#------------------------------------------------------------------------------
#$Date: 2019-11-28 12:47:45 +0200 (Thu, 28 Nov 2019) $
#$Revision: 243839 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/70/23/7702361.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_7702361
loop_
_publ_author_name
'Khan, M. Ishaque'
'Cevik, Sabri'
'Hayashi, Randy'
_publ_section_title
;
 First 12-tungstovanadate Keggin compound: synthesis and crystal structure
 of [Me4N]7[VW12O40]·15H2O
;
_journal_issue                   10
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              1651
_journal_paper_doi               10.1039/a808760a
_journal_year                    1999
_chemical_formula_moiety         '7(C4 H12 N)+ (V W12 O40)7- 15(H2 O)'
_chemical_formula_structural     '7(C4 H12 N)+ (V W12 O40)7- 15(H2 O)'
_chemical_formula_sum            'C28 H114 N7 O55 V W12'
_chemical_formula_weight         3686.40
_space_group_IT_number           11
_space_group_name_Hall           '-P 2yb'
_space_group_name_H-M_alt        'P 1 21/m 1'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 1 21/m 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 100.302(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   12.9094(2)
_cell_length_b                   20.8420(6)
_cell_length_c                   15.1180(2)
_cell_measurement_reflns_used    6390
_cell_measurement_temperature    133(2)
_cell_measurement_theta_max      25.0
_cell_measurement_theta_min      3.0
_cell_volume                     4002.04(14)
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      133(2)
_diffrn_measurement_device       'Siemens P4/CCD'
_diffrn_measurement_method       'phi scan frames'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0294
_diffrn_reflns_av_sigmaI/netI    0.0459
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            19354
_diffrn_reflns_theta_max         29.13
_diffrn_reflns_theta_min         2.39
_diffrn_standards_decay_%        0.04
_diffrn_standards_number         602
_exptl_absorpt_coefficient_mu    17.377
_exptl_absorpt_correction_T_max  0.121
_exptl_absorpt_correction_T_min  0.072
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    3.059
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'opaque prism'
_exptl_crystal_F_000             3364
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.15
_refine_diff_density_max         2.759
_refine_diff_density_min         -5.204
_refine_diff_density_rms         0.359
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.066
_refine_ls_goodness_of_fit_obs   1.103
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     496
_refine_ls_number_reflns         9705
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.084
_refine_ls_restrained_S_obs      1.103
_refine_ls_R_factor_all          0.0591
_refine_ls_R_factor_obs          0.0439
_refine_ls_shift/esd_max         0.001
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0616P)²+52.2021P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1271
_refine_ls_wR_factor_obs         0.1157
_reflns_number_observed          7841
_reflns_number_total             9710
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            808760a.txt
_cod_data_source_block           97278
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0616P)^2^+52.2021P] where P=(Fo^2^+2Fc^2^)/3'
was changed to 'calc'. A new data item '_refine_ls_weighting_details'
was created with the value set to
'w=1/[\s^2^(Fo^2^)+(0.0616P)^2^+52.2021P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 6909 2019-04-08 15:41:33Z antanas 
;
_cod_original_sg_symbol_H-M      P21/m
_cod_database_code               7702361
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z'
'-x, -y, -z'
'x, -y-1/2, z'
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_thermal_displace_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_refinement_flags
W1 W 0.30579(5) 0.2500 0.04904(4) 0.02183(14) Uani 1 d S
W2 W 0.22223(3) 0.16930(2) 0.21312(3) 0.01750(10) Uani 1 d .
W3 W 0.55701(4) 0.16183(2) 0.09442(3) 0.02309(11) Uani 1 d .
W4 W 0.47405(3) 0.08095(2) 0.25825(3) 0.01957(10) Uani 1 d .
W5 W 0.38192(3) 0.16951(2) 0.44160(3) 0.01610(10) Uani 1 d .
W6 W 0.70065(4) 0.16218(2) 0.30022(3) 0.02343(11) Uani 1 d .
W7 W 0.60823(5) 0.2500 0.48072(4) 0.02322(14) Uani 1 d S
V1 V 0.4653(2) 0.2500 0.2620(2) 0.0302(6) Uani 1 d S
O1 O 0.2544(7) 0.2500 -0.0632(6) 0.014(2) Uani 1 d S
O2 O 0.1183(5) 0.1174(3) 0.2057(5) 0.0157(13) Uani 1 d .
O3 O 0.5908(6) 0.1320(3) -0.0019(4) 0.0180(14) Uani 1 d .
O4 O 0.4515(5) 0.0005(3) 0.2653(4) 0.0148(13) Uani 1 d .
O5 O 0.3294(5) 0.1189(3) 0.5113(4) 0.0106(12) Uani 1 d .
O6 O 0.8244(5) 0.1326(3) 0.3381(5) 0.0184(14) Uani 1 d .
O7 O 0.7019(7) 0.2500 0.5744(6) 0.016(2) Uani 1 d S
O12 O 0.2174(5) 0.1855(3) 0.0867(4) 0.0118(12) Uani 1 d .
O13 O 0.4153(5) 0.1880(3) 0.0538(4) 0.0105(12) Uani 1 d .
