656 ?
O5 Na2 O2 114.81(17) 2_664 3_656 ?
O2 Na2 O2 100.0(3) . 3_656 ?
O6 Na2 C3 95.23(10) . 3_656 ?
O6 Na2 C3 95.23(10) 10_557 3_656 ?
O1 Na2 C3 175.6(3) . 3_656 ?
O1 Na2 C3 25.49(18) 3_656 3_656 ?
O5 Na2 C3 99.69(12) 9_667 3_656 ?
O5 Na2 C3 99.69(12) 2_664 3_656 ?
O2 Na2 C3 125.0(2) . 3_656 ?
O2 Na2 C3 25.07(17) 3_656 3_656 ?
O6 Na2 C3 95.23(10) . . ?
O6 Na2 C3 95.23(10) 10_557 . ?
O1 Na2 C3 25.49(18) . . ?
O1 Na2 C3 175.6(3) 3_656 . ?
O5 Na2 C3 99.69(12) 9_667 . ?
O5 Na2 C3 99.69(12) 2_664 . ?
O2 Na2 C3 25.07(17) . . ?
O2 Na2 C3 125.0(2) 3_656 . ?
C3 Na2 C3 150.1(3) 3_656 . ?
O6 Na2 Na1 33.6(4) . . ?
O6 Na2 Na1 105.0(4) 10_557 . ?
O1 Na2 Na1 81.47(14) . . ?
O1 Na2 Na1 81.47(14) 3_656 . ?
O5 Na2 Na1 13.5(3) 9_667 . ?
O5 Na2 Na1 85.0(3) 2_664 . ?
O2 Na2 Na1 121.47(9) . . ?
O2 Na2 Na1 121.47(9) 3_656 . ?
C3 Na2 Na1 102.09(13) 3_656 . ?
C3 Na2 Na1 102.09(13) . . ?
O6 Na2 Na1 105.0(4) . 10_557 ?
O6 Na2 Na1 33.6(4) 10_557 10_557 ?
O1 Na2 Na1 81.47(14) . 10_557 ?
O1 Na2 Na1 81.47(14) 3_656 10_557 ?
O5 Na2 Na1 85.0(3) 9_667 10_557 ?
O5 Na2 Na1 13.5(3) 2_664 10_557 ?
O2 Na2 Na1 121.47(9) . 10_557 ?
O2 Na2 Na1 121.47(9) 3_656 10_557 ?
C3 Na2 Na1 102.09(13) 3_656 10_557 ?
C3 Na2 Na1 102.09(13) . 10_557 ?
Na1 Na2 Na1 71.5(2) . 10_557 ?
O6 Na2 H6W 16(2) . . ?
O6 Na2 H6W 145(2) 10_557 . ?
O1 Na2 H6W 75(2) . . ?
O1 Na2 H6W 101(2) 3_656 . ?
O5 Na2 H6W 31(2) 9_667 . ?
O5 Na2 H6W 126(2) 2_664 . ?
O2 Na2 H6W 87(2) . . ?
O2 Na2 H6W 108(3) 3_656 . ?
C3 Na2 H6W 106(2) 3_656 . ?
C3 Na2 H6W 80(2) . . ?
Na1 Na2 H6W 44(2) . . ?
Na1 Na2 H6W 113(2) 10_557 . ?
C3 O1 Zn1 122.7(5) . . ?
C3 O1 Na2 99.3(4) . . ?
Zn1 O1 Na2 138.0(3) . . ?
C3 O2 Na2 83.9(4) . . ?
C6 O3 Zn1 120.4(4) . . ?
C6 O3 Na1 93.7(4) . . ?
Zn1 O3 Na1 145.8(3) . . ?
C6 O4 Na1 87.9(5) . . ?
C1 N1 N1 119.7(4) . 3_556 ?
C1 N1 Zn1 112.2(4) . . ?
N1 N1 Zn1 128.09(13) 3_556 . ?
C4 N2 N2 119.4(3) . 12 ?
C4 N2 Zn1 111.7(4) . . ?
N2 N2 Zn1 127.74(10) 12 . ?
N1 C1 C2 122.3(6) . . ?
N1 C1 C3 114.9(6) . . ?
C2 C1 C3 122.7(6) . . ?
C2 C2 C1 117.9(4) 3_556 . ?
C2 C2 H2 121.0 3_556 . ?
C1 C2 H2 121.0 . . ?
O2 C3 O1 126.3(7) . . ?
O2 C3 C1 119.1(6) . . ?
O1 C3 C1 114.6(6) . . ?
O2 C3 Na2 71.1(4) . . ?
O1 C3 Na2 55.2(4) . . ?
C1 C3 Na2 169.9(5) . . ?
N2 C4 C5 122.9(6) . . ?
N2 C4 C6 114.2(5) . . ?
C5 C4 C6 122.9(5) . . ?
C5 C5 C4 117.6(4) 12 . ?
C5 C5 H5 121.2 12 . ?
C4 C5 H5 121.2 . . ?
O4 C6 O3 127.0(8) . . ?
O4 C6 C4 116.9(8) . . ?
O3 C6 C4 116.1(5) . . ?
O4 C6 Na1 66.9(5) . . ?
O3 C6 Na1 60.5(4) . . ?
C4 C6 Na1 170.8(5) . . ?
O6 O5 Na1 164.9(16) 9_667 9_667 ?
O6 O5 Na1 81.7(12) 9_667 . ?
Na1 O5 Na1 83.3(6) 9_667 . ?
O6 O5 Na2 52.3(10) 9_667 9_667 ?
Na1 O5 Na2 142.8(8) 9_667 9_667 ?
Na1 O5 Na2 134.0(6) . 9_667 ?
O6 O5 H5W 127(9) 9_667 . ?
Na1 O5 H5W 60(9) 9_667 . ?
Na1 O5 H5W 113(9) . . ?
Na2 O5 H5W 97(10) 9_667 . ?
O5 O6 Na2 107.7(12) 9_667 . ?
O5 O6 Na1 9.3(10) 9_667 . ?
Na2 O6 Na1 117.0(6) . . ?
O5 O6 Na1 76.2(12) 9_667 9_667 ?
Na2 O6 Na1 176.1(7) . 9_667 ?
Na1 O6 Na1 66.9(4) . 9_667 ?
O5 O6 H6W 106(8) 9_667 . ?
Na2 O6 H6W 122(8) . . ?
Na1 O6 H6W 100(8) . . ?
Na1 O6 H6W 56(8) 9_667 . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O5 H5W O3 0.85(2) 1.90(5) 2.716(8) 162(13) 9_667
O6 H6W O4 0.85(2) 1.96(3) 2.801(9) 174(12) 4_567

_diffrn_measured_fraction_theta_max 0.996
_diffrn_reflns_theta_full        26.00
_diffrn_measured_fraction_theta_full 0.996
_refine_diff_density_max         1.091
_refine_diff_density_min         -1.034
_refine_diff_density_rms         0.122

# Attachment '5.cif'

data_5
_database_code_depnum_ccdc_archive 'CCDC 683332'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C18 H6 K2 Mn2 N6 O12'
_chemical_formula_weight         686.37

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'
Mn Mn 0.3368 0.7283 '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'
K K 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Orthorhombic
_symmetry_space_group_name_H-M   'Cmcm '

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

_cell_length_a                   10.720(3)
_cell_length_b                   15.228(5)
_cell_length_c                   13.331(4)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     2176.1(12)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    863
_cell_measurement_theta_min      2.675
_cell_measurement_theta_max      26.954

_exptl_crystal_description       needle
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.05
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.095
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1360
_exptl_absorpt_coefficient_mu    1.628
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.8541
_exptl_absorpt_correction_T_max  0.9230
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         '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_%        ?
_diffrn_reflns_number            5415
_diffrn_reflns_av_R_equivalents  0.0547
_diffrn_reflns_av_sigmaI/netI    0.0348
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         2.32
_diffrn_reflns_theta_max         27.10
_reflns_number_total             1318
_reflns_number_gt                1079
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_structure_solution    'Bruker SHELXTL'
_computing_structure_refinement  'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0579P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         1318
_refine_ls_number_parameters     103
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0405
_refine_ls_R_factor_gt           0.0337
_refine_ls_wR_factor_ref         0.0874
_refine_ls_wR_factor_gt          0.0853
_refine_ls_goodness_of_fit_ref   0.982
_refine_ls_restrained_S_all      0.982
_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
Mn1 Mn 0.19128(4) 0.48046(3) 0.7500 0.02630(17) Uani 1 2 d S . .
K1 K 0.5000 0.59274(6) 1.10962(6) 0.0437(2) Uani 1 2 d S . .
O1 O 0.31031(18) 0.36882(13) 0.7500 0.0326(5) Uani 1 2 d S . .
O2 O 0.3250(2) 0.22293(15) 0.7500 0.0483(7) Uani 1 2 d S . .
O3 O 0.30728(13) 0.53518(10) 0.86366(15) 0.0381(4) Uani 1 1 d . . .
O4 O 0.32512(16) 0.64048(12) 0.97898(15) 0.0503(5) Uani 1 1 d . . .
N1 N 0.0625(2) 0.36069(14) 0.7500 0.0236(5) Uani 1 2 d S . .
N2 N 0.06232(15) 0.54821(10) 0.86450(12) 0.0258(4) Uani 1 1 d . . .
C1 C 0.1242(3) 0.28542(18) 0.7500 0.0243(6) Uani 1 2 d S . .
C2 C 0.0633(3) 0.20443(19) 0.7500 0.0309(7) Uani 1 2 d S . .
H2 H 0.1080 0.1521 0.7500 0.037 Uiso 1 2 calc SR . .
C3 C 0.2664(3) 0.2920(2) 0.7500 0.0277(6) Uani 1 2 d S . .
C4 C 0.1240(2) 0.60260(13) 0.92391(15) 0.0274(5) Uani 1 1 d . . .
C5 C 0.0635(2) 0.66442(13) 0.98378(15) 0.0344(5) Uani 1 1 d . . .
H5 H 0.1084 0.7043 1.0224 0.041 Uiso 1 1 calc R . .
C6 C 0.2649(2) 0.59280(14) 0.92249(17) 0.0331(5) Uani 1 1 d . . .


