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        'Natalya V. Izarova'
_publ_contact_author_address     
;Juelich-Aachen Research Alliance (JARA-FIT) 
and Peter Gruenberg Institure PGI-6, 
Forschungszentrum Juelich, D-52425 Juelich, 
Germany
;
_publ_contact_author_email       n.izarova@fz-juelich.de
_publ_contact_author_phone       '+49-2461-61-46-79'
_publ_requested_journal              
;
Dalton Transactions
;
# TITLE AND AUTHOR LIST

_publ_section_title
;
Tin(II)-functionalization of the archetypal {P8W48} Polyoxotungstate; 
;
_publ_section_title_footnote
; ?
;        
loop_
_publ_author_name
_publ_author_address

'Izarova, Natalya V.'
;
Peter Gruenberg Institure PGI-6
Forschungszentrum Juelich
D-52425 Juelich
Germany
;

'Larissa Klass'
;
Institute of Inorganic Chemistry
RWTH Aachen University 
D-52074 Aachen 
Germany
;

'de Oliveira, Pedro'
;
Equipe d Electrochimie et de Photoelectrochimie
Laboratoire de Chimie-Physique 
Universite Paris-Sud, UMR 8000 CNRS
F-91405 Orsay
France
;

'Mbomekalle, Israel-Martyr'
;
Equipe d Electrochimie et de Photoelectrochimie
Laboratoire de Chimie-Physique 
Universite Paris-Sud, UMR 8000 CNRS
F-91405 Orsay
France
;
'Peters, Volker'
;
Institute of Inorganic Chemistry
RWTH Aachen University 
D-52074 Aachen 
Germany
;

'Haarmann, Frank'
;
Institute of Inorganic Chemistry
RWTH Aachen University 
D-52074 Aachen 
Germany
;
'Koegerler, Paul'
;
Institute of Inorganic Chemistry
RWTH Aachen University
D-52074 Aachen
Germany
;
  
data_Sn6P8W48 
 
_audit_creation_method            SHELXL-97 
_chemical_name_systematic 
; 
 ? 
; 
_chemical_name_common             ? 
_chemical_melting_point           ? 
_chemical_formula_moiety          ? 
_chemical_formula_sum 
 'H126 K11 Li23 O250 P8 Sn6 W48' 
_chemical_formula_weight          14501.43 
 
loop_ 
 _atom_type_symbol 
 _atom_type_description 
 _atom_type_scat_dispersion_real 
 _atom_type_scat_dispersion_imag 
 _atom_type_scat_source 
 'H'  'H'   0.0000   0.0000 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'Li'  'Li'  -0.0003   0.0001 
 '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' 
 'K'  'K'   0.2009   0.2494 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'Sn'  'Sn'  -0.6537   1.4246 
 '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            tetragonal 
_symmetry_space_group_name_H-M    I4/mmm 
 
loop_ 
 _symmetry_equiv_pos_as_xyz 
 'x, y, z' 
 '-x, -y, z' 
 '-y, x, z' 
 'y, -x, z' 
 '-x, y, -z' 
 'x, -y, -z' 
 'y, x, -z' 
 '-y, -x, -z' 
 'x+1/2, y+1/2, z+1/2' 
 '-x+1/2, -y+1/2, z+1/2' 
 '-y+1/2, x+1/2, z+1/2' 
 'y+1/2, -x+1/2, z+1/2' 
 '-x+1/2, y+1/2, -z+1/2' 
 'x+1/2, -y+1/2, -z+1/2' 
 'y+1/2, x+1/2, -z+1/2' 
 '-y+1/2, -x+1/2, -z+1/2' 
 '-x, -y, -z' 
 'x, y, -z' 
 'y, -x, -z' 
 '-y, x, -z' 
 'x, -y, z' 
 '-x, y, z' 
 '-y, -x, z' 
 'y, x, z' 
 '-x+1/2, -y+1/2, -z+1/2' 
 'x+1/2, y+1/2, -z+1/2' 
 'y+1/2, -x+1/2, -z+1/2' 
 '-y+1/2, x+1/2, -z+1/2' 
 'x+1/2, -y+1/2, z+1/2' 
 '-x+1/2, y+1/2, z+1/2' 
 '-y+1/2, -x+1/2, z+1/2' 
 'y+1/2, x+1/2, z+1/2' 
 
