#------------------------------------------------------------------------------
#$Date: 2018-10-05 15:19:55 +0300 (Fri, 05 Oct 2018) $
#$Revision: 211332 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/34/27/4342755.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_4342755
loop_
_publ_author_name
'Winter, Ross S.'
'Long, De-Liang'
'Cronin, Leroy'
_publ_section_title
;
 Synthesis and Characterization of a Series of [M2(β-SiW8O31)2](n-)
 Clusters and Mechanistic Insight into the Reorganization of {β-SiW8O31}
 into {α-SiW9O34}.
;
_journal_issue                   8
_journal_name_full               'Inorganic chemistry'
_journal_page_first              4151
_journal_page_last               4155
_journal_paper_doi               10.1021/acs.inorgchem.5b00405
_journal_volume                  54
_journal_year                    2015
_chemical_formula_sum            'Cu4 H82 Na12 O109 Si2 W18'
_chemical_formula_weight         5722.17
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 92.337(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   13.0719(2)
_cell_length_b                   17.7002(3)
_cell_length_c                   21.0088(4)
_cell_measurement_reflns_used    18414
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      29.0
_cell_measurement_theta_min      3.11
_cell_volume                     4856.87(14)
_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_collection
;
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_molecular_graphics    Diamond3
_computing_publication_material  WinGX
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-2008 (Sheldick, 2008)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini ultra'
_diffrn_measurement_method       'ω & π scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0518
_diffrn_reflns_av_unetI/netI     0.0380
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            49932
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.999
_diffrn_reflns_theta_min         2.780
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    22.283
_exptl_absorpt_correction_T_max  0.261
_exptl_absorpt_correction_T_min  0.101
_exptl_absorpt_correction_type   analytical
_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_crystal_colour            blue
_exptl_crystal_density_diffrn    3.913
_exptl_crystal_density_method    none
_exptl_crystal_description       block
_exptl_crystal_F_000             5124
_exptl_crystal_size_max          0.207
_exptl_crystal_size_mid          0.105
_exptl_crystal_size_min          0.086
_refine_diff_density_max         1.94
_refine_diff_density_min         -1.03
_refine_diff_density_rms         0.24
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     666
_refine_ls_number_reflns         9514
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.0359
_refine_ls_R_factor_gt           0.0269
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0217P)²+26.7531P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0583
_refine_ls_wR_factor_ref         0.0616
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8091
_reflns_number_total             9514
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            Cu4W18.cif
_cod_data_source_block           rw1090e2
_cod_depositor_comments
;Adding full bibliography for 4342749--4342755.cif.

The following automatic conversions were performed:

'_atom_sites_solution_primary' value 'direct methods' was changed to
'direct'.

Automatic conversion script
Id: cif_fix_values 6452 2018-10-05 10:23:21Z andrius 
;
_cod_database_code               4342755
_shelx_shelxl_version_number     2014/7
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_estimated_absorpt_t_min   0.091
_shelx_estimated_absorpt_t_max   0.250
loop_
_space_group_symop_operation_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'
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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
W1 W -0.32531(2) 0.13209(2) 0.06091(2) 0.01383(8) Uani 1 1 d . . .
W2 W -0.21336(2) 0.24486(2) 0.17386(2) 0.01531(8) Uani 1 1 d . . .
W3 W -0.21612(2) 0.05231(2) 0.18940(2) 0.01383(8) Uani 1 1 d . . .
W4 W -0.04948(2) 0.33111(2) 0.05339(2) 0.01585(8) Uani 1 1 d . . .
W5 W -0.16136(2) 0.21715(2) -0.05876(2) 0.01354(8) Uani 1 1 d . . .
W6 W 0.09480(2) 0.22059(2) -0.04119(2) 0.01395(8) Uani 1 1 d . . .
W7 W 0.06954(2) 0.24324(2) 0.19923(2) 0.01448(8) Uani 1 1 d . . .
W8 W 0.21241(2) 0.13585(2) 0.10251(2) 0.01317(8) Uani 1 1 d . . .
W9 W 0.06539(2) 0.05159(2) 0.20911(2) 0.01327(8) Uani 1 1 d . . .
Cu1 Cu -0.19407(7) -0.03752(6) 0.04103(5) 0.0141(2) Uani 1 1 d . . .
Cu2 Cu -0.04873(7) 0.03602(6) -0.05774(5) 0.0140(2) Uani 1 1 d . . .
Na1 Na 0.0456(3) 0.5576(2) 0.19824(17) 0.0131(8) Uani 0.8 1 d P A 1
Na2 Na -0.1286(2) 0.2704(2) 0.40486(16) 0.0231(8) Uani 1 1 d . A 1
Na3 Na 0.0321(2) 0.4134(2) 0.32289(17) 0.0255(8) Uani 1 1 d . A 1
Na4 Na 0.0531(3) -0.1180(2) 0.32105(19) 0.0245(9) Uani 0.9 1 d P A 1
Na5 Na -0.0384(3) 0.2509(2) -0.21462(18) 0.0172(8) Uani 0.85 1 d P B 1
Na6 Na -0.1265(10) 0.0558(7) 0.4209(6) 0.030(3) Uani 0.3 1 d P A 1
Na7 Na 0.1260(6) 0.1536(4) 0.5165(4) 0.0268(19) Uani 0.45 1 d P A 1
Na8 Na 0.1923(9) 0.5599(8) 0.0667(6) 0.049(3) Uiso 0.35 1 d P A 1
Na8' Na 0.2310(8) 0.4711(7) 0.0869(5) 0.034(3) Uiso 0.35 1 d P C 2
Si1 Si -0.05486(15) 0.12850(13) 0.07422(10) 0.0114(4) Uani 1 1 d . . .
