#------------------------------------------------------------------------------
#$Date: 2016-03-21 19:19:44 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178845 $
#$URL: svn://www.crystallography.net/cod/cif/4/10/99/4109974.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_4109974
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_moiety         '6 C16 H36 N +, H2 O38 W10 Zr2 6-, C2 H3 N'
_chemical_formula_sum            'C98 H221 N7 O38 W10 Zr2'
_chemical_formula_weight         4126.75
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_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                 123.664(14)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   42.705(9)
_cell_length_b                   16.063(4)
_cell_length_c                   24.531(10)
_cell_measurement_reflns_used    265
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      28.50
_cell_measurement_theta_min      2.50
_cell_volume                     14006(8)
_computing_cell_refinement       EvalCCD
_computing_data_collection       'Nonius COLLECT'
_computing_data_reduction        EvalCCD
_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 0.960
_diffrn_measured_fraction_theta_max 0.960
_diffrn_measurement_device_type  'Nonius KappaCCD diffractometer'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0801
_diffrn_reflns_av_sigmaI/netI    0.0679
_diffrn_reflns_limit_h_max       50
_diffrn_reflns_limit_h_min       -50
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            48162
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         3.90
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    8.385
_exptl_absorpt_correction_T_max  0.188
_exptl_absorpt_correction_T_min  0.093
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.959
_exptl_crystal_description       block
_exptl_crystal_F_000             7940
_exptl_crystal_size_max          0.54
_exptl_crystal_size_mid          0.50
_exptl_crystal_size_min          0.30
_refine_diff_density_max         2.195
_refine_diff_density_min         -2.276
_refine_diff_density_rms         0.304
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.119
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     722
_refine_ls_number_reflns         11842
_refine_ls_number_restraints     54
_refine_ls_restrained_S_all      1.116
_refine_ls_R_factor_all          0.0966
_refine_ls_R_factor_gt           0.0543
_refine_ls_shift/su_max          0.024
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0491P)²+847.7634P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1258
_refine_ls_wR_factor_ref         0.1622
_reflns_number_gt                8312
_reflns_number_total             11842
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            ja0725495si20070418_010810_2.cif
_cod_data_source_block           rje392_anion3
_cod_original_cell_volume        14006(7)
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               4109974
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_group
Zr1 Zr 0.55060(4) 0.51491(8) 0.53944(6) 0.0218(3) Uani 1 1 d . .
W1 W 0.621823(17) 0.60541(4) 0.67797(3) 0.02687(16) Uani 1 1 d . .
W2 W 0.607577(18) 0.65745(4) 0.53563(3) 0.03006(17) Uani 1 1 d . .
W3 W 0.614201(16) 0.45833(4) 0.50609(3) 0.02569(16) Uani 1 1 d . .
W4 W 0.628856(16) 0.40639(3) 0.64948(3) 0.02433(15) Uani 1 1 d . .
W5 W 0.683816(16) 0.54787(4) 0.64296(3) 0.02649(16) Uani 1 1 d . .
O1A O 0.5064(6) 0.459(3) 0.5431(14) 0.044(9) Uani 0.54(6) 1 d PU 1
O1B O 0.5022(8) 0.513(4) 0.5486(15) 0.047(11) Uani 0.46(6) 1 d PU 2
O2 O 0.6277(3) 0.6586(7) 0.7442(6) 0.042(3) Uani 1 1 d . .
O3 O 0.6029(3) 0.7487(7) 0.4951(6) 0.044(3) Uani 1 1 d . .
O4 O 0.6144(3) 0.4071(7) 0.4451(6) 0.041(3) Uani 1 1 d . .
O5 O 0.6395(3) 0.3164(6) 0.6952(5) 0.038(3) Uani 1 1 d . .
O6 O 0.7311(3) 0.5572(7) 0.6799(5) 0.033(2) Uani 1 1 d . .
O7 O 0.6748(3) 0.6048(6) 0.7018(5) 0.033(2) Uani 1 1 d . .
O8 O 0.6154(3) 0.6936(6) 0.6176(5) 0.033(2) Uani 1 1 d . .
O9 O 0.5707(3) 0.5845(6) 0.6267(5) 0.029(2) Uani 1 1 d . .
O10 O 0.6312(3) 0.4916(7) 0.7082(5) 0.036(3) Uani 1 1 d . .
