#------------------------------------------------------------------------------
#$Date: 2016-03-23 15:47:14 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179347 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/44/4324479.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_4324479
loop_
_publ_author_name
'Richard Villanneau'
'David Racimor'
'Elisabeth Messner-Henning'
'Hélène Rousselière'
'Sébastien Picart'
'René Thouvenot'
'Anna Proust'
_publ_contact_author
;
 R. Villanneau
;
_publ_contact_author_email       richard.villanneau@upmc.fr
_publ_contact_author_fax         '+33 (0) 1 44 27 38 41'
_publ_contact_author_phone       '+33 (0) 1 44 27 35 22'
_publ_section_title
;
 Insights into the Coordination Chemistry of Phosphonate Derivatives of
 Heteropolyoxotungstates
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1164
_journal_page_last               1166
_journal_paper_doi               10.1021/ic102223w
_journal_volume                  50
_journal_year                    2011
_chemical_formula_moiety
'La2, P2 W18 O68, 4(P1 O1 C4 H9), 10(N1 O1 C3 H7), 6(H2 O1), 4(N1 C16 H36)'
_chemical_formula_sum            'C110 H262 La2 N14 O88 P6 W18'
_chemical_formula_weight         6962.28
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   none
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.792(11)
_cell_angle_beta                 97.239(13)
_cell_angle_gamma                107.305(12)
_cell_formula_units_Z            1
_cell_length_a                   14.233(2)
_cell_length_b                   16.8840(16)
_cell_length_c                   22.433(3)
_cell_measurement_reflns_used    202
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      21
_cell_measurement_theta_min      3
_cell_volume                     5098.3(12)
_computing_cell_refinement
'Dirax/lsq (Duisenberg & Schreurs, 1989-2000)'
_computing_data_collection       'Collect (Nonius BV, 1997-2000)'
_computing_data_reduction        'EvalCCD (Duisenberg & Schreurs 1990-2000)'
_computing_molecular_graphics    'DIAMOND (Brandenburg, 1999)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR-92 (Giacovazzo, 1993)'
_diffrn_ambient_temperature      200(2)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.977
_diffrn_measured_fraction_theta_max 0.977
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'CCD rotation images, thick slices'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0607
_diffrn_reflns_av_sigmaI/netI    0.0818
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            83239
_diffrn_reflns_theta_full        30.00
_diffrn_reflns_theta_max         30.00
_diffrn_reflns_theta_min         2.53
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    10.643
_exptl_absorpt_correction_T_max  0.0610
_exptl_absorpt_correction_T_min  0.0349
_exptl_absorpt_correction_type   sphere
_exptl_absorpt_process_details
;
Interpolation using  Int.Tab. Vol. C (1992) p. 523,Tab. 6.3.3.3
for values of muR in the range 0-2.5, and Int.Tab. Vol.II (1959)
p.302; Table 5.3.6 B for muR in the range 2.6-10.0.
The interpolation procedure of C.W.Dwiggins Jr (Acta Cryst.(1975)
A31,146-148) is used with some modification.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    2.268
_exptl_crystal_description       prism
_exptl_crystal_F_000             3260
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.45
_exptl_crystal_size_min          0.25
_refine_diff_density_max         3.331
_refine_diff_density_min         -4.008
_refine_diff_density_rms         0.376
_refine_ls_extinction_coef       0.00027(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     979
_refine_ls_number_reflns         29073
_refine_ls_number_restraints     25
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.0924
_refine_ls_R_factor_gt           0.0589
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0832P)²+24.9243P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1485
_refine_ls_wR_factor_ref         0.1653
_reflns_number_gt                20584
_reflns_number_total             29073
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic102223w_si_002.cif
_cod_data_source_block           (^n^Bu~4~N)~2~-2-^t^Bu-DMF
_cod_original_cell_volume        5098.4(12)
_cod_database_code               4324479
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -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_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
W1 W 0.24947(3) 0.87180(2) 0.325141(17) 0.03203(10) Uani 1 1 d . . .
W2 W 0.45516(3) 0.95546(2) 0.258146(18) 0.03249(9) Uani 1 1 d . . .
W3 W 0.23183(3) 0.88484(3) 0.173402(18) 0.03405(10) Uani 1 1 d . . .
W4 W 0.36713(3) 0.71824(2) 0.390713(16) 0.03026(9) Uani 1 1 d . . .
W5 W 0.56863(3) 0.80941(2) 0.326902(16) 0.03046(9) Uani 1 1 d . . .
W6 W 0.54973(3) 0.81689(3) 0.161244(17) 0.03259(9) Uani 1 1 d . . .
W7 W 0.32654(3) 0.74105(3) 0.080554(16) 0.03318(10) Uani 1 1 d . . .
W8 W 0.10185(3) 0.66540(3) 0.154742(18) 0.03528(10) Uani 1 1 d . . .
W9 W 0.12441(3) 0.64607(3) 0.303178(18) 0.03333(10) Uani 1 1 d . . .
La1 La 0.37209(5) 0.44227(4) 0.21542(3) 0.03769(14) Uani 1 1 d . . .
P1 P 0.33798(16) 0.74133(14) 0.23724(9) 0.0229(4) Uani 1 1 d . . .
P2 P 0.1248(2) 0.49294(17) 0.21265(13) 0.0388(6) Uani 1 1 d . . .
C1 C 0.0174(10) 0.3972(8) 0.2033(7) 0.061(4) Uani 1 1 d . . .
