# Electronic Supplementary Material (ESI) for CrystEngComm
# This journal is © The Royal Society of Chemistry 2011


data_global
_journal_name_full               CrystEngComm

_journal_coden_Cambridge         1350
_journal_volume                  ?
_journal_page_first              ?
_journal_year                    ?

_publ_contact_author_name        'Dr Tong-Bu Lu'
_publ_contact_author_email       lutongbu@mail.sysu.edu.cn

_publ_section_title              
;
Three porous metal-organic frameworks
based on azobenzenetricarboxylate ligand: synthesis,
structures, and magnetic property
;
loop_
_publ_author_name
'Miao Meng'
'Di-Chang Zhong'
'Tong-Bu Lu'

# Attachment '- 1.cif'

data_l04171m
_database_code_depnum_ccdc_archive 'CCDC 832310'
#TrackingRef '- 1.cif'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C15 H18 Cd N2 O11'
_chemical_formula_weight         514.71

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'
Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   P2(1)/c

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

_cell_length_a                   9.7727(18)
_cell_length_b                   18.576(3)
_cell_length_c                   10.561(2)
_cell_angle_alpha                90.00
_cell_angle_beta                 98.148(3)
_cell_angle_gamma                90.00
_cell_volume                     1897.8(6)
_cell_formula_units_Z            4
_cell_measurement_temperature    110(2)
_cell_measurement_reflns_used    3524
_cell_measurement_theta_min      2.19
_cell_measurement_theta_max      26.96

_exptl_crystal_description       block
_exptl_crystal_colour            orange
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.20
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.801
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             992
_exptl_absorpt_coefficient_mu    1.214
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.7274
_exptl_absorpt_correction_T_max  0.7933
_exptl_absorpt_process_details   'SADABS (SHELDRICK,1996)'

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      110(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         0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        0
_diffrn_reflns_number            9981
_diffrn_reflns_av_R_equivalents  0.0385
_diffrn_reflns_av_sigmaI/netI    0.0551
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_theta_min         2.11
_diffrn_reflns_theta_max         27.07
_reflns_number_total             4122
_reflns_number_gt                2956
_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^)+(0.0657P)^2^+2.3647P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         4122
_refine_ls_number_parameters     290
_refine_ls_number_restraints     24
_refine_ls_R_factor_all          0.0723
_refine_ls_R_factor_gt           0.0447
_refine_ls_wR_factor_ref         0.1314
_refine_ls_wR_factor_gt          0.1191
_refine_ls_goodness_of_fit_ref   1.107
_refine_ls_restrained_S_all      1.115
_refine_ls_shift/su_max          0.009
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Cd1 Cd 0.61144(4) 0.214677(18) 1.19064(3) 0.02052(14) Uani 1 1 d . . .
C1 C 0.7418(5) 0.0831(3) 1.0234(5) 0.0209(11) Uani 1 1 d . . .
C2 C 0.8331(5) 0.0604(3) 0.9314(5) 0.0170(10) Uani 1 1 d . . .
C3 C 0.9085(6) 0.1129(3) 0.8780(5) 0.0226(11) Uani 1 1 d . . .
H3 H 0.8999 0.1619 0.9015 0.027 Uiso 1 1 calc R . .
C4 C 0.9959(6) 0.0948(3) 0.7910(5) 0.0235(12) Uani 1 1 d . . .
H4 H 1.0477 0.1310 0.7555 0.028 Uiso 1 1 calc R . .
C5 C 1.0074(5) 0.0229(3) 0.7559(5) 0.0189(11) Uani 1 1 d . . .
C6 C 0.9335(5) -0.0303(3) 0.8099(5) 0.0199(11) Uani 1 1 d . . .
H6 H 0.9429 -0.0793 0.7869 0.024 Uiso 1 1 calc R . .
C7 C 0.8459(5) -0.0116(3) 0.8974(5) 0.0175(10) Uani 1 1 d . . .
H7 H 0.7949 -0.0478 0.9339 0.021 Uiso 1 1 calc R . .
C8 C 1.2378(5) 0.0233(3) 0.5252(5) 0.0170(10) Uani 1 1 d . . .
C9 C 1.3086(5) 0.0764(3) 0.4685(5) 0.0183(10) Uani 1 1 d . . .
H9 H 1.3010 0.1253 0.4932 0.022 Uiso 1 1 calc R . .
C10 C 1.3901(5) 0.0585(2) 0.3762(5) 0.0151(10) Uani 1 1 d . . .
C11 C 1.4645(5) 0.1155(3) 0.3125(5) 0.0182(10) Uani 1 1 d . . .
C12 C 1.4014(5) -0.0136(3) 0.3403(5) 0.0169(10) Uani 1 1 d . . .
H12 H 1.4570 -0.0261 0.2767 0.020 Uiso 1 1 calc R . .
C13 C 1.3313(5) -0.0671(2) 0.3975(5) 0.0164(10) Uani 1 1 d . . .
C14 C 1.3481(5) -0.1445(3) 0.3601(5) 0.0175(10) Uani 1 1 d . . .
C15 C 1.2489(5) -0.0491(3) 0.4893(5) 0.0171(10) Uani 1 1 d . . .
H15 H 1.2001 -0.0854 0.5277 0.021 Uiso 1 1 calc R . .
N1 N 1.0926(4) -0.0014(2) 0.6655(4) 0.0208(10) Uani 1 1 d . . .
N2 N 1.1540(5) 0.0468(2) 0.6166(4) 0.0229(10) Uani 1 1 d . . .
O1 O 0.7394(4) 0.14530(18) 1.0607(3) 0.0238(8) Uani 1 1 d . . .
O2 O 0.6660(4) 0.03151(18) 1.0631(4) 0.0297(9) Uani 1 1 d . . .
H2 H 0.6115 0.0492 1.1094 0.045 Uiso 1 1 calc R . .
O3 O 1.2792(4) -0.19271(18) 0.4106(3) 0.0218(8) Uani 1 1 d . . .
O4 O 1.4305(4) -0.16035(18) 0.2852(4) 0.0258(8) Uani 1 1 d . . .
O5 O 1.5276(4) 0.09803(18) 0.2203(3) 0.0268(9) Uani 1 1 d . . .
O6 O 1.4636(4) 0.17987(18) 0.3484(3) 0.0245(8) Uani 1 1 d . . .
O7 O 0.4232(4) 0.22388(19) 1.0315(4) 0.0285(9) Uani 1 1 d . . .
O8 O 0.7863(4) 0.2090(2) 1.3529(4) 0.0309(9) Uani 1 1 d . . .
O1W O 0.3654(8) 0.1232(4) 0.8582(7) 0.050(2) Uani 0.67 1 d P . .
O1W' O 0.3781(16) 0.1568(9) 0.9478(16) 0.057(4) Uani 0.33 1 d P . .
O2W O 0.0625(15) 0.2099(7) 0.3899(16) 0.132(5) Uani 0.67 1 d PU . .
O2W' O 0.001(2) 0.2138(10) 0.224(2) 0.090(6) Uani 0.33 1 d PU . .
O3W O 0.1885(13) 0.2535(8) 0.1733(14) 0.127(4) Uani 0.67 1 d PU . .
O3W' O 0.091(2) 0.2503(14) 0.074(2) 0.109(7) Uani 0.33 1 d PU . .

