# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2018

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_1
_database_code_depnum_ccdc_archive 'CCDC 1818604'
_audit_update_record             
;
2018-06-07 deposited with the CCDC.
2018-06-08 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C24 H60 Ce2 K N4 O68 P Ti2 W10'
_chemical_formula_weight         3777.21

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'
Ce Ce -0.2486 2.6331 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
K K 0.2009 0.2494 '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'
Ti Ti 0.2776 0.4457 '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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           12
_space_group_name_H-M_alt        'C 2/m'
_space_group_name_Hall           '-C 2y'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z'
'-x, -y, -z'
'x, -y, z'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z'

_cell_length_a                   21.8889(3)
_cell_length_b                   30.2502(5)
_cell_length_c                   15.2713(4)
_cell_angle_alpha                90
_cell_angle_beta                 133.3600(10)
_cell_angle_gamma                90
_cell_volume                     7351.8(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    200(2)
_cell_measurement_reflns_used    14132
_cell_measurement_theta_min      2.275
_cell_measurement_theta_max      25.00

_exptl_crystal_description       block
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    3.413
_exptl_crystal_F_000             6838
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.02
_exptl_absorpt_coefficient_mu    17.192
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.443
_exptl_absorpt_correction_T_max  0.709
_exptl_absorpt_process_details   'SADABS; Sheldrick, 1996'

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      200(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'Bruker Smart Apex CCD'
_diffrn_measurement_method       ω-2θ
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            14132
_diffrn_reflns_av_unetI/netI     0.0447
_diffrn_reflns_av_R_equivalents  0.0316
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_k_max       34
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         2.275
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.931
_diffrn_measured_fraction_theta_full 0.906
_diffrn_reflns_Laue_measured_fraction_max 0.931
_diffrn_reflns_Laue_measured_fraction_full 0.906
_diffrn_reflns_point_group_measured_fraction_max 0.931
_diffrn_reflns_point_group_measured_fraction_full 0.906
_reflns_number_total             6159
_reflns_number_gt                5408
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
During the refinement, the command 'omit -3 50' was used to omit the weak reflections above 50 degree.
In the structure, there are two disordered W sites (W5, W6). W(5) site is occupied by W and Ti atom with
 occupancy factors of 0.75 and 0.25. W(6) site is occupied  by W and Ti atom with occupancy factors of
 0.25 and 0.75. Some O atoms on the polyoxoanions and water molecules are retrained with the 
command 'isor', which leds to a  restraint value of 66. Rint after the absorption correction process is 0.0316,
 which indicates that the absorption correction process is effective. In the final refinement, 5.5 crystal water
 molecules are determined  from the residual peaks with reasonable positions and thermal parameters.
 The highest two residual peaks are close to Ce(2) with the distance of 1.28 A and 0.98 A,
 indicative an featureless peak. These largest residual peaks are mainly due to the series 
termination errors. 
;

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXS-2014 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
;
 ?
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0768P)²+414.7732P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         6159
_refine_ls_number_parameters     518
_refine_ls_number_restraints     66
_refine_ls_R_factor_all          0.0522
_refine_ls_R_factor_gt           0.0458
_refine_ls_wR_factor_ref         0.1332
_refine_ls_wR_factor_gt          0.1281
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_restrained_S_all      1.026
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
W1 W 0.08407(3) 0.26139(2) 0.94599(5) 0.01150(15) Uani 1 1 d . . . . .
W2 W 0.14089(3) 0.26063(2) 1.21812(5) 0.01221(16) Uani 1 1 d . . . . .
W3 W 0.21484(3) 0.17884(2) 1.15346(5) 0.01113(16) Uani 1 1 d . . . . .
W4 W -0.05546(3) 0.17299(2) 0.71872(5) 0.01066(15) Uani 1 1 d . . . . .
W5 W 0.07399(4) 0.09243(2) 0.92882(6) 0.00861(17) Uani 0.75 1 d . . P A 1
Ti1 Ti 0.07399(4) 0.09243(2) 0.92882(6) 0.00861(17) Uani 0.25 1 d . . P A 2
W6 W -0.12817(8) 0.09353(4) 0.78467(11) 0.0107(3) Uani 0.25 1 d . U P A 3
Ti2 Ti -0.12817(8) 0.09353(4) 0.78467(11) 0.0107(3) Uani 0.75 1 d . U P A 4
Ce1 Ce -0.31341(7) 0.0000 0.61584(10) 0.0156(3) Uani 1 2 d S T P A .
Ce2 Ce 0.21813(8) 0.0000 0.92157(12) 0.0254(3) Uani 1 2 d S T P A .
P1 P 0.0000 0.17621(16) 1.0000 0.0075(10) Uani 1 2 d S T P A .
K1 K -0.1001(4) 0.0000 0.6557(6) 0.0421(14) Uani 1 2 d S T P . .
O1 O -0.0196(5) 0.1472(3) 0.9017(7) 0.0100(18) Uani 1 1 d . U . . .
O2 O 0.0757(5) 0.2064(3) 1.0537(8) 0.015(2) Uani 1 1 d . . . . .
O3 O -0.0268(5) 0.2756(3) 0.8724(7) 0.0111(19) Uani 1 1 d . U . . .
O4 O -0.2025(6) 0.0551(3) 0.6872(8) 0.016(2) Uani 1 1 d . . . . .
O5 O 0.0309(5) 0.2160(3) 0.8274(7) 0.0104(19) Uani 1 1 d . . . . .
O6 O 0.1974(6) 0.2990(3) 1.3282(9) 0.021(2) Uani 1 1 d . . . . .
O7 O -0.1271(5) 0.2168(3) 0.7101(8) 0.015(2) Uani 1 1 d . . . . .
O8 O -0.0313(6) 0.0662(3) 0.8297(8) 0.015(2) Uani 1 1 d . U . . .
O9 O 0.1054(6) 0.3002(3) 0.8888(9) 0.021(2) Uani 1 1 d . . . . .
O10 O 0.2279(6) 0.2273(3) 1.2502(8) 0.016(2) Uani 1 1 d . . . . .
O11 O 0.1297(6) 0.0548(4) 0.9234(9) 0.020(2) Uani 1 1 d . . . . .
O12 O 0.0264(5) 0.1297(3) 0.7853(8) 0.013(2) Uani 1 1 d . . . . .
O13 O 0.1009(6) 0.0779(3) 1.0697(9) 0.017(2) Uani 1 1 d . . . . .
O14 O 0.1568(6) 0.1409(3) 1.0210(8) 0.017(2) Uani 1 1 d . . . . .
O15 O -0.1366(5) 0.1308(3) 0.6679(8) 0.015(2) Uani 1 1 d . . . . .
O16 O 0.3177(5) 0.1718(3) 1.2267(8) 0.015(2) Uani 1 1 d . . . . .
O17 O 0.1274(6) 0.2887(3) 1.0915(8) 0.015(2) Uani 1 1 d . . . . .
O18 O 0.2006(5) 0.1388(3) 1.2305(8) 0.017(2) Uani 1 1 d . . . . .
O19 O 0.1853(6) 0.2271(3) 1.0414(8) 0.014(2) Uani 1 1 d . . . . .
O20 O -0.0796(6) 0.1844(3) 0.5891(8) 0.017(2) Uani 1 1 d . . . . .
O21 O -0.4091(6) 0.0537(4) 0.4518(10) 0.028(3) Uani 1 1 d . . . . .
O22 O -0.5328(8) 0.0815(4) 0.3632(16) 0.064(5) Uani 1 1 d . . . . .
O23 O 0.2135(7) -0.0614(4) 0.8212(11) 0.036(3) Uani 1 1 d . . . . .
O24 O 0.1659(9) -0.0794(5) 0.6420(13) 0.050(4) Uani 1 1 d . . . . .
C1 C -0.4576(9) 0.0849(5) 0.4151(14) 0.021(3) Uani 1 1 d . . . . .
C2 C -0.4246(9) 0.1290(6) 0.4316(14) 0.024(3) Uani 1 1 d . U . . .
C3 C -0.3384(9) 0.1361(6) 0.5017(14) 0.026(4) Uani 1 1 d . . . . .
H3A H -0.3022 0.1120 0.5348 0.031 Uiso 1 1 calc R U . . .
C4 C -0.3544(9) 0.2130(5) 0.4776(12) 0.020(3) Uani 1 1 d . . . . .
H4A H -0.3306 0.2408 0.4924 0.024 Uiso 1 1 calc R U . . .
C5 C -0.4397(9) 0.2089(6) 0.4092(14) 0.027(4) Uani 1 1 d . . . . .
H5A H -0.4737 0.2339 0.3779 0.032 Uiso 1 1 calc R U . . .
C6 C -0.4746(10) 0.1670(5) 0.3874(15) 0.027(4) Uani 1 1 d . U . . .
H6A H -0.5317 0.1643 0.3429 0.032 Uiso 1 1 calc R U . . .
C7 C 0.1856(11) -0.0894(6) 0.7359(16) 0.036(4) Uani 1 1 d . . . . .
C8 C 0.1777(10) -0.1367(5) 0.7557(14) 0.025(3) Uani 1 1 d . . . . .
C9 C 0.1975(9) -0.1491(5) 0.8597(13) 0.020(3) Uani 1 1 d . . . . .
H9A H 0.2197 -0.1288 0.9211 0.024 Uiso 1 1 calc R U . . .
C10 C 0.1529(9) -0.2219(6) 0.7843(14) 0.024(3) Uani 1 1 d . . . . .
H10A H 0.1442 -0.2506 0.7956 0.029 Uiso 1 1 calc R U . . .
C11 C 0.1345(10) -0.2113(6) 0.6826(15) 0.033(4) Uani 1 1 d . . . . .
H11A H 0.1138 -0.2323 0.6234 0.039 Uiso 1 1 calc R U . . .
C12 C 0.1476(11) -0.1682(6) 0.6696(16) 0.034(4) Uani 1 1 d . . . . .
H12A H 0.1357 -0.1602 0.6004 0.041 Uiso 1 1 calc R U . . .
N1 N -0.3072(8) 0.1771(4) 0.5218(12) 0.026(3) Uani 1 1 d . . . . .
H1A H -0.2541 0.1800 0.5653 0.031 Uiso 1 1 calc R U . . .
N2 N 0.1837(7) -0.1911(4) 0.8696(11) 0.021(3) Uani 1 1 d . . . . .
H2A H 0.1951 -0.1988 0.9337 0.025 Uiso 1 1 calc R U . . .
O2W O -0.3190(7) -0.0726(4) 0.7065(11) 0.030(3) Uani 1 1 d . . . . .
H2WA H -0.3525 -0.0962 0.6562 0.036 Uiso 1 1 d R U . A .
H2WB H -0.2876 -0.0745 0.7886 0.036 Uiso 1 1 d R U . . .
O3W O -0.4181(9) 0.0000 0.6335(16) 0.029(4) Uani 1 2 d S T P . .
H3WA H -0.4658 -0.0176 0.5825 0.034 Uiso 0.5 1 d R U P A .
H3WB H -0.4095 0.0176 0.6911 0.034 Uiso 0.5 1 d R U P . .
O1W O -0.2821(8) 0.0000 0.4854(11) 0.014(3) Uani 1 2 d S TU P . .
O4W O -0.2058(9) 0.0000 0.8469(13) 0.023(3) Uani 1 2 d S T P . .
H4WA H -0.1958 -0.0258 0.8883 0.028 Uiso 0.5 1 d R U P A .
H4WB H -0.1768 0.0258 0.8893 0.028 Uiso 0.5 1 d R U P . .
O6W O 0.3546(10) 0.0000 0.9818(16) 0.041(5) Uani 1 2 d S T P . .
H6WA H 0.3571 0.0000 0.9234 0.050 Uiso 1 2 d R U P A .
H6WB H 0.4039 0.0000 1.0630 0.050 Uiso 1 2 d R U P . .
O7W O 0.3101(8) 0.0520(5) 1.0924(12) 0.051(4) Uani 1 1 d . . . . .
H7WA H 0.2917 0.0806 1.0861 0.061 Uiso 1 1 d R U . A .
H7WB H 0.3631 0.0430 1.1630 0.061 Uiso 1 1 d R U . . .
OW1 O -0.1913(16) 0.0000 0.399(2) 0.073(7) Uani 1 2 d S TU P . .
OW2 O 0.2540(13) 0.4181(5) 0.4425(18) 0.077(6) Uani 1 1 d . . . . .
OW3 O 0.4161(13) 0.1060(6) 0.111(2) 0.098(7) Uani 1 1 d . . . . .
OW4 O 0.0198(13) 0.0714(7) 0.3951(17) 0.091(6) Uani 1 1 d . U . . .
OW5 O 0.0202(15) 0.5000 0.212(2) 0.075(7) Uani 1 2 d S T P . .
OW6 O 0.5840(19) 0.0853(10) 0.229(3) 0.155(11) Uiso 1 1 d . . . . .
OW7 O 0.619(2) 0.1133(12) 0.106(3) 0.071(9) Uiso 0.5 1 d . . P . .
O5W O 0.0932(16) 0.0000 0.740(3) 0.073(7) Uani 1 2 d S TU P . .
H5WA H 0.0785 0.0218 0.6855 0.087 Uiso 0.5 1 d R U P A .
H5WB H 0.0546 -0.0218 0.7173 0.087 Uiso 0.5 1 d R U P . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
W1 O9 1.710(9) . ?
W1 O3 1.895(8) . ?
W1 O5 1.904(9) . ?
W1 O17 1.905(9) . ?
W1 O19 1.919(9) . ?
W1 O2 2.433(9) . ?
W2 O6 1.688(10) . ?
W2 O7 1.872(10) 2_557 ?
W2 O10 1.898(9) . ?
W2 O3 1.901(8) 2_557 ?
W2 O17 1.940(9) . ?
W2 O2 2.473(10) . ?
W3 O16 1.706(9) . ?
W3 O18 1.857(9) . ?
W3 O14 1.868(9) . ?
W3 O10 1.959(9) . ?
W3 O19 1.988(9) . ?
W3 O2 2.433(9) . ?
W4 O20 1.697(9) . ?
W4 O12 1.860(9) . ?
W4 O15 1.869(9) . ?
W4 O5 1.928(9) . ?
W4 O7 1.987(9) . ?
W4 O1 2.454(8) . ?
W5 O11 1.711(10) . ?
W5 O13 1.851(10) . ?
W5 O8 1.855(9) . ?
W5 O14 1.978(10) . ?
W5 O12 2.006(9) . ?
W5 O1 2.438(8) . ?
W6 O4 1.698(10) . ?
W6 O8 1.910(9) . ?
W6 O13 1.924(10) 2_557 ?
W6 O18 1.985(9) 2_557 ?
W6 O15 2.009(9) . ?
W6 O1 2.375(9) . ?
Ce1 O21 2.468(11) . ?
Ce1 O21 2.468(11) 6 ?
Ce1 O3W 2.484(13) . ?
Ce1 O4 2.496(9) 6 ?
Ce1 O4 2.496(9) . ?
Ce1 O1W 2.511(12) . ?
Ce1 O4W 2.566(15) . ?
Ce1 O2W 2.643(11) 6 ?
Ce1 O2W 2.643(11) . ?
Ce2 O5W 2.18(3) . ?
Ce2 O23 2.367(11) 6 ?
Ce2 O23 2.367(11) . ?
Ce2 O6W 2.448(15) . ?
Ce2 O7W 2.475(14) 6 ?
Ce2 O7W 2.475(14) . ?
Ce2 O11 2.563(10) 6 ?
Ce2 O11 2.563(10) . ?
P1 O1 1.525(9) 2_557 ?
P1 O1 1.525(9) . ?
P1 O2 1.545(9) 2_557 ?
P1 O2 1.545(9) . ?
O3 W2 1.901(8) 2_557 ?
O7 W2 1.872(9) 2_557 ?
O13 Ti2 1.924(10) 2_557 ?
O13 W6 1.924(10) 2_557 ?
O18 Ti2 1.985(9) 2_557 ?
O18 W6 1.985(9) 2_557 ?
O21 C1 1.232(18) . ?
O22 C1 1.248(18) . ?
O23 C7 1.30(2) . ?
O24 C7 1.22(2) . ?
C1 C2 1.46(2) . ?
C2 C6 1.40(2) . ?
C2 C3 1.41(2) . ?
C3 N1 1.34(2) . ?
C3 H3A 0.9300 . ?
C4 N1 1.32(2) . ?
C4 C5 1.38(2) . ?
C4 H4A 0.9300 . ?
C5 C6 1.40(2) . ?
C5 H5A 0.9300 . ?
C6 H6A 0.9300 . ?
C7 C8 1.50(2) . ?
C8 C12 1.37(2) . ?
C8 C9 1.38(2) . ?
C9 N2 1.34(2) . ?
C9 H9A 0.9300 . ?
C10 N2 1.35(2) . ?
C10 C11 1.35(2) . ?
C10 H10A 0.9300 . ?
C11 C12 1.38(3) . ?
C11 H11A 0.9300 . ?
C12 H12A 0.9300 . ?
N1 H1A 0.8600 . ?
N2 H2A 0.8600 . ?
O2W H2WA 0.9300 . ?
O2W H2WB 0.9300 . ?
O3W H3WA 0.9300 . ?
O3W H3WB 0.9300 . ?
O4W H4WA 0.9300 . ?
O4W H4WB 0.9300 . ?
O6W H6WA 0.9300 . ?
O6W H6WB 0.9300 . ?
O7W H7WA 0.9300 . ?
O7W H7WB 0.9300 . ?
O5W H5WA 0.9300 . ?
O5W H5WB 0.9300 . ?