O1 O -0.4535(4) 0.1386(3) 0.0359(3) 0.0188(13) Uani 1 1 d . . .
O2 O -0.2845(4) 0.0478(3) 0.0226(3) 0.0167(12) Uani 1 1 d . . .
O3 O -0.2655(4) 0.1996(3) 0.0016(3) 0.0149(12) Uani 1 1 d . . .
O4 O -0.3408(4) 0.0788(3) 0.1405(3) 0.0165(12) Uani 1 1 d . . .
O5 O -0.1642(4) 0.1354(3) 0.1103(3) 0.0150(12) Uani 1 1 d . . .
O6 O -0.2618(4) 0.3156(3) 0.2214(3) 0.0185(13) Uani 1 1 d . . .
O7 O -0.1593(4) 0.3019(3) 0.1058(3) 0.0148(12) Uani 1 1 d . . .
O8 O -0.0749(4) 0.2404(3) 0.2061(3) 0.0154(12) Uani 1 1 d . . .
O9 O -0.3272(4) 0.2229(3) 0.1203(3) 0.0164(12) Uani 1 1 d . . .
O10 O -0.2374(4) 0.1580(3) 0.2243(3) 0.0165(12) Uani 1 1 d . . .
O11 O -0.2692(4) 0.0050(3) 0.2519(3) 0.0195(13) Uani 1 1 d . . .
O12 O -0.0781(4) 0.0619(3) 0.2200(3) 0.0162(12) Uani 1 1 d . . .
O13 O -0.1945(4) -0.0226(3) 0.1335(3) 0.0157(12) Uani 1 1 d . . .
O14 O 0.0607(4) 0.3203(3) -0.0011(3) 0.0160(12) Uani 1 1 d . . .
O15 O -0.1430(4) 0.3174(3) -0.0182(3) 0.0167(12) Uani 1 1 d . . .
O16 O -0.0542(4) 0.4285(3) 0.0607(3) 0.0214(13) Uani 1 1 d . . .
O17 O -0.0461(4) 0.2001(3) 0.0253(3) 0.0150(12) Uani 1 1 d . . .
O18 O 0.0376(4) 0.3041(3) 0.1245(3) 0.0191(13) Uani 1 1 d . . .
O19 O -0.2371(4) 0.2461(3) -0.1238(3) 0.0200(13) Uani 1 1 d . . .
O20 O -0.1446(4) 0.1177(3) -0.0723(3) 0.0165(12) Uani 1 1 d . . .
O21 O -0.0263(4) 0.2381(3) -0.0936(3) 0.0146(12) Uani 1 1 d . . .
O22 O 0.0967(4) 0.1196(3) -0.0551(3) 0.0156(12) Uani 1 1 d . . .
O23 O -0.3123(4) 0.2449(3) 0.4108(3) 0.0191(13) Uani 1 1 d . . .
O24 O 0.1726(4) 0.2055(3) 0.0384(3) 0.0147(12) Uani 1 1 d . . .
O25 O 0.1024(4) 0.3124(3) 0.2537(3) 0.0208(13) Uani 1 1 d . . .
O26 O 0.1968(4) 0.2231(3) 0.1641(3) 0.0159(12) Uani 1 1 d . . .
O27 O 0.0403(4) 0.1368(3) 0.1278(3) 0.0128(12) Uani 1 1 d . . .
O28 O 0.0787(4) 0.1555(3) 0.2498(3) 0.0167(12) Uani 1 1 d . . .
O29 O 0.1838(4) 0.0568(3) 0.0511(3) 0.0153(12) Uani 1 1 d . . .
O30 O -0.1466(4) 0.3879(4) 0.4634(3) 0.0227(14) Uani 1 1 d . . .
O31 O 0.3452(4) 0.1426(3) 0.1010(3) 0.0176(13) Uani 1 1 d . . .
O32 O 0.2022(4) 0.0760(3) 0.1794(3) 0.0149(12) Uani 1 1 d . . .
O33 O 0.1028(4) 0.0010(3) 0.2765(3) 0.0166(12) Uani 1 1 d . . .
O34 O 0.0470(4) -0.0186(3) 0.1490(3) 0.0153(12) Uani 1 1 d . . .
O35 O -0.0482(4) 0.0479(3) 0.0365(2) 0.0118(11) Uani 1 1 d . . .
O51 O -0.0478(4) 0.4440(4) 0.2102(3) 0.0256(14) Uani 1 1 d . . .
O52 O 0.0278(5) 0.4763(4) 0.4318(3) 0.0274(15) Uani 1 1 d . . .
O53 O 0.2132(5) 0.4325(4) 0.3349(3) 0.0333(16) Uani 1 1 d . . .
