#------------------------------------------------------------------------------
#$Date: 2016-03-23 15:47:14 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179347 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/44/4324480.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_4324480
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(P1 O1 C6 H5), 2(N1 O1 C3 H7), 2(H1 O1), 4(N1 C16 H36)'
_chemical_formula_sum            'C94 H180 N6 O76 P6 W18 Zr2'
_chemical_formula_weight         6288.00
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/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                 102.763(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   24.2257(14)
_cell_length_b                   24.138(7)
_cell_length_c                   15.099(3)
_cell_measurement_reflns_used    140
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      16
_cell_measurement_theta_min      3
_cell_volume                     8611(3)
_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    'SIR92 (Giacovazzo et al, 1993)'
_diffrn_ambient_temperature      200(2)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_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  0.0762
_diffrn_reflns_av_sigmaI/netI    0.0669
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            91896
_diffrn_reflns_theta_full        27.52
_diffrn_reflns_theta_max         27.52
_diffrn_reflns_theta_min         1.92
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    12.216
_exptl_absorpt_correction_T_max  0.0514
_exptl_absorpt_correction_T_min  0.0285
_exptl_absorpt_correction_type   cylinder
_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    2.425
_exptl_crystal_description       plate-like
_exptl_crystal_F_000             5792
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_refine_diff_density_max         3.250
_refine_diff_density_min         -2.660
_refine_diff_density_rms         0.304
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     640
_refine_ls_number_reflns         19648
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.1085
_refine_ls_R_factor_gt           0.0648
_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)+(0.0719P)²+235.7613P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1599
_refine_ls_wR_factor_ref         0.1865
_reflns_number_gt                12729
_reflns_number_total             19648
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic102223w_si_003.cif
_cod_data_source_block           (^n^Bu~4~N)~4~-1-Ph-DMF
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4324480
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -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
W1 W 0.16380(3) 0.52879(4) 0.46875(6) 0.0575(2) Uani 1 1 d .
W2 W 0.21205(3) 0.39462(4) 0.48697(5) 0.0511(2) Uani 1 1 d .
W3 W 0.23798(3) 0.47819(3) 0.67351(5) 0.04543(18) Uani 1 1 d .
W4 W 0.24097(3) 0.55317(4) 0.28391(5) 0.0517(2) Uani 1 1 d .
W5 W 0.28687(3) 0.42055(3) 0.30411(5) 0.04645(18) Uani 1 1 d .
W6 W 0.36977(3) 0.36520(3) 0.52318(4) 0.03730(15) Uani 1 1 d .
W7 W 0.39481(2) 0.44840(3) 0.70507(4) 0.03157(14) Uani 1 1 d .
W8 W 0.33910(3) 0.59203(3) 0.68897(5) 0.04072(16) Uani 1 1 d .
W9 W 0.27050(3) 0.64181(3) 0.48465(5) 0.04915(19) Uani 1 1 d .
Zr1 Zr 0.51151(6) 0.43984(6) 0.57506(9) 0.0290(3) Uani 1 1 d .
P1 P 0.31249(15) 0.50265(16) 0.4996(3) 0.0307(8) Uani 1 1 d .
P2 P 0.40984(18) 0.64684(18) 0.5470(3) 0.0385(9) Uani 1 1 d .
C1 C 0.4508(8) 0.7095(8) 0.5667(12) 0.051(4) Uiso 1 1 d .
C2 C 0.5087(11) 0.7084(11) 0.5968(18) 0.084(7) Uiso 1 1 d .
C3 C 0.5417(14) 0.7634(15) 0.622(2) 0.111(10) Uiso 1 1 d .
C4 C 0.5096(16) 0.8077(15) 0.618(2) 0.119(11) Uiso 1 1 d .
C5 C 0.4573(15) 0.8083(15) 0.587(2) 0.116(10) Uiso 1 1 d .
C6 C 0.4213(11) 0.7612(11) 0.5604(18) 0.084(7) Uiso 1 1 d .