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
Cd1 0.0345(2) 0.01071(19) 0.0192(2) 0.00003(15) 0.01360(15) -0.00259(16)
C1 0.025(3) 0.020(3) 0.019(3) 0.000(2) 0.009(2) -0.001(2)
C2 0.015(2) 0.018(2) 0.019(3) -0.001(2) 0.006(2) 0.0008(19)
C3 0.030(3) 0.015(2) 0.025(3) -0.004(2) 0.009(2) 0.000(2)
C4 0.029(3) 0.016(2) 0.028(3) -0.003(2) 0.013(2) -0.001(2)
C5 0.017(3) 0.021(3) 0.020(3) 0.003(2) 0.006(2) 0.004(2)
C6 0.022(3) 0.019(2) 0.020(3) -0.001(2) 0.008(2) 0.003(2)
C7 0.020(3) 0.018(2) 0.016(2) 0.0006(19) 0.006(2) 0.001(2)
C8 0.019(3) 0.018(2) 0.015(2) -0.0010(19) 0.006(2) 0.001(2)
C9 0.027(3) 0.012(2) 0.017(2) -0.0032(19) 0.010(2) -0.002(2)
C10 0.017(2) 0.014(2) 0.014(2) 0.0021(18) 0.0039(19) 0.0031(19)
C11 0.020(3) 0.017(2) 0.019(2) 0.001(2) 0.008(2) 0.001(2)
C12 0.018(3) 0.017(2) 0.017(2) -0.0004(18) 0.006(2) 0.0017(19)
C13 0.021(3) 0.013(2) 0.016(2) 0.0021(19) 0.004(2) 0.002(2)
C14 0.023(3) 0.011(2) 0.018(2) -0.0003(19) 0.000(2) 0.005(2)
C15 0.020(3) 0.013(2) 0.020(3) 0.0024(19) 0.007(2) -0.0003(19)
N1 0.025(2) 0.019(2) 0.021(2) 0.0031(17) 0.0125(19) 0.0011(18)
N2 0.032(3) 0.015(2) 0.025(2) -0.0014(18) 0.016(2) 0.0007(18)
O1 0.033(2) 0.0158(17) 0.026(2) -0.0040(15) 0.0166(17) -0.0020(16)
O2 0.036(2) 0.0180(19) 0.042(2) -0.0072(17) 0.029(2) -0.0064(16)
O3 0.037(2) 0.0104(15) 0.0206(18) 0.0015(14) 0.0110(16) 0.0012(15)
O4 0.040(2) 0.0130(17) 0.029(2) -0.0045(15) 0.0198(18) 0.0001(16)
O5 0.045(2) 0.0149(17) 0.027(2) -0.0023(15) 0.0239(18) -0.0014(16)
O6 0.037(2) 0.0151(18) 0.0244(19) -0.0025(15) 0.0161(17) -0.0040(16)
O7 0.032(2) 0.025(2) 0.029(2) 0.0047(17) 0.0070(17) -0.0040(17)
O8 0.040(2) 0.030(2) 0.025(2) 0.0015(17) 0.0120(18) -0.0022(18)
O1W 0.061(5) 0.038(4) 0.057(5) -0.022(4) 0.031(4) -0.019(3)
O1W' 0.059(10) 0.059(10) 0.057(10) -0.010(8) 0.020(8) -0.008(8)
O2W 0.131(6) 0.123(6) 0.140(6) -0.002(4) 0.016(5) 0.007(4)
O2W' 0.090(8) 0.093(8) 0.089(8) -0.005(5) 0.019(5) 0.004(5)
O3W 0.111(6) 0.146(6) 0.124(6) -0.022(5) 0.013(4) 0.025(5)
O3W' 0.106(8) 0.109(8) 0.110(8) -0.006(5) 0.009(5) 0.000(5)

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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cd1 O8 2.245(4) . ?
Cd1 O7 2.316(4) . ?
Cd1 O5 2.353(3) 1_456 ?
Cd1 O3 2.360(3) 2_756 ?
Cd1 O1 2.366(3) . ?
Cd1 O4 2.377(3) 2_756 ?
Cd1 O6 2.442(3) 1_456 ?
Cd1 C14 2.711(5) 2_756 ?
C1 O1 1.223(6) . ?
C1 O2 1.315(6) . ?
C1 C2 1.470(7) . ?
C2 C3 1.390(7) . ?
C2 C7 1.395(7) . ?
C3 C4 1.381(7) . ?
C3 H3 0.9500 . ?
C4 C5 1.396(6) . ?
C4 H4 0.9500 . ?
C5 C6 1.392(7) . ?
C5 N1 1.426(6) . ?
C6 C7 1.389(7) . ?
C6 H6 0.9500 . ?
C7 H7 0.9500 . ?
C8 C9 1.388(7) . ?
C8 C15 1.406(7) . ?
C8 N2 1.420(6) . ?
C9 C10 1.385(6) . ?
C9 H9 0.9500 . ?
C10 C12 1.402(6) . ?
C10 C11 1.496(7) . ?
C11 O6 1.256(6) . ?
C11 O5 1.266(6) . ?
C12 C13 1.392(7) . ?
C12 H12 0.9500 . ?
C13 C15 1.386(6) . ?
C13 C14 1.506(6) . ?
C14 O4 1.242(6) . ?
C14 O3 1.281(6) . ?
C14 Cd1 2.711(5) 2_746 ?
C15 H15 0.9500 . ?
N1 N2 1.232(6) . ?
O2 H2 0.8400 . ?
O3 Cd1 2.360(3) 2_746 ?
O4 Cd1 2.377(3) 2_746 ?
O5 Cd1 2.353(3) 1_654 ?
O6 Cd1 2.442(3) 1_654 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O8 Cd1 O7 176.55(13) . . ?
O8 Cd1 O5 95.56(14) . 1_456 ?
O7 Cd1 O5 84.77(13) . 1_456 ?
O8 Cd1 O3 92.01(13) . 2_756 ?
O7 Cd1 O3 88.96(13) . 2_756 ?
O5 Cd1 O3 156.96(12) 1_456 2_756 ?
O8 Cd1 O1 90.55(14) . . ?
O7 Cd1 O1 92.88(13) . . ?
O5 Cd1 O1 78.36(11) 1_456 . ?
O3 Cd1 O1 79.84(12) 2_756 . ?
O8 Cd1 O4 95.05(14) . 2_756 ?
O7 Cd1 O4 82.78(13) . 2_756 ?
O5 Cd1 O4 144.72(13) 1_456 2_756 ?
O3 Cd1 O4 55.44(12) 2_756 2_756 ?
O1 Cd1 O4 135.04(12) . 2_756 ?
O8 Cd1 O6 85.79(14) . 1_456 ?
O7 Cd1 O6 91.64(13) . 1_456 ?
O5 Cd1 O6 54.17(11) 1_456 1_456 ?
O3 Cd1 O6 148.41(12) 2_756 1_456 ?
O1 Cd1 O6 131.63(11) . 1_456 ?
O4 Cd1 O6 93.30(12) 2_756 1_456 ?
O8 Cd1 C14 94.55(14) . 2_756 ?
O7 Cd1 C14 84.76(13) . 2_756 ?
O5 Cd1 C14 168.06(14) 1_456 2_756 ?
O3 Cd1 C14 28.19(13) 2_756 2_756 ?
O1 Cd1 C14 107.88(14) . 2_756 ?
O4 Cd1 C14 27.26(13) 2_756 2_756 ?
O6 Cd1 C14 120.49(13) 1_456 2_756 ?
O1 C1 O2 123.3(4) . . ?
O1 C1 C2 121.6(4) . . ?
O2 C1 C2 115.1(4) . . ?
C3 C2 C7 119.8(4) . . ?
C3 C2 C1 118.2(4) . . ?
C7 C2 C1 122.0(4) . . ?
C4 C3 C2 120.8(5) . . ?
C4 C3 H3 119.6 . . ?
C2 C3 H3 119.6 . . ?
C3 C4 C5 119.4(5) . . ?
C3 C4 H4 120.3 . . ?
C5 C4 H4 120.3 . . ?
C6 C5 C4 120.3(5) . . ?
C6 C5 N1 115.9(4) . . ?
C4 C5 N1 123.9(5) . . ?
C7 C6 C5 120.0(5) . . ?
C7 C6 H6 120.0 . . ?
C5 C6 H6 120.0 . . ?
C6 C7 C2 119.8(4) . . ?
C6 C7 H7 120.1 . . ?
C2 C7 H7 120.1 . . ?
C9 C8 C15 120.1(4) . . ?
C9 C8 N2 116.4(4) . . ?
C15 C8 N2 123.4(4) . . ?
C10 C9 C8 120.3(4) . . ?
C10 C9 H9 119.8 . . ?
C8 C9 H9 119.8 . . ?
C9 C10 C12 119.7(4) . . ?
C9 C10 C11 120.8(4) . . ?
C12 C10 C11 119.5(4) . . ?
O6 C11 O5 120.1(4) . . ?
O6 C11 C10 120.8(4) . . ?
O5 C11 C10 119.0(4) . . ?
C13 C12 C10 120.2(4) . . ?
C13 C12 H12 119.9 . . ?
C10 C12 H12 119.9 . . ?
C15 C13 C12 120.1(4) . . ?
C15 C13 C14 120.6(4) . . ?
C12 C13 C14 119.3(4) . . ?
O4 C14 O3 121.7(4) . . ?
O4 C14 C13 119.9(4) . . ?
O3 C14 C13 118.4(4) . . ?
O4 C14 Cd1 61.2(2) . 2_746 ?
O3 C14 Cd1 60.5(2) . 2_746 ?
C13 C14 Cd1 176.0(3) . 2_746 ?
C13 C15 C8 119.6(4) . . ?
C13 C15 H15 120.2 . . ?
C8 C15 H15 120.2 . . ?
N2 N1 C5 114.6(4) . . ?
N1 N2 C8 115.1(4) . . ?
C1 O1 Cd1 137.5(3) . . ?
C1 O2 H2 109.5 . . ?
C14 O3 Cd1 91.3(3) . 2_746 ?
C14 O4 Cd1 91.5(3) . 2_746 ?
C11 O5 Cd1 94.8(3) . 1_654 ?
C11 O6 Cd1 90.9(3) . 1_654 ?