O54 O 0.1844(6) 0.4679(5) 0.1868(6) 0.084(4) Uani 1 1 d . A 1
O55 O 0.0280(4) 0.5564(4) 0.3073(3) 0.0240(14) Uani 1 1 d . A 1
O56 O 0.1727(4) 0.6531(4) 0.2157(3) 0.0265(15) Uani 1 1 d . A 1
O57' O 0.0888(9) 0.5552(7) 0.0916(6) 0.021(3) Uiso 0.5 1 d P C 2
O57 O 0.0140(11) 0.5658(8) 0.0898(7) 0.039(4) Uiso 0.5 1 d P A 1
O58 O 0.0569(4) 0.1388(4) -0.2200(3) 0.0267(15) Uani 1 1 d . B 1
O59 O -0.0747(6) 0.2188(5) 0.5071(3) 0.049(2) Uani 1 1 d . A 1
O60 O 0.0912(5) 0.3431(4) -0.1955(3) 0.0314(16) Uani 1 1 d . B 1
O61 O 0.0520(4) 0.3028(4) 0.3959(3) 0.0278(15) Uani 1 1 d . . .
O62 O -0.1043(5) 0.1690(4) 0.3367(3) 0.0381(17) Uani 1 1 d . . .
O63 O -0.1474(4) 0.3693(4) 0.3293(3) 0.0243(14) Uani 1 1 d . . .
O64 O 0.1736(5) -0.1665(4) 0.2496(4) 0.046(2) Uani 1 1 d . . .
O65 O 0.2004(7) -0.1499(5) 0.4020(4) 0.065(3) Uani 1 1 d . . .
O66 O 0.0179(4) -0.2511(4) 0.3300(3) 0.0264(15) Uani 1 1 d . . .
O67 O -0.1132(8) -0.0832(6) 0.3611(5) 0.040(3) Uiso 0.65 1 d P A 1
O67' O -0.047(2) -0.0699(16) 0.3945(14) 0.071(8) Uiso 0.35 1 d P D 2
O68 O 0.0643(18) -0.0280(16) 0.4361(13) 0.081(7) Uiso 0.4 1 d P A 1
O69 O 0.1941(9) 0.4443(7) -0.0129(6) 0.063(3) Uiso 0.7 1 d P A 1
O70 O -0.2045(18) 0.0362(15) 0.3801(12) 0.076(7) Uiso 0.4 1 d P E 2
O71 O 0.1547(16) 0.0886(13) 0.3963(10) 0.105(7) Uiso 0.6 1 d P A 1
O71' O 0.097(3) 0.135(2) 0.3752(19) 0.138(13) Uiso 0.4 1 d P F 2
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
W W -0.8490 6.8722 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu 0.3201 1.2651 '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'
Si Si 0.0817 0.0704 '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'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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
O1 W1 O2 102.7(3) . .
O1 W1 O3 100.1(2) . .
O2 W1 O3 95.2(2) . .
O1 W1 O4 99.2(2) . .
O2 W1 O4 91.5(2) . .
O3 W1 O4 157.6(2) . .
O1 W1 O9 95.6(2) . .
O2 W1 O9 161.2(2) . .
O3 W1 O9 85.5(2) . .
O4 W1 O9 81.5(2) . .
O1 W1 O5 169.5(2) . .
O2 W1 O5 86.6(2) . .
O3 W1 O5 83.6(2) . .
O4 W1 O5 75.5(2) . .
O9 W1 O5 74.8(2) . .
O6 W2 O9 101.3(2) . .
O6 W2 O10 101.0(3) . .
O9 W2 O10 91.3(2) . .
O6 W2 O8 100.9(2) . .
O9 W2 O8 157.7(2) . .
O10 W2 O8 86.8(2) . .
O6 W2 O7 101.8(3) . .
O9 W2 O7 88.2(2) . .
O10 W2 O7 156.9(2) . .
O8 W2 O7 85.0(2) . .
O6 W2 O5 172.6(2) . .
O9 W2 O5 74.2(2) . .
O10 W2 O5 73.6(2) . .
O8 W2 O5 83.9(2) . .
O7 W2 O5 84.1(2) . .
O11 W3 O13 102.6(3) . .
O11 W3 O12 101.0(2) . .
O13 W3 O12 96.6(2) . .
O11 W3 O4 99.5(2) . .
O13 W3 O4 89.0(2) . .
O12 W3 O4 157.0(2) . .
O11 W3 O10 96.1(2) . .
O13 W3 O10 160.1(2) . .
O12 W3 O10 86.4(2) . .
O4 W3 O10 81.1(2) . .
O11 W3 O5 169.1(2) . .
O13 W3 O5 86.7(2) . .
O12 W3 O5 83.4(2) . .
O4 W3 O5 74.6(2) . .
O10 W3 O5 74.1(2) . .
O16 W4 O14 100.7(3) . .
O16 W4 O18 101.7(3) . .
O14 W4 O18 90.2(2) . .
O16 W4 O15 99.9(3) . .
O14 W4 O15 89.4(2) . .
O18 W4 O15 158.1(2) . .
O16 W4 O7 100.9(3) . .
O14 W4 O7 158.5(2) . .
O18 W4 O7 85.4(2) . .
O15 W4 O7 87.0(2) . .
O16 W4 O17 170.8(2) . .
O14 W4 O17 74.3(2) . .
O18 W4 O17 86.2(2) . .
O15 W4 O17 72.6(2) . .
O7 W4 O17 84.4(2) . .
O16 W4 Na8 60.9(3) . 3_565
O14 W4 Na8 90.9(3) . 3_565
O18 W4 Na8 162.5(3) . 3_565
O15 W4 Na8 39.4(3) . 3_565
O7 W4 Na8 99.6(3) . 3_565
O17 W4 Na8 110.9(2) . 3_565
O19 W5 O20 103.5(3) . .
