# Electronic Supplementary Material (ESI) for New Journal of Chemistry.
# This journal is © The Royal Society of Chemistry and the Centre National de la Recherche Scientifique 2014

#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  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.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_0012ljm

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            0012ljm
_chemical_melting_point          ?
_chemical_formula_moiety         'C6 H26 As2 N9 Na9 Ni3 O73 W18'
_chemical_formula_sum            'C6 H26 As2 N9 Na9 Ni3 O73 W18'
_chemical_formula_weight         5234.22

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'
As As 0.0499 2.0058 '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'
Na Na 0.0362 0.0249 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 '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'
W W -0.8490 6.8722 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Trigonal
_symmetry_space_group_name_H-M   'P 63/m'
_symmetry_space_group_name_Hall  '-P 6c'
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'x-y, x, z+1/2'
'-y, x-y, z'
'-x, -y, z+1/2'
'-x+y, -x, z'
'y, -x+y, z+1/2'
'-x, -y, -z'
'-x+y, -x, -z-1/2'
'y, -x+y, -z'
'x, y, -z-1/2'
'x-y, x, -z'
'-y, x-y, -z-1/2'

_cell_length_a                   13.9035(10)
_cell_length_b                   13.9035(10)
_cell_length_c                   33.499(5)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_volume                     5608.1(10)
_cell_formula_units_Z            2
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    7192
_cell_measurement_theta_min      2.43
_cell_measurement_theta_max      28.30

_exptl_crystal_description       block
_exptl_crystal_colour            orange
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.34
_exptl_crystal_size_min          0.32
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    3.100
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             4576.9
_exptl_absorpt_coefficient_mu    19.566
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.0337
_exptl_absorpt_correction_T_max  0.0521
_exptl_absorpt_process_details   
'Higashi, T. (1995). Program for Absorption Correction. Rigaku Corporation, Tokyo, Japan.'

_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            36180
_diffrn_reflns_av_R_equivalents  0.1015
_diffrn_reflns_av_unetI/netI     0.0570
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -42
_diffrn_reflns_limit_l_max       44
_diffrn_reflns_theta_min         2.43
_diffrn_reflns_theta_max         28.35
_reflns_number_total             4763
_reflns_number_gt                3699
_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 F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0654P)²+203.1337P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         4763
_refine_ls_number_parameters     175
_refine_ls_number_restraints     48
_refine_ls_R_factor_all          0.0759
_refine_ls_R_factor_gt           0.0574
_refine_ls_wR_factor_ref         0.1091
_refine_ls_wR_factor_gt          0.0928
_refine_ls_goodness_of_fit_ref   1.074
_refine_ls_restrained_S_all      1.107
_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
As1 As 0.3333 0.6667 0.16945(6) 0.0109(4) Uani 1 3 d SU . .
W1 W 0.26378(5) 0.38703(4) 0.157423(16) 0.01449(15) Uani 1 1 d U . .
W2 W 0.05505(5) 0.44502(5) 0.157450(16) 0.01474(15) Uani 1 1 d U . .
W5 W 0.21202(5) 0.49238(5) 0.073841(16) 0.01939(16) Uani 1 1 d U . .
Ni1 Ni 0.4096(2) 0.49859(19) 0.2500 0.0110(5) Uani 1 2 d S . .
Na1 Na 0.1288(6) 0.3703(6) 0.2500 0.0109(4) Uani 1 2 d SU . .
O1 O 0.2564(10) 0.2586(9) 0.1598(4) 0.030(3) Uani 1 1 d . . .
O2 O 0.3707(8) 0.5838(8) 0.0682(3) 0.021(2) Uani 1 1 d U . .
O3 O 0.2912(8) 0.4349(9) 0.2078(3) 0.0184(19) Uani 1 1 d U . .
O4 O 0.1062(8) 0.3385(7) 0.1624(3) 0.017(2) Uani 1 1 d U . .
O5 O 0.0912(9) 0.4891(9) 0.2082(3) 0.0189(18) Uani 1 1 d U . .
O6 O 0.0709(8) 0.4301(8) 0.0979(3) 0.020(2) Uani 1 1 d U . .
O7 O 0.2463(10) 0.5401(10) 0.1429(4) 0.0348(13) Uani 1 1 d U . .
O8 O 0.2356(7) 0.3831(7) 0.0980(2) 0.0109(4) Uani 1 1 d . . .
O9 O -0.0865(9) 0.3569(9) 0.1592(3) 0.027(2) Uani 1 1 d . . .
O10 O 0.4180(10) 0.4789(10) 0.1432(4) 0.0348(13) Uani 1 1 d . . .
O11 O 0.1734(11) 0.4378(11) 0.0262(3) 0.034(3) Uani 1 1 d . . .
C1 C 0.4658(15) 0.3296(16) 0.2171(6) 0.037(4) Uani 1 1 d . . .
H1A H 0.4621 0.3479 0.1907 0.045 Uiso 1 1 calc R . .
N1 N 0.4520(13) 0.3798(14) 0.2500 0.018(3) Uani 1 2 d S . .
N2 N 0.4860(18) 0.2478(16) 0.22978(15) 0.066(6) Uani 1 1 d D . .
H2A H 0.4968 0.2040 0.2147 0.079 Uiso 0.50 1 calc PR . .
O1W O 0.0000 0.0000 0.1079(11) 0.065(10) Uani 1 3 d S . .
H1WA H -0.0156 0.0512 0.1044 0.077 Uiso 0.33 1 d PR . .
H1WB H -0.0435 -0.0651 0.0992 0.077 Uiso 0.33 1 d PR . .
O2W O 0.0000 0.0000 0.2150(13) 0.120(15) Uani 1 3 d S . .
H2WA H -0.0070 0.0538 0.2235 0.144 Uiso 0.33 1 d PR . .
H2WB H -0.0453 -0.0659 0.2225 0.144 Uiso 0.33 1 d PR . .
O4W O 0.175(3) 0.198(3) 0.2500 0.035(5) Uani 0.50 2 d SPU . .
H4WA H 0.1826 0.1720 0.2717 0.042 Uiso 0.50 1 d PR . .
O5W O -0.026(3) 0.211(3) 0.2500 0.029(4) Uani 0.50 2 d SPU . .
H5WA H -0.0714 0.1960 0.2690 0.034 Uiso 0.50 1 d PR . .
H5WB H -0.0409 0.1654 0.2310 0.034 Uiso 0.50 1 d PR . .
Na2 Na 0.1600(12) 0.0388(12) 0.1393(5) 0.0348(13) Uani 0.477(13) 1 d PU . 2
Na2' Na 0.1428(11) 0.0332(11) 0.1716(4) 0.0348(13) Uani 0.523(13) 1 d PU . 1


_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. 
;

# SQUEEZE RESULTS (APPEND TO CIF) 
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
1 -0.016 -0.011 0.000 779.6 -1.0
2 -0.051 0.107 0.500 779.7 1.2
_platon_squeeze_details          
; ? 
;

