#------------------------------------------------------------------------------
#$Date: 2016-03-21 19:19:44 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178845 $
#$URL: svn://www.crystallography.net/cod/cif/4/10/99/4109977.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_4109977
loop_
_publ_author_name
'R. John Errington'
'Sagar S. Petkar'
'Paul S. Middleton'
'William McFarlane'
'William Clegg'
'Robert A. Coxall'
'Ross W. Harrington'
_publ_section_title
;
 Synthesis and Reactivity of the Methoxozirconium Pentatungstate
 (nBu4N)6[{(μ-MeO)ZrW5O18}2]: Insights into Proton-Transfer Reactions,
 Solution Dynamics, and Assembly of {ZrW5O18}2- Building Blocks
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              12181
_journal_page_last               12196
_journal_paper_doi               10.1021/ja0725495
_journal_volume                  129
_journal_year                    2007
_chemical_formula_sum            'C55 H115 N3 O19 W5 Zr'
_chemical_formula_weight         2132.97
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           62
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2n'
_symmetry_space_group_name_H-M   'P n m a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   23.8193(11)
_cell_length_b                   17.1071(8)
_cell_length_c                   17.2814(8)
_cell_measurement_reflns_used    9654
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      25.63
_cell_measurement_theta_min      2.32
_cell_volume                     7041.8(6)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL and local programs'
_computing_structure_refinement  'Bruker SHELXTL'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker SMART 1K CCD diffractometer'
_diffrn_measurement_method       'ω rotation with narrow frames'
_diffrn_radiation_monochromator  'silicon 111'
_diffrn_radiation_source         'Daresbury SRS station 9.8'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.6934
_diffrn_reflns_av_R_equivalents  0.0867
_diffrn_reflns_av_sigmaI/netI    0.0494
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            34974
_diffrn_reflns_theta_full        22.66
_diffrn_reflns_theta_max         22.66
_diffrn_reflns_theta_min         1.67
_diffrn_standards_decay_%        20
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    8.342
_exptl_absorpt_correction_T_max  0.85
_exptl_absorpt_correction_T_min  0.43
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.012
_exptl_crystal_description       plate
_exptl_crystal_F_000             4112
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.02
_refine_diff_density_max         3.018
_refine_diff_density_min         -5.021
_refine_diff_density_rms         0.308
_refine_ls_extinction_coef       0.00011(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.344
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     416
_refine_ls_number_reflns         5245
_refine_ls_number_restraints     283
_refine_ls_restrained_S_all      1.312
_refine_ls_R_factor_all          0.1098
_refine_ls_R_factor_gt           0.0995
_refine_ls_shift/su_max          0.022
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0000P)²+660.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2147
_refine_ls_wR_factor_ref         0.2178
_reflns_number_gt                4510
_reflns_number_total             5245
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            ja0725495si20070418_010810_5.cif
_cod_data_source_block           rje313_anion5
_cod_database_code               4109977
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z'
'x+1/2, -y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -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 0.30942(7) 0.2500 0.21757(8) 0.0267(4) Uani 1 2 d S . .
W2 W 0.32440(5) 0.34664(7) 0.38268(6) 0.0376(4) Uani 1 1 d . . .
W3 W 0.20159(5) 0.34658(7) 0.29331(7) 0.0415(4) Uani 1 1 d . . .
Zr Zr 0.21840(17) 0.2500 0.4564(2) 0.0306(10) Uani 1 2 d S . .
O1 O 0.3414(12) 0.2500 0.1288(15) 0.053(8) Uani 1 2 d S . .
O2 O 0.3712(11) 0.4158(15) 0.4104(13) 0.078(9) Uani 1 1 d . . .
O3 O 0.1574(11) 0.4173(17) 0.2559(15) 0.089(9) Uani 1 1 d . . .
O4 O 0.1730(12) 0.2500 0.5556(17) 0.053(8) Uani 1 2 d S . .