O19 W5 O3 99.8(2) . .
O20 W5 O3 92.4(2) . .
O19 W5 O21 98.2(2) . .
O20 W5 O21 90.5(2) . .
O3 W5 O21 160.5(2) . .
O19 W5 O15 97.5(2) . .
O20 W5 O15 158.9(2) . .
O3 W5 O15 86.4(2) . .
O21 W5 O15 84.1(2) . .
O19 W5 O17 169.3(2) . .
O20 W5 O17 85.0(2) . .
O3 W5 O17 86.1(2) . .
O21 W5 O17 75.0(2) . .
O15 W5 O17 73.8(2) . .
O23 W6 O22 103.9(3) 4_665 .
O23 W6 O21 101.1(2) 4_665 .
O22 W6 O21 94.8(2) . .
O23 W6 O24 101.3(2) 4_665 .
O22 W6 O24 89.6(2) . .
O21 W6 O24 155.4(2) . .
O23 W6 O14 96.2(3) 4_665 .
O22 W6 O14 159.6(2) . .
O21 W6 O14 84.7(2) . .
O24 W6 O14 82.9(2) . .
O23 W6 O17 167.8(2) 4_665 .
O22 W6 O17 87.8(2) . .
O21 W6 O17 73.8(2) . .
O24 W6 O17 82.2(2) . .
O14 W6 O17 72.5(2) . .
O25 W7 O26 101.3(2) . .
O25 W7 O28 101.8(3) . .
O26 W7 O28 91.6(2) . .
O25 W7 O8 101.0(2) . .
O26 W7 O8 157.2(2) . .
O28 W7 O8 88.6(2) . .
O25 W7 O18 100.6(3) . .
O26 W7 O18 87.2(2) . .
O28 W7 O18 157.4(2) . .
O8 W7 O18 84.0(2) . .
O25 W7 O27 173.1(2) . .
O26 W7 O27 74.3(2) . .
O28 W7 O27 73.3(2) . .
O8 W7 O27 83.9(2) . .
O18 W7 O27 84.7(2) . .
O31 W8 O29 103.0(2) . .
O31 W8 O24 100.9(2) . .
O29 W8 O24 92.0(2) . .
O31 W8 O32 98.9(2) . .
O29 W8 O32 93.1(2) . .
O24 W8 O32 157.9(2) . .
O31 W8 O26 94.9(2) . .
O29 W8 O26 162.0(2) . .
O24 W8 O26 85.8(2) . .
O32 W8 O26 82.7(2) . .
O31 W8 O27 167.1(2) . .
O29 W8 O27 87.9(2) . .
O24 W8 O27 85.3(2) . .
O32 W8 O27 73.46(19) . .
O26 W8 O27 74.1(2) . .
O33 W9 O34 104.2(3) . .
O33 W9 O12 101.4(2) . .
O34 W9 O12 92.7(2) . .
O33 W9 O32 98.2(2) . .
O34 W9 O32 91.5(2) . .
O12 W9 O32 158.3(2) . .
O33 W9 O28 96.2(2) . .
O34 W9 O28 159.4(2) . .
O12 W9 O28 86.0(2) . .
O32 W9 O28 82.6(2) . .
O33 W9 O27 168.0(2) . .
O34 W9 O27 85.4(2) . .
O12 W9 O27 85.1(2) . .
O32 W9 O27 73.95(19) . .
O28 W9 O27 74.0(2) . .
O22 Cu1 O2 175.8(2) 3 .
O22 Cu1 O13 88.7(2) 3 .
O2 Cu1 O13 93.8(2) . .
O22 Cu1 O29 87.2(2) 3 3
O2 Cu1 O29 90.2(2) . 3
O13 Cu1 O29 175.7(2) . 3
O22 Cu1 O35 87.8(2) 3 .
O2 Cu1 O35 88.9(2) . .
O13 Cu1 O35 89.3(2) . .
O29 Cu1 O35 89.1(2) 3 .
O20 Cu2 O34 89.7(2) . 3
O20 Cu2 O35 176.2(2) . 3
O34 Cu2 O35 94.0(2) 3 3
O20 Cu2 O35 93.2(2) . .
O34 Cu2 O35 176.8(2) 3 .
O35 Cu2 O35 83.1(2) 3 .
O20 Cu2 O22 92.9(2) . .
O34 Cu2 O22 94.5(2) 3 .
O35 Cu2 O22 87.63(19) 3 .
O35 Cu2 O22 86.7(2) . .
O20 Cu2 O29 92.7(2) . 3
O34 Cu2 O29 89.3(2) 3 3
O35 Cu2 O29 86.57(19) 3 3
O35 Cu2 O29 89.3(2) . 3
O22 Cu2 O29 173.29(18) . 3
O20 Cu2 Cu2 134.69(18) . 3
O34 Cu2 Cu2 135.54(17) 3 3
O35 Cu2 Cu2 41.56(15) 3 3
O35 Cu2 Cu2 41.53(15) . 3
O22 Cu2 Cu2 86.19(13) . 3
O29 Cu2 Cu2 87.23(13) 3 3
O57 Na1 O55 163.7(4) . .
O57 Na1 O51 95.0(4) . .
O55 Na1 O51 79.3(2) . .
O57 Na1 O56 101.7(4) . .
O55 Na1 O56 87.2(2) . .