O22 O 0.1492(7) 0.2500 0.2176(6) 0.010(2) Uani 1 d S
O24 O 0.3358(5) 0.1123(3) 0.2105(4) 0.0105(12) Uani 1 d .
O25 O 0.2702(5) 0.1743(3) 0.3393(4) 0.0099(12) Uani 1 d .
O33 O 0.5921(7) 0.2500 0.0873(6) 0.013(2) Uani 1 d S
O34 O 0.5075(5) 0.0841(3) 0.1394(4) 0.0114(12) Uani 1 d .
O36 O 0.6879(5) 0.1480(3) 0.1748(4) 0.0133(13) Uani 1 d .
O45 O 0.4467(5) 0.1113(3) 0.3716(4) 0.0109(12) Uani 1 d .
O46 O 0.6234(5) 0.0822(3) 0.3064(4) 0.0119(12) Uani 1 d .
O55 O 0.3317(7) 0.2500 0.4821(6) 0.012(2) Uani 1 d S
O57 O 0.5143(5) 0.1864(3) 0.5165(4) 0.0113(12) Uani 1 d .
O66 O 0.7283(7) 0.2500 0.2836(6) 0.011(2) Uani 1 d S
O67 O 0.6622(5) 0.1870(3) 0.4110(4) 0.0102(12) Uani 1 d .
O122 O 0.3464(7) 0.2500 0.2043(5) 0.008(2) Uani 1 d S
O346 O 0.5273(5) 0.1862(3) 0.2373(4) 0.0096(12) Uani 1 d .
O557 O 0.4596(7) 0.2500 0.3686(5) 0.007(2) Uani 1 d S
N1 N 0.7450(7) 0.0453(4) 0.5859(6) 0.020(2) Uani 1 d .
C11 C 0.6329(8) 0.0351(5) 0.5381(7) 0.020(2) Uani 1 d .
H11A H 0.5856(8) 0.0415(5) 0.5797(7) 0.030 Uiso 1 d R
H11B H 0.6168(8) 0.0653(5) 0.4897(7) 0.030 Uiso 1 d R
H11C H 0.6250(8) -0.0077(5) 0.5146(7) 0.030 Uiso 1 d R
C12 C 0.7731(9) -0.0004(5) 0.6589(8) 0.025(2) Uani 1 d .
H12A H 0.7277(9) 0.0055(5) 0.7021(8) 0.037 Uiso 1 d R
H12B H 0.7650(9) -0.0433(5) 0.6353(8) 0.037 Uiso 1 d R
H12C H 0.8449(9) 0.0062(5) 0.6874(8) 0.037 Uiso 1 d R
C13 C 0.8180(11) 0.0345(11) 0.5191(9) 0.069(6) Uani 1 d .
H13A H 0.8897(11) 0.0406(11) 0.5484(9) 0.103 Uiso 1 d R
H13B H 0.8093(11) -0.0084(11) 0.4957(9) 0.103 Uiso 1 d R
H13C H 0.8011(11) 0.0647(11) 0.4707(9) 0.103 Uiso 1 d R
C14 C 0.7535(16) 0.1120(7) 0.6219(15) 0.095(9) Uani 1 d .
H14A H 0.7072(16) 0.1180(7) 0.6643(15) 0.142 Uiso 1 d R
H14B H 0.8248(16) 0.1197(7) 0.6509(15) 0.142 Uiso 1 d R
H14C H 0.7349(16) 0.1414(7) 0.5727(15) 0.142 Uiso 1 d R
N2 N 0.2690(7) 0.0410(4) -0.0797(6) 0.022(2) Uani 1 d .
C21 C 0.2218(11) -0.0187(6) -0.1258(9) 0.039(3) Uani 1 d .
H21A H 0.1525(11) -0.0251(6) -0.1126(9) 0.059 Uiso 1 d R
H21B H 0.2174(11) -0.0142(6) -0.1896(9) 0.059 Uiso 1 d R
H21C H 0.2651(11) -0.0550(6) -0.1050(9) 0.059 Uiso 1 d R
C22 C 0.3769(12) 0.0497(10) -0.1011(11) 0.062(5) Uani 1 d .
H22A H 0.4086(12) 0.0876(10) -0.0719(11) 0.092 Uiso 1 d R
H22B H 0.4195(12) 0.0130(10) -0.0803(11) 0.092 Uiso 1 d R
H22C H 0.3718(12) 0.0539(10) -0.1649(11) 0.092 Uiso 1 d R
C23 C 0.2774(13) 0.0377(8) 0.0193(9) 0.047(4) Uani 1 d .
H23A H 0.3080(13) 0.0767(8) 0.0456(9) 0.070 Uiso 1 d R
H23B H 0.2088(13) 0.0321(8) 0.0343(9) 0.070 Uiso 1 d R
H23C H 0.3214(13) 0.0021(8) 0.0421(9) 0.070 Uiso 1 d R
C24 C 0.1988(15) 0.0967(7) -0.1136(12) 0.061(5) Uani 1 d .