C2 C -0.0757(9) 0.4238(9) 0.2025(7) 0.068(4) Uani 1 1 d . . .
C3 C 0.0335(13) 0.3421(10) 0.2547(9) 0.083(5) Uani 1 1 d . . .
C4 C 0.0193(14) 0.3561(10) 0.1408(9) 0.096(7) Uani 1 1 d . . .
P3 P 0.5030(2) 0.60836(16) 0.34510(11) 0.0337(5) Uani 1 1 d . . .
C5 C 0.5784(9) 0.5679(8) 0.4014(5) 0.047(3) Uani 1 1 d . . .
C6 C 0.6144(10) 0.6333(8) 0.4563(5) 0.057(3) Uani 1 1 d . . .
C7 C 0.6669(11) 0.5572(10) 0.3722(7) 0.070(4) Uani 1 1 d . . .
C8 C 0.5154(11) 0.4835(9) 0.4183(6) 0.060(3) Uani 1 1 d . . .
O1 O 0.2006(6) 0.9146(5) 0.3780(3) 0.0434(17) Uani 1 1 d . . .
O2 O 0.5329(6) 1.0537(5) 0.2702(4) 0.0480(19) Uani 1 1 d . . .
O3 O 0.1688(6) 0.9409(5) 0.1312(4) 0.053(2) Uani 1 1 d . . .
O4 O 0.3560(6) 0.7078(5) 0.4653(3) 0.0445(18) Uani 1 1 d . . .
O5 O 0.6869(5) 0.8572(5) 0.3616(3) 0.0418(17) Uani 1 1 d . . .
O6 O 0.6558(6) 0.8872(5) 0.1418(4) 0.0483(19) Uani 1 1 d . . .
O7 O 0.2917(6) 0.7612(5) 0.0079(3) 0.050(2) Uani 1 1 d . . .
O8 O -0.0039(6) 0.6441(5) 0.1057(4) 0.051(2) Uani 1 1 d . . .
O9 O 0.0358(6) 0.6156(5) 0.3485(4) 0.049(2) Uani 1 1 d . . .
O12 O 0.3675(5) 0.9540(4) 0.3211(3) 0.0361(15) Uani 1 1 d . . .
O13 O 0.1881(5) 0.8981(4) 0.2543(3) 0.0372(15) Uani 1 1 d . . .
O14 O 0.3238(5) 0.8103(4) 0.3754(3) 0.0354(15) Uani 1 1 d . . .
O19 O 0.1560(5) 0.7597(5) 0.3144(3) 0.0369(15) Uani 1 1 d . . .
O21 O 0.3232(4) 0.8276(4) 0.2461(3) 0.0270(13) Uani 1 1 d . . .
O23 O 0.3479(5) 0.9710(4) 0.2039(3) 0.0374(15) Uani 1 1 d . . .
O25 O 0.5184(5) 0.8989(4) 0.3171(3) 0.0328(14) Uani 1 1 d . . .
O26 O 0.5018(5) 0.9114(4) 0.2000(3) 0.0342(14) Uani 1 1 d . . .
O37 O 0.2870(5) 0.8411(4) 0.1200(3) 0.0349(15) Uani 1 1 d . . .
O38 O 0.1303(5) 0.7789(5) 0.1696(3) 0.0396(16) Uani 1 1 d . . .
O41 O 0.4174(5) 0.6206(4) 0.3763(3) 0.0350(15) Uani 1 1 d . . .
O45 O 0.5016(5) 0.7823(4) 0.3973(3) 0.0333(14) Uani 1 1 d . . .
O49 O 0.2419(5) 0.6483(4) 0.3548(3) 0.0334(14) Uani 1 1 d . . .
O51 O 0.5727(5) 0.6935(4) 0.3290(3) 0.0333(14) Uani 1 1 d . . .
O54 O 0.4033(5) 0.7296(4) 0.2928(2) 0.0264(12) Uani 1 1 d . . .
O56 O 0.5866(5) 0.8087(4) 0.2478(3) 0.0327(14) Uani 1 1 d . . .
O61 O 0.5689(6) 0.7223(5) 0.1456(3) 0.0416(17) Uani 1 1 d . . .
O67 O 0.4583(5) 0.8182(4) 0.0931(3) 0.0346(15) Uani 1 1 d . . .
O71 O 0.3589(6) 0.6495(5) 0.0718(3) 0.0402(16) Uani 1 1 d . . .
O76 O 0.3878(4) 0.7390(4) 0.1818(2) 0.0236(12) Uani 1 1 d . . .
O78 O 0.1984(5) 0.6828(4) 0.1049(3) 0.0365(15) Uani 1 1 d . . .
O81 O 0.1048(5) 0.5482(5) 0.1609(3) 0.0393(16) Uani 1 1 d . . .
O89 O 0.0465(5) 0.6465(5) 0.2292(3) 0.0391(16) Uani 1 1 d . . .
O91 O 0.1223(5) 0.5340(4) 0.2741(3) 0.0396(16) Uani 1 1 d . . .
O98 O 0.2358(5) 0.6785(4) 0.2309(3) 0.0298(13) Uani 1 1 d . . .
O100 O 0.4363(6) 0.5748(5) 0.1630(4) 0.0470(18) Uani 1 1 d . . .
O101 O 0.2963(7) 0.3910(6) 0.3105(4) 0.055(2) Uani 1 1 d . . .
N1 N 0.2114(8) 0.4012(7) 0.3860(5) 0.055(3) Uani 1 1 d . . .