O51 Na1 O56 160.4(3) . .
O57 Na1 O54 92.7(5) . .
O55 Na1 O54 101.4(4) . .
O51 Na1 O54 81.2(3) . .
O56 Na1 O54 87.7(3) . .
O57 Na1 O60 80.4(4) . 3_565
O55 Na1 O60 86.0(2) . 3_565
O51 Na1 O60 103.1(2) . 3_565
O56 Na1 O60 89.9(2) . 3_565
O54 Na1 O60 172.1(4) . 3_565
O57 Na1 Na5 91.9(4) . 3_565
O55 Na1 Na5 84.6(2) . 3_565
O51 Na1 Na5 144.7(2) . 3_565
O56 Na1 Na5 45.78(17) . 3_565
O54 Na1 Na5 133.1(2) . 3_565
O60 Na1 Na5 44.14(17) 3_565 3_565
O57 Na1 Na8 44.4(4) . .
O55 Na1 Na8 151.7(3) . .
O51 Na1 Na8 113.8(3) . .
O56 Na1 Na8 72.9(3) . .
O54 Na1 Na8 58.9(4) . .
O60 Na1 Na8 113.3(3) 3_565 .
Na5 Na1 Na8 95.1(2) 3_565 .
O57 Na1 Na3 137.6(4) . .
O55 Na1 Na3 43.61(18) . .
O51 Na1 Na3 45.08(17) . .
O56 Na1 Na3 115.9(2) . .
O54 Na1 Na3 71.0(3) . .
O60 Na1 Na3 116.74(19) 3_565 .
Na5 Na1 Na3 128.16(14) 3_565 .
Na8 Na1 Na3 129.0(3) . .
O62 Na2 O63 99.8(3) . .
O62 Na2 O59 102.3(3) . .
O63 Na2 O59 153.5(3) . .
O62 Na2 O30 171.7(3) . .
O63 Na2 O30 72.4(2) . .
O59 Na2 O30 84.5(3) . .
O62 Na2 O61 88.7(3) . .
O63 Na2 O61 81.3(2) . .
O59 Na2 O61 84.8(3) . .
O30 Na2 O61 87.3(2) . .
O62 Na2 O23 92.7(2) . .
O63 Na2 O23 95.4(2) . .
O59 Na2 O23 97.8(3) . .
O30 Na2 O23 90.9(2) . .
O61 Na2 O23 176.6(3) . .
O62 Na2 Na3 98.3(2) . .
O63 Na2 Na3 40.44(15) . .
O59 Na2 Na3 121.0(2) . .
O30 Na2 Na3 73.91(17) . .
O61 Na2 Na3 41.04(17) . .
O23 Na2 Na3 135.67(19) . .
O62 Na2 Na6 44.4(3) . .
O63 Na2 Na6 142.7(3) . .
O59 Na2 Na6 62.8(3) . .
O30 Na2 Na6 143.8(3) . .
O61 Na2 Na6 103.7(3) . .
O23 Na2 Na6 79.4(3) . .
Na3 Na2 Na6 135.3(2) . .
O53 Na3 O63 166.3(3) . .
O53 Na3 O61 88.2(2) . .
O63 Na3 O61 78.2(2) . .
O53 Na3 O25 77.1(2) . .
O63 Na3 O25 100.2(2) . .
O61 Na3 O25 76.4(2) . .
O53 Na3 O52 84.4(2) . .
O63 Na3 O52 91.9(2) . .
O61 Na3 O52 78.2(2) . .
O25 Na3 O52 148.9(2) . .
O53 Na3 O55 83.7(2) . .
O63 Na3 O55 107.7(2) . .
O61 Na3 O55 149.2(2) . .
O25 Na3 O55 129.8(2) . .
O52 Na3 O55 71.4(2) . .
O53 Na3 O51 115.1(2) . .
O63 Na3 O51 76.7(2) . .
O61 Na3 O51 138.6(2) . .
O25 Na3 O51 76.3(2) . .
O52 Na3 O51 134.6(2) . .
O55 Na3 O51 70.8(2) . .
O53 Na3 Na1 84.3(2) . .
O63 Na3 Na1 109.28(19) . .
O61 Na3 Na1 168.2(2) . .
O25 Na3 Na1 93.03(18) . .
O52 Na3 Na1 109.94(19) . .
O55 Na3 Na1 38.68(15) . .
O51 Na3 Na1 40.11(15) . .
O53 Na3 Na2 128.1(2) . .
O63 Na3 Na2 38.27(16) . .
O61 Na3 Na2 40.04(15) . .
O25 Na3 Na2 90.58(18) . .
O52 Na3 Na2 81.33(18) . .
O55 Na3 Na2 135.93(18) . .
O51 Na3 Na2 110.24(17) . .
Na1 Na3 Na2 147.29(12) . .
O64 Na4 O33 82.8(2) . .
O64 Na4 O66 80.2(3) . .
O33 Na4 O66 160.4(3) . .
O64 Na4 O67 158.4(4) . .
O33 Na4 O67 99.9(3) . .
O66 Na4 O67 92.5(3) . .
O64 Na4 O58 77.7(3) . 3
O33 Na4 O58 87.4(2) . 3
O66 Na4 O58 79.6(2) . 3
O67 Na4 O58 81.0(3) . 3
O64 Na4 O65 80.9(3) . .
O33 Na4 O65 104.0(3) . .
O66 Na4 O65 82.8(3) . .