_diffrn_measured_fraction_theta_max 0.986
_diffrn_reflns_theta_full        27.07
_diffrn_measured_fraction_theta_full 0.986
_refine_diff_density_max         1.453
_refine_diff_density_min         -0.799
_refine_diff_density_rms         0.152

#start Validation Reply Form

_vrf_PLAT430_l04171m             
;
PROBLEM: Short Inter D...A Contact O2W' .. O3W' .. 2.03 Ang.
RESPONSE: The lattice water molecules are disordered and the H atoms of
coordinated/lattice water molecules were not added.
;

# Attachment '- 2.cif'

data_exp_13084
_database_code_depnum_ccdc_archive 'CCDC 832311'
#TrackingRef '- 2.cif'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C34 H47 Cd3 N5 O25'
_chemical_formula_weight         1262.97

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cd Cd 0.1185 4.6533 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   c2

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

_cell_length_a                   19.0321(4)
_cell_length_b                   7.14890(10)
_cell_length_c                   18.7460(4)
_cell_angle_alpha                90.00
_cell_angle_beta                 119.292(3)
_cell_angle_gamma                90.00
_cell_volume                     2224.43(10)
_cell_formula_units_Z            2
_cell_measurement_temperature    123(2)
_cell_measurement_reflns_used    682
_cell_measurement_theta_min      2.7
_cell_measurement_theta_max      62.67

_exptl_crystal_description       block
_exptl_crystal_colour            orange
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.16
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.886
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1194
_exptl_absorpt_coefficient_mu    12.233
_exptl_absorpt_correction_type   MULTI-SCAN
_exptl_absorpt_correction_T_min  0.1431
_exptl_absorpt_correction_T_max  0.2450
_exptl_absorpt_process_details   'SADABS (SHELDRICK, 1996)'

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      123(2)
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_type           CuK\a
_diffrn_radiation_source         'Enhance (Cu) X-ray Source'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Gemini S Ultra'
_diffrn_measurement_method       '\w and \p scan'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        0
_diffrn_reflns_number            6037
_diffrn_reflns_av_R_equivalents  0.0217
_diffrn_reflns_av_sigmaI/netI    0.0235
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         2.70
_diffrn_reflns_theta_max         62.67
_reflns_number_total             3007
_reflns_number_gt                2958
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker FRAMBO'
_computing_cell_refinement       'Bruker FRAMBO'
_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^)+(0.0462P)^2^+14.8327P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.032(11)
_refine_ls_number_reflns         3007
_refine_ls_number_parameters     297
_refine_ls_number_restraints     18
_refine_ls_R_factor_all          0.0304
_refine_ls_R_factor_gt           0.0299
_refine_ls_wR_factor_ref         0.0872
_refine_ls_wR_factor_gt          0.0867
_refine_ls_goodness_of_fit_ref   1.158
_refine_ls_restrained_S_all      1.162
_refine_ls_shift/su_max          0.010
_refine_ls_shift/su_mean         0.001

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Cd1 Cd 0.65256(2) 0.73880(7) 0.87447(3) 0.01758(14) Uani 1 1 d . . .
Cd2 Cd 0.5000 0.40075(9) 0.0000 0.01888(18) Uani 1 2 d S . .
C1 C 0.7403(4) 0.5703(10) 0.8110(4) 0.0174(14) Uani 1 1 d . . .
C2 C 0.7858(4) 0.5102(10) 0.7685(4) 0.0144(14) Uani 1 1 d . . .
C3 C 0.8674(4) 0.4665(9) 0.8109(4) 0.0147(14) Uani 1 1 d . . .
H3 H 0.8944 0.4678 0.8678 0.018 Uiso 1 1 calc R . .
C4 C 0.9094(4) 0.4211(11) 0.7702(4) 0.0165(13) Uani 1 1 d . . .
C5 C 0.9971(4) 0.3699(10) 0.8141(4) 0.0164(14) Uani 1 1 d . . .
C6 C 0.8689(4) 0.4190(11) 0.6841(4) 0.0178(14) Uani 1 1 d . . .
H6 H 0.8964 0.3886 0.6562 0.021 Uiso 1 1 calc R . .
C7 C 0.7875(4) 0.4628(10) 0.6414(4) 0.0191(15) Uani 1 1 d . . .
C8 C 0.7451(4) 0.5071(11) 0.6829(5) 0.0217(17) Uani 1 1 d . . .
H8 H 0.6903 0.5342 0.6538 0.026 Uiso 1 1 calc R . .
C9 C 0.7356(4) 0.4664(10) 0.4312(4) 0.0200(16) Uani 1 1 d . . .
C10 C 0.7787(5) 0.4937(12) 0.3910(4) 0.0252(17) Uani 1 1 d . . .
H10 H 0.8340 0.5140 0.4206 0.030 Uiso 1 1 calc R . .
C11 C 0.7397(4) 0.4911(11) 0.3062(4) 0.0219(16) Uani 1 1 d . . .
H11 H 0.7689 0.5134 0.2792 0.026 Uiso 1 1 calc R . .
C12 C 0.6572(4) 0.4553(10) 0.2612(4) 0.0190(15) Uani 1 1 d . . .
C13 C 0.6148(4) 0.4439(10) 0.1703(4) 0.0187(15) Uani 1 1 d . . .
C14 C 0.6143(4) 0.4261(13) 0.3038(4) 0.0273(17) Uani 1 1 d . . .
H14 H 0.5590 0.4057 0.2747 0.033 Uiso 1 1 calc R . .
C15 C 0.6533(4) 0.4275(13) 0.3878(4) 0.0264(17) Uani 1 1 d . . .
H15 H 0.6250 0.4027 0.4155 0.032 Uiso 1 1 calc R . .
N1 N 0.7410(4) 0.4645(9) 0.5544(4) 0.0215(14) Uani 1 1 d . . .
N2 N 0.7819(4) 0.4697(9) 0.5191(4) 0.0222(13) Uani 1 1 d . . .
O1 O 0.7748(3) 0.5639(7) 0.8887(3) 0.0175(10) Uani 1 1 d . . .
O2 O 0.6699(3) 0.6242(8) 0.7688(3) 0.0276(13) Uani 1 1 d . . .
O3 O 1.0379(3) 0.3826(8) 0.8920(3) 0.0215(11) Uani 1 1 d . . .
O4 O 1.0283(3) 0.3136(8) 0.7731(3) 0.0290(13) Uani 1 1 d . . .
O5 O 0.6527(3) 0.4550(8) 0.1317(3) 0.0266(13) Uani 1 1 d . . .
O6 O 0.5385(3) 0.4204(9) 0.1332(3) 0.0244(11) Uani 1 1 d . . .
O7 O 0.7085(3) 1.0182(8) 0.8643(3) 0.0241(11) Uani 1 1 d . . .
O8 O 0.7313(3) 0.7782(8) 1.0134(3) 0.0257(12) Uani 1 1 d . . .
O9 O 0.6064(3) 0.4478(8) 0.8819(4) 0.0331(13) Uani 1 1 d . . .
O10 O 0.5000 0.7145(13) 0.0000 0.045(2) Uani 1 2 d S . .
O11 O 0.4154(3) 0.1887(8) 0.0089(3) 0.0326(14) Uani 1 1 d . . .
O1W O 0.6007(4) 0.2276(12) 0.7411(4) 0.0567(17) Uani 1 1 d . . .
C16 C 0.5000 0.428(3) 0.5000 0.132(4) Uani 1 2 d SDU . .
C17 C 0.4850(12) 0.737(3) 0.4263(5) 0.132(4) Uani 1 1 d DU . .
N3 N 0.5000 0.620(3) 0.5000 0.132(4) Uani 1 2 d SD . .
O12 O 0.4840(17) 0.328(4) 0.4386(14) 0.132(4) Uani 0.50 1 d PD . .
O13 O 0.489(2) 0.929(11) 0.423(2) 0.115(8) Uani 0.20 1 d PD . .
C18 C 0.5000 1.007(5) 0.5000 0.115(8) Uani 1 2 d SD . .
O13' O 0.5282(16) 1.053(8) 0.420(2) 0.115(8) Uani 0.30 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
Cd1 0.0150(2) 0.0256(3) 0.0146(2) -0.0012(2) 0.00920(17) 0.0012(2)
Cd2 0.0266(4) 0.0212(4) 0.0109(3) 0.000 0.0108(3) 0.000
C1 0.021(3) 0.020(4) 0.013(3) -0.004(3) 0.009(3) -0.001(3)
C2 0.021(3) 0.015(4) 0.012(3) -0.002(3) 0.011(3) 0.000(3)
C3 0.018(3) 0.015(4) 0.010(3) 0.000(3) 0.005(3) 0.001(3)
C4 0.017(3) 0.021(4) 0.012(3) -0.002(3) 0.007(3) -0.001(3)
C5 0.019(3) 0.017(4) 0.015(3) -0.001(3) 0.010(3) 0.000(3)
C6 0.022(3) 0.016(4) 0.020(3) -0.001(3) 0.015(3) 0.002(3)
C7 0.021(4) 0.023(4) 0.011(3) 0.000(3) 0.007(3) -0.002(3)
C8 0.014(3) 0.032(5) 0.018(4) 0.003(3) 0.008(3) 0.003(3)
C9 0.027(4) 0.020(4) 0.011(3) 0.000(3) 0.008(3) 0.003(3)
C10 0.021(4) 0.038(5) 0.015(4) -0.002(3) 0.007(3) -0.001(3)
C11 0.018(4) 0.034(4) 0.014(4) -0.001(3) 0.009(3) 0.000(3)
C12 0.024(4) 0.019(4) 0.015(3) 0.003(3) 0.010(3) 0.006(3)
C13 0.024(4) 0.019(4) 0.015(3) 0.000(3) 0.011(3) 0.003(3)
C14 0.019(3) 0.046(5) 0.016(3) -0.003(4) 0.008(3) 0.003(3)
C15 0.026(4) 0.043(5) 0.012(3) 0.012(3) 0.011(3) 0.006(3)
N1 0.025(3) 0.030(4) 0.009(3) -0.002(2) 0.008(3) 0.004(3)
N2 0.023(3) 0.029(4) 0.014(3) -0.006(3) 0.009(3) 0.000(3)
O1 0.019(2) 0.024(3) 0.011(2) -0.003(2) 0.0089(19) -0.002(2)
O2 0.019(3) 0.048(4) 0.015(2) 0.001(2) 0.008(2) 0.016(2)
O3 0.019(2) 0.029(3) 0.016(2) -0.001(2) 0.008(2) 0.003(2)
O4 0.022(3) 0.050(4) 0.019(3) -0.002(2) 0.013(2) 0.008(2)
O5 0.023(3) 0.044(4) 0.016(2) -0.001(2) 0.012(2) 0.003(2)
O6 0.023(3) 0.039(3) 0.011(2) -0.001(2) 0.008(2) -0.004(2)
O7 0.026(3) 0.026(3) 0.025(3) -0.001(2) 0.016(2) -0.004(2)
O8 0.030(3) 0.032(4) 0.014(2) -0.002(2) 0.010(2) 0.004(2)
O9 0.029(3) 0.029(3) 0.045(3) 0.004(3) 0.021(3) -0.003(2)
O10 0.098(7) 0.022(5) 0.029(4) 0.000 0.042(5) 0.000
O11 0.027(3) 0.038(4) 0.018(3) 0.006(2) -0.001(2) -0.009(2)
O1W 0.060(4) 0.036(4) 0.058(4) 0.003(4) 0.017(3) 0.001(4)
C16 0.121(5) 0.142(6) 0.140(5) 0.000 0.070(4) 0.000
C17 0.121(5) 0.142(6) 0.140(5) 0.000 0.070(4) 0.000
N3 0.121(5) 0.142(6) 0.140(5) 0.000 0.070(4) 0.000
O12 0.121(5) 0.142(6) 0.140(5) 0.000 0.070(4) 0.000
O13 0.023(7) 0.19(3) 0.114(14) 0.00(2) 0.022(9) 0.024(16)
C18 0.023(7) 0.19(3) 0.114(14) 0.00(2) 0.022(9) 0.024(16)
O13' 0.023(7) 0.19(3) 0.114(14) 0.00(2) 0.022(9) 0.024(16)