O5 O 0.2628(10) 0.2500 0.3400(12) 0.020(5) Uani 1 2 d S . .
O6 O 0.2524(8) 0.3261(10) 0.2051(9) 0.035(4) Uani 1 1 d . . .
O7 O 0.3490(7) 0.3252(11) 0.2760(10) 0.039(5) Uani 1 1 d . . .
O8 O 0.1669(11) 0.2500 0.2634(14) 0.039(7) Uani 1 2 d S . .
O9 O 0.2651(9) 0.4033(10) 0.3351(11) 0.048(6) Uani 1 1 d . . .
O10 O 0.3620(11) 0.2500 0.4056(15) 0.042(7) Uani 1 2 d S . .
O11 O 0.1744(8) 0.3299(13) 0.3927(10) 0.048(5) Uani 1 1 d . . .
O12 O 0.2796(8) 0.3317(11) 0.4702(10) 0.040(5) Uani 1 1 d . . .
C1 C 0.121(2) 0.2500 0.581(2) 0.044(8) Uani 1 2 d SU . .
C2 C 0.115(2) 0.2500 0.664(2) 0.051(8) Uani 1 2 d SU . .
H2 H 0.1460 0.2500 0.6984 0.061 Uiso 1 2 calc SR . .
C3 C 0.057(2) 0.2500 0.691(3) 0.067(10) Uani 1 2 d SU . .
H3 H 0.0507 0.2500 0.7452 0.080 Uiso 1 2 calc SR . .
C4 C 0.015(2) 0.2500 0.645(3) 0.073(10) Uani 1 2 d SU . .
C5 C 0.021(2) 0.2500 0.563(3) 0.069(10) Uani 1 2 d SU . .
H5 H -0.0099 0.2500 0.5287 0.083 Uiso 1 2 calc SR . .
C6 C 0.0751(19) 0.2500 0.536(3) 0.048(8) Uani 1 2 d SU . .
H6 H 0.0806 0.2500 0.4814 0.058 Uiso 1 2 calc SR . .
C7 C -0.048(3) 0.2500 0.676(4) 0.11(2) Uani 1 2 d SU . .
H7A H -0.0745 0.2500 0.6324 0.167 Uiso 0.50 2 calc SPR . .
H7B H -0.0547 0.2968 0.7077 0.167 Uiso 0.25 1 calc PR . .
H7C H -0.0547 0.2032 0.7077 0.167 Uiso 0.25 1 calc PR . .
H7D H -0.0480 0.2500 0.7329 0.167 Uiso 0.50 2 calc SPR . .
H7E H -0.0679 0.2032 0.6575 0.167 Uiso 0.25 1 calc PR . .
H7F H -0.0679 0.2968 0.6575 0.167 Uiso 0.25 1 calc PR . .
N1 N 0.6815(11) 0.4984(15) -0.0856(15) 0.052(5) Uani 1 1 d U . .
C8 C 0.7158(13) 0.5713(18) -0.0589(19) 0.053(6) Uani 1 1 d U . .
H8A H 0.6891 0.6137 -0.0463 0.064 Uiso 1 1 calc R . .
H8B H 0.7390 0.5893 -0.1030 0.064 Uiso 1 1 calc R . .
C9 C 0.7553(15) 0.5587(16) 0.0124(17) 0.050(7) Uani 1 1 d U . .
H9A H 0.7334 0.5397 0.0572 0.060 Uiso 1 1 calc R . .
H9B H 0.7844 0.5193 -0.0001 0.060 Uiso 1 1 calc R . .
C10 C 0.7826(19) 0.6360(19) 0.032(2) 0.083(10) Uani 1 1 d U . .
H10A H 0.7537 0.6754 0.0446 0.099 Uiso 1 1 calc R . .
H10B H 0.8046 0.6553 -0.0131 0.099 Uiso 1 1 calc R . .
C11 C 0.821(2) 0.623(3) 0.101(2) 0.113(16) Uani 1 1 d U . .