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
As1 O7 1.796(12) 5_565 ?
As1 O7 1.796(12) . ?
As1 O7 1.796(12) 3_665 ?
W1 O1 1.738(11) . ?
W1 O3 1.785(10) . ?
W1 O10 1.928(13) . ?
W1 O4 1.950(10) . ?
W1 O8 2.026(8) . ?
W1 O7 2.311(13) . ?
W2 O9 1.722(11) . ?
W2 O5 1.793(10) . ?
W2 O10 1.925(12) 5_565 ?
W2 O4 1.945(10) . ?
W2 O6 2.030(10) . ?
W2 O7 2.353(12) . ?
W5 O11 1.732(11) . ?
W5 O6 1.884(10) . ?
W5 O8 1.888(9) . ?
W5 O2 1.906(10) 5_565 ?
W5 O2 1.927(10) . ?
W5 O7 2.388(12) . ?
Ni1 O5 1.996(10) 12_666 ?
Ni1 O5 1.996(10) 3_665 ?
Ni1 O3 2.008(10) . ?
Ni1 O3 2.008(10) 10_556 ?
Ni1 N1 2.012(16) . ?
Ni1 Na1 3.371(8) 3_665 ?
Na1 O5W 2.18(3) . ?
Na1 O5 2.414(11) 10_556 ?
Na1 O5 2.414(11) . ?
Na1 O3 2.424(11) 10_556 ?
Na1 O3 2.424(11) . ?
Na1 O4W 2.77(4) . ?
Na1 O4 2.960(10) . ?
Na1 O4 2.960(10) 10_556 ?
Na1 Ni1 3.371(8) 8_566 ?
Na1 W1 3.572(4) 10_556 ?
Na1 W2 3.579(4) 10_556 ?
O1 Na2' 2.742(17) . ?
O1 Na2 2.741(18) . ?
O2 W5 1.906(10) 3_665 ?
O4 Na2 2.775(18) 3 ?
O4 Na2' 2.795(17) 3 ?
O5 Ni1 1.996(10) 8_566 ?
O10 W2 1.925(12) 3_665 ?
C1 N2 1.37(2) . ?
C1 N1 1.369(19) . ?
C1 H1A 0.9300 . ?
N1 C1 1.369(19) 10_556 ?
N2 N2 1.354(10) 10_556 ?
N2 H2A 0.8600 . ?
O1W Na2 2.27(2) 5 ?
O1W Na2 2.27(2) . ?
O1W Na2 2.27(2) 3 ?
O1W Na2' 2.79(3) 3 ?
O1W Na2' 2.79(3) 5 ?
O1W Na2' 2.79(3) . ?
O1W H1WA 0.8500 . ?
O1W H1WB 0.8500 . ?
O2W Na2' 2.31(3) 5 ?
O2W Na2' 2.31(3) 3 ?
O2W Na2' 2.31(3) . ?
O2W H2WA 0.8500 . ?
O2W H2WB 0.8500 . ?
O4W H4WA 0.8412 . ?
O5W Na2' 2.96(2) 3 ?
O5W Na2' 2.96(2) 12_556 ?
O5W H5WA 0.8500 . ?
O5W H5WB 0.8501 . ?
Na2 O4 2.776(17) 5 ?
Na2 Na2 3.48(3) 5 ?
Na2 Na2 3.48(3) 3 ?
Na2' O4 2.795(17) 5 ?
Na2' O5W 2.96(2) 8_556 ?
Na2' Na2' 3.12(2) 3 ?
Na2' Na2' 3.12(2) 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
O7 As1 O7 97.6(5) 5_565 . ?
O7 As1 O7 97.6(5) 5_565 3_665 ?
O7 As1 O7 97.6(5) . 3_665 ?
O1 W1 O3 103.4(5) . . ?
O1 W1 O10 99.6(5) . . ?
O3 W1 O10 91.5(5) . . ?
O1 W1 O4 99.3(5) . . ?
O3 W1 O4 92.4(4) . . ?
O10 W1 O4 159.3(5) . . ?
O1 W1 O8 96.1(5) . . ?
O3 W1 O8 160.5(4) . . ?
O10 W1 O8 84.9(4) . . ?
O4 W1 O8 84.6(4) . . ?
O1 W1 O7 167.5(5) . . ?
O3 W1 O7 87.5(4) . . ?
O10 W1 O7 86.1(5) . . ?
O4 W1 O7 73.7(4) . . ?
O8 W1 O7 73.1(4) . . ?
O9 W2 O5 103.7(5) . . ?
O9 W2 O10 100.4(5) . 5_565 ?
O5 W2 O10 91.7(5) . 5_565 ?
O9 W2 O4 100.3(5) . . ?
O5 W2 O4 91.9(4) . . ?
O10 W2 O4 157.5(5) 5_565 . ?
O9 W2 O6 96.0(5) . . ?
O5 W2 O6 160.3(4) . . ?
O10 W2 O6 84.5(5) 5_565 . ?
O4 W2 O6 84.7(4) . . ?
O9 W2 O7 167.1(5) . . ?
O5 W2 O7 87.7(4) . . ?
O10 W2 O7 85.2(5) 5_565 . ?
O4 W2 O7 72.8(4) . . ?
O6 W2 O7 72.8(4) . . ?
O11 W5 O6 99.7(5) . . ?
O11 W5 O8 100.5(5) . . ?
O6 W5 O8 90.4(4) . . ?
O11 W5 O2 101.1(5) . 5_565 ?
O6 W5 O2 89.3(4) . 5_565 ?
O8 W5 O2 158.1(4) . 5_565 ?
O11 W5 O2 101.6(5) . . ?
O6 W5 O2 158.5(4) . . ?
O8 W5 O2 88.3(4) . . ?
O2 W5 O2 84.1(6) 5_565 . ?
O11 W5 O7 171.4(5) . . ?
O6 W5 O7 74.4(4) . . ?
O8 W5 O7 73.6(4) . . ?
O2 W5 O7 85.3(4) 5_565 . ?
O2 W5 O7 84.7(4) . . ?
O5 Ni1 O5 89.0(6) 12_666 3_665 ?
O5 Ni1 O3 159.8(4) 12_666 . ?
O5 Ni1 O3 87.2(4) 3_665 . ?
O5 Ni1 O3 87.2(4) 12_666 10_556 ?
O5 Ni1 O3 159.8(4) 3_665 10_556 ?
O3 Ni1 O3 89.5(6) . 10_556 ?
O5 Ni1 N1 101.6(5) 12_666 . ?
O5 Ni1 N1 101.6(5) 3_665 . ?
O3 Ni1 N1 98.6(5) . . ?
O3 Ni1 N1 98.6(5) 10_556 . ?
O5 Ni1 Na1 45.0(3) 12_666 3_665 ?
O5 Ni1 Na1 45.0(3) 3_665 3_665 ?
O3 Ni1 Na1 125.2(3) . 3_665 ?
O3 Ni1 Na1 125.2(3) 10_556 3_665 ?
N1 Ni1 Na1 113.5(5) . 3_665 ?
O5W Na1 O5 104.7(7) . 10_556 ?
O5W Na1 O5 104.7(8) . . ?
O5 Na1 O5 70.9(5) 10_556 . ?
O5W Na1 O3 129.7(6) . 10_556 ?
O5 Na1 O3 83.6(4) 10_556 10_556 ?
O5 Na1 O3 124.4(5) . 10_556 ?
O5W Na1 O3 129.7(6) . . ?
O5 Na1 O3 124.4(5) 10_556 . ?
O5 Na1 O3 83.6(4) . . ?
O3 Na1 O3 71.3(5) 10_556 . ?
O5W Na1 O4W 70.1(11) . . ?
O5 Na1 O4W 144.5(3) 10_556 . ?
O5 Na1 O4W 144.5(3) . . ?
O3 Na1 O4W 75.2(6) 10_556 . ?
O3 Na1 O4W 75.2(6) . . ?
O5W Na1 O4 82.6(2) . . ?
O5 Na1 O4 129.4(4) 10_556 . ?
O5 Na1 O4 59.0(3) . . ?
O3 Na1 O4 130.0(4) 10_556 . ?
O3 Na1 O4 59.1(3) . . ?
O4W Na1 O4 85.6(2) . . ?
O5W Na1 O4 82.6(2) . 10_556 ?
O5 Na1 O4 59.0(3) 10_556 10_556 ?
O5 Na1 O4 129.4(4) . 10_556 ?
O3 Na1 O4 59.1(3) 10_556 10_556 ?
O3 Na1 O4 130.0(4) . 10_556 ?
O4W Na1 O4 85.6(2) . 10_556 ?
O4 Na1 O4 164.7(5) . 10_556 ?
O5W Na1 Ni1 113.3(9) . 8_566 ?
O5 Na1 Ni1 35.8(3) 10_556 8_566 ?
O5 Na1 Ni1 35.8(3) . 8_566 ?
O3 Na1 Ni1 102.1(3) 10_556 8_566 ?
O3 Na1 Ni1 102.1(3) . 8_566 ?
O4W Na1 Ni1 176.6(8) . 8_566 ?
O4 Na1 Ni1 94.7(2) . 8_566 ?
O4 Na1 Ni1 94.7(2) 10_556 8_566 ?
O5W Na1 W1 106.5(4) . 10_556 ?
O5 Na1 W1 74.8(2) 10_556 10_556 ?
O5 Na1 W1 138.2(3) . 10_556 ?
O3 Na1 W1 26.9(2) 10_556 10_556 ?
O3 Na1 W1 96.9(3) . 10_556 ?
O4W Na1 W1 73.5(3) . 10_556 ?
O4 Na1 W1 152.0(3) . 10_556 ?
O4 Na1 W1 33.1(2) 10_556 10_556 ?
Ni1 Na1 W1 105.09(13) 8_566 10_556 ?
O5W Na1 W2 90.8(4) . 10_556 ?
O5 Na1 W2 26.8(2) 10_556 10_556 ?
O5 Na1 W2 96.4(3) . 10_556 ?
O3 Na1 W2 74.7(2) 10_556 10_556 ?
O3 Na1 W2 138.3(3) . 10_556 ?
O4W Na1 W2 118.32(17) . 10_556 ?
O4 Na1 W2 151.4(3) . 10_556 ?
O4 Na1 W2 32.9(2) 10_556 10_556 ?
Ni1 Na1 W2 62.33(10) 8_566 10_556 ?
W1 Na1 W2 56.38(2) 10_556 10_556 ?
O5W Na1 Na2' 43.9(4) . 3 ?
O5 Na1 Na2' 139.7(4) 10_556 3 ?
O5 Na1 Na2' 91.3(3) . 3 ?
O3 Na1 Na2' 134.2(4) 10_556 3 ?
O3 Na1 Na2' 87.3(3) . 3 ?
O4W Na1 Na2' 60.0(5) . 3 ?
O4 Na1 Na2' 42.7(3) . 3 ?
O4 Na1 Na2' 122.0(3) 10_556 3 ?
Ni1 Na1 Na2' 122.2(2) 8_566 3 ?
W1 Na1 Na2' 130.5(3) 10_556 3 ?
W2 Na1 Na2' 134.3(3) 10_556 3 ?
W1 O1 Na2' 152.3(7) . . ?
W1 O1 Na2 151.4(7) . . ?
W5 O2 W5 153.0(6) 3_665 . ?
W1 O3 Ni1 143.7(6) . . ?
W1 O3 Na1 115.3(5) . . ?
Ni1 O3 Na1 99.2(4) . . ?
W2 O4 W1 120.3(5) . . ?
W2 O4 Na2 117.5(5) . 3 ?
W1 O4 Na2 115.6(5) . 3 ?
W2 O4 Na2' 124.5(5) . 3 ?
W1 O4 Na2' 115.1(5) . 3 ?
W2 O4 Na1 91.3(4) . . ?
W1 O4 Na1 91.0(4) . . ?
Na2 O4 Na1 113.9(5) 3 . ?
Na2' O4 Na1 91.3(4) 3 . ?
W2 O5 Ni1 143.7(6) . 8_566 ?
W2 O5 Na1 115.8(5) . . ?
Ni1 O5 Na1 99.3(4) 8_566 . ?
W5 O6 W2 120.9(5) . . ?
As1 O7 W1 117.9(6) . . ?
As1 O7 W2 117.8(6) . . ?
W1 O7 W2 92.8(4) . . ?
As1 O7 W5 134.0(7) . . ?
W1 O7 W5 92.7(4) . . ?
W2 O7 W5 91.8(4) . . ?
W5 O8 W1 120.6(4) . . ?
W2 O10 W1 144.3(7) 3_665 . ?
N2 C1 N1 108.3(15) . . ?
N2 C1 H1A 125.9 . . ?
N1 C1 H1A 125.9 . . ?
C1 N1 C1 107(2) 10_556 . ?
C1 N1 Ni1 126.3(10) 10_556 . ?
C1 N1 Ni1 126.3(10) . . ?
N2 N2 C1 108.1(8) 10_556 . ?
N2 N2 H2A 125.9 10_556 . ?
C1 N2 H2A 125.9 . . ?
Na2 O1W Na2 100.2(11) 5 . ?
Na2 O1W Na2 100.2(11) 5 3 ?
Na2 O1W Na2 100.2(11) . 3 ?
Na2 O1W Na2' 86.3(11) 5 3 ?
Na2 O1W Na2' 85.7(11) . 3 ?
Na2 O1W Na2' 86.3(11) . 5 ?
Na2 O1W Na2' 85.7(11) 3 5 ?
Na2' O1W Na2' 67.9(9) 3 5 ?
Na2 O1W Na2' 85.7(11) 5 . ?
Na2 O1W Na2' 86.3(11) 3 . ?
Na2' O1W Na2' 67.9(9) 3 . ?
Na2' O1W Na2' 67.9(9) 5 . ?
Na2 O1W H1WA 120.7 5 . ?
Na2 O1W H1WA 119.7 . . ?
Na2' O1W H1WA 57.8 3 . ?
Na2' O1W H1WA 115.1 5 . ?
Na2' O1W H1WA 115.2 . . ?
Na2 O1W H1WB 48.0 5 . ?
Na2 O1W H1WB 120.3 . . ?
Na2 O1W H1WB 130.0 3 . ?
Na2' O1W H1WB 128.3 3 . ?
Na2' O1W H1WB 70.2 5 . ?
Na2' O1W H1WB 120.5 . . ?
H1WA O1W H1WB 120.0 . . ?
Na2' O2W Na2' 84.7(13) 5 3 ?
Na2' O2W Na2' 84.7(13) 5 . ?
Na2' O2W Na2' 84.7(13) 3 . ?
Na2' O2W H2WA 130.6 5 . ?
Na2' O2W H2WA 58.9 3 . ?
Na2' O2W H2WA 120.0 . . ?
Na2' O2W H2WB 56.4 5 . ?
Na2' O2W H2WB 127.7 3 . ?
Na2' O2W H2WB 120.0 . . ?