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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cd1 O4 2.256(5) 3_455 ?
Cd1 O9 2.289(6) . ?
Cd1 O8 2.299(5) . ?
Cd1 O2 2.312(5) . ?
Cd1 O7 2.315(5) . ?
Cd1 O1 2.537(5) . ?
Cd1 O3 2.575(5) 3_455 ?
Cd2 O6 2.236(4) . ?
Cd2 O6 2.236(4) 2_655 ?
Cd2 O10 2.243(9) . ?
Cd2 O11 2.275(5) . ?
Cd2 O11 2.275(5) 2_655 ?
C1 O2 1.238(8) . ?
C1 O1 1.273(8) . ?
C1 C2 1.498(9) . ?
C2 C3 1.391(9) . ?
C2 C8 1.399(10) . ?
C3 C4 1.387(9) . ?
C3 H3 0.9300 . ?
C4 C6 1.407(9) . ?
C4 C5 1.501(9) . ?
C5 O4 1.245(8) . ?
C5 O3 1.279(8) . ?
C6 C7 1.388(10) . ?
C6 H6 0.9300 . ?
C7 C8 1.405(10) . ?
C7 N1 1.425(9) . ?
C8 H8 0.9300 . ?
C9 C10 1.373(11) . ?
C9 C15 1.394(11) . ?
C9 N2 1.438(9) . ?
C10 C11 1.387(10) . ?
C10 H10 0.9300 . ?
C11 C12 1.396(10) . ?
C11 H11 0.9300 . ?
C12 C14 1.409(10) . ?
C12 C13 1.488(9) . ?
C13 O5 1.250(8) . ?
C13 O6 1.278(9) . ?
C14 C15 1.374(10) . ?
C14 H14 0.9300 . ?
C15 H15 0.9300 . ?
N1 N2 1.245(8) . ?
O3 Cd1 2.575(5) 3_545 ?
O4 Cd1 2.257(5) 3_545 ?
C16 O12 1.257(10) . ?
C16 O12 1.257(10) 2_656 ?
C16 N3 1.374(10) . ?
C17 N3 1.517(10) . ?
N3 C17 1.517(10) 2_656 ?
O13 C18 1.456(10) . ?
C18 O13 1.456(10) 2_656 ?
C18 O13' 1.85(4) 2_656 ?
C18 O13' 1.85(4) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O4 Cd1 O9 89.5(2) 3_455 . ?
O4 Cd1 O8 139.32(17) 3_455 . ?
O9 Cd1 O8 95.7(2) . . ?
O4 Cd1 O2 83.84(17) 3_455 . ?
O9 Cd1 O2 87.1(2) . . ?
O8 Cd1 O2 136.60(17) . . ?
O4 Cd1 O7 93.5(2) 3_455 . ?
O9 Cd1 O7 174.27(19) . . ?
O8 Cd1 O7 85.20(19) . . ?
O2 Cd1 O7 88.3(2) . . ?
O4 Cd1 O1 137.28(16) 3_455 . ?
O9 Cd1 O1 84.57(18) . . ?
O8 Cd1 O1 83.40(16) . . ?
O2 Cd1 O1 53.68(15) . . ?
O7 Cd1 O1 89.92(17) . . ?
O4 Cd1 O3 53.72(16) 3_455 3_455 ?
O9 Cd1 O3 88.88(19) . 3_455 ?
O8 Cd1 O3 85.98(16) . 3_455 ?
O2 Cd1 O3 137.41(16) . 3_455 ?
O7 Cd1 O3 96.83(18) . 3_455 ?
O1 Cd1 O3 166.90(14) . 3_455 ?
O6 Cd2 O6 172.8(3) . 2_655 ?
O6 Cd2 O10 86.39(16) . . ?
O6 Cd2 O10 86.39(16) 2_655 . ?
O6 Cd2 O11 79.48(19) . . ?
O6 Cd2 O11 105.46(19) 2_655 . ?
O10 Cd2 O11 131.77(16) . . ?
O6 Cd2 O11 105.46(19) . 2_655 ?
O6 Cd2 O11 79.48(19) 2_655 2_655 ?
O10 Cd2 O11 131.77(16) . 2_655 ?
O11 Cd2 O11 96.5(3) . 2_655 ?
O2 C1 O1 122.3(6) . . ?
O2 C1 C2 118.4(6) . . ?
O1 C1 C2 119.4(6) . . ?
C3 C2 C8 119.3(6) . . ?
C3 C2 C1 122.3(6) . . ?
C8 C2 C1 118.3(6) . . ?
C4 C3 C2 121.4(6) . . ?
C4 C3 H3 119.3 . . ?
C2 C3 H3 119.3 . . ?
C3 C4 C6 119.6(6) . . ?
C3 C4 C5 122.7(6) . . ?
C6 C4 C5 117.6(6) . . ?
O4 C5 O3 121.4(6) . . ?
O4 C5 C4 118.6(6) . . ?
O3 C5 C4 120.0(6) . . ?
C7 C6 C4 119.3(6) . . ?
C7 C6 H6 120.3 . . ?
C4 C6 H6 120.3 . . ?
C6 C7 C8 120.8(6) . . ?
C6 C7 N1 123.7(6) . . ?
C8 C7 N1 115.4(6) . . ?
C2 C8 C7 119.5(6) . . ?
C2 C8 H8 120.2 . . ?
C7 C8 H8 120.2 . . ?
C10 C9 C15 120.6(7) . . ?
C10 C9 N2 115.5(6) . . ?
C15 C9 N2 123.8(6) . . ?
C9 C10 C11 120.0(7) . . ?
C9 C10 H10 120.0 . . ?
C11 C10 H10 120.0 . . ?
C10 C11 C12 120.5(7) . . ?
C10 C11 H11 119.7 . . ?
C12 C11 H11 119.7 . . ?
C11 C12 C14 118.5(6) . . ?
C11 C12 C13 121.5(6) . . ?
C14 C12 C13 120.0(6) . . ?
O5 C13 O6 121.1(6) . . ?
O5 C13 C12 121.1(6) . . ?
O6 C13 C12 117.8(6) . . ?
C15 C14 C12 120.7(7) . . ?
C15 C14 H14 119.7 . . ?
C12 C14 H14 119.7 . . ?
C14 C15 C9 119.6(7) . . ?
C14 C15 H15 120.2 . . ?
C9 C15 H15 120.2 . . ?
N2 N1 C7 114.2(6) . . ?
N1 N2 C9 114.6(6) . . ?
C1 O1 Cd1 85.9(4) . . ?
C1 O2 Cd1 97.2(4) . . ?
C5 O3 Cd1 84.5(4) . 3_545 ?
C5 O4 Cd1 100.2(4) . 3_545 ?
C13 O6 Cd2 106.3(4) . . ?
O12 C16 O12 111(4) . 2_656 ?
O12 C16 N3 124.5(18) . . ?
O12 C16 N3 124.5(18) 2_656 . ?
C16 N3 C17 123.4(6) . 2_656 ?
C16 N3 C17 123.4(6) . . ?
C17 N3 C17 113.3(13) 2_656 . ?
O13 C18 O13 135(7) . 2_656 ?
O13 C18 O13' 155(3) . 2_656 ?
O13 C18 O13' 40(3) 2_656 2_656 ?
O13 C18 O13' 40(3) . . ?
O13 C18 O13' 155(3) 2_656 . ?
O13' C18 O13' 160(4) 2_656 . ?