H24A H 0.2273(15) 0.1355(7) -0.0850(12) 0.091 Uiso 1 d R
H24B H 0.1943(15) 0.1005(7) -0.1775(12) 0.091 Uiso 1 d R
H24C H 0.1298(15) 0.0894(7) -0.1003(12) 0.091 Uiso 1 d R
N3 N 0.4667(11) 0.2500 0.7574(8) 0.026(3) Uani 1 d S
C31 C 0.4735(13) 0.2500 0.8566(10) 0.026(3) Uani 1 d S
H31A H 0.5111(13) 0.2125 0.8816(10) 0.039 Uiso 1 d R
H31B H 0.4039(13) 0.2500 0.8709(10) 0.039 Uiso 1 d SR
C32 C 0.5753(17) 0.2500 0.7364(13) 0.044(5) Uani 1 d S
H32A H 0.6123(17) 0.2126 0.7622(13) 0.065 Uiso 1 d R
H32B H 0.5718(17) 0.2500 0.6724(13) 0.065 Uiso 1 d SR
C33 C 0.4085(14) 0.1912(9) 0.7185(10) 0.058(5) Uani 1 d .
H33A H 0.4459(14) 0.1538(9) 0.7438(10) 0.087 Uiso 1 d R
H33B H 0.3389(14) 0.1910(9) 0.7325(10) 0.087 Uiso 1 d R
H33C H 0.4041(14) 0.1910(9) 0.6544(10) 0.087 Uiso 1 d R
N4 N 0.0350(9) 0.2500 0.4870(8) 0.016(2) Uani 1 d S
C41 C -0.0768(11) 0.2500 0.5041(11) 0.022(3) Uani 1 d S
H41A H -0.1124(11) 0.2124 0.4775(11) 0.033 Uiso 1 d R
H41B H -0.0770(11) 0.2500 0.5676(11) 0.033 Uiso 1 d SR
C42 C 0.0395(16) 0.2500 0.3882(10) 0.030(4) Uani 1 d S
H42A H 0.0045(16) 0.2124 0.3610(10) 0.046 Uiso 1 d R
H42B H 0.1113(16) 0.2500 0.3793(10) 0.046 Uiso 1 d SR
C43 C 0.0917(11) 0.1919(7) 0.5296(9) 0.043(4) Uani 1 d .
H43A H 0.0899(11) 0.1919(7) 0.5929(9) 0.064 Uiso 1 d R
H43B H 0.0578(11) 0.1538(7) 0.5027(9) 0.064 Uiso 1 d R
H43C H 0.1635(11) 0.1926(7) 0.5208(9) 0.064 Uiso 1 d R
N5 N 0.8936(9) 0.2500 0.0346(9) 0.027(3) Uani 1 d S
C51 C 0.7918(12) 0.2500 -0.0313(10) 0.027(3) Uani 1 d S
H51A H 0.7884(12) 0.2124 -0.0684(10) 0.040 Uiso 1 d R
H51B H 0.7338(12) 0.2500 0.0005(10) 0.040 Uiso 1 d SR
C52 C 0.9847(13) 0.2500 -0.0149(13) 0.035(4) Uani 1 d S
H52A H 0.9814(13) 0.2124 -0.0520(13) 0.053 Uiso 1 d R
H52B H 1.0495(13) 0.2500 0.0276(13) 0.053 Uiso 1 d SR
C53 C 0.8945(13) 0.1898(12) 0.0860(14) 0.100(10) Uani 1 d .
H53A H 0.9581(13) 0.1868(12) 0.1298(14) 0.151 Uiso 1 d R
H53B H 0.8348(13) 0.1879(12) 0.1157(14) 0.151 Uiso 1 d R
H53C H 0.8914(13) 0.1548(12) 0.0442(14) 0.151 Uiso 1 d R
O1S O 0.2924(6) 0.0474(4) 0.6675(5) 0.026(2) Uani 1 d .
H1SA H 0.3031(6) 0.0685(4) 0.6219(5) 0.031 Uiso 1 d R
H1SB H 0.3170(6) 0.0096(4) 0.6752(5) 0.031 Uiso 1 d R
O2S O 0.0733(7) 0.0543(4) 0.6539(6) 0.035(2) Uani 1 d .
H2SA H 0.0494(7) 0.0165(4) 0.6574(6) 0.042 Uiso 1 d R
H2SB H 0.1398(7) 0.0523(4) 0.6581(6) 0.042 Uiso 1 d R
O3S O 1.0031(8) 0.0691(4) 0.3354(8) 0.050(3) Uani 1 d .
H3SA H 1.0374(8) 0.0834(4) 0.2965(8) 0.060 Uiso 1 d R
H3SB H 0.9462(8) 0.0893(4) 0.3365(8) 0.060 Uiso 1 d R
O4S O 0.6547(8) 0.1023(4) -0.1630(6) 0.044(2) Uani 1 d .
H4SA H 0.6352(8) 0.1115(4) -0.1137(6) 0.053 Uiso 1 d R
H4SB H 0.6230(8) 0.0717(4) -0.1937(6) 0.053 Uiso 1 d R
O5S O 0.1251(12) 0.2500 -0.2315(8) 0.047(4) Uani 1 d S
H5SA H 0.1646(12) 0.2500 -0.1801(8) 0.057 Uiso 1 d SR
H5SB H 0.0830(12) 0.2183 -0.2384(8) 0.057 Uiso 0.50 d PR
O6S O -0.0103(8) 0.1483(6) 0.7460(8) 0.055(3) Uani 1 d .
