# Electronic Supplementary Material (ESI) for ChemComm.
# This journal is © The Royal Society of Chemistry 2014

data_global


# publcif _publ_body_element loop end

#==========================================================================

_audit_creation_method           'manual editing of SHELXL-97 file'

# PROCESSING SUMMARY (IUCr Office Use Only)

_journal_data_validation_number  ?

_journal_date_recd_electronic    ?
_journal_date_to_coeditor        ?
_journal_date_from_coeditor      ?
_journal_date_accepted           ?
_journal_date_printers_first     ?
_journal_date_printers_final     ?
_journal_date_proofs_out         ?
_journal_date_proofs_in          ?
_journal_coeditor_name           ?
_journal_coeditor_code           ?
_journal_coeditor_notes          
?
_journal_techeditor_code         ?
_iucr_compatibility_tag          ?
_journal_techeditor_notes        
?
_journal_coden_ASTM              ?
_journal_name_full               ?
_journal_year                    ?
_journal_volume                  ?
_journal_issue                   ?
_journal_page_first              ?
_journal_page_last               ?
_journal_paper_category          ?
_journal_suppl_publ_number       ?
_journal_suppl_publ_pages        ?

#===========================================================================

# SUBMISSION DETAILS

_publ_contact_author_name        'Maxim N. Sokolov'
_publ_contact_author_address     
;Nikolaev Institute of Inorganic Chemistry SB RAS
630090 Novosibirsk 
Russia
;
_publ_contact_author_email       caesar@niic.nsc.ru
_publ_contact_author_phone       '+7-383-316-58-45'
_publ_contact_author_fax         '+7-383-330-94-89'
_publ_requested_journal              
;
Chemical Communications
;
_publ_requested_category             
;
Communication
;

# TITLE AND AUTHOR LIST

_publ_section_title
;
An Ir(IV)-containing Polyoxometalate; 
;
_publ_section_title_footnote
; ?
;        
loop_
_publ_author_name
_publ_author_address
'Adonin, Sergey A.'
;
Nikolaev Institute of Inorganic Chemistry SB RAS
630090 Novosibirsk
Russia
;
'Izarova, Natalya V.'
;
Peter Gruenberg Institute � PGI 6
Forschungszentrum Juelich
D-52425 Juelich
Germany
;
'Besson, Claire'
;
Peter Gruenberg Institute � PGI 6
Forschungszentrum Juelich
D-52425 Juelich
Germany
;
'Abramov, Pavel A.'
;
Nikolaev Institute of Inorganic Chemistry SB RAS
630090 Novosibirsk
Russia
;
'Koegerler, Paul'
;
Institute of Inorganic Chemistry
RWTH Aachen University
D-52074 Aachen
Germany
;
'Fedin, Vladimir P.'
;
Nikolaev Institute of Inorganic Chemistry SB RAS
630090 Novosibirsk
Russia
;
'Sokolov, Maxim N.'
;
Nikolaev Institute of Inorganic Chemistry SB RAS
630090 Novosibirsk
Russia
;

 
data_IrW6 
  
_audit_creation_method            SHELXL-97 
_chemical_name_systematic 
; 
 ? 
; 
_chemical_name_common             ? 
_chemical_melting_point           ? 
_chemical_formula_moiety          ? 
_chemical_formula_sum 
 'H52 Ir Na8 O50 W6' 
_chemical_formula_weight          2331.64 
  
loop_ 
 _atom_type_symbol 
 _atom_type_description 
 _atom_type_scat_dispersion_real 
 _atom_type_scat_dispersion_imag 
 _atom_type_scat_source 
 'O'  'O'   0.0492   0.0322 
 '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'   0.1353   0.1239 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'W'  'W'  -5.4734   5.5774 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'Ir'  'Ir'  -4.7710   6.5667 
 '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                    10.7874(2) 
_cell_length_b                    11.7736(2) 
_cell_length_c                    17.9983(3) 
_cell_angle_alpha                 90.00 
_cell_angle_beta                  93.574(2) 
_cell_angle_gamma                 90.00 
_cell_volume                      2281.46(7) 
_cell_formula_units_Z             2 
_cell_measurement_temperature     120(2) 
_cell_measurement_reflns_used     14236 
_cell_measurement_theta_min       3.7670 
_cell_measurement_theta_max       73.3820  
  
