#------------------------------------------------------------------------------
#$Date: 2016-03-23 15:47:14 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179347 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/44/4324482.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_4324482
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
'Zr2, P2 W18 O68, 4(P O C4 H9), 2(H2 O), 2(H O), 4(N C16 H36), 4(C2 N H3)'
_chemical_formula_sum            'C88 H198 N8 O76 P6 W18 Zr2'
_chemical_formula_weight         6262.10
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      15
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   none
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 115.937(8)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   28.125(6)
_cell_length_b                   22.992(3)
_cell_length_c                   28.543(3)
_cell_measurement_reflns_used    379
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      22
_cell_measurement_theta_min      3
_cell_volume                     16598(5)
_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 0.994
_diffrn_measured_fraction_theta_max 0.994
_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  0.0615
_diffrn_reflns_av_sigmaI/netI    0.0592
_diffrn_reflns_limit_h_max       36
_diffrn_reflns_limit_h_min       -39
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       40
_diffrn_reflns_limit_l_min       -40
_diffrn_reflns_number            137090
_diffrn_reflns_theta_full        30.00
_diffrn_reflns_theta_max         30.00
_diffrn_reflns_theta_min         2.78
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    12.675
_exptl_absorpt_correction_T_max  0.149
_exptl_absorpt_correction_T_min  0.0958
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
R.H. Blessing, Acta Cryst. (1995), A51, 33-38
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    2.506
_exptl_crystal_description       prism
_exptl_crystal_F_000             11568
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.15
_refine_diff_density_max         2.014
_refine_diff_density_min         -1.563
_refine_diff_density_rms         0.249
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     752
_refine_ls_number_reflns         24107
_refine_ls_number_restraints     20
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.0842
_refine_ls_R_factor_gt           0.0403
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0294P)²+276.3872P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0787
_refine_ls_wR_factor_ref         0.0904
_reflns_number_gt                16208
_reflns_number_total             24107
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic102223w_si_005.cif
_cod_data_source_block           (^n^Bu~4~N)~4~-1-^t^Bu-H~2~O
_cod_original_cell_volume        16598(4)
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               4324482
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
W1 W 0.566732(13) 0.349962(15) 0.133477(12) 0.02819(8) Uani 1 1 d . . .
W2 W 0.583105(13) 0.203637(15) 0.133242(13) 0.02926(8) Uani 1 1 d . . .
W3 W 0.681811(13) 0.287547(14) 0.217441(11) 0.02584(7) Uani 1 1 d . . .
W4 W 0.534429(13) 0.352701(16) -0.006786(12) 0.03206(8) Uani 1 1 d . . .
W5 W 0.551008(13) 0.209474(16) -0.004370(12) 0.03045(8) Uani 1 1 d . . .
W6 W 0.676868(13) 0.140870(13) 0.085050(12) 0.02479(7) Uani 1 1 d . . .
W7 W 0.772887(12) 0.226654(14) 0.164502(10) 0.02242(7) Uani 1 1 d . . .
W8 W 0.752953(13) 0.384084(14) 0.169643(11) 0.02770(7) Uani 1 1 d . . .
W9 W 0.640927(14) 0.441951(13) 0.082000(12) 0.02940(8) Uani 1 1 d . . .
Zr1 Zr 0.77896(3) 0.18722(3) 0.04046(2) 0.01595(13) Uani 1 1 d . . .
P1 P 0.65261(7) 0.29240(8) 0.08534(6) 0.0165(3) Uani 1 1 d . . .
P2 P 0.74068(9) 0.42204(8) 0.05453(8) 0.0272(4) Uani 1 1 d . . .
P3 P 0.58252(8) 0.29264(10) -0.08037(7) 0.0258(4) Uani 1 1 d . . .
O1 O 0.5220(2) 0.3889(3) 0.1458(2) 0.0411(15) Uani 1 1 d . . .
O2 O 0.5479(3) 0.1523(3) 0.1472(2) 0.0449(16) Uani 1 1 d . . .
O3 O 0.7076(2) 0.2885(3) 0.2836(2) 0.0385(15) Uani 1 1 d . . .
O4 O 0.4806(3) 0.3945(3) -0.0406(2) 0.0530(19) Uani 1 1 d . . .
O5 O 0.5065(3) 0.1585(3) -0.0401(2) 0.0502(17) Uani 1 1 d . . .
O6 O 0.6670(3) 0.0681(2) 0.0864(2) 0.0421(15) Uani 1 1 d . . .
O7 O 0.8291(2) 0.2076(3) 0.2173(2) 0.0381(14) Uani 1 1 d . . .