H6SA H 0.0158(8) 0.1193(6) 0.7172(8) 0.066 Uiso 1 d R
H6SB H -0.0445(8) 0.1338(6) 0.7848(8) 0.066 Uiso 0.50 d PR
H6SC H 0.0319(8) 0.1800(6) 0.7529(8) 0.066 Uiso 0.50 d PR
O7S O 0.1219(10) -0.1021(7) 0.1290(11) 0.098(6) Uani 1 d .
H7SA H 0.1888(10) -0.1023(7) 0.1390(11) 0.117 Uiso 1 d R
H7SB H 0.0876(10) -0.1165(7) 0.1677(11) 0.117 Uiso 0.50 d PR
H7SC H 0.0939(10) -0.0657(7) 0.1148(11) 0.117 Uiso 0.50 d PR
O8S O 0.0328(10) 0.0129(9) 0.0843(11) 0.115(7) Uani 1 d .
H8SA H 0.0577(10) 0.0431(9) 0.1196(11) 0.138 Uiso 1 d R
H8SB H 0.0607(10) -0.0235(9) 0.0985(11) 0.138 Uiso 0.50 d PR
H8SC H 0.0112(10) 0.0045(9) 0.0291(11) 0.138 Uiso 0.50 d PR
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'
V V 0.3005 0.5294 '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'
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 O13 101.1(3) . 4_565
O1 W1 O13 101.0(3) . .
O13 W1 O13 85.3(4) 4_565 .
O1 W1 O12 98.6(3) . .
O13 W1 O12 160.3(3) 4_565 .
O13 W1 O12 89.4(3) . .
O1 W1 O12 98.6(3) . 4_565
O13 W1 O12 89.4(3) 4_565 4_565
O13 W1 O12 160.3(3) . 4_565
O12 W1 O12 89.2(4) . 4_565
O1 W1 O122 170.4(4) . .
O13 W1 O122 86.0(2) 4_565 .
O13 W1 O122 86.0(2) . .
O12 W1 O122 74.8(2) . .
O12 W1 O122 74.7(2) 4_565 .
O2 W2 O24 101.7(3) . .
O2 W2 O25 102.2(3) . .
O24 W2 O25 86.6(3) . .
O2 W2 O12 99.2(3) . .
O24 W2 O12 88.7(3) . .
O25 W2 O12 158.6(3) . .
O2 W2 O22 99.8(3) . .
O24 W2 O22 158.5(3) . .
O25 W2 O22 89.4(3) . .
O12 W2 O22 87.3(3) . .
O2 W2 O122 170.4(3) . .
O24 W2 O122 84.8(2) . .
O25 W2 O122 85.1(3) . .
O12 W2 O122 73.7(3) . .
O22 W2 O122 73.8(3) . .
O3 W3 O33 101.7(3) . .
O3 W3 O13 101.9(3) . .
O33 W3 O13 86.0(3) . .
O3 W3 O34 98.5(3) . .
O33 W3 O34 159.8(3) . .
O13 W3 O34 89.7(3) . .
O3 W3 O36 98.9(3) . .
O33 W3 O36 89.4(3) . .
O13 W3 O36 159.2(3) . .
O34 W3 O36 87.7(3) . .
O3 W3 O346 169.6(3) . .
O33 W3 O346 85.5(3) . .
O13 W3 O346 85.9(2) . .
O34 W3 O346 74.5(2) . .
O36 W3 O346 73.5(2) . .
O4 W4 O24 101.6(3) . .
O4 W4 O45 101.9(3) . .
O24 W4 O45 85.2(3) . .
O4 W4 O34 99.3(3) . .
O24 W4 O34 89.2(3) . .
O45 W4 O34 158.7(3) . .
O4 W4 O46 99.2(3) . .
O24 W4 O46 159.2(3) . .
O45 W4 O46 89.4(3) . .
O34 W4 O46 88.6(3) . .
O4 W4 O346 170.8(3) . .
O24 W4 O346 84.6(2) . .
O45 W4 O346 85.3(2) . .
O34 W4 O346 73.8(2) . .
O46 W4 O346 75.0(2) . .
O5 W5 O45 102.2(3) . .
O5 W5 O57 99.2(3) . .
O45 W5 O57 90.7(3) . .
O5 W5 O25 101.8(3) . .
O45 W5 O25 85.8(3) . .
O57 W5 O25 159.0(3) . .
O5 W5 O55 98.4(3) . .
O45 W5 O55 159.3(3) . .
O57 W5 O55 88.1(3) . .
O25 W5 O55 88.0(3) . .
O5 W5 O557 170.0(3) . .
O45 W5 O557 85.8(2) . .
O57 W5 O557 74.5(3) . .
O25 W5 O557 84.6(3) . .
O55 W5 O557 73.9(3) . .
O6 W6 O66 101.9(3) . .
O6 W6 O36 100.8(3) . .
O66 W6 O36 90.2(3) . .
O6 W6 O67 100.3(3) . .
O66 W6 O67 86.5(3) . .
O36 W6 O67 158.9(3) . .
O6 W6 O46 97.5(3) . .
O66 W6 O46 160.5(3) . .
O36 W6 O46 87.7(3) . .
O67 W6 O46 88.5(3) . .
O6 W6 O346 170.6(3) . .
O66 W6 O346 85.9(3) . .