C9 C 0.2666(9) 0.4339(8) 0.3428(5) 0.047(3) Uani 1 1 d . . .
C10 C 0.1752(13) 0.4582(11) 0.4225(7) 0.078(5) Uani 1 1 d . . .
C11 C 0.1789(12) 0.3124(9) 0.3948(7) 0.068(4) Uani 1 1 d . . .
O102 O 0.2194(6) 0.4725(5) 0.2109(4) 0.0454(18) Uani 1 1 d . . .
O103 O 0.4641(6) 0.5489(4) 0.2909(3) 0.0391(16) Uani 1 1 d . . .
O104 O 0.2767(8) 0.2935(5) 0.1941(5) 0.068(3) Uani 1 1 d . . .
N2 N 0.2228(12) 0.1608(11) 0.2149(7) 0.090(4) Uiso 1 1 d D . .
C12 C 0.2584(16) 0.2386(15) 0.2286(10) 0.098(6) Uiso 1 1 d . . .
C13 C 0.2002(18) 0.0912(16) 0.2573(11) 0.118(7) Uiso 1 1 d . . .
C14A C 0.236(5) 0.126(4) 0.1565(19) 0.13(2) Uiso 0.40 1 d PD . .
C14B C 0.150(3) 0.130(3) 0.1617(14) 0.115(12) Uiso 0.60 1 d PD . .
O105 O 0.4811(9) 0.3687(7) 0.2722(5) 0.078(3) Uani 1 1 d D . .
N3 N 0.5821(18) 0.2885(15) 0.2748(11) 0.160 Uiso 1 1 d D . .
C15 C 0.5563(18) 0.3520(18) 0.2925(13) 0.150(10) Uiso 1 1 d D . .
C16 C 0.669(2) 0.2571(18) 0.2929(13) 0.142(9) Uiso 1 1 d D . .
C17 C 0.530(2) 0.233(2) 0.2178(13) 0.160 Uiso 1 1 d D . .
O106 O 0.4848(10) 0.4072(8) 0.1487(6) 0.090(4) Uani 1 1 d D . .
N4A N 0.494(3) 0.338(2) 0.0519(15) 0.099(7) Uiso 0.50 1 d P A 1
C18A C 0.438(3) 0.364(3) 0.1011(15) 0.102(12) Uiso 0.50 1 d PD A 1
C19A C 0.440(3) 0.291(2) -0.0052(16) 0.080(9) Uiso 0.50 1 d P A 1
C20A C 0.595(3) 0.353(3) 0.061(2) 0.103(12) Uiso 0.50 1 d P A 1
N4B N 0.599(3) 0.438(2) 0.0827(15) 0.099(7) Uiso 0.50 1 d P A 2
C18B C 0.525(2) 0.4515(18) 0.1121(12) 0.059(6) Uiso 0.50 1 d P A 2
C19B C 0.650(3) 0.376(2) 0.0990(16) 0.080(9) Uiso 0.50 1 d P A 2
C20B C 0.632(3) 0.488(3) 0.037(2) 0.109(13) Uiso 0.50 1 d P A 2
O107 O 0.2930(7) 0.4253(6) 0.1043(4) 0.058(2) Uani 1 1 d . . .
C21 C 0.2396(10) 0.4661(9) 0.0807(6) 0.056(3) Uiso 1 1 d . A .
N5A N 0.1729(13) 0.4287(12) 0.0366(8) 0.036(4) Uiso 0.50 1 d P A 1
C22A C 0.154(2) 0.3437(18) 0.0165(12) 0.057(6) Uiso 0.50 1 d P A 1
C23A C 0.114(2) 0.482(2) 0.0114(13) 0.061(7) Uiso 0.50 1 d P A 1
N5B N 0.2057(14) 0.4665(13) 0.0173(8) 0.043(4) Uiso 0.50 1 d P A 2
C22B C 0.228(2) 0.4086(18) -0.0239(12) 0.059(6) Uiso 0.50 1 d P A 2
C23B C 0.150(2) 0.5192(18) -0.0099(12) 0.052(6) Uiso 0.50 1 d P A 2
N6 N 0.8770(8) 0.8259(8) 0.2414(6) 0.065(3) Uani 1 1 d . . .
C24 C 0.7863(11) 0.7467(11) 0.2272(10) 0.087(6) Uani 1 1 d . . .
C25 C 0.8118(14) 0.6650(15) 0.2208(14) 0.138(11) Uani 1 1 d . . .
C26 C 0.7163(14) 0.5940(14) 0.2117(11) 0.105(7) Uani 1 1 d . . .
C27 C 0.735(2) 0.5140(19) 0.208(2) 0.21(2) Uani 1 1 d . . .
C28 C 0.9451(11) 0.8100(13) 0.2943(7) 0.082(5) Uani 1 1 d . . .
C29 C 0.8966(12) 0.7910(15) 0.3500(10) 0.104(7) Uani 1 1 d . . .
C30 C 0.9693(14) 0.7904(16) 0.4027(10) 0.111(8) Uani 1 1 d . . .
C31 C 0.9221(17) 0.7587(18) 0.4590(11) 0.125(9) Uani 1 1 d . . .
C32 C 0.9350(11) 0.8397(15) 0.1882(9) 0.101(7) Uani 1 1 d . . .
C33 C 0.8803(16) 0.853(2) 0.1296(10) 0.142(11) Uani 1 1 d . . .