H2WA O2W H2WB 120.0 . . ?
Na1 O4W H4WA 120.3 . . ?
Na1 O5W Na2' 105.5(7) . 3 ?
Na1 O5W Na2' 105.5(7) . 12_556 ?
Na2' O5W Na2' 125.1(12) 3 12_556 ?
Na1 O5W H5WA 119.2 . . ?
Na2' O5W H5WA 134.7 3 . ?
Na2' O5W H5WA 51.0 12_556 . ?
Na1 O5W H5WB 120.8 . . ?
Na2' O5W H5WB 111.8 12_556 . ?
H5WA O5W H5WB 120.0 . . ?
O1W Na2 O1 104.9(6) . . ?
O1W Na2 O4 128.7(6) . 5 ?
O1 Na2 O4 125.9(6) . 5 ?
O1W Na2 Na2 39.9(6) . 5 ?
O1 Na2 Na2 127.9(6) . 5 ?
O4 Na2 Na2 95.4(6) 5 5 ?
O1W Na2 Na2 39.9(6) . 3 ?
O1 Na2 Na2 70.1(6) . 3 ?
O4 Na2 Na2 151.0(6) 5 3 ?
Na2 Na2 Na2 59.999(1) 5 3 ?
O2W Na2' O1 105.3(5) . . ?
O2W Na2' O4 124.4(7) . 5 ?
O1 Na2' O4 125.1(6) . 5 ?
O2W Na2' O1W 88.8(11) . . ?
O1 Na2' O1W 92.0(5) . . ?
O4 Na2' O1W 109.2(6) 5 . ?
O2W Na2' O5W 77.6(11) . 8_556 ?
O1 Na2' O5W 99.0(8) . 8_556 ?
O4 Na2' O5W 73.4(7) 5 8_556 ?
O1W Na2' O5W 164.3(9) . 8_556 ?
O2W Na2' Na2' 47.7(7) . 3 ?
O1 Na2' Na2' 73.3(6) . 3 ?
O4 Na2' Na2' 159.0(6) 5 3 ?
O1W Na2' Na2' 56.1(5) . 3 ?
O5W Na2' Na2' 116.6(6) 8_556 3 ?
O2W Na2' Na2' 47.7(7) . 5 ?
O1 Na2' Na2' 132.6(6) . 5 ?
O4 Na2' Na2' 99.9(7) 5 5 ?
O1W Na2' Na2' 56.1(5) . 5 ?
O5W Na2' Na2' 108.4(7) 8_556 5 ?
Na2' Na2' Na2' 60.000(1) 3 5 ?
O2W Na2' Na1 88.7(8) . 8_556 ?
O1 Na2' Na1 123.9(5) . 8_556 ?
O4 Na2' Na1 45.9(3) 5 8_556 ?
O1W Na2' Na1 143.3(4) . 8_556 ?
O5W Na2' Na1 30.7(6) 8_556 8_556 ?
Na2' Na2' Na1 136.0(3) 3 8_556 ?
Na2' Na2' Na1 97.0(5) 5 8_556 ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O3 W1 O1 Na2' 87.5(15) . . . . ?
O10 W1 O1 Na2' -178.6(15) . . . . ?
O4 W1 O1 Na2' -7.2(16) . . . . ?
O8 W1 O1 Na2' -92.8(15) . . . . ?
O7 W1 O1 Na2' -62(3) . . . . ?
O3 W1 O1 Na2 137.8(14) . . . . ?
O10 W1 O1 Na2 -128.3(14) . . . . ?
O4 W1 O1 Na2 43.1(15) . . . . ?
O8 W1 O1 Na2 -42.4(15) . . . . ?
O7 W1 O1 Na2 -12(3) . . . . ?
O11 W5 O2 W5 129.5(13) . . . 3_665 ?
O6 W5 O2 W5 -43(2) . . . 3_665 ?
O8 W5 O2 W5 -130.2(13) . . . 3_665 ?
O2 W5 O2 W5 29.3(15) 5_565 . . 3_665 ?
O7 W5 O2 W5 -56.5(13) . . . 3_665 ?
O1 W1 O3 Ni1 74.7(10) . . . . ?
O10 W1 O3 Ni1 -25.5(10) . . . . ?
O4 W1 O3 Ni1 174.8(10) . . . . ?
O8 W1 O3 Ni1 -104.5(13) . . . . ?
O7 W1 O3 Ni1 -111.6(10) . . . . ?
O1 W1 O3 Na1 -85.3(6) . . . . ?
O10 W1 O3 Na1 174.5(6) . . . . ?
O4 W1 O3 Na1 14.8(5) . . . . ?
O8 W1 O3 Na1 95.4(12) . . . . ?
O7 W1 O3 Na1 88.4(6) . . . . ?
O5 Ni1 O3 W1 125.3(12) 12_666 . . . ?
O5 Ni1 O3 W1 45.8(10) 3_665 . . . ?
O3 Ni1 O3 W1 -154.2(7) 10_556 . . . ?
N1 Ni1 O3 W1 -55.5(10) . . . . ?
Na1 Ni1 O3 W1 71.4(11) 3_665 . . . ?
O5 Ni1 O3 Na1 -72.9(12) 12_666 . . . ?
O5 Ni1 O3 Na1 -152.5(5) 3_665 . . . ?
O3 Ni1 O3 Na1 7.6(6) 10_556 . . . ?
N1 Ni1 O3 Na1 106.2(5) . . . . ?
Na1 Ni1 O3 Na1 -126.8(3) 3_665 . . . ?
O5W Na1 O3 W1 35.0(11) . . . . ?
O5 Na1 O3 W1 -130.4(5) 10_556 . . . ?
O5 Na1 O3 W1 -68.8(6) . . . . ?
O3 Na1 O3 W1 161.5(3) 10_556 . . . ?
O4W Na1 O3 W1 82.5(7) . . . . ?
O4 Na1 O3 W1 -11.3(4) . . . . ?
O4 Na1 O3 W1 153.5(5) 10_556 . . . ?
Ni1 Na1 O3 W1 -99.6(5) 8_566 . . . ?
W1 Na1 O3 W1 153.3(4) 10_556 . . . ?
W2 Na1 O3 W1 -161.3(3) 10_556 . . . ?
Na2' Na1 O3 W1 22.8(5) 3 . . . ?
O5W Na1 O3 Ni1 -133.2(9) . . . . ?
O5 Na1 O3 Ni1 61.4(6) 10_556 . . . ?
O5 Na1 O3 Ni1 123.0(4) . . . . ?
O3 Na1 O3 Ni1 -6.6(5) 10_556 . . . ?
O4W Na1 O3 Ni1 -85.7(6) . . . . ?
O4 Na1 O3 Ni1 -179.5(5) . . . . ?
O4 Na1 O3 Ni1 -14.6(7) 10_556 . . . ?
Ni1 Na1 O3 Ni1 92.2(4) 8_566 . . . ?
W1 Na1 O3 Ni1 -14.9(4) 10_556 . . . ?
W2 Na1 O3 Ni1 30.5(7) 10_556 . . . ?
Na2' Na1 O3 Ni1 -145.4(4) 3 . . . ?
O9 W2 O4 W1 174.2(6) . . . . ?
O5 W2 O4 W1 -81.5(6) . . . . ?
O10 W2 O4 W1 17.6(15) 5_565 . . . ?
O6 W2 O4 W1 79.1(6) . . . . ?
O7 W2 O4 W1 5.5(5) . . . . ?
O9 W2 O4 Na2 24.0(7) . . . 3 ?
O5 W2 O4 Na2 128.3(6) . . . 3 ?
O10 W2 O4 Na2 -132.6(11) 5_565 . . 3 ?
O6 W2 O4 Na2 -71.1(6) . . . 3 ?
O7 W2 O4 Na2 -144.7(7) . . . 3 ?
O9 W2 O4 Na2' -1.4(7) . . . 3 ?
O5 W2 O4 Na2' 102.9(6) . . . 3 ?
O10 W2 O4 Na2' -158.0(11) 5_565 . . 3 ?
O6 W2 O4 Na2' -96.5(6) . . . 3 ?
O7 W2 O4 Na2' -170.1(7) . . . 3 ?
O9 W2 O4 Na1 -93.9(4) . . . . ?
O5 W2 O4 Na1 10.4(4) . . . . ?
O10 W2 O4 Na1 109.5(12) 5_565 . . . ?
O6 W2 O4 Na1 171.0(4) . . . . ?
O7 W2 O4 Na1 97.4(4) . . . . ?
O1 W1 O4 W2 -174.9(6) . . . . ?
O3 W1 O4 W2 81.2(6) . . . . ?
O10 W1 O4 W2 -19.5(16) . . . . ?
O8 W1 O4 W2 -79.5(6) . . . . ?
O7 W1 O4 W2 -5.6(5) . . . . ?
O1 W1 O4 Na2 -24.2(7) . . . 3 ?
O3 W1 O4 Na2 -128.1(6) . . . 3 ?
O10 W1 O4 Na2 131.3(12) . . . 3 ?
O8 W1 O4 Na2 71.2(6) . . . 3 ?
O7 W1 O4 Na2 145.2(7) . . . 3 ?
O1 W1 O4 Na2' 1.1(7) . . . 3 ?
O3 W1 O4 Na2' -102.8(6) . . . 3 ?
O10 W1 O4 Na2' 156.5(12) . . . 3 ?
O8 W1 O4 Na2' 96.5(5) . . . 3 ?
O7 W1 O4 Na2' 170.4(6) . . . 3 ?
O1 W1 O4 Na1 93.0(5) . . . . ?
O3 W1 O4 Na1 -10.9(4) . . . . ?
O10 W1 O4 Na1 -111.5(12) . . . . ?
O8 W1 O4 Na1 -171.6(4) . . . . ?
O7 W1 O4 Na1 -97.6(4) . . . . ?
O5W Na1 O4 W2 103.2(9) . . . . ?
O5 Na1 O4 W2 0.2(6) 10_556 . . . ?
O5 Na1 O4 W2 -9.0(4) . . . . ?
O3 Na1 O4 W2 -119.8(5) 10_556 . . . ?
O3 Na1 O4 W2 -111.0(4) . . . . ?
O4W Na1 O4 W2 173.6(8) . . . . ?
O4 Na1 O4 W2 118.3(17) 10_556 . . . ?
Ni1 Na1 O4 W2 -9.7(3) 8_566 . . . ?
W1 Na1 O4 W2 -145.3(5) 10_556 . . . ?
W2 Na1 O4 W2 25.1(8) 10_556 . . . ?
Na2' Na1 O4 W2 124.6(5) 3 . . . ?
O5W Na1 O4 W1 -136.5(9) . . . . ?
O5 Na1 O4 W1 120.5(5) 10_556 . . . ?
O5 Na1 O4 W1 111.4(4) . . . . ?
O3 Na1 O4 W1 0.5(6) 10_556 . . . ?
O3 Na1 O4 W1 9.3(3) . . . . ?
O4W Na1 O4 W1 -66.1(8) . . . . ?
O4 Na1 O4 W1 -121.4(17) 10_556 . . . ?
Ni1 Na1 O4 W1 110.6(3) 8_566 . . . ?
W1 Na1 O4 W1 -24.9(8) 10_556 . . . ?
W2 Na1 O4 W1 145.4(5) 10_556 . . . ?
Na2' Na1 O4 W1 -115.1(5) 3 . . . ?
O5W Na1 O4 Na2 -17.8(10) . . . 3 ?
O5 Na1 O4 Na2 -120.8(6) 10_556 . . 3 ?
O5 Na1 O4 Na2 -130.0(6) . . . 3 ?
O3 Na1 O4 Na2 119.2(6) 10_556 . . 3 ?
O3 Na1 O4 Na2 128.0(6) . . . 3 ?
O4W Na1 O4 Na2 52.6(9) . . . 3 ?
O4 Na1 O4 Na2 -3(2) 10_556 . . 3 ?
Ni1 Na1 O4 Na2 -130.8(5) 8_566 . . 3 ?
W1 Na1 O4 Na2 93.7(8) 10_556 . . 3 ?
W2 Na1 O4 Na2 -95.9(7) 10_556 . . 3 ?
Na2' Na1 O4 Na2 3.6(4) 3 . . 3 ?
O5W Na1 O4 Na2' -21.4(9) . . . 3 ?
O5 Na1 O4 Na2' -124.4(6) 10_556 . . 3 ?
O5 Na1 O4 Na2' -133.6(5) . . . 3 ?
O3 Na1 O4 Na2' 115.6(6) 10_556 . . 3 ?
O3 Na1 O4 Na2' 124.4(5) . . . 3 ?
O4W Na1 O4 Na2' 49.0(8) . . . 3 ?
O4 Na1 O4 Na2' -6(2) 10_556 . . 3 ?
Ni1 Na1 O4 Na2' -134.3(4) 8_566 . . 3 ?
W1 Na1 O4 Na2' 90.1(7) 10_556 . . 3 ?
W2 Na1 O4 Na2' -99.5(7) 10_556 . . 3 ?
O9 W2 O5 Ni1 -77.2(11) . . . 8_566 ?
O10 W2 O5 Ni1 23.9(10) 5_565 . . 8_566 ?
O4 W2 O5 Ni1 -178.2(10) . . . 8_566 ?
O6 W2 O5 Ni1 102.5(14) . . . 8_566 ?
O7 W2 O5 Ni1 109.1(10) . . . 8_566 ?
O9 W2 O5 Na1 86.9(6) . . . . ?
O10 W2 O5 Na1 -172.0(6) 5_565 . . . ?
O4 W2 O5 Na1 -14.2(6) . . . . ?
O6 W2 O5 Na1 -93.4(13) . . . . ?
O7 W2 O5 Na1 -86.9(6) . . . . ?
O5W Na1 O5 W2 -60.9(7) . . . . ?
O5 Na1 O5 W2 -161.7(3) 10_556 . . . ?
O3 Na1 O5 W2 130.6(5) 10_556 . . . ?
O3 Na1 O5 W2 68.5(6) . . . . ?
O4W Na1 O5 W2 15.3(16) . . . . ?
O4 Na1 O5 W2 10.8(4) . . . . ?
O4 Na1 O5 W2 -153.4(5) 10_556 . . . ?
Ni1 Na1 O5 W2 -170.5(8) 8_566 . . . ?
W1 Na1 O5 W2 161.7(3) 10_556 . . . ?
W2 Na1 O5 W2 -153.5(5) 10_556 . . . ?
Na2' Na1 O5 W2 -18.6(5) 3 . . . ?
O5W Na1 O5 Ni1 109.6(6) . . . 8_566 ?
O5 Na1 O5 Ni1 8.8(5) 10_556 . . 8_566 ?
O3 Na1 O5 Ni1 -58.8(6) 10_556 . . 8_566 ?
O3 Na1 O5 Ni1 -121.0(4) . . . 8_566 ?
O4W Na1 O5 Ni1 -174.2(13) . . . 8_566 ?