_geom_special_details            
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Mn1 O1 2.126(2) . ?
Mn1 O3 2.1298(17) . ?
Mn1 O3 2.1298(17) 10_557 ?
Mn1 N1 2.287(2) . ?
Mn1 N2 2.3032(17) . ?
Mn1 N2 2.3032(17) 10_557 ?
Mn1 K1 3.9619(11) 9_667 ?
Mn1 K1 3.9619(11) 2_664 ?
K1 O4 2.6601(19) . ?
K1 O4 2.6601(19) 12_655 ?
K1 O1 2.8248(17) 9_667 ?
K1 O1 2.8248(17) 11_566 ?
K1 O3 2.8618(17) 4_567 ?
K1 O3 2.8618(17) 9_667 ?
K1 K1 3.7426(19) 10_558 ?
K1 Mn1 3.9619(11) 9_667 ?
K1 Mn1 3.9619(11) 11_566 ?
K1 K1 4.0644(19) 9_667 ?
O1 C3 1.262(4) . ?
O1 K1 2.8248(17) 9_667 ?
O1 K1 2.8248(17) 2_664 ?
O2 C3 1.225(4) . ?
O3 C6 1.261(3) . ?
O3 K1 2.8618(17) 9_667 ?
O4 C6 1.229(3) . ?
N1 C1 1.323(4) . ?
N1 N1 1.340(5) 3_556 ?
N2 C4 1.323(3) . ?
N2 N2 1.336(3) 12 ?
C1 C2 1.395(4) . ?
C1 C3 1.528(4) . ?
C2 C2 1.356(6) 3_556 ?
C2 H2 0.9300 . ?
C4 C5 1.394(3) . ?
C4 C6 1.519(3) . ?
C5 C5 1.362(5) 12 ?
C5 H5 0.9300 . ?

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 Mn1 O3 87.85(6) . . ?
O1 Mn1 O3 87.85(6) . 10_557 ?
O3 Mn1 O3 90.70(10) . 10_557 ?
O1 Mn1 N1 74.01(9) . . ?
O3 Mn1 N1 131.63(5) . . ?
O3 Mn1 N1 131.63(5) 10_557 . ?
O1 Mn1 N2 135.93(4) . . ?
O3 Mn1 N2 72.77(7) . . ?
O3 Mn1 N2 130.29(6) 10_557 . ?
N1 Mn1 N2 89.71(6) . . ?
O1 Mn1 N2 135.93(4) . 10_557 ?
O3 Mn1 N2 130.29(6) . 10_557 ?
O3 Mn1 N2 72.77(7) 10_557 10_557 ?
N1 Mn1 N2 89.71(6) . 10_557 ?
N2 Mn1 N2 83.01(8) . 10_557 ?
O1 Mn1 K1 43.41(4) . 9_667 ?
O3 Mn1 K1 44.47(4) . 9_667 ?
O3 Mn1 K1 87.62(5) 10_557 9_667 ?
N1 Mn1 K1 106.25(5) . 9_667 ?
N2 Mn1 K1 108.32(5) . 9_667 ?
N2 Mn1 K1 160.11(4) 10_557 9_667 ?
O1 Mn1 K1 43.41(4) . 2_664 ?
O3 Mn1 K1 87.62(5) . 2_664 ?
O3 Mn1 K1 44.47(4) 10_557 2_664 ?
N1 Mn1 K1 106.25(5) . 2_664 ?
N2 Mn1 K1 160.11(4) . 2_664 ?
N2 Mn1 K1 108.32(5) 10_557 2_664 ?
K1 Mn1 K1 56.37(3) 9_667 2_664 ?
O4 K1 O4 89.62(9) . 12_655 ?
O4 K1 O1 152.18(6) . 9_667 ?
O4 K1 O1 82.52(6) 12_655 9_667 ?
O4 K1 O1 82.52(6) . 11_566 ?
O4 K1 O1 152.18(6) 12_655 11_566 ?
O1 K1 O1 92.09(7) 9_667 11_566 ?
O4 K1 O3 76.04(6) . 4_567 ?
O4 K1 O3 140.92(6) 12_655 4_567 ?
O1 K1 O3 125.33(6) 9_667 4_567 ?
O1 K1 O3 62.54(5) 11_566 4_567 ?
O4 K1 O3 140.92(6) . 9_667 ?
O4 K1 O3 76.04(6) 12_655 9_667 ?
O1 K1 O3 62.54(5) 9_667 9_667 ?
O1 K1 O3 125.33(6) 11_566 9_667 ?
O3 K1 O3 92.43(7) 4_567 9_667 ?
O4 K1 K1 130.90(5) . 10_558 ?
O4 K1 K1 130.90(5) 12_655 10_558 ?
O1 K1 K1 48.51(3) 9_667 10_558 ?
O1 K1 K1 48.51(3) 11_566 10_558 ?
O3 K1 K1 82.85(4) 4_567 10_558 ?
O3 K1 K1 82.85(4) 9_667 10_558 ?
O4 K1 Mn1 167.11(5) . 9_667 ?
O4 K1 Mn1 78.32(5) 12_655 9_667 ?
O1 K1 Mn1 31.14(4) 9_667 9_667 ?
O1 K1 Mn1 110.29(4) 11_566 9_667 ?
O3 K1 Mn1 110.65(5) 4_567 9_667 ?
O3 K1 Mn1 31.42(3) 9_667 9_667 ?
K1 K1 Mn1 61.814(14) 10_558 9_667 ?
O4 K1 Mn1 78.31(5) . 11_566 ?
O4 K1 Mn1 167.11(5) 12_655 11_566 ?
O1 K1 Mn1 110.29(4) 9_667 11_566 ?
O1 K1 Mn1 31.14(4) 11_566 11_566 ?
O3 K1 Mn1 31.42(3) 4_567 11_566 ?
O3 K1 Mn1 110.65(5) 9_667 11_566 ?
K1 K1 Mn1 61.814(14) 10_558 11_566 ?
Mn1 K1 Mn1 113.30(3) 9_667 11_566 ?
O4 K1 K1 73.69(5) . 9_667 ?
O4 K1 K1 73.69(5) 12_655 9_667 ?
O1 K1 K1 128.34(4) 9_667 9_667 ?
O1 K1 K1 128.34(4) 11_566 9_667 ?
O3 K1 K1 67.45(4) 4_567 9_667 ?
O3 K1 K1 67.45(4) 9_667 9_667 ?
K1 K1 K1 135.98(3) 10_558 9_667 ?
Mn1 K1 K1 98.29(2) 9_667 9_667 ?
Mn1 K1 K1 98.29(2) 11_566 9_667 ?
C3 O1 Mn1 121.19(19) . . ?
C3 O1 K1 117.45(12) . 9_667 ?
Mn1 O1 K1 105.45(7) . 9_667 ?
C3 O1 K1 117.45(12) . 2_664 ?
Mn1 O1 K1 105.45(7) . 2_664 ?
K1 O1 K1 82.98(6) 9_667 2_664 ?
C6 O3 Mn1 120.30(14) . . ?
C6 O3 K1 130.98(15) . 9_667 ?
Mn1 O3 K1 104.11(6) . 9_667 ?
C6 O4 K1 127.56(15) . . ?
C1 N1 N1 119.97(16) . 3_556 ?
C1 N1 Mn1 112.91(18) . . ?
N1 N1 Mn1 127.12(6) 3_556 . ?
C4 N2 N2 119.96(12) . 12 ?
C4 N2 Mn1 112.18(14) . . ?
N2 N2 Mn1 126.88(4) 12 . ?
N1 C1 C2 122.1(3) . . ?
N1 C1 C3 116.2(2) . . ?
C2 C1 C3 121.6(2) . . ?
C2 C2 C1 117.89(16) 3_556 . ?
C2 C2 H2 121.1 3_556 . ?
C1 C2 H2 121.1 . . ?
O2 C3 O1 127.2(3) . . ?
O2 C3 C1 117.1(3) . . ?
O1 C3 C1 115.7(2) . . ?
N2 C4 C5 122.3(2) . . ?
N2 C4 C6 115.34(18) . . ?
C5 C4 C6 122.40(19) . . ?
C5 C5 C4 117.69(13) 12 . ?
C5 C5 H5 121.2 12 . ?
C4 C5 H5 121.2 . . ?
O4 C6 O3 127.1(2) . . ?
O4 C6 C4 117.2(2) . . ?
O3 C6 C4 115.73(19) . . ?