_diffrn_measured_fraction_theta_max 0.986
_diffrn_reflns_theta_full        62.67
_diffrn_measured_fraction_theta_full 0.986
_refine_diff_density_max         0.967
_refine_diff_density_min         -0.800
_refine_diff_density_rms         0.125

#start Validation Reply Form

_vrf_PLAT306_exp_13084           
;
PROBLEM: Isolated Oxygen Atom (H-atoms Missing ?) ....... O1W.
RESPONSE: The H atoms of the lattice water molecule were not added.
;
_vrf_PLAT430_exp_13084           
;
PROBLEM: Short Inter D...A Contact O12 .. O13' .. 2.23 Ang.
RESPONSE: The DMF and methanol molecules are disordered, and their
H atoms were not added.
;

# end Validation Reply Form


# end Validation Reply Form

# Attachment '- 3.cif'

data_1
_database_code_depnum_ccdc_archive 'CCDC 832312'
#TrackingRef '- 3.cif'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C60 H82 Mn6 N8 O51'
_chemical_formula_weight         2060.94

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   Cc

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

_cell_length_a                   30.3206(18)
_cell_length_b                   7.2470(3)
_cell_length_c                   19.3370(9)
_cell_angle_alpha                90.00
_cell_angle_beta                 106.844(2)
_cell_angle_gamma                90.00
_cell_volume                     4066.7(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    153(2)
_cell_measurement_reflns_used    1102
_cell_measurement_theta_min      3.02
_cell_measurement_theta_max      27.48

_exptl_crystal_description       block
_exptl_crystal_colour            orange
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.12
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.639
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2714
_exptl_absorpt_coefficient_mu    1.058
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.8324
_exptl_absorpt_correction_T_max  0.8835
_exptl_absorpt_process_details   Higashi,T.(1995).

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      153(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  'Rigaku RAXIS-RAPID Imaging Plate'
_diffrn_measurement_method       \W
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        0
_diffrn_reflns_number            11738
_diffrn_reflns_av_R_equivalents  0.0492
_diffrn_reflns_av_sigmaI/netI    0.0840
_diffrn_reflns_limit_h_min       -39
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_theta_min         3.02
_diffrn_reflns_theta_max         27.48
_reflns_number_total             7504
_reflns_number_gt                5877
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    '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^)+(0.1083P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.02(3)
_refine_ls_number_reflns         7504
_refine_ls_number_parameters     586
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0800
_refine_ls_R_factor_gt           0.0519
_refine_ls_wR_factor_ref         0.1813
_refine_ls_wR_factor_gt          0.1312
_refine_ls_goodness_of_fit_ref   1.076
_refine_ls_restrained_S_all      1.076
_refine_ls_shift/su_max          0.010
_refine_ls_shift/su_mean         0.001