O11 O 0.6624(3) 0.6452(6) 0.5863(5) 0.034(2) Uani 1 1 d . .
O12 O 0.5586(3) 0.6283(6) 0.5047(5) 0.034(2) Uani 1 1 d . .
O13 O 0.5781(3) 0.4105(6) 0.6028(5) 0.029(2) Uani 1 1 d . .
O14 O 0.6800(3) 0.4453(6) 0.6789(5) 0.027(2) Uani 1 1 d . .
O15 O 0.6687(3) 0.4874(6) 0.5643(5) 0.033(2) Uani 1 1 d . .
O16 O 0.6081(3) 0.5746(6) 0.4785(4) 0.027(2) Uani 1 1 d . .
O17 O 0.5647(3) 0.4528(6) 0.4796(4) 0.031(2) Uani 1 1 d . .
O18 O 0.6259(3) 0.3723(6) 0.5709(5) 0.032(2) Uani 1 1 d . .
O19 O 0.6165(3) 0.5317(5) 0.5908(4) 0.022(2) Uani 1 1 d . .
N1 N 0.7570(3) 0.2942(8) 0.6963(6) 0.031(3) Uani 1 1 d . .
N2 N 0.5093(4) 0.2034(8) 0.4522(7) 0.037(3) Uani 1 1 d . .
N3 N 0.6597(4) 0.6231(8) 0.3884(6) 0.032(3) Uani 1 1 d . .
C1 C 0.7967(4) 0.2854(9) 0.7091(8) 0.032(4) Uani 1 1 d . .
H1A H 0.8137 0.2608 0.7531 0.039 Uiso 1 1 calc R .
H1B H 0.7951 0.2459 0.6767 0.039 Uiso 1 1 calc R .
C2 C 0.8139(5) 0.3654(11) 0.7054(11) 0.049(5) Uani 1 1 d . .
H2A H 0.8130 0.4076 0.7339 0.059 Uiso 1 1 calc R .
H2B H 0.7990 0.3866 0.6599 0.059 Uiso 1 1 calc R .
C3 C 0.8544(5) 0.3533(11) 0.7266(11) 0.056(5) Uani 1 1 d . .
H3A H 0.8694 0.3339 0.7727 0.067 Uiso 1 1 calc R .
H3B H 0.8553 0.3094 0.6993 0.067 Uiso 1 1 calc R .
C4 C 0.8717(7) 0.4308(15) 0.7212(15) 0.087(8) Uani 1 1 d . .
H4A H 0.8966 0.4179 0.7301 0.130 Uiso 1 1 calc R .
H4B H 0.8744 0.4718 0.7531 0.130 Uiso 1 1 calc R .
H4C H 0.8556 0.4536 0.6769 0.130 Uiso 1 1 calc R .
C5 C 0.7584(5) 0.3507(9) 0.7475(7) 0.032(4) Uani 1 1 d . .
H5A H 0.7327 0.3558 0.7380 0.038 Uiso 1 1 calc R .
H5B H 0.7666 0.4069 0.7438 0.038 Uiso 1 1 calc R .
C6 C 0.7850(6) 0.3198(11) 0.8182(9) 0.049(5) Uani 1 1 d . .
H6A H 0.7781 0.2624 0.8221 0.059 Uiso 1 1 calc R .
H6B H 0.8112 0.3190 0.8296 0.059 Uiso 1 1 calc R .
C7 C 0.7826(6) 0.3759(13) 0.8647(10) 0.059(5) Uani 1 1 d . .
H7A H 0.7885 0.4334 0.8587 0.071 Uiso 1 1 calc R .
H7B H 0.7563 0.3757 0.8526 0.071 Uiso 1 1 calc R .
C8 C 0.8078(7) 0.3537(15) 0.9352(11) 0.075(7) Uani 1 1 d . .
H8A H 0.7999 0.3842 0.9604 0.113 Uiso 1 1 calc R .
H8B H 0.8337 0.3686 0.9511 0.113 Uiso 1 1 calc R .
H8C H 0.8062 0.2937 0.9407 0.113 Uiso 1 1 calc R .
C9 C 0.7443(4) 0.2060(9) 0.7000(8) 0.035(4) Uani 1 1 d . .
H9A H 0.7420 0.1719 0.6644 0.042 Uiso 1 1 calc R .