O67 Na4 O65 118.6(4) . .
O58 Na4 O65 154.3(3) 3 .
O64 Na4 O68 135.5(5) . .
O33 Na4 O68 80.7(6) . .
O66 Na4 O68 118.5(6) . .
O67 Na4 O68 65.7(6) . .
O58 Na4 O68 141.7(5) 3 .
O65 Na4 O68 63.8(5) . .
O64 Na4 Na5 47.6(2) . 3
O33 Na4 Na5 112.1(2) . 3
O66 Na4 Na5 48.60(18) . 3
O67 Na4 Na5 113.0(3) . 3
O58 Na4 Na5 45.90(17) 3 3
O65 Na4 Na5 108.5(2) . 3
O68 Na4 Na5 166.9(6) . 3
O58 Na5 O60 102.3(3) . .
O58 Na5 O64 81.1(3) . 3
O60 Na5 O64 171.3(3) . 3
O58 Na5 O56 165.9(3) . 3_565
O60 Na5 O56 91.8(3) . 3_565
O64 Na5 O56 84.8(2) 3 3_565
O58 Na5 O66 82.7(2) . 3
O60 Na5 O66 93.5(2) . 3
O64 Na5 O66 78.9(3) 3 3
O56 Na5 O66 95.6(2) 3_565 3
O58 Na5 O21 87.8(2) . .
O60 Na5 O21 83.0(2) . .
O64 Na5 O21 105.3(3) 3 .
O56 Na5 O21 95.0(2) 3_565 .
O66 Na5 O21 169.0(2) 3 .
O58 Na5 Na4 51.02(19) . 3
O60 Na5 Na4 129.5(2) . 3
O64 Na5 Na4 46.96(19) 3 3
O56 Na5 Na4 118.4(2) 3_565 3
O66 Na5 Na4 47.54(18) 3 3
O21 Na5 Na4 128.4(2) . 3
O58 Na5 Na1 149.6(2) . 3_565
O60 Na5 Na1 47.32(18) . 3_565
O64 Na5 Na1 128.7(2) 3 3_565
O56 Na5 Na1 44.48(17) 3_565 3_565
O66 Na5 Na1 95.9(2) 3 3_565
O21 Na5 Na1 89.35(17) . 3_565
Na4 Na5 Na1 142.11(15) 3 3_565
O62 Na6 O67 110.6(5) . .
O62 Na6 O69 116.4(5) . 4_566
O67 Na6 O69 107.2(5) . 4_566
O62 Na6 O68 109.6(7) . .
O67 Na6 O68 61.8(6) . .
O69 Na6 O68 133.1(8) 4_566 .
O62 Na6 Na2 37.1(2) . .
O67 Na6 Na2 147.6(5) . .
O69 Na6 Na2 92.4(4) 4_566 .
O68 Na6 Na2 121.4(6) . .
O62 Na6 Na7 157.1(5) . 3_556
O67 Na6 Na7 46.8(3) . 3_556
O69 Na6 Na7 79.7(4) 4_566 3_556
O68 Na6 Na7 59.5(6) . 3_556
Na2 Na6 Na7 165.5(4) . 3_556
O62 Na6 Na7 84.5(4) . .
O67 Na6 Na7 121.6(4) . .
O69 Na6 Na7 115.3(5) 4_566 .
O68 Na6 Na7 60.0(6) . .
Na2 Na6 Na7 68.4(2) . .
Na7 Na6 Na7 103.9(3) 3_556 .
O71 Na7 O59 104.9(5) . .
O71 Na7 O67 129.9(6) . 3_556
O59 Na7 O67 98.6(3) . 3_556
O71 Na7 O3 100.4(5) . 4_666
O59 Na7 O3 94.6(3) . 4_666
O67 Na7 O3 121.2(4) 3_556 4_666
O71 Na7 Na8 39.2(5) . 2_545
O59 Na7 Na8 144.1(4) . 2_545
O67 Na7 Na8 108.3(4) 3_556 2_545
O3 Na7 Na8 91.5(3) 4_666 2_545
O71 Na7 Na6 85.2(5) . 3_556
O59 Na7 Na6 113.1(3) . 3_556
O67 Na7 Na6 44.8(3) 3_556 3_556
O3 Na7 Na6 149.5(3) 4_666 3_556
Na8 Na7 Na6 73.9(3) 2_545 3_556
O71 Na7 Na6 62.0(5) . .
O59 Na7 Na6 55.2(3) . .
O67 Na7 Na6 100.2(3) 3_556 .
O3 Na7 Na6 133.0(3) 4_666 .
Na8 Na7 Na6 96.0(3) 2_545 .
Na6 Na7 Na6 76.1(3) 3_556 .
O71 Na8 O57 143.5(9) 2 .
O71 Na8 O15 99.4(8) 2 3_565
O57 Na8 O15 78.8(5) . 3_565
O71 Na8 O69 112.0(8) 2 .
O57 Na8 O69 101.2(6) . .
O15 Na8 O69 115.3(6) 3_565 .
O71 Na8 O54 83.7(7) 2 .
O57 Na8 O54 77.7(5) . .
O15 Na8 O54 143.5(6) 3_565 .
O69 Na8 O54 96.5(5) . .
O71 Na8 Na1 104.6(7) 2 .
O57 Na8 Na1 42.1(4) . .
O15 Na8 Na1 101.4(4) 3_565 .