H11A H 0.8394 0.6719 0.1149 0.170 Uiso 1 1 calc R . .
H11B H 0.8497 0.5837 0.0872 0.170 Uiso 1 1 calc R . .
H11C H 0.7989 0.6036 0.1447 0.170 Uiso 1 1 calc R . .
C12 C 0.6458(15) 0.4730(19) -0.0179(19) 0.062(7) Uani 1 1 d U . .
H12A H 0.6247 0.4260 -0.0344 0.074 Uiso 1 1 calc R . .
H12B H 0.6716 0.4563 0.0238 0.074 Uiso 1 1 calc R . .
C13 C 0.6057(17) 0.527(2) 0.016(2) 0.078(9) Uani 1 1 d U . .
H13A H 0.5798 0.5474 -0.0237 0.093 Uiso 1 1 calc R . .
H13B H 0.6252 0.5711 0.0412 0.093 Uiso 1 1 calc R . .
C14 C 0.5722(18) 0.477(3) 0.079(2) 0.092(11) Uani 1 1 d U . .
H14A H 0.5480 0.4371 0.0533 0.110 Uiso 1 1 calc R . .
H14B H 0.5981 0.4501 0.1147 0.110 Uiso 1 1 calc R . .
C15 C 0.540(2) 0.533(3) 0.117(3) 0.114(16) Uani 1 1 d U . .
H15A H 0.5177 0.5076 0.1570 0.171 Uiso 1 1 calc R . .
H15B H 0.5153 0.5586 0.0794 0.171 Uiso 1 1 calc R . .
H15C H 0.5651 0.5717 0.1401 0.171 Uiso 1 1 calc R . .
C16 C 0.6452(13) 0.5308(19) -0.1514(18) 0.053(7) Uani 1 1 d U . .
H16A H 0.6694 0.5563 -0.1905 0.064 Uiso 1 1 calc R . .
H16B H 0.6189 0.5705 -0.1308 0.064 Uiso 1 1 calc R . .
C17 C 0.6114(16) 0.463(2) -0.190(2) 0.076(9) Uani 1 1 d U . .
H17A H 0.6376 0.4215 -0.2062 0.091 Uiso 1 1 calc R . .
H17B H 0.5850 0.4408 -0.1517 0.091 Uiso 1 1 calc R . .
C18 C 0.5788(17) 0.492(2) -0.260(2) 0.093(12) Uani 1 1 d U . .
H18A H 0.5546 0.5361 -0.2433 0.111 Uiso 1 1 calc R . .
H18B H 0.6058 0.5126 -0.2983 0.111 Uiso 1 1 calc R . .
C19 C 0.543(2) 0.431(3) -0.298(3) 0.117(17) Uani 1 1 d U . .
H19A H 0.5210 0.4550 -0.3404 0.176 Uiso 1 1 calc R . .
H19B H 0.5166 0.4085 -0.2602 0.176 Uiso 1 1 calc R . .
H19C H 0.5664 0.3893 -0.3194 0.176 Uiso 1 1 calc R . .
C20 C 0.7189(15) 0.4368(19) -0.107(2) 0.062(7) Uani 1 1 d U . .
H20A H 0.6960 0.3895 -0.1160 0.075 Uiso 1 1 calc R . .
H20B H 0.7428 0.4257 -0.0610 0.075 Uiso 1 1 calc R . .
C21 C 0.7571(17) 0.447(2) -0.175(2) 0.080(9) Uani 1 1 d U . .
H21A H 0.7349 0.4668 -0.2195 0.096 Uiso 1 1 calc R . .
H21B H 0.7859 0.4870 -0.1625 0.096 Uiso 1 1 calc R . .
C22 C 0.7850(19) 0.373(2) -0.197(3) 0.100(12) Uani 1 1 d U . .
H22A H 0.7557 0.3336 -0.2069 0.120 Uiso 1 1 calc R . .