H9B H 0.7640 0.1804 0.7422 0.042 Uiso 1 1 calc R .
C10 C 0.7070(5) 0.2043(10) 0.6945(9) 0.043(4) Uani 1 1 d . .
H10A H 0.6884 0.2393 0.6572 0.051 Uiso 1 1 calc R .
H10B H 0.7105 0.2271 0.7350 0.051 Uiso 1 1 calc R .
C11 C 0.6923(5) 0.1132(11) 0.6839(9) 0.047(4) Uani 1 1 d . .
H11A H 0.6844 0.0946 0.6395 0.056 Uiso 1 1 calc R .
H11B H 0.7131 0.0764 0.7161 0.056 Uiso 1 1 calc R .
C12 C 0.6601(6) 0.1047(12) 0.6912(11) 0.066(6) Uani 1 1 d . .
H12A H 0.6507 0.0474 0.6812 0.098 Uiso 1 1 calc R .
H12B H 0.6399 0.1430 0.6609 0.098 Uiso 1 1 calc R .
H12C H 0.6684 0.1183 0.7363 0.098 Uiso 1 1 calc R .
C13 C 0.7293(4) 0.3336(9) 0.6285(7) 0.031(3) Uani 1 1 d . .
H13A H 0.7054 0.3461 0.6245 0.037 Uiso 1 1 calc R .
H13B H 0.7399 0.3869 0.6257 0.037 Uiso 1 1 calc R .
C14 C 0.7209(6) 0.2784(12) 0.5715(8) 0.050(5) Uani 1 1 d . .
H14A H 0.7448 0.2555 0.5802 0.060 Uiso 1 1 calc R .
H14B H 0.7050 0.2311 0.5678 0.060 Uiso 1 1 calc R .
C15 C 0.7013(6) 0.3252(13) 0.5087(9) 0.055(5) Uani 1 1 d . .
H15A H 0.7185 0.3692 0.5118 0.066 Uiso 1 1 calc R .
H15B H 0.6792 0.3533 0.5034 0.066 Uiso 1 1 calc R .
C16 C 0.6882(6) 0.2747(13) 0.4476(8) 0.059(5) Uani 1 1 d . .
H16A H 0.6745 0.3109 0.4090 0.088 Uiso 1 1 calc R .
H16B H 0.6715 0.2301 0.4440 0.088 Uiso 1 1 calc R .
H16C H 0.7100 0.2504 0.4501 0.088 Uiso 1 1 calc R .
C17 C 0.5436(5) 0.1665(10) 0.4559(10) 0.045(4) Uani 1 1 d . .
H17A H 0.5567 0.1281 0.4938 0.054 Uiso 1 1 calc R .
H17B H 0.5347 0.1332 0.4159 0.054 Uiso 1 1 calc R .
C18 C 0.5715(5) 0.2308(11) 0.4626(12) 0.061(6) Uani 1 1 d . .
H18A H 0.5730 0.2775 0.4903 0.073 Uiso 1 1 calc R .
H18B H 0.5630 0.2534 0.4189 0.073 Uiso 1 1 calc R .
C19 C 0.6125(7) 0.1896(16) 0.4951(14) 0.080(7) Uani 1 1 d . .
H19A H 0.6313 0.2327 0.5037 0.096 Uiso 1 1 calc R .
H19B H 0.6205 0.1623 0.5371 0.096 Uiso 1 1 calc R .
C20 C 0.6096(10) 0.132(3) 0.4510(16) 0.147(16) Uani 1 1 d . .
H20A H 0.6344 0.1070 0.4680 0.221 Uiso 1 1 calc R .
H20B H 0.6006 0.1591 0.4091 0.221 Uiso 1 1 calc R .
H20C H 0.5919 0.0881 0.4445 0.221 Uiso 1 1 calc R .
C21 C 0.5215(5) 0.2473(10) 0.5160(9) 0.046(4) Uani 1 1 d . .
H21A H 0.4988 0.2680 0.5130 0.055 Uiso 1 1 calc R .
H21B H 0.5369 0.2963 0.5208 0.055 Uiso 1 1 calc R .
C22 C 0.5445(5) 0.1931(12) 0.5789(9) 0.056(5) Uani 1 1 d . .
H22A H 0.5318 0.1388 0.5714 0.067 Uiso 1 1 calc R .