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 0.82317(4) 0.66192(13) 0.91008(5) 0.0176(2) Uani 1 1 d . . .
Mn2 Mn 0.70797(4) 0.57859(14) 0.95095(5) 0.0186(2) Uani 1 1 d . . .
Mn3 Mn 0.71546(4) 1.11527(14) 0.76928(5) 0.0179(2) Uani 1 1 d . . .
C1 C 0.8040(3) 0.3641(9) 0.7839(4) 0.0217(15) Uani 1 1 d . . .
C2 C 0.8265(3) 0.2792(9) 0.7303(4) 0.0179(14) Uani 1 1 d . . .
C3 C 0.8734(2) 0.2390(9) 0.7507(4) 0.0185(14) Uani 1 1 d . . .
H3 H 0.8917 0.2602 0.7977 0.022 Uiso 1 1 calc R . .
C4 C 0.8926(3) 0.1651(10) 0.6980(4) 0.0243(16) Uani 1 1 d . . .
C5 C 0.8670(2) 0.1447(10) 0.6286(4) 0.0181(14) Uani 1 1 d . . .
H5 H 0.8807 0.1042 0.5942 0.022 Uiso 1 1 calc R . .
C6 C 0.8196(3) 0.1841(9) 0.6081(4) 0.0177(14) Uani 1 1 d . . .
C7 C 0.7918(3) 0.1634(9) 0.5308(4) 0.0192(14) Uani 1 1 d . . .
C8 C 0.7993(2) 0.2478(8) 0.6590(3) 0.0142(12) Uani 1 1 d . . .
H8 H 0.7678 0.2698 0.6460 0.017 Uiso 1 1 calc R . .
C9 C 1.0096(2) 0.0306(9) 0.7847(4) 0.0195(14) Uani 1 1 d . . .
C10 C 1.0363(3) 0.0008(12) 0.8539(4) 0.0297(17) Uani 1 1 d . . .
H10 H 1.0244 0.0200 0.8925 0.036 Uiso 1 1 calc R . .
C11 C 1.0814(3) -0.0584(11) 0.8660(5) 0.0302(17) Uani 1 1 d . . .
H11 H 1.0993 -0.0836 0.9129 0.036 Uiso 1 1 calc R . .
C12 C 1.1001(3) -0.0805(10) 0.8091(4) 0.0242(16) Uani 1 1 d . . .
C13 C 1.1494(3) -0.1475(9) 0.8242(4) 0.0227(15) Uani 1 1 d . . .
C14 C 1.0725(3) -0.0523(10) 0.7383(4) 0.0248(15) Uani 1 1 d . . .
H14 H 1.0847 -0.0726 0.6999 0.030 Uiso 1 1 calc R . .
C15 C 1.0270(3) 0.0059(11) 0.7244(4) 0.0257(16) Uani 1 1 d . . .
H15 H 1.0087 0.0279 0.6775 0.031 Uiso 1 1 calc R . .
C16 C 0.6513(2) 0.8508(9) 0.8315(4) 0.0212(15) Uani 1 1 d . . .
C17 C 0.6034(2) 0.9195(9) 0.7978(4) 0.0186(14) Uani 1 1 d . . .
C18 C 0.5865(3) 0.9497(10) 0.7226(4) 0.0229(15) Uani 1 1 d . . .
H18 H 0.6059 0.9328 0.6938 0.027 Uiso 1 1 calc R . .
C19 C 0.5418(3) 1.0035(10) 0.6916(4) 0.0260(16) Uani 1 1 d . . .
H19 H 0.5311 1.0215 0.6419 0.031 Uiso 1 1 calc R . .
C20 C 0.5121(3) 1.0314(9) 0.7342(4) 0.0195(14) Uani 1 1 d . . .
C21 C 0.5281(2) 1.0017(10) 0.8093(4) 0.0216(14) Uani 1 1 d . . .
H21 H 0.5085 1.0196 0.8379 0.026 Uiso 1 1 calc R . .
C22 C 0.5735(3) 0.9451(11) 0.8407(4) 0.0255(16) Uani 1 1 d . . .
H22 H 0.5841 0.9242 0.8902 0.031 Uiso 1 1 calc R . .
C23 C 0.3958(3) 1.1644(9) 0.7053(4) 0.0197(14) Uani 1 1 d . . .
C24 C 0.3724(2) 1.1235(9) 0.6320(4) 0.0169(13) Uani 1 1 d . . .
H24 H 0.3883 1.0705 0.6026 0.020 Uiso 1 1 calc R . .
C25 C 0.3248(2) 1.1635(9) 0.6038(4) 0.0172(14) Uani 1 1 d . . .
C26 C 0.3000(3) 1.0995(9) 0.5306(4) 0.0215(15) Uani 1 1 d . . .
C27 C 0.3016(2) 1.2447(10) 0.6478(4) 0.0186(14) Uani 1 1 d . . .
H27 H 0.2705 1.2723 0.6291 0.022 Uiso 1 1 calc R . .
C28 C 0.3242(2) 1.2854(9) 0.7196(4) 0.0168(13) Uani 1 1 d . . .
C29 C 0.2986(3) 1.3704(8) 0.7678(3) 0.0162(14) Uani 1 1 d . . .
C30 C 0.3709(2) 1.2433(9) 0.7487(3) 0.0164(13) Uani 1 1 d . . .
H30 H 0.3856 1.2677 0.7972 0.020 Uiso 1 1 calc R . .
N1 N 0.9403(2) 0.1202(8) 0.7114(3) 0.0211(12) Uani 1 1 d . . .
N2 N 0.9619(2) 0.0835(8) 0.7749(3) 0.0220(13) Uani 1 1 d . . .
N3 N 0.4661(2) 1.0863(8) 0.6983(4) 0.0251(13) Uani 1 1 d . . .
N4 N 0.4422(2) 1.1222(8) 0.7389(3) 0.0210(12) Uani 1 1 d . . .
O1 O 0.83087(18) 0.4336(7) 0.8408(3) 0.0206(10) Uani 1 1 d . . .
O2 O 0.76083(18) 0.3628(6) 0.7680(3) 0.0197(10) Uani 1 1 d . . .
O3 O 0.74939(18) 0.2037(7) 0.5138(3) 0.0218(10) Uani 1 1 d . . .
O4 O 0.81157(18) 0.1127(6) 0.4836(2) 0.0176(10) Uani 1 1 d . . .
O5 O 1.16234(19) -0.1921(8) 0.7692(3) 0.0300(12) Uani 1 1 d . . .
O6 O 1.17380(18) -0.1540(7) 0.8873(2) 0.0214(11) Uani 1 1 d . . .
O7 O 0.65936(18) 0.7772(7) 0.8928(3) 0.0241(11) Uani 1 1 d . . .
O8 O 0.68054(17) 0.8618(7) 0.7960(3) 0.0213(11) Uani 1 1 d . . .
O9 O 0.32291(19) 1.0217(7) 0.4936(3) 0.0253(11) Uani 1 1 d . . .
O10 O 0.25682(19) 1.1229(7) 0.5086(3) 0.0235(11) Uani 1 1 d . . .
O11 O 0.25803(19) 1.4246(7) 0.7369(3) 0.0255(11) Uani 1 1 d . . .
O12 O 0.31799(19) 1.3780(6) 0.8351(3) 0.0201(11) Uani 1 1 d . . .
O13 O 0.74517(18) 0.6193(6) 0.8626(3) 0.0189(10) Uani 1 1 d . . .
O14 O 0.8974(2) 0.6845(8) 0.9531(3) 0.0319(13) Uani 1 1 d . . .
O15 O 0.66862(19) 0.5508(8) 1.0276(3) 0.0282(12) Uani 1 1 d . . .
O16 O 0.7510(2) 1.1234(7) 0.8840(3) 0.0258(12) Uani 1 1 d . . .
O17 O 0.6780(2) 1.1102(8) 0.6533(3) 0.0297(13) Uani 1 1 d . . .
O1W O 0.8765(2) 0.8428(8) 0.4579(3) 0.0333(13) Uani 1 1 d . . .
O2W O 0.9418(2) 0.9806(9) 0.9125(3) 0.0371(14) Uani 1 1 d . . .
O3W O 0.9482(3) 0.3901(11) 0.0378(4) 0.0517(18) Uani 1 1 d . . .