_diffrn_measured_fraction_theta_max 1.000
_diffrn_reflns_theta_full        27.10
_diffrn_measured_fraction_theta_full 1.000
_refine_diff_density_max         0.809
_refine_diff_density_min         -0.553
_refine_diff_density_rms         0.090


# Attachment '6.cif'

data_6
_database_code_depnum_ccdc_archive 'CCDC 683333'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C18 H6 K2 N6 O12 Zn2'
_chemical_formula_weight         707.23

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'
Zn Zn 0.2839 1.4301 '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'
K K 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Orthorhombic
_symmetry_space_group_name_H-M   'Cmcm '

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

_cell_length_a                   10.7037(10)
_cell_length_b                   15.0640(14)
_cell_length_c                   13.2866(16)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     2142.3(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    273(2)
_cell_measurement_reflns_used    2238
_cell_measurement_theta_min      2.33
_cell_measurement_theta_max      30.10

_exptl_crystal_description       needle
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.05
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.193
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1400
_exptl_absorpt_coefficient_mu    2.714
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.7730
_exptl_absorpt_correction_T_max  0.8762
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      273(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         '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_%        ?
_diffrn_reflns_number            4077
_diffrn_reflns_av_R_equivalents  0.0209
_diffrn_reflns_av_sigmaI/netI    0.0200
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         2.33
_diffrn_reflns_theta_max         25.99
_reflns_number_total             1124
_reflns_number_gt                1006
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'Bruker SHELXTL'
_computing_structure_refinement  'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0386P)²+2.4174P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         1124
_refine_ls_number_parameters     103
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0285
_refine_ls_R_factor_gt           0.0245
_refine_ls_wR_factor_ref         0.0680
_refine_ls_wR_factor_gt          0.0648
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_restrained_S_all      1.058
_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 0.18927(3) 0.48146(2) 0.7500 0.02693(15) Uani 1 2 d S . .
K1 K 0.5000 0.59078(6) 1.11061(6) 0.0420(2) Uani 1 2 d S . .
O1 O 0.30916(18) 0.37461(14) 0.7500 0.0324(5) Uani 1 2 d S . .
O2 O 0.3255(2) 0.22729(15) 0.7500 0.0449(7) Uani 1 2 d S . .
O3 O 0.30656(14) 0.53474(11) 0.85824(16) 0.0386(4) Uani 1 1 d . . .
O4 O 0.32603(17) 0.63867(12) 0.97662(16) 0.0490(5) Uani 1 1 d . . .
N1 N 0.0625(2) 0.36594(14) 0.7500 0.0220(5) Uani 1 2 d S . .
N2 N 0.06248(17) 0.54773(10) 0.86053(14) 0.0254(4) Uani 1 1 d . . .
C1 C 0.1245(3) 0.28937(18) 0.7500 0.0228(6) Uani 1 2 d S . .
C2 C 0.0637(3) 0.20769(19) 0.7500 0.0283(7) Uani 1 2 d S . .
H2 H 0.1086 0.1548 0.7500 0.034 Uiso 1 2 calc SR . .
C3 C 0.2658(3) 0.2966(2) 0.7500 0.0268(6) Uani 1 2 d S . .
C4 C 0.1241(2) 0.60215(12) 0.92098(17) 0.0264(5) Uani 1 1 d . . .
C5 C 0.0632(2) 0.66419(14) 0.98204(17) 0.0330(5) Uani 1 1 d . . .
H5 H 0.1081 0.7041 1.0213 0.040 Uiso 1 1 calc R . .
C6 C 0.2646(2) 0.59190(14) 0.91881(18) 0.0323(5) Uani 1 1 d . . .


_geom_special_details            
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Zn1 O1 2.058(2) . ?
Zn1 O3 2.0709(18) . ?
Zn1 O3 2.0709(18) 10_557 ?
Zn1 N1 2.207(2) . ?
Zn1 N2 2.2350(18) 10_557 ?
Zn1 N2 2.2350(18) . ?
Zn1 K1 3.9593(6) 9_667 ?
Zn1 K1 3.9593(6) 2_664 ?
K1 O4 2.6753(19) . ?
K1 O4 2.6753(19) 12_655 ?
K1 O1 2.8061(16) 9_667 ?
K1 O1 2.8061(16) 11_566 ?
K1 O3 2.8344(17) 4_567 ?
K1 O3 2.8344(17) 9_667 ?
K1 K1 3.7040(17) 10_558 ?
K1 Zn1 3.9593(6) 9_667 ?
K1 Zn1 3.9593(6) 11_566 ?
K1 K1 4.0150(17) 9_667 ?
O1 C3 1.263(4) . ?
O1 K1 2.8061(16) 9_667 ?
O1 K1 2.8061(16) 2_664 ?
O2 C3 1.225(4) . ?
O3 C6 1.261(3) . ?
O3 K1 2.8344(17) 9_667 ?
O4 C6 1.232(3) . ?
N1 C1 1.331(4) . ?
N1 N1 1.338(5) 3_556 ?
N2 C4 1.324(3) . ?
N2 N2 1.337(4) 12 ?
C1 C2 1.392(4) . ?
C1 C3 1.516(5) . ?
C2 C2 1.364(6) 3_556 ?
C4 C5 1.399(3) . ?
C4 C6 1.512(4) . ?
C5 C5 1.353(5) 12 ?

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 O3 85.71(6) . . ?
O1 Zn1 O3 85.71(6) . 10_557 ?
O3 Zn1 O3 87.97(11) . 10_557 ?
O1 Zn1 N1 76.51(9) . . ?
O3 Zn1 N1 132.72(6) . . ?
O3 Zn1 N1 132.72(6) 10_557 . ?
O1 Zn1 N2 136.70(5) . 10_557 ?
O3 Zn1 N2 130.64(6) . 10_557 ?
O3 Zn1 N2 74.85(7) 10_557 10_557 ?
N1 Zn1 N2 88.79(6) . 10_557 ?
O1 Zn1 N2 136.70(5) . . ?
O3 Zn1 N2 74.85(7) . . ?
O3 Zn1 N2 130.64(6) 10_557 . ?
N1 Zn1 N2 88.79(6) . . ?
N2 Zn1 N2 82.15(9) 10_557 . ?
O1 Zn1 K1 42.39(4) . 9_667 ?
O3 Zn1 K1 43.32(5) . 9_667 ?
O3 Zn1 K1 85.54(5) 10_557 9_667 ?
N1 Zn1 K1 107.45(6) . 9_667 ?
N2 Zn1 K1 160.09(5) 10_557 9_667 ?
N2 Zn1 K1 109.00(5) . 9_667 ?
O1 Zn1 K1 42.39(4) . 2_664 ?
O3 Zn1 K1 85.54(5) . 2_664 ?
O3 Zn1 K1 43.32(5) 10_557 2_664 ?
N1 Zn1 K1 107.45(6) . 2_664 ?
N2 Zn1 K1 109.00(5) 10_557 2_664 ?
N2 Zn1 K1 160.09(5) . 2_664 ?
K1 Zn1 K1 55.78(2) 9_667 2_664 ?
O4 K1 O4 88.22(10) . 12_655 ?
O4 K1 O1 153.61(7) . 9_667 ?
O4 K1 O1 83.25(6) 12_655 9_667 ?
O4 K1 O1 83.25(6) . 11_566 ?
O4 K1 O1 153.61(7) 12_655 11_566 ?
O1 K1 O1 93.43(6) 9_667 11_566 ?
O4 K1 O3 76.62(6) . 4_567 ?
O4 K1 O3 141.77(7) 12_655 4_567 ?
O1 K1 O3 124.01(6) 9_667 4_567 ?
O1 K1 O3 59.72(6) 11_566 4_567 ?
O4 K1 O3 141.77(7) . 9_667 ?
O4 K1 O3 76.62(6) 12_655 9_667 ?
O1 K1 O3 59.72(6) 9_667 9_667 ?
O1 K1 O3 124.01(6) 11_566 9_667 ?
O3 K1 O3 93.86(7) 4_567 9_667 ?
O4 K1 K1 131.72(5) . 10_558 ?
O4 K1 K1 131.72(5) 12_655 10_558 ?
O1 K1 K1 48.70(3) 9_667 10_558 ?
O1 K1 K1 48.70(3) 11_566 10_558 ?
O3 K1 K1 81.60(5) 4_567 10_558 ?
O3 K1 K1 81.60(5) 9_667 10_558 ?
O4 K1 Zn1 165.95(5) . 9_667 ?
O4 K1 Zn1 78.50(5) 12_655 9_667 ?
O1 K1 Zn1 29.64(4) 9_667 9_667 ?
O1 K1 Zn1 110.72(4) 11_566 9_667 ?
O3 K1 Zn1 111.22(4) 4_567 9_667 ?
O3 K1 Zn1 30.08(4) 9_667 9_667 ?
K1 K1 Zn1 62.111(12) 10_558 9_667 ?
O4 K1 Zn1 78.50(5) . 11_566 ?
O4 K1 Zn1 165.95(5) 12_655 11_566 ?
O1 K1 Zn1 110.72(4) 9_667 11_566 ?
O1 K1 Zn1 29.64(4) 11_566 11_566 ?
O3 K1 Zn1 30.08(4) 4_567 11_566 ?
O3 K1 Zn1 111.22(4) 9_667 11_566 ?
K1 K1 Zn1 62.111(11) 10_558 11_566 ?
Zn1 K1 Zn1 114.29(2) 9_667 11_566 ?
O4 K1 K1 72.33(5) . 9_667 ?
O4 K1 K1 72.33(5) 12_655 9_667 ?
O1 K1 K1 127.57(4) 9_667 9_667 ?
O1 K1 K1 127.57(4) 11_566 9_667 ?
O3 K1 K1 69.66(4) 4_567 9_667 ?
O3 K1 K1 69.66(4) 9_667 9_667 ?
K1 K1 K1 137.06(2) 10_558 9_667 ?
Zn1 K1 K1 98.93(2) 9_667 9_667 ?
Zn1 K1 K1 98.93(2) 11_566 9_667 ?
C3 O1 Zn1 119.87(19) . . ?
C3 O1 K1 116.13(13) . 9_667 ?
Zn1 O1 K1 107.97(7) . 9_667 ?
C3 O1 K1 116.13(13) . 2_664 ?
Zn1 O1 K1 107.97(7) . 2_664 ?
K1 O1 K1 82.60(6) 9_667 2_664 ?
C6 O3 Zn1 119.48(14) . . ?
C6 O3 K1 128.48(16) . 9_667 ?
Zn1 O3 K1 106.60(7) . 9_667 ?
C6 O4 K1 129.19(15) . . ?
C1 N1 N1 119.91(16) . 3_556 ?
C1 N1 Zn1 112.15(19) . . ?
N1 N1 Zn1 127.95(6) 3_556 . ?
C4 N2 N2 119.89(12) . 12 ?
C4 N2 Zn1 111.88(14) . . ?
N2 N2 Zn1 127.39(5) 12 . ?
N1 C1 C2 122.2(3) . . ?
N1 C1 C3 115.8(2) . . ?
C2 C1 C3 122.0(3) . . ?
C2 C2 C1 117.86(17) 3_556 . ?
O2 C3 O1 127.0(3) . . ?
O2 C3 C1 117.3(3) . . ?
O1 C3 C1 115.7(2) . . ?
N2 C4 C5 122.2(2) . . ?
N2 C4 C6 114.89(19) . . ?
C5 C4 C6 122.9(2) . . ?
C5 C5 C4 117.78(13) 12 . ?
O4 C6 O3 126.7(2) . . ?
O4 C6 C4 117.4(2) . . ?
O3 C6 C4 115.83(19) . . ?