O36 W6 O346 73.7(2) . .
O67 W6 O346 85.3(2) . .
O46 W6 O346 75.0(2) . .
O7 W7 O67 100.8(3) . 4_565
O7 W7 O67 100.8(3) . .
O67 W7 O67 87.8(4) 4_565 .
O7 W7 O57 99.0(3) . 4_565
O67 W7 O57 89.5(3) 4_565 4_565
O67 W7 O57 160.2(3) . 4_565
O7 W7 O57 99.0(3) . .
O67 W7 O57 160.2(3) 4_565 .
O67 W7 O57 89.5(3) . .
O57 W7 O57 86.3(4) 4_565 .
O7 W7 O557 170.4(4) . .
O67 W7 O557 86.1(2) 4_565 .
O67 W7 O557 86.1(2) . .
O57 W7 O557 74.2(2) 4_565 .
O57 W7 O557 74.2(2) . .
O122 V1 O557 109.1(5) . .
O122 V1 O346 109.4(3) . .
O557 V1 O346 109.8(3) . .
O122 V1 O346 109.4(3) . 4_565
O557 V1 O346 109.8(3) . 4_565
O346 V1 O346 109.4(5) . 4_565
W1 O12 W2 120.1(3) . .
W3 O13 W1 150.4(4) . .
W2 O22 W2 120.7(4) . 4_565
W2 O24 W4 151.5(3) . .
W2 O25 W5 150.3(4) . .
W3 O33 W3 150.5(5) . 4_565
W3 O34 W4 120.5(3) . .
W6 O36 W3 121.2(3) . .
W5 O45 W4 151.4(4) . .
W4 O46 W6 118.5(3) . .
W5 O55 W5 120.0(5) 4_565 .
W5 O57 W7 120.0(3) . .
W6 O66 W6 151.1(5) 4_565 .
W7 O67 W6 149.2(4) . .
V1 O122 W1 124.5(5) . .
V1 O122 W2 124.0(3) . .
W1 O122 W2 91.4(2) . .
V1 O122 W2 124.0(3) . 4_565
W1 O122 W2 91.4(2) . 4_565
W2 O122 W2 91.7(3) . 4_565
V1 O346 W3 124.2(3) . .
V1 O346 W6 123.9(3) . .
W3 O346 W6 91.5(2) . .
V1 O346 W4 124.5(3) . .
W3 O346 W4 91.3(2) . .
W6 O346 W4 91.6(2) . .
V1 O557 W7 123.0(5) . .
V1 O557 W5 124.7(3) . 4_565
W7 O557 W5 91.4(2) . 4_565
V1 O557 W5 124.7(3) . .
W7 O557 W5 91.4(2) . .
W5 O557 W5 92.1(3) 4_565 .
C12 N1 C14 110.1(11) . .
C12 N1 C11 111.0(8) . .
C14 N1 C11 107.9(10) . .
C12 N1 C13 107.9(10) . .
C14 N1 C13 111.6(15) . .
C11 N1 C13 108.4(9) . .
C23 N2 C22 108.7(10) . .
C23 N2 C21 112.3(10) . .
C22 N2 C21 108.4(10) . .
C23 N2 C24 108.2(11) . .
C22 N2 C24 111.2(13) . .
C21 N2 C24 108.1(9) . .
C31 N3 C32 109.0(13) . .
C31 N3 C33 109.3(9) . 4_565
C32 N3 C33 109.9(10) . 4_565
C31 N3 C33 109.3(9) . .
C32 N3 C33 109.9(10) . .
C33 N3 C33 109.5(17) 4_565 .
C43 N4 C43 107.8(15) 4_565 .
C43 N4 C42 108.9(8) 4_565 .
C43 N4 C42 108.9(8) . .
C43 N4 C41 109.5(8) 4_565 .
C43 N4 C41 109.5(8) . .
C42 N4 C41 112.2(12) . .
C53 N5 C53 116.6(24) 4_565 .
C53 N5 C51 105.9(10) 4_565 .
C53 N5 C51 105.9(10) . .
C53 N5 C52 109.2(10) 4_565 .
C53 N5 C52 109.2(10) . .
C51 N5 C52 109.9(13) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
W1 O1 1.708(9) .
W1 O13 1.907(6) 4_565
W1 O13 1.907(6) .
W1 O12 1.914(6) .
W1 O12 1.914(6) 4_565
W1 O122 2.311(8) .
W2 O2 1.712(7) .
W2 O24 1.893(6) .
W2 O25 1.900(6) .
W2 O12 1.931(6) .
W2 O22 1.936(4) .
W2 O122 2.344(6) .
W3 O3 1.710(7) .
W3 O33 1.900(2) .
W3 O13 1.902(6) .
W3 O34 1.910(6) .
W3 O36 1.919(6) .
W3 O346 2.317(6) .
W4 O4 1.708(7) .
W4 O24 1.916(6) .
W4 O45 1.918(6) .
W4 O34 1.923(6) .
W4 O46 1.935(6) .
W4 O346 2.336(6) .
W5 O5 1.714(6) .
W5 O45 1.899(6) .
W5 O57 1.906(6) .
W5 O25 1.920(6) .
W5 O55 1.937(4) .
W5 O557 2.331(6) .