O8 O 0.8044(3) 0.4169(3) 0.2182(2) 0.0450(16) Uani 1 1 d . . .
O9 O 0.6209(3) 0.5120(3) 0.0733(2) 0.0480(17) Uani 1 1 d . . .
O12 O 0.5427(2) 0.2740(3) 0.1326(2) 0.0341(13) Uani 1 1 d . . .
O13 O 0.6210(2) 0.3414(2) 0.19952(19) 0.0297(12) Uani 1 1 d . . .
O14 O 0.5331(2) 0.3485(3) 0.0571(2) 0.0352(14) Uani 1 1 d . . .
O19 O 0.6060(2) 0.4116(2) 0.11864(19) 0.0303(12) Uani 1 1 d . . .
O21 O 0.62966(19) 0.2866(2) 0.12599(17) 0.0210(10) Uani 1 1 d . . .
O23 O 0.6305(2) 0.2273(2) 0.2020(2) 0.0312(13) Uani 1 1 d . . .
O25 O 0.5451(2) 0.2075(3) 0.0579(2) 0.0323(13) Uani 1 1 d . . .
O26 O 0.6332(2) 0.1630(2) 0.1236(2) 0.0284(12) Uani 1 1 d . . .
O37 O 0.7278(2) 0.2438(2) 0.20359(18) 0.0257(11) Uani 1 1 d . . .
O38 O 0.7155(2) 0.3552(2) 0.20429(19) 0.0285(12) Uani 1 1 d . . .
O41 O 0.5545(2) 0.3414(3) -0.06555(19) 0.0308(13) Uani 1 1 d . . .
O45 O 0.5063(2) 0.2766(3) -0.0255(2) 0.0365(14) Uani 1 1 d . . .
O49 O 0.5894(2) 0.4082(2) 0.02034(19) 0.0313(13) Uani 1 1 d . . .
O51 O 0.5747(2) 0.2344(2) -0.05818(19) 0.0270(12) Uani 1 1 d . . .
O54 O 0.60570(18) 0.2890(2) 0.03173(17) 0.0201(10) Uani 1 1 d . . .
O56 O 0.6133(2) 0.1655(2) 0.02609(19) 0.0276(12) Uani 1 1 d . . .
O61 O 0.7161(2) 0.1451(2) 0.05001(19) 0.0245(11) Uani 1 1 d . . .
O67 O 0.7370(2) 0.1544(2) 0.15016(19) 0.0290(12) Uani 1 1 d . . .
O71 O 0.79254(19) 0.2212(2) 0.11284(18) 0.0219(10) Uani 1 1 d . . .
O76 O 0.69162(18) 0.2434(2) 0.09382(17) 0.0176(10) Uani 1 1 d . . .
O78 O 0.7781(2) 0.3095(2) 0.16801(18) 0.0255(11) Uani 1 1 d . . .
O81 O 0.7718(2) 0.4032(2) 0.11181(19) 0.0270(12) Uani 1 1 d . . .
O89 O 0.7052(2) 0.4484(2) 0.1440(2) 0.0332(13) Uani 1 1 d . . .
O91 O 0.6872(2) 0.4488(2) 0.0452(2) 0.0312(13) Uani 1 1 d . . .
O98 O 0.67923(19) 0.3514(2) 0.09424(17) 0.0207(10) Uani 1 1 d . . .
O100 O 0.7910(2) 0.2667(2) 0.0082(2) 0.0315(12) Uani 1 1 d . . .
O101 O 0.8164(2) 0.1079(2) 0.0912(2) 0.0363(14) Uani 1 1 d . . .
O102 O 0.86066(19) 0.1925(2) 0.06176(18) 0.0240(11) Uani 1 1 d . . .
O103 O 0.7669(2) 0.1288(2) -0.01870(19) 0.0251(11) Uani 1 1 d . . .
C1 C 0.7801(4) 0.4785(4) 0.0445(4) 0.046(2) Uani 1 1 d . . .
C2 C 0.7534(6) 0.5000(5) -0.0125(5) 0.071(4) Uani 1 1 d . . .
C3 C 0.8353(5) 0.4531(5) 0.0583(5) 0.063(3) Uani 1 1 d . . .
C4 C 0.7833(6) 0.5299(5) 0.0816(5) 0.076(4) Uani 1 1 d . . .
C5 C 0.5512(3) 0.2839(4) -0.1505(3) 0.038(2) Uani 1 1 d . . .
C6 C 0.4912(3) 0.2742(6) -0.1680(4) 0.057(3) Uani 1 1 d . . .