P3 P 0.36686(17) 0.52118(18) 0.2471(3) 0.0380(9) Uani 1 1 d .
C7 C 0.3848(7) 0.5258(7) 0.1383(11) 0.042(4) Uani 1 1 d .
C8 C 0.3408(8) 0.5212(13) 0.0585(13) 0.084(8) Uani 1 1 d .
C9 C 0.3557(9) 0.5274(12) -0.0304(14) 0.079(7) Uani 1 1 d .
C10 C 0.4116(9) 0.5384(9) -0.0317(13) 0.058(5) Uani 1 1 d .
C11 C 0.4531(8) 0.5422(8) 0.0431(13) 0.051(4) Uani 1 1 d .
C12 C 0.4407(7) 0.5380(7) 0.1322(11) 0.041(4) Uani 1 1 d .
N1 N 0.5845(12) 0.2834(8) 0.6908(15) 0.096(8) Uani 1 1 d .
C13 C 0.5782(10) 0.3376(9) 0.6794(14) 0.071(6) Uani 1 1 d .
C14 C 0.6427(13) 0.2599(12) 0.721(2) 0.108(10) Uani 1 1 d .
C15 C 0.5405(16) 0.2452(13) 0.6734(17) 0.118(13) Uani 1 1 d .
O1 O 0.0964(5) 0.5523(8) 0.4393(11) 0.086(5) Uani 1 1 d .
O2 O 0.1713(5) 0.3359(7) 0.4680(9) 0.072(4) Uani 1 1 d .
O3 O 0.2130(5) 0.4726(6) 0.7704(8) 0.055(3) Uani 1 1 d .
O4 O 0.2002(5) 0.5874(7) 0.1933(9) 0.068(4) Uani 1 1 d .
O5 O 0.2756(6) 0.3694(6) 0.2237(8) 0.064(4) Uani 1 1 d .
O6 O 0.3727(6) 0.2945(5) 0.5145(9) 0.057(3) Uani 1 1 d .
O7 O 0.4167(5) 0.4304(5) 0.8172(7) 0.044(3) Uani 1 1 d .
O8 O 0.3525(6) 0.6242(5) 0.7928(9) 0.057(3) Uani 1 1 d .
O9 O 0.2407(7) 0.7062(7) 0.4567(11) 0.080(5) Uani 1 1 d .
O12 O 0.1527(5) 0.4540(7) 0.4458(8) 0.070(4) Uani 1 1 d .
O13 O 0.1737(5) 0.5183(6) 0.5943(8) 0.057(3) Uani 1 1 d .
O14 O 0.1890(5) 0.5358(6) 0.3539(8) 0.058(4) Uani 1 1 d .
O19 O 0.2086(5) 0.5986(6) 0.4909(9) 0.055(3) Uani 1 1 d .
O21 O 0.2540(4) 0.4824(5) 0.5216(7) 0.040(3) Uani 1 1 d .
O23 O 0.2062(5) 0.4132(6) 0.6087(9) 0.058(3) Uani 1 1 d .
O25 O 0.2309(5) 0.4064(6) 0.3685(8) 0.054(3) Uani 1 1 d .
O26 O 0.2843(4) 0.3680(5) 0.5227(7) 0.045(3) Uani 1 1 d .
O37 O 0.3089(4) 0.4487(5) 0.7032(7) 0.043(3) Uani 1 1 d .
O38 O 0.2743(5) 0.5505(5) 0.6910(8) 0.045(3) Uani 1 1 d .
O41 O 0.3152(5) 0.5593(5) 0.2429(8) 0.051(3) Uani 1 1 d .
O45 O 0.2413(4) 0.4809(6) 0.2374(8) 0.057(3) Uani 1 1 d .
O49 O 0.2694(5) 0.6116(5) 0.3670(8) 0.052(3) Uani 1 1 d .
O51 O 0.3505(5) 0.4606(5) 0.2595(8) 0.046(3) Uani 1 1 d .