_exptl_crystal_description        block 
_exptl_crystal_colour             green 
_exptl_crystal_size_max           0.68 
_exptl_crystal_size_mid           0.28 
_exptl_crystal_size_min           0.09 
_exptl_crystal_density_meas       ? 
_exptl_crystal_density_diffrn     3.394 
_exptl_crystal_density_method     'not measured' 
_exptl_crystal_F_000              2122 
_exptl_absorpt_coefficient_mu     34.588 
_exptl_absorpt_correction_type    analytical 
_exptl_absorpt_correction_T_min   0.0066 
_exptl_absorpt_correction_T_max   0.1508 
_exptl_absorpt_process_details    
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
Analytical numeric absorption correction using a multifaceted crystal
			model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
;
_exptl_special_details 
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
Analytical numeric absorption correction using a multifaceted crystal
			model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
;
  
_diffrn_ambient_temperature       120(2) 
_diffrn_radiation_wavelength      1.54178 
_diffrn_radiation_type            CuK\a 
_diffrn_radiation_source          'SuperNova (Cu) X-ray Source' 
_diffrn_radiation_monochromator   'mirror' 
_diffrn_measurement_device_type   'SuperNova, Dual, Cu at zero, Atlas' 
_diffrn_measurement_method        'φ and ω scans' 
_diffrn_detector_area_resol_mean  10.4623 
_diffrn_reflns_number             13283 
_diffrn_reflns_av_R_equivalents   0.0652 
_diffrn_reflns_av_sigmaI/netI     0.0376 
_diffrn_reflns_limit_h_min        -12 
_diffrn_reflns_limit_h_max        12 
_diffrn_reflns_limit_k_min        -10 
_diffrn_reflns_limit_k_max        14 
_diffrn_reflns_limit_l_min        -20 
_diffrn_reflns_limit_l_max        21 
_diffrn_reflns_theta_min          7.27 
_diffrn_reflns_theta_max          68.24 
_reflns_number_total              4163 
_reflns_number_gt                 4120 
_reflns_threshold_expression      >2sigma(I) 
  
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_structure_solution     'SHELXS-97 (Sheldrick, 2008)' 
_computing_structure_refinement   'SHELXL-97 (Sheldrick, 2008)'  
 
  
_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)+(0.1276P)²+54.6549P] where P=(Fo²+2Fc²)/3' 
_atom_sites_solution_primary      direct 
_atom_sites_solution_secondary    difmap 
_atom_sites_solution_hydrogens    notdet 
_refine_ls_hydrogen_treatment     ? 
_refine_ls_extinction_method      none 
_refine_ls_extinction_coef        ? 
_refine_ls_number_reflns          4163 
_refine_ls_number_parameters      230 