_diffrn_measured_fraction_theta_max 0.965
_diffrn_reflns_theta_full        25.99
_diffrn_measured_fraction_theta_full 0.965
_refine_diff_density_max         0.632
_refine_diff_density_min         -0.393
_refine_diff_density_rms         0.065

# Attachment '7.cif'

data_7
_database_code_depnum_ccdc_archive 'CCDC 683334'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C18 H14 Mn2 N8 O12'
_chemical_formula_weight         644.25

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           monoclinic
_symmetry_space_group_name_H-M   P2(1)/n

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

_cell_length_a                   9.3716(17)
_cell_length_b                   13.332(3)
_cell_length_c                   18.101(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 101.150(3)
_cell_angle_gamma                90.00
_cell_volume                     2219.0(7)
_cell_formula_units_Z            4
_cell_measurement_temperature    273(2)
_cell_measurement_reflns_used    1109
_cell_measurement_theta_min      2.288
_cell_measurement_theta_max      22.06

_exptl_crystal_description       recthedral
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.05
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.928
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1296
_exptl_absorpt_coefficient_mu    1.226
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.8872
_exptl_absorpt_correction_T_max  0.9412
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      273(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         '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_%        2.5
_diffrn_reflns_number            12271
_diffrn_reflns_av_R_equivalents  0.0736
_diffrn_reflns_av_sigmaI/netI    0.0954
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         1.91
_diffrn_reflns_theta_max         26.01
_reflns_number_total             4353
_reflns_number_gt                2325
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_structure_solution    'Bruker SHELXTL'
_computing_structure_refinement  'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0989P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         4353
_refine_ls_number_parameters     361
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1360
_refine_ls_R_factor_gt           0.0674
_refine_ls_wR_factor_ref         0.2008
_refine_ls_wR_factor_gt          0.1638
_refine_ls_goodness_of_fit_ref   0.988
_refine_ls_restrained_S_all      0.988
_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
Mn1 Mn 0.56122(10) 0.23814(7) 0.39560(5) 0.0329(3) Uani 1 1 d . . .
Mn2 Mn 0.37410(10) 0.26201(7) 0.58259(5) 0.0340(3) Uani 1 1 d . . .
O1 O 0.7125(5) 0.3379(4) 0.3638(2) 0.0505(13) Uani 1 1 d . . .
O2 O 0.8922(5) 0.4459(4) 0.4056(3) 0.0581(14) Uani 1 1 d . . .
O3 O 0.4028(5) 0.3867(4) 0.6597(3) 0.0497(13) Uani 1 1 d . . .
O4 O 0.5544(5) 0.5056(4) 0.7142(3) 0.0695(17) Uani 1 1 d . . .
O11 O 0.4506(5) 0.2302(3) 0.2822(2) 0.0456(12) Uani 1 1 d . . .
O12 O 0.2393(5) 0.2274(4) 0.2012(3) 0.0548(14) Uani 1 1 d . . .
O13 O 0.1492(5) 0.2667(3) 0.5838(2) 0.0454(12) Uani 1 1 d . . .
O14 O -0.0763(5) 0.2343(4) 0.5205(3) 0.0559(14) Uani 1 1 d . . .
O21 O 0.6937(5) 0.1141(4) 0.3721(3) 0.0530(13) Uani 1 1 d . . .
O22 O 0.8520(5) -0.0048(4) 0.4222(3) 0.0688(17) Uani 1 1 d . . .
O23 O 0.4049(5) 0.1620(4) 0.6746(3) 0.0516(13) Uani 1 1 d . . .
O24 O 0.5574(5) 0.0552(4) 0.7447(3) 0.0635(15) Uani 1 1 d . . .
N1 N 0.6058(5) 0.3595(4) 0.4880(3) 0.0299(12) Uani 1 1 d . . .
N2 N 0.5422(5) 0.3687(4) 0.5480(3) 0.0304(12) Uani 1 1 d . . .
N11 N 0.3179(5) 0.2431(3) 0.3988(3) 0.0276(11) Uani 1 1 d . . .
N12 N 0.2561(5) 0.2470(3) 0.4606(3) 0.0263(11) Uani 1 1 d . . .
N21 N 0.5964(5) 0.1320(3) 0.4982(3) 0.0298(12) Uani 1 1 d . . .
N22 N 0.5380(5) 0.1423(3) 0.5597(3) 0.0282(11) Uani 1 1 d . . .
N3 N 0.6060(6) 0.3826(4) 0.2015(3) 0.0503(15) Uani 1 1 d . . .
N4 N 0.6167(7) 0.0933(4) 0.2057(3) 0.0534(16) Uani 1 1 d . . .
C1 C 0.7805(8) 0.3976(5) 0.4115(4) 0.0434(18) Uani 1 1 d . . .
C2 C 0.7220(6) 0.4138(4) 0.4829(3) 0.0308(14) Uani 1 1 d . . .
C3 C 0.7853(7) 0.4800(5) 0.5401(4) 0.0438(18) Uani 1 1 d . . .
H3A H 0.8690 0.5157 0.5369 0.053 Uiso 1 1 calc R . .
C4 C 0.7206(7) 0.4900(5) 0.5998(4) 0.0417(17) Uani 1 1 d . . .
H4A H 0.7586 0.5337 0.6387 0.050 Uiso 1 1 calc R . .
C5 C 0.5955(6) 0.4339(5) 0.6030(4) 0.0377(16) Uani 1 1 d . . .
C6 C 0.5103(7) 0.4430(6) 0.6646(4) 0.0482(19) Uani 1 1 d . . .
C11 C 0.3134(7) 0.2310(4) 0.2654(3) 0.0324(15) Uani 1 1 d . . .
C12 C 0.2342(7) 0.2332(4) 0.3301(3) 0.0307(14) Uani 1 1 d . . .
C13 C 0.0838(7) 0.2233(5) 0.3202(4) 0.0418(17) Uani 1 1 d . . .
H9A H 0.0272 0.2155 0.2723 0.050 Uiso 1 1 calc R . .
C14 C 0.0210(7) 0.2256(5) 0.3826(4) 0.0438(17) Uani 1 1 d . . .
H10A H -0.0788 0.2176 0.3784 0.053 Uiso 1 1 calc R . .
C15 C 0.1113(7) 0.2400(4) 0.4523(4) 0.0324(15) Uani 1 1 d . . .
C16 C 0.0550(7) 0.2471(5) 0.5251(4) 0.0420(17) Uani 1 1 d . . .
C21 C 0.7554(8) 0.0579(6) 0.4251(4) 0.0487(19) Uani 1 1 d . . .
C22 C 0.7072(7) 0.0692(4) 0.4992(3) 0.0347(15) Uani 1 1 d . . .
C23 C 0.7706(7) 0.0189(5) 0.5645(4) 0.0445(18) Uani 1 1 d . . .
H15A H 0.8525 -0.0209 0.5654 0.053 Uiso 1 1 calc R . .
C24 C 0.7123(7) 0.0283(5) 0.6265(4) 0.0421(17) Uani 1 1 d . . .
H16A H 0.7522 -0.0048 0.6710 0.051 Uiso 1 1 calc R . .
C25 C 0.5907(6) 0.0889(4) 0.6218(3) 0.0325(15) Uani 1 1 d . . .
C26 C 0.5101(7) 0.1032(6) 0.6863(4) 0.0446(18) Uani 1 1 d . . .


