# Electronic Supplementary Material (ESI) for Dalton Transactions
# This journal is © The Royal Society of Chemistry 2013


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#  This CIF contains data from an original supplementary publication 
#  deposited with the CCDC, and may include chemical, crystal,   
#  experimental, refinement, atomic coordinates, 
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted. 
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data_njy1
_database_code_depnum_ccdc_archive 'CCDC 909647'
#TrackingRef '909647.cif'
_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            
'C6 H46 Mn2 Mo8 N4 O48'
_chemical_formula_weight         1819.82
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'
Mo Mo -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_symmetry_cell_setting           Triclinic
_symmetry_space_group_name_H-M   P-1
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
_cell_length_a                   9.348(5)
_cell_length_b                   11.652(6)
_cell_length_c                   13.167(7)
_cell_angle_alpha                110.481(7)
_cell_angle_beta                 94.255(8)
_cell_angle_gamma                112.600(6)
_cell_volume                     1203.7(11)
_cell_formula_units_Z            1
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    5135
_cell_measurement_theta_min      2.41
_cell_measurement_theta_max      28.36
_exptl_crystal_description       rod
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.12
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.502
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             874
_exptl_absorpt_coefficient_mu    2.640
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.6625
_exptl_absorpt_correction_T_max  0.7424
_exptl_absorpt_process_details   SADABS
_exptl_special_details           
;
?
;
_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            6066
_diffrn_reflns_av_R_equivalents  0.0190
_diffrn_reflns_av_unetI/netI     0.0337
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         2.43
_diffrn_reflns_theta_max         25.00
_reflns_number_total             4185
_reflns_number_gt                3863
_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^)+(0.0447P)^2^+1.4024P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   notdet
_refine_ls_hydrogen_treatment    noref
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         4185
_refine_ls_number_parameters     307
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0294
_refine_ls_R_factor_gt           0.0270
_refine_ls_wR_factor_ref         0.0751
_refine_ls_wR_factor_gt          0.0736
_refine_ls_goodness_of_fit_ref   1.009
_refine_ls_restrained_S_all      1.009
_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
Mo1 Mo 0.19848(4) 0.59785(3) 0.15798(2) 0.01724(10) Uani 1 1 d . . .
Mo2 Mo 0.11920(4) 0.24435(3) 0.04445(3) 0.01924(10) Uani 1 1 d . . .
Mo3 Mo -0.10366(4) 0.34061(3) 0.21486(3) 0.02007(10) Uani 1 1 d . . .
Mo4 Mo -0.21850(4) 0.58416(3) 0.15014(3) 0.01983(10) Uani 1 1 d . . .
Mn1 Mn 0.28230(7) 0.44815(6) 0.30873(5) 0.02169(14) Uani 1 1 d . . .
O1 O 0.3638(3) 0.7410(3) 0.2421(2) 0.0282(6) Uani 1 1 d . . .
O2 O 0.2247(3) 0.5707(3) 0.0197(2) 0.0229(6) Uani 1 1 d . . .
O3 O 0.2987(3) 0.4619(3) 0.1597(2) 0.0201(5) Uani 1 1 d . . .
O4 O 0.0445(3) 0.6517(3) 0.1634(2) 0.0235(6) Uani 1 1 d . . .
O5 O 0.0011(3) 0.3812(3) 0.0787(2) 0.0197(5) Uani 1 1 d . . .
O6 O 0.1348(3) 0.5340(3) 0.2880(2) 0.0203(5) Uani 1 1 d . . .
O7 O 0.1818(3) 0.3056(3) -0.0661(2) 0.0242(6) Uani 1 1 d . . .
O8 O -0.0531(3) 0.1028(3) -0.0290(2) 0.0317(7) Uani 1 1 d . . .
O9 O 0.2589(3) 0.1881(3) 0.0660(2) 0.0294(6) Uani 1 1 d . . .
O10 O 0.0741(3) 0.2813(3) 0.1982(2) 0.0213(5) Uani 1 1 d . . .
O11 O -0.2568(3) 0.1851(3) 0.1314(3) 0.0326(7) Uani 1 1 d . . .
O12 O -0.1050(4) 0.3556(3) 0.3484(2) 0.0336(7) Uani 1 1 d . . .
O13 O -0.1880(3) 0.4577(3) 0.2011(2) 0.0239(6) Uani 1 1 d . . .
O14 O -0.1846(4) 0.7124(3) 0.2772(2) 0.0371(7) Uani 1 1 d . . .
O15 O -0.4218(3) 0.5024(3) 0.1088(3) 0.0338(7) Uani 1 1 d . . .
O16 O 0.2140(4) 0.4228(4) 0.5169(3) 0.0478(9) Uani 1 1 d . . .
O17 O 0.4768(5) 0.2995(4) 0.3067(3) 0.0540(10) Uani 1 1 d . . .
O18 O 0.5626(4) 0.7078(4) 0.4445(3) 0.0561(10) Uani 1 1 d . . .
C1 C 0.2373(5) 0.4317(4) 0.4356(3) 0.0291(9) Uani 1 1 d . . .
C2 C 0.4008(5) 0.3568(4) 0.3054(3) 0.0312(9) Uani 1 1 d . . .
C3 C 0.4545(5) 0.6058(5) 0.3915(4) 0.0314(10) Uani 1 1 d . . .
O1W O 0.1716(5) 0.7302(3) 0.4835(3) 0.0472(9) Uani 1 1 d . . .
O2W O 0.4914(4) 0.1917(3) -0.0526(3) 0.0448(8) Uani 1 1 d . . .
O3W O 0.0243(5) 0.0824(4) 0.2803(3) 0.0539(9) Uani 1 1 d . . .
O4W O -0.3936(5) -0.0174(4) -0.1120(4) 0.0624(11) Uani 1 1 d . . .
O5W O -0.2939(5) 0.9139(4) 0.2687(4) 0.0647(11) Uani 1 1 d . . .
O6W O 0.2291(5) 0.9558(4) 0.2771(3) 0.0602(10) Uani 1 1 d . . .
N1 N -0.0192(6) 0.8729(4) 0.4983(3) 0.0521(12) Uani 1 1 d . . .