_refine_ls_number_restraints      42 
_refine_ls_R_factor_all           0.0671 
_refine_ls_R_factor_gt            0.0666 
_refine_ls_wR_factor_ref          0.1862 
_refine_ls_wR_factor_gt           0.1855 
_refine_ls_goodness_of_fit_ref    1.127 
_refine_ls_restrained_S_all       1.121 
_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 
Ir1 Ir 0.0000 0.5000 0.0000 0.0045(2) Uani 1 2 d S . . 
W1 W -0.09465(5) 0.25849(4) -0.06663(3) 0.0058(2) Uani 1 1 d . . . 
W2 W -0.06270(5) 0.29491(4) 0.11255(3) 0.0062(2) Uani 1 1 d . . . 
W3 W 0.04024(5) 0.53506(4) 0.17831(3) 0.0059(2) Uani 1 1 d . . . 
O1 O 0.0355(7) 0.3324(7) 0.0146(4) 0.0052(16) Uani 1 1 d U . . 
O1H O -0.0244(7) 0.1237(7) -0.0551(4) 0.0071(16) Uani 1 1 d U . . 
O1T O -0.2339(8) 0.2315(8) -0.1184(5) 0.0152(18) Uani 1 1 d . . . 
O2 O 0.1293(7) 0.5596(7) 0.0770(4) 0.0053(15) Uani 1 1 d U . . 
O2T O -0.1734(8) 0.2873(7) 0.1817(5) 0.0103(17) Uani 1 1 d U . . 
O2H O 0.0086(7) 0.1609(7) 0.1191(5) 0.0112(17) Uani 1 1 d . . . 
O3 O -0.0923(7) 0.4738(7) 0.0924(4) 0.0042(15) Uani 1 1 d U . . 
O3H O -0.0696(8) 0.5325(8) 0.2479(5) 0.0122(18) Uani 1 1 d . . . 
O3T O 0.1803(8) 0.5647(7) 0.2306(5) 0.0112(17) Uani 1 1 d . . . 
O12 O -0.1806(7) 0.2648(7) 0.0263(4) 0.0037(15) Uani 1 1 d U . . 
O13 O 0.0067(7) 0.3102(7) -0.1453(4) 0.0039(15) Uani 1 1 d U . . 
O23 O 0.0726(8) 0.3720(7) 0.1711(4) 0.0088(16) Uani 1 1 d . . . 
Na1 Na 0.1400(4) 0.0647(4) 0.0394(3) 0.0122(9) Uani 1 1 d . . . 
Na2 Na 0.0811(5) 0.0244(4) -0.1503(3) 0.0127(10) Uani 1 1 d . . . 
Na3 Na 0.5328(5) 0.5165(4) 0.1628(3) 0.0144(10) Uani 1 1 d . . . 
Na4 Na -0.6156(4) 0.2329(4) -0.0805(3) 0.0136(10) Uani 1 1 d . . . 
O1W O 0.2987(8) 0.2674(8) 0.1913(5) 0.0164(19) Uiso 1 1 d . . . 
O2W O 0.2623(8) 0.2306(8) 0.0275(5) 0.0131(18) Uiso 1 1 d . . . 
O3W O -0.3252(8) 0.5692(8) 0.0779(5) 0.0127(17) Uiso 1 1 d . . . 
O4W O 0.3738(8) 0.5154(8) 0.0665(5) 0.0148(18) Uiso 1 1 d . . . 
O5W O -0.4403(9) 0.2774(8) -0.0009(5) 0.0180(19) Uiso 1 1 d . . . 
O6W O -0.2275(9) 0.0340(8) 0.0538(5) 0.0166(19) Uiso 1 1 d . . . 
O7W O 0.3020(8) -0.0065(8) 0.1206(5) 0.0166(19) Uiso 1 1 d . . . 
O8W O 0.4114(8) 0.4564(8) 0.2620(5) 0.0149(18) Uiso 1 1 d . . . 
O9W O 0.2132(8) 0.1876(8) -0.1702(5) 0.0157(19) Uiso 1 1 d . . . 
O10W O 0.4710(9) 0.7162(8) 0.1784(5) 0.019(2) Uiso 1 1 d . . . 
O11W O 0.1825(9) -0.0658(8) -0.2419(5) 0.020(2) Uiso 1 1 d . . . 
O12W O -0.5537(9) 0.0393(8) -0.1050(5) 0.020(2) Uiso 1 1 d . . . 
O13W O 0.5684(9) 0.3117(9) 0.1530(6) 0.023(2) Uiso 1 1 d . . . 
  