H22B H 0.8075 0.3550 -0.1521 0.120 Uiso 1 1 calc R . .
C23 C 0.8235(19) 0.378(3) -0.267(3) 0.115(16) Uani 1 1 d U . .
H23A H 0.8398 0.3260 -0.2774 0.172 Uiso 1 1 calc R . .
H23B H 0.8537 0.4154 -0.2577 0.172 Uiso 1 1 calc R . .
H23C H 0.8018 0.3943 -0.3127 0.172 Uiso 1 1 calc R . .
N2 N 0.4721(17) 0.7500 -0.385(2) 0.078(9) Uani 1 2 d SU . .
C24 C 0.514(2) 0.7500 -0.451(3) 0.083(11) Uani 1 2 d SU A .
H24A H 0.5379 0.7034 -0.4460 0.100 Uiso 0.50 1 calc PR . .
H24B H 0.5379 0.7966 -0.4460 0.100 Uiso 0.50 1 calc PR . .
C25 C 0.488(2) 0.7500 -0.532(3) 0.088(13) Uani 1 2 d SU . .
H25A H 0.4810 0.8043 -0.5497 0.106 Uiso 0.50 1 calc PR A .
H25B H 0.4520 0.7213 -0.5324 0.106 Uiso 0.50 1 calc PR . .
C26 C 0.534(3) 0.706(5) -0.593(4) 0.086(14) Uani 0.50 1 d PU A -1
H26A H 0.5439 0.6534 -0.5722 0.104 Uiso 0.50 1 calc PR A -1
H26B H 0.5171 0.6991 -0.6442 0.104 Uiso 0.50 1 calc PR A -1
C27 C 0.583(2) 0.7500 -0.600(3) 0.089(16) Uani 1 2 d SU . .
H27A H 0.6095 0.7233 -0.6349 0.134 Uiso 0.50 1 calc PR A -1
H27B H 0.6010 0.7560 -0.5489 0.134 Uiso 0.50 1 calc PR A -1
H27C H 0.5742 0.8017 -0.6207 0.134 Uiso 0.50 1 calc PR A -1
C28 C 0.506(2) 0.7500 -0.315(3) 0.088(11) Uani 1 2 d SU . .
H28A H 0.5306 0.7966 -0.3156 0.106 Uiso 0.50 1 calc PR . .
H28B H 0.5306 0.7034 -0.3156 0.106 Uiso 0.50 1 calc PR . .
C29 C 0.474(2) 0.7500 -0.240(3) 0.105(14) Uani 1 2 d SU B .
H29A H 0.4495 0.7033 -0.2385 0.125 Uiso 0.50 1 calc PR . .
H29B H 0.4495 0.7967 -0.2385 0.125 Uiso 0.50 1 calc PR . .
C30 C 0.512(3) 0.7500 -0.167(4) 0.103(18) Uani 1 2 d SU . .
H30A H 0.5467 0.7809 -0.1764 0.124 Uiso 0.50 1 calc PR B .
H30B H 0.4921 0.7734 -0.1223 0.124 Uiso 0.50 1 calc PR . .
C31 C 0.525(4) 0.681(6) -0.152(5) 0.10(2) Uani 0.50 1 d PU B -1
H31A H 0.5494 0.6788 -0.1072 0.148 Uiso 0.50 1 calc PR B -1
H31B H 0.5438 0.6579 -0.1972 0.148 Uiso 0.50 1 calc PR B -1
H31C H 0.4903 0.6511 -0.1416 0.148 Uiso 0.50 1 calc PR B -1
C32 C 0.4323(19) 0.818(3) -0.390(3) 0.109(11) Uani 1 1 d U . .
H32A H 0.4045 0.8136 -0.3481 0.131 Uiso 1 1 calc R . .
H32B H 0.4116 0.8141 -0.4399 0.131 Uiso 1 1 calc R . .
C33 C 0.458(3) 0.899(4) -0.386(4) 0.158(14) Uani 1 1 d U . .