N2 N 0.5329(6) 1.0384(5) 0.4112(4) 0.0635(14) Uani 1 1 d . . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Mo1 0.01358(17) 0.02064(18) 0.01796(17) 0.00968(13) 0.00125(12) 0.00684(14)
Mo2 0.01729(18) 0.02123(18) 0.02126(18) 0.01069(14) 0.00309(13) 0.00900(14)
Mo3 0.01587(18) 0.02671(19) 0.02233(18) 0.01532(15) 0.00491(13) 0.00921(14)
Mo4 0.01738(18) 0.02808(19) 0.02011(18) 0.01267(14) 0.00613(13) 0.01317(14)
Mn1 0.0183(3) 0.0286(3) 0.0206(3) 0.0125(2) 0.0001(2) 0.0113(3)
O1 0.0235(15) 0.0276(15) 0.0252(14) 0.0089(12) 0.0002(12) 0.0060(12)
O2 0.0228(14) 0.0270(14) 0.0229(13) 0.0139(12) 0.0062(11) 0.0115(12)
O3 0.0171(13) 0.0252(14) 0.0193(13) 0.0111(11) 0.0022(10) 0.0092(11)
O4 0.0180(13) 0.0277(14) 0.0294(15) 0.0159(12) 0.0051(11) 0.0110(12)
O5 0.0157(13) 0.0246(14) 0.0216(13) 0.0119(11) 0.0041(10) 0.0095(11)
O6 0.0179(13) 0.0268(14) 0.0202(13) 0.0121(11) 0.0027(10) 0.0119(11)
O7 0.0253(15) 0.0281(14) 0.0243(14) 0.0134(12) 0.0075(11) 0.0141(12)
O8 0.0266(16) 0.0281(15) 0.0348(16) 0.0113(13) 0.0044(13) 0.0084(13)
O9 0.0271(15) 0.0362(16) 0.0360(16) 0.0201(13) 0.0083(12) 0.0201(13)
O10 0.0186(13) 0.0265(14) 0.0228(13) 0.0147(11) 0.0043(10) 0.0100(11)
O11 0.0212(15) 0.0308(16) 0.0431(18) 0.0164(14) 0.0061(13) 0.0078(13)
O12 0.0350(17) 0.0521(19) 0.0303(16) 0.0281(15) 0.0130(13) 0.0245(15)
O13 0.0194(14) 0.0327(15) 0.0292(14) 0.0189(12) 0.0099(11) 0.0146(12)
O14 0.054(2) 0.0399(18) 0.0238(15) 0.0131(13) 0.0126(14) 0.0267(16)
O15 0.0187(15) 0.0513(19) 0.0428(18) 0.0289(15) 0.0094(13) 0.0176(14)
O16 0.054(2) 0.068(2) 0.0314(18) 0.0305(18) 0.0112(16) 0.0267(19)
O17 0.056(2) 0.062(2) 0.052(2) 0.0156(19) -0.0020(18) 0.044(2)
O18 0.037(2) 0.043(2) 0.059(2) 0.0106(18) -0.0148(18) 0.0032(18)
C1 0.025(2) 0.034(2) 0.029(2) 0.0151(18) 0.0005(17) 0.0132(18)
C2 0.028(2) 0.038(2) 0.028(2) 0.0134(19) -0.0008(17) 0.017(2)
C3 0.026(2) 0.039(3) 0.034(2) 0.018(2) 0.0018(19) 0.016(2)
O1W 0.063(2) 0.045(2) 0.0314(17) 0.0169(15) 0.0173(16) 0.0199(18)
O2W 0.0399(19) 0.044(2) 0.054(2) 0.0224(17) 0.0196(16) 0.0182(16)
O3W 0.053(2) 0.054(2) 0.072(3) 0.039(2) 0.0212(19) 0.0274(19)
O4W 0.049(2) 0.062(2) 0.070(3) 0.023(2) 0.008(2) 0.021(2)
O5W 0.049(2) 0.055(2) 0.081(3) 0.023(2) 0.010(2) 0.020(2)
O6W 0.068(3) 0.051(2) 0.066(3) 0.023(2) 0.011(2) 0.031(2)
N1 0.069(3) 0.042(2) 0.029(2) 0.0104(19) -0.010(2) 0.016(2)
N2 0.047(3) 0.044(3) 0.069(3) -0.002(2) 0.003(2) 0.014(2)
_geom_special_details            
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Mo1 O1 1.694(3) . ?
Mo1 O4 1.775(3) . ?
Mo1 O2 1.789(3) . ?
Mo1 O6 2.131(3) . ?
Mo1 O3 2.133(3) . ?
Mo1 O5 2.271(3) . ?
Mo2 O8 1.691(3) . ?
Mo2 O9 1.718(3) . ?
Mo2 O7 1.872(3) . ?
Mo2 O10 2.029(3) . ?
Mo2 O5 2.212(3) . ?
Mo2 O3 2.281(3) . ?
Mo3 O12 1.706(3) . ?
Mo3 O11 1.709(3) . ?
Mo3 O13 1.869(3) . ?
Mo3 O10 2.030(3) . ?
Mo3 O5 2.212(3) . ?
Mo3 O6 2.297(3) . ?
Mo4 O15 1.705(3) . ?
Mo4 O14 1.714(3) . ?
Mo4 O13 1.921(3) . ?
Mo4 O7 1.925(3) 2_565 ?
Mo4 O4 2.246(3) . ?
Mo4 O2 2.310(3) 2_565 ?
Mn1 C3 1.794(5) . ?
Mn1 C2 1.802(4) . ?
Mn1 C1 1.809(4) . ?
Mn1 O3 2.036(3) . ?
Mn1 O6 2.042(3) . ?
Mn1 O10 2.092(3) . ?
O2 Mo4 2.310(3) 2_565 ?
O7 Mo4 1.925(3) 2_565 ?
O16 C1 1.140(5) . ?
O17 C2 1.149(5) . ?
O18 C3 1.146(5) . ?
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 Mo1 O4 103.93(14) . . ?
O1 Mo1 O2 104.57(13) . . ?
O4 Mo1 O2 102.80(12) . . ?
O1 Mo1 O6 94.74(12) . . ?
O4 Mo1 O6 88.90(11) . . ?
O2 Mo1 O6 154.03(11) . . ?
O1 Mo1 O3 94.90(13) . . ?
O4 Mo1 O3 154.30(11) . . ?
O2 Mo1 O3 88.92(11) . . ?
O6 Mo1 O3 72.04(10) . . ?
O1 Mo1 O5 162.94(11) . . ?
O4 Mo1 O5 86.61(11) . . ?
O2 Mo1 O5 85.68(11) . . ?
O6 Mo1 O5 71.77(10) . . ?
O3 Mo1 O5 71.35(10) . . ?
O8 Mo2 O9 106.11(15) . . ?
O8 Mo2 O7 101.47(14) . . ?
O9 Mo2 O7 100.82(13) . . ?
O8 Mo2 O10 97.78(13) . . ?
O9 Mo2 O10 95.71(12) . . ?
O7 Mo2 O10 149.93(11) . . ?
O8 Mo2 O5 93.45(13) . . ?
O9 Mo2 O5 157.70(12) . . ?
O7 Mo2 O5 85.28(11) . . ?
O10 Mo2 O5 70.62(10) . . ?
O8 Mo2 O3 162.63(12) . . ?
O9 Mo2 O3 89.65(12) . . ?
O7 Mo2 O3 82.18(11) . . ?
O10 Mo2 O3 72.92(10) . . ?
O5 Mo2 O3 69.78(10) . . ?
O12 Mo3 O11 105.44(15) . . ?
O12 Mo3 O13 103.35(13) . . ?
O11 Mo3 O13 101.12(14) . . ?
O12 Mo3 O10 96.94(12) . . ?
O11 Mo3 O10 96.67(13) . . ?
O13 Mo3 O10 148.21(11) . . ?
O12 Mo3 O5 156.25(13) . . ?
O11 Mo3 O5 96.26(13) . . ?
O13 Mo3 O5 81.36(11) . . ?
O10 Mo3 O5 70.62(10) . . ?
O12 Mo3 O6 87.30(13) . . ?
O11 Mo3 O6 164.35(12) . . ?
O13 Mo3 O6 84.31(11) . . ?
O10 Mo3 O6 72.36(11) . . ?
O5 Mo3 O6 69.84(9) . . ?
O15 Mo4 O14 102.63(16) . . ?
O15 Mo4 O13 97.46(13) . . ?
O14 Mo4 O13 98.94(13) . . ?
O15 Mo4 O7 98.34(13) . 2_565 ?
O14 Mo4 O7 96.38(14) . 2_565 ?
O13 Mo4 O7 154.98(11) . 2_565 ?
O15 Mo4 O4 165.56(13) . . ?
O14 Mo4 O4 91.81(14) . . ?
O13 Mo4 O4 80.08(11) . . ?
O7 Mo4 O4 79.78(10) 2_565 . ?
O15 Mo4 O2 85.62(13) . 2_565 ?
O14 Mo4 O2 171.48(14) . 2_565 ?
O13 Mo4 O2 81.87(11) . 2_565 ?
O7 Mo4 O2 80.13(11) 2_565 2_565 ?
O4 Mo4 O2 79.95(10) . 2_565 ?
C3 Mn1 C2 89.9(2) . . ?
C3 Mn1 C1 89.3(2) . . ?
C2 Mn1 C1 89.0(2) . . ?
C3 Mn1 O3 96.02(16) . . ?
C2 Mn1 O3 97.65(16) . . ?
C1 Mn1 O3 171.46(15) . . ?
C3 Mn1 O6 96.06(16) . . ?
C2 Mn1 O6 171.59(15) . . ?
C1 Mn1 O6 96.97(15) . . ?
O3 Mn1 O6 75.86(10) . . ?
C3 Mn1 O10 170.83(15) . . ?
C2 Mn1 O10 96.85(16) . . ?
C1 Mn1 O10 97.00(16) . . ?
O3 Mn1 O10 76.98(10) . . ?
O6 Mn1 O10 76.63(11) . . ?
Mo1 O2 Mo4 146.04(14) . 2_565 ?
Mn1 O3 Mo1 104.28(11) . . ?
Mn1 O3 Mo2 98.47(11) . . ?
Mo1 O3 Mo2 109.06(11) . . ?