C34 C 0.935(2) 0.861(2) 0.0809(9) 0.151(12) Uani 1 1 d D . .
C35 C 0.879(3) 0.871(2) 0.0179(11) 0.171(14) Uani 1 1 d D . .
C36 C 0.8337(9) 0.8969(10) 0.2535(7) 0.063(4) Uani 1 1 d . . .
C37 C 0.9108(15) 0.9819(13) 0.2662(10) 0.096(6) Uani 1 1 d . . .
C38 C 0.847(3) 1.0387(16) 0.2832(15) 0.165(12) Uani 1 1 d U . .
C39 C 0.926(3) 1.129(2) 0.301(2) 0.232(18) Uani 1 1 d U . .
N7 N 0.4554(14) 0.0471(12) 0.0243(8) 0.096(5) Uiso 0.50 1 d P . .
C70 C 0.4554(14) 0.0471(12) 0.0243(8) 0.096(5) Uiso 0.50 1 d P . .
C40 C 0.422(3) 0.120(3) 0.0203(18) 0.213(15) Uiso 1 1 d DU . .
C41 C 0.369(2) 0.1523(19) 0.0667(13) 0.146(10) Uiso 1 1 d DU A .
C42 C 0.383(2) 0.246(2) 0.0621(12) 0.072(8) Uiso 0.50 1 d PD . .
C43 C 0.377(3) 0.280(2) -0.0020(12) 0.072(8) Uiso 0.50 1 d PD A .
C44 C 0.512(3) -0.023(3) 0.0286(17) 0.091(11) Uiso 0.50 1 d P . .
C45 C 0.499(2) 0.047(2) 0.0893(13) 0.065(7) Uiso 0.50 1 d P . .
C46 C 0.597(3) 0.114(3) 0.098(2) 0.104(12) Uiso 0.50 1 d P . .
C47 C 0.670(3) 0.100(2) 0.1544(19) 0.102(12) Uiso 0.50 1 d PD . .
C48 C 0.758(2) 0.182(2) 0.1627(16) 0.084(9) Uiso 0.50 1 d PD . .
C49 C 0.341(2) -0.023(2) 0.0271(13) 0.066(7) Uiso 0.50 1 d P . .
C50 C 0.270(3) -0.049(3) -0.0311(19) 0.099(12) Uiso 0.50 1 d P . .
C51 C 0.168(2) -0.0961(19) -0.0273(13) 0.067(7) Uiso 0.50 1 d PD . .
C52 C 0.068(2) -0.159(3) -0.047(2) 0.111(13) Uiso 0.50 1 d PD . .
N8 N 0.5739(11) 0.0418(9) 0.4772(6) 0.071(4) Uiso 0.50 1 d PD . .
C80 C 0.5739(11) 0.0418(9) 0.4772(6) 0.071(4) Uiso 0.50 1 d P . .
C53 C 0.6697(19) 0.1064(19) 0.4914(16) 0.173(12) Uiso 1 1 d D . .
C54 C 0.7314(16) 0.1374(14) 0.4421(10) 0.100(6) Uiso 1 1 d . . .
C55 C 0.823(3) 0.214(2) 0.4686(15) 0.078(9) Uiso 0.50 1 d P . .
C56 C 0.889(3) 0.256(3) 0.4183(19) 0.102(12) Uiso 0.50 1 d P . .
C57 C 0.478(2) -0.024(2) 0.4674(14) 0.074(8) Uiso 0.50 1 d P . .
C58 C 0.515(3) 0.063(2) 0.4239(15) 0.077(9) Uiso 0.50 1 d P . .
C59 C 0.487(2) 0.141(2) 0.4381(14) 0.071(8) Uiso 0.50 1 d P . .
C60 C 0.433(3) 0.165(2) 0.3827(18) 0.095(11) Uiso 0.50 1 d PD . .
C61 C 0.409(4) 0.246(3) 0.397(2) 0.123(15) Uiso 0.50 1 d PD . .
C62 C 0.610(3) -0.029(2) 0.4535(17) 0.092(11) Uiso 0.50 1 d PD . .
C63 C 0.648(3) -0.078(3) 0.505(2) 0.133(17) Uiso 0.50 1 d PD . .
C64 C 0.760(3) -0.059(4) 0.505(3) 0.18(3) Uiso 0.50 1 d PD . .
C65 C 0.782(5) -0.118(4) 0.553(3) 0.15(2) Uiso 0.50 1 d PD . .
O200 O 0.066(3) 0.547(2) 0.5226(15) 0.131(11) Uiso 0.50 1 d P . .
O201 O 0.284(3) 0.616(3) 0.570(2) 0.173(16) Uiso 0.50 1 d P . .
O202 O 1.030(7) -0.057(6) 0.560(4) 0.36(4) Uiso 0.50 1 d P . .
O203 O 0.931(5) -0.042(4) 0.514(3) 0.28(3) Uiso 0.50 1 d P . .
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'
La La -0.2871 2.4523 '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'
P P 0.1023 0.0942 '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 102.5(3) . .
O1 W1 O12 101.5(3) . .
O13 W1 O12 93.6(3) . .
O1 W1 O19 100.8(3) . .
O13 W1 O19 89.1(3) . .
O12 W1 O19 156.4(3) . .
O1 W1 O14 101.1(3) . .
O13 W1 O14 155.3(3) . .
O12 W1 O14 89.0(3) . .
O19 W1 O14 79.2(3) . .
O1 W1 O21 173.2(3) . .
O13 W1 O21 73.5(2) . .