_cell_length_a                    26.9749(3) 
_cell_length_b                    26.9749(3) 
_cell_length_c                    21.0538(3) 
_cell_angle_alpha                 90.00 
_cell_angle_beta                  90.00 
_cell_angle_gamma                 90.00 
_cell_volume                      15319.7(3) 
_cell_formula_units_Z             2 
_cell_measurement_temperature     120.00(10) 
_cell_measurement_reflns_used     19267 
_cell_measurement_theta_min       3.0730 
_cell_measurement_theta_max       28.9930
 
_exptl_crystal_description        block 
_exptl_crystal_colour             orange 
_exptl_crystal_size_max           0.24 
_exptl_crystal_size_mid           0.13 
_exptl_crystal_size_min           0.08 
_exptl_crystal_density_meas       ? 
_exptl_crystal_density_diffrn     3.144 
_exptl_crystal_density_method     'not measured' 
_exptl_crystal_F_000              12752 
_exptl_absorpt_coefficient_mu     18.702 
_exptl_absorpt_correction_type    'multi-scan' 
_exptl_absorpt_correction_T_min   0.0959 
_exptl_absorpt_correction_T_max   0.3161 
_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)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
 
_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       120.00(10) 
_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   'SuperNova, Dual, Cu at zero, Atlas' 
_diffrn_measurement_method        'φ and ω scans'  
_diffrn_detector_area_resol_mean  ? 
_diffrn_reflns_number             92892 
_diffrn_reflns_av_R_equivalents   0.1162 
_diffrn_reflns_av_sigmaI/netI     0.0484 
_diffrn_reflns_limit_h_min        -36 
_diffrn_reflns_limit_h_max        36 
_diffrn_reflns_limit_k_min        -36 
_diffrn_reflns_limit_k_max        33 
_diffrn_reflns_limit_l_min        -26 
_diffrn_reflns_limit_l_max        29 
_diffrn_reflns_theta_min          2.88 
_diffrn_reflns_theta_max          29.55 
_reflns_number_total              5641 
_reflns_number_gt                 4039 
_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. 

 Due to heavy disorder we could not locate all the O atoms of terminal OH
 ligands on Sn(II) centers as well as most of the O atoms of crystal water
 molecules.
; 
 
_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)+(0.0671P)²+2388.5801P] 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          5641 
_refine_ls_number_parameters      125 
_refine_ls_number_restraints      1 
_refine_ls_R_factor_all           0.1141 
_refine_ls_R_factor_gt            0.0785 
_refine_ls_wR_factor_ref          0.2117 
_refine_ls_wR_factor_gt           0.1905 
_refine_ls_goodness_of_fit_ref    1.090 
_refine_ls_restrained_S_all       1.091 
_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 
Sn1 Sn 0.0000 0.1970(8) 0.0815(7) 0.082(2) Uiso 0.239(9) 2 d SP . 1 
O1SN O 0.0188(18) 0.237(2) 0.158(2) 0.036(12) Uiso 0.239(9) 1 d P . 1 
Sn1B Sn 0.0000 0.1703(5) 0.0933(5) 0.082(2) Uiso 0.362(9) 2 d SP . 2 
O2SN O 1.157(3) -0.007(7) -0.281(4) 0.08(3) Uiso 0.181(5) 1 d P . 2 
Sn1C Sn 0.0000 0.1801(9) 0.2354(11) 0.082(2) Uiso 0.146(6) 2 d SP . 3 
W1 W 0.06823(3) 0.32739(4) 0.07948(3) 0.0440(2) Uani 1 1 d . . . 
W2 W 0.20301(3) 0.30165(3) 0.07957(3) 0.0358(2) Uani 1 1 d . . . 
W3 W 0.11540(3) 0.21420(3) 0.16128(3) 0.0344(2) Uani 1 1 d . . . 
P1 P 0.1199(3) 0.2297(3) 0.0000 0.0330(15) Uani 1 2 d S . . 
O1T O 0.0577(6) 0.3756(6) 0.1310(7) 0.049(4) Uiso 1 1 d . . . 
O2T O 0.2289(5) 0.3447(5) 0.1316(6) 0.033(3) Uiso 1 1 d . . . 
O3T O 0.1203(5) 0.2326(5) 0.2402(7) 0.043(3) Uiso 1 1 d . . . 
O3 O 0.0589(6) 0.1798(6) 0.1634(7) 0.053(4) Uiso 1 1 d . . . 
O1P1 O 0.0784(6) 0.2720(7) 0.0000 0.032(4) Uiso 1 2 d S . . 
O11 O 0.0000 0.3081(8) 0.0698(10) 0.047(5) Uiso 1 2 d S . . 
O12 O 0.1391(5) 0.3348(5) 0.0726(6) 0.034(3) Uiso 1 1 d . . . 
O13 O 0.0796(5) 0.2726(5) 0.1344(6) 0.035(3) Uiso 1 1 d . . . 
O2P1 O 0.1714(6) 0.2540(6) 0.0000 0.026(3) Uiso 1 2 d S . . 
O22 O 0.2611(4) 0.2611(4) 0.0712(7) 0.027(3) Uiso 1 2 d S . . 
O23 O 0.1735(5) 0.2562(4) 0.1331(6) 0.032(3) Uiso 1 1 d . . . 
O3P1 O 0.1128(5) 0.1979(5) 0.0594(6) 0.034(3) Uiso 1 1 d . . . 
O33 O 0.1590(5) 0.1590(5) 0.1643(9) 0.045(5) Uiso 1 2 d S . . 
O112 O 0.0613(7) 0.3624(7) 0.0000 0.037(4) Uiso 1 2 d S . . 
O222 O 0.2213(6) 0.3330(6) 0.0000 0.030(4) Uiso 1 2 d S . . 
K1 K 0.3226(3) 0.3226(3) 0.1755(5) 0.035(2) Uani 0.50 2 d SP . . 
K2 K 0.1856(4) 0.3144(4) 0.2500 0.048(3) Uani 0.50 2 d SP . . 
K3 K -0.0489(4) 0.0489(4) 0.0754(10) 0.053(5) Uani 0.38 2 d SP . . 
O1W O 0.2500 0.2500 0.2500 0.077(11) Uiso 1 4 d S . . 
O2W O 0.100(3) 0.100(3) 0.0000 0.07(3) Uiso 0.38 4 d SP . . 
 