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
_geom_angle_publ_flag
O9 W1 O3 103.2(4) . . ?
O9 W1 O5 102.2(4) . . ?
O3 W1 O5 84.4(4) . . ?
O9 W1 O17 101.9(4) . . ?
O3 W1 O17 90.1(4) . . ?
O5 W1 O17 155.9(4) . . ?
O9 W1 O19 100.4(4) . . ?
O3 W1 O19 156.2(4) . . ?
O5 W1 O19 88.0(4) . . ?
O17 W1 O19 87.6(4) . . ?
O9 W1 O2 171.6(4) . . ?
O3 W1 O2 84.1(3) . . ?
O5 W1 O2 82.5(3) . . ?
O17 W1 O2 73.5(4) . . ?
O19 W1 O2 72.5(3) . . ?
O6 W2 O7 102.0(4) . 2_557 ?
O6 W2 O10 100.9(4) . . ?
O7 W2 O10 90.5(4) 2_557 . ?
O6 W2 O3 105.0(4) . 2_557 ?
O7 W2 O3 86.3(4) 2_557 2_557 ?
O10 W2 O3 154.1(4) . 2_557 ?
O6 W2 O17 101.4(4) . . ?
O7 W2 O17 156.7(4) 2_557 . ?
O10 W2 O17 86.0(4) . . ?
O3 W2 O17 86.9(4) 2_557 . ?
O6 W2 O2 170.1(4) . . ?
O7 W2 O2 84.9(4) 2_557 . ?
O10 W2 O2 71.8(3) . . ?
O3 W2 O2 82.3(3) 2_557 . ?
O17 W2 O2 72.1(4) . . ?
O16 W3 O18 102.9(4) . . ?
O16 W3 O14 104.1(4) . . ?
O18 W3 O14 90.0(4) . . ?
O16 W3 O10 98.9(4) . . ?
O18 W3 O10 90.6(4) . . ?
O14 W3 O10 156.2(4) . . ?
O16 W3 O19 99.1(4) . . ?
O18 W3 O19 157.9(4) . . ?
O14 W3 O19 86.6(4) . . ?
O10 W3 O19 83.9(4) . . ?
O16 W3 O2 167.1(4) . . ?
O18 W3 O2 86.4(4) . . ?
O14 W3 O2 84.4(4) . . ?
O10 W3 O2 71.8(3) . . ?
O19 W3 O2 71.5(3) . . ?
O20 W4 O12 101.1(4) . . ?
O20 W4 O15 102.0(4) . . ?
O12 W4 O15 91.8(4) . . ?
O20 W4 O5 101.7(4) . . ?
O12 W4 O5 89.9(4) . . ?
O15 W4 O5 155.4(4) . . ?
O20 W4 O7 100.8(4) . . ?
O12 W4 O7 157.8(4) . . ?
O15 W4 O7 86.9(4) . . ?
O5 W4 O7 82.5(4) . . ?
O20 W4 O1 173.1(4) . . ?
O12 W4 O1 73.7(3) . . ?
O15 W4 O1 74.1(3) . . ?
O5 W4 O1 82.9(3) . . ?
O7 W4 O1 84.7(3) . . ?
O11 W5 O13 103.3(4) . . ?
O11 W5 O8 101.8(4) . . ?
O13 W5 O8 94.2(4) . . ?
O11 W5 O14 101.1(4) . . ?
O13 W5 O14 86.7(4) . . ?
O8 W5 O14 156.2(4) . . ?
O11 W5 O12 100.0(4) . . ?
O13 W5 O12 156.2(4) . . ?
O8 W5 O12 85.8(4) . . ?
O14 W5 O12 84.0(4) . . ?
O11 W5 O1 170.8(4) . . ?
O13 W5 O1 85.3(3) . . ?
O8 W5 O1 73.9(4) . . ?
O14 W5 O1 82.5(3) . . ?
O12 W5 O1 71.8(3) . . ?
O4 W6 O8 100.3(4) . . ?
O4 W6 O13 101.3(4) . 2_557 ?
O8 W6 O13 95.2(4) . 2_557 ?
O4 W6 O18 99.4(4) . 2_557 ?
O8 W6 O18 160.1(4) . 2_557 ?
O13 W6 O18 83.9(4) 2_557 2_557 ?
O4 W6 O15 99.0(4) . . ?
O8 W6 O15 88.0(4) . . ?
O13 W6 O15 158.5(4) 2_557 . ?
O18 W6 O15 85.9(4) 2_557 . ?
O4 W6 O1 171.0(4) . . ?
O8 W6 O1 74.6(4) . . ?
O13 W6 O1 86.7(4) 2_557 . ?
O18 W6 O1 85.5(3) 2_557 . ?
O15 W6 O1 73.7(3) . . ?
O21 Ce1 O21 82.3(5) . 6 ?
O21 Ce1 O3W 84.7(4) . . ?
O21 Ce1 O3W 84.7(4) 6 . ?
O21 Ce1 O4 140.9(3) . 6 ?
O21 Ce1 O4 84.1(3) 6 6 ?
O3W Ce1 O4 130.2(3) . 6 ?
O21 Ce1 O4 84.1(3) . . ?
O21 Ce1 O4 140.9(3) 6 . ?
O3W Ce1 O4 130.2(3) . . ?
O4 Ce1 O4 83.8(4) 6 . ?
O21 Ce1 O1W 72.5(3) . . ?
O21 Ce1 O1W 72.5(3) 6 . ?
O3W Ce1 O1W 149.3(5) . . ?
O4 Ce1 O1W 68.5(3) 6 . ?
O4 Ce1 O1W 68.5(3) . . ?
O21 Ce1 O4W 137.2(3) . . ?
O21 Ce1 O4W 137.2(3) 6 . ?
O3W Ce1 O4W 84.0(5) . . ?
O4 Ce1 O4W 72.6(3) 6 . ?
O4 Ce1 O4W 72.6(3) . . ?
O1W Ce1 O4W 126.7(4) . . ?
O21 Ce1 O2W 70.9(4) . 6 ?
O21 Ce1 O2W 140.0(3) 6 6 ?
O3W Ce1 O2W 64.2(3) . 6 ?
O4 Ce1 O2W 135.0(3) 6 6 ?
O4 Ce1 O2W 66.3(3) . 6 ?
O1W Ce1 O2W 123.5(2) . 6 ?
O4W Ce1 O2W 67.0(3) . 6 ?
O21 Ce1 O2W 140.0(3) . . ?
O21 Ce1 O2W 70.9(4) 6 . ?
O3W Ce1 O2W 64.2(3) . . ?
O4 Ce1 O2W 66.3(3) 6 . ?
O4 Ce1 O2W 135.0(3) . . ?
O1W Ce1 O2W 123.5(2) . . ?
O4W Ce1 O2W 67.0(3) . . ?
O2W Ce1 O2W 112.3(5) 6 . ?
O5W Ce2 O23 73.6(4) . 6 ?
O5W Ce2 O23 73.6(4) . . ?
O23 Ce2 O23 103.5(6) 6 . ?
O5W Ce2 O6W 128.3(6) . . ?
O23 Ce2 O6W 75.0(4) 6 . ?
O23 Ce2 O6W 75.0(4) . . ?
O5W Ce2 O7W 138.0(4) . 6 ?
O23 Ce2 O7W 145.5(4) 6 6 ?
O23 Ce2 O7W 80.0(5) . 6 ?
O6W Ce2 O7W 72.8(4) . 6 ?
O5W Ce2 O7W 138.0(4) . . ?
O23 Ce2 O7W 80.0(5) 6 . ?
O23 Ce2 O7W 145.5(4) . . ?
O6W Ce2 O7W 72.8(4) . . ?
O7W Ce2 O7W 79.0(7) 6 . ?
O5W Ce2 O11 73.5(4) . 6 ?
O23 Ce2 O11 144.9(4) 6 6 ?
O23 Ce2 O11 78.6(3) . 6 ?
O6W Ce2 O11 137.0(3) . 6 ?
O7W Ce2 O11 69.6(4) 6 6 ?
O7W Ce2 O11 118.3(4) . 6 ?
O5W Ce2 O11 73.5(4) . . ?
O23 Ce2 O11 78.6(3) 6 . ?
O23 Ce2 O11 144.9(4) . . ?
O6W Ce2 O11 137.0(3) . . ?
O7W Ce2 O11 118.3(4) 6 . ?
O7W Ce2 O11 69.6(4) . . ?
O11 Ce2 O11 80.6(4) 6 . ?
O1 P1 O1 109.6(7) 2_557 . ?
O1 P1 O2 109.7(4) 2_557 2_557 ?
O1 P1 O2 110.1(5) . 2_557 ?
O1 P1 O2 110.1(5) 2_557 . ?
O1 P1 O2 109.7(5) . . ?
O2 P1 O2 107.6(8) 2_557 . ?
P1 O1 W6 126.4(4) . . ?
P1 O1 W5 126.0(5) . . ?
P1 O1 W4 126.2(5) . . ?
W6 O1 W4 89.3(3) . . ?
W5 O1 W4 89.1(3) . . ?
P1 O2 W3 123.8(5) . . ?
P1 O2 W1 126.6(5) . . ?
W3 O2 W1 90.9(3) . . ?
P1 O2 W2 126.3(5) . . ?
W3 O2 W2 89.4(3) . . ?
W1 O2 W2 88.5(3) . . ?
W1 O3 W2 152.2(6) . 2_557 ?
W6 O4 Ce1 154.0(5) . . ?
W1 O5 W4 154.6(5) . . ?
W2 O7 W4 150.5(5) 2_557 . ?
W2 O10 W3 127.0(5) . . ?
W5 O11 Ce2 177.9(6) . . ?
W4 O12 W5 125.1(4) . . ?
W3 O14 W5 146.7(5) . . ?
W4 O15 W6 122.2(5) . . ?
W1 O17 W2 125.8(5) . . ?
W3 O18 Ti2 147.6(5) . 2_557 ?
W3 O18 W6 147.6(5) . 2_557 ?
W1 O19 W3 125.0(4) . . ?
C1 O21 Ce1 146.3(10) . . ?
C7 O23 Ce2 160.2(12) . . ?
O21 C1 O22 125.1(15) . . ?
O21 C1 C2 117.0(13) . . ?
O22 C1 C2 117.9(13) . . ?
C6 C2 C3 115.9(15) . . ?
C6 C2 C1 122.7(13) . . ?
C3 C2 C1 121.2(14) . . ?
N1 C3 C2 121.3(14) . . ?
N1 C3 H3A 119.3 . . ?
C2 C3 H3A 119.3 . . ?
N1 C4 C5 119.1(14) . . ?
N1 C4 H4A 120.4 . . ?
C5 C4 H4A 120.4 . . ?
C4 C5 C6 119.7(15) . . ?
C4 C5 H5A 120.2 . . ?
C6 C5 H5A 120.2 . . ?
C5 C6 C2 120.8(14) . . ?
C5 C6 H6A 119.6 . . ?
C2 C6 H6A 119.6 . . ?
O24 C7 O23 123.9(18) . . ?
O24 C7 C8 118.6(16) . . ?
O23 C7 C8 117.4(14) . . ?
C12 C8 C9 118.7(16) . . ?
C12 C8 C7 121.1(15) . . ?
C9 C8 C7 120.2(14) . . ?
N2 C9 C8 118.1(14) . . ?
N2 C9 H9A 121.0 . . ?
C8 C9 H9A 121.0 . . ?
N2 C10 C11 120.4(16) . . ?
N2 C10 H10A 119.8 . . ?
C11 C10 H10A 119.8 . . ?
C10 C11 C12 117.6(16) . . ?
C10 C11 H11A 121.2 . . ?
C12 C11 H11A 121.2 . . ?
C8 C12 C11 122.0(16) . . ?
C8 C12 H12A 119.0 . . ?
C11 C12 H12A 119.0 . . ?
C4 N1 C3 123.1(13) . . ?
C4 N1 H1A 118.5 . . ?
C3 N1 H1A 118.5 . . ?
C9 N2 C10 123.3(13) . . ?
C9 N2 H2A 118.3 . . ?
C10 N2 H2A 118.3 . . ?
Ce1 O2W H2WA 120.0 . . ?
Ce1 O2W H2WB 120.0 . . ?
H2WA O2W H2WB 120.0 . . ?
Ce1 O3W H3WA 120.0 . . ?
Ce1 O3W H3WB 120.0 . . ?
H3WA O3W H3WB 120.0 . . ?
Ce1 O4W H4WA 120.0 . . ?
Ce1 O4W H4WB 120.0 . . ?
H4WA O4W H4WB 120.0 . . ?
Ce2 O6W H6WA 120.0 . . ?
Ce2 O6W H6WB 120.0 . . ?
H6WA O6W H6WB 120.0 . . ?
Ce2 O7W H7WA 120.0 . . ?
Ce2 O7W H7WB 120.0 . . ?
H7WA O7W H7WB 120.0 . . ?
Ce2 O5W H5WA 120.0 . . ?
Ce2 O5W H5WB 120.0 . . ?
H5WA O5W H5WB 120.0 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O1 P1 O1 W6_c 58.8(5) 2_557 . . . ?
O2 P1 O1 W6 -62.0(7) 2_557 . . . ?
O2 P1 O1 W6 179.8(5) . . . . ?
O1 P1 O1 W5 -59.0(4) 2_557 . . . ?
O2 P1 O1 W5 -179.8(5) 2_557 . . . ?
O2 P1 O1 W5 62.0(7) . . . . ?
O1 P1 O1 W4 -179.6(7) 2_557 . . . ?
O2 P1 O1 W4 59.6(7) 2_557 . . . ?
O2 P1 O1 W4 -58.6(7) . . . . ?
O1 P1 O2 W3 60.0(7) 2_557 . . . ?
O1 P1 O2 W3 -60.7(7) . . . . ?
O2 P1 O2 W3 179.5(7) 2_557 . . . ?
O1 P1 O2 W1 -178.7(5) 2_557 . . . ?
O1 P1 O2 W1 60.6(7) . . . . ?
O2 P1 O2 W1 -59.2(5) 2_557 . . . ?
O1 P1 O2 W2 -58.4(8) 2_557 . . . ?
O1 P1 O2 W2 -179.1(5) . . . . ?
O2 P1 O2 W2 61.1(5) 2_557 . . . ?
O9 W1 O3 W2 127.2(10) . . . 2_557 ?
O5 W1 O3 W2 25.9(10) . . . 2_557 ?
O17 W1 O3 W2 -130.6(10) . . . 2_557 ?
O19 W1 O3 W2 -46.1(16) . . . 2_557 ?
O2 W1 O3 W2 -57.1(10) . . . 2_557 ?
O8 W6 O4 Ce1 119.8(11) . . . . ?
O13 W6 O4 Ce1 22.3(12) 2_557 . . . ?
O18 W6 O4 Ce1 -63.3(12) 2_557 . . . ?
O15 W6 O4 Ce1 -150.6(11) . . . . ?
O11 W5 O8 W6 -174.6(6) . . . . ?
O13 W5 O8 W6 80.9(6) . . . . ?
O14 W5 O8 W6 -10.5(12) . . . . ?
O12 W5 O8 W6 -75.3(6) . . . . ?
O1 W5 O8 W6 -3.0(5) . . . . ?
O6 W2 O10 W3 -174.4(6) . . . . ?
O7 W2 O10 W3 83.3(6) 2_557 . . . ?
O3 W2 O10 W3 0.7(13) 2_557 . . . ?
O17 W2 O10 W3 -73.6(6) . . . . ?
O2 W2 O10 W3 -1.2(5) . . . . ?
O20 W4 O12 W5 -170.0(6) . . . . ?
O15 W4 O12 W5 -67.3(6) . . . . ?
O5 W4 O12 W5 88.2(6) . . . . ?
O7 W4 O12 W5 18.7(14) . . . . ?
O1 W4 O12 W5 5.5(5) . . . . ?
O11 W5 O13 Ti2 140.3(11) . . . 2_557 ?
O8 W5 O13 Ti2 -116.6(11) . . . 2_557 ?
O14 W5 O13 Ti2 39.6(11) . . . 2_557 ?
O12 W5 O13 Ti2 -27.6(17) . . . 2_557 ?
O1 W5 O13 Ti2 -43.1(11) . . . 2_557 ?
O11 W5 O13 W6 140.3(11) . . . 2_557 ?
O8 W5 O13 W6 -116.6(11) . . . 2_557 ?
O14 W5 O13 W6 39.6(11) . . . 2_557 ?
O12 W5 O13 W6 -27.6(17) . . . 2_557 ?
O1 W5 O13 W6 -43.1(11) . . . 2_557 ?
O16 W3 O14 W5 127.1(10) . . . . ?
O18 W3 O14 W5 23.8(10) . . . . ?
O10 W3 O14 W5 -67.8(15) . . . . ?
O19 W3 O14 W5 -134.3(10) . . . . ?
O2 W3 O14 W5 -62.6(10) . . . . ?
O20 W4 O15 W6 166.3(5) . . . . ?
O12 W4 O15 W6 64.5(5) . . . . ?
O5 W4 O15 W6 -29.0(12) . . . . ?
O7 W4 O15 W6 -93.3(5) . . . . ?
O1 W4 O15 W6 -7.9(4) . . . . ?
O16 W3 O18 Ti2 -138.3(10) . . . 2_557 ?
O14 W3 O18 Ti2 -33.8(10) . . . 2_557 ?
O10 W3 O18 Ti2 122.4(10) . . . 2_557 ?
O19 W3 O18 Ti2 47.3(17) . . . 2_557 ?
O2 W3 O18 Ti2 50.6(10) . . . 2_557 ?
O16 W3 O18 W6 -138.3(10) . . . 2_557 ?
O14 W3 O18 W6 -33.8(10) . . . 2_557 ?
O10 W3 O18 W6 122.4(10) . . . 2_557 ?
O19 W3 O18 W6 47.3(17) . . . 2_557 ?
O2 W3 O18 W6 50.6(10) . . . 2_557 ?
Ce1 O21 C1 O22 -83(3) . . . . ?
Ce1 O21 C1 C2 98.8(19) . . . . ?
O21 C1 C2 C6 175.9(15) . . . . ?
O22 C1 C2 C6 -3(2) . . . . ?
O21 C1 C2 C3 -9(2) . . . . ?
O22 C1 C2 C3 172.3(17) . . . . ?
C6 C2 C3 N1 -1(2) . . . . ?
C1 C2 C3 N1 -176.8(14) . . . . ?
N1 C4 C5 C6 0(2) . . . . ?
C4 C5 C6 C2 -1(2) . . . . ?
C3 C2 C6 C5 2(2) . . . . ?
C1 C2 C6 C5 177.5(15) . . . . ?
Ce2 O23 C7 O24 61(4) . . . . ?
Ce2 O23 C7 C8 -119(3) . . . . ?
O24 C7 C8 C12 -1(2) . . . . ?
O23 C7 C8 C12 179.1(15) . . . . ?
O24 C7 C8 C9 -178.5(15) . . . . ?
O23 C7 C8 C9 2(2) . . . . ?
C12 C8 C9 N2 -2(2) . . . . ?
C7 C8 C9 N2 175.2(13) . . . . ?
N2 C10 C11 C12 -1(2) . . . . ?
C9 C8 C12 C11 2(2) . . . . ?
C7 C8 C12 C11 -175.5(15) . . . . ?
C10 C11 C12 C8 0(2) . . . . ?
C5 C4 N1 C3 1(2) . . . . ?
C2 C3 N1 C4 0(2) . . . . ?
C8 C9 N2 C10 1(2) . . . . ?
C11 C10 N2 C9 0(2) . . . . ?