O4W O 0.6836(3) 0.9185(9) 0.5288(4) 0.063(3) Uani 1 1 d . . .
O5W O 0.6744(4) 0.3918(11) 0.1627(4) 0.084(4) Uani 1 1 d . . .
O6W O 0.5965(3) 0.7449(16) 0.0537(4) 0.075(3) Uani 1 1 d . . .
O8W O 0.5339(7) 0.980(3) 0.9937(9) 0.071(5) Uani 0.50 1 d P . .
O7W O 0.5260(5) 0.438(2) 0.0378(7) 0.066(4) Uani 0.60 1 d P . .
O7W' O 0.5142(6) 0.622(3) 0.0282(11) 0.062(6) Uani 0.40 1 d P . .
O9W O 0.5972(8) 0.177(3) 0.0402(15) 0.120(9) Uani 0.60 1 d P . .
O9W' O 0.5764(10) 0.301(4) 0.0595(15) 0.095(9) Uani 0.40 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
Mn1 0.0147(5) 0.0209(5) 0.0181(5) 0.0002(4) 0.0065(4) 0.0003(4)
Mn2 0.0114(5) 0.0241(5) 0.0203(5) 0.0016(5) 0.0048(4) 0.0006(4)
Mn3 0.0121(5) 0.0216(5) 0.0211(5) -0.0001(4) 0.0068(4) 0.0030(4)
C1 0.021(4) 0.018(3) 0.033(4) 0.015(3) 0.018(3) 0.008(3)
C2 0.016(3) 0.018(3) 0.020(3) -0.001(3) 0.007(3) -0.007(3)
C3 0.018(4) 0.018(3) 0.023(3) 0.001(3) 0.010(3) -0.002(3)
C4 0.020(4) 0.022(3) 0.037(4) 0.006(3) 0.017(3) 0.006(3)
C5 0.014(3) 0.027(3) 0.015(3) -0.001(3) 0.008(3) 0.003(3)
C6 0.017(4) 0.022(3) 0.015(3) -0.002(3) 0.006(3) -0.004(3)
C7 0.018(4) 0.017(3) 0.023(3) 0.000(3) 0.007(3) 0.001(3)
C8 0.009(3) 0.015(3) 0.017(3) -0.002(3) 0.002(2) -0.005(2)
C9 0.013(3) 0.018(3) 0.028(3) -0.002(3) 0.006(3) -0.001(3)
C10 0.018(4) 0.044(4) 0.029(4) 0.007(4) 0.010(3) 0.007(3)
C11 0.015(4) 0.037(4) 0.039(4) 0.002(4) 0.009(3) 0.006(3)
C12 0.013(4) 0.024(3) 0.037(4) -0.008(3) 0.010(3) -0.004(3)
C13 0.014(4) 0.015(3) 0.040(4) -0.004(3) 0.010(3) 0.001(3)
C14 0.018(4) 0.032(4) 0.027(4) 0.002(3) 0.010(3) 0.005(3)
C15 0.021(4) 0.034(4) 0.022(3) -0.007(3) 0.005(3) -0.004(3)
C16 0.008(3) 0.021(3) 0.033(4) -0.010(3) 0.005(3) -0.005(3)
C17 0.011(3) 0.017(3) 0.027(3) 0.007(3) 0.003(3) 0.006(3)
C18 0.018(4) 0.030(4) 0.022(3) 0.009(3) 0.008(3) 0.010(3)
C19 0.025(4) 0.032(4) 0.019(3) 0.002(3) 0.004(3) 0.007(3)
C20 0.020(4) 0.021(3) 0.019(3) 0.000(3) 0.008(3) 0.000(3)
C21 0.011(3) 0.033(4) 0.022(3) -0.002(3) 0.006(3) -0.001(3)
C22 0.019(4) 0.030(4) 0.027(4) 0.001(3) 0.005(3) 0.001(3)
C23 0.018(4) 0.015(3) 0.025(3) -0.005(3) 0.005(3) -0.002(3)
C24 0.012(3) 0.016(3) 0.023(3) 0.000(3) 0.005(3) 0.004(2)
C25 0.014(4) 0.021(3) 0.016(3) 0.002(3) 0.005(3) 0.002(3)
C26 0.023(4) 0.014(3) 0.030(4) 0.003(3) 0.011(3) -0.002(3)
C27 0.007(3) 0.026(3) 0.023(3) -0.002(3) 0.005(3) -0.002(3)
C28 0.015(3) 0.019(3) 0.017(3) 0.004(3) 0.006(3) 0.009(3)
C29 0.024(4) 0.014(3) 0.013(3) 0.000(3) 0.008(3) -0.004(3)
C30 0.021(4) 0.020(3) 0.008(3) 0.005(3) 0.004(3) 0.000(3)
N1 0.014(3) 0.029(3) 0.018(3) 0.001(3) 0.001(2) 0.001(2)
N2 0.011(3) 0.022(3) 0.032(3) -0.003(3) 0.005(3) 0.002(2)
N3 0.011(3) 0.030(3) 0.034(3) 0.002(3) 0.006(3) 0.004(3)
N4 0.010(3) 0.030(3) 0.024(3) 0.001(3) 0.005(2) 0.007(2)
O1 0.019(3) 0.026(2) 0.014(2) -0.008(2) -0.0010(19) -0.001(2)
O2 0.016(3) 0.023(2) 0.024(3) -0.001(2) 0.012(2) 0.0001(19)
O3 0.014(3) 0.035(3) 0.016(2) -0.003(2) 0.003(2) -0.002(2)
O4 0.022(3) 0.019(2) 0.012(2) -0.0048(19) 0.0052(19) 0.0006(19)
O5 0.018(3) 0.039(3) 0.037(3) -0.004(3) 0.015(2) 0.007(2)
O6 0.020(3) 0.029(2) 0.012(2) -0.001(2) -0.002(2) 0.002(2)
O7 0.020(3) 0.031(3) 0.021(2) 0.011(2) 0.006(2) 0.005(2)
O8 0.009(2) 0.030(3) 0.025(3) 0.006(2) 0.007(2) 0.0006(19)
O9 0.022(3) 0.027(3) 0.028(3) -0.006(2) 0.009(2) -0.002(2)
O10 0.020(3) 0.031(3) 0.016(2) 0.003(2) 0.000(2) 0.000(2)
O11 0.015(3) 0.030(3) 0.034(3) -0.004(2) 0.010(2) 0.004(2)
O12 0.024(3) 0.021(2) 0.016(2) 0.001(2) 0.009(2) 0.001(2)
O13 0.016(3) 0.019(2) 0.020(2) -0.003(2) 0.003(2) -0.0036(19)
O14 0.015(3) 0.040(3) 0.038(3) 0.000(3) 0.004(2) -0.002(2)
O15 0.021(3) 0.043(3) 0.023(3) 0.003(3) 0.010(2) 0.002(2)
O16 0.028(3) 0.028(3) 0.021(2) -0.001(2) 0.006(2) 0.007(2)
O17 0.031(3) 0.041(3) 0.017(2) -0.003(2) 0.005(2) 0.003(3)
O1W 0.029(3) 0.035(3) 0.037(3) 0.011(3) 0.010(3) -0.001(2)
O2W 0.027(3) 0.042(3) 0.045(4) 0.002(3) 0.016(3) -0.002(3)
O3W 0.035(4) 0.069(5) 0.049(4) -0.007(4) 0.009(3) 0.006(3)
O4W 0.107(8) 0.041(4) 0.060(5) -0.012(4) 0.052(5) -0.018(4)
O5W 0.170(11) 0.045(4) 0.026(4) -0.007(3) 0.010(5) -0.001(5)
O6W 0.025(4) 0.150(9) 0.042(4) -0.042(5) 0.000(3) 0.015(5)
O8W 0.057(11) 0.106(13) 0.054(9) -0.004(10) 0.023(8) 0.007(10)
O7W 0.039(8) 0.113(12) 0.039(6) -0.002(7) 0.000(6) -0.012(8)
O7W' 0.029(10) 0.083(14) 0.057(11) -0.046(11) -0.014(8) 0.007(9)
O9W 0.077(15) 0.110(15) 0.19(2) 0.078(16) 0.066(16) 0.035(12)
O9W' 0.070(18) 0.090(17) 0.088(17) 0.030(15) -0.036(14) -0.023(15)