O12 W1 O21 73.6(2) . .
O19 W1 O21 84.8(2) . .
O14 W1 O21 83.6(2) . .
O2 W2 O26 104.2(4) . .
O2 W2 O23 101.9(4) . .
O26 W2 O23 92.8(3) . .
O2 W2 O25 100.6(3) . .
O26 W2 O25 89.9(3) . .
O23 W2 O25 155.9(3) . .
O2 W2 O12 100.3(3) . .
O26 W2 O12 155.3(3) . .
O23 W2 O12 84.9(3) . .
O25 W2 O12 82.7(3) . .
O2 W2 O21 169.6(3) . .
O26 W2 O21 84.7(3) . .
O23 W2 O21 71.9(3) . .
O25 W2 O21 84.5(2) . .
O12 W2 O21 71.2(2) . .
O3 W3 O37 103.8(4) . .
O3 W3 O23 99.8(4) . .
O37 W3 O23 96.2(3) . .
O3 W3 O38 100.3(4) . .
O37 W3 O38 87.5(3) . .
O23 W3 O38 158.1(3) . .
O3 W3 O13 100.0(3) . .
O37 W3 O13 155.5(3) . .
O23 W3 O13 85.0(3) . .
O38 W3 O13 83.0(3) . .
O3 W3 O21 169.0(3) . .
O37 W3 O21 85.5(3) . .
O23 W3 O21 73.1(3) . .
O38 W3 O21 85.7(3) . .
O13 W3 O21 71.4(2) . .
O4 W4 O14 101.3(3) . .
O4 W4 O45 99.3(3) . .
O14 W4 O45 92.3(3) . .
O4 W4 O49 101.1(3) . .
O14 W4 O49 89.7(3) . .
O45 W4 O49 158.6(3) . .
O4 W4 O41 98.8(3) . .
O14 W4 O41 159.9(3) . .
O45 W4 O41 85.2(3) . .
O49 W4 O41 85.7(3) . .
O4 W4 O54 172.1(3) . .
O14 W4 O54 84.3(2) . .
O45 W4 O54 74.7(2) . .
O49 W4 O54 84.3(2) . .
O41 W4 O54 75.8(2) . .
O5 W5 O56 101.9(3) . .
O5 W5 O25 101.5(3) . .
O56 W5 O25 90.8(3) . .
O5 W5 O45 99.4(3) . .
O56 W5 O45 158.3(3) . .
O25 W5 O45 89.1(3) . .
O5 W5 O51 98.0(3) . .
O56 W5 O51 88.9(3) . .
O25 W5 O51 160.0(3) . .
O45 W5 O51 83.9(3) . .
O5 W5 O54 170.5(3) . .
O56 W5 O54 85.6(3) . .
O25 W5 O54 84.0(3) . .
O45 W5 O54 72.8(2) . .
O51 W5 O54 76.1(2) . .
O6 W6 O61 102.2(4) . .
O6 W6 O67 100.2(3) . .
O61 W6 O67 99.0(3) . .
O6 W6 O56 102.2(3) . .
O61 W6 O56 91.0(3) . .
O67 W6 O56 152.9(3) . .
O6 W6 O26 93.1(3) . .
O61 W6 O26 162.6(3) . .
O67 W6 O26 86.3(3) . .
O56 W6 O26 77.6(3) . .
O6 W6 O76 169.0(3) . .
O61 W6 O76 87.1(3) . .
O67 W6 O76 72.2(2) . .
O56 W6 O76 83.3(2) . .
O26 W6 O76 78.7(2) . .
O7 W7 O71 102.7(3) . .
O7 W7 O67 99.0(4) . .
O71 W7 O67 98.2(3) . .
O7 W7 O78 101.1(4) . .
O71 W7 O78 93.3(3) . .
O67 W7 O78 153.9(3) . .
O7 W7 O37 94.8(3) . .
O71 W7 O37 161.8(3) . .
O67 W7 O37 83.6(3) . .
O78 W7 O37 78.4(3) . .
O7 W7 O76 169.8(3) . .
O71 W7 O76 85.0(3) . .
O67 W7 O76 73.1(2) . .
O78 W7 O76 84.8(2) . .
O37 W7 O76 78.1(2) . .
O8 W8 O78 102.8(4) . .
O8 W8 O38 101.3(4) . .
O78 W8 O38 90.7(3) . .
O8 W8 O89 99.8(4) . .
O78 W8 O89 156.9(3) . .
O38 W8 O89 89.7(3) . .
O8 W8 O81 96.5(4) . .
O78 W8 O81 88.8(3) . .
O38 W8 O81 161.8(3) . .
O89 W8 O81 83.7(3) . .
O8 W8 O98 171.4(3) . .
O78 W8 O98 83.5(3) . .
O38 W8 O98 84.2(3) . .
O89 W8 O98 73.5(2) . .
O81 W8 O98 77.7(3) . .
O9 W9 O19 100.2(3) . .
O9 W9 O89 100.8(4) . .
O19 W9 O89 91.6(3) . .
O9 W9 O49 102.7(4) . .
O19 W9 O49 89.9(3) . .
O89 W9 O49 155.8(3) . .
O9 W9 O91 97.6(4) . .
O19 W9 O91 162.1(3) . .
O89 W9 O91 84.8(3) . .
O49 W9 O91 86.4(3) . .
O9 W9 O98 173.4(3) . .
O19 W9 O98 84.0(3) . .
O89 W9 O98 73.9(2) . .