_refine_diff_density_max         6.211
_refine_diff_density_min         -4.338
_refine_diff_density_rms         0.395

_shelxl_version_number           2014-3

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_2
_database_code_depnum_ccdc_archive 'CCDC 1818605'
_audit_update_record             
;
2018-06-07 deposited with the CCDC.
2018-06-08 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C24 H62 K N4 Nd2 O69 P Ti2 W10'
_chemical_formula_weight         3803.53

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'
Nd Nd -0.1943 3.0179 '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'
Ti Ti 0.2776 0.4457 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
K K 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           12
_space_group_name_H-M_alt        'C 2/m'
_space_group_name_Hall           '-C 2y'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z'
'-x, -y, -z'
'x, -y, z'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z'

_cell_length_a                   21.916(13)
_cell_length_b                   30.097(19)
_cell_length_c                   15.243(9)
_cell_angle_alpha                90
_cell_angle_beta                 133.528(7)
_cell_angle_gamma                90
_cell_volume                     7290(8)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    18523
_cell_measurement_theta_min      1.449
_cell_measurement_theta_max      25.00

_exptl_crystal_description       'block '
_exptl_crystal_colour            'light purple'
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    3.466
_exptl_crystal_F_000             6894
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.14
_exptl_absorpt_coefficient_mu    17.516
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.021
_exptl_absorpt_correction_T_max  0.086
_exptl_absorpt_process_details   'SADABS; Sheldrick, 1996'

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'Bruker Smart Apex CCD'
_diffrn_measurement_method       ω-2θ
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            18523
_diffrn_reflns_av_unetI/netI     0.1214
_diffrn_reflns_av_R_equivalents  0.1022
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_k_max       35
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         1.449
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measured_fraction_theta_full 0.963
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_Laue_measured_fraction_full 0.963
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_point_group_measured_fraction_full 0.963
_reflns_number_total             6503
_reflns_number_gt                4931
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
During the refinement, the command 'omit -3 50' was used to omit the weak reflections above 50 degree.
In the structure, there are two disordered W sites (W5, W6). W(5) site is occupied by W and Ti atom with
 occupancy factors of 0.78 and 0.22. W(6) site is occupied  by W and Ti atom with occupancy factors of
 0.22 and 0.78. Some O atoms on the polyoxoanions, C and N atoms on the organic ligands, and coordinated water molecules
 are retrained with the command 'isor', which leds to a  restraint value of 150. Rint after the absorption correction 
process is 0.1022, which indicates that the absorption correction process is effective.In the final refinement,
6 crystal water  molecules are determined  from the residual peaks with reasonable positions and thermal parameters.
 The highest residual peak is close to W(3) with the distance of  0.94 A, indicative an featureless peak.
The deepest hole is also close to the heavy metal center W(4). 
;