H22B H 0.5698 0.1823 0.5879 0.067 Uiso 1 1 calc R .
C23 C 0.5487(7) 0.2338(13) 0.6370(10) 0.065(6) Uani 1 1 d . .
H23A H 0.5234 0.2448 0.6278 0.078 Uiso 1 1 calc R .
H23B H 0.5615 0.2880 0.6445 0.078 Uiso 1 1 calc R .
C24 C 0.5709(6) 0.1812(15) 0.6987(9) 0.064(6) Uani 1 1 d . .
H24A H 0.5558 0.1720 0.7171 0.095 Uiso 1 1 calc R .
H24B H 0.5942 0.2102 0.7310 0.095 Uiso 1 1 calc R .
H24C H 0.5770 0.1274 0.6880 0.095 Uiso 1 1 calc R .
C25 C 0.4843(5) 0.1286(11) 0.4417(9) 0.045(4) Uani 1 1 d . .
H25A H 0.4777 0.1000 0.4009 0.054 Uiso 1 1 calc R .
H25B H 0.4991 0.0891 0.4783 0.054 Uiso 1 1 calc R .
C26 C 0.4483(5) 0.1475(12) 0.4371(10) 0.049(5) Uani 1 1 d . .
H26A H 0.4326 0.1859 0.4001 0.059 Uiso 1 1 calc R .
H26B H 0.4541 0.1747 0.4779 0.059 Uiso 1 1 calc R .
C27 C 0.4268(7) 0.0647(13) 0.4264(12) 0.070(6) Uani 1 1 d . .
H27A H 0.4204 0.0397 0.3845 0.083 Uiso 1 1 calc R .
H27B H 0.4437 0.0255 0.4620 0.083 Uiso 1 1 calc R .
C28 C 0.3910(7) 0.0748(14) 0.4249(16) 0.094(9) Uani 1 1 d . .
H28A H 0.3816 0.0198 0.4268 0.141 Uiso 1 1 calc R .
H28B H 0.3719 0.1030 0.3843 0.141 Uiso 1 1 calc R .
H28C H 0.3962 0.1081 0.4626 0.141 Uiso 1 1 calc R .
C29 C 0.4891(5) 0.2677(9) 0.3999(9) 0.045(4) Uani 1 1 d . .
H29A H 0.5068 0.3135 0.4087 0.054 Uiso 1 1 calc R .
H29B H 0.4686 0.2913 0.4027 0.054 Uiso 1 1 calc R .
C30 C 0.4719(5) 0.2360(11) 0.3291(8) 0.044(4) Uani 1 1 d . .
H30A H 0.4906 0.2015 0.3276 0.053 Uiso 1 1 calc R .
H30B H 0.4497 0.2009 0.3155 0.053 Uiso 1 1 calc R .
C31 C 0.4604(6) 0.3077(14) 0.2827(10) 0.060(5) Uani 1 1 d . .
H31A H 0.4831 0.3388 0.2931 0.071 Uiso 1 1 calc R .
H31B H 0.4443 0.3460 0.2883 0.071 Uiso 1 1 calc R .
C32 C 0.4386(8) 0.2775(16) 0.2102(10) 0.080(7) Uani 1 1 d . .
H32A H 0.4345 0.3248 0.1816 0.120 Uiso 1 1 calc R .
H32B H 0.4143 0.2541 0.1978 0.120 Uiso 1 1 calc R .
H32C H 0.4534 0.2348 0.2056 0.120 Uiso 1 1 calc R .
C33 C 0.6220(4) 0.5841(10) 0.3645(7) 0.032(4) Uani 1 1 d . .
H33A H 0.6105 0.6146 0.3843 0.038 Uiso 1 1 calc R .
H33B H 0.6262 0.5260 0.3806 0.038 Uiso 1 1 calc R .
C34 C 0.5939(5) 0.5832(12) 0.2899(8) 0.045(4) Uani 1 1 d . .
H34A H 0.5860 0.6410 0.2741 0.054 Uiso 1 1 calc R .
H34B H 0.6063 0.5602 0.2691 0.054 Uiso 1 1 calc R .
C35 C 0.5591(7) 0.5310(16) 0.2698(10) 0.084(8) Uani 1 1 d . .
H35A H 0.5665 0.4720 0.2814 0.100 Uiso 1 1 calc R .