 
_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 
Sn1 O1SN 2.01(5) . ? 
Sn1 O1SN 2.01(5) 22 ? 
Sn1 O3 2.39(2) 22 ? 
Sn1 O3 2.39(2) . ? 
O1SN O1SN 1.01(10) 22 ? 
Sn1B O2SN 32.54(9) . ? 
Sn1B O2SN 32.54(9) 22 ? 
Sn1B O3 2.182(17) 22 ? 
Sn1B O3 2.182(17) . ? 
Sn1B K3 3.551(14) . ? 
Sn1B K3 3.551(14) 4 ? 
O2SN O2SN 62.41(18) 22 ? 
O2SN K3 33.41(9) . ? 
O2SN K3 30.85(9) 4 ? 
Sn1C O3 2.19(2) 22 ? 
Sn1C O3 2.19(2) . ? 
W1 O1T 1.718(15) . ? 
W1 O13 1.902(13) . ? 
W1 O11 1.924(6) . ? 
W1 O112 1.930(9) . ? 
W1 O12 1.926(12) . ? 
W1 O1P1 2.260(12) . ? 
W2 O2T 1.743(12) . ? 
W2 O23 1.846(12) . ? 
W2 O22 1.919(3) . ? 
W2 O222 1.940(9) . ? 
W2 O12 1.948(13) . ? 
W2 O2P1 2.277(11) . ? 
W2 K2 3.635(3) . ? 
W2 K1 3.847(9) . ? 
W3 O3T 1.740(14) . ? 
W3 O3 1.786(16) . ? 
W3 O33 1.899(3) . ? 
W3 O13 1.932(13) . ? 
W3 O23 2.024(12) . ? 
W3 O3P1 2.191(12) . ? 
W3 K2 3.792(3) . ? 
W3 K1 3.949(9) 25 ? 
P1 O3P1 1.529(13) 18 ? 
P1 O3P1 1.529(13) . ? 
P1 O2P1 1.537(17) . ? 
P1 O1P1 1.598(19) . ? 
O2T K1 2.755(14) . ? 
O2T K2 2.872(12) . ? 
O3T K1 2.783(15) 25 ? 
O3T K2 2.831(14) . ? 
O1P1 W1 2.260(12) 18 ? 
O11 W1 1.924(6) 22 ? 
O2P1 W2 2.277(11) 18 ? 
O22 W2 1.919(3) 24 ? 
O22 K1 3.213(19) . ? 
O23 K2 2.937(13) . ? 
O33 W3 1.899(3) 24 ? 
O112 W1 1.930(9) 18 ? 
O222 W2 1.940(9) 18 ? 
K1 O2T 2.755(14) 24 ? 
K1 O3T 2.782(15) 16 ? 
K1 O3T 2.782(15) 25 ? 
K1 O1W 3.182(12) . ? 
K1 W2 3.847(9) 24 ? 
K1 W3 3.949(9) 25 ? 
K1 W3 3.949(9) 16 ? 
K1 K2 4.020(14) 25 ? 
K1 K2 4.020(14) . ? 
K2 O1W 2.457(16) . ? 
K2 O3T 2.831(14) 16 ? 
K2 O2T 2.872(12) 16 ? 
K2 O23 2.937(13) 16 ? 
K2 W2 3.635(3) 16 ? 
K2 W3 3.792(3) 16 ? 
K3 O2SN 33.41(9) 23 ? 
K3 O2W 2.53(9) 3 ? 
K3 K3 2.64(2) 4 ? 
K3 K3 2.64(2) 3 ? 
K3 O2SN 30.85(9) 22 ? 
K3 O2SN 30.85(9) 3 ? 
K3 K3 3.17(4) 18 ? 
K3 Sn1B 3.551(14) 3 ? 
K3 K3 3.73(3) 2 ? 
K3 K3 4.13(4) 20 ? 
O1W K2 2.457(16) 25 ? 
O1W K1 3.182(12) 25 ? 
O2W K3 2.53(9) 19 ? 
O2W K3 2.53(9) 4 ? 
 