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXS-2014 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
;
 ?
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0361P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         6503
_refine_ls_number_parameters     533
_refine_ls_number_restraints     150
_refine_ls_R_factor_all          0.0729
_refine_ls_R_factor_gt           0.0540
_refine_ls_wR_factor_ref         0.1419
_refine_ls_wR_factor_gt          0.1297
_refine_ls_goodness_of_fit_ref   1.002
_refine_ls_restrained_S_all      0.996
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
W1 W 0.35876(4) 0.24005(2) -0.21809(6) 0.01124(18) Uani 1 1 d . . . . .
W2 W 0.28603(4) 0.32205(2) -0.15177(6) 0.00969(17) Uani 1 1 d . . . . .
W3 W 0.41678(4) 0.23915(2) 0.05445(6) 0.01054(18) Uani 1 1 d . . . . .
W4 W 0.55588(4) 0.32795(2) 0.28121(6) 0.00960(17) Uani 1 1 d . . . . .
W5 W 0.42674(5) 0.40899(2) 0.07180(7) 0.00857(19) Uani 0.78 1 d . . P A 1
Ti1 Ti 0.42674(5) 0.40899(2) 0.07180(7) 0.00857(19) Uani 0.22 1 d . . P A 2
W6 W 0.62789(9) 0.40769(4) 0.21493(14) 0.0064(3) Uani 0.22 1 d . . P A 3
Ti2 Ti 0.62789(9) 0.40769(4) 0.21493(14) 0.0064(3) Uani 0.78 1 d . . P A 4
Nd1 Nd 0.81335(7) 0.5000 0.38297(11) 0.0113(3) Uani 1 2 d S T P A .
Nd2 Nd 0.28405(8) 0.5000 0.08113(12) 0.0161(3) Uani 1 2 d S T P A .
K1 K 0.6027(4) 0.5000 0.3484(6) 0.0342(15) Uani 1 2 d S T P A .
P1 P 0.5000 0.32448(15) 0.0000 0.0058(11) Uani 1 2 d S T P A .
O1 O 0.5192(6) 0.3530(3) 0.0979(9) 0.009(2) Uani 1 1 d . U . . .
O2 O 0.4244(6) 0.2944(3) -0.0543(9) 0.010(2) Uani 1 1 d . U . . .
O3 O 0.3991(6) 0.4241(3) -0.0689(9) 0.011(2) Uani 1 1 d . . . . .
O4 O 0.3446(6) 0.3600(3) -0.0201(9) 0.012(2) Uani 1 1 d . U . . .
O5 O 0.7037(6) 0.4458(3) 0.3129(9) 0.010(2) Uani 1 1 d . U . . .
O6 O 0.2726(7) 0.2735(3) -0.2497(9) 0.012(2) Uani 1 1 d . . . . .
O7 O 0.5323(6) 0.4349(3) 0.1716(9) 0.010(2) Uani 1 1 d . U . . .
O8 O 0.3716(6) 0.4466(3) 0.0790(9) 0.011(2) Uani 1 1 d . U . . .
O9 O 0.5794(7) 0.3154(3) 0.4109(10) 0.015(2) Uani 1 1 d . U . . .
O10 O 0.3010(7) 0.2010(3) -0.3297(10) 0.017(2) Uani 1 1 d . U . . .
O11 O 0.1837(7) 0.3297(3) -0.2239(10) 0.015(2) Uani 1 1 d . . . . .
O12 O 0.3947(7) 0.1996(3) 0.1117(10) 0.018(3) Uani 1 1 d . . . . .
O13 O 0.6286(6) 0.2846(3) 0.2906(9) 0.010(2) Uani 1 1 d . U . . .
O14 O 0.5276(6) 0.2242(3) 0.1275(9) 0.009(2) Uani 1 1 d . U . . .
O15 O 0.4701(6) 0.2851(3) 0.1722(9) 0.012(2) Uani 1 1 d . U . . .
O16 O 0.3162(7) 0.2742(3) -0.0410(9) 0.013(2) Uani 1 1 d . . . . .
O17 O 0.4740(7) 0.3714(3) 0.2137(10) 0.014(2) Uani 1 1 d . . . . .
O18 O 0.3002(7) 0.3613(3) -0.2290(9) 0.013(2) Uani 1 1 d . . . . .
O19 O 0.6375(6) 0.3701(3) 0.3329(9) 0.011(2) Uani 1 1 d . . . . .
O20 O 0.3737(6) 0.2111(3) -0.0899(9) 0.012(2) Uani 1 1 d . U . . .
O21 O 0.9089(7) 0.5533(4) 0.5431(11) 0.022(3) Uani 1 1 d . U . . .
O22 O 1.0325(8) 0.5807(4) 0.6358(13) 0.038(3) Uani 1 1 d . U . . .
O23 O 0.3349(9) 0.4215(4) 0.3593(12) 0.033(3) Uani 1 1 d . . . . .
O24 O 0.2870(8) 0.4386(4) 0.1785(11) 0.024(3) Uani 1 1 d . . . . .
N1 N 0.8077(10) 0.6767(5) 0.4787(14) 0.028(4) Uani 1 1 d . . . . .
H1A H 0.7542 0.6798 0.4319 0.034 Uiso 1 1 calc R U . . .
N2 N 0.3156(9) 0.3087(5) 0.1300(14) 0.021(3) Uani 1 1 d . U . . .
H2A H 0.3038 0.3009 0.0654 0.026 Uiso 1 1 calc R U . . .
C1 C 0.9582(10) 0.5839(5) 0.5818(15) 0.016(4) Uani 1 1 d . U . . .
C2 C 0.9251(10) 0.6299(5) 0.5681(14) 0.016(4) Uani 1 1 d . U . . .
C3 C 0.8400(10) 0.6367(5) 0.5022(16) 0.021(4) Uani 1 1 d . . . . .
H3A H 0.8050 0.6122 0.4741 0.026 Uiso 1 1 calc R U . . .
C4 C 0.8557(11) 0.7117(5) 0.5253(15) 0.021(4) Uani 1 1 d . U . . .
H4A H 0.8321 0.7394 0.5130 0.025 Uiso 1 1 calc R U . . .
C5 C 0.9418(11) 0.7088(5) 0.5932(16) 0.020(4) Uani 1 1 d . . . . .
H5A H 0.9745 0.7343 0.6207 0.025 Uiso 1 1 calc R U . . .
C6 C 0.9760(11) 0.6687(5) 0.6177(16) 0.023(4) Uani 1 1 d . . . . .
H6A H 1.0339 0.6661 0.6680 0.028 Uiso 1 1 calc R U . . .
C7 C 0.3156(11) 0.4130(6) 0.2621(19) 0.028(5) Uani 1 1 d . . . . .
C8 C 0.3227(12) 0.3626(5) 0.2452(16) 0.022(4) Uani 1 1 d . . . . .
C9 C 0.3018(11) 0.3506(5) 0.1414(17) 0.024(4) Uani 1 1 d . U . . .
H9A H 0.2784 0.3711 0.0797 0.029 Uiso 1 1 calc R U . . .
C10 C 0.3470(11) 0.2789(6) 0.2155(15) 0.022(4) Uani 1 1 d . . . . .
H10A H 0.3562 0.2500 0.2053 0.027 Uiso 1 1 calc R U . . .
C11 C 0.3660(11) 0.2899(6) 0.3178(17) 0.025(4) Uani 1 1 d . U . . .
H11A H 0.3874 0.2691 0.3782 0.030 Uiso 1 1 calc R U . . .
C12 C 0.3523(12) 0.3329(5) 0.3288(17) 0.023(4) Uani 1 1 d . . . . .
H12A H 0.3644 0.3413 0.3981 0.027 Uiso 1 1 calc R U . . .
O1W O 0.8190(7) 0.5721(3) 0.2926(11) 0.020(3) Uani 1 1 d . U . . .
H1WA H 0.7813 0.5919 0.2611 0.024 Uiso 1 1 d R U . A .
H1WB H 0.8583 0.5756 0.2945 0.024 Uiso 1 1 d R U . . .
O2W O 0.7899(11) 0.5000 0.5236(16) 0.024(4) Uani 1 2 d S T P A .
O3W O 0.7073(10) 0.5000 0.1547(14) 0.018(4) Uani 1 2 d S TU P . .
H3WA H 0.6550 0.5000 0.1144 0.021 Uiso 1 2 d R U P A .
H3WB H 0.7239 0.5000 0.1182 0.021 Uiso 1 2 d R U P . .
O4W O 0.9190(10) 0.5000 0.3708(17) 0.027(4) Uani 1 2 d S T P . .
H4WA H 0.9665 0.5179 0.4227 0.032 Uiso 0.5 1 calc R U P A .
H4WB H 0.9116 0.4821 0.3143 0.032 Uiso 0.5 1 calc R U P . .
O5W O 0.4210(13) 0.5000 0.2848(17) 0.036(5) Uani 1 2 d S T P A .
O6W O 0.1927(9) 0.4489(5) -0.0898(12) 0.040(4) Uani 1 1 d . . . . .
H6WA H 0.2140 0.4290 -0.1015 0.048 Uiso 1 1 d R U . A .
H6WB H 0.1395 0.4510 -0.1376 0.048 Uiso 1 1 d R U . . .
O7W O 0.1458(11) 0.5000 0.0176(15) 0.028(4) Uani 1 2 d S TU P . .
H7WA H 0.1149 0.4770 -0.0148 0.034 Uiso 0.5 1 d R U P A .
H7WB H 0.1290 0.5230 0.0281 0.034 Uiso 0.5 1 d R U P . .
OW1 O 0.2473(13) 0.4174(5) 0.4360(18) 0.064(5) Uani 1 1 d . . . . .
OW2 O 0.0864(12) 0.3944(6) -0.1072(19) 0.073(6) Uani 1 1 d . . . . .
OW3 O 0.5259(13) 0.5694(5) 0.4002(15) 0.075(6) Uani 1 1 d . . . . .
OW4 O 0.6962(18) 0.5000 0.601(2) 0.068(7) Uani 1 2 d S T P A .
OW6 O 0.920(2) 0.5821(10) 0.779(3) 0.060(10) Uani 0.5 1 d . . P . .
OW5 O 0.110(3) 0.3854(13) 0.099(3) 0.190(15) Uani 1 1 d . U . . .
OW7 O 0.9874(18) 0.5000 0.789(2) 0.100(11) Uani 1 2 d S T P . .
OW8 O 0.863(2) 0.5000 0.810(3) 0.121(12) Uani 1 2 d S TU P . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
W1 O10 1.707(10) . ?
W1 O13 1.876(9) 2_655 ?
W1 O6 1.887(11) . ?
W1 O14 1.898(10) 2_655 ?
W1 O20 1.950(10) . ?
W1 O2 2.456(9) . ?
W2 O11 1.701(11) . ?
W2 O18 1.838(10) . ?
W2 O4 1.852(10) . ?
W2 O16 1.955(10) . ?
W2 O6 1.960(10) . ?
W2 O2 2.427(10) . ?
W3 O12 1.731(10) . ?
W3 O20 1.894(10) . ?
W3 O15 1.900(10) . ?
W3 O14 1.902(10) . ?
W3 O16 1.917(10) . ?
W3 O2 2.434(10) . ?
W4 O9 1.707(11) . ?
W4 O17 1.856(10) . ?
W4 O19 1.869(10) . ?
W4 O15 1.913(10) . ?
W4 O13 1.987(10) . ?
W4 O1 2.435(10) . ?
W5 O8 1.714(9) . ?
W5 O3 1.839(10) . ?
W5 O7 1.852(10) . ?
W5 O4 1.976(10) . ?
W5 O17 1.986(10) . ?
W5 O1 2.447(10) . ?
W6 O5 1.699(10) . ?
W6 O7 1.894(10) . ?
W6 O3 1.934(11) 2_655 ?
W6 O18 2.004(10) 2_655 ?
W6 O19 2.008(10) . ?
W6 O1 2.390(10) . ?
W6 K1 3.703(5) . ?
Nd1 O21 2.424(11) . ?
Nd1 O21 2.424(11) 6_565 ?
Nd1 O5 2.458(10) . ?
Nd1 O5 2.458(10) 6_565 ?
Nd1 O4W 2.446(17) . ?
Nd1 O3W 2.524(16) . ?
Nd1 O2W 2.525(17) . ?
Nd1 O1W 2.618(11) 6_565 ?
Nd1 O1W 2.618(11) . ?
Nd1 K1 4.272(7) . ?
Nd2 O24 2.344(12) . ?
Nd2 O24 2.344(12) 6_565 ?
Nd2 O5W 2.411(19) . ?
Nd2 O6W 2.445(12) 6_565 ?
Nd2 O6W 2.445(12) . ?
Nd2 O7W 2.465(18) . ?
Nd2 O8 2.520(10) . ?
Nd2 O8 2.520(10) 6_565 ?
K1 O7 2.785(11) . ?
K1 O7 2.785(11) 6_565 ?
K1 OW4 2.86(3) . ?
K1 O2W 2.979(19) . ?
K1 O5 3.083(12) . ?
K1 O5 3.083(12) 6_565 ?
K1 OW3 3.11(2) . ?
K1 OW3 3.11(2) 6_565 ?
K1 O5W 3.39(2) . ?
K1 Ti2 3.703(5) 6_565 ?
K1 W6 3.703(5) 6_565 ?
P1 O1 1.509(10) 2_655 ?
P1 O1 1.509(10) . ?
P1 O2 1.536(10) 2_655 ?
P1 O2 1.536(10) . ?
O3 Ti2 1.933(11) 2_655 ?
O3 W6 1.933(11) 2_655 ?
O13 W1 1.876(9) 2_655 ?
O14 W1 1.898(10) 2_655 ?
O18 Ti2 2.004(10) 2_655 ?
O18 W6 2.004(10) 2_655 ?
O21 C1 1.219(18) . ?
O22 C1 1.22(2) . ?
O23 C7 1.26(2) . ?
O24 C7 1.23(2) . ?
N1 C4 1.30(2) . ?
N1 C3 1.31(2) . ?
N1 H1A 0.8600 . ?
N2 C10 1.32(2) . ?
N2 C9 1.34(2) . ?
N2 H2A 0.8600 . ?
C1 C2 1.51(2) . ?
C2 C3 1.40(2) . ?
C2 C6 1.42(2) . ?
C3 H3A 0.9300 . ?
C4 C5 1.40(2) . ?
C4 H4A 0.9300 . ?
C5 C6 1.33(2) . ?
C5 H5A 0.9300 . ?
C6 H6A 0.9300 . ?
C7 C8 1.56(2) . ?
C8 C12 1.31(2) . ?
C8 C9 1.36(2) . ?
C9 H9A 0.9300 . ?
C10 C11 1.35(2) . ?
C10 H10A 0.9300 . ?
C11 C12 1.37(2) . ?
C11 H11A 0.9300 . ?
C12 H12A 0.9300 . ?
O1W H1WA 0.8499 . ?
O1W H1WB 0.8498 . ?
O3W H3WA 0.8499 . ?
O3W H3WB 0.8500 . ?
O4W H4WA 0.9300 . ?
O4W H4WB 0.9300 . ?
O6W H6WA 0.8497 . ?
O6W H6WB 0.8502 . ?
O7W H7WA 0.8500 . ?
O7W H7WB 0.8499 . ?