C7 C 0.5756(4) 0.2294(5) -0.1634(3) 0.055(3) Uani 1 1 d . . .
C8 C 0.5622(4) 0.3386(5) -0.1746(3) 0.058(3) Uani 1 1 d . . .
N1 N 0.6688(4) 0.6545(5) 0.1546(4) 0.065(3) Uiso 1 1 d . A .
C9 C 0.6306(7) 0.6088(8) 0.1511(7) 0.113(6) Uiso 1 1 d . . .
C10 C 0.6213(6) 0.6008(7) 0.1960(6) 0.094(5) Uiso 1 1 d . . .
C11 C 0.5757(8) 0.5527(9) 0.1805(8) 0.129(6) Uiso 1 1 d . . .
C12 C 0.5622(8) 0.5378(9) 0.2242(8) 0.133(7) Uiso 1 1 d . . .
C13 C 0.7249(6) 0.6429(7) 0.2032(6) 0.088(4) Uiso 1 1 d . . .
C14 C 0.7491(7) 0.5844(8) 0.2071(7) 0.116(6) Uiso 1 1 d D . .
C15 C 0.8018(9) 0.5700(12) 0.2552(9) 0.184(10) Uiso 1 1 d D . .
C16 C 0.8443(13) 0.5912(16) 0.2404(14) 0.258(16) Uiso 1 1 d D . .
C17 C 0.6792(7) 0.6521(8) 0.1050(7) 0.114(6) Uiso 1 1 d . . .
C18A C 0.6296(12) 0.6636(13) 0.0557(11) 0.088(8) Uiso 0.50 1 d PD A 1
C19A C 0.6390(14) 0.6647(17) 0.0062(11) 0.126(13) Uiso 0.50 1 d PD A 1
C20A C 0.5956(13) 0.6938(16) -0.0416(13) 0.115(11) Uiso 0.50 1 d PD A 1
C18B C 0.7295(14) 0.6947(16) 0.1098(14) 0.110(11) Uiso 0.50 1 d PD A 2
C19B C 0.740(2) 0.696(3) 0.0609(19) 0.24(3) Uiso 0.50 1 d PD A 2
C20B C 0.7814(18) 0.744(2) 0.0697(18) 0.155(16) Uiso 0.50 1 d PD A 2
C21 C 0.6704(7) 0.7196(8) 0.1698(7) 0.114(6) Uiso 1 1 d D . .
C22 C 0.6276(10) 0.7561(11) 0.1351(10) 0.191(11) Uiso 1 1 d D A .
C23 C 0.6212(9) 0.8146(10) 0.1564(9) 0.161(9) Uiso 1 1 d D . .
C24 C 0.6603(10) 0.8596(11) 0.1596(10) 0.172(9) Uiso 1 1 d D A .
N2 N 0.7938(4) 0.0304(5) 0.1571(4) 0.078(3) Uani 1 1 d . . .
C25 C 0.7871(6) -0.0042(6) 0.1813(5) 0.079(4) Uani 1 1 d . . .
C26 C 0.7826(10) -0.0465(8) 0.2163(9) 0.152(9) Uani 1 1 d . . .
N3 N 0.6053(5) 0.4630(5) -0.0847(4) 0.078(3) Uani 1 1 d . . .
C27 C 0.5764(6) 0.4883(6) -0.0720(5) 0.079(4) Uani 1 1 d . . .
C28 C 0.5408(5) 0.5181(6) -0.0559(5) 0.077(4) Uani 1 1 d . . .
N4 N 0.5000 0.2565(9) 0.2500 0.096(5) Uiso 1 2 d S . .
C29 C 0.4853(9) 0.2185(10) 0.2034(9) 0.141(7) Uiso 1 1 d . . .
C30 C 0.4333(11) 0.1818(12) 0.1965(11) 0.195(11) Uiso 1 1 d D . .
C31 C 0.4161(12) 0.1476(13) 0.1427(11) 0.220 Uiso 1 1 d D . .
C32 C 0.4441(12) 0.0888(14) 0.1677(12) 0.220 Uiso 1 1 d D . .
C33 C 0.4563(7) 0.2937(8) 0.2488(7) 0.113(6) Uiso 1 1 d . . .
C34 C 0.4337(9) 0.3308(11) 0.1957(9) 0.157(8) Uiso 1 1 d . . .
C35 C 0.4120(13) 0.3847(15) 0.2025(13) 0.220 Uiso 1 1 d . . .