  
_geom_special_details 
; 
 All esds (except the esd in the dihedral angle between two l.s. planes) 
 are estimated using the full covariance matrix.  The cell esds are taken 
 into account individually in the estimation of esds in distances, angles 
 and torsion angles; correlations between esds in cell parameters are only 
 used when they are defined by crystal symmetry.  An approximate (isotropic) 
 treatment of cell esds is used for estimating esds involving l.s. planes. 
; 
  
loop_ 
 _geom_bond_atom_site_label_1 
 _geom_bond_atom_site_label_2 
 _geom_bond_distance 
 _geom_bond_site_symmetry_2 
 _geom_bond_publ_flag 
Ir1 O3 2.015(8) . ? 
Ir1 O3 2.015(8) 3_565 ? 
Ir1 O1 2.024(8) . ? 
Ir1 O1 2.024(8) 3_565 ? 
Ir1 O2 2.029(8) . ? 
Ir1 O2 2.029(8) 3_565 ? 
Ir1 W1 3.2269(5) 3_565 ? 
Ir1 W1 3.2270(5) . ? 
W1 O1T 1.746(9) . ? 
W1 O1H 1.765(8) . ? 
W1 O13 1.940(7) . ? 
W1 O12 1.963(8) . ? 
W1 O1 2.146(8) . ? 
W1 O2 2.180(8) 3_565 ? 
W1 W3 3.2311(7) 3_565 ? 
W1 Na2 3.716(5) . ? 
W2 O2H 1.756(8) . ? 
W2 O2T 1.780(8) . ? 
W2 O23 1.968(8) . ? 
W2 O12 1.977(8) . ? 
W2 O3 2.157(8) . ? 
W2 O1 2.158(8) . ? 
W2 W3 3.2350(7) . ? 
W3 O3T 1.764(8) . ? 
W3 O3H 1.778(8) . ? 
W3 O23 1.957(8) . ? 
W3 O13 1.973(8) 3_565 ? 
W3 O2 2.132(8) . ? 
W3 O3 2.163(8) . ? 
W3 W1 3.2311(7) 3_565 ? 
O1H Na2 2.417(9) . ? 
O1H Na1 2.478(9) . ? 
O1H Na1 2.569(9) 3 ? 
O2 W1 2.180(8) 3_565 ? 
O2H Na1 2.367(10) . ? 
O2H Na2 2.465(10) 3 ? 
O13 W3 1.973(8) 3_565 ? 
Na1 O6W 2.291(10) 3 ? 
Na1 O7W 2.361(10) . ? 
Na1 O2W 2.374(10) . ? 
Na1 O1H 2.569(9) 3 ? 
Na1 Na2 3.372(7) 3 ? 
Na1 Na2 3.465(7) . ? 
Na1 Na1 3.595(10) 3 ? 
Na1 Na4 4.029(7) 1_655 ? 
Na2 O11W 2.295(11) . ? 
Na2 O8W 2.353(10) 4_565 ? 
Na2 O6W 2.374(10) 3 ? 
Na2 O9W 2.432(10) . ? 
Na2 O2H 2.465(10) 3 ? 
Na2 Na1 3.372(7) 3 ? 
Na2 Na3 3.406(6) 4_565 ? 
Na2 Na4 4.218(7) 1_655 ? 
Na3 O3W 2.316(10) 1_655 ? 
Na3 O11W 2.354(11) 4_666 ? 
Na3 O4W 2.362(10) . ? 
Na3 O8W 2.386(10) . ? 
Na3 O13W 2.448(12) . ? 
Na3 O10W 2.465(11) . ? 
Na3 Na2 3.406(6) 4_666 ? 
Na3 Na4 3.445(7) 3_565 ? 
Na4 O5W 2.360(11) . ? 
Na4 O2W 2.416(10) 1_455 ? 
Na4 O3W 2.417(10) 3_465 ? 
Na4 O12W 2.422(11) . ? 
Na4 O9W 2.435(10) 1_455 ? 
Na4 O10W 2.498(11) 3_565 ? 
Na4 Na3 3.445(7) 3_565 ? 
Na4 Na1 4.029(7) 1_455 ? 
Na4 Na2 4.218(7) 1_455 ? 
O2W Na4 2.416(10) 1_655 ? 
O3W Na3 2.316(10) 1_455 ? 
O3W Na4 2.417(10) 3_465 ? 
O6W Na1 2.291(10) 3 ? 
O6W Na2 2.374(10) 3 ? 
O8W Na2 2.353(10) 4_666 ? 
O9W Na4 2.435(10) 1_655 ? 
O10W Na4 2.498(11) 3_565 ? 
O11W Na3 2.354(11) 4_565 ? 
  