Mo1 O4 Mo4 144.44(15) . . ?
Mo2 O5 Mo3 99.27(10) . . ?
Mo2 O5 Mo1 106.69(11) . . ?
Mo3 O5 Mo1 106.50(10) . . ?
Mn1 O6 Mo1 104.16(11) . . ?
Mn1 O6 Mo3 98.86(11) . . ?
Mo1 O6 Mo3 108.36(11) . . ?
Mo2 O7 Mo4 158.93(16) . 2_565 ?
Mo3 O10 Mo2 112.28(12) . . ?
Mo3 O10 Mn1 106.43(12) . . ?
Mo2 O10 Mn1 105.19(12) . . ?
Mo3 O13 Mo4 157.73(16) . . ?
O16 C1 Mn1 177.8(4) . . ?
O17 C2 Mn1 178.0(4) . . ?
O18 C3 Mn1 178.6(4) . . ?
_diffrn_measured_fraction_theta_max 0.988
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.988
_refine_diff_density_max         0.789
_refine_diff_density_min         -0.805
_refine_diff_density_rms         0.118


data_njy1_2
_database_code_depnum_ccdc_archive 'CCDC 909648'
#TrackingRef '909648.cif'
_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            
'C6 H50 Mo8 N4 O50 Re2'
_chemical_formula_weight         2118.37
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Mo Mo -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Re Re -1.0185 7.2310 '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                   10.570(3)
_cell_length_b                   15.425(4)
_cell_length_c                   15.933(4)
_cell_angle_alpha                90.00
_cell_angle_beta                 91.290(4)
_cell_angle_gamma                90.00
_cell_volume                     2597.2(12)
_cell_formula_units_Z            2
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    9805
_cell_measurement_theta_min      2.34
_cell_measurement_theta_max      28.10
_exptl_crystal_description       block
_exptl_crystal_colour            orange
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.15
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.701
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1988
_exptl_absorpt_coefficient_mu    6.622
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.3236
_exptl_absorpt_correction_T_max  0.4366
_exptl_absorpt_process_details   SADABS
_exptl_special_details           
;
?
;
_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            12795
_diffrn_reflns_av_R_equivalents  0.0289
_diffrn_reflns_av_unetI/netI     0.0307
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         2.29
_diffrn_reflns_theta_max         25.00
_reflns_number_total             4557
_reflns_number_gt                4309
_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^)+(0.0433P)^2^+3.6405P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   notdet
_refine_ls_hydrogen_treatment    noref
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         4557
_refine_ls_number_parameters     316
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0272
_refine_ls_R_factor_gt           0.0252
_refine_ls_wR_factor_ref         0.0696
_refine_ls_wR_factor_gt          0.0686
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_restrained_S_all      1.041
_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
Re1 Re 0.272045(18) 0.724862(12) 0.113920(11) 0.01991(8) Uani 1 1 d . . .
Mo1 Mo 0.47335(4) 0.75344(3) -0.05171(2) 0.01925(11) Uani 1 1 d . . .
Mo2 Mo 0.31952(4) 0.93611(2) 0.04742(2) 0.01519(10) Uani 1 1 d . . .
Mo3 Mo 0.56777(4) 0.80740(3) 0.14740(2) 0.01907(11) Uani 1 1 d . . .
Mo4 Mo 0.57972(4) 1.05023(3) 0.18505(2) 0.01834(10) Uani 1 1 d . . .
O1 O 0.2827(3) 0.8055(2) 0.00104(19) 0.0189(7) Uani 1 1 d . . .
O1W O 0.7884(4) 0.5748(3) -0.2085(2) 0.0440(10) Uani 1 1 d . . .
O2W O 0.5203(5) 0.5582(3) -0.2065(3) 0.0506(11) Uani 1 1 d . . .
O3W O 1.1470(4) 0.5936(3) -0.1342(2) 0.0437(10) Uani 1 1 d . . .
O4W O 0.0886(4) 0.8353(3) -0.1047(3) 0.0503(12) Uani 1 1 d . . .
O2 O 0.4682(3) 0.7205(2) 0.0730(2) 0.0215(7) Uani 1 1 d . . .
O3 O 0.3561(3) 0.8479(2) 0.14923(19) 0.0192(7) Uani 1 1 d . . .
O4 O 0.5954(3) 0.9211(2) 0.1861(2) 0.0237(7) Uani 1 1 d . . .
O5 O 0.4488(3) 0.8363(2) -0.1367(2) 0.0262(8) Uani 1 1 d . . .
O6 O 0.1634(3) 0.9536(2) 0.0708(2) 0.0292(8) Uani 1 1 d . . .
O7 O 0.5114(3) 0.8709(2) 0.02573(19) 0.0182(7) Uani 1 1 d . . .
O8 O 0.3327(3) 0.9719(2) -0.05902(19) 0.0206(7) Uani 1 1 d . . .
O9 O 0.4066(3) 1.0169(2) 0.1041(2) 0.0207(7) Uani 1 1 d . . .
O10 O 0.4830(3) 1.0575(2) 0.2704(2) 0.0282(8) Uani 1 1 d . . .
O11 O 0.7154(4) 0.7787(2) 0.1120(3) 0.0330(9) Uani 1 1 d . . .
O12 O 0.6281(4) 0.7254(3) -0.0651(3) 0.0353(9) Uani 1 1 d . . .
O13 O 0.3868(4) 0.6658(2) -0.0902(2) 0.0315(8) Uani 1 1 d . . .
O14 O 0.7276(3) 1.0676(2) 0.2294(2) 0.0289(8) Uani 1 1 d . . .
O15 O 0.5508(4) 0.7522(3) 0.2401(2) 0.0338(9) Uani 1 1 d . . .
O16 O 0.1764(5) 0.5501(3) 0.0473(3) 0.0563(13) Uani 1 1 d . . .
O17 O 0.3058(5) 0.6272(3) 0.2807(3) 0.0589(13) Uani 1 1 d . . .
O18 O -0.0026(4) 0.7623(3) 0.1631(4) 0.0611(14) Uani 1 1 d . . .
C1 C 0.2128(5) 0.6167(4) 0.0700(3) 0.0313(12) Uani 1 1 d . . .
C2 C 0.2929(5) 0.6644(4) 0.2181(3) 0.0321(12) Uani 1 1 d . . .
C3 C 0.1010(5) 0.7471(4) 0.1440(4) 0.0332(13) Uani 1 1 d . . .
O5W O 0.5486(5) 0.5478(3) 0.0715(3) 0.0493(11) Uani 1 1 d . . .
O6W O 0.9198(5) 0.6527(3) -0.0683(3) 0.0573(12) Uani 1 1 d . . .
O7W O 0.8487(5) 0.8459(4) -0.0323(3) 0.0646(14) Uani 1 1 d . . .
N1 N 0.6843(5) 1.0936(4) 0.4145(3) 0.0480(13) Uani 1 1 d . . .