loop_ 
 _geom_angle_atom_site_label_1 
 _geom_angle_atom_site_label_2 
 _geom_angle_atom_site_label_3 
 _geom_angle 
 _geom_angle_site_symmetry_1 
 _geom_angle_site_symmetry_3 
 _geom_angle_publ_flag 
O1SN Sn1 O1SN 29(3) . 22 ? 
O1SN Sn1 O3 72.1(15) . 22 ? 
O1SN Sn1 O3 50.1(15) 22 22 ? 
O1SN Sn1 O3 50.1(15) . . ? 
O1SN Sn1 O3 72.1(15) 22 . ? 
O3 Sn1 O3 83.3(9) 22 . ? 
O1SN O1SN Sn1 75.4(14) 22 . ? 
O2SN Sn1B O2SN 147.1(4) . 22 ? 
O2SN Sn1B O3 151.5(5) . 22 ? 
O2SN Sn1B O3 58.9(5) 22 22 ? 
O2SN Sn1B O3 58.9(5) . . ? 
O2SN Sn1B O3 151.5(5) 22 . ? 
O3 Sn1B O3 93.3(9) 22 . ? 
O2SN Sn1B K3 101.2(4) . . ? 
O2SN Sn1B K3 58.8(4) 22 . ? 
O3 Sn1B K3 84.8(6) 22 . ? 
O3 Sn1B K3 116.7(7) . . ? 
O2SN Sn1B K3 58.8(4) . 4 ? 
O2SN Sn1B K3 101.2(4) 22 4 ? 
O3 Sn1B K3 116.7(7) 22 4 ? 
O3 Sn1B K3 84.8(6) . 4 ? 
K3 Sn1B K3 43.6(5) . 4 ? 
O2SN O2SN Sn1B 16.5(2) 22 . ? 
O2SN O2SN K3 13.24(17) 22 . ? 
Sn1B O2SN K3 5.98(3) . . ? 
O2SN O2SN K3 14.36(18) 22 4 ? 
Sn1B O2SN K3 5.65(4) . 4 ? 
K3 O2SN K3 1.121(18) . 4 ? 
O3 Sn1C O3 92.7(12) 22 . ? 
O1T W1 O13 103.4(6) . . ? 
O1T W1 O11 96.6(8) . . ? 
O13 W1 O11 90.5(7) . . ? 
O1T W1 O112 99.3(7) . . ? 
O13 W1 O112 157.3(6) . . ? 
O11 W1 O112 87.0(8) . . ? 
O1T W1 O12 97.6(6) . . ? 
O13 W1 O12 88.0(5) . . ? 
O11 W1 O12 165.7(7) . . ? 
O112 W1 O12 88.9(7) . . ? 
O1T W1 O1P1 171.3(6) . . ? 
O13 W1 O1P1 85.2(5) . . ? 
O11 W1 O1P1 81.9(7) . . ? 
O112 W1 O1P1 72.1(6) . . ? 
O12 W1 O1P1 83.8(6) . . ? 
O2T W2 O23 103.4(5) . . ? 
O2T W2 O22 96.3(6) . . ? 
O23 W2 O22 91.6(6) . . ? 
O2T W2 O222 98.7(6) . . ? 
O23 W2 O222 157.9(6) . . ? 
O22 W2 O222 87.8(7) . . ? 
O2T W2 O12 95.6(5) . . ? 
O23 W2 O12 88.2(5) . . ? 
O22 W2 O12 167.8(6) . . ? 
O222 W2 O12 87.8(6) . . ? 
O2T W2 O2P1 171.4(5) . . ? 
O23 W2 O2P1 85.0(5) . . ? 
O22 W2 O2P1 85.2(6) . . ? 
O222 W2 O2P1 72.9(5) . . ? 
O12 W2 O2P1 82.7(5) . . ? 
O2T W2 K2 50.8(4) . . ? 
O23 W2 K2 53.4(4) . . ? 
O22 W2 K2 104.5(5) . . ? 
O222 W2 K2 147.6(5) . . ? 