loop_ 
 _geom_angle_atom_site_label_1 
 _geom_angle_atom_site_label_2 
 _geom_angle_atom_site_label_3 
 _geom_angle 
 _geom_angle_site_symmetry_1 
 _geom_angle_site_symmetry_3 
 _geom_angle_publ_flag 
O3 Ir1 O3 179.999(1) . 3_565 ? 
O3 Ir1 O1 80.9(3) . . ? 
O3 Ir1 O1 99.1(3) 3_565 . ? 
O3 Ir1 O1 99.1(3) . 3_565 ? 
O3 Ir1 O1 80.9(3) 3_565 3_565 ? 
O1 Ir1 O1 179.999(1) . 3_565 ? 
O3 Ir1 O2 80.9(3) . . ? 
O3 Ir1 O2 99.1(3) 3_565 . ? 
O1 Ir1 O2 97.6(3) . . ? 
O1 Ir1 O2 82.4(3) 3_565 . ? 
O3 Ir1 O2 99.1(3) . 3_565 ? 
O3 Ir1 O2 80.9(3) 3_565 3_565 ? 
O1 Ir1 O2 82.4(3) . 3_565 ? 
O1 Ir1 O2 97.6(3) 3_565 3_565 ? 
O2 Ir1 O2 179.999(1) . 3_565 ? 
O3 Ir1 W1 89.4(2) . 3_565 ? 
O3 Ir1 W1 90.6(2) 3_565 3_565 ? 
O1 Ir1 W1 139.3(2) . 3_565 ? 
O1 Ir1 W1 40.7(2) 3_565 3_565 ? 
O2 Ir1 W1 41.7(2) . 3_565 ? 
O2 Ir1 W1 138.3(2) 3_565 3_565 ? 
O3 Ir1 W1 90.6(2) . . ? 
O3 Ir1 W1 89.4(2) 3_565 . ? 
O1 Ir1 W1 40.7(2) . . ? 
O1 Ir1 W1 139.3(2) 3_565 . ? 
O2 Ir1 W1 138.3(2) . . ? 
O2 Ir1 W1 41.7(2) 3_565 . ? 
W1 Ir1 W1 180.0 3_565 . ? 
O1T W1 O1H 104.3(4) . . ? 
O1T W1 O13 100.0(4) . . ? 
O1H W1 O13 96.3(3) . . ? 
O1T W1 O12 91.4(4) . . ? 
O1H W1 O12 99.0(3) . . ? 
O13 W1 O12 158.0(3) . . ? 
O1T W1 O1 160.2(4) . . ? 
O1H W1 O1 91.5(3) . . ? 
O13 W1 O1 89.7(3) . . ? 
O12 W1 O1 74.2(3) . . ? 
O1T W1 O2 89.8(4) . 3_565 ? 
O1H W1 O2 164.4(3) . 3_565 ? 
O13 W1 O2 74.4(3) . 3_565 ? 
O12 W1 O2 87.0(3) . 3_565 ? 
O1 W1 O2 76.2(3) . 3_565 ? 
O1T W1 Ir1 126.9(3) . . ? 
O1H W1 Ir1 128.7(3) . . ? 
O13 W1 Ir1 79.4(2) . . ? 
O12 W1 Ir1 78.8(2) . . ? 
O1 W1 Ir1 37.9(2) . . ? 
O2 W1 Ir1 38.3(2) 3_565 . ? 
O1T W1 W3 89.3(3) . 3_565 ? 
O1H W1 W3 131.0(3) . 3_565 ? 
O13 W1 W3 34.7(2) . 3_565 ? 
O12 W1 W3 127.9(2) . 3_565 ? 
O1 W1 W3 89.0(2) . 3_565 ? 
O2 W1 W3 40.9(2) 3_565 3_565 ? 
Ir1 W1 W3 60.185(12) . 3_565 ? 
O1T W1 Na2 95.3(3) . . ? 
O1H W1 Na2 32.3(3) . . ? 
O13 W1 Na2 67.2(2) . . ? 
O12 W1 Na2 130.8(2) . . ? 
O1 W1 Na2 104.4(2) . . ? 
O2 W1 Na2 141.5(2) 3_565 . ? 
Ir1 W1 Na2 130.27(8) . . ? 
W3 W1 Na2 100.88(8) 3_565 . ? 
O2H W2 O2T 102.6(4) . . ? 
O2H W2 O23 94.1(4) . . ? 
O2T W2 O23 99.0(4) . . ? 
O2H W2 O12 98.6(3) . . ? 
O2T W2 O12 96.5(4) . . ? 
O23 W2 O12 157.3(3) . . ? 
O2H W2 O3 161.4(3) . . ? 
O2T W2 O3 93.9(3) . . ? 
O23 W2 O3 74.7(3) . . ? 
O12 W2 O3 87.8(3) . . ? 
O2H W2 O1 90.2(4) . . ? 
O2T W2 O1 165.1(3) . . ? 
O23 W2 O1 87.6(3) . . ? 