_geom_special_details            
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Mn1 O1 2.104(4) . ?
Mn1 O11 2.116(4) . ?
Mn1 O21 2.159(5) . ?
Mn1 N11 2.293(5) . ?
Mn1 N1 2.306(5) . ?
Mn1 N21 2.307(5) . ?
Mn2 O23 2.110(5) . ?
Mn2 O13 2.113(4) . ?
Mn2 O3 2.153(5) . ?
Mn2 N12 2.280(5) . ?
Mn2 N2 2.297(5) . ?
Mn2 N22 2.307(5) . ?
O1 C1 1.254(8) . ?
O2 C1 1.250(7) . ?
O3 C6 1.245(8) . ?
O4 C6 1.237(8) . ?
O11 C11 1.263(7) . ?
O12 C11 1.234(7) . ?
O13 C16 1.270(8) . ?
O14 C16 1.229(8) . ?
O21 C21 1.266(8) . ?
O22 C21 1.240(8) . ?
O23 C26 1.246(8) . ?
O24 C26 1.243(7) . ?
N1 C2 1.325(7) . ?
N1 N2 1.343(6) . ?
N2 C5 1.343(7) . ?
N11 C12 1.344(7) . ?
N11 N12 1.355(6) . ?
N12 C15 1.339(7) . ?
N21 C22 1.331(7) . ?
N21 N22 1.341(6) . ?
N22 C25 1.341(7) . ?
C1 C2 1.514(9) . ?
C2 C3 1.402(8) . ?
C3 C4 1.344(9) . ?
C4 C5 1.401(9) . ?
C5 C6 1.497(9) . ?
C11 C12 1.502(9) . ?
C12 C13 1.392(8) . ?
C13 C14 1.371(9) . ?
C14 C15 1.390(9) . ?
C15 C16 1.514(9) . ?
C21 C22 1.504(9) . ?
C22 C23 1.389(8) . ?
C23 C24 1.346(9) . ?
C24 C25 1.386(8) . ?
C25 C26 1.519(9) . ?

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 Mn1 O11 89.77(17) . . ?
O1 Mn1 O21 89.2(2) . . ?
O11 Mn1 O21 87.89(17) . . ?
O1 Mn1 N11 135.64(18) . . ?
O11 Mn1 N11 73.92(18) . . ?
O21 Mn1 N11 129.76(18) . . ?
O1 Mn1 N1 73.60(18) . . ?
O11 Mn1 N1 136.43(17) . . ?
O21 Mn1 N1 130.53(17) . . ?
N11 Mn1 N1 90.17(17) . . ?
O1 Mn1 N21 127.50(17) . . ?
O11 Mn1 N21 135.82(17) . . ?
O21 Mn1 N21 71.98(18) . . ?
N11 Mn1 N21 89.16(17) . . ?
N1 Mn1 N21 82.48(17) . . ?
O23 Mn2 O13 89.71(18) . . ?
O23 Mn2 O3 89.7(2) . . ?
O13 Mn2 O3 88.31(17) . . ?
O23 Mn2 N12 132.56(18) . . ?
O13 Mn2 N12 73.42(17) . . ?
O3 Mn2 N12 132.23(17) . . ?
O23 Mn2 N2 127.60(17) . . ?
O13 Mn2 N2 136.25(18) . . ?
O3 Mn2 N2 72.08(18) . . ?
N12 Mn2 N2 91.14(17) . . ?
O23 Mn2 N22 73.15(18) . . ?
O13 Mn2 N22 136.24(18) . . ?
O3 Mn2 N22 130.24(17) . . ?
N12 Mn2 N22 88.88(17) . . ?
N2 Mn2 N22 82.20(17) . . ?
C1 O1 Mn1 119.5(4) . . ?
C6 O3 Mn2 120.7(4) . . ?
C11 O11 Mn1 121.2(4) . . ?
C16 O13 Mn2 121.2(4) . . ?
C21 O21 Mn1 120.0(4) . . ?
C26 O23 Mn2 121.0(4) . . ?
C2 N1 N2 120.4(5) . . ?
C2 N1 Mn1 111.7(4) . . ?
N2 N1 Mn1 127.2(4) . . ?
N1 N2 C5 119.9(5) . . ?
N1 N2 Mn2 126.8(4) . . ?
C5 N2 Mn2 112.1(4) . . ?
C12 N11 N12 120.1(5) . . ?
C12 N11 Mn1 112.3(4) . . ?
N12 N11 Mn1 127.4(3) . . ?
C15 N12 N11 119.4(5) . . ?
C15 N12 Mn2 113.9(4) . . ?
N11 N12 Mn2 126.7(3) . . ?
C22 N21 N22 119.7(5) . . ?
C22 N21 Mn1 112.8(4) . . ?
N22 N21 Mn1 126.1(3) . . ?
N21 N22 C25 119.9(5) . . ?
N21 N22 Mn2 127.8(3) . . ?
C25 N22 Mn2 111.5(4) . . ?
O2 C1 O1 126.1(7) . . ?
O2 C1 C2 116.6(6) . . ?
O1 C1 C2 117.3(6) . . ?
N1 C2 C3 121.9(6) . . ?
N1 C2 C1 114.8(5) . . ?
C3 C2 C1 123.3(6) . . ?
C4 C3 C2 117.7(6) . . ?
C3 C4 C5 119.4(6) . . ?
N2 C5 C4 120.6(6) . . ?
N2 C5 C6 115.4(6) . . ?
C4 C5 C6 124.0(6) . . ?
O4 C6 O3 127.7(7) . . ?
O4 C6 C5 116.3(7) . . ?
O3 C6 C5 116.0(6) . . ?
O12 C11 O11 126.0(6) . . ?
O12 C11 C12 117.5(6) . . ?
O11 C11 C12 116.5(5) . . ?
N11 C12 C13 121.6(6) . . ?
N11 C12 C11 115.8(5) . . ?
C13 C12 C11 122.6(6) . . ?
C14 C13 C12 118.5(6) . . ?
C13 C14 C15 117.9(6) . . ?
N12 C15 C14 122.5(6) . . ?
N12 C15 C16 114.5(6) . . ?
C14 C15 C16 123.0(6) . . ?
O14 C16 O13 127.6(7) . . ?
O14 C16 C15 116.4(6) . . ?
O13 C16 C15 116.0(6) . . ?
O22 C21 O21 126.6(7) . . ?
O22 C21 C22 116.9(7) . . ?
O21 C21 C22 116.4(6) . . ?
N21 C22 C23 121.4(6) . . ?
N21 C22 C21 114.7(6) . . ?
C23 C22 C21 123.9(6) . . ?
C24 C23 C22 119.2(6) . . ?
C23 C24 C25 117.7(6) . . ?
N22 C25 C24 121.8(6) . . ?
N22 C25 C26 114.8(5) . . ?
C24 C25 C26 123.4(6) . . ?
O24 C26 O23 127.5(7) . . ?
O24 C26 C25 116.2(6) . . ?
O23 C26 C25 116.3(6) . . ?