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
_geom_angle_publ_flag
O10 W1 O13 102.4(5) . 2_655 ?
O10 W1 O6 100.9(5) . . ?
O13 W1 O6 89.7(4) 2_655 . ?
O10 W1 O14 104.6(5) . 2_655 ?
O13 W1 O14 87.5(4) 2_655 2_655 ?
O6 W1 O14 154.3(4) . 2_655 ?
O10 W1 O20 100.9(5) . . ?
O13 W1 O20 156.7(4) 2_655 . ?
O6 W1 O20 86.7(4) . . ?
O14 W1 O20 85.8(4) 2_655 . ?
O10 W1 O2 170.2(4) . . ?
O13 W1 O2 84.3(4) 2_655 . ?
O6 W1 O2 71.7(4) . . ?
O14 W1 O2 82.6(4) 2_655 . ?
O20 W1 O2 72.7(4) . . ?
O11 W2 O18 103.1(5) . . ?
O11 W2 O4 103.8(5) . . ?
O18 W2 O4 90.1(4) . . ?
O11 W2 O16 99.8(5) . . ?
O18 W2 O16 156.9(5) . . ?
O4 W2 O16 87.0(4) . . ?
O11 W2 O6 99.7(5) . . ?
O18 W2 O6 89.6(4) . . ?
O4 W2 O6 155.9(4) . . ?
O16 W2 O6 83.9(4) . . ?
O11 W2 O2 167.8(4) . . ?
O18 W2 O2 85.5(4) . . ?
O4 W2 O2 84.6(4) . . ?
O16 W2 O2 71.5(4) . . ?
O6 W2 O2 71.3(4) . . ?
O12 W3 O20 101.0(5) . . ?
O12 W3 O15 103.2(5) . . ?
O20 W3 O15 155.9(4) . . ?
O12 W3 O14 103.3(5) . . ?
O20 W3 O14 89.3(4) . . ?
O15 W3 O14 85.0(4) . . ?
O12 W3 O16 100.8(5) . . ?
O20 W3 O16 88.4(4) . . ?
O15 W3 O16 87.4(4) . . ?
O14 W3 O16 155.9(4) . . ?
O12 W3 O2 171.0(4) . . ?
O20 W3 O2 74.1(4) . . ?
O15 W3 O2 82.0(4) . . ?
O14 W3 O2 84.4(4) . . ?
O16 W3 O2 71.9(4) . . ?
O9 W4 O17 101.7(5) . . ?
O9 W4 O19 103.0(5) . . ?
O17 W4 O19 92.0(4) . . ?
O9 W4 O15 100.9(5) . . ?
O17 W4 O15 89.8(4) . . ?
O19 W4 O15 155.2(4) . . ?
O9 W4 O13 100.6(5) . . ?
O17 W4 O13 157.4(5) . . ?
O19 W4 O13 85.9(4) . . ?
O15 W4 O13 83.1(4) . . ?
O9 W4 O1 174.5(4) . . ?
O17 W4 O1 73.5(4) . . ?
O19 W4 O1 74.8(4) . . ?
O15 W4 O1 82.1(4) . . ?
O13 W4 O1 84.3(4) . . ?
O8 W5 O3 103.3(5) . . ?
O8 W5 O7 101.9(5) . . ?
O3 W5 O7 94.3(4) . . ?
O8 W5 O4 101.6(5) . . ?
O3 W5 O4 87.2(4) . . ?
O7 W5 O4 155.5(4) . . ?
O8 W5 O17 99.7(5) . . ?
O3 W5 O17 156.4(4) . . ?
O7 W5 O17 85.8(4) . . ?
O4 W5 O17 83.3(4) . . ?
O8 W5 O1 170.3(4) . . ?
O3 W5 O1 86.0(4) . . ?
O7 W5 O1 74.4(4) . . ?
O4 W5 O1 81.3(4) . . ?
O17 W5 O1 71.3(4) . . ?
O5 W6 O7 101.0(5) . . ?
O5 W6 O3 100.2(5) . 2_655 ?
O7 W6 O3 95.7(4) . 2_655 ?
O5 W6 O18 99.0(5) . 2_655 ?
O7 W6 O18 159.7(4) . 2_655 ?
O3 W6 O18 84.0(4) 2_655 2_655 ?
O5 W6 O19 99.0(4) . . ?
O7 W6 O19 88.0(4) . . ?
O3 W6 O19 159.3(4) 2_655 . ?
O18 W6 O19 85.6(4) 2_655 . ?
O5 W6 O1 171.6(4) . . ?
O7 W6 O1 75.1(4) . . ?
O3 W6 O1 87.7(4) 2_655 . ?
O18 W6 O1 84.6(4) 2_655 . ?
O19 W6 O1 73.6(4) . . ?
O5 W6 K1 55.7(4) . . ?
O7 W6 K1 47.1(3) . . ?
O3 W6 K1 113.5(3) 2_655 . ?
O18 W6 K1 150.3(3) 2_655 . ?
O19 W6 K1 83.9(3) . . ?
O1 W6 K1 118.5(3) . . ?
O21 Nd1 O21 82.9(5) . 6_565 ?
O21 Nd1 O5 141.7(4) . . ?
O21 Nd1 O5 84.7(3) 6_565 . ?
O21 Nd1 O5 84.7(3) . 6_565 ?
O21 Nd1 O5 141.7(4) 6_565 6_565 ?
O5 Nd1 O5 83.1(5) . 6_565 ?
O21 Nd1 O4W 82.5(4) . . ?
O21 Nd1 O4W 82.5(4) 6_565 . ?
O5 Nd1 O4W 131.3(3) . . ?
O5 Nd1 O4W 131.3(3) 6_565 . ?
O21 Nd1 O3W 136.5(3) . . ?
O21 Nd1 O3W 136.5(3) 6_565 . ?
O5 Nd1 O3W 72.8(4) . . ?
O5 Nd1 O3W 72.8(4) 6_565 . ?
O4W Nd1 O3W 85.2(6) . . ?
O21 Nd1 O2W 71.7(4) . . ?
O21 Nd1 O2W 71.7(4) 6_565 . ?
O5 Nd1 O2W 70.1(4) . . ?
O5 Nd1 O2W 70.1(4) 6_565 . ?
O4W Nd1 O2W 145.2(6) . . ?
O3W Nd1 O2W 129.6(5) . . ?
O21 Nd1 O1W 139.2(4) . 6_565 ?
O21 Nd1 O1W 70.1(4) 6_565 6_565 ?
O5 Nd1 O1W 66.9(3) . 6_565 ?
O5 Nd1 O1W 135.0(4) 6_565 6_565 ?
O4W Nd1 O1W 64.6(3) . 6_565 ?
O3W Nd1 O1W 66.9(3) . 6_565 ?
O2W Nd1 O1W 123.9(2) . 6_565 ?
O21 Nd1 O1W 70.1(4) . . ?
O21 Nd1 O1W 139.2(4) 6_565 . ?
O5 Nd1 O1W 135.0(3) . . ?
O5 Nd1 O1W 66.9(3) 6_565 . ?
O4W Nd1 O1W 64.6(3) . . ?
O3W Nd1 O1W 66.9(3) . . ?
O2W Nd1 O1W 123.9(2) . . ?
O1W Nd1 O1W 112.0(5) 6_565 . ?
O21 Nd1 K1 103.6(3) . . ?
O21 Nd1 K1 103.6(3) 6_565 . ?
O5 Nd1 K1 45.2(2) . . ?
O5 Nd1 K1 45.2(2) 6_565 . ?
O4W Nd1 K1 171.7(4) . . ?
O3W Nd1 K1 86.5(4) . . ?
O2W Nd1 K1 43.1(4) . . ?
O1W Nd1 K1 111.9(2) 6_565 . ?
O1W Nd1 K1 111.9(2) . . ?
O24 Nd2 O24 104.1(5) . 6_565 ?
O24 Nd2 O5W 73.6(4) . . ?
O24 Nd2 O5W 73.6(4) 6_565 . ?
O24 Nd2 O6W 144.7(5) . 6_565 ?
O24 Nd2 O6W 79.8(4) 6_565 6_565 ?
O5W Nd2 O6W 138.7(4) . 6_565 ?
O24 Nd2 O6W 79.8(4) . . ?
O24 Nd2 O6W 144.7(5) 6_565 . ?
O5W Nd2 O6W 138.7(4) . . ?
O6W Nd2 O6W 78.0(7) 6_565 . ?
O24 Nd2 O7W 74.9(4) . . ?
O24 Nd2 O7W 74.9(4) 6_565 . ?
O5W Nd2 O7W 127.6(6) . . ?
O6W Nd2 O7W 72.4(4) 6_565 . ?
O6W Nd2 O7W 72.4(4) . . ?
O24 Nd2 O8 79.4(4) . . ?
O24 Nd2 O8 145.3(4) 6_565 . ?
O5W Nd2 O8 74.5(4) . . ?
O6W Nd2 O8 117.4(4) 6_565 . ?
O6W Nd2 O8 70.0(4) . . ?
O7W Nd2 O8 137.4(3) . . ?
O24 Nd2 O8 145.3(4) . 6_565 ?
O24 Nd2 O8 79.4(4) 6_565 6_565 ?
O5W Nd2 O8 74.5(4) . 6_565 ?
O6W Nd2 O8 70.0(4) 6_565 6_565 ?
O6W Nd2 O8 117.4(4) . 6_565 ?
O7W Nd2 O8 137.4(3) . 6_565 ?
O8 Nd2 O8 79.2(5) . 6_565 ?
O7 K1 O7 89.4(4) . 6_565 ?
O7 K1 OW4 135.2(2) . . ?
O7 K1 OW4 135.2(2) 6_565 . ?
O7 K1 O2W 111.7(3) . . ?
O7 K1 O2W 111.7(3) 6_565 . ?
OW4 K1 O2W 61.6(7) . . ?
O7 K1 O5 56.2(3) . . ?
O7 K1 O5 100.8(3) 6_565 . ?
OW4 K1 O5 107.5(5) . . ?
O2W K1 O5 56.3(3) . . ?
O7 K1 O5 100.8(3) . 6_565 ?
O7 K1 O5 56.2(3) 6_565 6_565 ?
OW4 K1 O5 107.5(5) . 6_565 ?
O2W K1 O5 56.3(3) . 6_565 ?
O5 K1 O5 63.9(4) . 6_565 ?
O7 K1 OW3 133.1(5) . . ?
O7 K1 OW3 74.8(4) 6_565 . ?
OW4 K1 OW3 70.7(5) . . ?
O2W K1 OW3 115.2(4) . . ?
O5 K1 OW3 168.7(4) . . ?
O5 K1 OW3 105.6(4) 6_565 . ?
O7 K1 OW3 74.8(4) . 6_565 ?
O7 K1 OW3 133.1(5) 6_565 6_565 ?
OW4 K1 OW3 70.7(5) . 6_565 ?
O2W K1 OW3 115.2(4) . 6_565 ?
O5 K1 OW3 105.6(4) . 6_565 ?
O5 K1 OW3 168.7(4) 6_565 6_565 ?
OW3 K1 OW3 84.5(6) . 6_565 ?
O7 K1 O5W 88.0(3) . . ?
O7 K1 O5W 88.0(3) 6_565 . ?
OW4 K1 O5W 89.8(7) . . ?
O2W K1 O5W 151.5(5) . . ?
O5 K1 O5W 142.6(3) . . ?
O5 K1 O5W 142.6(3) 6_565 . ?
OW3 K1 O5W 48.5(4) . . ?
OW3 K1 O5W 48.5(4) 6_565 . ?
O7 K1 Ti2 100.8(3) . 6_565 ?
O7 K1 Ti2 29.9(2) 6_565 6_565 ?
OW4 K1 Ti2 120.0(3) . 6_565 ?
O2W K1 Ti2 81.8(3) . 6_565 ?
O5 K1 Ti2 84.5(2) . 6_565 ?
O5 K1 Ti2 27.08(18) 6_565 6_565 ?
OW3 K1 Ti2 87.0(3) . 6_565 ?
OW3 K1 Ti2 163.0(4) 6_565 6_565 ?
O5W K1 Ti2 115.7(2) . 6_565 ?
O7 K1 W6 100.8(3) . 6_565 ?
O7 K1 W6 29.9(2) 6_565 6_565 ?
OW4 K1 W6 120.0(3) . 6_565 ?
O2W K1 W6 81.8(3) . 6_565 ?
O5 K1 W6 84.5(2) . 6_565 ?
O5 K1 W6 27.08(18) 6_565 6_565 ?
OW3 K1 W6 87.0(3) . 6_565 ?
OW3 K1 W6 163.0(4) 6_565 6_565 ?
O5W K1 W6 115.7(2) . 6_565 ?
O7 K1 W6 29.9(2) . . ?
O7 K1 W6 100.8(3) 6_565 . ?
OW4 K1 W6 120.0(3) . . ?
O2W K1 W6 81.8(3) . . ?
O5 K1 W6 27.08(18) . . ?
O5 K1 W6 84.5(2) 6_565 . ?
OW3 K1 W6 163.0(4) . . ?
OW3 K1 W6 87.0(3) 6_565 . ?
O5W K1 W6 115.7(2) . . ?
W6 K1 W6 97.22(16) 6_565 . ?
O1 P1 O1 110.6(8) 2_655 . ?
O1 P1 O2 109.3(5) 2_655 2_655 ?
O1 P1 O2 109.9(5) . 2_655 ?
O1 P1 O2 109.9(5) 2_655 . ?
O1 P1 O2 109.3(5) . . ?
O2 P1 O2 107.8(8) 2_655 . ?
P1 O1 W6 125.8(6) . . ?
P1 O1 W4 127.3(5) . . ?
W6 O1 W4 89.1(3) . . ?
P1 O1 W5 126.6(6) . . ?
W4 O1 W5 89.0(3) . . ?
P1 O2 W2 123.9(5) . . ?
P1 O2 W3 126.2(6) . . ?
W2 O2 W3 90.5(3) . . ?
P1 O2 W1 126.8(6) . . ?
W2 O2 W1 89.8(3) . . ?
W3 O2 W1 88.3(3) . . ?
W2 O4 W5 147.3(6) . . ?
W6 O5 Nd1 154.3(6) . . ?
W6 O5 K1 97.2(4) . . ?
Nd1 O5 K1 100.3(3) . . ?
W1 O6 W2 127.2(5) . . ?
W5 O7 K1 129.5(5) . . ?
W6 O7 K1 103.0(4) . . ?
W5 O8 Nd2 177.2(6) . . ?
W1 O13 W4 149.7(6) 2_655 . ?
W1 O14 W3 150.8(5) 2_655 . ?
W3 O15 W4 155.3(6) . . ?
W3 O16 W2 126.1(6) . . ?
W4 O17 W5 125.8(6) . . ?
W2 O18 Ti2 147.8(6) . 2_655 ?
W2 O18 W6 147.8(6) . 2_655 ?
W4 O19 W6 121.7(5) . . ?
W3 O20 W1 124.8(5) . . ?
C1 O21 Nd1 148.3(12) . . ?
C7 O24 Nd2 157.4(12) . . ?
C4 N1 C3 120.8(16) . . ?
C4 N1 H1A 119.6 . . ?
C3 N1 H1A 119.6 . . ?
C10 N2 C9 121.6(16) . . ?
C10 N2 H2A 119.2 . . ?
C9 N2 H2A 119.2 . . ?
O21 C1 O22 126.3(15) . . ?
O21 C1 C2 116.5(15) . . ?
O22 C1 C2 117.1(14) . . ?
C3 C2 C6 115.7(14) . . ?
C3 C2 C1 120.7(14) . . ?
C6 C2 C1 123.7(15) . . ?
N1 C3 C2 122.1(15) . . ?
N1 C3 H3A 118.9 . . ?
C2 C3 H3A 118.9 . . ?
N1 C4 C5 121.7(15) . . ?
N1 C4 H4A 119.2 . . ?
C5 C4 H4A 119.2 . . ?
C6 C5 C4 118.5(16) . . ?
C6 C5 H5A 120.7 . . ?
C4 C5 H5A 120.7 . . ?
C5 C6 C2 120.8(17) . . ?
C5 C6 H6A 119.6 . . ?
C2 C6 H6A 119.6 . . ?
O24 C7 O23 127.7(17) . . ?
O24 C7 C8 118.4(17) . . ?
O23 C7 C8 113.7(16) . . ?
C12 C8 C9 119.8(16) . . ?
C12 C8 C7 122.9(17) . . ?
C9 C8 C7 117.2(15) . . ?
N2 C9 C8 118.5(16) . . ?
N2 C9 H9A 120.7 . . ?
C8 C9 H9A 120.7 . . ?
N2 C10 C11 120.7(17) . . ?
N2 C10 H10A 119.7 . . ?
C11 C10 H10A 119.7 . . ?
C10 C11 C12 117.2(16) . . ?
C10 C11 H11A 121.4 . . ?
C12 C11 H11A 121.4 . . ?
C8 C12 C11 122.2(17) . . ?
C8 C12 H12A 118.9 . . ?
C11 C12 H12A 118.9 . . ?
Nd1 O1W H1WA 120.0 . . ?
Nd1 O1W H1WB 120.0 . . ?
H1WA O1W H1WB 120.0 . . ?
Nd1 O2W K1 101.5(6) . . ?
Nd1 O3W H3WA 120.0 . . ?
Nd1 O3W H3WB 120.0 . . ?
H3WA O3W H3WB 120.0 . . ?
Nd1 O4W H4WA 120.0 . . ?
Nd1 O4W H4WB 120.0 . . ?
H4WA O4W H4WB 120.0 . . ?
Nd2 O5W K1 123.0(7) . . ?
Nd2 O6W H6WA 120.1 . . ?
Nd2 O6W H6WB 119.9 . . ?
H6WA O6W H6WB 120.0 . . ?
Nd2 O7W H7WA 120.0 . . ?
Nd2 O7W H7WB 120.0 . . ?
H7WA O7W H7WB 120.0 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O1 P1 O1 W6_c -57.8(5) 2_655 . . . ?
O2 P1 O1 W6 63.0(8) 2_655 . . . ?
O2 P1 O1 W6 -178.9(6) . . . . ?
O1 P1 O1 W4 -179.5(8) 2_655 . . . ?
O2 P1 O1 W4 -58.8(8) 2_655 . . . ?
O2 P1 O1 W4 59.4(8) . . . . ?
O1 P1 O1 W5 58.1(5) 2_655 . . . ?
O2 P1 O1 W5 178.8(6) 2_655 . . . ?
O2 P1 O1 W5 -63.0(8) . . . . ?
O1 P1 O2 W2 -61.8(7) 2_655 . . . ?
O1 P1 O2 W2 59.8(8) . . . . ?
O2 P1 O2 W2 179.2(8) 2_655 . . . ?
O1 P1 O2 W3 178.1(6) 2_655 . . . ?
O1 P1 O2 W3 -60.4(8) . . . . ?
O2 P1 O2 W3 59.0(5) 2_655 . . . ?
O1 P1 O2 W1 58.0(8) 2_655 . . . ?
O1 P1 O2 W1 179.5(6) . . . . ?
O2 P1 O2 W1 -61.1(5) 2_655 . . . ?
O8 W5 O3 Ti2 -141.7(12) . . . 2_655 ?
O7 W5 O3 Ti2 115.0(12) . . . 2_655 ?
O4 W5 O3 Ti2 -40.4(12) . . . 2_655 ?
O17 W5 O3 Ti2 26(2) . . . 2_655 ?
O1 W5 O3 Ti2 41.1(12) . . . 2_655 ?
O8 W5 O3 W6 -141.7(12) . . . 2_655 ?
O7 W5 O3 W6 115.0(12) . . . 2_655 ?
O4 W5 O3 W6 -40.4(12) . . . 2_655 ?
O17 W5 O3 W6 26(2) . . . 2_655 ?
O1 W5 O3 W6 41.1(12) . . . 2_655 ?
O11 W2 O4 W5 -125.9(10) . . . . ?
O18 W2 O4 W5 -22.4(11) . . . . ?
O16 W2 O4 W5 134.7(11) . . . . ?
O6 W2 O4 W5 66.9(16) . . . . ?
O2 W2 O4 W5 63.1(10) . . . . ?
O7 W6 O5 Nd1 -119.2(12) . . . . ?
O3 W6 O5 Nd1 -21.2(13) 2_655 . . . ?
O18 W6 O5 Nd1 64.2(13) 2_655 . . . ?
O19 W6 O5 Nd1 151.1(12) . . . . ?
K1 W6 O5 Nd1 -132.7(14) . . . . ?
O7 W6 O5 K1 13.5(4) . . . . ?
O3 W6 O5 K1 111.5(4) 2_655 . . . ?
O18 W6 O5 K1 -163.0(4) 2_655 . . . ?
O19 W6 O5 K1 -76.2(4) . . . . ?
O10 W1 O6 W2 173.7(6) . . . . ?
O13 W1 O6 W2 -83.7(7) 2_655 . . . ?
O14 W1 O6 W2 0.0(14) 2_655 . . . ?
O20 W1 O6 W2 73.3(7) . . . . ?
O2 W1 O6 W2 0.4(5) . . . . ?
O8 W5 O7 W6 174.5(6) . . . . ?
O3 W5 O7 W6 -80.9(6) . . . . ?
O4 W5 O7 W6 11.6(14) . . . . ?
O17 W5 O7 W6 75.5(6) . . . . ?
O1 W5 O7 W6 3.8(5) . . . . ?
O8 W5 O7 K1 19.0(7) . . . . ?
O3 W5 O7 K1 123.6(6) . . . . ?
O4 W5 O7 K1 -143.9(8) . . . . ?
O17 W5 O7 K1 -80.1(6) . . . . ?
O1 W5 O7 K1 -151.8(6) . . . . ?
O5 W6 O7 W5 -176.1(6) . . . . ?
O3 W6 O7 W5 82.2(6) 2_655 . . . ?
O18 W6 O7 W5 -5.9(17) 2_655 . . . ?
O19 W6 O7 W5 -77.3(6) . . . . ?
O1 W6 O7 W5 -3.8(5) . . . . ?
K1 W6 O7 W5 -160.8(8) . . . . ?
O5 W6 O7 K1 -15.3(5) . . . . ?
O3 W6 O7 K1 -116.9(4) 2_655 . . . ?
O18 W6 O7 K1 154.9(11) 2_655 . . . ?
O19 W6 O7 K1 83.5(4) . . . . ?
O1 W6 O7 K1 157.0(4) . . . . ?
O12 W3 O15 W4 131.2(14) . . . . ?
O20 W3 O15 W4 -48(2) . . . . ?
O14 W3 O15 W4 28.8(14) . . . . ?
O16 W3 O15 W4 -128.3(14) . . . . ?
O2 W3 O15 W4 -56.2(13) . . . . ?
O9 W4 O17 W5 170.6(6) . . . . ?
O19 W4 O17 W5 66.9(7) . . . . ?
O15 W4 O17 W5 -88.4(7) . . . . ?
O13 W4 O17 W5 -17.1(15) . . . . ?
O1 W4 O17 W5 -6.6(5) . . . . ?
O11 W2 O18 Ti2 135.7(11) . . . 2_655 ?
O4 W2 O18 Ti2 31.5(11) . . . 2_655 ?
O16 W2 O18 Ti2 -51.1(18) . . . 2_655 ?
O6 W2 O18 Ti2 -124.4(11) . . . 2_655 ?
O2 W2 O18 Ti2 -53.1(11) . . . 2_655 ?
O11 W2 O18 W6 135.7(11) . . . 2_655 ?
O4 W2 O18 W6 31.5(11) . . . 2_655 ?
O16 W2 O18 W6 -51.1(18) . . . 2_655 ?
O6 W2 O18 W6 -124.4(11) . . . 2_655 ?
O2 W2 O18 W6 -53.1(11) . . . 2_655 ?
O9 W4 O19 W6 -166.3(6) . . . . ?
O17 W4 O19 W6 -63.8(6) . . . . ?
O15 W4 O19 W6 30.0(13) . . . . ?
O13 W4 O19 W6 93.7(6) . . . . ?
O1 W4 O19 W6 8.6(5) . . . . ?
O12 W3 O20 W1 169.0(7) . . . . ?
O15 W3 O20 W1 -11.4(15) . . . . ?
O14 W3 O20 W1 -87.6(6) . . . . ?
O16 W3 O20 W1 68.4(7) . . . . ?
O2 W3 O20 W1 -3.3(6) . . . . ?
Nd1 O21 C1 O22 -83(3) . . . . ?
Nd1 O21 C1 C2 101(2) . . . . ?
O21 C1 C2 C3 -7(2) . . . . ?
O22 C1 C2 C3 176.6(17) . . . . ?
O21 C1 C2 C6 174.1(16) . . . . ?
O22 C1 C2 C6 -2(3) . . . . ?
C4 N1 C3 C2 -6(3) . . . . ?
C6 C2 C3 N1 6(3) . . . . ?
C1 C2 C3 N1 -173.2(17) . . . . ?
C3 N1 C4 C5 6(3) . . . . ?
N1 C4 C5 C6 -5(3) . . . . ?
C4 C5 C6 C2 5(3) . . . . ?
C3 C2 C6 C5 -5(3) . . . . ?
C1 C2 C6 C5 173.7(17) . . . . ?
Nd2 O24 C7 O23 63(4) . . . . ?
Nd2 O24 C7 C8 -123(3) . . . . ?
O24 C7 C8 C12 -180.0(18) . . . . ?
O23 C7 C8 C12 -5(3) . . . . ?
O24 C7 C8 C9 4(3) . . . . ?
O23 C7 C8 C9 179.2(16) . . . . ?
C10 N2 C9 C8 2(2) . . . . ?
C12 C8 C9 N2 -3(3) . . . . ?
C7 C8 C9 N2 173.0(15) . . . . ?
C9 N2 C10 C11 0(3) . . . . ?
N2 C10 C11 C12 -1(3) . . . . ?
C9 C8 C12 C11 2(3) . . . . ?
C7 C8 C12 C11 -173.3(16) . . . . ?
C10 C11 C12 C8 0(3) . . . . ?