N2 N -0.0895(6) 0.9617(5) 0.1277(4) 0.0657(19) Uani 1 1 d . . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Re1 0.02304(13) 0.01682(12) 0.01985(12) 0.00199(7) 0.00039(8) -0.00401(7)
Mo1 0.0245(2) 0.0142(2) 0.0191(2) -0.00180(16) 0.00115(16) 0.00102(16)
Mo2 0.0158(2) 0.0143(2) 0.01546(19) -0.00022(15) 0.00062(14) -0.00018(14)
Mo3 0.0215(2) 0.0158(2) 0.0197(2) 0.00085(16) -0.00376(16) 0.00176(16)
Mo4 0.0235(2) 0.0174(2) 0.01404(19) -0.00130(15) -0.00099(15) -0.00087(16)
O1 0.0212(17) 0.0159(16) 0.0196(16) 0.0013(13) 0.0004(13) -0.0019(13)
O1W 0.049(3) 0.048(3) 0.035(2) 0.010(2) 0.0046(19) -0.002(2)
O2W 0.064(3) 0.044(3) 0.045(2) -0.004(2) 0.008(2) 0.002(2)
O3W 0.050(3) 0.051(3) 0.030(2) 0.0028(19) -0.0060(18) -0.008(2)
O4W 0.037(2) 0.077(3) 0.036(2) -0.009(2) -0.0079(18) 0.003(2)
O2 0.0278(19) 0.0134(16) 0.0233(17) 0.0018(13) -0.0009(14) 0.0022(13)
O3 0.0235(17) 0.0150(16) 0.0190(15) 0.0011(13) -0.0008(13) -0.0022(13)
O4 0.0277(18) 0.0219(18) 0.0213(16) 0.0010(14) -0.0065(14) -0.0018(14)
O5 0.042(2) 0.0189(17) 0.0175(16) -0.0004(14) 0.0014(14) 0.0000(15)
O6 0.0212(18) 0.032(2) 0.035(2) -0.0003(16) 0.0053(15) -0.0004(15)
O7 0.0192(16) 0.0141(16) 0.0214(16) 0.0012(13) 0.0001(13) 0.0007(13)
O8 0.0263(18) 0.0192(17) 0.0161(15) 0.0004(13) -0.0003(13) 0.0016(14)
O9 0.0239(17) 0.0162(17) 0.0219(16) -0.0035(13) -0.0015(13) -0.0020(13)
O10 0.033(2) 0.029(2) 0.0237(17) -0.0017(15) 0.0062(15) 0.0010(15)
O11 0.026(2) 0.032(2) 0.040(2) -0.0084(17) -0.0024(17) 0.0062(15)
O12 0.029(2) 0.039(2) 0.038(2) -0.0056(17) 0.0060(17) 0.0054(16)
O13 0.042(2) 0.0232(19) 0.0297(19) -0.0047(16) 0.0011(16) -0.0052(16)
O14 0.032(2) 0.030(2) 0.0245(17) -0.0033(16) -0.0031(15) -0.0081(15)
O15 0.048(2) 0.0264(19) 0.0266(19) 0.0099(16) -0.0086(17) -0.0040(18)
O16 0.098(4) 0.032(2) 0.038(2) -0.006(2) -0.002(2) -0.031(2)
O17 0.074(3) 0.065(3) 0.036(2) 0.029(2) -0.008(2) -0.020(3)
O18 0.031(3) 0.062(3) 0.092(4) 0.013(3) 0.018(3) 0.007(2)
C1 0.041(3) 0.031(3) 0.022(2) 0.004(2) 0.002(2) -0.008(2)
C2 0.035(3) 0.031(3) 0.031(3) 0.002(2) -0.002(2) -0.008(2)
C3 0.033(3) 0.028(3) 0.038(3) 0.007(3) 0.004(2) -0.007(2)
O5W 0.062(3) 0.032(2) 0.055(3) 0.002(2) 0.005(2) 0.009(2)
O6W 0.063(3) 0.058(3) 0.051(3) 0.004(2) 0.008(2) -0.007(2)
O7W 0.056(3) 0.078(4) 0.061(3) 0.006(3) 0.013(3) -0.007(3)
N1 0.058(4) 0.054(3) 0.032(3) -0.002(2) 0.002(2) -0.014(3)
N2 0.041(3) 0.103(5) 0.053(3) 0.008(4) 0.001(3) 0.032(4)
_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
Re1 C1 1.909(6) . ?
Re1 C2 1.912(6) . ?
Re1 C3 1.912(6) . ?
Re1 O3 2.165(3) . ?
Re1 O2 2.188(4) . ?
Re1 O1 2.192(3) . ?
Mo1 O12 1.710(4) . ?
Mo1 O13 1.736(4) . ?
Mo1 O5 1.876(3) . ?
Mo1 O2 2.053(3) . ?
Mo1 O7 2.223(3) . ?
Mo1 O1 2.343(3) . ?
Mo2 O6 1.721(3) . ?
Mo2 O9 1.783(3) . ?
Mo2 O8 1.792(3) . ?
Mo2 O3 2.146(3) . ?
Mo2 O1 2.178(3) . ?
Mo2 O7 2.297(3) . ?
Mo3 O15 1.717(4) . ?
Mo3 O11 1.728(4) . ?
Mo3 O4 1.880(3) . ?
Mo3 O2 2.062(3) . ?
Mo3 O7 2.240(3) . ?
Mo3 O3 2.324(3) . ?
Mo4 O14 1.722(4) . ?
Mo4 O10 1.723(3) . ?
Mo4 O5 1.933(3) 3_675 ?
Mo4 O4 1.999(3) . ?
Mo4 O8 2.256(3) 3_675 ?
Mo4 O9 2.274(3) . ?
O5 Mo4 1.933(3) 3_675 ?
O8 Mo4 2.256(3) 3_675 ?
O16 C1 1.153(7) . ?
O17 C2 1.156(7) . ?
O18 C3 1.167(7) . ?
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
C1 Re1 C2 85.6(2) . . ?
C1 Re1 C3 86.8(2) . . ?
C2 Re1 C3 87.8(2) . . ?
C1 Re1 O3 172.19(18) . . ?
C2 Re1 O3 99.40(18) . . ?
C3 Re1 O3 99.3(2) . . ?
C1 Re1 O2 99.76(19) . . ?
C2 Re1 O2 98.75(19) . . ?
C3 Re1 O2 171.03(18) . . ?
O3 Re1 O2 73.62(12) . . ?
C1 Re1 O1 102.57(17) . . ?
C2 Re1 O1 169.11(18) . . ?
C3 Re1 O1 99.79(19) . . ?
O3 Re1 O1 71.77(12) . . ?
O2 Re1 O1 72.95(12) . . ?
O12 Mo1 O13 104.91(18) . . ?
O12 Mo1 O5 101.50(18) . . ?
O13 Mo1 O5 102.27(17) . . ?
O12 Mo1 O2 95.98(17) . . ?
O13 Mo1 O2 97.12(15) . . ?
O5 Mo1 O2 149.44(13) . . ?
O12 Mo1 O7 96.51(15) . . ?
O13 Mo1 O7 156.56(15) . . ?
O5 Mo1 O7 82.29(13) . . ?
O2 Mo1 O7 70.89(12) . . ?
O12 Mo1 O1 164.66(15) . . ?
O13 Mo1 O1 86.72(15) . . ?
O5 Mo1 O1 85.38(13) . . ?
O2 Mo1 O1 72.30(12) . . ?
O7 Mo1 O1 70.61(11) . . ?
O6 Mo2 O9 105.52(16) . . ?
O6 Mo2 O8 104.57(16) . . ?
O9 Mo2 O8 102.33(15) . . ?
O6 Mo2 O3 95.36(15) . . ?
O9 Mo2 O3 88.75(14) . . ?
O8 Mo2 O3 153.42(13) . . ?
O6 Mo2 O1 93.05(15) . . ?
O9 Mo2 O1 154.81(14) . . ?
O8 Mo2 O1 88.91(13) . . ?
O3 Mo2 O1 72.42(12) . . ?
O6 Mo2 O7 162.80(15) . . ?
O9 Mo2 O7 86.26(13) . . ?
O8 Mo2 O7 84.54(13) . . ?
O3 Mo2 O7 72.01(12) . . ?
O1 Mo2 O7 72.28(12) . . ?
O15 Mo3 O11 105.4(2) . . ?
O15 Mo3 O4 101.46(17) . . ?
O11 Mo3 O4 102.19(16) . . ?
O15 Mo3 O2 96.33(16) . . ?
O11 Mo3 O2 95.68(16) . . ?
O4 Mo3 O2 150.29(14) . . ?
O15 Mo3 O7 158.38(16) . . ?
O11 Mo3 O7 93.11(16) . . ?
O4 Mo3 O7 84.98(13) . . ?
O2 Mo3 O7 70.39(12) . . ?
O15 Mo3 O3 90.17(16) . . ?
O11 Mo3 O3 161.70(15) . . ?
O4 Mo3 O3 83.54(13) . . ?
O2 Mo3 O3 72.72(12) . . ?
O7 Mo3 O3 69.88(11) . . ?
O14 Mo4 O10 102.42(17) . . ?
O14 Mo4 O5 98.91(16) . 3_675 ?
O10 Mo4 O5 99.52(16) . 3_675 ?
O14 Mo4 O4 94.42(15) . . ?
O10 Mo4 O4 96.25(15) . . ?
O5 Mo4 O4 156.61(13) 3_675 . ?
O14 Mo4 O8 90.11(15) . 3_675 ?
O10 Mo4 O8 167.14(15) . 3_675 ?