C36 C 0.3687(12) 0.4072(14) 0.1428(13) 0.220 Uiso 1 1 d . . .
N5 N 0.4916(9) 0.0106(11) 0.0274(9) 0.088(7) Uiso 0.50 1 d P . .
C37 C 0.5457(7) 0.0143(8) 0.0329(7) 0.109(5) Uiso 1 1 d D . .
C38 C 0.4779(9) 0.0726(12) 0.0296(10) 0.074(7) Uiso 0.50 1 d PD . .
C39 C 0.4193(10) 0.0787(14) 0.0163(13) 0.101(10) Uiso 0.50 1 d PD . .
C40 C 0.4120(15) 0.1454(14) 0.0123(15) 0.124(12) Uiso 0.50 1 d PD . .
C41 C 0.3550(17) 0.157(3) 0.002(2) 0.19(2) Uiso 0.50 1 d PD . .
C42 C 0.4879(13) -0.0268(14) 0.0746(13) 0.217(13) Uiso 1 1 d D . .
C43 C 0.5293(16) -0.0145(19) 0.1348(15) 0.32(2) Uiso 1 1 d D . .
C44 C 0.500(2) -0.058(2) 0.155(2) 0.19(2) Uiso 0.50 1 d PD . .
C45 C 0.535(2) -0.048(3) 0.212(2) 0.21(2) Uiso 0.50 1 d PD . .
C46 C 0.4285(17) 0.045(2) -0.0399(18) 0.156(16) Uiso 0.50 1 d PD . .
C47 C 0.3827(19) 0.054(2) -0.026(2) 0.165(18) Uiso 0.50 1 d PD . .
C48 C 0.3607(18) 0.116(2) -0.0324(18) 0.156(16) Uiso 0.50 1 d PD . .
C49 C 0.5407(17) -0.0192(17) 0.0751(14) 0.137(14) Uiso 0.50 1 d PD . .
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'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Zr Zr -2.9673 0.5597 '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 101.6(2) . .
O1 W1 O12 101.5(3) . .
O13 W1 O12 92.7(2) . .
O1 W1 O19 101.7(3) . .
O13 W1 O19 90.3(2) . .
O12 W1 O19 155.5(2) . .
O1 W1 O14 101.4(2) . .
O13 W1 O14 156.2(2) . .
O12 W1 O14 88.5(2) . .
O19 W1 O14 79.3(2) . .
O1 W1 O21 171.8(2) . .
O13 W1 O21 73.12(19) . .
O12 W1 O21 72.8(2) . .
O19 W1 O21 84.88(19) . .
O14 W1 O21 84.57(19) . .
O2 W2 O26 104.5(3) . .
O2 W2 O23 100.0(3) . .
O26 W2 O23 93.7(2) . .
O2 W2 O25 101.4(3) . .
O26 W2 O25 86.7(2) . .
O23 W2 O25 157.8(2) . .
O2 W2 O12 100.4(3) . .
O26 W2 O12 154.9(2) . .
O23 W2 O12 85.2(2) . .
O25 W2 O12 85.2(2) . .
O2 W2 O21 168.7(2) . .
O26 W2 O21 84.58(19) . .
O23 W2 O21 72.33(19) . .
O25 W2 O21 85.65(19) . .
O12 W2 O21 71.20(19) . .
O3 W3 O37 104.5(2) . .
O3 W3 O23 100.2(3) . .
O37 W3 O23 95.0(2) . .
O3 W3 O38 101.4(3) . .
O37 W3 O38 87.0(2) . .
O23 W3 O38 157.1(2) . .
O3 W3 O13 100.3(2) . .
O37 W3 O13 154.7(2) . .
O23 W3 O13 85.0(2) . .
O38 W3 O13 83.6(2) . .
O3 W3 O21 168.7(2) . .
O37 W3 O21 84.92(19) . .
O23 W3 O21 72.39(19) . .
O38 W3 O21 85.06(19) . .
O13 W3 O21 70.98(18) . .
O4 W4 O14 101.2(3) . .
O4 W4 O49 102.5(3) . .
O14 W4 O49 89.8(2) . .
O4 W4 O45 101.8(3) . .
O14 W4 O45 92.5(3) . .
O49 W4 O45 154.6(2) . .
O4 W4 O41 96.0(3) . .
O14 W4 O41 162.8(2) . .
O49 W4 O41 87.2(2) . .
O45 W4 O41 83.1(2) . .
O4 W4 O54 173.8(3) . .
O14 W4 O54 83.5(2) . .
O49 W4 O54 81.45(19) . .
O45 W4 O54 73.7(2) . .