H33A H 0.4996 0.8917 -0.3861 0.189 Uiso 1 1 calc R . .
H33B H 0.4483 0.9209 -0.3349 0.189 Uiso 1 1 calc R . .
C34 C 0.445(3) 0.966(4) -0.449(4) 0.166(17) Uani 1 1 d U . .
H34A H 0.4742 1.0070 -0.4529 0.199 Uiso 1 1 calc R . .
H34B H 0.4355 0.9453 -0.5012 0.199 Uiso 1 1 calc R . .
C35 C 0.399(2) 0.988(5) -0.407(3) 0.17(2) Uani 1 1 d U . .
H35A H 0.3788 1.0298 -0.4352 0.254 Uiso 1 1 calc R . .
H35B H 0.4111 1.0081 -0.3569 0.254 Uiso 1 1 calc R . .
H35C H 0.3740 0.9434 -0.4001 0.254 Uiso 1 1 calc R . .
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'
Zr Zr -4.4810 0.5380 '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 O5 178.8(11) . .
O1 W1 O6 102.6(8) . .
O1 W1 O6 102.6(8) . 7_565
O1 W1 O7 104.9(8) . .
O1 W1 O7 104.9(8) . 7_565
O5 W1 O6 76.5(6) . .
O5 W1 O6 76.6(6) . 7_565
O5 W1 O7 76.0(6) . .
O5 W1 O7 76.0(6) . 7_565
O6 W1 O6 86.9(11) . 7_565
O6 W1 O7 87.2(8) . .
O6 W1 O7 152.6(7) 7_565 .
O6 W1 O7 87.2(8) 7_565 7_565
O6 W1 O7 152.6(7) . 7_565
O7 W1 O7 85.9(12) . 7_565
Zr W2 O2 138.5(7) . .
Zr W2 O5 43.9(5) . .
Zr W2 O7 120.0(5) . .
Zr W2 O9 81.5(6) . .
Zr W2 O10 81.1(7) . .
Zr W2 O12 34.5(6) . .
O2 W2 O5 177.4(10) . .
O2 W2 O7 101.5(9) . .
O2 W2 O9 104.8(12) . .
O2 W2 O10 103.6(12) . .
O2 W2 O12 104.0(9) . .
O5 W2 O7 76.0(7) . .
O5 W2 O9 75.9(6) . .
O5 W2 O10 75.4(8) . .
O5 W2 O12 78.5(8) . .
O7 W2 O9 84.9(8) . .
O7 W2 O10 83.9(9) . .
O7 W2 O12 154.5(8) . .
O9 W2 O10 151.0(9) . .
O9 W2 O12 89.7(8) . .
O10 W2 O12 89.0(9) . .
Zr W3 O3 138.2(8) . .
Zr W3 O5 43.7(5) . .
Zr W3 O6 119.8(5) . .
Zr W3 O8 81.4(6) . .
Zr W3 O9 80.6(6) . .
Zr W3 O11 34.3(6) . .
O3 W3 O5 178.1(10) . .
O3 W3 O6 102.0(9) . .
O3 W3 O8 103.8(12) . .
O3 W3 O9 105.4(12) . .
O3 W3 O11 104.0(10) . .
O5 W3 O6 76.1(7) . .
O5 W3 O8 75.8(7) . .
O5 W3 O9 74.9(7) . .
O5 W3 O11 77.9(8) . .
O6 W3 O8 84.5(9) . .
O6 W3 O9 84.1(8) . .
O6 W3 O11 154.0(7) . .
O8 W3 O9 150.3(9) . .
O8 W3 O11 88.1(10) . .
O9 W3 O11 90.3(9) . .
W2 Zr W2 60.62(8) . 7_565
W2 Zr W3 60.48(6) . .
W2 Zr W3 90.79(9) . 7_565
W2 Zr W3 60.48(6) 7_565 7_565
W2 Zr W3 90.79(9) 7_565 .