W6 O6 1.712(7) .
W6 O66 1.890(2) .
W6 O36 1.897(6) .
W6 O67 1.903(6) .
W6 O46 1.952(6) .
W6 O346 2.324(6) .
W7 O7 1.690(9) .
W7 O67 1.892(6) 4_565
W7 O67 1.892(6) .
W7 O57 1.938(6) 4_565
W7 O57 1.938(6) .
W7 O557 2.321(8) .
V1 O122 1.625(9) .
V1 O557 1.626(8) .
V1 O346 1.630(6) .
V1 O346 1.630(6) 4_565
O22 W2 1.936(4) 4_565
O33 W3 1.900(2) 4_565
O55 W5 1.937(4) 4_565
O66 W6 1.890(2) 4_565
O122 W2 2.344(6) 4_565
O557 W5 2.331(6) 4_565
N1 C12 1.454(13) .
N1 C14 1.49(2) .
N1 C11 1.513(12) .
N1 C13 1.52(2) .
N2 C23 1.482(15) .
N2 C22 1.50(2) .
N2 C21 1.502(14) .
N2 C24 1.50(2) .
N3 C31 1.49(2) .
N3 C32 1.49(2) .
N3 C33 1.50(2) 4_565
N3 C33 1.50(2) .
N4 C43 1.500(13) 4_565
N4 C43 1.500(13) .
N4 C42 1.51(2) .
N4 C41 1.51(2) .
N5 C53 1.47(2) 4_565
N5 C53 1.47(2) .
N5 C51 1.50(2) .
N5 C52 1.50(2) .
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_4
O1 W1 O12 W2 -171.8(4) . .
O13 W1 O12 W2 12.8(10) 4_565 .
O13 W1 O12 W2 87.1(4) . .
O12 W1 O12 W2 -73.3(4) 4_565 .
O122 W1 O12 W2 1.1(3) . .
O2 W2 O12 W1 172.3(4) . .
O24 W2 O12 W1 -86.1(4) . .
O25 W2 O12 W1 -8.8(10) . .
O22 W2 O12 W1 72.8(4) . .
O122 W2 O12 W1 -1.1(3) . .
O3 W3 O13 W1 -133.8(7) . .
O33 W3 O13 W1 -32.7(8) . .
O34 W3 O13 W1 127.6(7) . .
O36 W3 O13 W1 45.0(13) . .
O346 W3 O13 W1 53.1(7) . .
O1 W1 O13 W3 133.6(7) . .
O13 W1 O13 W3 33.3(9) 4_565 .
O12 W1 O13 W3 -127.7(7) . .
O12 W1 O13 W3 -41.8(13) 4_565 .
O122 W1 O13 W3 -53.0(7) . .
O2 W2 O22 W2 -173.1(5) . 4_565
O24 W2 O22 W2 5.3(12) . 4_565
O25 W2 O22 W2 84.6(5) . 4_565
O12 W2 O22 W2 -74.2(5) . 4_565
O122 W2 O22 W2 -0.5(4) . 4_565
O2 W2 O24 W4 -129.4(7) . .
O25 W2 O24 W4 -27.7(7) . .
O12 W2 O24 W4 131.5(8) . .
O22 W2 O24 W4 52.2(13) . .
O122 W2 O24 W4 57.7(7) . .
O4 W4 O24 W2 129.4(7) . .
O45 W4 O24 W2 28.2(7) . .
O34 W4 O24 W2 -131.3(8) . .
O46 W4 O24 W2 -47.4(12) . .
O346 W4 O24 W2 -57.5(7) . .
O2 W2 O25 W5 128.9(7) . .
O24 W2 O25 W5 27.6(7) . .
O12 W2 O25 W5 -50.0(12) . .
O22 W2 O25 W5 -131.2(7) . .
O122 W2 O25 W5 -57.4(7) . .
O5 W5 O25 W2 -130.1(7) . .
O45 W5 O25 W2 -28.5(7) . .
O57 W5 O25 W2 52.3(12) . .
O55 W5 O25 W2 131.7(7) . .
O557 W5 O25 W2 57.6(7) . .
O3 W3 O33 W3 131.9(10) . 4_565
O13 W3 O33 W3 30.5(10) . 4_565
O34 W3 O33 W3 -47.5(17) . 4_565
O36 W3 O33 W3 -129.1(10) . 4_565
O346 W3 O33 W3 -55.6(10) . 4_565
O3 W3 O34 W4 171.3(4) . .
O33 W3 O34 W4 -9.3(12) . .
O13 W3 O34 W4 -86.7(4) . .
O36 W3 O34 W4 72.6(4) . .
O346 W3 O34 W4 -0.9(3) . .
O4 W4 O34 W3 -172.9(4) . .
O24 W4 O34 W3 85.5(4) . .
O45 W4 O34 W3 11.0(9) . .
O46 W4 O34 W3 -73.8(4) . .
O346 W4 O34 W3 0.9(3) . .
O6 W6 O36 W3 172.3(4) . .
O66 W6 O36 W3 -85.6(4) . .
O67 W6 O36 W3 -5.0(10) . .
O46 W6 O36 W3 75.0(4) . .
O346 W6 O36 W3 0.1(3) . .
O3 W3 O36 W6 -172.8(4) . .