O5 Mo4 O8 81.14(13) 3_675 3_675 ?
O4 Mo4 O8 79.70(13) . 3_675 ?
O14 Mo4 O9 168.39(14) . . ?
O10 Mo4 O9 88.77(15) . . ?
O5 Mo4 O9 82.08(13) 3_675 . ?
O4 Mo4 O9 81.09(12) . . ?
O8 Mo4 O9 78.57(12) 3_675 . ?
Mo2 O1 Re1 104.99(13) . . ?
Mo2 O1 Mo1 106.87(13) . . ?
Re1 O1 Mo1 99.20(12) . . ?
Mo1 O2 Mo3 111.80(15) . . ?
Mo1 O2 Re1 109.06(15) . . ?
Mo3 O2 Re1 106.48(14) . . ?
Mo2 O3 Re1 107.07(13) . . ?
Mo2 O3 Mo3 108.56(13) . . ?
Re1 O3 Mo3 98.67(12) . . ?
Mo3 O4 Mo4 156.16(18) . . ?
Mo1 O5 Mo4 157.26(19) . 3_675 ?
Mo1 O7 Mo3 99.52(12) . . ?
Mo1 O7 Mo2 106.91(13) . . ?
Mo3 O7 Mo2 106.24(12) . . ?
Mo2 O8 Mo4 146.93(18) . 3_675 ?
Mo2 O9 Mo4 147.68(18) . . ?
O16 C1 Re1 176.8(5) . . ?
O17 C2 Re1 179.4(6) . . ?
O18 C3 Re1 178.7(6) . . ?
_diffrn_measured_fraction_theta_max 0.995
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.995
_refine_diff_density_max         1.170
_refine_diff_density_min         -1.129
_refine_diff_density_rms         0.157


data_njy1_3
_database_code_depnum_ccdc_archive 'CCDC 909649'
#TrackingRef '909649.cif'
_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            
'C10 H54 Mn2 Na8 O62 W8'
_chemical_formula_weight         2931.10
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'
Na Na 0.0362 0.0249 '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'
P P 0.1023 0.0942 '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'
W W -0.8490 6.8722 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_symmetry_cell_setting           Triclinic
_symmetry_space_group_name_H-M   P-1
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
_cell_length_a                   9.491(2)
_cell_length_b                   12.290(3)
_cell_length_c                   13.967(3)
_cell_angle_alpha                71.437(3)
_cell_angle_beta                 87.357(3)
_cell_angle_gamma                71.161(3)
_cell_volume                     1458.8(6)
_cell_formula_units_Z            1
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    5785
_cell_measurement_theta_min      2.42
_cell_measurement_theta_max      28.45
_exptl_crystal_description       block
_exptl_crystal_colour            pink
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.16
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    3.332
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1336
_exptl_absorpt_coefficient_mu    16.310
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.1008
_exptl_absorpt_correction_T_max  0.1800
_exptl_absorpt_process_details   SADABS
_exptl_special_details           
;
?
;
_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            7435
_diffrn_reflns_av_R_equivalents  0.1699
_diffrn_reflns_av_unetI/netI     0.0968
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         1.85
_diffrn_reflns_theta_max         25.00
_reflns_number_total             5080
_reflns_number_gt                4621
_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. The ADP alerts of O2, O4, O5, O8, O17,
and C5 atoms were resolved by ISOR command, and the SIMU instruction is used for
resolving the high Ueq as compared to neighbors for O19.
;
_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^)+(0.1329P)^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     SHELXL
_refine_ls_extinction_coef       0.0017(3)
_refine_ls_extinction_expression 
Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_number_reflns         5080
_refine_ls_number_parameters     407
_refine_ls_number_restraints     42
_refine_ls_R_factor_all          0.0684
_refine_ls_R_factor_gt           0.0653
_refine_ls_wR_factor_ref         0.1764
_refine_ls_wR_factor_gt          0.1729
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_restrained_S_all      1.032
_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
W1 W 0.07365(6) -0.85448(4) -0.12136(4) 0.0126(2) Uani 1 1 d . . .
W2 W -0.30465(6) -0.71416(5) -0.16135(4) 0.0160(2) Uani 1 1 d . . .
W3 W -0.13718(6) -0.92428(5) -0.27336(4) 0.0157(2) Uani 1 1 d . . .
W4 W 0.15356(6) -1.18646(4) -0.10258(4) 0.0140(2) Uani 1 1 d . . .
Mn1 Mn -0.0737(2) -0.67455(18) -0.32946(15) 0.0191(5) Uani 1 1 d . . .
Na1 Na 0.1780(8) -1.5279(6) -0.0241(5) 0.0372(15) Uani 1 1 d . . .
Na2 Na 0.1501(10) -1.3369(8) -0.2829(5) 0.051(2) Uani 1 1 d . . .
Na3 Na 0.3873(10) -1.1497(8) -0.3438(6) 0.055(2) Uani 1 1 d U . .
Na4 Na 0.4608(8) -0.9050(7) -0.1989(6) 0.0457(18) Uani 1 1 d . . .
O1 O 0.2273(11) -0.8053(9) -0.1421(8) 0.024(2) Uani 1 1 d . . .
O2 O -0.0894(10) -0.6978(8) -0.1794(6) 0.0130(18) Uani 1 1 d U . .
O3 O 0.0348(11) -0.8536(8) -0.2631(7) 0.020(2) Uani 1 1 d . . .
O4 O 0.1615(10) -1.0195(7) -0.0842(6) 0.0114(18) Uani 1 1 d U . .
O5 O -0.3955(12) -0.5593(9) -0.2069(8) 0.028(2) Uani 1 1 d U . .
O6 O -0.4514(11) -0.7730(10) -0.1515(8) 0.028(2) Uani 1 1 d . . .
O7 O -0.2430(10) -0.7491(8) -0.2917(7) 0.018(2) Uani 1 1 d . . .
O8 O -0.1432(10) -0.8999(7) -0.1220(6) 0.0123(18) Uani 1 1 d U . .
O9 O -0.3024(12) -0.9589(9) -0.2559(8) 0.028(2) Uani 1 1 d . . .
O10 O -0.1021(14) -0.9158(11) -0.3995(8) 0.033(3) Uani 1 1 d . . .
O11 O 0.0002(11) -1.0755(9) -0.2093(7) 0.019(2) Uani 1 1 d . . .
O12 O 0.1264(14) -1.3165(10) -0.1094(8) 0.029(2) Uani 1 1 d . . .
O13 O 0.3061(11) -1.1855(10) -0.1754(8) 0.027(2) Uani 1 1 d . . .
O14 O -0.0218(10) -1.1566(8) -0.0041(7) 0.0152(19) Uani 1 1 d . . .
O15 O 0.2702(11) -1.2633(9) 0.0257(7) 0.020(2) Uani 1 1 d . . .
O16 O 0.2026(18) -0.6132(14) -0.3665(11) 0.060(4) Uani 1 1 d . . .
O17 O -0.0791(17) -0.6609(12) -0.5437(9) 0.048(3) Uani 1 1 d U . .
O18 O -0.2482(17) -0.4148(10) -0.4046(10) 0.051(4) Uani 1 1 d . . .
C1 C 0.0954(18) -0.6358(13) -0.3492(11) 0.025(3) Uani 1 1 d . . .
C2 C -0.069(2) -0.6732(15) -0.4567(12) 0.035(4) Uani 1 1 d . . .
C3 C -0.181(2) -0.5185(14) -0.3730(12) 0.030(4) Uani 1 1 d . . .
C4 C 0.780(4) -1.158(4) -0.421(3) 0.140(17) Uani 1 1 d . . .
H4A H 0.8819 -1.1811 -0.4374 0.209 Uiso 1 1 calc R . .
H4B H 0.7432 -1.0729 -0.4299 0.209 Uiso 1 1 calc R . .
H4C H 0.7208 -1.1765 -0.4636 0.209 Uiso 1 1 calc R . .
C5 C 0.769(3) -1.225(3) -0.316(2) 0.081(8) Uani 1 1 d U . .
O1W O 0.2060(15) -1.7315(12) 0.0699(10) 0.045(3) Uani 1 1 d . . .
O2W O 0.0467(13) -1.4811(10) 0.1143(8) 0.032(3) Uani 1 1 d . . .