O41 W4 O54 79.35(18) . .
O5 W5 O25 102.0(3) . .
O5 W5 O56 101.6(3) . .
O25 W5 O56 90.0(2) . .
O5 W5 O45 99.1(3) . .
O25 W5 O45 90.0(2) . .
O56 W5 O45 158.9(2) . .
O5 W5 O51 98.2(3) . .
O25 W5 O51 159.8(2) . .
O56 W5 O51 87.3(2) . .
O45 W5 O51 85.4(2) . .
O5 W5 O54 170.2(3) . .
O25 W5 O54 85.1(2) . .
O56 W5 O54 85.17(19) . .
O45 W5 O54 73.8(2) . .
O51 W5 O54 74.76(18) . .
O6 W6 O61 102.3(2) . .
O6 W6 O67 102.8(3) . .
O61 W6 O67 92.0(2) . .
O6 W6 O56 102.2(3) . .
O61 W6 O56 93.4(2) . .
O67 W6 O56 152.7(2) . .
O6 W6 O26 95.2(2) . .
O61 W6 O26 162.4(2) . .
O67 W6 O26 85.5(2) . .
O56 W6 O26 81.4(2) . .
O6 W6 O76 172.9(2) . .
O61 W6 O76 83.28(18) . .
O67 W6 O76 72.46(19) . .
O56 W6 O76 81.62(18) . .
O26 W6 O76 79.34(18) . .
O7 W7 O71 102.1(2) . .
O7 W7 O67 99.6(3) . .
O71 W7 O67 95.0(2) . .
O7 W7 O78 101.0(3) . .
O71 W7 O78 93.9(2) . .
O67 W7 O78 155.3(2) . .
O7 W7 O37 97.1(2) . .
O71 W7 O37 160.7(2) . .
O67 W7 O37 83.6(2) . .
O78 W7 O37 80.4(2) . .
O7 W7 O76 173.6(2) . .
O71 W7 O76 80.65(19) . .
O67 W7 O76 74.28(19) . .
O78 W7 O76 84.51(19) . .
O37 W7 O76 80.44(17) . .
O8 W8 O38 101.9(3) . .
O8 W8 O78 103.5(3) . .
O38 W8 O78 89.6(2) . .
O8 W8 O89 100.2(3) . .
O38 W8 O89 90.8(2) . .
O78 W8 O89 155.7(2) . .
O8 W8 O81 98.0(3) . .
O38 W8 O81 160.1(2) . .
O78 W8 O81 86.6(2) . .
O89 W8 O81 84.8(2) . .
O8 W8 O98 171.2(3) . .
O38 W8 O98 83.99(19) . .
O78 W8 O98 82.91(19) . .
O89 W8 O98 73.0(2) . .
O81 W8 O98 76.17(18) . .
O9 W9 O19 102.6(3) . .
O9 W9 O49 100.6(3) . .
O19 W9 O49 89.5(2) . .
O9 W9 O89 100.5(3) . .
O19 W9 O89 91.5(2) . .
O49 W9 O89 158.1(2) . .
O9 W9 O91 95.7(2) . .
O19 W9 O91 161.7(2) . .
O49 W9 O91 87.4(2) . .
O89 W9 O91 84.9(2) . .
O9 W9 O98 171.8(3) . .
O19 W9 O98 84.4(2) . .
O49 W9 O98 83.6(2) . .
O89 W9 O98 74.8(2) . .
O91 W9 O98 77.43(18) . .
O103 Zr1 O71 161.46(19) . .
O103 Zr1 O102 92.4(2) . .
O71 Zr1 O102 89.34(19) . .
O103 Zr1 O100 90.9(2) . 7_655
O71 Zr1 O100 100.2(2) . 7_655
O102 Zr1 O100 137.7(2) . 7_655
O103 Zr1 O61 87.76(19) . .
O71 Zr1 O61 81.14(19) . .
O102 Zr1 O61 148.1(2) . .
O100 Zr1 O61 74.2(2) 7_655 .
O103 Zr1 O100 101.8(2) . .
O71 Zr1 O100 96.4(2) . .
O102 Zr1 O100 73.6(2) . .
O100 Zr1 O100 64.5(2) 7_655 .
O61 Zr1 O100 137.6(2) . .
O103 Zr1 O101 82.2(2) . .
O71 Zr1 O101 80.6(2) . .
O102 Zr1 O101 73.8(2) . .
O100 Zr1 O101 148.3(2) 7_655 .
O61 Zr1 O101 74.6(2) . .
O100 Zr1 O101 147.3(2) . .