O54 O 0.3039(4) 0.4991(5) 0.3965(7) 0.041(3) Uani 1 1 d .
O56 O 0.3416(5) 0.3880(5) 0.3958(7) 0.044(3) Uani 1 1 d .
O61 O 0.4415(4) 0.3851(4) 0.5231(7) 0.037(2) Uani 1 1 d .
O67 O 0.3804(4) 0.3764(4) 0.6530(7) 0.036(2) Uani 1 1 d .
O71 O 0.4619(4) 0.4576(5) 0.6696(7) 0.040(2) Uani 1 1 d .
O76 O 0.3579(4) 0.4625(5) 0.5481(7) 0.039(2) Uani 1 1 d .
O78 O 0.3839(4) 0.5273(4) 0.7144(8) 0.038(2) Uani 1 1 d .
O81 O 0.4038(5) 0.6264(4) 0.6427(8) 0.043(3) Uani 1 1 d .
O89 O 0.2936(5) 0.6481(5) 0.6144(8) 0.046(3) Uani 1 1 d .
O91 O 0.3522(5) 0.6628(5) 0.4854(8) 0.046(3) Uani 1 1 d .
O98 O 0.3223(4) 0.5603(5) 0.5349(7) 0.040(3) Uani 1 1 d .
O100 O 0.4640(5) 0.4775(5) 0.4514(8) 0.048(3) Uani 1 1 d .
O101 O 0.5303(5) 0.3609(5) 0.6543(8) 0.047(3) Uani 1 1 d .
O102 O 0.5609(4) 0.3968(5) 0.4963(8) 0.044(3) Uani 1 1 d .
O103 O 0.5843(4) 0.4603(5) 0.6798(7) 0.041(2) Uani 1 1 d .
N2 N 0.7537(11) 0.8439(12) 0.5518(18) 0.112(8) Uiso 1 1 d .
C16 C 0.7649(15) 0.9096(16) 0.551(3) 0.123(11) Uiso 1 1 d .
C17 C 0.7822(19) 0.926(2) 0.471(3) 0.160(16) Uiso 1 1 d .
C18 C 0.8078(16) 0.9874(16) 0.501(3) 0.127(12) Uiso 1 1 d .
C19 C 0.8668(16) 0.9823(16) 0.555(3) 0.132(12) Uiso 1 1 d .
C20 C 0.7005(12) 0.8295(13) 0.475(2) 0.097(8) Uiso 1 1 d .
C21 C 0.6407(14) 0.8661(14) 0.476(2) 0.114(10) Uiso 1 1 d .
C22 C 0.6010(17) 0.8467(18) 0.391(3) 0.140(13) Uiso 1 1 d .
C23 C 0.5479(19) 0.8782(19) 0.385(3) 0.154(15) Uiso 1 1 d .
C24 C 0.7313(14) 0.8377(13) 0.650(2) 0.115(10) Uiso 1 1 d D
C25 C 0.7102(15) 0.7776(13) 0.664(2) 0.126(11) Uiso 1 1 d D
C26 C 0.6954(13) 0.7735(13) 0.7607(19) 0.099(9) Uiso 1 1 d D
C27 C 0.756(2) 0.770(2) 0.824(4) 0.20(2) Uiso 1 1 d .
C28 C 0.8004(17) 0.8101(16) 0.539(3) 0.130(12) Uiso 1 1 d .
C29 C 0.846(2) 0.813(2) 0.612(4) 0.21(2) Uiso 1 1 d D
C30 C 0.890(2) 0.786(2) 0.566(4) 0.213 Uiso 1 1 d D
C31 C 0.948(2) 0.814(2) 0.598(4) 0.210 Uiso 1 1 d D
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'
Na Na 0.0362 0.0249 '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 O12 100.7(8) . .
O1 W1 O13 102.3(6) . .
O12 W1 O13 92.2(6) . .
O1 W1 O14 102.0(6) . .