O12 W2 K2 85.2(4) . . ? 
O2P1 W2 K2 137.0(3) . . ? 
O2T W2 K1 40.2(4) . . ? 
O23 W2 K1 97.9(4) . . ? 
O22 W2 K1 56.5(5) . . ? 
O222 W2 K1 100.2(5) . . ? 
O12 W2 K1 135.6(4) . . ? 
O2P1 W2 K1 141.5(4) . . ? 
K2 W2 K1 64.9(2) . . ? 
O3T W3 O3 100.9(7) . . ? 
O3T W3 O33 98.3(7) . . ? 
O3 W3 O33 96.9(8) . . ? 
O3T W3 O13 94.9(6) . . ? 
O3 W3 O13 90.3(6) . . ? 
O33 W3 O13 163.5(7) . . ? 
O3T W3 O23 93.5(6) . . ? 
O3 W3 O23 163.8(6) . . ? 
O33 W3 O23 88.2(7) . . ? 
O13 W3 O23 81.1(5) . . ? 
O3T W3 O3P1 174.4(6) . . ? 
O3 W3 O3P1 83.9(6) . . ? 
O33 W3 O3P1 84.0(7) . . ? 
O13 W3 O3P1 82.0(5) . . ? 
O23 W3 O3P1 81.4(5) . . ? 
O3T W3 K2 44.6(5) . . ? 
O3 W3 K2 141.7(5) . . ? 
O33 W3 K2 103.4(7) . . ? 
O13 W3 K2 79.2(4) . . ? 
O23 W3 K2 50.1(3) . . ? 
O3P1 W3 K2 129.9(3) . . ? 
O3T W3 K1 37.7(5) . 25 ? 
O3 W3 K1 102.1(5) . 25 ? 
O33 W3 K1 60.7(6) . 25 ? 
O13 W3 K1 132.2(4) . 25 ? 
O23 W3 K1 93.8(4) . 25 ? 
O3P1 W3 K1 144.6(3) . 25 ? 
K2 W3 K1 62.5(2) . 25 ? 
O3P1 P1 O3P1 109.8(10) 18 . ? 
O3P1 P1 O2P1 110.6(6) 18 . ? 
O3P1 P1 O2P1 110.6(6) . . ? 
O3P1 P1 O1P1 108.3(7) 18 . ? 
O3P1 P1 O1P1 108.3(7) . . ? 
O2P1 P1 O1P1 109.2(10) . . ? 
W2 O2T K1 115.7(6) . . ? 
W2 O2T K2 101.1(5) . . ? 
K1 O2T K2 91.2(5) . . ? 
W3 O3T K1 119.9(7) . 25 ? 
W3 O3T K2 109.8(6) . . ? 
K1 O3T K2 91.5(5) 25 . ? 
W3 O3 Sn1B 131.7(9) . . ? 
W3 O3 Sn1C 129.3(10) . . ? 
Sn1B O3 Sn1C 86.6(8) . . ? 
W3 O3 Sn1 116.6(9) . . ? 
Sn1B O3 Sn1 18.5(4) . . ? 
Sn1C O3 Sn1 90.9(8) . . ? 
P1 O1P1 W1 123.8(6) . . ? 
P1 O1P1 W1 123.8(6) . 18 ? 
W1 O1P1 W1 95.5(7) . 18 ? 
W1 O11 W1 146.2(12) 22 . ? 
W1 O12 W2 145.6(7) . . ? 
W1 O13 W3 153.2(7) . . ? 
P1 O2P1 W2 125.4(5) . 18 ? 
P1 O2P1 W2 125.4(5) . . ? 
W2 O2P1 W2 94.8(6) 18 . ? 
W2 O22 W2 157.4(9) 24 . ? 
W2 O22 K1 93.7(5) 24 . ? 
W2 O22 K1 93.7(5) . . ? 
W2 O23 W3 152.2(7) . . ? 
W2 O23 K2 96.3(5) . . ? 
W3 O23 K2 98.0(4) . . ? 
P1 O3P1 W3 133.2(8) . . ? 
W3 O33 W3 166.1(12) . 24 ? 
W1 O112 W1 120.2(10) . 18 ? 