O33 W3 O36 W6 85.4(4) . .
O13 W3 O36 W6 8.4(10) . .
O34 W3 O36 W6 -74.5(4) . .
O346 W3 O36 W6 -0.1(3) . .
O5 W5 O45 W4 132.8(7) . .
O57 W5 O45 W4 -127.7(8) . .
O25 W5 O45 W4 31.6(7) . .
O55 W5 O45 W4 -41.2(14) . .
O557 W5 O45 W4 -53.3(8) . .
O4 W4 O45 W5 -132.1(7) . .
O24 W4 O45 W5 -31.3(7) . .
O34 W4 O45 W5 44.0(12) . .
O46 W4 O45 W5 128.6(8) . .
O346 W4 O45 W5 53.7(7) . .
O4 W4 O46 W6 171.7(4) . .
O24 W4 O46 W6 -11.5(9) . .
O45 W4 O46 W6 -86.3(4) . .
O34 W4 O46 W6 72.5(4) . .
O346 W4 O46 W6 -1.1(3) . .
O6 W6 O46 W4 -173.2(4) . .
O66 W6 O46 W4 11.4(12) . .
O36 W6 O46 W4 -72.7(4) . .
O67 W6 O46 W4 86.6(4) . .
O346 W6 O46 W4 1.1(3) . .
O5 W5 O55 W5 170.8(5) . 4_565
O45 W5 O55 W5 -15.2(13) . 4_565
O57 W5 O55 W5 71.8(5) . 4_565
O25 W5 O55 W5 -87.6(5) . 4_565
O557 W5 O55 W5 -2.6(4) . 4_565
O5 W5 O57 W7 -173.1(4) . .
O45 W5 O57 W7 84.5(4) . .
O25 W5 O57 W7 4.5(10) . .
O55 W5 O57 W7 -74.8(4) . .
O557 W5 O57 W7 -1.0(3) . .
O7 W7 O57 W5 174.1(4) . .
O67 W7 O57 W5 -2.8(10) 4_565 .
O67 W7 O57 W5 -85.1(4) . .
O57 W7 O57 W5 75.6(4) 4_565 .
O557 W7 O57 W5 1.0(3) . .
O6 W6 O66 W6 -131.1(10) . 4_565
O36 W6 O66 W6 127.9(10) . 4_565
O67 W6 O66 W6 -31.3(10) . 4_565
O46 W6 O66 W6 44.2(18) . 4_565
O346 W6 O66 W6 54.2(10) . 4_565
O7 W7 O67 W6 -129.1(7) . .
O67 W7 O67 W6 -28.5(8) 4_565 .
O57 W7 O67 W6 54.1(12) 4_565 .
O57 W7 O67 W6 131.9(7) . .
O557 W7 O67 W6 57.7(7) . .
O6 W6 O67 W7 130.1(7) . .
O66 W6 O67 W7 28.7(7) . .
O36 W6 O67 W7 -52.6(12) . .
O46 W6 O67 W7 -132.5(7) . .
O346 W6 O67 W7 -57.5(7) . .
O557 V1 O122 W1 180.0 . .
O346 V1 O122 W1 -59.9(3) . .
O346 V1 O122 W1 59.9(3) 4_565 .
O557 V1 O122 W2 -60.0(4) . .
O346 V1 O122 W2 60.1(6) . .
O346 V1 O122 W2 179.9(4) 4_565 .
O557 V1 O122 W2 60.0(4) . 4_565
O346 V1 O122 W2 -179.9(4) . 4_565
O346 V1 O122 W2 -60.1(6) 4_565 4_565
O1 W1 O122 V1 180.000(1) . .
O13 W1 O122 V1 -42.8(2) 4_565 .
O13 W1 O122 V1 42.8(2) . .
O12 W1 O122 V1 133.3(2) . .
O12 W1 O122 V1 -133.3(2) 4_565 .
O1 W1 O122 W2 45.88(15) . .
O13 W1 O122 W2 -176.9(2) 4_565 .
O13 W1 O122 W2 -91.3(2) . .
O12 W1 O122 W2 -0.8(2) . .
O12 W1 O122 W2 92.6(3) 4_565 .
O1 W1 O122 W2 -45.9(2) . 4_565
O13 W1 O122 W2 91.3(2) 4_565 4_565
O13 W1 O122 W2 176.9(2) . 4_565
O12 W1 O122 W2 -92.6(3) . 4_565
O12 W1 O122 W2 0.8(2) 4_565 4_565
O2 W2 O122 V1 -176.5(15) . .
O24 W2 O122 V1 -43.5(5) . .
O25 W2 O122 V1 43.6(5) . .
O12 W2 O122 V1 -133.6(5) . .
O22 W2 O122 V1 134.4(5) . .
O2 W2 O122 W1 -42.1(17) . .
O24 W2 O122 W1 91.0(2) . .
O25 W2 O122 W1 178.0(2) . .
O12 W2 O122 W1 0.8(2) . .
O22 W2 O122 W1 -91.1(3) . .
O2 W2 O122 W2 49.4(18) . 4_565
O24 W2 O122 W2 -177.6(3) . 4_565
O25 W2 O122 W2 -90.5(3) . 4_565
O12 W2 O122 W2 92.3(3) . 4_565
O22 W2 O122 W2 0.3(3) . 4_565
O122 V1 O346 W3 60.0(5) . .