_refine_diff_density_max         2.967
_refine_diff_density_min         -2.911
_refine_diff_density_rms         0.469

_shelxl_version_number           2014-3

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_3
_database_code_depnum_ccdc_archive 'CCDC 1818606'
_audit_update_record             
;
2018-06-07 deposited with the CCDC.
2018-06-08 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C24 H54 K N4 O65 P Sm2 Ti2 W10'
_chemical_formula_weight         3743.78

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'
Sm Sm -0.1638 3.4418 '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'
Ti Ti 0.2776 0.4457 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
K K 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           12
_space_group_name_H-M_alt        'C 2/m'
_space_group_name_Hall           '-C 2y'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z'
'-x, -y, -z'
'x, -y, z'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z'

_cell_length_a                   21.889(4)
_cell_length_b                   30.183(6)
_cell_length_c                   15.327(3)
_cell_angle_alpha                90
_cell_angle_beta                 133.421(2)
_cell_angle_gamma                90
_cell_volume                     7355(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    19022
_cell_measurement_theta_min      1.490
_cell_measurement_theta_max      25.00

_exptl_crystal_description       'block '
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    3.381
_exptl_crystal_F_000             6752
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.11
_exptl_absorpt_coefficient_mu    17.539
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.048
_exptl_absorpt_correction_T_max  0.145
_exptl_absorpt_process_details   'SADABS; Sheldrick, 1996'

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'Bruker Smart Apex CCD'
_diffrn_measurement_method       ω-2θ
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            19022
_diffrn_reflns_av_unetI/netI     0.0982
_diffrn_reflns_av_R_equivalents  0.0867
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_k_max       35
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         1.490
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measured_fraction_theta_full 0.966
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_Laue_measured_fraction_full 0.966
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_point_group_measured_fraction_full 0.966
_reflns_number_total             6577
_reflns_number_gt                5214
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
During the refinement, the command 'omit -3 50' was used to omit the weak reflections above 50 degree.
In the structure, there are two disordered W sites (W5, W6). W(5) site is occupied by W and Ti atom with
 occupancy factors of 0.8 and 0.2. W(6) site is occupied  by W and Ti atom with occupancy factors of
 0.2 and 0.8. Some O atoms on the polyoxoanions, C atoms on the organic ligands, water molecules and P1 atom
 are retrained with the command 'isor', which leds to a  restraint value of 144. Rint after the absorption 
correction process is 0.0867, which indicates that the absorption correction process is effective.
In the final refinement, 4 crystal water  molecules are determined  from the residual peaks with reasonable positions and thermal parameters.
 The highest residual peak is close to Sm(2) with the distance of 1.26 A, indicative an featureless peak.
 These largest residual peak are mainly due to the series termination errors. 
;