O4 Na1 O5 Ni1 -178.7(5) . . . 8_566 ?
O4 Na1 O5 Ni1 17.1(7) 10_556 . . 8_566 ?
W1 Na1 O5 Ni1 -27.8(7) 10_556 . . 8_566 ?
W2 Na1 O5 Ni1 17.0(4) 10_556 . . 8_566 ?
Na2' Na1 O5 Ni1 151.9(4) 3 . . 8_566 ?
O11 W5 O6 W2 172.3(6) . . . . ?
O8 W5 O6 W2 71.6(6) . . . . ?
O2 W5 O6 W2 -86.5(6) 5_565 . . . ?
O2 W5 O6 W2 -14.7(15) . . . . ?
O7 W5 O6 W2 -1.3(5) . . . . ?
O9 W2 O6 W5 -172.2(6) . . . . ?
O5 W2 O6 W5 8.1(16) . . . . ?
O10 W2 O6 W5 87.9(7) 5_565 . . . ?
O4 W2 O6 W5 -72.4(6) . . . . ?
O7 W2 O6 W5 1.3(5) . . . . ?
O7 As1 O7 W1 174.6(6) 5_565 . . . ?
O7 As1 O7 W1 75.8(10) 3_665 . . . ?
O7 As1 O7 W2 -75.4(10) 5_565 . . . ?
O7 As1 O7 W2 -174.1(6) 3_665 . . . ?
O7 As1 O7 W5 48.7(7) 5_565 . . . ?
O7 As1 O7 W5 -50.0(7) 3_665 . . . ?
O1 W1 O7 As1 -175(2) . . . . ?
O3 W1 O7 As1 34.5(7) . . . . ?
O10 W1 O7 As1 -57.2(7) . . . . ?
O4 W1 O7 As1 127.6(7) . . . . ?
O8 W1 O7 As1 -143.1(7) . . . . ?
O1 W1 O7 W2 61(2) . . . . ?
O3 W1 O7 W2 -89.2(4) . . . . ?
O10 W1 O7 W2 179.1(5) . . . . ?
O4 W1 O7 W2 4.0(4) . . . . ?
O8 W1 O7 W2 93.2(4) . . . . ?
O1 W1 O7 W5 -31(2) . . . . ?
O3 W1 O7 W5 178.8(5) . . . . ?
O10 W1 O7 W5 87.1(5) . . . . ?
O4 W1 O7 W5 -88.0(4) . . . . ?
O8 W1 O7 W5 1.2(3) . . . . ?
O9 W2 O7 As1 173.0(19) . . . . ?
O5 W2 O7 As1 -35.1(7) . . . . ?
O10 W2 O7 As1 56.8(7) 5_565 . . . ?
O4 W2 O7 As1 -127.8(8) . . . . ?
O6 W2 O7 As1 142.6(8) . . . . ?
O9 W2 O7 W1 -63(2) . . . . ?
O5 W2 O7 W1 88.7(5) . . . . ?
O10 W2 O7 W1 -179.4(5) 5_565 . . . ?
O4 W2 O7 W1 -4.0(4) . . . . ?
O6 W2 O7 W1 -93.6(5) . . . . ?
O9 W2 O7 W5 30(2) . . . . ?
O5 W2 O7 W5 -178.6(5) . . . . ?
O10 W2 O7 W5 -86.6(5) 5_565 . . . ?
O4 W2 O7 W5 88.8(4) . . . . ?
O6 W2 O7 W5 -0.9(4) . . . . ?
O6 W5 O7 As1 -131.9(10) . . . . ?
O8 W5 O7 As1 132.9(9) . . . . ?
O2 W5 O7 As1 -41.4(9) 5_565 . . . ?
O2 W5 O7 As1 43.2(9) . . . . ?
O6 W5 O7 W1 93.8(5) . . . . ?
O8 W5 O7 W1 -1.3(4) . . . . ?
O2 W5 O7 W1 -175.6(5) 5_565 . . . ?
O2 W5 O7 W1 -91.1(4) . . . . ?
O6 W5 O7 W2 0.9(4) . . . . ?
O8 W5 O7 W2 -94.2(4) . . . . ?
O2 W5 O7 W2 91.5(4) 5_565 . . . ?
O2 W5 O7 W2 176.0(5) . . . . ?
O11 W5 O8 W1 -171.8(6) . . . . ?
O6 W5 O8 W1 -71.9(6) . . . . ?
O2 W5 O8 W1 17.2(14) 5_565 . . . ?
O2 W5 O8 W1 86.7(5) . . . . ?
O7 W5 O8 W1 1.7(5) . . . . ?
O1 W1 O8 W5 171.6(6) . . . . ?
O3 W1 O8 W5 -9.2(15) . . . . ?
O10 W1 O8 W5 -89.3(6) . . . . ?
O4 W1 O8 W5 72.8(5) . . . . ?
O7 W1 O8 W5 -1.8(5) . . . . ?
O1 W1 O10 W2 -127.2(12) . . . 3_665 ?
O3 W1 O10 W2 -23.4(12) . . . 3_665 ?
O4 W1 O10 W2 77.4(18) . . . 3_665 ?
O8 W1 O10 W2 137.4(12) . . . 3_665 ?
O7 W1 O10 W2 64.0(12) . . . 3_665 ?
N2 C1 N1 C1 1(3) . . . 10_556 ?
N2 C1 N1 Ni1 -175.4(14) . . . . ?
O5 Ni1 N1 C1 46.4(17) 12_666 . . 10_556 ?
O5 Ni1 N1 C1 137.8(15) 3_665 . . 10_556 ?
O3 Ni1 N1 C1 -133.3(16) . . . 10_556 ?
O3 Ni1 N1 C1 -42.5(16) 10_556 . . 10_556 ?
Na1 Ni1 N1 C1 92.1(16) 3_665 . . 10_556 ?
O5 Ni1 N1 C1 -137.8(15) 12_666 . . . ?
O5 Ni1 N1 C1 -46.4(17) 3_665 . . . ?
O3 Ni1 N1 C1 42.5(16) . . . . ?
O3 Ni1 N1 C1 133.3(16) 10_556 . . . ?
Na1 Ni1 N1 C1 -92.1(16) 3_665 . . . ?
N1 C1 N2 N2 -0.7(17) . . . 10_556 ?
O5 Na1 O5W Na2' 149.8(8) 10_556 . . 3 ?
O5 Na1 O5W Na2' 76.1(10) . . . 3 ?
O3 Na1 O5W Na2' -116.3(5) 10_556 . . 3 ?
O3 Na1 O5W Na2' -17.8(14) . . . 3 ?
O4W Na1 O5W Na2' -67.1(8) . . . 3 ?
O4 Na1 O5W Na2' 21.0(8) . . . 3 ?
O4 Na1 O5W Na2' -155.1(10) 10_556 . . 3 ?
Ni1 Na1 O5W Na2' 112.9(8) 8_566 . . 3 ?
W1 Na1 O5W Na2' -132.0(6) 10_556 . . 3 ?
W2 Na1 O5W Na2' 173.0(8) 10_556 . . 3 ?
O5 Na1 O5W Na2' -76.1(10) 10_556 . . 12_556 ?
O5 Na1 O5W Na2' -149.8(8) . . . 12_556 ?
O3 Na1 O5W Na2' 17.8(14) 10_556 . . 12_556 ?
O3 Na1 O5W Na2' 116.3(5) . . . 12_556 ?
O4W Na1 O5W Na2' 67.1(8) . . . 12_556 ?
O4 Na1 O5W Na2' 155.1(10) . . . 12_556 ?
O4 Na1 O5W Na2' -20.9(8) 10_556 . . 12_556 ?
Ni1 Na1 O5W Na2' -112.9(8) 8_566 . . 12_556 ?
W1 Na1 O5W Na2' 2.1(11) 10_556 . . 12_556 ?
W2 Na1 O5W Na2' -52.9(9) 10_556 . . 12_556 ?
Na2' Na1 O5W Na2' 134.1(17) 3 . . 12_556 ?
Na2 O1W Na2 O1 -132.3(6) 5 . . . ?
Na2 O1W Na2 O1 -29.9(13) 3 . . . ?
Na2' O1W Na2 O1 -46.8(8) 3 . . . ?
Na2' O1W Na2 O1 -114.9(6) 5 . . . ?
Na2' O1W Na2 O1 -82.2(12) . . . . ?
Na2 O1W Na2 O4 39.7(18) 5 . . 5 ?
Na2 O1W Na2 O4 142.1(5) 3 . . 5 ?
Na2' O1W Na2 O4 125.2(9) 3 . . 5 ?
Na2' O1W Na2 O4 57.1(13) 5 . . 5 ?
Na2' O1W Na2 O4 89.9(15) . . . 5 ?
Na2 O1W Na2 Na2 102.4(17) 3 . . 5 ?
Na2' O1W Na2 Na2 85.5(12) 3 . . 5 ?
Na2' O1W Na2 Na2 17.4(7) 5 . . 5 ?
Na2' O1W Na2 Na2 50.2(13) . . . 5 ?
Na2 O1W Na2 Na2 -102.4(17) 5 . . 3 ?
Na2' O1W Na2 Na2 -16.9(6) 3 . . 3 ?
Na2' O1W Na2 Na2 -85.0(12) 5 . . 3 ?
Na2' O1W Na2 Na2 -52.2(13) . . . 3 ?
W1 O1 Na2 O1W -10.0(19) . . . . ?
Na2' O1 Na2 O1W 104.4(15) . . . . ?
W1 O1 Na2 O4 177.7(12) . . . 5 ?
Na2' O1 Na2 O4 -67.9(11) . . . 5 ?
W1 O1 Na2 Na2 -46.9(17) . . . 5 ?
Na2' O1 Na2 Na2 67.4(10) . . . 5 ?
W1 O1 Na2 Na2 -29.9(13) . . . 3 ?
Na2' O1 Na2 Na2 84.5(11) . . . 3 ?
Na2' O2W Na2' O1 134.3(5) 5 . . . ?
Na2' O2W Na2' O1 49.2(10) 3 . . . ?
Na2' O2W Na2' O4 -70.0(14) 5 . . 5 ?
Na2' O2W Na2' O4 -155.1(6) 3 . . 5 ?
Na2' O2W Na2' O1W 42.6(6) 5 . . . ?
Na2' O2W Na2' O1W -42.6(5) 3 . . . ?
Na2' O2W Na2' O5W -129.6(9) 5 . . 8_556 ?
Na2' O2W Na2' O5W 145.2(10) 3 . . 8_556 ?
Na2' O2W Na2' Na2' 85.1(11) 5 . . 3 ?
Na2' O2W Na2' Na2' -85.1(11) 3 . . 5 ?
Na2' O2W Na2' Na1 -100.8(7) 5 . . 8_556 ?
Na2' O2W Na2' Na1 174.1(7) 3 . . 8_556 ?
W1 O1 Na2' O2W -28.2(19) . . . . ?
Na2 O1 Na2' O2W -138.9(16) . . . . ?
W1 O1 Na2' O4 176.3(12) . . . 5 ?
Na2 O1 Na2' O4 65.6(11) . . . 5 ?
W1 O1 Na2' O1W 61.1(16) . . . . ?
Na2 O1 Na2' O1W -49.6(11) . . . . ?
W1 O1 Na2' O5W -107.7(16) . . . 8_556 ?
Na2 O1 Na2' O5W 141.6(14) . . . 8_556 ?
W1 O1 Na2' Na2' 7.5(14) . . . 3 ?
Na2 O1 Na2' Na2' -103.1(11) . . . 3 ?
W1 O1 Na2' Na2' 17.6(18) . . . 5 ?
Na2 O1 Na2' Na2' -93.0(11) . . . 5 ?
W1 O1 Na2' Na1 -127.2(14) . . . 8_556 ?
Na2 O1 Na2' Na1 122.2(13) . . . 8_556 ?
Na2 O1W Na2' O2W -50.7(7) 5 . . . ?
Na2 O1W Na2' O2W 178.6(14) . . . . ?
Na2 O1W Na2' O2W 49.8(6) 3 . . . ?
Na2' O1W Na2' O2W 37.1(2) 3 . . . ?
Na2' O1W Na2' O2W -37.1(2) 5 . . . ?
Na2 O1W Na2' O1 -156.0(7) 5 . . . ?
Na2 O1W Na2' O1 73.3(12) . . . . ?
Na2 O1W Na2' O1 -55.5(7) 3 . . . ?
Na2' O1W Na2' O1 -68.2(7) 3 . . . ?
Na2' O1W Na2' O1 -142.4(5) 5 . . . ?
Na2 O1W Na2' O4 75.5(8) 5 . . 5 ?
Na2 O1W Na2' O4 -55.2(11) . . . 5 ?
Na2 O1W Na2' O4 176.1(7) 3 . . 5 ?
Na2' O1W Na2' O4 163.3(6) 3 . . 5 ?
Na2' O1W Na2' O4 89.2(8) 5 . . 5 ?
Na2 O1W Na2' O5W -21(3) 5 . . 8_556 ?
Na2 O1W Na2' O5W -152(4) . . . 8_556 ?
Na2 O1W Na2' O5W 79(3) 3 . . 8_556 ?
Na2' O1W Na2' O5W 66(3) 3 . . 8_556 ?
Na2' O1W Na2' O5W -8(3) 5 . . 8_556 ?
Na2 O1W Na2' Na2' -87.8(8) 5 . . 3 ?
Na2 O1W Na2' Na2' 141.5(14) . . . 3 ?
Na2 O1W Na2' Na2' 12.8(6) 3 . . 3 ?
Na2' O1W Na2' Na2' -74.1(5) 5 . . 3 ?
Na2 O1W Na2' Na2' -13.6(6) 5 . . 5 ?
Na2 O1W Na2' Na2' -144.3(14) . . . 5 ?
Na2 O1W Na2' Na2' 86.9(8) 3 . . 5 ?
Na2' O1W Na2' Na2' 74.1(5) 3 . . 5 ?
Na2 O1W Na2' Na1 35.5(14) 5 . . 8_556 ?
Na2 O1W Na2' Na1 -95.2(16) . . . 8_556 ?
Na2 O1W Na2' Na1 136.0(8) 3 . . 8_556 ?
Na2' O1W Na2' Na1 123.3(8) 3 . . 8_556 ?
Na2' O1W Na2' Na1 49.1(12) 5 . . 8_556 ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N2 H2A O9 0.86 2.34 3.106(17) 148.7 5
O2W H2WA O4W 0.85 2.48 2.86(4) 108.3 .
O4W H4WA O1 0.84 2.56 3.187(17) 132.8 10_556