O69 Na8 Na1 121.4(5) . .
O54 Na8 Na1 43.8(2) . .
O71 Na8 Na7 54.8(6) 2 2
O57 Na8 Na7 141.2(6) . 2
O15 Na8 Na7 62.6(3) 3_565 2
O69 Na8 Na7 91.6(5) . 2
O54 Na8 Na7 137.5(5) . 2
Na1 Na8 Na7 146.9(5) . 2
O71 Na8 W4 124.3(8) 2 3_565
O57 Na8 W4 69.0(5) . 3_565
O15 Na8 W4 29.4(2) 3_565 3_565
O69 Na8 W4 89.3(4) . 3_565
O54 Na8 W4 146.7(4) . 3_565
Na1 Na8 W4 106.1(3) . 3_565
Na7 Na8 W4 74.7(3) 2 3_565
O65 Na8' O57' 150.0(6) 2 .
O35 Si1 O17 111.4(3) . .
O35 Si1 O27 110.8(3) . .
O17 Si1 O27 106.7(3) . .
O35 Si1 O5 110.6(3) . .
O17 Si1 O5 108.4(3) . .
O27 Si1 O5 108.8(3) . .
W1 O2 Cu1 138.4(3) . .
W1 O3 W5 148.0(3) . .
W1 O3 Na7 105.5(3) . 4_565
W5 O3 Na7 106.3(3) . 4_565
W1 O4 W3 117.3(3) . .
Si1 O5 W1 125.6(3) . .
Si1 O5 W3 124.2(3) . .
W1 O5 W3 91.02(18) . .
Si1 O5 W2 124.0(3) . .
W1 O5 W2 90.59(17) . .
W3 O5 W2 91.17(18) . .
W2 O7 W4 151.9(3) . .
W7 O8 W2 154.5(3) . .
W2 O9 W1 120.3(3) . .
W2 O10 W3 121.0(3) . .
W3 O12 W9 151.2(3) . .
W3 O13 Cu1 138.8(3) . .
W4 O14 W6 122.0(3) . .
W4 O15 W5 120.9(3) . .
W4 O15 Na8 111.1(4) . 3_565
W5 O15 Na8 125.8(4) . 3_565
Si1 O17 W5 121.6(3) . .
Si1 O17 W6 124.1(3) . .
W5 O17 W6 91.57(19) . .
Si1 O17 W4 126.3(3) . .
W5 O17 W4 92.53(18) . .
W6 O17 W4 91.13(19) . .
W4 O18 W7 151.5(3) . .
W5 O20 Cu2 142.3(3) . .
W6 O21 W5 119.2(3) . .
W6 O21 Na5 127.1(3) . .
W5 O21 Na5 111.5(2) . .
W6 O22 Cu1 136.5(3) . 3
W6 O22 Cu2 126.4(2) . .
Cu1 O22 Cu2 93.2(2) 3 .
W6 O23 Na2 132.9(3) 4_566 .
W8 O24 W6 145.7(3) . .
W7 O25 Na3 143.9(3) . .
W7 O26 W8 120.5(3) . .
Si1 O27 W9 122.0(3) . .
Si1 O27 W8 123.5(3) . .
W9 O27 W8 93.14(18) . .
Si1 O27 W7 125.9(3) . .
W9 O27 W7 92.04(19) . .
W8 O27 W7 91.00(17) . .
W7 O28 W9 120.5(3) . .
W8 O29 Cu1 134.6(3) . 3
W8 O29 Cu2 128.9(3) . 3
Cu1 O29 Cu2 91.0(2) 3 3
W8 O32 W9 118.5(2) . .
W9 O33 Na4 134.5(3) . .
W9 O34 Cu2 143.5(3) . 3
Si1 O35 Cu2 126.1(3) . 3
Si1 O35 Cu2 125.1(3) . .
Cu2 O35 Cu2 96.9(2) 3 .
Si1 O35 Cu1 117.7(3) . .
Cu2 O35 Cu1 91.2(2) 3 .
Cu2 O35 Cu1 90.11(19) . .
Na1 O51 Na3 94.8(2) . .
Na1 O54 Na8 77.3(4) . .
Na1 O55 Na3 97.7(2) . .
Na1 O56 Na5 89.7(2) . 3_565
Na1 O57 Na8 93.5(6) . .
Na5 O58 Na4 83.1(2) . 3
Na2 O59 Na7 116.6(3) . .
Na5 O60 Na1 88.5(2) . 3_565
Na2 O61 Na3 98.9(2) . .
Na2 O62 Na6 98.5(4) . .
Na2 O63 Na3 101.3(2) . .
Na4 O64 Na5 85.4(2) . 3
Na4 O66 Na5 83.9(2) . 3
Na4 O67 Na6 117.0(5) . .
Na4 O67 Na7 106.6(4) . 3_556
Na6 O67 Na7 88.4(4) . 3_556
Na4 O68 Na6 100.1(8) . .
Na8 O69 Na6 110.3(6) . 4_665
Na8 O71 Na7 85.9(8) 2_545 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
W1 O1 1.740(5) .
W1 O2 1.786(5) .
W1 O3 1.917(5) .
W1 O4 1.937(6) .
W1 O9 2.036(6) .
W1 O5 2.311(5) .
W2 O6 1.738(6) .
W2 O9 1.869(5) .
W2 O10 1.901(6) .
W2 O8 1.908(5) .
W2 O7 1.909(5) .