W2 O222 W2 119.4(9) . 18 ? 
O2T K1 O2T 106.5(6) 24 . ? 
O2T K1 O3T 146.9(6) 24 16 ? 
O2T K1 O3T 66.6(4) . 16 ? 
O2T K1 O3T 66.6(4) 24 25 ? 
O2T K1 O3T 146.9(6) . 25 ? 
O3T K1 O3T 100.7(7) 16 25 ? 
O2T K1 O1W 74.6(4) 24 . ? 
O2T K1 O1W 74.6(4) . . ? 
O3T K1 O1W 72.4(4) 16 . ? 
O3T K1 O1W 72.4(4) 25 . ? 
O2T K1 O22 53.8(3) 24 . ? 
O2T K1 O22 53.8(3) . . ? 
O3T K1 O22 116.5(4) 16 . ? 
O3T K1 O22 116.5(4) 25 . ? 
O1W K1 O22 72.6(4) . . ? 
O2T K1 W2 24.1(3) 24 24 ? 
O2T K1 W2 82.6(4) . 24 ? 
O3T K1 W2 136.1(5) 16 24 ? 
O3T K1 W2 88.1(3) 25 24 ? 
O1W K1 W2 69.7(2) . 24 ? 
O22 K1 W2 29.85(10) . 24 ? 
O2T K1 W2 82.6(4) 24 . ? 
O2T K1 W2 24.1(3) . . ? 
O3T K1 W2 88.1(3) 16 . ? 
O3T K1 W2 136.1(5) 25 . ? 
O1W K1 W2 69.7(2) . . ? 
O22 K1 W2 29.85(10) . . ? 
W2 K1 W2 58.56(15) 24 . ? 
O2T K1 W3 88.3(3) 24 25 ? 
O2T K1 W3 137.3(4) . 25 ? 
O3T K1 W3 79.1(4) 16 25 ? 
O3T K1 W3 22.5(3) 25 25 ? 
O1W K1 W3 71.2(2) . 25 ? 
O22 K1 W3 133.1(4) . 25 ? 
W2 K1 W3 107.97(17) 24 25 ? 
W2 K1 W3 140.8(3) . 25 ? 
O2T K1 W3 137.3(4) 24 16 ? 
O2T K1 W3 88.3(3) . 16 ? 
O3T K1 W3 22.5(3) 16 16 ? 
O3T K1 W3 79.1(4) 25 16 ? 
O1W K1 W3 71.2(2) . 16 ? 
O22 K1 W3 133.1(4) . 16 ? 
W2 K1 W3 140.8(3) 24 16 ? 
W2 K1 W3 107.97(17) . 16 ? 
W3 K1 W3 57.02(15) 25 16 ? 
O2T K1 K2 45.6(3) 24 25 ? 
O2T K1 K2 106.2(5) . 25 ? 
O3T K1 K2 103.4(5) 16 25 ? 
O3T K1 K2 44.7(3) 25 25 ? 
O1W K1 K2 37.7(2) . 25 ? 
O22 K1 K2 76.3(3) . 25 ? 
W2 K1 K2 54.99(13) 24 25 ? 
W2 K1 K2 91.4(3) . 25 ? 
W3 K1 K2 56.82(13) 25 25 ? 
W3 K1 K2 92.1(3) 16 25 ? 
O2T K1 K2 106.3(5) 24 . ? 
O2T K1 K2 45.6(3) . . ? 
O3T K1 K2 44.7(3) 16 . ? 
O3T K1 K2 103.4(5) 25 . ? 
O1W K1 K2 37.7(2) . . ? 
O22 K1 K2 76.3(3) . . ? 
W2 K1 K2 91.4(3) 24 . ? 
W2 K1 K2 54.99(13) . . ? 
W3 K1 K2 92.1(3) 25 . ? 
W3 K1 K2 56.82(13) 16 . ? 
K2 K1 K2 75.4(4) 25 . ? 
O1W K2 O3T 83.6(4) . . ? 
O1W K2 O3T 83.6(4) . 16 ? 
O3T K2 O3T 167.3(9) . 16 ? 
O1W K2 O2T 85.0(4) . . ? 
O3T K2 O2T 114.3(4) . . ? 