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        28.35
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         1.642
_refine_diff_density_min         -2.071
_refine_diff_density_rms         0.248
_database_code_depnum_ccdc_archive 'CCDC 1009128'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  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.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_ljm0015_0m

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C6 H37 As2 Mn3 N9 Na9 O78.5 W18'
_chemical_formula_sum            'C6 H37 As2 Mn3 N9 Na9 O78.5 W18'
_chemical_formula_weight         5322.10

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'
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'
Na Na 0.0362 0.0249 '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'
As As 0.0499 2.0058 '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           Hexagonal
_symmetry_space_group_name_H-M   P6(3)/m
_symmetry_space_group_name_Hall  '-P 6c'
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'-x, -y, z+1/2'
'y, -x+y, z+1/2'
'x-y, x, z+1/2'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'x, y, -z-1/2'
'-y, x-y, -z-1/2'
'-x+y, -x, -z-1/2'

_cell_length_a                   13.9494(8)
_cell_length_b                   13.9494(8)
_cell_length_c                   33.760(4)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_volume                     5689.1(8)
_cell_formula_units_Z            2
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    7098
_cell_measurement_theta_min      2.41
_cell_measurement_theta_max      27.87

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_exptl_crystal_density_meas      0
_exptl_crystal_density_diffrn    3.107
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             4672.0
_exptl_absorpt_coefficient_mu    19.130
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.0392
_exptl_absorpt_correction_T_max  0.0501
_exptl_absorpt_process_details   
'Higashi, T. (1995). Program for Absorption Correction. Rigaku Corporation, Tokyo, Japan.'

_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            40694
_diffrn_reflns_av_R_equivalents  0.0861
_diffrn_reflns_av_unetI/netI     0.0466
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -44
_diffrn_reflns_limit_l_max       45
_diffrn_reflns_theta_min         2.41
_diffrn_reflns_theta_max         28.32
_reflns_number_total             4819
_reflns_number_gt                3571
_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 F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0942P)²+479.0081P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     SHELXL
_refine_ls_extinction_coef       0.00007(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         4819
_refine_ls_number_parameters     187
_refine_ls_number_restraints     28
_refine_ls_R_factor_all          0.0682
_refine_ls_R_factor_gt           0.0433
_refine_ls_wR_factor_ref         0.1190
_refine_ls_wR_factor_gt          0.1012
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_restrained_S_all      1.043
_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
W1 W 0.05563(7) 0.44628(7) 0.34419(2) 0.0236(2) Uani 1 1 d . . .
W2 W 0.12521(7) 0.73788(7) 0.34391(2) 0.0231(2) Uani 1 1 d . . .
W3 W 0.28068(7) 0.78758(7) 0.42738(2) 0.0260(3) Uani 1 1 d . . .
As1 As 0.3333 0.6667 0.33221(12) 0.0271(7) Uani 1 3 d S . .
Mn1 Mn 0.0847(4) 0.5901(4) 0.2500 0.0239(9) Uani 1 2 d S . .
N1 N -0.097(2) 0.549(3) 0.2500 0.062(10) Uani 1 2 d SD . .
C2 C -0.147(2) 0.535(3) 0.2834(7) 0.062(9) Uani 1 1 d D . .
H2 H -0.1232 0.5379 0.3092 0.074 Uiso 1 1 calc R . .
N2 N -0.2409(19) 0.517(3) 0.2699(10) 0.086(11) Uani 1 1 d D . .
H2A H -0.2962 0.5058 0.2844 0.104 Uiso 1 1 calc R . .
O10 O 0.2441(13) 0.5400(13) 0.3580(5) 0.0271(7) Uani 1 1 d . . .
O6 O 0.1055(12) 0.3384(11) 0.3400(4) 0.022(3) Uani 1 1 d . . .
O8 O 0.1474(13) 0.7144(13) 0.2935(4) 0.029(3) Uani 1 1 d . . .
O15 O 0.3605(14) 0.9272(13) 0.4026(4) 0.027(3) Uani 1 1 d . . .
O13 O 0.1477(14) 0.7636(14) 0.4025(5) 0.031(3) Uani 1 1 d . . .
O11 O 0.0648(12) 0.5854(12) 0.3569(5) 0.025(3) Uani 1 1 d . . .
O14 O 0.2136(15) 0.6282(14) 0.4336(4) 0.031(3) Uani 1 1 d . . .
O7 O 0.0906(14) 0.4865(14) 0.2938(5) 0.030(3) Uani 1 1 d U . .
O9 O -0.0858(13) 0.3583(14) 0.3429(5) 0.036(4) Uani 1 1 d . . .
O12 O 0.0054(15) 0.7455(16) 0.3420(6) 0.042(4) Uani 1 1 d . . .
O4 O 0.2623(16) 0.8241(17) 0.4743(5) 0.043(4) Uani 1 1 d . . .
Na1 Na 0.1307(10) 0.3741(10) 0.2500 0.0271(7) Uani 1 2 d SU . .
O1W O 1.0000 1.0000 0.3924(16) 0.066(12) Uani 1 3 d S . .
H1WA H 1.0120 0.9615 0.3758 0.079 Uiso 0.33 1 d PR . .
H1WB H 0.9802 0.9764 0.4159 0.079 Uiso 0.33 1 d PR . .
O3W O -0.003(3) 0.434(3) 0.5688(12) 0.043(9) Uani 0.50 1 d P . .
H3WA H 0.0124 0.5014 0.5664 0.052 Uiso 0.50 1 d PR . .
H3WB H -0.0705 0.3834 0.5710 0.052 Uiso 0.50 1 d PR . .
O2W O 0.149(3) 0.036(3) 0.340(2) 0.17(3) Uani 1 1 d . . .
H2WA H 0.1583 0.0100 0.3610 0.208 Uiso 1 1 d R . .
H2WB H 0.1412 0.0018 0.3178 0.208 Uiso 1 1 d R . .
Na2 Na 0.1595(7) 0.6150(7) 0.5221(3) 0.0271(7) Uani 1 1 d . . .
O5 O 0.004(5) 0.217(5) 0.2500 0.043(6) Uani 0.50 2 d SPU . .
H5A H -0.0403 0.1881 0.2693 0.051 Uiso 0.25 1 d PR . .
H5B H 0.0031 0.1777 0.2307 0.051 Uiso 0.25 1 d PR . .