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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Mn1 O9 2.094(5) 4_565 ?
Mn1 O12 2.109(5) 3_545 ?
Mn1 O14 2.168(6) . ?
Mn1 O1 2.183(5) . ?
Mn1 O4 2.259(5) 2_565 ?
Mn1 O13 2.297(5) . ?
Mn2 O7 2.133(5) . ?
Mn2 O10 2.148(5) 4_565 ?
Mn2 O3 2.158(5) 2_565 ?
Mn2 O15 2.165(5) . ?
Mn2 O6 2.166(5) 3_455 ?
Mn2 O13 2.323(5) . ?
Mn3 O11 2.106(5) 3_545 ?
Mn3 O5 2.131(5) 3_465 ?
Mn3 O16 2.168(5) . ?
Mn3 O17 2.201(5) . ?
Mn3 O8 2.254(5) . ?
Mn3 O2 2.265(5) 1_565 ?
C1 O2 1.256(9) . ?
C1 O1 1.268(10) . ?
C1 C2 1.526(9) . ?
C2 C3 1.394(10) . ?
C2 C8 1.405(10) . ?
C3 C4 1.415(9) . ?
C3 H3 0.9300 . ?
C4 C5 1.350(11) . ?
C4 N1 1.430(10) . ?
C5 C6 1.403(10) . ?
C5 H5 0.9300 . ?
C6 C8 1.382(9) . ?
C6 C7 1.496(10) . ?
C7 O3 1.265(9) . ?
C7 O4 1.282(8) . ?
C8 H8 0.9300 . ?
C9 C10 1.365(11) . ?
C9 C15 1.424(10) . ?
C9 N2 1.456(9) . ?
C10 C11 1.387(11) . ?
C10 H10 0.9300 . ?
C11 C12 1.387(11) . ?
C11 H11 0.9300 . ?
C12 C14 1.397(11) . ?
C12 C13 1.515(10) . ?
C13 O6 1.231(10) . ?
C13 O5 1.279(9) . ?
C14 C15 1.392(11) . ?
C14 H14 0.9300 . ?
C15 H15 0.9300 . ?
C16 O7 1.258(9) . ?
C16 O8 1.271(9) . ?
C16 C17 1.494(10) . ?
C17 C22 1.406(10) . ?
C17 C18 1.412(10) . ?
C18 C19 1.371(11) . ?
C18 H18 0.9300 . ?
C19 C20 1.398(10) . ?
C19 H19 0.9300 . ?
C20 C21 1.408(10) . ?
C20 N3 1.425(10) . ?
C21 C22 1.395(10) . ?
C21 H21 0.9300 . ?
C22 H22 0.9300 . ?
C23 C30 1.402(9) . ?
C23 N4 1.402(10) . ?
C23 C24 1.420(10) . ?
C24 C25 1.416(10) . ?
C24 H24 0.9300 . ?
C25 C27 1.382(9) . ?
C25 C26 1.473(10) . ?
C26 O9 1.265(9) . ?
C26 O10 1.265(9) . ?
C27 C28 1.390(10) . ?
C27 H27 0.9300 . ?
C28 C30 1.398(10) . ?
C28 C29 1.506(9) . ?
C29 O12 1.265(8) . ?
C29 O11 1.265(9) . ?
C30 H30 0.9300 . ?
N1 N2 1.241(9) . ?
N3 N4 1.241(9) . ?
O2 Mn3 2.265(5) 1_545 ?
O3 Mn2 2.158(5) 2_564 ?
O4 Mn1 2.259(5) 2_564 ?
O5 Mn3 2.131(5) 3_535 ?
O6 Mn2 2.166(5) 3_545 ?
O9 Mn1 2.094(5) 4_464 ?
O10 Mn2 2.148(5) 4_464 ?
O11 Mn3 2.106(5) 3_455 ?
O12 Mn1 2.109(5) 3_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
O9 Mn1 O12 170.3(2) 4_565 3_545 ?
O9 Mn1 O14 89.3(2) 4_565 . ?
O12 Mn1 O14 94.0(2) 3_545 . ?
O9 Mn1 O1 91.0(2) 4_565 . ?
O12 Mn1 O1 98.11(19) 3_545 . ?
O14 Mn1 O1 90.5(2) . . ?
O9 Mn1 O4 86.44(18) 4_565 2_565 ?
O12 Mn1 O4 84.34(16) 3_545 2_565 ?
O14 Mn1 O4 92.1(2) . 2_565 ?
O1 Mn1 O4 176.25(19) . 2_565 ?
O9 Mn1 O13 89.4(2) 4_565 . ?
O12 Mn1 O13 87.82(19) 3_545 . ?
O14 Mn1 O13 176.4(2) . . ?
O1 Mn1 O13 86.18(18) . . ?
O4 Mn1 O13 91.09(18) 2_565 . ?
O7 Mn2 O10 179.5(2) . 4_565 ?
O7 Mn2 O3 90.2(2) . 2_565 ?
O10 Mn2 O3 90.2(2) 4_565 2_565 ?
O7 Mn2 O15 89.4(2) . . ?
O10 Mn2 O15 90.9(2) 4_565 . ?
O3 Mn2 O15 91.7(2) 2_565 . ?
O7 Mn2 O6 94.7(2) . 3_455 ?
O10 Mn2 O6 84.84(19) 4_565 3_455 ?
O3 Mn2 O6 173.4(2) 2_565 3_455 ?
O15 Mn2 O6 92.8(2) . 3_455 ?
O7 Mn2 O13 86.28(18) . . ?
O10 Mn2 O13 93.40(19) 4_565 . ?
O3 Mn2 O13 89.65(18) 2_565 . ?
O15 Mn2 O13 175.5(2) . . ?
O6 Mn2 O13 86.25(18) 3_455 . ?
O11 Mn3 O5 163.3(2) 3_545 3_465 ?
O11 Mn3 O16 99.0(2) 3_545 . ?
O5 Mn3 O16 97.8(2) 3_465 . ?
O11 Mn3 O17 82.3(2) 3_545 . ?
O5 Mn3 O17 81.0(2) 3_465 . ?
O16 Mn3 O17 178.7(2) . . ?
O11 Mn3 O8 84.4(2) 3_545 . ?
O5 Mn3 O8 97.4(2) 3_465 . ?
O16 Mn3 O8 85.1(2) . . ?
O17 Mn3 O8 94.7(2) . . ?
O11 Mn3 O2 95.16(19) 3_545 1_565 ?
O5 Mn3 O2 86.7(2) 3_465 1_565 ?
O16 Mn3 O2 82.3(2) . 1_565 ?
O17 Mn3 O2 97.9(2) . 1_565 ?
O8 Mn3 O2 167.18(19) . 1_565 ?
O2 C1 O1 125.2(6) . . ?
O2 C1 C2 118.0(7) . . ?
O1 C1 C2 116.7(6) . . ?
C3 C2 C8 120.3(6) . . ?
C3 C2 C1 120.8(6) . . ?
C8 C2 C1 118.9(7) . . ?
C2 C3 C4 118.3(6) . . ?
C2 C3 H3 120.8 . . ?
C4 C3 H3 120.8 . . ?
C5 C4 C3 121.2(7) . . ?
C5 C4 N1 114.6(6) . . ?
C3 C4 N1 124.1(7) . . ?
C4 C5 C6 120.4(6) . . ?
C4 C5 H5 119.8 . . ?
C6 C5 H5 119.8 . . ?
C8 C6 C5 119.8(6) . . ?
C8 C6 C7 120.4(6) . . ?
C5 C6 C7 119.8(6) . . ?
O3 C7 O4 122.0(7) . . ?
O3 C7 C6 118.3(6) . . ?
O4 C7 C6 119.7(6) . . ?
C6 C8 C2 119.8(6) . . ?
C6 C8 H8 120.1 . . ?
C2 C8 H8 120.1 . . ?
C10 C9 C15 121.8(7) . . ?
C10 C9 N2 117.0(7) . . ?
C15 C9 N2 121.1(7) . . ?
C9 C10 C11 119.4(7) . . ?
C9 C10 H10 120.3 . . ?
C11 C10 H10 120.3 . . ?
C12 C11 C10 120.8(8) . . ?
C12 C11 H11 119.6 . . ?
C10 C11 H11 119.6 . . ?
C11 C12 C14 119.6(7) . . ?
C11 C12 C13 119.3(7) . . ?
C14 C12 C13 120.9(7) . . ?
O6 C13 O5 125.0(7) . . ?
O6 C13 C12 118.7(7) . . ?
O5 C13 C12 116.3(7) . . ?
C15 C14 C12 120.8(7) . . ?
C15 C14 H14 119.6 . . ?
C12 C14 H14 119.6 . . ?
C14 C15 C9 117.5(7) . . ?
C14 C15 H15 121.2 . . ?
C9 C15 H15 121.2 . . ?
O7 C16 O8 124.0(7) . . ?
O7 C16 C17 116.8(6) . . ?
O8 C16 C17 119.1(7) . . ?
C22 C17 C18 118.9(7) . . ?
C22 C17 C16 119.9(7) . . ?
C18 C17 C16 121.1(6) . . ?
C19 C18 C17 120.9(7) . . ?
C19 C18 H18 119.6 . . ?
C17 C18 H18 119.6 . . ?
C18 C19 C20 120.4(7) . . ?
C18 C19 H19 119.8 . . ?
C20 C19 H19 119.8 . . ?
C19 C20 C21 119.8(7) . . ?
C19 C20 N3 117.3(6) . . ?
C21 C20 N3 122.8(6) . . ?
C22 C21 C20 119.7(6) . . ?
C22 C21 H21 120.2 . . ?
C20 C21 H21 120.2 . . ?
C21 C22 C17 120.3(7) . . ?
C21 C22 H22 119.8 . . ?
C17 C22 H22 119.8 . . ?
C30 C23 N4 116.9(6) . . ?
C30 C23 C24 118.9(6) . . ?
N4 C23 C24 124.2(6) . . ?
C25 C24 C23 120.0(6) . . ?
C25 C24 H24 120.0 . . ?
C23 C24 H24 120.0 . . ?
C27 C25 C24 119.6(6) . . ?
C27 C25 C26 121.0(7) . . ?
C24 C25 C26 119.0(6) . . ?
O9 C26 O10 123.6(7) . . ?
O9 C26 C25 118.2(7) . . ?
O10 C26 C25 118.2(6) . . ?
C25 C27 C28 120.8(6) . . ?
C25 C27 H27 119.6 . . ?
C28 C27 H27 119.6 . . ?
C27 C28 C30 120.4(6) . . ?
C27 C28 C29 120.7(6) . . ?
C30 C28 C29 118.9(6) . . ?
O12 C29 O11 124.7(6) . . ?
O12 C29 C28 119.1(6) . . ?
O11 C29 C28 116.2(6) . . ?
C28 C30 C23 120.3(6) . . ?
C28 C30 H30 119.8 . . ?
C23 C30 H30 119.8 . . ?
N2 N1 C4 116.3(6) . . ?
N1 N2 C9 113.9(6) . . ?
N4 N3 C20 114.8(6) . . ?
N3 N4 C23 116.3(6) . . ?
C1 O1 Mn1 132.7(5) . . ?
C1 O2 Mn3 126.7(4) . 1_545 ?
C7 O3 Mn2 134.2(5) . 2_564 ?
C7 O4 Mn1 115.5(4) . 2_564 ?
C13 O5 Mn3 125.4(5) . 3_535 ?
C13 O6 Mn2 125.8(5) . 3_545 ?
C16 O7 Mn2 134.4(5) . . ?
C16 O8 Mn3 128.5(5) . . ?
C26 O9 Mn1 147.6(5) . 4_464 ?
C26 O10 Mn2 125.0(4) . 4_464 ?
C29 O11 Mn3 131.3(5) . 3_455 ?
C29 O12 Mn1 126.5(4) . 3_455 ?
Mn1 O13 Mn2 112.7(2) . . ?

_diffrn_measured_fraction_theta_max 0.981
_diffrn_reflns_theta_full        27.48
_diffrn_measured_fraction_theta_full 0.981
_refine_diff_density_max         0.798
_refine_diff_density_min         -0.720
_refine_diff_density_rms         0.120

#start Validation Reply Form

_vrf_PLAT306_1                   
;
PROBLEM: Isolated Oxygen Atom (H-atoms Missing ?) ....... O1W.
RESPONSE: The H atoms of the lattice water molecules were not added.
;
_vrf_PLAT430_1                   
;
PROBLEM: Short Inter D...A Contact O1W .. O2W .. 2.71 Ang.
RESPONSE: The H atoms of the lattice water molecules were not added.
;

# end Validation Reply Form