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXS-2014 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
;
 ?
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0659P)²+203.1434P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         6577
_refine_ls_number_parameters     524
_refine_ls_number_restraints     144
_refine_ls_R_factor_all          0.0719
_refine_ls_R_factor_gt           0.0573
_refine_ls_wR_factor_ref         0.1564
_refine_ls_wR_factor_gt          0.1450
_refine_ls_goodness_of_fit_ref   1.020
_refine_ls_restrained_S_all      1.020
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
W1 W 0.41615(4) 0.23948(2) 0.55422(6) 0.01723(18) Uani 1 1 d . . . . .
W2 W 0.35903(4) 0.24037(2) 0.28287(6) 0.01804(19) Uani 1 1 d . . . . .
W3 W 0.28531(4) 0.32233(2) 0.34778(6) 0.01567(18) Uani 1 1 d . . . . .
W4 W 0.44419(4) 0.32833(2) 0.21935(5) 0.01480(18) Uani 1 1 d . . . . .
W5 W 0.42648(5) 0.40928(2) 0.57103(6) 0.0139(2) Uani 0.8 1 d . . P A 1
Ti1 Ti 0.42648(5) 0.40928(2) 0.57103(6) 0.0139(2) Uani 0.2 1 d . . P A 2
W6 W 0.37091(10) 0.40805(5) 0.28465(13) 0.0093(3) Uani 0.2 1 d . . P A 3
Ti2 Ti 0.37091(10) 0.40805(5) 0.28465(13) 0.0093(3) Uani 0.8 1 d . . P A 4
Sm1 Sm 0.18751(7) 0.5000 0.11798(11) 0.0206(3) Uani 1 2 d S T P A .
Sm2 Sm 0.28500(9) 0.5000 0.57979(13) 0.0319(3) Uani 1 2 d S T P A .
K1 K 0.3988(5) 0.5000 0.1556(7) 0.0555(19) Uani 1 2 d S T P A .
P1 P 0.5000 0.32489(17) 0.5000 0.0089(11) Uani 1 2 d S TU P A .
O1 O 0.4813(6) 0.3540(3) 0.4024(9) 0.015(2) Uani 1 1 d . U . . .
O2 O 0.4240(6) 0.2945(3) 0.4446(8) 0.013(2) Uani 1 1 d . . . . .
O3 O 0.3952(7) 0.2003(4) 0.6120(10) 0.025(3) Uani 1 1 d . U . . .
O4 O 0.3021(8) 0.2018(4) 0.1727(11) 0.032(3) Uani 1 1 d . . . . .
O5 O 0.3730(7) 0.2116(3) 0.4097(10) 0.022(2) Uani 1 1 d . . . . .
O6 O 0.4195(8) 0.3165(4) 0.0903(10) 0.025(3) Uani 1 1 d . . . . .
O7 O 0.2745(7) 0.2741(3) 0.2519(9) 0.022(2) Uani 1 1 d . . . . .
O8 O 0.5326(7) 0.4356(4) 0.6700(9) 0.020(2) Uani 1 1 d . U . . .
O9 O 0.2960(7) 0.4466(3) 0.1878(9) 0.019(2) Uani 1 1 d . . . . .
O10 O 0.1821(7) 0.3295(4) 0.2750(10) 0.023(3) Uani 1 1 d . . . . .
O11 O 0.3990(6) 0.4238(3) 0.4302(9) 0.017(2) Uani 1 1 d . . . . .
O12 O 0.2992(6) 0.3622(3) 0.2698(8) 0.016(2) Uani 1 1 d . . . . .
O13 O 0.3696(6) 0.4481(4) 0.5746(9) 0.021(2) Uani 1 1 d . U . . .
O14 O 0.5292(7) 0.2846(4) 0.3251(9) 0.022(3) Uani 1 1 d . . . . .
O15 O 0.3645(6) 0.3705(3) 0.1704(9) 0.018(2) Uani 1 1 d . . . . .
O16 O 0.3144(7) 0.2740(3) 0.4600(9) 0.020(2) Uani 1 1 d . . . . .
O17 O 0.5265(6) 0.3720(3) 0.2855(9) 0.016(2) Uani 1 1 d . U . . .
O18 O 0.5263(6) 0.2242(4) 0.6262(9) 0.017(2) Uani 1 1 d . U . . .
O19 O 0.3733(6) 0.2854(4) 0.2117(9) 0.021(2) Uani 1 1 d . . . . .
O20 O 0.3463(7) 0.3604(3) 0.4824(9) 0.020(2) Uani 1 1 d . . . . .
O21 O 0.0936(9) 0.4479(4) -0.0374(13) 0.045(4) Uani 1 1 d . . . . .
O22 O -0.0334(9) 0.4198(5) -0.1397(16) 0.061(4) Uani 1 1 d . U . . .
O23 O 0.2856(10) 0.4397(5) 0.6733(14) 0.051(4) Uani 1 1 d . . . . .
O24 O 0.3275(16) 0.4231(7) 0.850(2) 0.098(7) Uani 1 1 d . U . . .
C1 C 0.0439(11) 0.4164(6) -0.0793(17) 0.028(4) Uani 1 1 d . U . . .
C2 C 0.0778(11) 0.3709(6) -0.0637(15) 0.029(4) Uani 1 1 d . . . . .
C3 C 0.1623(11) 0.3652(6) 0.0015(17) 0.034(4) Uani 1 1 d . U . . .
H3A H 0.1985 0.3893 0.0325 0.040 Uiso 1 1 calc R U . . .
C4 C 0.1437(13) 0.2869(6) -0.0253(16) 0.033(5) Uani 1 1 d . . . . .
H4A H 0.1685 0.2592 -0.0079 0.040 Uiso 1 1 calc R U . . .
C5 C 0.0603(12) 0.2910(7) -0.0952(18) 0.040(5) Uani 1 1 d . . . . .
H5A H 0.0260 0.2660 -0.1306 0.048 Uiso 1 1 calc R U . . .
C6 C 0.0247(12) 0.3332(6) -0.115(2) 0.041(5) Uani 1 1 d . . . . .
H6A H -0.0326 0.3362 -0.1607 0.050 Uiso 1 1 calc R U . . .
C7 C 0.3085(15) 0.4123(8) 0.753(2) 0.048(6) Uani 1 1 d . U . . .
C8 C 0.3176(13) 0.3661(7) 0.7397(17) 0.039(5) Uani 1 1 d . U . . .
C9 C 0.3014(12) 0.3507(7) 0.6409(17) 0.035(4) Uani 1 1 d . . . . .
H9A H 0.2793 0.3701 0.5780 0.042 Uiso 1 1 calc R U . . .
C10 C 0.3466(12) 0.2792(7) 0.7165(18) 0.037(5) Uani 1 1 d . U . . .
H10A H 0.3575 0.2504 0.7084 0.045 Uiso 1 1 calc R U . . .
C11 C 0.3615(13) 0.2923(7) 0.8169(18) 0.045(5) Uani 1 1 d . U . . .
H11A H 0.3810 0.2718 0.8767 0.054 Uiso 1 1 calc R U . . .
C12 C 0.3477(16) 0.3343(7) 0.8273(18) 0.054(7) Uani 1 1 d . . . . .
H12A H 0.3586 0.3425 0.8953 0.065 Uiso 1 1 calc R U . . .
N1 N 0.1898(10) 0.3239(5) 0.0183(15) 0.041(4) Uani 1 1 d . . . . .
H1A H 0.2429 0.3207 0.0619 0.049 Uiso 1 1 calc R U . . .
N2 N 0.3159(10) 0.3099(6) 0.6327(15) 0.041(4) Uani 1 1 d . . . . .
H2A H 0.3050 0.3023 0.5691 0.050 Uiso 1 1 calc R U . . .
O1W O 0.0843(11) 0.5000 0.1310(18) 0.038(5) Uani 1 2 d S T P . .
H1WA H 0.0368 0.5178 0.0797 0.046 Uiso 0.5 1 calc R U P A .
H1WB H 0.0918 0.4822 0.1872 0.046 Uiso 0.5 1 calc R U P . .
O2W O 0.2888(10) 0.5000 0.3419(14) 0.025(4) Uani 1 2 d S TU P . .
H2WA H 0.3415 0.5000 0.3838 0.030 Uiso 1 2 d R U P A .
H2WB H 0.2707 0.5000 0.3763 0.030 Uiso 1 2 d R U P . .
O3W O 0.2134(11) 0.5000 -0.0157(15) 0.027(4) Uani 1 2 d S T P A .
O4W O 0.1814(9) 0.4283(4) 0.2090(13) 0.047(4) Uani 1 1 d . . . . .
H4WA H 0.2193 0.4086 0.2411 0.056 Uiso 1 1 d R U . A .
H4WB H 0.1417 0.4248 0.2064 0.056 Uiso 1 1 d R U . . .
O6W O 0.1482(14) 0.5000 0.518(2) 0.070(7) Uani 1 2 d S T P . .
H6WA H 0.1169 0.4772 0.4848 0.084 Uiso 0.5 1 d R U P A .
H6WB H 0.1319 0.5228 0.5298 0.084 Uiso 0.5 1 d R U P . .
O7W O 0.1926(11) 0.4505(7) 0.4096(16) 0.085(6) Uani 1 1 d . . . . .
H7WA H 0.2133 0.4308 0.3966 0.101 Uiso 1 1 d R U . A .
H7WB H 0.1396 0.4528 0.3629 0.101 Uiso 1 1 d R U . . .
OW1 O 0.087(2) 0.3937(10) 0.389(3) 0.071(10) Uani 0.5 1 d . U P . .
OW2 O 0.497(3) 0.0000 1.287(4) 0.167(17) Uani 1 2 d S TU P . .
OW3 O 0.4838(18) 0.5728(8) 0.095(2) 0.127(9) Uani 1 1 d . U . . .
OW4 O 0.2626(19) 0.5807(9) -0.047(2) 0.133(9) Uani 1 1 d . U . . .
OW5 O 0.327(4) 0.5000 -0.082(4) 0.079(15) Uani 0.5 2 d S TU P A .
OW6 O -0.088(4) 0.414(2) 0.267(6) 0.16(2) Uani 0.5 1 d . U P . .
OW7 O 0.128(4) 0.5000 0.676(6) 0.10(2) Uani 0.5 2 d S TU P . .
O5W O 0.4048(17) 0.5000 0.750(3) 0.080(7) Uani 1 2 d S TU P . .
H5WA H 0.4201 0.5217 0.8054 0.096 Uiso 0.5 1 calc R U P A .
H5WB H 0.4433 0.4783 0.7716 0.096 Uiso 0.5 1 calc R U P . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
W1 O3 1.718(10) . ?
W1 O18 1.895(10) . ?
W1 O5 1.905(11) . ?
W1 O14 1.915(11) 2_656 ?
W1 O16 1.927(11) . ?
W1 O2 2.450(10) . ?
W2 O4 1.693(12) . ?
W2 O7 1.866(11) . ?
W2 O19 1.897(11) . ?
W2 O18 1.916(10) 2_656 ?
W2 O5 1.951(10) . ?
W2 O2 2.446(9) . ?
W3 O10 1.711(11) . ?
W3 O12 1.862(10) . ?
W3 O20 1.890(11) . ?
W3 O7 1.963(10) . ?
W3 O16 1.995(10) . ?
W3 O2 2.436(10) . ?
W4 O6 1.692(11) . ?
W4 O15 1.851(10) . ?
W4 O17 1.870(10) . ?
W4 O14 1.919(11) . ?
W4 O19 1.964(11) . ?
W4 O1 2.449(9) . ?
W5 O13 1.738(11) . ?
W5 O11 1.851(10) . ?
W5 O8 1.867(11) . ?
W5 O20 1.956(11) . ?
W5 O17 2.013(10) 2_656 ?
W5 O1 2.427(10) 2_656 ?
W6 O9 1.703(10) . ?
W6 O8 1.903(11) 2_656 ?
W6 O11 1.923(10) . ?
W6 O12 1.985(10) . ?
W6 O15 2.008(10) . ?
W6 O1 2.400(10) . ?
W6 K1 3.695(5) . ?
Sm1 O21 2.374(14) 6_565 ?
Sm1 O21 2.374(14) . ?
Sm1 O1W 2.401(17) . ?
Sm1 O9 2.426(10) 6_565 ?
Sm1 O9 2.426(10) . ?
Sm1 O3W 2.473(15) . ?
Sm1 O2W 2.497(16) . ?
Sm1 O4W 2.627(13) 6_565 ?
Sm1 O4W 2.627(13) . ?
Sm1 K1 4.250(8) . ?
Sm2 O5W 2.07(3) . ?
Sm2 O23 2.310(14) 6_565 ?
Sm2 O23 2.310(14) . ?
Sm2 O7W 2.424(18) . ?
Sm2 O7W 2.424(18) 6_565 ?
Sm2 O6W 2.44(2) . ?
Sm2 O13 2.468(11) . ?
Sm2 O13 2.468(11) 6_565 ?
K1 O8 2.767(12) 5_666 ?
K1 O8 2.767(12) 2_656 ?
K1 OW5 2.80(4) . ?
K1 O3W 2.95(2) . ?
K1 O9 3.072(12) . ?
K1 O9 3.072(12) 6_565 ?
K1 OW3 3.39(3) 6_565 ?
K1 OW3 3.39(3) . ?
K1 OW4 3.43(3) 6_565 ?
K1 OW4 3.43(3) . ?
P1 O1 1.529(10) 2_656 ?
P1 O1 1.529(10) . ?
P1 O2 1.546(10) . ?
P1 O2 1.546(10) 2_656 ?
O1 Ti1 2.427(10) 2_656 ?
O1 W5 2.427(10) 2_656 ?
O8 Ti2 1.903(11) 2_656 ?
O8 W6 1.903(11) 2_656 ?
O8 K1 2.767(12) 5_666 ?
O14 W1 1.915(11) 2_656 ?
O17 Ti1 2.013(10) 2_656 ?
O17 W5 2.013(10) 2_656 ?
O18 W2 1.916(10) 2_656 ?
O21 C1 1.24(2) . ?
O22 C1 1.26(2) . ?
O23 C7 1.26(2) . ?
O24 C7 1.29(3) . ?
C1 C2 1.50(2) . ?
C2 C3 1.38(2) . ?
C2 C6 1.42(2) . ?
C3 N1 1.33(2) . ?
C4 N1 1.34(2) . ?
C4 C5 1.34(3) . ?
C5 C6 1.41(3) . ?
C7 C8 1.44(3) . ?
C8 C9 1.38(3) . ?
C8 C12 1.39(3) . ?
C9 N2 1.30(3) . ?
C10 N2 1.33(3) . ?
C10 C11 1.39(3) . ?
C11 C12 1.34(3) . ?