_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. 
;

# SQUEEZE RESULTS (APPEND TO CIF) 
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
1 0.000 0.000 0.000 10.3 2.8
2 -0.002 0.790 0.250 13.2 6.6
3 0.000 0.000 0.500 10.3 3.1
4 0.002 0.210 0.750 13.2 5.6
5 0.333 0.667 0.532 166.6 56.3
6 0.333 0.667 0.968 167.1 57.1
7 0.209 0.207 0.250 13.1 6.4
8 0.207 -0.002 0.750 13.1 5.6
9 0.667 0.333 0.032 166.6 57.8
10 0.667 0.333 0.468 167.1 55.5
11 0.333 0.667 0.657 23.1 2.3
12 0.333 0.667 0.843 22.3 3.6
13 0.667 0.333 0.157 23.1 4.6
14 0.667 0.333 0.343 22.3 5.9
15 0.792 0.002 0.250 13.2 6.4
16 0.790 0.792 0.750 13.1 5.7
_platon_squeeze_details          
; ? 
;

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 O9 1.726(16) . ?
W1 O7 1.782(17) . ?
W1 O11 1.929(14) . ?
W1 O6 1.954(14) . ?
W1 O15 2.006(15) 2_665 ?
W1 O10 2.325(15) . ?
W2 O12 1.729(16) . ?
W2 O8 1.790(15) . ?
W2 O11 1.906(14) . ?
W2 O6 1.940(15) 3_565 ?
W2 O13 2.008(15) . ?
W2 O10 2.315(15) 3_565 ?
W2 Na1 3.620(6) 3_565 ?
W3 O4 1.720(17) . ?
W3 O15 1.888(16) . ?
W3 O14 1.888(17) 3_565 ?
W3 O13 1.907(17) . ?
W3 O14 1.945(17) . ?
W3 O10 2.411(15) 3_565 ?
As1 O10 1.798(16) 2_665 ?
As1 O10 1.798(16) . ?
As1 O10 1.798(16) 3_565 ?
Mn1 O7 2.098(16) 10_556 ?
Mn1 O7 2.098(16) . ?
Mn1 O8 2.100(16) . ?
Mn1 O8 2.100(16) 10_556 ?
Mn1 N1 2.31(3) . ?
Mn1 Na1 3.383(13) 3_565 ?
N1 C2 1.289(18) 10_556 ?
N1 C2 1.289(18) . ?
C2 N2 1.279(19) . ?
C2 H2 0.9300 . ?
N2 N2 1.34(7) 10_556 ?
N2 H2A 0.8600 . ?
O10 W2 2.315(15) 2_665 ?
O10 W3 2.411(15) 2_665 ?
O6 W2 1.940(14) 2_665 ?
O8 Na1 2.392(19) 3_565 ?
O15 W1 2.006(15) 3_565 ?
O14 W3 1.888(17) 2_665 ?
O7 Na1 2.415(18) . ?
O4 Na2 3.00(2) . ?
Na1 O5 2.01(6) . ?
Na1 O8 2.392(19) 2_665 ?
Na1 O8 2.392(19) 11_666 ?
Na1 O7 2.415(18) 10_556 ?
Na1 Mn1 3.383(13) 2_665 ?
Na1 W2 3.620(6) 2_665 ?
Na1 W2 3.620(6) 11_666 ?
Na1 W1 3.644(6) 10_556 ?
Na1 H5A 2.5808 . ?
Na1 H5B 2.4948 . ?
O1W H1WA 0.8502 . ?
O1W H1WB 0.8497 . ?
O3W Na2 2.88(4) . ?
O3W H3WA 0.8500 . ?
O3W H3WB 0.8500 . ?
O2W H2WA 0.8498 . ?
O2W H2WB 0.8501 . ?
Na2 Na2 3.735(15) 3_565 ?
Na2 Na2 3.735(15) 2_665 ?
Na2 H3WA 2.3901 . ?
O5 H5A 0.8500 . ?
O5 H5B 0.8500 . ?

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 W1 O7 103.6(8) . . ?
O9 W1 O11 101.4(8) . . ?
O7 W1 O11 91.5(7) . . ?
O9 W1 O6 99.9(8) . . ?
O7 W1 O6 91.5(6) . . ?
O11 W1 O6 157.1(6) . . ?
O9 W1 O15 96.1(7) . 2_665 ?
O7 W1 O15 160.3(7) . 2_665 ?
O11 W1 O15 85.4(6) . 2_665 ?
O6 W1 O15 84.1(6) . 2_665 ?
O9 W1 O10 167.0(7) . . ?
O7 W1 O10 87.7(7) . . ?
O11 W1 O10 84.4(6) . . ?
O6 W1 O10 73.1(6) . . ?
O15 W1 O10 72.6(6) 2_665 . ?
O12 W2 O8 103.8(8) . . ?
O12 W2 O11 100.1(8) . . ?
O8 W2 O11 92.1(7) . . ?
O12 W2 O6 99.0(8) . 3_565 ?
O8 W2 O6 91.9(7) . 3_565 ?
O11 W2 O6 159.0(6) . 3_565 ?
O12 W2 O13 95.4(8) . . ?
O8 W2 O13 160.8(7) . . ?
O11 W2 O13 85.1(7) . . ?
O6 W2 O13 84.4(7) 3_565 . ?
O12 W2 O10 167.0(8) . 3_565 ?
O8 W2 O10 87.3(6) . 3_565 ?
O11 W2 O10 86.0(6) . 3_565 ?
O6 W2 O10 73.6(6) 3_565 3_565 ?
O13 W2 O10 73.6(6) . 3_565 ?
O12 W2 Na1 98.4(7) . 3_565 ?
O8 W2 Na1 35.2(5) . 3_565 ?
O11 W2 Na1 127.0(5) . 3_565 ?
O6 W2 Na1 58.0(5) 3_565 3_565 ?
O13 W2 Na1 141.4(5) . 3_565 ?
O10 W2 Na1 86.7(4) 3_565 3_565 ?
O4 W3 O15 101.5(8) . . ?
O4 W3 O14 101.2(8) . 3_565 ?
O15 W3 O14 89.0(7) . 3_565 ?
O4 W3 O13 100.4(8) . . ?
O15 W3 O13 90.4(7) . . ?
O14 W3 O13 158.0(6) 3_565 . ?
O4 W3 O14 100.4(8) . . ?
O15 W3 O14 157.8(6) . . ?
O14 W3 O14 83.7(10) 3_565 . ?
O13 W3 O14 88.7(7) . . ?
O4 W3 O10 170.8(8) . 3_565 ?
O15 W3 O10 72.5(6) . 3_565 ?
O14 W3 O10 85.9(6) 3_565 3_565 ?
O13 W3 O10 73.0(6) . 3_565 ?
O14 W3 O10 86.1(6) . 3_565 ?
O10 As1 O10 98.5(7) 2_665 . ?
O10 As1 O10 98.5(7) 2_665 3_565 ?
O10 As1 O10 98.5(7) . 3_565 ?
O7 Mn1 O7 89.6(9) 10_556 . ?
O7 Mn1 O8 156.6(7) 10_556 . ?
O7 Mn1 O8 86.1(6) . . ?
O7 Mn1 O8 86.1(6) 10_556 10_556 ?
O7 Mn1 O8 156.6(7) . 10_556 ?
O8 Mn1 O8 88.7(9) . 10_556 ?
O7 Mn1 N1 104.3(9) 10_556 . ?
O7 Mn1 N1 104.3(9) . . ?
O8 Mn1 N1 99.0(9) . . ?
O8 Mn1 N1 99.0(9) 10_556 . ?
O7 Mn1 Na1 124.4(5) 10_556 3_565 ?
O7 Mn1 Na1 124.4(5) . 3_565 ?
O8 Mn1 Na1 44.5(4) . 3_565 ?
O8 Mn1 Na1 44.5(4) 10_556 3_565 ?
N1 Mn1 Na1 106.9(11) . 3_565 ?
C2 N1 C2 122(3) 10_556 . ?
C2 N1 Mn1 119.1(14) 10_556 . ?
C2 N1 Mn1 119.1(14) . . ?
N2 C2 N1 98.2(18) . . ?
N2 C2 H2 130.9 . . ?
N1 C2 H2 130.9 . . ?
C2 N2 N2 110.8(15) . 10_556 ?
C2 N2 H2A 124.5 . . ?
N2 N2 H2A 124.7 10_556 . ?
As1 O10 W2 117.7(7) . 2_665 ?
As1 O10 W1 119.2(7) . . ?
W2 O10 W1 93.1(6) 2_665 . ?
As1 O10 W3 132.9(8) . 2_665 ?
W2 O10 W3 92.3(5) 2_665 2_665 ?
W1 O10 W3 92.3(5) . 2_665 ?
W2 O6 W1 119.7(7) 2_665 . ?
W2 O8 Mn1 141.0(9) . . ?
W2 O8 Na1 119.2(8) . 3_565 ?
Mn1 O8 Na1 97.5(6) . 3_565 ?
W3 O15 W1 122.6(8) . 3_565 ?
W3 O13 W2 121.1(8) . . ?
W2 O11 W1 147.2(9) . . ?
W3 O14 W3 152.6(10) 2_665 . ?
W1 O7 Mn1 142.3(9) . . ?
W1 O7 Na1 119.8(8) . . ?
Mn1 O7 Na1 96.7(7) . . ?
W3 O4 Na2 106.1(9) . . ?
O5 Na1 O8 121.7(12) . 2_665 ?
O5 Na1 O8 121.7(12) . 11_666 ?
O8 Na1 O8 75.7(8) 2_665 11_666 ?
O5 Na1 O7 110.1(13) . 10_556 ?
O8 Na1 O7 128.0(8) 2_665 10_556 ?
O8 Na1 O7 82.2(6) 11_666 10_556 ?
O5 Na1 O7 110.1(13) . . ?
O8 Na1 O7 82.2(6) 2_665 . ?
O8 Na1 O7 128.0(8) 11_666 . ?
O7 Na1 O7 75.5(8) 10_556 . ?
O5 Na1 Mn1 135.0(16) . 2_665 ?
O8 Na1 Mn1 38.0(4) 2_665 2_665 ?
O8 Na1 Mn1 38.0(4) 11_666 2_665 ?
O7 Na1 Mn1 105.1(5) 10_556 2_665 ?
O7 Na1 Mn1 105.1(5) . 2_665 ?
O5 Na1 W2 101.7(7) . 2_665 ?
O8 Na1 W2 25.6(4) 2_665 2_665 ?
O8 Na1 W2 99.9(5) 11_666 2_665 ?
O7 Na1 W2 141.1(6) 10_556 2_665 ?
O7 Na1 W2 72.9(4) . 2_665 ?
Mn1 Na1 W2 63.06(18) 2_665 2_665 ?
O5 Na1 W2 101.7(7) . 11_666 ?
O8 Na1 W2 99.9(5) 2_665 11_666 ?
O8 Na1 W2 25.6(4) 11_666 11_666 ?
O7 Na1 W2 72.9(4) 10_556 11_666 ?
O7 Na1 W2 141.1(6) . 11_666 ?
Mn1 Na1 W2 63.06(18) 2_665 11_666 ?
W2 Na1 W2 122.3(3) 2_665 11_666 ?
O5 Na1 W1 94.8(8) . 10_556 ?
O8 Na1 W1 140.9(6) 2_665 10_556 ?
O8 Na1 W1 72.8(4) 11_666 10_556 ?
O7 Na1 W1 25.1(4) 10_556 10_556 ?
O7 Na1 W1 99.4(5) . 10_556 ?
Mn1 Na1 W1 106.3(2) 2_665 10_556 ?
W2 Na1 W1 163.4(4) 2_665 10_556 ?
W2 Na1 W1 55.24(4) 11_666 10_556 ?
O5 Na1 H5A 15.9 . . ?
O8 Na1 H5A 114.4 2_665 . ?
O8 Na1 H5A 136.2 11_666 . ?
O7 Na1 H5A 114.2 10_556 . ?
O7 Na1 H5A 95.8 . . ?
Mn1 Na1 H5A 139.1 2_665 . ?
W2 Na1 H5A 91.2 2_665 . ?
W2 Na1 H5A 117.5 11_666 . ?
W1 Na1 H5A 104.4 10_556 . ?
O5 Na1 H5B 17.9 . . ?
O8 Na1 H5B 124.3 2_665 . ?
O8 Na1 H5B 104.1 11_666 . ?
O7 Na1 H5B 106.5 10_556 . ?
O7 Na1 H5B 127.1 . . ?
Mn1 Na1 H5B 123.9 2_665 . ?
W2 Na1 H5B 110.4 2_665 . ?
W2 Na1 H5B 83.8 11_666 . ?
W1 Na1 H5B 86.0 10_556 . ?
H5A Na1 H5B 33.7 . . ?
H1WA O1W H1WB 120.0 . . ?
Na2 O3W H3WA 47.9 . . ?
Na2 O3W H3WB 146.9 . . ?
H3WA O3W H3WB 120.0 . . ?
H2WA O2W H2WB 120.0 . . ?
O3W Na2 O4 158.7(8) . . ?
O3W Na2 Na2 142.6(8) . 3_565 ?
O4 Na2 Na2 52.5(4) . 3_565 ?
O3W Na2 Na2 99.8(7) . 2_665 ?
O4 Na2 Na2 101.5(4) . 2_665 ?
Na2 Na2 Na2 59.999(2) 3_565 2_665 ?
O3W Na2 H3WA 15.3 . . ?
O4 Na2 H3WA 144.8 . . ?
Na2 Na2 H3WA 141.2 3_565 . ?
Na2 Na2 H3WA 112.5 2_665 . ?
Na1 O5 H5A 123.9 . . ?
Na1 O5 H5B 115.5 . . ?
H5A O5 H5B 120.0 . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O2W H2WA O1W 0.85 2.39 2.59(7) 93.9 1_445
O3W H3WB O13 0.85 1.99 2.66(4) 134.8 7_566
O3W H3WB O14 0.85 1.93 2.61(4) 136.4 7_566
O3W H3WA O15 0.85 2.10 2.66(4) 122.6 8_456
O5 H5A O2W 0.85 2.61 3.28(7) 137.0 2
O1W H1WA O2W 0.85 2.05 2.59(7) 120.4 3_665
N2 H2A O9 0.86 2.40 3.15(4) 147.1 2_565
O5 H5A O6 0.85 3.16 3.42(3) 100.7 .