O3W O 0.4133(17) -1.5652(14) 0.0650(12) 0.057(4) Uani 1 1 d . . .
O4W O 0.2749(15) -1.5588(11) -0.1751(10) 0.043(3) Uani 1 1 d . . .
O5W O 0.3999(16) -1.3584(14) -0.3423(11) 0.055(4) Uani 1 1 d . . .
O6W O 0.1425(13) -1.1318(11) -0.3943(9) 0.040(3) Uani 1 1 d . . .
O7W O 0.456(3) -1.135(2) -0.5320(15) 0.116(9) Uani 1 1 d . . .
O8W O 0.3241(15) -0.9431(12) -0.3185(10) 0.045(3) Uani 1 1 d . . .
O9W O 0.4840(17) -1.0871(17) -0.0635(12) 0.066(5) Uani 1 1 d . . .
O20 O 0.8944(17) -1.2967(13) -0.2598(10) 0.053(4) Uani 1 1 d . . .
O19 O 0.624(2) -1.2073(19) -0.2824(13) 0.084(4) Uani 1 1 d U . .
O10W O 0.5546(14) -1.2394(12) -0.1209(9) 0.044(3) Uani 1 1 d . . .
O11W O -0.453(2) -0.6397(19) -0.4542(13) 0.086(6) Uani 1 1 d . . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
W1 0.0161(3) 0.0133(3) 0.0093(3) -0.0011(2) 0.0005(2) -0.0085(2)
W2 0.0174(3) 0.0173(3) 0.0114(3) -0.0026(2) -0.0027(2) -0.0046(2)
W3 0.0198(4) 0.0171(3) 0.0104(3) -0.0032(2) -0.0032(2) -0.0069(2)
W4 0.0188(3) 0.0142(3) 0.0098(3) -0.0030(2) 0.0001(2) -0.0073(2)
Mn1 0.0283(12) 0.0184(10) 0.0088(10) 0.0016(8) -0.0006(8) -0.0110(9)
Na1 0.046(4) 0.035(3) 0.034(4) -0.012(3) 0.016(3) -0.019(3)
Na2 0.068(6) 0.064(5) 0.024(4) -0.008(4) 0.002(4) -0.033(5)
Na3 0.052(5) 0.072(5) 0.038(4) 0.000(4) -0.009(4) -0.031(4)
Na4 0.035(4) 0.061(5) 0.059(5) -0.033(4) 0.012(4) -0.027(4)
O1 0.020(5) 0.033(6) 0.027(6) -0.009(5) 0.009(4) -0.020(5)
O2 0.015(2) 0.013(2) 0.012(2) -0.0038(18) -0.0007(17) -0.0047(18)
O3 0.021(5) 0.020(5) 0.014(5) 0.003(4) -0.006(4) -0.009(4)
O4 0.015(4) 0.002(3) 0.012(4) 0.000(3) 0.001(3) 0.002(3)
O5 0.030(5) 0.014(4) 0.027(5) 0.001(4) -0.007(4) 0.003(4)
O6 0.015(5) 0.044(6) 0.034(6) -0.019(5) 0.006(4) -0.018(5)
O7 0.018(5) 0.012(4) 0.019(5) -0.005(4) 0.000(4) 0.001(4)
O8 0.016(4) 0.010(4) 0.005(4) 0.001(3) 0.000(3) 0.000(3)
O9 0.028(6) 0.028(5) 0.031(6) -0.011(5) 0.001(5) -0.014(5)
O10 0.051(8) 0.049(7) 0.013(5) -0.015(5) 0.007(5) -0.029(6)
O11 0.023(5) 0.024(5) 0.012(5) -0.005(4) -0.004(4) -0.011(4)
O12 0.054(7) 0.025(5) 0.016(5) -0.008(4) -0.003(5) -0.022(5)
O13 0.013(5) 0.032(6) 0.035(6) -0.012(5) 0.002(4) -0.008(4)
O14 0.020(5) 0.017(4) 0.016(5) -0.008(4) 0.005(4) -0.012(4)
O15 0.026(5) 0.026(5) 0.014(5) -0.010(4) 0.001(4) -0.011(4)
O16 0.060(10) 0.067(10) 0.053(9) 0.004(8) 0.007(8) -0.045(9)
O17 0.078(8) 0.050(6) 0.024(6) -0.012(5) 0.008(5) -0.033(6)
O18 0.072(10) 0.015(6) 0.041(8) 0.009(5) -0.006(7) 0.004(6)
C1 0.037(9) 0.022(7) 0.016(7) -0.001(6) -0.002(6) -0.014(7)
C2 0.049(11) 0.033(9) 0.020(9) 0.005(7) 0.002(7) -0.023(8)
C3 0.040(10) 0.026(8) 0.022(8) 0.002(7) -0.002(7) -0.015(7)
C4 0.13(3) 0.16(4) 0.08(3) -0.05(3) -0.06(2) 0.03(3)
C5 0.079(11) 0.082(11) 0.085(12) -0.024(8) 0.013(8) -0.032(9)
O1W 0.043(8) 0.048(8) 0.059(9) -0.025(7) -0.003(6) -0.027(6)
O2W 0.047(7) 0.038(6) 0.026(6) -0.018(5) 0.007(5) -0.025(6)
O3W 0.065(10) 0.063(9) 0.071(10) -0.041(8) 0.022(8) -0.042(8)
O4W 0.043(7) 0.043(7) 0.039(7) -0.015(6) 0.000(6) -0.008(6)
O5W 0.046(8) 0.065(9) 0.042(8) -0.003(7) -0.008(6) -0.013(7)
O6W 0.038(7) 0.051(8) 0.023(6) -0.011(6) -0.001(5) -0.005(6)
O7W 0.14(2) 0.15(2) 0.068(13) 0.015(13) -0.022(13) -0.104(19)
O8W 0.043(8) 0.052(8) 0.050(8) -0.019(7) 0.010(6) -0.026(7)
O9W 0.045(9) 0.102(13) 0.057(10) -0.008(9) -0.001(7) -0.048(9)
O20 0.062(10) 0.048(8) 0.038(8) -0.005(6) -0.010(7) -0.010(7)
O19 0.066(8) 0.108(9) 0.057(8) -0.002(7) -0.007(7) -0.023(8)
O10W 0.036(7) 0.052(8) 0.031(7) -0.002(6) -0.012(5) -0.007(6)
O11W 0.063(11) 0.109(15) 0.062(12) -0.025(11) -0.031(9) 0.004(10)
_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
W1 O1 1.730(9) . ?
W1 O4 1.832(8) . ?
W1 O14 1.833(9) 2_535 ?
W1 O2 1.990(9) . ?
W1 O3 2.026(9) . ?
W1 O8 2.301(9) . ?
W1 Mn1 3.095(2) . ?
W1 Na4 3.694(7) . ?
W2 O5 1.729(10) . ?
W2 O6 1.747(9) . ?
W2 O15 1.854(9) 2_535 ?
W2 O7 2.020(9) . ?
W2 O2 2.113(9) . ?
W2 O8 2.210(8) . ?
W2 Mn1 3.169(2) . ?
W3 O9 1.740(10) . ?
W3 O10 1.755(10) . ?
W3 O11 1.854(10) . ?
W3 O7 1.997(9) . ?
W3 O3 2.111(9) . ?
W3 O8 2.224(8) . ?
W3 Mn1 3.165(2) . ?
W4 O12 1.731(9) . ?
W4 O13 1.731(10) . ?
W4 O15 1.939(10) . ?
W4 O11 1.956(10) . ?
W4 O14 2.124(9) . ?
W4 O4 2.172(8) . ?
W4 Na2 3.574(8) . ?
Mn1 C2 1.770(17) . ?
Mn1 C3 1.772(16) . ?
Mn1 C1 1.802(16) . ?
Mn1 O3 2.022(10) . ?
Mn1 O2 2.028(9) . ?
Mn1 O7 2.065(10) . ?
Na1 O4W 2.354(14) . ?
Na1 O1W 2.359(15) . ?
Na1 O2W 2.376(13) . ?
Na1 O12 2.382(12) . ?
Na1 O3W 2.445(17) . ?
Na1 O2W 2.481(13) 2_525 ?