O103 Zr1 Zr1 97.50(14) . 7_655
O71 Zr1 Zr1 99.82(14) . 7_655
O102 Zr1 Zr1 105.57(14) . 7_655
O100 Zr1 Zr1 32.30(14) 7_655 7_655
O61 Zr1 Zr1 106.07(14) . 7_655
O100 Zr1 Zr1 32.15(15) . 7_655
O101 Zr1 Zr1 179.26(14) . 7_655
O76 P1 O98 111.6(3) . .
O76 P1 O54 111.7(3) . .
O98 P1 O54 111.2(3) . .
O76 P1 O21 108.9(3) . .
O98 P1 O21 106.6(3) . .
O54 P1 O21 106.5(3) . .
O103 P2 O91 110.8(3) 7_655 .
O103 P2 O81 110.4(3) 7_655 .
O91 P2 O81 110.8(3) . .
O103 P2 C1 111.3(4) 7_655 .
O91 P2 C1 107.9(4) . .
O81 P2 C1 105.5(4) . .
O102 P3 O41 109.6(3) 7_655 .
O102 P3 O51 112.2(3) 7_655 .
O41 P3 O51 109.8(3) . .
O102 P3 C5 110.3(3) 7_655 .
O41 P3 C5 109.0(4) . .
O51 P3 C5 105.7(4) . .
W1 O12 W2 124.2(3) . .
W1 O13 W3 124.3(3) . .
W4 O14 W1 153.0(3) . .
W9 O19 W1 152.1(3) . .
P1 O21 W3 124.1(3) . .
P1 O21 W2 123.9(3) . .
W3 O21 W2 90.61(15) . .
P1 O21 W1 125.6(3) . .
W3 O21 W1 91.24(15) . .
W2 O21 W1 91.37(16) . .
W2 O23 W3 124.2(2) . .
W5 O25 W2 145.7(3) . .
W2 O26 W6 154.7(3) . .
W3 O37 W7 152.9(3) . .
W8 O38 W3 146.0(3) . .
P3 O41 W4 133.8(3) . .
W4 O45 W5 121.3(3) . .
W9 O49 W4 144.7(3) . .
P3 O51 W5 136.0(3) . .
P1 O54 W5 127.0(3) . .
P1 O54 W4 129.0(3) . .
W5 O54 W4 91.11(16) . .
W5 O56 W6 152.2(3) . .
W6 O61 Zr1 147.7(3) . .
W7 O67 W6 120.9(2) . .
W7 O71 Zr1 148.7(3) . .
P1 O76 W7 129.0(3) . .
P1 O76 W6 129.5(3) . .
W7 O76 W6 89.27(16) . .
W8 O78 W7 153.9(3) . .
P2 O81 W8 135.1(3) . .
W9 O89 W8 121.2(3) . .
P2 O91 W9 133.5(3) . .
P1 O98 W9 128.4(3) . .
P1 O98 W8 127.5(3) . .
W9 O98 W8 90.98(16) . .
Zr1 O100 Zr1 115.5(2) 7_655 .
P3 O102 Zr1 169.2(3) 7_655 .
P2 O103 Zr1 169.6(3) 7_655 .
C3 C1 C2 111.3(9) . .
C3 C1 C4 111.1(9) . .
C2 C1 C4 109.1(9) . .
C3 C1 P2 107.9(7) . .
C2 C1 P2 110.3(7) . .
C4 C1 P2 107.1(6) . .
C8 C5 C7 111.1(8) . .
C8 C5 C6 112.2(8) . .
C7 C5 C6 109.9(8) . .
C8 C5 P3 108.0(6) . .
C7 C5 P3 107.5(6) . .
C6 C5 P3 107.8(6) . .
C9 N1 C21 129.6(12) . .
C9 N1 C17 109.5(12) . .
C21 N1 C17 106.9(11) . .
C9 N1 C13 110.7(11) . .
C21 N1 C13 91.2(10) . .
C17 N1 C13 105.8(10) . .
C10 C9 N1 116.4(15) . .
C9 C10 C11 106.3(15) . .
C12 C11 C10 113.1(16) . .
C14 C13 N1 117.4(13) . .
C13 C14 C15 119.2(18) . .
C16 C15 C14 105(2) . .
C18A C17 N1 111.9(16) . .
C18A C17 C18B 112(2) . .
N1 C17 C18B 113.0(17) . .
C17 C18A C19A 113(2) . .
C20A C19A C18A 116(3) . .
C19B C18B C17 115(3) . .
C20B C19B C18B 107(4) . .