H35B H 0.5481 0.5503 0.2940 0.100 Uiso 1 1 calc R .
C36 C 0.5300(8) 0.5380(18) 0.1971(11) 0.095(9) Uani 1 1 d . .
H36A H 0.5113 0.4935 0.1833 0.143 Uiso 1 1 calc R .
H36B H 0.5423 0.5327 0.1734 0.143 Uiso 1 1 calc R .
H36C H 0.5174 0.5922 0.1874 0.143 Uiso 1 1 calc R .
C37 C 0.6561(5) 0.7136(10) 0.3664(7) 0.039(4) Uani 1 1 d . .
H37A H 0.6433 0.7152 0.3182 0.046 Uiso 1 1 calc R .
H37B H 0.6816 0.7374 0.3862 0.046 Uiso 1 1 calc R .
C38 C 0.6340(5) 0.7676(10) 0.3855(9) 0.041(4) Uani 1 1 d . .
H38A H 0.6426 0.7566 0.4315 0.050 Uiso 1 1 calc R .
H38B H 0.6068 0.7546 0.3571 0.050 Uiso 1 1 calc R .
C39 C 0.6409(6) 0.8597(11) 0.3772(9) 0.056(5) Uani 1 1 d . .
H39A H 0.6678 0.8729 0.4089 0.067 Uiso 1 1 calc R .
H39B H 0.6353 0.8677 0.3326 0.067 Uiso 1 1 calc R .
C40 C 0.6172(8) 0.9194(13) 0.3873(13) 0.082(7) Uani 1 1 d . .
H40A H 0.6283 0.9752 0.3963 0.123 Uiso 1 1 calc R .
H40B H 0.6164 0.9008 0.4245 0.123 Uiso 1 1 calc R .
H40C H 0.5917 0.9210 0.3478 0.123 Uiso 1 1 calc R .
C41 C 0.6832(4) 0.6177(9) 0.4642(7) 0.032(4) Uani 1 1 d . .
H41A H 0.6679 0.6394 0.4801 0.038 Uiso 1 1 calc R .
H41B H 0.6888 0.5584 0.4772 0.038 Uiso 1 1 calc R .
C42 C 0.7204(5) 0.6662(11) 0.4976(8) 0.043(4) Uani 1 1 d . .
H42A H 0.7152 0.7266 0.4904 0.052 Uiso 1 1 calc R .
H42B H 0.7347 0.6498 0.4784 0.052 Uiso 1 1 calc R .
C43 C 0.7437(5) 0.6472(11) 0.5715(9) 0.048(5) Uani 1 1 d . .
H43A H 0.7277 0.6545 0.5887 0.057 Uiso 1 1 calc R .
H43B H 0.7648 0.6874 0.5943 0.057 Uiso 1 1 calc R .
C44 C 0.7599(6) 0.5567(12) 0.5865(9) 0.057(5) Uani 1 1 d . .
H44A H 0.7755 0.5480 0.6339 0.085 Uiso 1 1 calc R .
H44B H 0.7753 0.5489 0.5685 0.085 Uiso 1 1 calc R .
H44C H 0.7391 0.5167 0.5663 0.085 Uiso 1 1 calc R .
C45 C 0.6794(5) 0.5766(10) 0.3616(8) 0.035(4) Uani 1 1 d . .
H45A H 0.7052 0.5994 0.3828 0.042 Uiso 1 1 calc R .
H45B H 0.6660 0.5885 0.3142 0.042 Uiso 1 1 calc R .
C46 C 0.6824(5) 0.4818(10) 0.3710(9) 0.045(4) Uani 1 1 d . .
H46A H 0.6579 0.4559 0.3386 0.054 Uiso 1 1 calc R .
H46B H 0.6887 0.4682 0.4154 0.054 Uiso 1 1 calc R .
C47 C 0.7129(6) 0.4466(12) 0.3624(10) 0.055(5) Uani 1 1 d . .
H47A H 0.7119 0.4765 0.3263 0.065 Uiso 1 1 calc R .
H47B H 0.7075 0.3871 0.3500 0.065 Uiso 1 1 calc R .
C48 C 0.7529(6) 0.4547(12) 0.4255(9) 0.058(5) Uani 1 1 d . .
H48A H 0.7713 0.4303 0.4180 0.086 Uiso 1 1 calc R .