O12 W1 O14 88.8(6) . .
O13 W1 O14 155.1(5) . .
O1 W1 O19 102.6(7) . .
O12 W1 O19 155.4(5) . .
O13 W1 O19 90.1(6) . .
O14 W1 O19 79.1(5) . .
O1 W1 O21 170.7(6) . .
O12 W1 O21 72.2(4) . .
O13 W1 O21 72.6(4) . .
O14 W1 O21 84.1(4) . .
O19 W1 O21 85.3(4) . .
O2 W2 O26 103.7(6) . .
O2 W2 O23 101.0(6) . .
O26 W2 O23 93.8(5) . .
O2 W2 O25 102.0(6) . .
O26 W2 O25 85.4(5) . .
O23 W2 O25 156.4(6) . .
O2 W2 O12 100.9(7) . .
O26 W2 O12 154.9(5) . .
O23 W2 O12 86.1(5) . .
O25 W2 O12 84.9(5) . .
O2 W2 O21 169.7(6) . .
O26 W2 O21 85.0(4) . .
O23 W2 O21 72.4(5) . .
O25 W2 O21 84.0(5) . .
O12 W2 O21 71.0(5) . .
O3 W3 O37 104.6(5) . .
O3 W3 O23 101.2(6) . .
O37 W3 O23 93.2(5) . .
O3 W3 O38 100.9(6) . .
O37 W3 O38 86.7(5) . .
O23 W3 O38 157.1(5) . .
O3 W3 O13 100.1(5) . .
O37 W3 O13 155.1(5) . .
O23 W3 O13 85.4(6) . .
O38 W3 O13 85.2(5) . .
O3 W3 O21 168.6(5) . .
O37 W3 O21 84.8(4) . .
O23 W3 O21 71.3(4) . .
O38 W3 O21 85.9(4) . .
O13 W3 O21 71.2(4) . .
O4 W4 O14 102.6(6) . .
O4 W4 O45 101.4(7) . .
O14 W4 O45 93.6(6) . .
O4 W4 O49 103.2(7) . .
O14 W4 O49 89.1(5) . .
O45 W4 O49 154.0(5) . .
O4 W4 O41 96.6(5) . .
O14 W4 O41 160.8(5) . .
O45 W4 O41 82.9(5) . .
O49 W4 O41 86.1(5) . .
O4 W4 O54 172.4(6) . .
O14 W4 O54 83.1(4) . .
O45 W4 O54 72.9(4) . .
O49 W4 O54 81.7(4) . .
O41 W4 O54 77.8(4) . .
O5 W5 O56 101.4(6) . .
O5 W5 O25 102.5(6) . .
O56 W5 O25 90.9(5) . .
O5 W5 O45 100.8(6) . .
O56 W5 O45 156.8(5) . .
O25 W5 O45 90.7(5) . .
O5 W5 O51 96.9(5) . .
O56 W5 O51 88.8(5) . .
O25 W5 O51 160.2(5) . .
O45 W5 O51 82.0(5) . .
O5 W5 O54 171.5(5) . .
O56 W5 O54 84.0(4) . .
O25 W5 O54 83.7(5) . .
O45 W5 O54 73.1(5) . .
O51 W5 O54 76.6(4) . .
O6 W6 O61 102.1(5) . .
O6 W6 O67 102.6(5) . .
O61 W6 O67 92.9(4) . .
O6 W6 O56 102.4(6) . .
O61 W6 O56 92.9(5) . .
O67 W6 O56 152.6(5) . .
O6 W6 O26 95.2(6) . .
O61 W6 O26 162.7(5) . .
O67 W6 O26 84.7(4) . .
O56 W6 O26 81.8(4) . .
O6 W6 O76 172.8(5) . .
O61 W6 O76 83.6(4) . .
O67 W6 O76 72.5(4) . .
O56 W6 O76 81.5(4) . .
O26 W6 O76 79.3(4) . .
O7 W7 O71 102.6(5) . .