W2 Zr O4 137.8(6) . .
W2 Zr O4 137.8(6) 7_565 .
W2 Zr O5 45.3(4) . .
W2 Zr O5 45.3(4) 7_565 .
W2 Zr O11 81.3(5) . .
W2 Zr O11 121.5(5) . 7_565
W2 Zr O11 81.3(5) 7_565 7_565
W2 Zr O11 121.5(5) 7_565 .
W2 Zr O12 31.4(5) . .
W2 Zr O12 80.8(5) . 7_565
W2 Zr O12 80.8(5) 7_565 .
W2 Zr O12 31.4(5) 7_565 7_565
W3 Zr W3 60.24(8) . 7_565
W3 Zr O4 131.2(7) . .
W3 Zr O4 131.2(7) 7_565 .
W3 Zr O5 45.5(4) . .
W3 Zr O5 45.5(4) 7_565 .
W3 Zr O11 30.8(5) . .
W3 Zr O11 30.8(5) 7_565 7_565
W3 Zr O11 79.1(6) 7_565 .
W3 Zr O11 79.1(6) . 7_565
W3 Zr O12 80.9(5) . .
W3 Zr O12 122.1(5) 7_565 .
W3 Zr O12 80.9(5) 7_565 7_565
W3 Zr O12 122.1(5) . 7_565
O4 Zr O5 175.5(11) . .
O4 Zr O11 100.5(8) . .
O4 Zr O11 100.5(8) . 7_565
O4 Zr O12 106.5(8) . .
O4 Zr O12 106.5(8) . 7_565
O5 Zr O11 76.2(6) . .
O5 Zr O11 76.2(6) . 7_565
O5 Zr O12 76.7(6) . .
O5 Zr O12 76.7(6) . 7_565
O11 Zr O11 83.9(13) . 7_565
O11 Zr O12 88.3(8) . .
O11 Zr O12 152.8(7) 7_565 .
O11 Zr O12 88.3(8) 7_565 7_565
O11 Zr O12 152.8(7) . 7_565
O12 Zr O12 86.9(11) . 7_565
Zr O4 C1 142(3) . .
W1 O5 W2 89.3(7) . .
W1 O5 W2 89.3(7) . 7_565
W1 O5 W3 89.1(6) . .
W1 O5 W3 89.1(6) . 7_565
W1 O5 Zr 179.9(11) . .
W2 O5 W2 90.4(8) . 7_565
W2 O5 W3 90.03(5) . .
W2 O5 W3 178.3(10) . 7_565
W2 O5 W3 90.03(5) 7_565 7_565
W2 O5 W3 178.3(10) 7_565 .
W2 O5 Zr 90.7(6) . .
W2 O5 Zr 90.7(6) 7_565 .
W3 O5 W3 89.5(8) . 7_565
W3 O5 Zr 90.9(7) . .
W3 O5 Zr 90.9(7) 7_565 .
W1 O6 W3 118.3(8) . .
W1 O7 W2 118.6(9) . .
W3 O8 W3 118.9(13) . 7_565
W2 O9 W3 119.1(9) . .
W2 O10 W2 118.7(14) . 7_565
W3 O11 Zr 115.0(9) . .
W2 O12 Zr 114.1(8) . .
O4 C1 C2 116(4) . .
O4 C1 C6 125(4) . .
C2 C1 C6 120(4) . .
C1 C2 C3 115(5) . .
C2 C3 C4 123(5) . .
C3 C4 C5 122(5) . .
C3 C4 C7 122(5) . .
C5 C4 C7 116(6) . .
C4 C5 C6 116(5) . .
C1 C6 C5 124(5) . .
C8 N1 C12 107(3) . .
C8 N1 C16 103(2) . .
C8 N1 C20 110(3) . .
C12 N1 C16 111(2) . .
C12 N1 C20 110(2) . .
C16 N1 C20 116(3) . .
N1 C8 C9 116(2) . .
C8 C9 C10 108(3) . .