C22 C21 N1 117.0(17) . .
C21 C22 C23 117(2) . .
C24 C23 C22 115(2) . .
N2 C25 C26 175(2) . .
N3 C27 C28 178.6(14) . .
C33 N4 C33 109.7(19) . 2_655
C33 N4 C29 114.4(11) . .
C33 N4 C29 105.1(11) 2_655 .
C33 N4 C29 105.1(11) . 2_655
C33 N4 C29 114.4(11) 2_655 2_655
C29 N4 C29 108(2) . 2_655
N4 C29 C30 107.2(17) . .
C31 C30 C29 105(2) . .
C32 C31 C30 96(2) . .
N4 C33 C34 108.0(15) . .
C35 C34 C33 110(2) . .
C34 C35 C36 107(3) . .
C37 N5 C38 102.6(19) . .
C37 N5 C49 57.8(13) . .
C38 N5 C49 121(2) . .
C37 N5 C42 112(2) . .
C38 N5 C42 111(2) . .
C49 N5 C42 54.6(17) . .
C37 N5 C37 106.6(17) . 5_655
C38 N5 C37 108.3(19) . 5_655
C49 N5 C37 130(2) . 5_655
C42 N5 C37 115(2) . 5_655
C37 N5 N5 58.5(14) . 5_655
C38 N5 N5 117(2) . 5_655
C49 N5 N5 99(2) . 5_655
C42 N5 N5 133(3) . 5_655
C37 N5 N5 48.1(12) 5_655 5_655
N5 C37 C49 66(2) . .
N5 C37 C46 112(2) . 5_655
C49 C37 C46 69(2) . 5_655
N5 C37 N5 73.4(17) . 5_655
C49 C37 N5 115(2) . 5_655
C46 C37 N5 83(2) 5_655 5_655
N5 C38 C39 111(2) . .
N5 C38 C46 74(2) . .
C39 C38 C46 65(2) . .
C47 C39 C38 120(3) . .
C47 C39 C40 109(3) . .
C38 C39 C40 102(2) . .
C47 C39 C48 55.3(18) . .
C38 C39 C48 138(3) . .
C40 C39 C48 55(2) . .
C47 C39 C46 52.3(19) . .
C38 C39 C46 69(2) . .
C40 C39 C46 114(3) . .
C48 C39 C46 88(2) . .
C41 C40 C39 106(3) . .
C41 C40 C48 54(3) . .
C39 C40 C48 72(2) . .
C48 C41 C40 66(3) . .
C49 C42 C43 74(2) . .
C49 C42 N5 62(2) . .
C43 C42 N5 120(3) . .
C44 C43 C42 91(3) . .
C44 C43 C49 129(3) . .
C42 C43 C49 49.8(19) . .
C45 C44 C43 95(4) . .
C37 C46 C47 120(4) 5_655 .
C37 C46 C49 55.0(17) 5_655 5_655
C47 C46 C49 156(4) . 5_655
C37 C46 C39 119(3) 5_655 .
C49 C46 C39 160(3) 5_655 .
C37 C46 C38 94(3) 5_655 .
C47 C46 C38 90(3) . .
C49 C46 C38 113(3) 5_655 .
C39 C46 C38 46.5(13) . .
C39 C47 C46 84(3) . .
C39 C47 C48 80(3) . .
C46 C47 C48 116(4) . .
C41 C48 C47 134(5) . .
C41 C48 C40 60(2) . .
C47 C48 C40 97(3) . .
C41 C48 C39 97(3) . .
C47 C48 C39 45(2) . .
C40 C48 C39 52.8(16) . .
C37 C49 C42 120(3) . .
C37 C49 N5 56.2(15) . .
C42 C49 N5 64(2) . .
C37 C49 C46 56(2) . 5_655
C42 C49 C46 136(4) . 5_655
N5 C49 C46 97(2) . 5_655
C37 C49 C43 145(3) . .
C42 C49 C43 56.5(15) . .
N5 C49 C43 109(3) . .
C46 C49 C43 154(3) 5_655 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
W1 O1 1.700(5) .
W1 O13 1.846(5) .
W1 O12 1.869(6) .
W1 O19 1.953(6) .
W1 O14 1.961(5) .
W1 O21 2.373(5) .
W2 O2 1.697(6) .
W2 O26 1.808(5) .
W2 O23 1.907(6) .
W2 O25 1.940(5) .
W2 O12 1.973(6) .
W2 O21 2.373(5) .
W3 O3 1.702(5) .
W3 O37 1.813(5) .
W3 O23 1.908(6) .