O7 W7 O67 99.5(5) . .
O71 W7 O67 94.8(4) . .
O7 W7 O78 101.2(5) . .
O71 W7 O78 92.7(5) . .
O67 W7 O78 155.9(5) . .
O7 W7 O37 96.0(5) . .
O71 W7 O37 161.2(4) . .
O67 W7 O37 84.6(5) . .
O78 W7 O37 81.0(4) . .
O7 W7 O76 172.7(5) . .
O71 W7 O76 81.5(4) . .
O67 W7 O76 74.0(4) . .
O78 W7 O76 84.5(4) . .
O37 W7 O76 80.2(4) . .
O8 W8 O38 102.6(6) . .
O8 W8 O78 101.8(6) . .
O38 W8 O78 90.0(5) . .
O8 W8 O89 100.6(6) . .
O38 W8 O89 90.7(5) . .
O78 W8 O89 157.0(5) . .
O8 W8 O81 97.2(6) . .
O38 W8 O81 160.2(5) . .
O78 W8 O81 87.5(4) . .
O89 W8 O81 84.2(5) . .
O8 W8 O98 171.5(5) . .
O38 W8 O98 83.2(4) . .
O78 W8 O98 84.3(4) . .
O89 W8 O98 73.0(4) . .
O81 W8 O98 77.0(4) . .
O9 W9 O19 102.8(7) . .
O9 W9 O49 101.3(6) . .
O19 W9 O49 89.3(5) . .
O9 W9 O89 101.0(6) . .
O19 W9 O89 92.8(5) . .
O49 W9 O89 156.5(5) . .
O9 W9 O91 97.5(6) . .
O19 W9 O91 159.6(5) . .
O49 W9 O91 85.1(5) . .
O89 W9 O91 84.9(5) . .
O9 W9 O98 172.0(7) . .
O19 W9 O98 83.9(5) . .
O49 W9 O98 83.0(4) . .
O89 W9 O98 74.0(4) . .
O91 W9 O98 76.1(4) . .
O71 Zr1 O102 162.3(4) . .
O71 Zr1 O100 99.2(5) . 3_666
O102 Zr1 O100 97.8(5) . 3_666
O71 Zr1 O103 87.3(4) . .
O102 Zr1 O103 93.0(4) . .
O100 Zr1 O103 73.0(4) 3_666 .
O71 Zr1 O61 81.4(4) . .
O102 Zr1 O61 89.5(4) . .
O100 Zr1 O61 136.9(4) 3_666 .
O103 Zr1 O61 149.3(4) . .
O71 Zr1 O100 103.0(5) . .
O102 Zr1 O100 88.9(4) . .
O100 Zr1 O100 64.2(5) 3_666 .
O103 Zr1 O100 137.0(4) . .
O61 Zr1 O100 73.6(4) . .
O71 Zr1 O101 83.7(4) . .
O102 Zr1 O101 79.1(4) . .
O100 Zr1 O101 149.1(4) 3_666 .
O103 Zr1 O101 76.5(4) . .
O61 Zr1 O101 74.0(4) . .
O100 Zr1 O101 145.5(4) . .
O71 Zr1 Zr1 103.1(3) . 3_666
O102 Zr1 Zr1 93.9(3) . 3_666
O100 Zr1 Zr1 32.3(3) 3_666 3_666
O103 Zr1 Zr1 105.2(3) . 3_666
O61 Zr1 Zr1 105.2(3) . 3_666
O100 Zr1 Zr1 31.9(3) . 3_666
O101 Zr1 Zr1 173.0(3) . 3_666
O98 P1 O76 112.4(6) . .
O98 P1 O54 113.1(6) . .
O76 P1 O54 112.0(6) . .
O98 P1 O21 106.9(6) . .
O76 P1 O21 106.5(6) . .
O54 P1 O21 105.4(6) . .
O102 P2 O91 111.3(6) 3_666 .
O102 P2 O81 109.3(6) 3_666 .