H48B H 0.7540 0.4253 0.4615 0.086 Uiso 1 1 calc R .
H48C H 0.7589 0.5136 0.4369 0.086 Uiso 1 1 calc R .
N4 N 0.4825(12) 0.047(2) 0.608(3) 0.112(16) Uani 0.50 1 d PDU .
C49 C 0.4737(10) 0.107(2) 0.6170(17) 0.060(10) Uani 0.50 1 d PDU .
C50 C 0.4678(11) 0.182(2) 0.642(2) 0.073(12) Uani 0.50 1 d PDU .
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'
W W -0.8490 6.8722 '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'
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
O1A Zr1 O1A 64.1(10) . 5_666
O1A Zr1 O9 93.1(11) . .
O1A Zr1 O9 116.9(12) 5_666 .
O1A Zr1 O12 136.4(10) . .
O1A Zr1 O12 78.7(8) 5_666 .
O1A Zr1 O13 77.2(9) . .
O1A Zr1 O13 135.1(9) 5_666 .
O1A Zr1 O17 115.2(13) . .
O1A Zr1 O17 92.8(11) 5_666 .
O1A Zr1 O19 147.0(7) . .
O1A Zr1 O19 148.8(6) 5_666 .
O1B Zr1 O1B 64.7(14) . 5_666
O1B Zr1 O9 77.5(10) . .
O1B Zr1 O9 137.6(12) 5_666 .
O1B Zr1 O12 115.1(15) . .
O1B Zr1 O12 95.2(14) 5_666 .
O1B Zr1 O13 94.7(14) . .
O1B Zr1 O13 114.6(15) 5_666 .
O1B Zr1 O17 135.0(11) . .
O1B Zr1 O17 75.4(11) 5_666 .
O1B Zr1 O19 148.3(8) . .
O1B Zr1 O19 146.9(8) 5_666 .
O9 Zr1 O12 83.6(4) . .
O9 Zr1 O13 85.9(4) . .
O9 Zr1 O17 146.4(4) . .
O9 Zr1 O19 73.0(3) . .
O12 Zr1 O13 145.1(4) . .
O12 Zr1 O17 87.4(4) . .
O12 Zr1 O19 73.0(3) . .
O13 Zr1 O17 83.2(4) . .
O13 Zr1 O19 72.1(3) . .
O17 Zr1 O19 73.4(4) . .
O2 W1 O7 100.2(5) . .
O2 W1 O8 103.9(5) . .
O2 W1 O9 103.4(5) . .
O2 W1 O10 102.5(5) . .
O2 W1 O19 177.7(5) . .
O7 W1 O8 83.4(4) . .
O7 W1 O9 156.4(4) . .
O7 W1 O10 85.5(4) . .
O7 W1 O19 77.6(4) . .
O8 W1 O9 90.0(4) . .
O8 W1 O10 152.7(4) . .
O8 W1 O19 76.9(4) . .
O9 W1 O10 90.3(4) . .
O9 W1 O19 78.8(4) . .
O10 W1 O19 76.5(4) . .
O3 W2 O8 104.1(5) . .
O3 W2 O11 99.6(5) . .
O3 W2 O12 103.7(5) . .
O3 W2 O16 102.2(5) . .
O3 W2 O19 177.3(4) . .
O8 W2 O11 85.0(4) . .
O8 W2 O12 90.5(4) . .
O8 W2 O16 153.0(4) . .
O8 W2 O19 77.2(4) . .
O11 W2 O12 156.7(4) . .
O11 W2 O16 84.4(4) . .
O11 W2 O19 78.1(4) . .
O12 W2 O16 89.6(4) . .
O12 W2 O19 78.6(4) . .
O16 W2 O19 76.3(3) . .
O4 W3 O15 99.8(5) . .
O4 W3 O16 102.9(5) . .
O4 W3 O17 103.2(5) . .
O4 W3 O18 104.4(5) . .
O4 W3 O19 177.4(4) . .
O15 W3 O16 84.5(4) . .
O15 W3 O17 157.0(4) . .
O15 W3 O18 85.0(4) . .
O15 W3 O19 77.9(4) . .
O16 W3 O17 91.0(4) . .
O16 W3 O18 152.1(4) . .
O16 W3 O19 76.0(3) . .
O17 W3 O18 88.8(4) . .