C9 C10 C11 107(3) . .
N1 C12 C13 120(3) . .
C12 C13 C14 105(3) . .
C13 C14 C15 103(4) . .
N1 C16 C17 110(2) . .
C16 C17 C18 111(3) . .
C17 C18 C19 115(3) . .
N1 C20 C21 119(3) . .
C20 C21 C22 112(3) . .
C21 C22 C23 116(4) . .
C24 N2 C28 106(4) . .
C24 N2 C32 111(3) . .
C24 N2 C32 111(3) . 7_575
C28 N2 C32 114(3) . .
C28 N2 C32 114(3) . 7_575
C32 N2 C32 102(5) . 7_575
N2 C24 C25 116(4) . .
C24 C25 C26 108(4) . .
C24 C25 C26 108(4) . 7_575
C26 C25 C26 53(6) . 7_575
C25 C26 C27 111(6) . .
C26 C27 C26 66(7) . 7_575
N2 C28 C29 116(4) . .
C28 C29 C30 114(5) . .
C29 C30 C31 107(6) . .
C29 C30 C31 107(6) . 7_575
C31 C30 C31 144(10) . 7_575
N2 C32 C33 117(4) . .
C32 C33 C34 122(6) . .
C33 C34 C35 90(5) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
W1 O1 1.71(3) .
W1 O5 2.39(2) .
W1 O6 1.893(17) .
W1 O6 1.893(17) 7_565
W1 O7 1.888(18) .
W1 O7 1.888(18) 7_565
W2 Zr 3.276(4) .
W2 O2 1.69(2) .
W2 O5 2.330(16) .
W2 O7 1.969(16) .
W2 O9 1.90(2) .
W2 O10 1.922(14) .
W2 O12 1.868(16) .
W3 Zr 3.292(3) .
W3 O3 1.73(2) .
W3 O5 2.347(16) .
W3 O6 1.978(17) .
W3 O8 1.918(12) .
W3 O9 1.94(2) .
W3 O11 1.858(17) .
Zr W2 3.276(4) 7_565
Zr W3 3.292(3) 7_565
Zr O4 2.03(3) .
Zr O5 2.27(2) .
Zr O11 2.045(18) .
Zr O11 2.045(18) 7_565
Zr O12 2.034(18) .
Zr O12 2.034(18) 7_565
O4 C1 1.31(5) .
O5 W2 2.330(16) 7_565
O5 W3 2.347(16) 7_565
O8 W3 1.918(13) 7_565
O10 W2 1.922(14) 7_565
C1 C2 1.44(6) .
C1 C6 1.35(6) .
C2 C3 1.44(7) .
C3 C4 1.30(7) .
C4 C5 1.42(7) .
C4 C7 1.60(7) .
C5 C6 1.36(6) .
N1 C8 1.56(4) .
N1 C12 1.51(4) .
N1 C16 1.53(4) .
N1 C20 1.43(4) .
C8 C9 1.56(4) .
C9 C10 1.51(4) .
C10 C11 1.52(5) .
C12 C13 1.45(5) .
C13 C14 1.59(5) .
C14 C15 1.39(6) .
C16 C17 1.56(5) .
C17 C18 1.52(5) .
C18 C19 1.51(5) .
C20 C21 1.50(5) .
C21 C22 1.48(5) .
C22 C23 1.53(6) .
N2 C24 1.51(6) .
N2 C28 1.46(6) .
N2 C32 1.51(5) .
N2 C32 1.51(5) 7_575
C24 C25 1.53(6) .
C25 C26 1.69(8) .
C25 C26 1.69(8) 7_575
C26 C27 1.39(8) .
C27 C26 1.39(8) 7_575
C28 C29 1.50(7) .
C29 C30 1.56(8) .
C30 C31 1.25(10) .
C30 C31 1.25(10) 7_575
C32 C33 1.52(7) .
C33 C34 1.62(8) .
C34 C35 1.37(7) .