O3T K2 O2T 64.5(4) 16 . ? 
O1W K2 O2T 85.0(4) . 16 ? 
O3T K2 O2T 64.5(4) . 16 ? 
O3T K2 O2T 114.3(4) 16 16 ? 
O2T K2 O2T 170.0(8) . 16 ? 
O1W K2 O23 72.5(4) . 16 ? 
O3T K2 O23 118.7(4) . 16 ? 
O3T K2 O23 56.9(4) 16 16 ? 
O2T K2 O23 118.6(4) . 16 ? 
O2T K2 O23 58.0(3) 16 16 ? 
O1W K2 O23 72.5(4) . . ? 
O3T K2 O23 56.9(4) . . ? 
O3T K2 O23 118.7(4) 16 . ? 
O2T K2 O23 58.0(3) . . ? 
O2T K2 O23 118.6(4) 16 . ? 
O23 K2 O23 145.1(8) 16 . ? 
O1W K2 W2 80.9(3) . 16 ? 
O3T K2 W2 91.7(3) . 16 ? 
O3T K2 W2 86.3(3) 16 16 ? 
O2T K2 W2 148.8(4) . 16 ? 
O2T K2 W2 28.1(2) 16 16 ? 
O23 K2 W2 30.3(2) 16 16 ? 
O23 K2 W2 140.2(4) . 16 ? 
O1W K2 W2 80.9(3) . . ? 
O3T K2 W2 86.3(3) . . ? 
O3T K2 W2 91.7(3) 16 . ? 
O2T K2 W2 28.1(2) . . ? 
O2T K2 W2 148.8(4) 16 . ? 
O23 K2 W2 140.2(4) 16 . ? 
O23 K2 W2 30.3(2) . . ? 
W2 K2 W2 161.8(5) 16 . ? 
O1W K2 W3 81.3(2) . 16 ? 
O3T K2 W3 150.3(4) . 16 ? 
O3T K2 W3 25.6(3) 16 16 ? 
O2T K2 W3 89.7(3) . 16 ? 
O2T K2 W3 88.8(3) 16 16 ? 
O23 K2 W3 31.9(2) 16 16 ? 
O23 K2 W3 139.3(4) . 16 ? 
W2 K2 W3 60.71(5) 16 16 ? 
W2 K2 W3 116.19(13) . 16 ? 
O1W K2 W3 81.3(2) . . ? 
O3T K2 W3 25.6(3) . . ? 
O3T K2 W3 150.3(4) 16 . ? 
O2T K2 W3 88.8(3) . . ? 
O2T K2 W3 89.7(3) 16 . ? 
O23 K2 W3 139.3(4) 16 . ? 
O23 K2 W3 31.9(2) . . ? 
W2 K2 W3 116.19(13) 16 . ? 
W2 K2 W3 60.71(5) . . ? 
W3 K2 W3 162.6(5) 16 . ? 
O1W K2 K1 52.3(2) . . ? 
O3T K2 K1 125.9(5) . . ? 
O3T K2 K1 43.8(3) 16 . ? 
O2T K2 K1 43.2(3) . . ? 
O2T K2 K1 128.5(5) 16 . ? 
O23 K2 K1 80.2(4) 16 . ? 
O23 K2 K1 78.7(4) . . ? 
W2 K2 K1 107.8(3) 16 . ? 
W2 K2 K1 60.08(19) . . ? 
W3 K2 K1 60.64(18) 16 . ? 
W3 K2 K1 107.8(3) . . ? 
O2SN K3 O2SN 82.1(6) . 23 ? 
O2SN K3 O2W 114.8(11) . 3 ? 
O2SN K3 O2W 114.8(11) 23 3 ? 
O2SN K3 K3 13.24(17) . 4 ? 
O2SN K3 K3 87.4(3) 23 4 ? 
O2W K3 K3 123.4(8) 3 4 ? 
O2SN K3 K3 87.4(3) . 3 ? 
O2SN K3 K3 13.24(17) 23 3 ? 
O2W K3 K3 123.4(8) 3 3 ? 
K3 K3 K3 89.997(1) 4 3 ? 
O2SN K3 O2SN 152.4(4) . 22 ? 