_diffrn_measured_fraction_theta_max 0.995
_diffrn_reflns_theta_full        26.01
_diffrn_measured_fraction_theta_full 0.995
_refine_diff_density_max         0.600
_refine_diff_density_min         -0.509
_refine_diff_density_rms         0.112

# Attachment '8.cif'

data_8
_database_code_depnum_ccdc_archive 'CCDC 683335'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C18 H14 N8 O12 Zn2'
_chemical_formula_weight         665.11

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'
Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_H-M   Cmcm

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

_cell_length_a                   10.9117(12)
_cell_length_b                   14.9509(15)
_cell_length_c                   13.3255(13)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     2173.9(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    273(2)
_cell_measurement_reflns_used    4555
_cell_measurement_theta_min      2.310
_cell_measurement_theta_max      26.903

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.032
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1336
_exptl_absorpt_coefficient_mu    2.297
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.7701
_exptl_absorpt_correction_T_max  0.8028
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         '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_%        ?
_diffrn_reflns_number            5319
_diffrn_reflns_av_R_equivalents  0.0321
_diffrn_reflns_av_sigmaI/netI    0.0308
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         2.31
_diffrn_reflns_theta_max         27.13
_reflns_number_total             1311
_reflns_number_gt                1015
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_structure_solution    'Bruker SHELXTL'
_computing_structure_refinement  'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0506P)²+30.8145P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         1311
_refine_ls_number_parameters     103
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0859
_refine_ls_R_factor_gt           0.0653
_refine_ls_wR_factor_ref         0.1646
_refine_ls_wR_factor_gt          0.1506
_refine_ls_goodness_of_fit_ref   1.075
_refine_ls_restrained_S_all      1.075
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Zn1 Zn 0.18478(8) 0.47986(6) 0.7500 0.0456(4) Uani 1 2 d S . .
O1 O 0.3005(5) 0.3727(4) 0.7500 0.062(3) Uani 1 2 d S . .
O2 O 0.3204(6) 0.2262(4) 0.7500 0.079(3) Uani 1 2 d S . .
O3 O 0.2986(4) 0.5347(3) 0.8568(7) 0.082(3) Uani 1 1 d . . .
O4 O 0.3173(7) 0.6412(4) 0.9720(9) 0.098(4) Uani 1 1 d . . .
N1 N 0.0617(5) 0.3634(4) 0.7500 0.0271(13) Uani 1 2 d S . .
N2 N 0.0609(4) 0.5474(3) 0.8599(4) 0.0332(10) Uani 1 1 d . . .
N3 N 0.5000 0.5919(6) 1.1058(8) 0.061(2) Uani 1 2 d S . .
C1 C 0.1214(7) 0.2874(5) 0.7500 0.041(2) Uani 1 2 d S . .
C2 C 0.0627(8) 0.2055(6) 0.7500 0.065(3) Uani 1 2 d S . .
H2 H 0.1069 0.1523 0.7500 0.109 Uiso 1 2 calc SR . .
C3 C 0.2606(7) 0.2946(5) 0.7500 0.045(2) Uani 1 2 d S . .
C4 C 0.1204(6) 0.6028(4) 0.9196(5) 0.0506(18) Uani 1 1 d . . .
C5 C 0.0623(8) 0.6646(4) 0.9799(5) 0.069(2) Uani 1 1 d . . .
H5 H 0.1066 0.7047 1.0190 0.083 Uiso 1 1 calc R . .
C6 C 0.2592(8) 0.5928(4) 0.9151(10) 0.077(3) Uani 1 1 d . . .


_geom_special_details            
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Zn1 O1 2.040(6) . ?
Zn1 O3 2.059(6) . ?
Zn1 O3 2.059(6) 10_557 ?
Zn1 N1 2.199(6) . ?
Zn1 N2 2.234(5) . ?
Zn1 N2 2.234(5) 10_557 ?
O1 C3 1.247(10) . ?
O2 C3 1.213(10) . ?
O3 C6 1.243(12) . ?
O4 C6 1.223(9) . ?
N1 C1 1.310(9) . ?
N1 N1 1.346(11) 3_556 ?
N2 C4 1.319(7) . ?
N2 N2 1.330(9) 12 ?
C1 C2 1.381(11) . ?
C1 C3 1.522(11) . ?
C2 C2 1.369(18) 3_556 ?
C2 H2 0.9300 . ?
C4 C5 1.378(9) . ?
C4 C6 1.523(11) . ?
C5 C5 1.360(17) 12 ?
C5 H5 0.9300 . ?

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 O3 86.51(17) . . ?
O1 Zn1 O3 86.51(17) . 10_557 ?
O3 Zn1 O3 87.5(5) . 10_557 ?
O1 Zn1 N1 75.9(2) . . ?
O3 Zn1 N1 133.1(2) . . ?
O3 Zn1 N1 133.1(2) 10_557 . ?
O1 Zn1 N2 136.84(12) . . ?
O3 Zn1 N2 74.4(2) . . ?
O3 Zn1 N2 129.65(18) 10_557 . ?
N1 Zn1 N2 89.34(15) . . ?
O1 Zn1 N2 136.84(12) . 10_557 ?
O3 Zn1 N2 129.65(18) . 10_557 ?
O3 Zn1 N2 74.4(2) 10_557 10_557 ?
N1 Zn1 N2 89.34(15) . 10_557 ?
N2 Zn1 N2 81.9(2) . 10_557 ?
C3 O1 Zn1 121.3(5) . . ?
C6 O3 Zn1 120.2(4) . . ?
C1 N1 N1 119.8(4) . 3_556 ?
C1 N1 Zn1 112.5(5) . . ?
N1 N1 Zn1 127.64(14) 3_556 . ?
C4 N2 N2 119.5(4) . 12 ?
C4 N2 Zn1 112.5(4) . . ?
N2 N2 Zn1 127.21(11) 12 . ?
N1 C1 C2 122.5(7) . . ?
N1 C1 C3 115.8(7) . . ?
C2 C1 C3 121.7(7) . . ?
C2 C2 C1 117.6(5) 3_556 . ?
C2 C2 H2 121.2 3_556 . ?
C1 C2 H2 121.2 . . ?
O2 C3 O1 127.0(8) . . ?
O2 C3 C1 118.5(8) . . ?
O1 C3 C1 114.5(7) . . ?
N2 C4 C5 123.1(7) . . ?
N2 C4 C6 113.8(6) . . ?
C5 C4 C6 123.1(7) . . ?
C5 C5 C4 117.4(4) 12 . ?
C5 C5 H5 121.3 12 . ?
C4 C5 H5 121.3 . . ?
O4 C6 O3 128.4(9) . . ?
O4 C6 C4 115.7(9) . . ?
O3 C6 C4 115.9(6) . . ?

_diffrn_measured_fraction_theta_max 0.992
_diffrn_reflns_theta_full        27.13
_diffrn_measured_fraction_theta_full 0.992
_refine_diff_density_max         0.894
_refine_diff_density_min         -0.991
_refine_diff_density_rms         0.120


# Attachment '9.cif'

data_9
_database_code_depnum_ccdc_archive 'CCDC 683336'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C18 H10 Mn2 N6 Na2 O14'
_chemical_formula_weight         690.18

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'
Na Na 0.0362 0.0249 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   P2(1)/n

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

_cell_length_a                   9.5936(17)
_cell_length_b                   13.010(2)
_cell_length_c                   18.569(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 101.359(2)
_cell_angle_gamma                90.00
_cell_volume                     2272.3(7)
_cell_formula_units_Z            4
_cell_measurement_temperature    273(2)
_cell_measurement_reflns_used    1928
_cell_measurement_theta_min      2.234
_cell_measurement_theta_max      26.299