O12 W2 O1 73.7(3) . . ? 
O3 W2 O1 74.8(3) . . ? 
O2H W2 W3 128.5(3) . . ? 
O2T W2 W3 91.1(3) . . ? 
O23 W2 W3 34.4(2) . . ? 
O12 W2 W3 129.3(2) . . ? 
O3 W2 W3 41.6(2) . . ? 
O1 W2 W3 86.9(2) . . ? 
O3T W3 O3H 102.4(4) . . ? 
O3T W3 O23 94.5(4) . . ? 
O3H W3 O23 99.2(4) . . ? 
O3T W3 O13 100.0(4) . 3_565 ? 
O3H W3 O13 93.3(4) . 3_565 ? 
O23 W3 O13 158.4(3) . 3_565 ? 
O3T W3 O2 90.7(4) . . ? 
O3H W3 O2 163.8(4) . . ? 
O23 W3 O2 89.1(3) . . ? 
O13 W3 O2 74.8(3) 3_565 . ? 
O3T W3 O3 162.3(3) . . ? 
O3H W3 O3 93.3(4) . . ? 
O23 W3 O3 74.8(3) . . ? 
O13 W3 O3 87.0(3) 3_565 . ? 
O2 W3 O3 75.3(3) . . ? 
O3T W3 W1 90.0(3) . 3_565 ? 
O3H W3 W1 127.3(3) . 3_565 ? 
O23 W3 W1 131.1(2) . 3_565 ? 
O13 W3 W1 34.0(2) 3_565 3_565 ? 
O2 W3 W1 42.0(2) . 3_565 ? 
O3 W3 W1 86.8(2) . 3_565 ? 
O3T W3 W2 129.1(3) . . ? 
O3H W3 W2 90.8(3) . . ? 
O23 W3 W2 34.6(2) . . ? 
O13 W3 W2 128.4(2) 3_565 . ? 
O2 W3 W2 88.2(2) . . ? 
O3 W3 W2 41.4(2) . . ? 
W1 W3 W2 120.092(19) 3_565 . ? 
Ir1 O1 W1 101.4(3) . . ? 
Ir1 O1 W2 101.9(3) . . ? 
W1 O1 W2 98.1(3) . . ? 
W1 O1H Na2 124.7(4) . . ? 
W1 O1H Na1 128.0(4) . . ? 
Na2 O1H Na1 90.1(3) . . ? 
W1 O1H Na1 125.6(4) . 3 ? 
Na2 O1H Na1 85.1(3) . 3 ? 
Na1 O1H Na1 90.8(3) . 3 ? 
Ir1 O2 W3 102.1(3) . . ? 
Ir1 O2 W1 100.0(3) . 3_565 ? 
W3 O2 W1 97.1(3) . 3_565 ? 
W2 O2H Na1 131.7(5) . . ? 
W2 O2H Na2 129.4(4) . 3 ? 
Na1 O2H Na2 88.5(3) . 3 ? 
Ir1 O3 W2 102.3(3) . . ? 
Ir1 O3 W3 101.6(3) . . ? 
W2 O3 W3 97.0(3) . . ? 
W1 O12 W2 111.2(4) . . ? 
W1 O13 W3 111.3(4) . 3_565 ? 
W3 O23 W2 111.0(4) . . ? 
O6W Na1 O7W 87.2(4) 3 . ? 
O6W Na1 O2H 167.3(4) 3 . ? 
O7W Na1 O2H 104.0(3) . . ? 
O6W Na1 O2W 95.5(4) 3 . ? 
O7W Na1 O2W 87.4(3) . . ? 
O2H Na1 O2W 91.0(3) . . ? 
O6W Na1 O1H 87.1(3) 3 . ? 
O7W Na1 O1H 174.0(4) . . ? 
O2H Na1 O1H 81.5(3) . . ? 
O2W Na1 O1H 94.9(3) . . ? 
O6W Na1 O1H 82.4(3) 3 3 ? 
O7W Na1 O1H 88.3(3) . 3 ? 
O2H Na1 O1H 91.9(3) . 3 ? 
O2W Na1 O1H 175.3(4) . 3 ? 
O1H Na1 O1H 89.2(3) . 3 ? 
O6W Na1 Na2 127.9(3) 3 3 ? 
O7W Na1 Na2 92.6(3) . 3 ? 
O2H Na1 Na2 47.0(2) . 3 ? 
O2W Na1 Na2 136.6(3) . 3 ? 
O1H Na1 Na2 89.5(2) . 3 ? 
O1H Na1 Na2 45.6(2) 3 3 ? 
O6W Na1 Na2 43.0(3) 3 . ? 
O7W Na1 Na2 130.1(3) . . ? 
O2H Na1 Na2 125.6(3) . . ? 
O2W Na1 Na2 95.3(3) . . ? 
O1H Na1 Na2 44.2(2) . . ? 
O1H Na1 Na2 86.0(2) 3 . ? 
Na2 Na1 Na2 116.58(16) 3 . ? 
O6W Na1 Na1 82.6(3) 3 3 ? 
O7W Na1 Na1 131.7(3) . 3 ? 