O49 W9 O98 82.2(2) . .
O91 W9 O98 78.2(3) . .
O102 La1 O103 96.7(3) . .
O102 La1 O104 88.5(3) . .
O103 La1 O104 146.3(3) . .
O102 La1 O105 144.4(3) . .
O103 La1 O105 79.8(3) . .
O104 La1 O105 76.9(4) . .
O102 La1 O106 141.4(4) . .
O103 La1 O106 111.1(4) . .
O104 La1 O106 82.9(4) . .
O105 La1 O106 69.5(4) . .
O102 La1 O100 87.3(3) . .
O103 La1 O100 72.2(2) . .
O104 La1 O100 141.4(3) . .
O105 La1 O100 124.0(4) . .
O106 La1 O100 76.9(3) . .
O102 La1 O101 72.2(3) . .
O103 La1 O101 76.8(3) . .
O104 La1 O101 73.2(3) . .
O105 La1 O101 72.5(3) . .
O106 La1 O101 138.6(3) . .
O100 La1 O101 140.3(3) . .
O102 La1 O107 72.3(3) . .
O103 La1 O107 140.5(3) . .
O104 La1 O107 72.7(3) . .
O105 La1 O107 130.8(3) . .
O106 La1 O107 69.2(4) . .
O100 La1 O107 69.5(3) . .
O101 La1 O107 130.7(3) . .
O54 P1 O98 111.8(4) . .
O54 P1 O76 110.4(3) . .
O98 P1 O76 111.5(3) . .
O54 P1 O21 106.6(3) . .
O98 P1 O21 106.5(3) . .
O76 P1 O21 109.8(3) . .
O102 P2 O91 111.7(4) . .
O102 P2 O81 112.2(4) . .
O91 P2 O81 110.4(4) . .
O102 P2 C1 110.7(6) . .
O91 P2 C1 105.4(5) . .
O81 P2 C1 106.1(6) . .
C2 C1 C3 114.3(13) . .
C2 C1 C4 110.3(14) . .
C3 C1 C4 111.6(14) . .
C2 C1 P2 107.2(9) . .
C3 C1 P2 107.5(10) . .
C4 C1 P2 105.4(10) . .
O103 P3 O41 111.2(4) . .
O103 P3 O51 112.0(4) . .
O41 P3 O51 110.9(4) . .
O103 P3 C5 110.8(5) . .
O41 P3 C5 106.0(5) . .
O51 P3 C5 105.7(5) . .
C8 C5 C7 109.4(11) . .
C8 C5 C6 112.7(11) . .
C7 C5 C6 111.4(11) . .
C8 C5 P3 108.5(9) . .
C7 C5 P3 107.4(9) . .
C6 C5 P3 107.2(8) . .
W1 O12 W2 124.2(3) . .
W1 O13 W3 123.1(3) . .
W4 O14 W1 152.3(3) . .
W9 O19 W1 153.1(4) . .
P1 O21 W3 123.3(3) . .
P1 O21 W1 126.6(4) . .
W3 O21 W1 91.5(2) . .
P1 O21 W2 124.1(3) . .
W3 O21 W2 90.2(2) . .
W1 O21 W2 90.6(2) . .
W3 O23 W2 124.3(4) . .
W5 O25 W2 143.2(4) . .
W2 O26 W6 153.2(4) . .
W3 O37 W7 153.3(4) . .
W8 O38 W3 144.9(4) . .
P3 O41 W4 134.4(4) . .
W4 O45 W5 121.5(3) . .
W4 O49 W9 143.8(4) . .
P3 O51 W5 136.4(4) . .
P1 O54 W4 127.9(3) . .
P1 O54 W5 127.3(4) . .
W4 O54 W5 90.95(19) . .
W5 O56 W6 154.9(4) . .
W6 O67 W7 122.0(4) . .
P1 O76 W7 129.7(3) . .
P1 O76 W6 130.0(3) . .
W7 O76 W6 89.5(2) . .
W8 O78 W7 153.8(4) . .
P2 O81 W8 135.8(4) . .
W9 O89 W8 122.5(3) . .
P2 O91 W9 135.4(5) . .
P1 O98 W8 127.8(4) . .
P1 O98 W9 128.2(3) . .
W8 O98 W9 90.0(2) . .
C9 O101 La1 123.2(8) . .
C9 N1 C11 122.6(11) . .
C9 N1 C10 118.0(11) . .
C11 N1 C10 119.2(11) . .
O101 C9 N1 121.5(12) . .
P2 O102 La1 176.0(5) . .
P3 O103 La1 167.9(5) . .
C12 O104 La1 129.0(12) . .
C12 N2 C14B 121(2) . .
C12 N2 C14A 121(3) . .
C14B N2 C14A 51(3) . .
C12 N2 C13 127.5(18) . .
C14B N2 C13 104(2) . .
C14A N2 C13 108(3) . .
O104 C12 N2 127(2) . .
C14B C14A N2 63.5(17) . .
C14A C14B N2 65.6(18) . .
C15 O105 La1 159.8(18) . .
C15 N3 C16 134(2) . .
C15 N3 C17 123(3) . .
C16 N3 C17 102(2) . .
O105 C15 N3 125(3) . .
C18B O106 C18A 81(3) . .
C18B O106 La1 124.7(15) . .
C18A O106 La1 113(2) . .
C20A N4A C19A 117(3) . .
C20A N4A C18A 122(3) . .
C19A N4A C18A 122(3) . .