_exptl_crystal_description       rhombic
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.05
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.017
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1376
_exptl_absorpt_coefficient_mu    1.242
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.8858
_exptl_absorpt_correction_T_max  0.9405
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      273(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         '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_%        2.5
_diffrn_reflns_number            12486
_diffrn_reflns_av_R_equivalents  0.0493
_diffrn_reflns_av_sigmaI/netI    0.0594
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         1.92
_diffrn_reflns_theta_max         26.00
_reflns_number_total             4418
_reflns_number_gt                2988
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_structure_solution    'Bruker SHELXTL'
_computing_structure_refinement  'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0847P)²+3.8551P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         4418
_refine_ls_number_parameters     379
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0941
_refine_ls_R_factor_gt           0.0610
_refine_ls_wR_factor_ref         0.1746
_refine_ls_wR_factor_gt          0.1517
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_restrained_S_all      1.045
_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 0.56385(8) 0.23833(6) 0.39815(4) 0.0235(2) Uani 1 1 d . . .
Mn2 Mn 0.37999(8) 0.26228(6) 0.58174(4) 0.0239(2) Uani 1 1 d . . .
Na1 Na 0.8333(3) 0.41997(19) 0.27594(13) 0.0419(6) Uani 1 1 d . . .
O1 O 0.7168(4) 0.3389(3) 0.3694(2) 0.0354(10) Uani 1 1 d . . .
O2 O 0.8935(4) 0.4469(4) 0.4098(2) 0.0462(11) Uani 1 1 d . . .
O3 O 0.4178(4) 0.3867(3) 0.6589(2) 0.0393(10) Uani 1 1 d . . .
O4 O 0.5665(4) 0.5094(4) 0.7119(2) 0.0495(12) Uani 1 1 d . . .
O5 O 0.8076(5) 0.6025(3) 0.2695(2) 0.0467(11) Uani 1 1 d . . .
O11 O 0.4539(4) 0.2267(3) 0.2892(2) 0.0342(9) Uani 1 1 d . . .
O12 O 0.2513(4) 0.2256(3) 0.2076(2) 0.0384(10) Uani 1 1 d . . .
O13 O 0.1616(4) 0.2685(3) 0.5807(2) 0.0352(10) Uani 1 1 d . . .
O14 O -0.0610(4) 0.2408(3) 0.5213(2) 0.0434(11) Uani 1 1 d . . .
O21 O 0.7025(4) 0.1158(3) 0.3794(2) 0.0377(10) Uani 1 1 d . . .
O22 O 0.8576(5) -0.0058(4) 0.4290(2) 0.0518(12) Uani 1 1 d . . .
O23 O 0.4172(4) 0.1628(3) 0.6734(2) 0.0359(10) Uani 1 1 d . . .
O24 O 0.5675(4) 0.0561(4) 0.7422(2) 0.0475(12) Uani 1 1 d . . .
N1 N 0.6103(4) 0.3622(3) 0.4899(2) 0.0237(10) Uani 1 1 d . . .
N2 N 0.5482(4) 0.3720(3) 0.5485(2) 0.0244(9) Uani 1 1 d . . .
N11 N 0.3231(4) 0.2401(3) 0.4012(2) 0.0204(9) Uani 1 1 d . . .
N12 N 0.2636(4) 0.2460(3) 0.4604(2) 0.0207(9) Uani 1 1 d . . .
N21 N 0.6026(4) 0.1309(3) 0.5008(2) 0.0240(9) Uani 1 1 d . . .
N22 N 0.5456(4) 0.1400(3) 0.5608(2) 0.0222(9) Uani 1 1 d . . .
C1 C 0.7862(6) 0.3996(4) 0.4168(3) 0.0312(13) Uani 1 1 d . . .
C2 C 0.7272(6) 0.4154(4) 0.4865(3) 0.0281(12) Uani 1 1 d . . .
C3 C 0.7937(6) 0.4790(4) 0.5430(3) 0.0350(14) Uani 1 1 d . . .
H3A H 0.8781 0.5129 0.5405 0.042 Uiso 1 1 calc R . .
C4 C 0.7306(6) 0.4901(4) 0.6024(3) 0.0343(14) Uani 1 1 d . . .
H4A H 0.7700 0.5324 0.6416 0.041 Uiso 1 1 calc R . .
C5 C 0.6050(5) 0.4357(4) 0.6024(3) 0.0248(11) Uani 1 1 d . . .
C6 C 0.5238(6) 0.4452(5) 0.6634(3) 0.0348(14) Uani 1 1 d . . .
C11 C 0.3206(6) 0.2284(4) 0.2709(3) 0.0261(12) Uani 1 1 d . . .
C12 C 0.2417(5) 0.2296(4) 0.3346(3) 0.0216(11) Uani 1 1 d . . .
C13 C 0.0944(6) 0.2203(4) 0.3241(3) 0.0304(12) Uani 1 1 d . . .
H9A H 0.0390 0.2123 0.2773 0.036 Uiso 1 1 calc R . .
C14 C 0.0342(6) 0.2233(4) 0.3848(3) 0.0312(13) Uani 1 1 d . . .
H10A H -0.0633 0.2152 0.3810 0.037 Uiso 1 1 calc R . .
C15 C 0.1239(5) 0.2389(4) 0.4530(3) 0.0248(12) Uani 1 1 d . . .
C16 C 0.0676(6) 0.2494(4) 0.5249(3) 0.0308(13) Uani 1 1 d . . .
C21 C 0.7627(6) 0.0589(5) 0.4312(3) 0.0339(13) Uani 1 1 d . . .
C22 C 0.7152(6) 0.0708(4) 0.5037(3) 0.0273(12) Uani 1 1 d . . .
C23 C 0.7827(6) 0.0229(4) 0.5672(3) 0.0316(13) Uani 1 1 d . . .
H15A H 0.8650 -0.0152 0.5683 0.038 Uiso 1 1 calc R . .
C24 C 0.7256(6) 0.0330(4) 0.6284(3) 0.0329(13) Uani 1 1 d . . .
H16A H 0.7675 0.0025 0.6726 0.039 Uiso 1 1 calc R . .
C25 C 0.6027(5) 0.0905(4) 0.6218(3) 0.0259(12) Uani 1 1 d . . .
C26 C 0.5248(6) 0.1044(5) 0.6849(3) 0.0322(13) Uani 1 1 d . . .
Na2 Na 0.5250(3) 0.22796(19) 0.17400(13) 0.0422(6) Uani 1 1 d . . .
O6 O 0.6006(4) 0.3987(3) 0.1996(2) 0.0413(10) Uani 1 1 d . . .


_geom_special_details            
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Mn1 O11 2.095(4) . ?
Mn1 O1 2.112(4) . ?
Mn1 O21 2.148(4) . ?
Mn1 N11 2.321(4) . ?
Mn1 N1 2.323(4) . ?
Mn1 N21 2.334(4) . ?
Mn2 O13 2.093(4) . ?
Mn2 O23 2.112(4) . ?
Mn2 O3 2.146(4) . ?
Mn2 N12 2.319(4) . ?
Mn2 N2 2.327(4) . ?
Mn2 N22 2.334(4) . ?
Na1 O5 2.388(5) . ?
Na1 O6 2.413(5) . ?
Na1 O23 2.457(4) 4_665 ?
Na1 O2 2.464(5) . ?
Na1 O24 2.467(5) 4_665 ?
Na1 O1 2.477(4) . ?
Na1 C26 2.748(6) 4_665 ?
Na1 C1 2.754(6) . ?
Na1 Na2 4.045(4) . ?
O1 C1 1.270(7) . ?
O2 C1 1.228(6) . ?
O3 C6 1.260(7) . ?
O4 C6 1.237(7) . ?
O5 Na2 2.384(5) 2_655 ?
O11 C11 1.257(6) . ?
O11 Na2 2.370(4) . ?
O12 C11 1.232(6) . ?
O12 Na2 2.817(5) . ?
O13 C16 1.259(7) . ?
O13 Na2 2.369(4) 4_566 ?
O14 C16 1.227(7) . ?
O14 Na2 2.822(5) 4_566 ?
O21 C21 1.260(7) . ?
O22 C21 1.247(7) . ?
O23 C26 1.266(7) . ?
O23 Na1 2.457(4) 4_566 ?
O24 C26 1.234(6) . ?
O24 Na1 2.468(5) 4_566 ?
N1 C2 1.330(6) . ?
N1 N2 1.346(6) . ?
N2 C5 1.330(6) . ?
N11 C12 1.332(7) . ?
N11 N12 1.337(6) . ?
N12 C15 1.324(7) . ?
N21 C22 1.326(6) . ?
N21 N22 1.340(5) . ?
N22 C25 1.325(6) . ?
C1 C2 1.525(7) . ?
C2 C3 1.390(7) . ?
C3 C4 1.367(8) . ?
C4 C5 1.398(7) . ?
C5 C6 1.500(7) . ?
C11 C12 1.525(7) . ?
C11 Na2 2.912(5) . ?
C12 C13 1.394(7) . ?
C13 C14 1.366(8) . ?
C14 C15 1.399(8) . ?
C15 C16 1.540(7) . ?
C16 Na2 2.893(6) 4_566 ?
C21 C22 1.512(7) . ?
C22 C23 1.377(7) . ?
C23 C24 1.361(8) . ?
C24 C25 1.381(7) . ?
C25 C26 1.520(7) . ?
C26 Na1 2.748(6) 4_566 ?
Na2 O6 2.355(5) . ?
Na2 O13 2.369(4) 4_665 ?
Na2 O5 2.384(5) 2_645 ?
Na2 O14 2.822(5) 4_665 ?
Na2 C16 2.893(6) 4_665 ?