O2H Na1 Na1 85.5(3) . 3 ? 
O2W Na1 Na1 140.5(3) . 3 ? 
O1H Na1 Na1 45.6(2) . 3 ? 
O1H Na1 Na1 43.6(2) 3 3 ? 
Na2 Na1 Na1 59.55(16) 3 3 ? 
Na2 Na1 Na1 57.03(15) . 3 ? 
O6W Na1 Na4 62.9(3) 3 1_655 ? 
O7W Na1 Na4 91.3(3) . 1_655 ? 
O2H Na1 Na4 121.7(3) . 1_655 ? 
O2W Na1 Na4 33.0(2) . 1_655 ? 
O1H Na1 Na4 87.7(2) . 1_655 ? 
O1H Na1 Na4 145.2(3) 3 1_655 ? 
Na2 Na1 Na4 168.69(19) 3 1_655 ? 
Na2 Na1 Na4 68.03(13) . 1_655 ? 
Na1 Na1 Na4 124.0(2) 3 1_655 ? 
O11W Na2 O8W 87.0(4) . 4_565 ? 
O11W Na2 O6W 93.8(4) . 3 ? 
O8W Na2 O6W 166.6(4) 4_565 3 ? 
O11W Na2 O1H 178.6(4) . . ? 
O8W Na2 O1H 92.8(3) 4_565 . ? 
O6W Na2 O1H 86.7(3) 3 . ? 
O11W Na2 O9W 87.1(4) . . ? 
O8W Na2 O9W 105.3(4) 4_565 . ? 
O6W Na2 O9W 88.2(3) 3 . ? 
O1H Na2 O9W 91.7(3) . . ? 
O11W Na2 O2H 88.0(4) . 3 ? 
O8W Na2 O2H 86.5(3) 4_565 3 ? 
O6W Na2 O2H 80.2(3) 3 3 ? 
O1H Na2 O2H 93.3(3) . 3 ? 
O9W Na2 O2H 167.0(4) . 3 ? 
O11W Na2 Na1 131.9(3) . 3 ? 
O8W Na2 Na1 83.0(3) 4_565 3 ? 
O6W Na2 Na1 86.5(3) 3 3 ? 
O1H Na2 Na1 49.4(2) . 3 ? 
O9W Na2 Na1 140.9(3) . 3 ? 
O2H Na2 Na1 44.6(2) 3 3 ? 
O11W Na2 Na3 43.6(3) . 4_565 ? 
O8W Na2 Na3 44.4(2) 4_565 4_565 ? 
O6W Na2 Na3 137.3(3) 3 4_565 ? 
O1H Na2 Na3 136.0(3) . 4_565 ? 
O9W Na2 Na3 91.2(3) . 4_565 ? 
O2H Na2 Na3 93.6(3) 3 4_565 ? 
Na1 Na2 Na3 118.07(18) 3 4_565 ? 
O11W Na2 Na1 134.8(3) . . ? 
O8W Na2 Na1 137.3(3) 4_565 . ? 
O6W Na2 Na1 41.1(3) 3 . ? 
O1H Na2 Na1 45.7(2) . . ? 
O9W Na2 Na1 88.0(3) . . ? 
O2H Na2 Na1 87.0(2) 3 . ? 
Na1 Na2 Na1 63.42(16) 3 . ? 
Na3 Na2 Na1 178.21(19) 4_565 . ? 
O11W Na2 W1 155.8(3) . . ? 
O8W Na2 W1 78.8(3) 4_565 . ? 
O6W Na2 W1 104.6(3) 3 . ? 
O1H Na2 W1 23.0(2) . . ? 
O9W Na2 W1 78.0(2) . . ? 
O2H Na2 W1 110.3(3) 3 . ? 
Na1 Na2 W1 66.01(12) 3 . ? 
Na3 Na2 W1 117.03(15) 4_565 . ? 
Na1 Na2 W1 64.31(11) . . ? 
O11W Na2 Na4 95.0(3) . 1_655 ? 
O8W Na2 Na4 134.5(3) 4_565 1_655 ? 
O6W Na2 Na4 58.9(3) 3 1_655 ? 
O1H Na2 Na4 84.2(2) . 1_655 ? 
O9W Na2 Na4 30.0(2) . 1_655 ? 
O2H Na2 Na4 139.0(3) 3 1_655 ? 
Na1 Na2 Na4 124.69(17) 3 1_655 ? 
Na3 Na2 Na4 116.36(16) 4_565 1_655 ? 
Na1 Na2 Na4 62.36(13) . 1_655 ? 
W1 Na2 Na4 81.60(11) . 1_655 ? 
O3W Na3 O11W 87.9(4) 1_655 4_666 ? 
O3W Na3 O4W 89.8(3) 1_655 . ? 
O11W Na3 O4W 165.9(4) 4_666 . ? 
O3W Na3 O8W 171.9(4) 1_655 . ? 
O11W Na3 O8W 84.9(4) 4_666 . ? 
O4W Na3 O8W 98.1(4) . . ? 
O3W Na3 O13W 96.0(4) 1_655 . ? 
O11W Na3 O13W 101.1(4) 4_666 . ? 