O557 V1 O346 W3 179.6(4) . .
O346 V1 O346 W3 -59.8(6) 4_565 .
O122 V1 O346 W6 179.8(4) . .
O557 V1 O346 W6 -60.6(5) . .
O346 V1 O346 W6 59.9(6) 4_565 .
O122 V1 O346 W4 -60.0(5) . .
O557 V1 O346 W4 59.6(5) . .
O346 V1 O346 W4 -179.89(8) 4_565 .
O3 W3 O346 V1 178.0(14) . .
O33 W3 O346 V1 43.2(5) . .
O13 W3 O346 V1 -43.1(4) . .
O34 W3 O346 V1 -133.9(5) . .
O36 W3 O346 V1 133.9(5) . .
O3 W3 O346 W6 44.1(17) . .
O33 W3 O346 W6 -90.6(3) . .
O13 W3 O346 W6 -176.9(3) . .
O34 W3 O346 W6 92.3(3) . .
O36 W3 O346 W6 0.0(2) . .
O3 W3 O346 W4 -47.5(16) . .
O33 W3 O346 W4 177.7(3) . .
O13 W3 O346 W4 91.4(2) . .
O34 W3 O346 W4 0.6(2) . .
O36 W3 O346 W4 -91.6(3) . .
O6 W6 O346 V1 171.0(16) . .
O66 W6 O346 V1 -42.8(5) . .
O36 W6 O346 V1 -134.1(5) . .
O67 W6 O346 V1 44.0(4) . .
O46 W6 O346 V1 133.8(4) . .
O6 W6 O346 W3 -54.9(18) . .
O66 W6 O346 W3 91.3(3) . .
O36 W6 O346 W3 0.0(2) . .
O67 W6 O346 W3 178.1(3) . .
O46 W6 O346 W3 -92.1(3) . .
O6 W6 O346 W4 36.5(18) . .
O66 W6 O346 W4 -177.3(3) . .
O36 W6 O346 W4 91.3(3) . .
O67 W6 O346 W4 -90.5(2) . .
O46 W6 O346 W4 -0.8(2) . .
O4 W4 O346 V1 175.4(15) . .
O24 W4 O346 V1 42.9(4) . .
O45 W4 O346 V1 -42.7(4) . .
O34 W4 O346 V1 133.7(4) . .
O46 W4 O346 V1 -133.4(4) . .
O4 W4 O346 W3 41.1(17) . .
O24 W4 O346 W3 -91.4(2) . .
O45 W4 O346 W3 -177.0(2) . .
O34 W4 O346 W3 -0.6(2) . .
O46 W4 O346 W3 92.3(2) . .
O4 W4 O346 W6 -50.5(17) . .
O24 W4 O346 W6 177.1(2) . .
O45 W4 O346 W6 91.5(2) . .
O34 W4 O346 W6 -92.2(2) . .
O46 W4 O346 W6 0.8(2) . .
O122 V1 O557 W7 180.0 . .
O346 V1 O557 W7 60.2(3) . .
O346 V1 O557 W7 -60.2(3) 4_565 .
O122 V1 O557 W5 -61.0(4) . 4_565
O346 V1 O557 W5 179.1(4) . 4_565
O346 V1 O557 W5 58.8(6) 4_565 4_565
O122 V1 O557 W5 61.0(4) . .
O346 V1 O557 W5 -58.8(6) . .
O346 V1 O557 W5 -179.1(4) 4_565 .
O7 W7 O557 V1 180.000(2) . .
O67 W7 O557 V1 44.1(2) 4_565 .
O67 W7 O557 V1 -44.0(2) . .
O57 W7 O557 V1 134.7(2) 4_565 .
O57 W7 O557 V1 -134.7(2) . .
O7 W7 O557 W5 46.05(15) . 4_565
O67 W7 O557 W5 -89.9(2) 4_565 4_565
O67 W7 O557 W5 -178.0(2) . 4_565
O57 W7 O557 W5 0.7(2) 4_565 4_565
O57 W7 O557 W5 91.4(3) . 4_565
O7 W7 O557 W5 -46.05(15) . .
O67 W7 O557 W5 178.0(2) 4_565 .
O67 W7 O557 W5 89.9(2) . .
O57 W7 O557 W5 -91.4(3) 4_565 .
O57 W7 O557 W5 -0.7(2) . .
O5 W5 O557 V1 -174.8(14) . .
O45 W5 O557 V1 41.7(5) . .
O57 W5 O557 V1 133.5(5) . .
O25 W5 O557 V1 -44.5(5) . .
O55 W5 O557 V1 -133.9(6) . .
O5 W5 O557 W7 52.4(17) . .
O45 W5 O557 W7 -91.1(2) . .
O57 W5 O557 W7 0.7(2) . .
O25 W5 O557 W7 -177.3(2) . .
O55 W5 O557 W7 93.3(3) . .
O5 W5 O557 W5 -39.1(17) . 4_565
O45 W5 O557 W5 177.4(3) . 4_565
O57 W5 O557 W5 -90.7(3) . 4_565
O25 W5 O557 W5 91.3(3) . 4_565
O55 W5 O557 W5 1.9(3) . 4_565