Na1 Na1 3.306(14) 2_525 ?
Na1 Na2 3.596(10) . ?
Na2 O20 2.343(18) 1_455 ?
Na2 O5W 2.436(17) . ?
Na2 O6W 2.486(15) . ?
Na2 O12 2.507(12) . ?
Na2 O17 2.554(14) 2_534 ?
Na2 O4W 2.563(16) . ?
Na2 Na3 3.607(11) . ?
Na3 O19 2.25(2) . ?
Na3 O6W 2.380(14) . ?
Na3 O13 2.391(14) . ?
Na3 O5W 2.522(18) . ?
Na3 O8W 2.549(16) . ?
Na3 O7W 2.64(2) . ?
Na4 O9 2.309(13) 1_655 ?
Na4 O6 2.317(12) 1_655 ?
Na4 O9W 2.379(19) . ?
Na4 O1 2.397(12) . ?
Na4 O8W 2.406(15) . ?
O6 Na4 2.317(12) 1_455 ?
O9 Na4 2.309(13) 1_455 ?
O14 W1 1.833(9) 2_535 ?
O15 W2 1.854(9) 2_535 ?
O16 C1 1.13(2) . ?
O17 C2 1.18(2) . ?
O17 Na2 2.554(14) 2_534 ?
O18 C3 1.17(2) . ?
C4 C5 1.45(5) . ?
C4 H4A 0.9600 . ?
C4 H4B 0.9600 . ?
C4 H4C 0.9600 . ?
C5 O20 1.33(3) . ?
C5 O19 1.40(3) . ?
O2W Na1 2.481(13) 2_525 ?
O20 Na2 2.343(18) 1_655 ?
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 W1 O4 101.7(4) . . ?
O1 W1 O14 103.3(4) . 2_535 ?
O4 W1 O14 98.1(4) . 2_535 ?
O1 W1 O2 100.4(4) . . ?
O4 W1 O2 155.3(4) . . ?
O14 W1 O2 87.5(4) 2_535 . ?
O1 W1 O3 98.8(4) . . ?
O4 W1 O3 88.7(4) . . ?
O14 W1 O3 155.1(4) 2_535 . ?
O2 W1 O3 77.1(4) . . ?
O1 W1 O8 170.2(4) . . ?
O4 W1 O8 83.5(3) . . ?
O14 W1 O8 84.0(4) 2_535 . ?
O2 W1 O8 73.1(3) . . ?
O3 W1 O8 72.9(3) . . ?
O1 W1 Mn1 90.3(4) . . ?
O4 W1 Mn1 128.8(3) . . ?
O14 W1 Mn1 127.5(3) 2_535 . ?
O2 W1 Mn1 40.1(2) . . ?
O3 W1 Mn1 40.1(3) . . ?
O8 W1 Mn1 80.0(2) . . ?
O1 W1 Na4 31.5(4) . . ?
O4 W1 Na4 74.3(3) . . ?
O14 W1 Na4 122.1(3) 2_535 . ?
O2 W1 Na4 122.7(3) . . ?
O3 W1 Na4 82.8(3) . . ?
O8 W1 Na4 147.4(2) . . ?
Mn1 W1 Na4 95.37(14) . . ?
O5 W2 O6 102.5(5) . . ?
O5 W2 O15 101.1(5) . 2_535 ?
O6 W2 O15 99.1(5) . 2_535 ?
O5 W2 O7 100.6(5) . . ?
O6 W2 O7 92.9(4) . . ?
O15 W2 O7 152.2(4) 2_535 . ?
O5 W2 O2 94.1(4) . . ?
O6 W2 O2 161.4(4) . . ?
O15 W2 O2 85.8(4) 2_535 . ?
O7 W2 O2 75.6(4) . . ?
O5 W2 O8 166.2(4) . . ?
O6 W2 O8 89.9(4) . . ?
O15 W2 O8 82.8(4) 2_535 . ?
O7 W2 O8 72.2(3) . . ?
O2 W2 O8 72.8(3) . . ?
O5 W2 Mn1 87.4(4) . . ?
O6 W2 Mn1 132.4(3) . . ?
O15 W2 Mn1 124.8(3) 2_535 . ?
O7 W2 Mn1 39.6(3) . . ?
O2 W2 Mn1 39.1(2) . . ?
O8 W2 Mn1 79.6(2) . . ?
O9 W3 O10 103.6(5) . . ?
O9 W3 O11 100.5(5) . . ?
O10 W3 O11 99.1(5) . . ?
O9 W3 O7 92.4(4) . . ?
O10 W3 O7 99.9(5) . . ?
O11 W3 O7 153.8(4) . . ?
O9 W3 O3 162.4(4) . . ?
O10 W3 O3 91.3(4) . . ?
O11 W3 O3 86.1(4) . . ?
O7 W3 O3 75.6(4) . . ?
O9 W3 O8 91.2(4) . . ?
O10 W3 O8 163.7(4) . . ?
O11 W3 O8 84.7(4) . . ?
O7 W3 O8 72.3(3) . . ?
O3 W3 O8 73.0(3) . . ?
O9 W3 Mn1 131.8(3) . . ?
O10 W3 Mn1 85.4(4) . . ?
O11 W3 Mn1 125.1(3) . . ?
O7 W3 Mn1 39.6(3) . . ?
O3 W3 Mn1 39.0(3) . . ?
O8 W3 Mn1 79.5(2) . . ?
O12 W4 O13 100.0(5) . . ?
O12 W4 O15 96.0(5) . . ?
O13 W4 O15 94.9(5) . . ?
O12 W4 O11 94.8(5) . . ?
O13 W4 O11 97.2(5) . . ?
O15 W4 O11 162.2(4) . . ?
O12 W4 O14 92.8(5) . . ?
O13 W4 O14 166.9(4) . . ?
O15 W4 O14 81.0(4) . . ?
O11 W4 O14 84.3(4) . . ?
O12 W4 O4 172.7(5) . . ?
O13 W4 O4 87.2(4) . . ?
O15 W4 O4 84.1(4) . . ?
O11 W4 O4 83.4(4) . . ?
O14 W4 O4 80.0(3) . . ?
O12 W4 Na2 39.9(4) . . ?
O13 W4 Na2 70.7(4) . . ?
O15 W4 Na2 124.1(3) . . ?
O11 W4 Na2 72.6(3) . . ?
O14 W4 Na2 121.9(3) . . ?
O4 W4 Na2 144.4(3) . . ?
C2 Mn1 C3 88.5(8) . . ?
C2 Mn1 C1 86.6(7) . . ?
C3 Mn1 C1 90.2(7) . . ?
C2 Mn1 O3 98.0(6) . . ?
C3 Mn1 O3 172.6(6) . . ?
C1 Mn1 O3 93.8(6) . . ?
C2 Mn1 O2 171.6(6) . . ?
C3 Mn1 O2 96.8(6) . . ?
C1 Mn1 O2 99.9(5) . . ?
O3 Mn1 O2 76.3(4) . . ?
C2 Mn1 O7 96.2(6) . . ?
C3 Mn1 O7 99.7(6) . . ?
C1 Mn1 O7 169.8(6) . . ?
O3 Mn1 O7 76.1(4) . . ?
O2 Mn1 O7 76.5(4) . . ?
C2 Mn1 W1 136.9(6) . . ?
C3 Mn1 W1 134.0(5) . . ?
C1 Mn1 W1 87.0(5) . . ?
O3 Mn1 W1 40.2(3) . . ?
O2 Mn1 W1 39.2(2) . . ?
O7 Mn1 W1 84.2(3) . . ?
C2 Mn1 W3 87.2(5) . . ?
C3 Mn1 W3 136.4(5) . . ?
C1 Mn1 W3 132.8(5) . . ?
O3 Mn1 W3 41.1(3) . . ?
O2 Mn1 W3 84.4(2) . . ?
O7 Mn1 W3 38.0(2) . . ?
W1 Mn1 W3 66.89(4) . . ?
C2 Mn1 W2 133.1(6) . . ?
C3 Mn1 W2 88.4(5) . . ?
C1 Mn1 W2 140.2(5) . . ?
O3 Mn1 W2 84.5(3) . . ?
O2 Mn1 W2 41.1(2) . . ?
O7 Mn1 W2 38.6(3) . . ?