O2SN K3 O2SN 86.65(8) 23 22 ? 
O2W K3 O2SN 48.8(5) 3 22 ? 
K3 K3 O2SN 165.64(18) 4 22 ? 
K3 K3 O2SN 87.2(3) 3 22 ? 
O2SN K3 O2SN 86.65(8) . 3 ? 
O2SN K3 O2SN 152.4(4) 23 3 ? 
O2W K3 O2SN 48.8(5) 3 3 ? 
K3 K3 O2SN 87.2(3) 4 3 ? 
K3 K3 O2SN 165.64(18) 3 3 ? 
O2SN K3 O2SN 92.0(7) 22 3 ? 
O2SN K3 K3 77.02(16) . 18 ? 
O2SN K3 K3 77.02(16) 23 18 ? 
O2W K3 K3 51.1(16) 3 18 ? 
K3 K3 K3 89.997(1) 4 18 ? 
K3 K3 K3 89.997(1) 3 18 ? 
O2SN K3 K3 75.93(17) 22 18 ? 
O2SN K3 K3 75.93(17) 3 18 ? 
O2SN K3 Sn1B 154.8(4) . 3 ? 
O2SN K3 Sn1B 72.8(4) 23 3 ? 
O2W K3 Sn1B 76.3(6) 3 3 ? 
K3 K3 Sn1B 157.3(3) 4 3 ? 
K3 K3 Sn1B 68.2(3) 3 3 ? 
O2SN K3 Sn1B 27.6(4) 22 3 ? 
O2SN K3 Sn1B 115.5(5) 3 3 ? 
K3 K3 Sn1B 96.1(4) 18 3 ? 
O2SN K3 Sn1B 72.8(4) . . ? 
O2SN K3 Sn1B 154.8(4) 23 . ? 
O2W K3 Sn1B 76.3(6) 3 . ? 
K3 K3 Sn1B 68.2(3) 4 . ? 
K3 K3 Sn1B 157.3(3) 3 . ? 
O2SN K3 Sn1B 115.5(5) 22 . ? 
O2SN K3 Sn1B 27.6(4) 3 . ? 
K3 K3 Sn1B 96.1(4) 18 . ? 
Sn1B K3 Sn1B 132.3(5) 3 . ? 
O2SN K3 K3 43.9(3) . 2 ? 
O2SN K3 K3 43.9(3) 23 2 ? 
O2W K3 K3 141.1(16) 3 2 ? 
K3 K3 K3 44.998(1) 4 2 ? 
K3 K3 K3 45.0 3 2 ? 
O2SN K3 K3 130.6(3) 22 2 ? 
O2SN K3 K3 130.6(3) 3 2 ? 
K3 K3 K3 90.0 18 2 ? 
Sn1B K3 K3 112.9(3) 3 2 ? 
Sn1B K3 K3 112.9(3) . 2 ? 
O2SN K3 K3 78.4(3) . 20 ? 
O2SN K3 K3 37.4(5) 23 20 ? 
O2W K3 K3 82.4(15) 3 20 ? 
K3 K3 K3 90.0 4 20 ? 
K3 K3 K3 50.3(5) 3 20 ? 
O2SN K3 K3 77.4(3) 22 20 ? 
O2SN K3 K3 115.6(5) 3 20 ? 
K3 K3 K3 39.7(5) 18 20 ? 
Sn1B K3 K3 81.1(3) 3 20 ? 
Sn1B K3 K3 132.2(7) . 20 ? 
K3 K3 K3 63.1(3) 2 20 ? 
K2 O1W K2 180.000(1) 25 . ? 
K2 O1W K1 90.000(1) 25 . ? 
K2 O1W K1 90.000(1) . . ? 
K2 O1W K1 90.000(1) 25 25 ? 
K2 O1W K1 90.000(1) . 25 ? 
K1 O1W K1 179.999(1) . 25 ? 
K3 O2W K3 78(3) 19 4 ? 
 
_diffrn_measured_fraction_theta_max    0.960 
_diffrn_reflns_theta_full              29.55 
_diffrn_measured_fraction_theta_full   0.960 
_refine_diff_density_max    4.261 
_refine_diff_density_min   -4.401 
_refine_diff_density_rms    0.461 