W2 O5 2.453(6) .
W3 O11 1.726(6) .
W3 O13 1.802(6) .
W3 O12 1.898(5) .
W3 O4 1.948(5) .
W3 O10 2.032(6) .
W3 O5 2.339(5) .
W4 O16 1.732(6) .
W4 O14 1.885(5) .
W4 O18 1.902(5) .
W4 O15 1.914(5) .
W4 O7 1.916(5) .
W4 O17 2.393(6) .
W4 Na8 3.632(13) 3_565
W5 O19 1.732(6) .
W5 O20 1.798(6) .
W5 O3 1.923(5) .
W5 O21 1.973(5) .
W5 O15 1.980(6) .
W5 O17 2.295(5) .
W6 O23 1.722(5) 4_665
W6 O22 1.811(6) .
W6 O21 1.916(5) .
W6 O24 1.939(5) .
W6 O14 2.014(6) .
W6 O17 2.384(5) .
W7 O25 1.718(6) .
W7 O26 1.882(5) .
W7 O28 1.883(6) .
W7 O8 1.900(5) .
W7 O18 1.936(6) .
W7 O27 2.429(5) .
W8 O31 1.742(5) .
W8 O29 1.797(5) .
W8 O24 1.884(5) .
W8 O32 1.941(5) .
W8 O26 2.030(6) .
W8 O27 2.333(5) .
W9 O33 1.729(5) .
W9 O34 1.782(6) .
W9 O12 1.908(5) .
W9 O32 1.966(5) .
W9 O28 2.032(6) .
W9 O27 2.293(5) .
Cu1 O22 1.946(5) 3
Cu1 O2 1.947(6) .
Cu1 O13 1.960(5) .
Cu1 O29 1.976(5) 3
Cu1 O35 2.438(5) .
Cu2 O20 1.929(5) .
Cu2 O34 1.942(5) 3
Cu2 O35 1.990(5) 3
Cu2 O35 1.992(5) .
Cu2 O22 2.408(5) .
Cu2 O29 2.420(5) 3
Cu2 Cu2 2.9803(19) 3
Na1 O57 2.303(15) .
Na1 O55 2.312(7) .
Na1 O51 2.370(7) .
Na1 O56 2.388(7) .
Na1 O54 2.431(9) .
Na1 O60 2.506(8) 3_565
Na1 Na5 3.408(5) 3_565
Na1 Na8 3.427(14) .
Na1 Na3 3.666(5) .
Na2 O62 2.326(8) .
Na2 O63 2.370(7) .
Na2 O59 2.412(8) .
Na2 O30 2.433(7) .
Na2 O61 2.444(6) .
Na2 O23 2.452(6) .
Na2 Na3 3.753(5) .
Na2 Na6 3.813(13) .
Na3 O53 2.393(7) .
Na3 O63 2.482(6) .
Na3 O61 2.494(7) .
Na3 O25 2.503(7) .
Na3 O52 2.547(7) .
Na3 O55 2.552(7) .
Na3 O51 2.605(7) .
Na4 O64 2.380(8) .
Na4 O33 2.405(7) .
Na4 O66 2.409(7) .
Na4 O67 2.442(11) .
Na4 O58 2.542(8) 3
Na4 O65 2.579(11) .
Na4 O68 2.89(3) .
Na4 Na5 3.246(6) 3
Na5 O58 2.348(7) .
Na5 O60 2.374(7) .
Na5 O64 2.406(8) 3
Na5 O56 2.443(7) 3_565
Na5 O66 2.449(7) 3
Na5 O21 2.552(7) .
Na5 Na4 3.246(6) 3
Na5 Na1 3.408(5) 3_565
Na6 O62 2.696(15) .
Na6 O67 2.772(17) .
Na6 O69 2.774(18) 4_566
Na6 O68 2.91(3) .
Na6 Na7 3.933(15) 3_556
Na6 Na7 4.169(14) .
Na7 O71 2.81(2) .
Na7 O59 2.866(11) .
Na7 O67 2.869(14) 3_556
Na7 O3 2.982(9) 4_666
Na7 Na8 3.432(15) 2_545
Na7 Na6 3.933(15) 3_556
Na8 O71 2.18(2) 2
Na8 O57 2.402(19) .
Na8 O15 2.473(14) 3_565
Na8 O69 2.644(19) .
Na8 O54 3.007(18) .
Na8 Na7 3.432(15) 2
Na8 W4 3.632(13) 3_565
Na8' O65 2.330(14) 2
Na8' O57' 2.388(16) .
Si1 O35 1.636(6) .
Si1 O17 1.638(6) .
Si1 O27 1.650(5) .
Si1 O5 1.650(5) .
O3 Na7 2.982(9) 4_565
O15 Na8 2.473(14) 3_565
O22 Cu1 1.946(5) 3
O23 W6 1.722(5) 4_566
O29 Cu1 1.976(5) 3
O29 Cu2 2.420(5) 3
O34 Cu2 1.942(5) 3
O35 Cu2 1.990(5) 3
O56 Na5 2.443(7) 3_565
O58 Na4 2.542(8) 3
O60 Na1 2.507(8) 3_565
O64 Na5 2.406(8) 3
O65 Na8' 2.330(14) 2_545
O66 Na5 2.449(7) 3
O67 Na7 2.869(14) 3_556
O69 Na6 2.774(18) 4_665
O71 Na8 2.18(2) 2_545