O91 P2 O81 112.2(6) . .
O102 P2 C1 111.5(8) 3_666 .
O91 P2 C1 106.4(8) . .
O81 P2 C1 105.9(8) . .
C2 C1 C6 120(2) . .
C2 C1 P2 121.5(17) . .
C6 C1 P2 118.2(16) . .
C1 C2 C3 120(2) . .
C4 C3 C2 115(3) . .
C5 C4 C3 125(4) . .
C4 C5 C6 127(4) . .
C1 C6 C5 114(2) . .
O103 P3 O51 112.2(7) 3_666 .
O103 P3 O41 110.7(7) 3_666 .
O51 P3 O41 110.1(7) . .
O103 P3 C7 110.1(7) 3_666 .
O51 P3 C7 107.0(7) . .
O41 P3 C7 106.5(7) . .
C12 C7 C8 120.8(15) . .
C12 C7 P3 120.3(12) . .
C8 C7 P3 118.7(13) . .
C7 C8 C9 118.2(18) . .
C10 C9 C8 118.1(17) . .
C11 C10 C9 123.8(17) . .
C10 C11 C12 120.5(16) . .
C7 C12 C11 118.4(15) . .
C13 N1 C15 125(3) . .
C13 N1 C14 119(3) . .
C15 N1 C14 116(2) . .
O101 C13 N1 123(3) . .
W1 O12 W2 124.7(6) . .
W1 O13 W3 125.5(6) . .
W4 O14 W1 154.0(7) . .
W9 O19 W1 152.6(7) . .
P1 O21 W2 126.0(6) . .
P1 O21 W3 123.1(6) . .
W2 O21 W3 91.2(3) . .
P1 O21 W1 124.3(6) . .
W2 O21 W1 91.6(3) . .
W3 O21 W1 90.5(3) . .
W3 O23 W2 124.9(6) . .
W5 O25 W2 147.6(6) . .
W2 O26 W6 154.6(6) . .
W3 O37 W7 153.3(6) . .
W8 O38 W3 146.6(6) . .
P3 O41 W4 135.1(7) . .
W4 O45 W5 122.9(6) . .
W4 O49 W9 145.0(7) . .
P3 O51 W5 136.1(7) . .
P1 O54 W5 128.4(7) . .
P1 O54 W4 127.8(6) . .
W5 O54 W4 91.0(4) . .
W5 O56 W6 151.3(7) . .
W6 O61 Zr1 147.5(5) . .
W7 O67 W6 120.9(5) . .
W7 O71 Zr1 148.2(6) . .
P1 O76 W7 130.1(6) . .
P1 O76 W6 130.0(6) . .
W7 O76 W6 89.1(4) . .
W8 O78 W7 151.7(6) . .
P2 O81 W8 133.1(7) . .
W9 O89 W8 122.5(5) . .
P2 O91 W9 133.5(7) . .
P1 O98 W9 129.1(6) . .
P1 O98 W8 128.7(6) . .
W9 O98 W8 90.6(4) . .
Zr1 O100 Zr1 115.8(5) 3_666 .
C13 O101 Zr1 126.9(12) . .
P2 O102 Zr1 164.4(8) 3_666 .
P3 O103 Zr1 175.7(7) 3_666 .
C28 N2 C20 108(3) . .
C28 N2 C16 115(3) . .
C20 N2 C16 109(2) . .
C28 N2 C24 119(3) . .
C20 N2 C24 105(2) . .
C16 N2 C24 101(2) . .
C17 C16 N2 111(3) . .
C16 C17 C18 101(4) . .
C19 C18 C17 110(3) . .
N2 C20 C21 116(2) . .
C22 C21 C20 103(3) . .
C23 C22 C21 106(3) . .
C25 C24 N2 113(2) . .
C24 C25 C26 110(3) . .
C27 C26 C25 101(3) . .
C29 C28 N2 112(4) . .
C28 C29 C30 97(4) . .