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        28.32
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         2.325
_refine_diff_density_min         -1.341
_refine_diff_density_rms         0.248
_database_code_depnum_ccdc_archive 'CCDC 1009129'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  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.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_ljm001410_0m

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C6 H34 As2 Co3 N9 Na9 O77 W18'
_chemical_formula_sum            'C6 H34 As2 Co3 N9 Na9 O77 W18'
_chemical_formula_weight         5307.06

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'
Na Na 0.0362 0.0249 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
As As 0.0499 2.0058 '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           Hexagonal
_symmetry_space_group_name_H-M   P6(3)/m
_symmetry_space_group_name_Hall  '-P 6c'
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'-x, -y, z+1/2'
'y, -x+y, z+1/2'
'x-y, x, z+1/2'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'x, y, -z-1/2'
'-y, x-y, -z-1/2'
'-x+y, -x, -z-1/2'

_cell_length_a                   13.9307(5)
_cell_length_b                   13.9307(5)
_cell_length_c                   33.554(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_volume                     5639.2(5)
_cell_formula_units_Z            2
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    8571
_cell_measurement_theta_min      2.43
_cell_measurement_theta_max      28.02

_exptl_crystal_description       block
_exptl_crystal_colour            blue
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.24
_exptl_crystal_density_meas      0
_exptl_crystal_density_diffrn    3.128
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             4649.0
_exptl_absorpt_coefficient_mu    19.403
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.0543
_exptl_absorpt_correction_T_max  0.0697
_exptl_absorpt_process_details   
'Higashi, T. (1995). Program for Absorption Correction. Rigaku Corporation, Tokyo, Japan.'

_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            40515
_diffrn_reflns_av_R_equivalents  0.0847
_diffrn_reflns_av_unetI/netI     0.0487
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -44
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_theta_min         2.43
_diffrn_reflns_theta_max         28.39
_reflns_number_total             4805
_reflns_number_gt                3650
_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 F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0550P)²+245.7718P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     SHELXL
_refine_ls_extinction_coef       0.00015(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         4805
_refine_ls_number_parameters     192
_refine_ls_number_restraints     25
_refine_ls_R_factor_all          0.0686
_refine_ls_R_factor_gt           0.0457
_refine_ls_wR_factor_ref         0.1013
_refine_ls_wR_factor_gt          0.0932
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_restrained_S_all      1.048
_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
As1 As 0.6667 0.3333 0.66884(7) 0.0183(4) Uani 1 3 d S . .
W1 W 0.44650(5) 0.05531(4) 0.656906(17) 0.02257(16) Uani 1 1 d . . .
W2 W 0.73798(5) 0.12479(5) 0.657044(17) 0.02241(16) Uani 1 1 d . . .
W3 W 0.78816(5) 0.28114(5) 0.573443(17) 0.02673(17) Uani 1 1 d . . .
Co1 Co 0.5906(2) 0.0865(2) 0.7500 0.0212(5) Uani 1 2 d S . .
Na1 Na 0.3806(6) 0.1341(6) 0.7500 0.0183(4) Uani 1 2 d SU . .
O1 O 0.7464(10) 0.0049(9) 0.6596(4) 0.040(3) Uani 1 1 d . . .
O2 O 0.3584(9) -0.0867(8) 0.6583(3) 0.035(3) Uani 1 1 d . . .
O3 O 0.7867(9) 0.4174(9) 0.5675(3) 0.031(2) Uani 1 1 d . . .
O4 O 0.3390(11) 0.1046(11) 0.6613(4) 0.0522(18) Uani 1 1 d . . .
O5 O 0.7536(7) 0.2946(7) 0.6424(3) 0.0201(18) Uani 1 1 d . . .
O6 O 0.5848(8) 0.0638(8) 0.6435(3) 0.026(2) Uani 1 1 d . . .
O7 O 0.8250(10) 0.2642(10) 0.5260(4) 0.041(3) Uani 1 1 d . . .
O8 O 0.9285(9) 0.3597(9) 0.5978(3) 0.032(2) Uani 1 1 d . . .
O9 O 0.7662(9) 0.1493(9) 0.5979(3) 0.033(2) Uani 1 1 d . . .
O10 O 0.4893(9) 0.0911(9) 0.7076(3) 0.029(2) Uani 1 1 d U . .
O11 O 0.7106(11) 0.1462(11) 0.7073(4) 0.0522(18) Uani 1 1 d . . .
C1 C 0.5351(17) -0.1422(14) 0.7178(7) 0.048(5) Uani 1 1 d . . .
H1 H 0.5388 -0.1203 0.6914 0.3(3) Uiso 1 1 calc R . .
N1 N 0.5472(15) -0.0787(14) 0.7500 0.032(4) Uani 1 2 d S . .
N2 N 0.5171(19) -0.2412(14) 0.72979(15) 0.085(7) Uani 1 1 d D . .
H2 H 0.5073 -0.2952 0.7146 0.00(5) Uiso 0.50 1 calc PR . .
O1W O 1.0000 0.0000 0.6087(11) 0.075(10) Uani 1 3 d S . .
H1WA H 0.9964 0.0517 0.5966 0.090 Uiso 0.33 1 d PR . .
H1WB H 1.0496 -0.0158 0.6024 0.090 Uiso 0.33 1 d PR . .
Na2 Na 0.8573(12) -0.1101(12) 0.6677(5) 0.0522(18) Uani 0.564(14) 1 d P . 2
O3W O 0.565(3) 0.994(3) 0.5690(13) 0.094(12) Uani 0.50 1 d PU A 2
H3WA H 0.5540 1.0312 0.5866 0.113 Uiso 0.50 1 d PR A 2
H3WB H 0.5841 1.0193 0.5456 0.113 Uiso 0.50 1 d PR A 2
Na2' Na 0.8344(14) -0.1237(15) 0.6368(6) 0.0522(18) Uani 0.436(14) 1 d P . 1
O2W O 0.178(4) 0.202(4) 0.7500 0.062(5) Uani 0.50 2 d SPU . .
O2W' O 0.217(4) 0.153(3) 0.7500 0.062(5) Uani 0.50 2 d SPU . .
H2WA H 0.1799 0.1424 0.7287 0.074 Uiso 0.50 1 d PR . .
H2WB H 0.1976 0.1721 0.7713 0.074 Uiso 0.50 1 d PR . .
O4W O 0.218(2) -0.015(2) 0.7500 0.094(6) Uani 1 2 d SU . .
H4WA H 0.1998 -0.0607 0.7692 0.113 Uiso 0.50 1 d PR . .
H4WB H 0.1726 -0.0284 0.7308 0.113 Uiso 0.50 1 d PR . .


_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. 
;

# SQUEEZE RESULTS (APPEND TO CIF) 
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
1 0.000 0.000 0.000 18.5 4.8
2 0.000 0.000 0.500 18.5 5.0
3 0.333 0.667 0.558 162.1 48.1
4 0.333 0.667 0.942 162.1 47.8
5 0.667 0.333 0.058 162.0 51.0
6 0.667 0.333 0.442 162.0 49.2
_platon_squeeze_details          
; ? 
;