O17 W3 O19 79.2(4) . .
O18 W3 O19 76.5(3) . .
O5 W4 O10 102.7(5) . .
O5 W4 O13 103.5(5) . .
O5 W4 O14 100.8(5) . .
O5 W4 O18 104.9(5) . .
O5 W4 O19 177.7(5) . .
O10 W4 O13 89.7(4) . .
O10 W4 O14 85.1(4) . .
O10 W4 O18 151.8(4) . .
O10 W4 O19 75.7(4) . .
O13 W4 O14 155.8(4) . .
O13 W4 O18 89.2(4) . .
O13 W4 O19 78.3(4) . .
O14 W4 O18 84.4(4) . .
O14 W4 O19 77.4(3) . .
O18 W4 O19 76.5(4) . .
O6 W5 O7 103.4(5) . .
O6 W5 O11 105.0(5) . .
O6 W5 O14 102.1(5) . .
O6 W5 O15 102.6(4) . .
O6 W5 O19 178.9(4) . .
O7 W5 O11 86.8(4) . .
O7 W5 O14 87.7(4) . .
O7 W5 O15 154.0(4) . .
O7 W5 O19 76.9(4) . .
O11 W5 O14 152.9(4) . .
O11 W5 O15 85.7(4) . .
O11 W5 O19 76.1(4) . .
O14 W5 O15 87.7(4) . .
O14 W5 O19 76.8(4) . .
O15 W5 O19 77.1(4) . .
Zr1 O1A Zr1 115.9(10) . 5_666
Zr1 O1B Zr1 115.3(14) . 5_666
W1 O7 W5 116.7(5) . .
W1 O8 W2 116.1(5) . .
Zr1 O9 W1 116.5(4) . .
W1 O10 W4 117.8(5) . .
W2 O11 W5 117.2(5) . .
Zr1 O12 W2 116.9(5) . .
Zr1 O13 W4 118.1(5) . .
W4 O14 W5 117.4(5) . .
W3 O15 W5 116.4(5) . .
W2 O16 W3 117.3(4) . .
Zr1 O17 W3 116.4(5) . .
W3 O18 W4 117.2(5) . .
Zr1 O19 W1 91.7(3) . .
Zr1 O19 W2 91.5(3) . .
Zr1 O19 W3 91.0(3) . .
Zr1 O19 W4 91.5(3) . .
Zr1 O19 W5 179.6(5) . .
W1 O19 W2 89.7(3) . .
W1 O19 W3 177.3(4) . .
W1 O19 W4 90.0(3) . .
W1 O19 W5 88.7(3) . .
W2 O19 W3 90.4(3) . .
W2 O19 W4 177.0(4) . .
W2 O19 W5 88.7(3) . .
W3 O19 W4 89.8(3) . .
W3 O19 W5 88.6(3) . .
W4 O19 W5 88.3(3) . .
C1 N1 C5 110.4(12) . .
C1 N1 C9 106.6(10) . .
C1 N1 C13 110.8(12) . .
C5 N1 C9 110.7(12) . .
C5 N1 C13 107.5(10) . .
C9 N1 C13 110.9(12) . .
C17 N2 C21 110.2(13) . .
C17 N2 C25 105.1(11) . .
C17 N2 C29 113.5(13) . .
C21 N2 C25 110.2(13) . .
C21 N2 C29 105.6(12) . .
C25 N2 C29 112.3(13) . .
C33 N3 C37 112.4(12) . .
C33 N3 C41 106.6(11) . .
C33 N3 C45 110.9(12) . .
C37 N3 C41 110.4(11) . .
C37 N3 C45 106.6(11) . .
C41 N3 C45 110.1(12) . .
N1 C1 C2 115.2(12) . .
C1 C2 C3 111.8(14) . .
C2 C3 C4 113.0(16) . .
N1 C5 C6 113.9(12) . .
C5 C6 C7 110.2(14) . .
C6 C7 C8 115.5(17) . .
N1 C9 C10 113.4(12) . .
C9 C10 C11 109.8(14) . .
C10 C11 C12 112.3(16) . .
N1 C13 C14 113.6(12) . .
C13 C14 C15 111.7(15) . .
C14 C15 C16 116.3(16) . .
N2 C17 C18 114.2(14) . .
C17 C18 C19 110.4(16) . .