W1 Mn1 W2 66.34(4) . . ?
W3 Mn1 W2 64.22(4) . . ?
O4W Na1 O1W 98.3(5) . . ?
O4W Na1 O2W 171.7(6) . . ?
O1W Na1 O2W 85.2(5) . . ?
O4W Na1 O12 86.9(4) . . ?
O1W Na1 O12 173.8(5) . . ?
O2W Na1 O12 89.3(4) . . ?
O4W Na1 O3W 98.1(5) . . ?
O1W Na1 O3W 85.1(5) . . ?
O2W Na1 O3W 89.7(5) . . ?
O12 Na1 O3W 97.6(5) . . ?
O4W Na1 O2W 78.4(5) . 2_525 ?
O1W Na1 O2W 88.6(4) . 2_525 ?
O2W Na1 O2W 94.2(4) . 2_525 ?
O12 Na1 O2W 89.1(4) . 2_525 ?
O3W Na1 O2W 172.3(5) . 2_525 ?
O4W Na1 Na1 124.0(5) . 2_525 ?
O1W Na1 Na1 85.5(4) . 2_525 ?
O2W Na1 Na1 48.4(3) . 2_525 ?
O12 Na1 Na1 88.8(4) . 2_525 ?
O3W Na1 Na1 137.7(5) . 2_525 ?
O2W Na1 Na1 45.8(3) 2_525 2_525 ?
O4W Na1 Na2 45.3(4) . . ?
O1W Na1 Na2 139.7(4) . . ?
O2W Na1 Na2 128.6(4) . . ?
O12 Na1 Na2 44.0(3) . . ?
O3W Na1 Na2 112.5(4) . . ?
O2W Na1 Na2 70.0(3) 2_525 . ?
Na1 Na1 Na2 101.0(3) 2_525 . ?
O20 Na2 O5W 168.6(6) 1_455 . ?
O20 Na2 O6W 98.7(5) 1_455 . ?
O5W Na2 O6W 73.8(5) . . ?
O20 Na2 O12 76.7(5) 1_455 . ?
O5W Na2 O12 113.1(6) . . ?
O6W Na2 O12 103.8(5) . . ?
O20 Na2 O17 83.9(5) 1_455 2_534 ?
O5W Na2 O17 86.1(5) . 2_534 ?
O6W Na2 O17 77.9(4) . 2_534 ?
O12 Na2 O17 160.6(6) . 2_534 ?
O20 Na2 O4W 105.5(5) 1_455 . ?
O5W Na2 O4W 82.6(5) . . ?
O6W Na2 O4W 155.7(6) . . ?
O12 Na2 O4W 79.9(4) . . ?
O17 Na2 O4W 106.7(5) 2_534 . ?
O20 Na2 W4 86.5(4) 1_455 . ?
O5W Na2 W4 100.0(4) . . ?
O6W Na2 W4 78.2(3) . . ?
O12 Na2 W4 26.3(2) . . ?
O17 Na2 W4 152.6(5) 2_534 . ?
O4W Na2 W4 100.7(4) . . ?
O20 Na2 Na1 82.0(4) 1_455 . ?
O5W Na2 Na1 109.1(5) . . ?
O6W Na2 Na1 144.3(4) . . ?
O12 Na2 Na1 41.3(3) . . ?
O17 Na2 Na1 137.1(4) 2_534 . ?
O4W Na2 Na1 40.8(3) . . ?
W4 Na2 Na1 66.21(16) . . ?
O20 Na2 Na3 133.4(5) 1_455 . ?
O5W Na2 Na3 44.3(4) . . ?
O6W Na2 Na3 41.0(3) . . ?
O12 Na2 Na3 90.1(4) . . ?
O17 Na2 Na3 102.7(4) 2_534 . ?
O4W Na2 Na3 115.9(4) . . ?
W4 Na2 Na3 66.4(2) . . ?
Na1 Na2 Na3 116.3(3) . . ?
O19 Na3 O6W 168.2(8) . . ?
O19 Na3 O13 89.8(6) . . ?
O6W Na3 O13 86.5(5) . . ?
O19 Na3 O5W 94.9(7) . . ?
O6W Na3 O5W 74.1(5) . . ?
O13 Na3 O5W 91.9(5) . . ?
O19 Na3 O8W 92.4(7) . . ?
O6W Na3 O8W 97.6(6) . . ?
O13 Na3 O8W 76.7(5) . . ?
O5W Na3 O8W 166.5(6) . . ?
O19 Na3 O7W 95.1(8) . . ?
O6W Na3 O7W 87.2(6) . . ?
O13 Na3 O7W 171.0(6) . . ?
O5W Na3 O7W 80.2(6) . . ?
O8W Na3 O7W 110.6(7) . . ?
O19 Na3 Na2 125.2(6) . . ?
O6W Na3 Na2 43.3(4) . . ?
O13 Na3 Na2 65.9(3) . . ?
O5W Na3 Na2 42.4(4) . . ?
O8W Na3 Na2 124.6(4) . . ?
O7W Na3 Na2 105.2(5) . . ?
O9 Na4 O6 81.9(4) 1_655 1_655 ?
O9 Na4 O9W 98.9(6) 1_655 . ?
O6 Na4 O9W 112.4(6) 1_655 . ?
O9 Na4 O1 166.2(5) 1_655 . ?
O6 Na4 O1 85.2(4) 1_655 . ?
O9W Na4 O1 90.5(5) . . ?
O9 Na4 O8W 100.3(5) 1_655 . ?
O6 Na4 O8W 149.8(6) 1_655 . ?
O9W Na4 O8W 97.2(5) . . ?
O1 Na4 O8W 88.5(5) . . ?
O9 Na4 W1 171.3(4) 1_655 . ?
O6 Na4 W1 106.8(3) 1_655 . ?
O9W Na4 W1 77.9(4) . . ?
O1 Na4 W1 22.2(2) . . ?
O8W Na4 W1 72.4(4) . . ?
W1 O1 Na4 126.3(5) . . ?
W1 O2 Mn1 100.8(4) . . ?
W1 O2 W2 113.3(4) . . ?
Mn1 O2 W2 99.9(4) . . ?
Mn1 O3 W1 99.7(4) . . ?
Mn1 O3 W3 100.0(4) . . ?
W1 O3 W3 113.0(4) . . ?
W1 O4 W4 145.4(5) . . ?
W2 O6 Na4 144.3(6) . 1_455 ?
W3 O7 W2 113.9(5) . . ?
W3 O7 Mn1 102.4(4) . . ?
W2 O7 Mn1 101.7(4) . . ?
W2 O8 W3 98.8(3) . . ?
W2 O8 W1 98.9(3) . . ?
W3 O8 W1 99.4(3) . . ?
W3 O9 Na4 144.5(6) . 1_455 ?
W3 O11 W4 151.9(5) . . ?
W4 O12 Na1 144.0(6) . . ?
W4 O12 Na2 113.8(5) . . ?
Na1 O12 Na2 94.7(4) . . ?
W4 O13 Na3 144.7(6) . . ?
W1 O14 W4 146.5(5) 2_535 . ?
W2 O15 W4 153.4(6) 2_535 . ?
C2 O17 Na2 165.3(12) . 2_534 ?
O16 C1 Mn1 176.1(15) . . ?
O17 C2 Mn1 172.6(17) . . ?
O18 C3 Mn1 177.4(16) . . ?
C5 C4 H4A 109.5 . . ?
C5 C4 H4B 109.5 . . ?
H4A C4 H4B 109.5 . . ?
C5 C4 H4C 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
O20 C5 O19 125(3) . . ?
O20 C5 C4 119(3) . . ?
O19 C5 C4 116(3) . . ?
Na1 O2W Na1 85.8(4) . 2_525 ?
Na1 O4W Na2 93.9(5) . . ?
Na2 O5W Na3 93.3(6) . . ?
Na3 O6W Na2 95.7(5) . . ?
Na4 O8W Na3 123.1(6) . . ?
C5 O20 Na2 135.5(16) . 1_655 ?
C5 O19 Na3 140.0(18) . . ?
_diffrn_measured_fraction_theta_max 0.984
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.984
_refine_diff_density_max         4.785
_refine_diff_density_min         -6.780
_refine_diff_density_rms         0.567