C20A N4A C42 135(3) . .
C19A N4A C42 66(2) . .
C18A N4A C42 72(2) . .
C20A N4A C43 142(3) . .
C18A N4A C43 96(2) . .
C42 N4A C43 48.3(11) . .
O106 C18A N4A 121(3) . .
C43 C19A N4A 106(4) . .
C43 C19A C42 56(3) . .
N4A C19A C42 68(2) . .
C20B N4B C18B 119(4) . .
C20B N4B C19B 117(3) . .
C18B N4B C19B 124(3) . .
O106 C18B N4B 124(3) . .
C21 O107 La1 125.2(7) . .
O107 C21 N5A 116.1(14) . .
O107 C21 N5B 126.5(13) . .
C21 N5A C22A 124.2(19) . .
C21 N5A C23A 112.1(18) . .
C22A N5A C23A 123.6(19) . .
C21 N5B C23B 125.8(17) . .
C21 N5B C22B 118.1(18) . .
C23B N5B C22B 116.1(19) . .
C28 N6 C32 106.8(11) . .
C28 N6 C36 114.2(12) . .
C32 N6 C36 112.8(14) . .
C28 N6 C24 108.2(14) . .
C32 N6 C24 108.9(13) . .
C36 N6 C24 105.8(9) . .
C25 C24 N6 115.3(12) . .
C26 C25 C24 108.6(14) . .
C27 C26 C25 111.9(18) . .
C29 C28 N6 113.3(12) . .
C30 C29 C28 111.5(14) . .
C29 C30 C31 113.8(17) . .
C33 C32 N6 116.4(12) . .
C34 C33 C32 114.7(16) . .
C33 C34 C35 116(2) . .
C37 C36 N6 114.4(12) . .
C36 C37 C38 102.9(17) . .
C37 C38 C39 105(3) . .
C44 N7 C40 116(3) 2_655 .
C44 N7 C45 129(2) 2_655 .
C40 N7 C45 106(2) . .
C44 N7 C44 61(3) 2_655 .
C40 N7 C44 170(3) . .
C45 N7 C44 72.8(19) . .
C44 N7 C49 105(2) 2_655 .
C40 N7 C49 96(2) . .
C45 N7 C49 98.4(19) . .
C44 N7 C49 94(2) . .
N7 C40 C41 127(3) . .
C42 C41 C40 111(3) . .
C41 C42 C43 118(3) . .
C41 C42 C19A 114(2) . .
C41 C42 N4A 133(3) . .
C43 C42 N4A 67(2) . .
C19A C42 N4A 46.7(16) . .
C19A C43 C42 96(4) . .
C19A C43 N4A 49(3) . .
C42 C43 N4A 65.1(19) . .
C70 C44 C44 65(3) 2_655 2_655
N7 C44 C44 65(3) 2_655 2_655
C70 C44 N7 119(3) 2_655 .
N7 C44 N7 119(3) 2_655 .
C44 C44 N7 53(2) 2_655 .
C70 C44 C45 158(3) 2_655 .
N7 C44 C45 158(3) 2_655 .
C44 C44 C45 101(4) 2_655 .
N7 C44 C45 51.0(16) . .
C46 C45 N7 106(3) . .
C46 C45 C44 103(3) . .
N7 C45 C44 56.2(16) . .
C45 C46 C47 112(3) . .
C48 C47 C46 105(3) . .
C50 C49 N7 119(3) . .
C51 C50 C49 118(3) . .
C50 C51 C52 157(3) . .
C53 N8 C57 176(2) . .
C53 N8 C58 110(2) . .
C57 N8 C58 73(2) . .
C53 N8 C57 111(2) . 2_656
C57 N8 C57 66(2) . 2_656
C58 N8 C57 116(2) . 2_656
C53 N8 C62 99(2) . .
C57 N8 C62 82(2) . .
C58 N8 C62 105(2) . .
C57 N8 C62 115(2) 2_656 .
N8 C53 C54 120(2) . .
C53 C54 C55 109(2) . .
C54 C55 C56 112(3) . .
N8 C57 C80 114(2) . 2_656
N8 C57 N8 114(2) . 2_656
N8 C57 C57 58(2) . 2_656
C80 C57 C57 56(2) 2_656 2_656
N8 C57 C57 56(2) 2_656 2_656
N8 C57 C58 53.8(17) . .
C80 C57 C58 135(2) 2_656 .
N8 C57 C58 135(2) 2_656 .
C57 C57 C58 97(3) 2_656 .
N8 C57 C62 50.8(16) . .
C80 C57 C62 130(2) 2_656 .
N8 C57 C62 130(2) 2_656 .
C57 C57 C62 91(3) 2_656 .
C58 C57 C62 80(2) . .
N8 C58 C59 111(2) . .
N8 C58 C57 53.0(17) . .
C59 C58 C57 119(3) . .
C60 C59 C58 110(3) . .
C59 C60 C61 109(3) . .
N8 C62 C63 113(3) . .
N8 C62 C57 47.3(14) . .
C63 C62 C57 108(3) . .
C64 C63 C62 107(2) . .
C63 C64 C65 99(4) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
W1 O1 1.701(6) .
W1 O13 1.840(7) .
W1 O12 1.847(7) .
W1 O19 1.955(7) .
W1 O14 1.964(7) .
W1 O21 2.387(6) .
W2 O2 1.694(8) .
W2 O26 1.784(6) .
W2 O23 1.912(7) .
W2 O25 1.928(7) .