C29 C30 C31 110(5) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
W1 O1 1.692(13) .
W1 O12 1.847(17) .
W1 O13 1.875(12) .
W1 O14 1.969(12) .
W1 O19 1.993(13) .
W1 O21 2.429(10) .
W2 O2 1.714(14) .
W2 O26 1.830(11) .
W2 O23 1.927(13) .
W2 O25 1.962(12) .
W2 O12 2.028(15) .
W2 O21 2.358(11) .
W3 O3 1.708(11) .
W3 O37 1.821(11) .
W3 O23 1.917(14) .
W3 O38 1.947(12) .
W3 O13 1.992(12) .
W3 O21 2.412(11) .
W4 O4 1.712(12) .
W4 O14 1.862(11) .
W4 O45 1.882(15) .
W4 O49 1.911(14) .
W4 O41 2.033(11) .
W4 O54 2.402(11) .
W5 O5 1.711(14) .
W5 O56 1.866(12) .
W5 O25 1.866(11) .
W5 O45 1.966(13) .
W5 O51 2.055(11) .
W5 O54 2.336(12) .
W6 O6 1.715(12) .
W6 O61 1.803(10) .
W6 O67 1.939(10) .
W6 O56 1.972(11) .
W6 O26 2.071(10) .
W6 O76 2.406(11) .
W7 O7 1.715(11) .
W7 O71 1.834(10) .
W7 O67 1.909(10) .
W7 O78 1.931(10) .
W7 O37 2.075(10) .
W7 O76 2.366(11) .
W8 O8 1.714(12) .
W8 O38 1.867(11) .
W8 O78 1.893(10) .
W8 O89 1.940(11) .
W8 O81 2.029(11) .
W8 O98 2.396(11) .
W9 O9 1.726(14) .
W9 O19 1.845(12) .
W9 O49 1.916(13) .
W9 O89 1.921(12) .
W9 O91 2.041(11) .
W9 O98 2.366(11) .
Zr1 O71 2.103(10) .
Zr1 O102 2.133(11) .
Zr1 O100 2.144(11) 3_666
Zr1 O103 2.151(10) .
Zr1 O61 2.156(10) .
Zr1 O100 2.165(11) .
Zr1 O101 2.243(11) .
P1 O98 1.490(12) .
P1 O76 1.526(11) .
P1 O54 1.527(11) .
P1 O21 1.600(10) .
P2 O102 1.499(12) 3_666
P2 O91 1.545(12) .
P2 O81 1.565(12) .
P2 C1 1.798(19) .
C1 C2 1.38(3) .
C1 C6 1.43(3) .
C2 C3 1.55(4) .
C3 C4 1.32(4) .
C4 C5 1.25(4) .
C5 C6 1.44(4) .
P3 O103 1.496(11) 3_666
P3 O51 1.536(12) .
P3 O41 1.543(13) .
P3 C7 1.793(16) .
C7 C12 1.41(2) .
C7 C8 1.43(2) .
C8 C9 1.47(3) .
C9 C10 1.38(3) .
C10 C11 1.34(3) .
C11 C12 1.45(2) .
N1 C13 1.32(3) .
N1 C15 1.39(4) .
N1 C14 1.49(4) .
C13 O101 1.27(2) .
O100 Zr1 2.144(11) 3_666
O102 P2 1.499(12) 3_666
O103 P3 1.496(11) 3_666
N2 C28 1.44(4) .
N2 C20 1.57(4) .
N2 C16 1.61(4) .
N2 C24 1.69(4) .
C16 C17 1.42(5) .
C17 C18 1.63(5) .
C18 C19 1.49(5) .
C20 C21 1.70(4) .
C21 C22 1.50(5) .
C22 C23 1.48(5) .
C24 C25 1.569(19) .
C25 C26 1.579(18) .
C26 C27 1.57(6) .
C28 C29 1.38(6) .
C29 C30 1.54(2) .
C30 C31 1.55(2) .