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
O11 Mn1 O1 92.46(15) . . ?
O11 Mn1 O21 90.02(15) . . ?
O1 Mn1 O21 86.30(16) . . ?
O11 Mn1 N11 73.13(14) . . ?
O1 Mn1 N11 138.09(15) . . ?
O21 Mn1 N11 131.46(15) . . ?
O11 Mn1 N1 138.21(16) . . ?
O1 Mn1 N1 73.35(14) . . ?
O21 Mn1 N1 126.71(15) . . ?
N11 Mn1 N1 91.36(14) . . ?
O11 Mn1 N21 135.61(16) . . ?
O1 Mn1 N21 124.83(15) . . ?
O21 Mn1 N21 71.56(14) . . ?
N11 Mn1 N21 89.17(14) . . ?
N1 Mn1 N21 80.78(15) . . ?
O13 Mn2 O23 92.34(15) . . ?
O13 Mn2 O3 90.80(15) . . ?
O23 Mn2 O3 86.82(17) . . ?
O13 Mn2 N12 72.86(15) . . ?
O23 Mn2 N12 134.41(16) . . ?
O3 Mn2 N12 134.73(16) . . ?
O13 Mn2 N2 135.98(16) . . ?
O23 Mn2 N2 125.01(15) . . ?
O3 Mn2 N2 71.29(14) . . ?
N12 Mn2 N2 91.42(15) . . ?
O13 Mn2 N22 137.54(15) . . ?
O23 Mn2 N22 72.78(14) . . ?
O3 Mn2 N22 126.48(15) . . ?
N12 Mn2 N22 89.39(14) . . ?
N2 Mn2 N22 81.01(15) . . ?
O5 Na1 O6 90.58(17) . . ?
O5 Na1 O23 116.33(16) . 4_665 ?
O6 Na1 O23 84.29(15) . 4_665 ?
O5 Na1 O2 84.87(17) . . ?
O6 Na1 O2 127.95(16) . . ?
O23 Na1 O2 142.83(18) 4_665 . ?
O5 Na1 O24 87.27(17) . 4_665 ?
O6 Na1 O24 130.44(16) . 4_665 ?
O23 Na1 O24 53.51(14) 4_665 4_665 ?
O2 Na1 O24 101.17(16) . 4_665 ?
O5 Na1 O1 113.70(16) . . ?
O6 Na1 O1 82.51(14) . . ?
O23 Na1 O1 128.17(17) 4_665 . ?
O2 Na1 O1 53.29(13) . . ?
O24 Na1 O1 142.21(18) 4_665 . ?
O5 Na1 C26 99.15(17) . 4_665 ?
O6 Na1 C26 106.17(17) . 4_665 ?
O23 Na1 C26 27.42(15) 4_665 4_665 ?
O2 Na1 C26 125.78(18) . 4_665 ?
O24 Na1 C26 26.69(15) 4_665 4_665 ?
O1 Na1 C26 146.11(19) . 4_665 ?
O5 Na1 C1 96.23(17) . . ?
O6 Na1 C1 103.95(17) . . ?
O23 Na1 C1 146.53(18) 4_665 . ?
O2 Na1 C1 26.48(15) . . ?
O24 Na1 C1 125.52(18) 4_665 . ?
O1 Na1 C1 27.45(14) . . ?
C26 Na1 C1 145.86(19) 4_665 . ?
O5 Na1 Na2 122.12(14) . . ?
O6 Na1 Na2 31.54(11) . . ?
O23 Na1 Na2 71.79(11) 4_665 . ?
O2 Na1 Na2 124.36(12) . . ?
O24 Na1 Na2 125.27(13) 4_665 . ?
O1 Na1 Na2 71.07(11) . . ?
C26 Na1 Na2 99.00(14) 4_665 . ?
C1 Na1 Na2 98.25(14) . . ?
C1 O1 Mn1 120.3(3) . . ?
C1 O1 Na1 88.5(3) . . ?
Mn1 O1 Na1 150.82(19) . . ?
C1 O2 Na1 90.0(3) . . ?
C6 O3 Mn2 121.8(3) . . ?
Na2 O5 Na1 127.2(2) 2_655 . ?
C11 O11 Mn1 123.4(3) . . ?
C11 O11 Na2 102.4(3) . . ?
Mn1 O11 Na2 133.74(18) . . ?
C11 O12 Na2 81.9(3) . . ?
C16 O13 Mn2 123.6(3) . . ?
C16 O13 Na2 101.3(3) . 4_566 ?
Mn2 O13 Na2 133.7(2) . 4_566 ?
C16 O14 Na2 80.8(3) . 4_566 ?
C21 O21 Mn1 121.1(3) . . ?
C26 O23 Mn2 120.5(3) . . ?
C26 O23 Na1 89.2(3) . 4_566 ?
Mn2 O23 Na1 149.78(19) . 4_566 ?
C26 O24 Na1 89.4(3) . 4_566 ?
C2 N1 N2 120.0(4) . . ?
C2 N1 Mn1 111.6(3) . . ?
N2 N1 Mn1 127.4(3) . . ?
C5 N2 N1 119.1(4) . . ?
C5 N2 Mn2 112.7(3) . . ?
N1 N2 Mn2 126.6(3) . . ?
C12 N11 N12 120.1(4) . . ?
C12 N11 Mn1 112.4(3) . . ?
N12 N11 Mn1 127.5(3) . . ?
C15 N12 N11 119.9(4) . . ?
C15 N12 Mn2 113.0(3) . . ?
N11 N12 Mn2 127.0(3) . . ?
C22 N21 N22 118.8(4) . . ?
C22 N21 Mn1 112.6(3) . . ?
N22 N21 Mn1 126.9(3) . . ?
C25 N22 N21 120.0(4) . . ?
C25 N22 Mn2 111.7(3) . . ?
N21 N22 Mn2 127.0(3) . . ?
O2 C1 O1 125.0(5) . . ?
O2 C1 C2 118.8(5) . . ?
O1 C1 C2 116.2(5) . . ?
O2 C1 Na1 63.5(3) . . ?
O1 C1 Na1 64.0(3) . . ?
C2 C1 Na1 162.0(4) . . ?
N1 C2 C3 122.8(5) . . ?
N1 C2 C1 115.3(5) . . ?
C3 C2 C1 121.9(5) . . ?
C4 C3 C2 117.5(5) . . ?
C3 C4 C5 117.8(5) . . ?
N2 C5 C4 122.7(5) . . ?
N2 C5 C6 115.0(5) . . ?
C4 C5 C6 122.3(5) . . ?
O4 C6 O3 127.0(5) . . ?
O4 C6 C5 117.3(5) . . ?
O3 C6 C5 115.7(5) . . ?
O12 C11 O11 125.9(5) . . ?
O12 C11 C12 118.9(5) . . ?
O11 C11 C12 115.2(5) . . ?
O12 C11 Na2 73.3(3) . . ?
O11 C11 Na2 52.6(3) . . ?
C12 C11 Na2 167.8(4) . . ?
N11 C12 C13 122.2(4) . . ?
N11 C12 C11 115.5(4) . . ?
C13 C12 C11 122.3(5) . . ?
C14 C13 C12 117.6(5) . . ?
C13 C14 C15 117.9(5) . . ?
N12 C15 C14 122.2(5) . . ?
N12 C15 C16 115.2(4) . . ?
C14 C15 C16 122.6(5) . . ?
O14 C16 O13 127.8(5) . . ?
O14 C16 C15 117.7(5) . . ?
O13 C16 C15 114.5(5) . . ?
O14 C16 Na2 74.4(3) . 4_566 ?
O13 C16 Na2 53.4(3) . 4_566 ?
C15 C16 Na2 167.8(4) . 4_566 ?
O22 C21 O21 126.8(5) . . ?
O22 C21 C22 116.7(5) . . ?
O21 C21 C22 116.6(5) . . ?
N21 C22 C23 122.9(5) . . ?
N21 C22 C21 114.2(5) . . ?
C23 C22 C21 122.9(5) . . ?
C24 C23 C22 118.2(5) . . ?
C23 C24 C25 117.1(5) . . ?
N22 C25 C24 122.7(5) . . ?
N22 C25 C26 114.7(4) . . ?
C24 C25 C26 122.6(5) . . ?
O24 C26 O23 124.9(5) . . ?
O24 C26 C25 118.3(5) . . ?
O23 C26 C25 116.7(5) . . ?
O24 C26 Na1 63.9(3) . 4_566 ?
O23 C26 Na1 63.4(3) . 4_566 ?
C25 C26 Na1 161.8(4) . 4_566 ?
O6 Na2 O13 86.37(15) . 4_665 ?
O6 Na2 O11 87.49(15) . . ?
O13 Na2 O11 163.55(18) 4_665 . ?
O6 Na2 O5 113.76(18) . 2_645 ?
O13 Na2 O5 85.03(15) 4_665 2_645 ?
O11 Na2 O5 83.51(15) . 2_645 ?
O6 Na2 O12 103.23(15) . . ?
O13 Na2 O12 146.76(17) 4_665 . ?
O11 Na2 O12 49.68(13) . . ?
O5 Na2 O12 118.16(15) 2_645 . ?
O6 Na2 O14 94.84(15) . 4_665 ?
O13 Na2 O14 49.99(13) 4_665 4_665 ?
O11 Na2 O14 145.95(16) . 4_665 ?
O5 Na2 O14 125.40(16) 2_645 4_665 ?
O12 Na2 O14 97.09(14) . 4_665 ?
O6 Na2 C16 90.08(16) . 4_665 ?
O13 Na2 C16 25.25(14) 4_665 4_665 ?
O11 Na2 C16 169.98(19) . 4_665 ?
O5 Na2 C16 106.34(16) 2_645 4_665 ?
O12 Na2 C16 121.79(17) . 4_665 ?
O14 Na2 C16 24.76(14) 4_665 4_665 ?
O6 Na2 C11 95.25(16) . . ?
O13 Na2 C11 171.42(19) 4_665 . ?
O11 Na2 C11 24.93(14) . . ?
O5 Na2 C11 101.93(16) 2_645 . ?
O12 Na2 C11 24.76(13) . . ?
O14 Na2 C11 121.44(16) 4_665 . ?
C16 Na2 C11 146.18(19) 4_665 . ?
O6 Na2 Na1 32.40(11) . . ?
O13 Na2 Na1 82.61(12) 4_665 . ?
O11 Na2 Na1 84.02(12) . . ?
O5 Na2 Na1 81.36(13) 2_645 . ?
O12 Na2 Na1 122.04(11) . . ?
O14 Na2 Na1 115.04(11) 4_665 . ?
C16 Na2 Na1 99.04(13) 4_665 . ?
C11 Na2 Na1 103.24(13) . . ?
Na2 O6 Na1 116.06(19) . . ?

_diffrn_measured_fraction_theta_max 0.992
_diffrn_reflns_theta_full        26.00
_diffrn_measured_fraction_theta_full 0.992
_refine_diff_density_max         0.814
_refine_diff_density_min         -0.557
_refine_diff_density_rms         0.115