O4W Na3 O13W 93.0(4) . . ? 
O8W Na3 O13W 81.8(4) . . ? 
O3W Na3 O10W 90.8(4) 1_655 . ? 
O11W Na3 O10W 81.9(4) 4_666 . ? 
O4W Na3 O10W 84.2(3) . . ? 
O8W Na3 O10W 91.9(4) . . ? 
O13W Na3 O10W 172.7(4) . . ? 
O3W Na3 Na2 128.6(3) 1_655 4_666 ? 
O11W Na3 Na2 42.2(3) 4_666 4_666 ? 
O4W Na3 Na2 141.6(3) . 4_666 ? 
O8W Na3 Na2 43.7(2) . 4_666 ? 
O13W Na3 Na2 85.2(3) . 4_666 ? 
O10W Na3 Na2 92.8(3) . 4_666 ? 
O3W Na3 Na4 44.5(3) 1_655 3_565 ? 
O11W Na3 Na4 85.3(3) 4_666 3_565 ? 
O4W Na3 Na4 83.4(3) . 3_565 ? 
O8W Na3 Na4 138.1(3) . 3_565 ? 
O13W Na3 Na4 140.0(3) . 3_565 ? 
O10W Na3 Na4 46.4(3) . 3_565 ? 
Na2 Na3 Na4 121.19(19) 4_666 3_565 ? 
O5W Na4 O2W 88.3(4) . 1_455 ? 
O5W Na4 O3W 88.7(4) . 3_465 ? 
O2W Na4 O3W 80.6(3) 1_455 3_465 ? 
O5W Na4 O12W 95.7(4) . . ? 
O2W Na4 O12W 107.8(4) 1_455 . ? 
O3W Na4 O12W 170.6(4) 3_465 . ? 
O5W Na4 O9W 175.9(4) . 1_455 ? 
O2W Na4 O9W 95.9(3) 1_455 1_455 ? 
O3W Na4 O9W 91.9(3) 3_465 1_455 ? 
O12W Na4 O9W 83.1(4) . 1_455 ? 
O5W Na4 O10W 82.1(3) . 3_565 ? 
O2W Na4 O10W 165.1(4) 1_455 3_565 ? 
O3W Na4 O10W 87.7(3) 3_465 3_565 ? 
O12W Na4 O10W 84.6(3) . 3_565 ? 
O9W Na4 O10W 93.8(3) 1_455 3_565 ? 
O5W Na4 Na3 81.5(3) . 3_565 ? 
O2W Na4 Na3 121.6(3) 1_455 3_565 ? 
O3W Na4 Na3 42.1(2) 3_465 3_565 ? 
O12W Na4 Na3 130.3(3) . 3_565 ? 
O9W Na4 Na3 96.2(3) 1_455 3_565 ? 
O10W Na4 Na3 45.7(3) 3_565 3_565 ? 
O5W Na4 Na1 108.1(3) . 1_455 ? 
O2W Na4 Na1 32.4(2) 1_455 1_455 ? 
O3W Na4 Na1 106.3(3) 3_465 1_455 ? 
O12W Na4 Na1 80.3(3) . 1_455 ? 
O9W Na4 Na1 75.7(3) 1_455 1_455 ? 
O10W Na4 Na1 162.5(3) 3_565 1_455 ? 
Na3 Na4 Na1 147.88(18) 3_565 1_455 ? 
O5W Na4 Na2 152.5(3) . 1_455 ? 
O2W Na4 Na2 77.4(3) 1_455 1_455 ? 
O3W Na4 Na2 111.4(3) 3_465 1_455 ? 
O12W Na4 Na2 67.4(3) . 1_455 ? 
O9W Na4 Na2 29.9(2) 1_455 1_455 ? 
O10W Na4 Na2 115.9(3) 3_565 1_455 ? 
Na3 Na4 Na2 125.98(17) 3_565 1_455 ? 
Na1 Na4 Na2 49.62(11) 1_455 1_455 ? 
Na1 O2W Na4 114.5(4) . 1_655 ? 
Na3 O3W Na4 93.4(4) 1_455 3_465 ? 
Na1 O6W Na2 95.9(4) 3 3 ? 
Na2 O8W Na3 91.9(4) 4_666 . ? 
Na2 O9W Na4 120.1(4) . 1_655 ? 
Na3 O10W Na4 87.9(3) . 3_565 ? 
Na2 O11W Na3 94.2(4) . 4_565 ? 
  
_diffrn_measured_fraction_theta_max    0.998 
_diffrn_reflns_theta_full              68.24 
_diffrn_measured_fraction_theta_full   0.998 
_refine_diff_density_max    5.200 
_refine_diff_density_min   -4.811 
_refine_diff_density_rms    0.652 