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
As1 O5 1.789(9) 3_665 ?
As1 O5 1.789(9) . ?
As1 O5 1.789(9) 2_655 ?
W1 O2 1.730(10) . ?
W1 O10 1.789(10) . ?
W1 O6 1.924(10) . ?
W1 O4 1.940(14) . ?
W1 O8 2.021(11) 3_665 ?
W1 O5 2.357(9) 3_665 ?
W2 O1 1.734(10) . ?
W2 O11 1.785(14) . ?
W2 O6 1.915(10) . ?
W2 O4 1.953(14) 2_655 ?
W2 O9 2.019(11) . ?
W2 O5 2.318(9) . ?
W2 Na1 3.572(4) 2_655 ?
W3 O7 1.725(11) . ?
W3 O8 1.883(11) . ?
W3 O9 1.892(11) . ?
W3 O3 1.916(11) 3_665 ?
W3 O3 1.919(11) . ?
W3 O5 2.389(9) . ?
Co1 O10 2.027(10) . ?
Co1 O10 2.027(10) 10_557 ?
Co1 O11 2.038(14) 10_557 ?
Co1 O11 2.038(14) . ?
Co1 N1 2.067(18) . ?
Co1 Na1 3.336(8) 2_655 ?
Na1 O4W 2.18(3) . ?
Na1 O10 2.362(11) . ?
Na1 O10 2.362(11) 10_557 ?
Na1 O11 2.380(15) 12_667 ?
Na1 O11 2.380(15) 3_665 ?
Na1 O2W' 2.42(5) . ?
Na1 Co1 3.336(7) 3_665 ?
Na1 W2 3.572(3) 12_667 ?
Na1 W2 3.572(3) 3_665 ?
Na1 W1 3.579(3) 10_557 ?
O1 Na2' 2.74(2) . ?
O1 Na2 2.739(18) . ?
O3 W3 1.916(11) 2_655 ?
O4 W2 1.953(14) 3_665 ?
O4 Na2 2.79(2) 2_545 ?
O4 Na2' 2.78(2) 2_545 ?
O5 W1 2.357(9) 2_655 ?
O8 W1 2.021(11) 2_655 ?
O11 Na1 2.380(15) 2_655 ?
C1 N2 1.33(2) . ?
C1 N1 1.35(2) . ?
N1 C1 1.35(2) 10_557 ?
N2 N2 1.356(10) 10_557 ?
O1W Na2' 2.28(2) 3_765 ?
O1W Na2' 2.28(2) 2_645 ?
O1W Na2' 2.28(2) . ?
O1W Na2 2.68(3) 2_645 ?
O1W Na2 2.68(3) 3_765 ?
O1W Na2 2.68(3) . ?
Na2 O4 2.79(2) 3_655 ?
Na2 Na2 3.13(2) 2_645 ?
Na2 Na2 3.13(2) 3_765 ?
Na2' O4 2.78(2) 3_655 ?
Na2' Na2' 3.60(3) 3_765 ?
Na2' Na2' 3.60(3) 2_645 ?
O2W O2W' 1.06(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
O5 As1 O5 97.5(4) 3_665 . ?
O5 As1 O5 97.5(4) 3_665 2_655 ?
O5 As1 O5 97.5(4) . 2_655 ?
O2 W1 O10 103.9(5) . . ?
O2 W1 O6 101.1(5) . . ?
O10 W1 O6 91.2(4) . . ?
O2 W1 O4 99.8(6) . . ?
O10 W1 O4 92.2(5) . . ?
O6 W1 O4 157.3(5) . . ?
O2 W1 O8 95.7(5) . 3_665 ?
O10 W1 O8 160.3(5) . 3_665 ?
O6 W1 O8 85.5(4) . 3_665 ?
O4 W1 O8 83.7(5) . 3_665 ?
O2 W1 O5 166.7(4) . 3_665 ?
O10 W1 O5 87.8(4) . 3_665 ?
O6 W1 O5 84.6(4) . 3_665 ?
O4 W1 O5 73.1(5) . 3_665 ?
O8 W1 O5 72.6(4) 3_665 3_665 ?
O1 W2 O11 103.8(6) . . ?
O1 W2 O6 100.4(5) . . ?
O11 W2 O6 90.9(5) . . ?
O1 W2 O4 99.2(6) . 2_655 ?
O11 W2 O4 92.9(6) . 2_655 ?
O6 W2 O4 158.5(5) . 2_655 ?
O1 W2 O9 96.3(5) . . ?
O11 W2 O9 160.0(5) . . ?
O6 W2 O9 85.4(4) . . ?
O4 W2 O9 83.8(5) 2_655 . ?
O1 W2 O5 167.6(5) . . ?
O11 W2 O5 87.1(5) . . ?
O6 W2 O5 85.3(4) . . ?
O4 W2 O5 73.8(5) 2_655 . ?
O9 W2 O5 73.0(4) . . ?
O1 W2 Na1 99.0(4) . 2_655 ?
O11 W2 Na1 36.3(5) . 2_655 ?
O6 W2 Na1 126.8(3) . 2_655 ?
O4 W2 Na1 57.8(4) 2_655 2_655 ?
O9 W2 Na1 140.3(3) . 2_655 ?
O5 W2 Na1 86.0(3) . 2_655 ?
O7 W3 O8 100.7(5) . . ?
O7 W3 O9 100.5(5) . . ?
O8 W3 O9 89.6(5) . . ?
O7 W3 O3 100.5(5) . 3_665 ?
O8 W3 O3 158.7(4) . 3_665 ?
O9 W3 O3 88.7(5) . 3_665 ?
O7 W3 O3 101.0(5) . . ?
O8 W3 O3 89.5(5) . . ?
O9 W3 O3 158.3(4) . . ?
O3 W3 O3 84.3(6) 3_665 . ?
O7 W3 O5 171.8(5) . . ?
O8 W3 O5 74.1(4) . . ?
O9 W3 O5 73.4(4) . . ?
O3 W3 O5 85.0(4) 3_665 . ?
O3 W3 O5 85.5(4) . . ?
O10 Co1 O10 89.2(6) . 10_557 ?
O10 Co1 O11 157.4(5) . 10_557 ?
O10 Co1 O11 86.3(5) 10_557 10_557 ?
O10 Co1 O11 86.3(5) . . ?
O10 Co1 O11 157.4(5) 10_557 . ?
O11 Co1 O11 89.4(8) 10_557 . ?
O10 Co1 N1 102.4(5) . . ?
O10 Co1 N1 102.4(5) 10_557 . ?
O11 Co1 N1 100.2(5) 10_557 . ?
O11 Co1 N1 100.2(5) . . ?
O10 Co1 Na1 124.4(3) . 2_655 ?
O10 Co1 Na1 124.4(3) 10_557 2_655 ?
O11 Co1 Na1 45.0(4) 10_557 2_655 ?
O11 Co1 Na1 45.0(4) . 2_655 ?
N1 Co1 Na1 110.0(5) . 2_655 ?
O4W Na1 O10 104.7(7) . . ?
O4W Na1 O10 104.7(7) . 10_557 ?
O10 Na1 O10 74.0(5) . 10_557 ?
O4W Na1 O11 125.0(7) . 12_667 ?
O10 Na1 O11 129.6(5) . 12_667 ?
O10 Na1 O11 85.0(4) 10_557 12_667 ?
O4W Na1 O11 125.0(7) . 3_665 ?
O10 Na1 O11 85.0(4) . 3_665 ?
O10 Na1 O11 129.6(5) 10_557 3_665 ?
O11 Na1 O11 74.1(7) 12_667 3_665 ?
O4W Na1 O2W' 61.0(13) . . ?
O10 Na1 O2W' 141.7(4) . . ?
O10 Na1 O2W' 141.7(4) 10_557 . ?
O11 Na1 O2W' 78.0(9) 12_667 . ?
O11 Na1 O2W' 78.0(9) 3_665 . ?
O4W Na1 Co1 140.2(9) . 3_665 ?
O10 Na1 Co1 106.9(3) . 3_665 ?
O10 Na1 Co1 106.9(3) 10_557 3_665 ?
O11 Na1 Co1 37.3(4) 12_667 3_665 ?
O11 Na1 Co1 37.3(4) 3_665 3_665 ?
O2W' Na1 Co1 79.1(10) . 3_665 ?
O4W Na1 W2 103.2(4) . 12_667 ?
O10 Na1 W2 142.5(3) . 12_667 ?
O10 Na1 W2 75.1(3) 10_557 12_667 ?
O11 Na1 W2 26.4(3) 12_667 12_667 ?
O11 Na1 W2 99.0(4) 3_665 12_667 ?
O2W' Na1 W2 74.6(4) . 12_667 ?
Co1 Na1 W2 63.18(10) 3_665 12_667 ?
O4W Na1 W2 103.2(4) . 3_665 ?
O10 Na1 W2 75.1(3) . 3_665 ?
O10 Na1 W2 142.5(3) 10_557 3_665 ?
O11 Na1 W2 99.0(4) 12_667 3_665 ?
O11 Na1 W2 26.4(3) 3_665 3_665 ?
O2W' Na1 W2 74.6(4) . 3_665 ?
Co1 Na1 W2 63.18(10) 3_665 3_665 ?
W2 Na1 W2 121.7(2) 12_667 3_665 ?
O4W Na1 W1 90.7(4) . 10_557 ?
O10 Na1 W1 98.8(3) . 10_557 ?
O10 Na1 W1 26.1(2) 10_557 10_557 ?
O11 Na1 W1 74.8(3) 12_667 10_557 ?
O11 Na1 W1 142.1(4) 3_665 10_557 ?
O2W' Na1 W1 115.7(3) . 10_557 ?
Co1 Na1 W1 107.62(12) 3_665 10_557 ?
W2 Na1 W1 56.29(2) 12_667 10_557 ?
W2 Na1 W1 165.7(2) 3_665 10_557 ?
W2 O1 Na2' 152.3(8) . . ?
W2 O1 Na2 153.9(7) . . ?
W3 O3 W3 152.4(6) 2_655 . ?
W1 O4 W2 120.1(7) . 3_665 ?
W1 O4 Na2 125.7(7) . 2_545 ?
W2 O4 Na2 114.0(7) 3_665 2_545 ?
W1 O4 Na2' 117.3(7) . 2_545 ?
W2 O4 Na2' 116.2(7) 3_665 2_545 ?
As1 O5 W2 118.0(4) . . ?
As1 O5 W1 117.8(4) . 2_655 ?
W2 O5 W1 92.4(3) . 2_655 ?
As1 O5 W3 134.3(5) . . ?
W2 O5 W3 92.6(3) . . ?
W1 O5 W3 91.8(3) 2_655 . ?
W2 O6 W1 146.2(5) . . ?
W3 O8 W1 121.5(5) . 2_655 ?
W3 O9 W2 120.9(5) . . ?
W1 O10 Co1 143.0(6) . . ?
W1 O10 Na1 118.5(5) . . ?
Co1 O10 Na1 97.5(4) . . ?
W2 O11 Co1 142.8(8) . . ?
W2 O11 Na1 117.3(7) . 2_655 ?
Co1 O11 Na1 97.8(6) . 2_655 ?
N2 C1 N1 109.5(18) . . ?
C1 N1 C1 106(2) . 10_557 ?
C1 N1 Co1 126.9(11) . . ?
C1 N1 Co1 126.9(11) 10_557 . ?
C1 N2 N2 107.5(10) . 10_557 ?
Na2' O1W Na2' 104.1(11) 3_765 2_645 ?
Na2' O1W Na2' 104.1(11) 3_765 . ?
Na2' O1W Na2' 104.1(11) 2_645 . ?
Na2' O1W Na2 89.3(12) 3_765 2_645 ?
Na2' O1W Na2 90.9(12) . 2_645 ?
Na2' O1W Na2 90.9(12) 2_645 3_765 ?
Na2' O1W Na2 89.3(12) . 3_765 ?
Na2 O1W Na2 71.4(10) 2_645 3_765 ?
Na2' O1W Na2 90.9(12) 3_765 . ?
Na2' O1W Na2 89.3(12) 2_645 . ?
Na2 O1W Na2 71.4(10) 2_645 . ?
Na2 O1W Na2 71.4(10) 3_765 . ?
O1W Na2 O1 93.8(5) . . ?
O1W Na2 O4 112.4(7) . 3_655 ?
O1 Na2 O4 126.3(7) . 3_655 ?
O1W Na2 Na2 54.3(5) . 2_645 ?
O1 Na2 Na2 131.7(6) . 2_645 ?
O4 Na2 Na2 100.8(7) 3_655 2_645 ?
O1W Na2 Na2 54.3(5) . 3_765 ?
O1 Na2 Na2 72.1(6) . 3_765 ?
O4 Na2 Na2 160.4(7) 3_655 3_765 ?
Na2 Na2 Na2 60.000(4) 2_645 3_765 ?
O1W Na2' O1 103.6(7) . . ?
O1W Na2' O4 127.6(8) . 3_655 ?
O1 Na2' O4 126.8(8) . 3_655 ?
O1W Na2' Na2' 37.9(6) . 3_765 ?
O1 Na2' Na2' 68.8(7) . 3_765 ?
O4 Na2' Na2' 149.3(7) 3_655 3_765 ?
O1W Na2' Na2' 37.9(6) . 2_645 ?
O1 Na2' Na2' 126.2(7) . 2_645 ?
O4 Na2' Na2' 93.9(8) 3_655 2_645 ?
Na2' Na2' Na2' 60.000(4) 3_765 2_645 ?
O2W O2W' Na1 152(4) . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N2 H2 O2 0.86 2.32 3.092(16) 149.7 3_655

_diffrn_measured_fraction_theta_max 0.996
_diffrn_reflns_theta_full        28.39
_diffrn_measured_fraction_theta_full 0.996
_refine_diff_density_max         2.066
_refine_diff_density_min         -1.414
_refine_diff_density_rms         0.212
_database_code_depnum_ccdc_archive 'CCDC 1009130'