W2 O12 1.994(7) .
W2 O21 2.389(6) .
W3 O3 1.707(8) .
W3 O37 1.776(6) .
W3 O23 1.890(7) .
W3 O38 1.930(8) .
W3 O13 2.022(7) .
W3 O21 2.355(6) .
W4 O4 1.707(7) .
W4 O14 1.856(7) .
W4 O45 1.884(7) .
W4 O49 1.892(7) .
W4 O41 2.019(6) .
W4 O54 2.316(5) .
W5 O5 1.713(7) .
W5 O56 1.826(6) .
W5 O25 1.859(6) .
W5 O45 1.937(7) .
W5 O51 1.976(7) .
W5 O54 2.360(6) .
W6 O6 1.730(8) .
W6 O61 1.736(7) .
W6 O67 1.883(7) .
W6 O56 1.963(6) .
W6 O26 2.127(6) .
W6 O76 2.395(6) .
W7 O7 1.712(8) .
W7 O71 1.754(7) .
W7 O67 1.923(7) .
W7 O78 1.946(7) .
W7 O37 2.145(6) .
W7 O76 2.333(5) .
W8 O8 1.689(7) .
W8 O78 1.840(7) .
W8 O38 1.853(7) .
W8 O89 1.926(7) .
W8 O81 1.997(7) .
W8 O98 2.350(6) .
W9 O9 1.685(7) .
W9 O19 1.841(7) .
W9 O89 1.877(7) .
W9 O49 1.900(7) .
W9 O91 1.983(7) .
W9 O98 2.366(6) .
La1 O102 2.367(8) .
La1 O103 2.404(7) .
La1 O104 2.481(9) .
La1 O105 2.502(9) .
La1 O106 2.512(9) .
La1 O100 2.520(8) .
La1 O101 2.558(8) .
La1 O107 2.577(9) .
P1 O54 1.511(6) .
P1 O98 1.513(7) .
P1 O76 1.513(6) .
P1 O21 1.546(6) .
P2 O102 1.490(8) .
P2 O91 1.544(7) .
P2 O81 1.551(8) .
P2 C1 1.853(13) .
C1 C2 1.52(2) .
C1 C3 1.53(2) .
C1 C4 1.56(2) .
P3 O103 1.502(7) .
P3 O41 1.542(7) .
P3 O51 1.561(8) .
P3 C5 1.825(11) .
C5 C8 1.522(19) .
C5 C7 1.546(19) .
C5 C6 1.571(17) .
O101 C9 1.213(14) .
N1 C9 1.345(15) .
N1 C11 1.455(17) .
N1 C10 1.497(17) .
O104 C12 1.21(2) .
N2 C12 1.28(2) .
N2 C14B 1.457(18) .
N2 C14A 1.483(19) .
N2 C13 1.51(3) .
C14A C14B 1.26(6) .
O105 C15 1.223(17) .
N3 C15 1.305(17) .
N3 C16 1.496(18) .
N3 C17 1.538(18) .
O106 C18B 1.20(3) .
O106 C18A 1.276(18) .
N4A C20A 1.37(5) .
N4A C19A 1.49(5) .
N4A C18A 1.58(5) .
N4A C42 1.89(5) .
N4A C43 1.91(5) .
C19A C43 0.86(4) .
N4B C20B 1.37(5) .
N4B C18B 1.39(4) .
N4B C19B 1.46(5) .
O107 C21 1.246(16) .
C21 N5A 1.29(2) .
C21 N5B 1.44(2) .
N5A C22A 1.43(3) .
N5A C23A 1.47(3) .
N5B C23B 1.45(3) .
N5B C22B 1.46(3) .
N6 C28 1.514(19) .
N6 C32 1.52(2) .
N6 C36 1.537(18) .
N6 C24 1.55(2) .
C24 C25 1.54(2) .
C25 C26 1.51(3) .
C26 C27 1.45(3) .
C28 C29 1.50(3) .
C29 C30 1.47(3) .
C30 C31 1.53(3) .
C32 C33 1.49(3) .
C33 C34 1.40(3) .
C34 C35 1.569(18) .
C36 C37 1.52(2) .
C37 C38 1.57(4) .
C38 C39 1.61(4) .
N7 C44 1.43(4) 2_655
N7 C40 1.45(4) .
N7 C45 1.51(3) .
N7 C44 1.61(4) .
N7 C49 1.71(4) .
C40 C41 1.540(19) .
C41 C42 1.54(4) .
C42 C43 1.559(19) .
C44 C70 1.43(4) 2_655
C44 N7 1.43(4) 2_655
C44 C44 1.56(8) 2_655
C45 C46 1.50(5) .
C46 C47 1.60(6) .
C47 C48 1.559(19) .
C49 C50 1.52(5) .
C50 C51 1.44(5) .
C51 C52 1.514(19) .
N8 C53 1.465(18) .
N8 C57 1.47(4) .
N8 C58 1.48(4) .
N8 C57 1.51(3) 2_656
N8 C62 1.55(4) .
C53 C54 1.50(4) .
C54 C55 1.58(4) .
C55 C56 1.60(5) .
C57 C80 1.51(3) 2_656
C57 N8 1.51(3) 2_656
C57 C57 1.62(6) 2_656
C58 C59 1.52(5) .
C59 C60 1.50(5) .
C60 C61 1.533(19) .
C62 C63 1.554(19) .
C63 C64 1.54(2) .
C64 C65 1.55(2) .
O202 O203 1.73(10) .