C18 C19 C20 107(2) . .
N2 C21 C22 115.5(13) . .
C21 C22 C23 112.3(16) . .
C22 C23 C24 112.7(18) . .
N2 C25 C26 116.3(14) . .
C25 C26 C27 108.8(15) . .
C26 C27 C28 114.0(18) . .
N2 C29 C30 115.1(13) . .
C29 C30 C31 110.6(15) . .
C30 C31 C32 111.4(18) . .
N3 C33 C34 115.4(12) . .
C33 C34 C35 111.6(15) . .
C34 C35 C36 111(2) . .
N3 C37 C38 112.8(13) . .
C37 C38 C39 107.8(14) . .
C38 C39 C40 113.2(18) . .
N3 C41 C42 113.8(13) . .
C41 C42 C43 109.4(14) . .
C42 C43 C44 112.0(15) . .
N3 C45 C46 116.1(13) . .
C45 C46 C47 110.5(15) . .
C46 C47 C48 112.5(15) . .
N4 C49 C50 169(5) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Zr1 O1A 2.14(2) .
Zr1 O1A 2.18(2) 5_666
Zr1 O1B 2.20(3) .
Zr1 O1B 2.13(3) 5_666
Zr1 O9 2.128(10) .
Zr1 O12 2.118(11) .
Zr1 O13 2.141(10) .
Zr1 O17 2.121(10) .
Zr1 O19 2.376(9) .
W1 O2 1.727(10) .
W1 O7 1.998(10) .
W1 O8 1.957(10) .
W1 O9 1.848(10) .
W1 O10 1.929(11) .
W1 O19 2.341(9) .
W2 O3 1.720(10) .
W2 O8 1.935(11) .
W2 O11 1.958(11) .
W2 O12 1.845(11) .
W2 O16 1.940(10) .
W2 O19 2.343(9) .
W3 O4 1.710(10) .
W3 O15 1.997(11) .
W3 O16 1.954(10) .
W3 O17 1.837(11) .
W3 O18 1.952(11) .
W3 O19 2.345(9) .
W4 O5 1.729(10) .
W4 O10 1.948(11) .
W4 O13 1.808(11) .
W4 O14 1.983(10) .
W4 O18 1.938(10) .
W4 O19 2.357(9) .
W5 O6 1.702(10) .
W5 O7 1.919(10) .
W5 O11 1.951(11) .
W5 O14 1.918(10) .
W5 O15 1.925(10) .
W5 O19 2.429(9) .
O1A Zr1 2.18(2) 5_666
O1B Zr1 2.13(3) 5_666
N1 C1 1.550(18) .
N1 C5 1.524(19) .
N1 C9 1.536(19) .
N1 C13 1.544(18) .
N2 C17 1.53(2) .
N2 C21 1.52(2) .
N2 C25 1.53(2) .
N2 C29 1.49(2) .
N3 C33 1.510(19) .
N3 C37 1.529(19) .
N3 C41 1.550(19) .
N3 C45 1.522(19) .
C1 C2 1.51(2) .
C2 C3 1.52(2) .
C3 C4 1.49(3) .
C5 C6 1.54(2) .
C6 C7 1.50(2) .
C7 C8 1.49(3) .
C9 C10 1.52(2) .
C10 C11 1.56(2) .
C11 C12 1.49(3) .
C13 C14 1.52(2) .
C14 C15 1.49(2) .
C15 C16 1.51(3) .
C17 C18 1.52(2) .
C18 C19 1.61(3) .
C19 C20 1.38(4) .
C21 C22 1.56(2) .
C22 C23 1.49(3) .
C23 C24 1.52(3) .
C25 C26 1.51(2) .
C26 C27 1.55(3) .
C27 C28 1.52(3) .
C29 C30 1.55(2) .
C30 C31 1.50(3) .
C31 C32 1.56(3) .
C33 C34 1.53(2) .
C34 C35 1.53(3) .
C35 C36 1.51(3) .
C37 C38 1.53(2) .
C38 C39 1.54(2) .
C39 C40 1.51(3) .
C41 C42 1.54(2) .
C42 C43 1.54(2) .
C43 C44 1.56(3) .
C45 C46 1.53(2) .
C46 C47 1.54(2) .
C47 C48 1.55(3) .
N4 C49 1.105(9) .
C49 C50 1.434(9) .