W3 O38 1.942(6) .
W3 O13 1.987(5) .
W3 O21 2.370(5) .
W4 O4 1.694(6) .
W4 O14 1.842(5) .
W4 O49 1.889(6) .
W4 O45 1.897(6) .
W4 O41 2.006(5) .
W4 O54 2.333(5) .
W5 O5 1.691(6) .
W5 O25 1.856(5) .
W5 O56 1.876(6) .
W5 O45 1.914(6) .
W5 O51 2.006(5) .
W5 O54 2.320(5) .
W6 O6 1.700(6) .
W6 O61 1.786(5) .
W6 O67 1.914(6) .
W6 O56 1.927(6) .
W6 O26 2.040(5) .
W6 O76 2.388(5) .
W7 O7 1.696(5) .
W7 O71 1.791(4) .
W7 O67 1.894(6) .
W7 O78 1.909(5) .
W7 O37 2.061(5) .
W7 O76 2.326(5) .
W8 O8 1.683(6) .
W8 O38 1.854(5) .
W8 O78 1.864(5) .
W8 O89 1.915(6) .
W8 O81 1.991(5) .
W8 O98 2.364(5) .
W9 O9 1.688(6) .
W9 O19 1.856(5) .
W9 O49 1.889(6) .
W9 O89 1.902(6) .
W9 O91 2.004(5) .
W9 O98 2.299(5) .
Zr1 O103 2.067(5) .
Zr1 O71 2.082(5) .
Zr1 O102 2.108(5) .
Zr1 O100 2.129(5) 7_655
Zr1 O61 2.136(5) .
Zr1 O100 2.138(5) .
Zr1 O101 2.280(5) .
P1 O76 1.516(5) .
P1 O98 1.517(5) .
P1 O54 1.524(5) .
P1 O21 1.561(4) .
P2 O103 1.505(5) 7_655
P2 O91 1.537(6) .
P2 O81 1.541(6) .
P2 C1 1.809(8) .
P3 O102 1.487(5) 7_655
P3 O41 1.533(5) .
P3 O51 1.537(6) .
P3 C5 1.811(8) .
O100 Zr1 2.129(5) 7_655
O102 P3 1.487(5) 7_655
O103 P2 1.505(5) 7_655
C1 C3 1.539(15) .
C1 C2 1.544(15) .
C1 C4 1.564(13) .
C5 C8 1.530(14) .
C5 C7 1.548(13) .
C5 C6 1.551(12) .
N1 C9 1.474(19) .
N1 C21 1.56(2) .
N1 C17 1.569(19) .
N1 C13 1.604(17) .
C9 C10 1.43(2) .
C10 C11 1.60(2) .
C11 C12 1.49(2) .
C13 C14 1.49(2) .
C14 C15 1.552(17) .
C15 C16 1.511(18) .
C17 C18A 1.51(3) .
C17 C18B 1.67(4) .
C18A C19A 1.545(18) .
C19A C20A 1.530(19) .
C18B C19B 1.55(2) .
C19B C20B 1.54(2) .
C21 C22 1.445(17) .
C22 C23 1.518(17) .
C23 C24 1.483(17) .
N2 C25 1.121(14) .
C25 C26 1.439(17) .
N3 C27 1.179(15) .
C27 C28 1.446(17) .
N4 C33 1.49(2) .
N4 C33 1.49(2) 2_655
N4 C29 1.49(2) .
N4 C29 1.49(2) 2_655
C29 C30 1.62(3) .
C30 C31 1.599(18) .
C31 C32 1.568(18) .
C33 C34 1.61(3) .
C34 C35 1.43(3) .
C35 C36 1.69(4) .
N5 C37 1.46(3) .
N5 C38 1.49(3) .
N5 C49 1.61(4) .
N5 C42 1.64(4) .
N5 C37 1.68(3) 5_655
N5 N5 1.88(5) 5_655
C37 C49 1.490(18) .
C37 C46 1.51(5) 5_655
C37 N5 1.68(3) 5_655
C38 C39 1.527(18) .
C39 C47 1.33(5) .
C39 C40 1.544(19) .
C40 C41 1.524(19) .
C40 C48 1.60(6) .
C41 C48 1.42(6) .
C42 C49 1.49(4) .
C42 C43 1.625(19) .
C43 C44 1.558(19) .
C44 C45 1.52(2) .
C46 C37 1.51(5) 5_655
C46 C47 1.514(19) .
C46 C49 1.69(5) 5_655
C47 C48 1.539(19) .
C49 C46 1.69(5) 5_655