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
_geom_angle_publ_flag
O3 W1 O18 102.5(5) . . ?
O3 W1 O5 101.6(5) . . ?
O18 W1 O5 89.1(4) . . ?
O3 W1 O14 101.7(5) . 2_656 ?
O18 W1 O14 84.9(4) . 2_656 ?
O5 W1 O14 156.7(4) . 2_656 ?
O3 W1 O16 100.3(5) . . ?
O18 W1 O16 157.1(4) . . ?
O5 W1 O16 88.5(5) . . ?
O14 W1 O16 88.4(4) 2_656 . ?
O3 W1 O2 171.5(4) . . ?
O18 W1 O2 84.5(4) . . ?
O5 W1 O2 73.4(4) . . ?
O14 W1 O2 83.6(4) 2_656 . ?
O16 W1 O2 73.1(4) . . ?
O4 W2 O7 101.5(5) . . ?
O4 W2 O19 102.6(5) . . ?
O7 W2 O19 89.4(5) . . ?
O4 W2 O18 104.4(5) . 2_656 ?
O7 W2 O18 154.0(4) . 2_656 ?
O19 W2 O18 87.1(4) . 2_656 ?
O4 W2 O5 101.1(5) . . ?
O7 W2 O5 86.9(5) . . ?
O19 W2 O5 156.3(4) . . ?
O18 W2 O5 86.1(4) 2_656 . ?
O4 W2 O2 170.4(5) . . ?
O7 W2 O2 71.2(4) . . ?
O19 W2 O2 83.9(4) . . ?
O18 W2 O2 82.8(4) 2_656 . ?
O5 W2 O2 72.7(4) . . ?
O10 W3 O12 103.0(5) . . ?
O10 W3 O20 105.1(5) . . ?
O12 W3 O20 90.2(4) . . ?
O10 W3 O7 100.4(5) . . ?
O12 W3 O7 89.3(5) . . ?
O20 W3 O7 154.0(5) . . ?
O10 W3 O16 98.7(5) . . ?
O12 W3 O16 158.2(4) . . ?
O20 W3 O16 86.3(4) . . ?
O7 W3 O16 84.7(4) . . ?
O10 W3 O2 167.1(4) . . ?
O12 W3 O2 85.9(4) . . ?
O20 W3 O2 84.0(4) . . ?
O7 W3 O2 70.0(4) . . ?
O16 W3 O2 72.4(4) . . ?
O6 W4 O15 102.5(5) . . ?
O6 W4 O17 101.4(5) . . ?
O15 W4 O17 91.3(4) . . ?
O6 W4 O14 100.8(5) . . ?
O15 W4 O14 155.7(4) . . ?
O17 W4 O14 90.7(4) . . ?
O6 W4 O19 100.8(5) . . ?
O15 W4 O19 86.8(5) . . ?
O17 W4 O19 157.7(4) . . ?
O14 W4 O19 82.2(4) . . ?
O6 W4 O1 173.7(4) . . ?
O15 W4 O1 74.0(4) . . ?
O17 W4 O1 73.6(4) . . ?
O14 W4 O1 83.4(4) . . ?
O19 W4 O1 84.5(4) . . ?
O13 W5 O11 102.2(5) . . ?
O13 W5 O8 101.8(5) . . ?
O11 W5 O8 94.2(4) . . ?
O13 W5 O20 102.2(5) . . ?
O11 W5 O20 87.2(4) . . ?
O8 W5 O20 155.1(4) . . ?
O13 W5 O17 100.5(5) . 2_656 ?
O11 W5 O17 156.7(4) . 2_656 ?
O8 W5 O17 86.2(4) . 2_656 ?
O20 W5 O17 83.0(4) . 2_656 ?
O13 W5 O1 171.6(4) . 2_656 ?
O11 W5 O1 85.7(4) . 2_656 ?
O8 W5 O1 74.3(4) . 2_656 ?
O20 W5 O1 81.0(4) . 2_656 ?
O17 W5 O1 72.0(4) 2_656 2_656 ?
O9 W6 O8 100.5(5) . 2_656 ?
O9 W6 O11 101.0(5) . . ?
O8 W6 O11 94.5(4) 2_656 . ?
O9 W6 O12 99.5(5) . . ?
O8 W6 O12 159.9(4) 2_656 . ?
O11 W6 O12 84.4(4) . . ?
O9 W6 O15 100.2(5) . . ?
O8 W6 O15 87.7(4) 2_656 . ?
O11 W6 O15 157.9(4) . . ?
O12 W6 O15 86.1(4) . . ?
O9 W6 O1 171.2(4) . . ?
O8 W6 O1 74.4(4) 2_656 . ?
O11 W6 O1 86.7(4) . . ?
O12 W6 O1 85.4(4) . . ?
O15 W6 O1 72.7(4) . . ?
O9 W6 K1 55.6(4) . . ?
O8 W6 K1 46.9(3) 2_656 . ?
O11 W6 K1 113.4(3) . . ?
O12 W6 K1 150.6(3) . . ?
O15 W6 K1 84.0(3) . . ?
O1 W6 K1 117.5(3) . . ?
O21 Sm1 O21 82.9(7) 6_565 . ?
O21 Sm1 O1W 82.4(5) 6_565 . ?
O21 Sm1 O1W 82.4(5) . . ?
O21 Sm1 O9 85.0(4) 6_565 6_565 ?
O21 Sm1 O9 142.4(4) . 6_565 ?
O1W Sm1 O9 130.9(3) . 6_565 ?
O21 Sm1 O9 142.4(4) 6_565 . ?
O21 Sm1 O9 85.0(4) . . ?
O1W Sm1 O9 130.9(3) . . ?
O9 Sm1 O9 83.3(5) 6_565 . ?
O21 Sm1 O3W 72.7(5) 6_565 . ?
O21 Sm1 O3W 72.7(5) . . ?
O1W Sm1 O3W 146.5(6) . . ?
O9 Sm1 O3W 69.7(4) 6_565 . ?
O9 Sm1 O3W 69.7(4) . . ?
O21 Sm1 O2W 135.8(4) 6_565 . ?
O21 Sm1 O2W 135.8(4) . . ?
O1W Sm1 O2W 83.3(6) . . ?
O9 Sm1 O2W 73.6(4) 6_565 . ?
O9 Sm1 O2W 73.6(4) . . ?
O3W Sm1 O2W 130.2(5) . . ?
O21 Sm1 O4W 70.3(5) 6_565 6_565 ?
O21 Sm1 O4W 138.8(4) . 6_565 ?
O1W Sm1 O4W 64.0(4) . 6_565 ?
O9 Sm1 O4W 67.0(4) 6_565 6_565 ?
O9 Sm1 O4W 134.8(4) . 6_565 ?
O3W Sm1 O4W 124.3(3) . 6_565 ?
O2W Sm1 O4W 65.9(4) . 6_565 ?
O21 Sm1 O4W 138.8(4) 6_565 . ?
O21 Sm1 O4W 70.3(5) . . ?
O1W Sm1 O4W 64.0(4) . . ?
O9 Sm1 O4W 134.8(4) 6_565 . ?
O9 Sm1 O4W 67.0(4) . . ?
O3W Sm1 O4W 124.3(3) . . ?
O2W Sm1 O4W 65.9(4) . . ?
O4W Sm1 O4W 110.9(7) 6_565 . ?
O21 Sm1 K1 104.3(3) 6_565 . ?
O21 Sm1 K1 104.3(3) . . ?
O1W Sm1 K1 170.9(5) . . ?
O9 Sm1 K1 45.3(2) 6_565 . ?
O9 Sm1 K1 45.3(2) . . ?
O3W Sm1 K1 42.6(4) . . ?
O2W Sm1 K1 87.6(4) . . ?
O4W Sm1 K1 112.1(3) 6_565 . ?
O4W Sm1 K1 112.1(3) . . ?
O5W Sm2 O23 75.8(5) . 6_565 ?
O5W Sm2 O23 75.8(5) . . ?
O23 Sm2 O23 103.9(7) 6_565 . ?
O5W Sm2 O7W 139.0(5) . . ?
O23 Sm2 O7W 142.9(6) 6_565 . ?
O23 Sm2 O7W 80.0(6) . . ?
O5W Sm2 O7W 139.0(5) . 6_565 ?
O23 Sm2 O7W 80.0(6) 6_565 6_565 ?
O23 Sm2 O7W 142.9(6) . 6_565 ?
O7W Sm2 O7W 76.1(10) . 6_565 ?
O5W Sm2 O6W 129.9(8) . . ?
O23 Sm2 O6W 73.9(5) 6_565 . ?
O23 Sm2 O6W 73.9(5) . . ?
O7W Sm2 O6W 71.9(6) . . ?
O7W Sm2 O6W 71.9(6) 6_565 . ?
O5W Sm2 O13 73.3(5) . . ?
O23 Sm2 O13 146.6(5) 6_565 . ?
O23 Sm2 O13 80.6(4) . . ?
O7W Sm2 O13 70.3(5) . . ?
O7W Sm2 O13 116.5(5) 6_565 . ?
O6W Sm2 O13 137.3(3) . . ?
O5W Sm2 O13 73.3(5) . 6_565 ?
O23 Sm2 O13 80.6(4) 6_565 6_565 ?
O23 Sm2 O13 146.6(5) . 6_565 ?
O7W Sm2 O13 116.5(5) . 6_565 ?
O7W Sm2 O13 70.3(5) 6_565 6_565 ?
O6W Sm2 O13 137.3(3) . 6_565 ?
O13 Sm2 O13 78.7(5) . 6_565 ?
O8 K1 O8 89.2(5) 5_666 2_656 ?
O8 K1 OW5 134.6(3) 5_666 . ?
O8 K1 OW5 134.6(3) 2_656 . ?
O8 K1 O3W 111.1(4) 5_666 . ?
O8 K1 O3W 111.1(4) 2_656 . ?
OW5 K1 O3W 69.0(12) . . ?
O8 K1 O9 100.6(4) 5_666 . ?
O8 K1 O9 56.4(3) 2_656 . ?
OW5 K1 O9 112.8(10) . . ?
O3W K1 O9 55.4(3) . . ?
O8 K1 O9 56.4(3) 5_666 6_565 ?
O8 K1 O9 100.6(4) 2_656 6_565 ?
OW5 K1 O9 112.8(10) . 6_565 ?
O3W K1 O9 55.4(3) . 6_565 ?
O9 K1 O9 63.3(4) . 6_565 ?
O8 K1 OW3 133.1(6) 5_666 6_565 ?
O8 K1 OW3 76.9(4) 2_656 6_565 ?
OW5 K1 OW3 64.6(9) . 6_565 ?
O3W K1 OW3 115.7(5) . 6_565 ?
O9 K1 OW3 107.7(4) . 6_565 ?
O9 K1 OW3 169.5(5) 6_565 6_565 ?
O8 K1 OW3 76.9(4) 5_666 . ?
O8 K1 OW3 133.1(6) 2_656 . ?
OW5 K1 OW3 64.6(9) . . ?
O3W K1 OW3 115.7(5) . . ?
O9 K1 OW3 169.5(5) . . ?
O9 K1 OW3 107.7(4) 6_565 . ?
OW3 K1 OW3 80.8(8) 6_565 . ?
O8 K1 OW4 158.6(5) 5_666 6_565 ?
O8 K1 OW4 86.2(5) 2_656 6_565 ?
OW5 K1 OW4 57.3(8) . 6_565 ?
O3W K1 OW4 52.1(5) . 6_565 ?
O9 K1 OW4 59.7(5) . 6_565 ?
O9 K1 OW4 104.0(5) 6_565 6_565 ?
OW3 K1 OW4 65.9(6) 6_565 6_565 ?
OW3 K1 OW4 120.8(6) . 6_565 ?
O8 K1 OW4 86.2(5) 5_666 . ?
O8 K1 OW4 158.6(5) 2_656 . ?
OW5 K1 OW4 57.3(8) . . ?
O3W K1 OW4 52.1(5) . . ?
O9 K1 OW4 104.0(5) . . ?
O9 K1 OW4 59.7(5) 6_565 . ?
OW3 K1 OW4 120.8(6) 6_565 . ?
OW3 K1 OW4 65.9(6) . . ?
OW4 K1 OW4 90.6(9) 6_565 . ?
O8 K1 W6 100.9(3) 5_666 . ?
O8 K1 W6 30.1(2) 2_656 . ?
OW5 K1 W6 122.9(5) . . ?
O3W K1 W6 81.0(2) . . ?
O9 K1 W6 27.2(2) . . ?
O9 K1 W6 84.2(3) 6_565 . ?
OW3 K1 W6 89.0(4) 6_565 . ?
OW3 K1 W6 162.9(5) . . ?
OW4 K1 W6 65.8(4) 6_565 . ?
OW4 K1 W6 131.2(5) . . ?
O1 P1 O1 109.8(8) 2_656 . ?
O1 P1 O2 110.1(5) 2_656 . ?
O1 P1 O2 109.9(5) . . ?
O1 P1 O2 109.9(5) 2_656 2_656 ?
O1 P1 O2 110.0(5) . 2_656 ?
O2 P1 O2 107.1(8) . 2_656 ?
P1 O1 W6 125.5(5) . . ?
P1 O1 Ti1 126.8(5) . 2_656 ?
P1 O1 W5 126.8(5) . 2_656 ?
P1 O1 W4 126.4(6) . . ?
W6 O1 W4 89.1(3) . . ?
Ti1 O1 W4 89.6(3) 2_656 . ?
W5 O1 W4 89.6(3) 2_656 . ?
P1 O2 W3 123.3(6) . . ?
P1 O2 W2 127.6(5) . . ?
W3 O2 W2 90.0(3) . . ?
P1 O2 W1 125.6(5) . . ?
W3 O2 W1 90.3(3) . . ?
W2 O2 W1 88.7(3) . . ?
W1 O5 W2 125.1(5) . . ?
W2 O7 W3 128.8(6) . . ?
W5 O8 K1 129.1(5) . 5_666 ?
Ti2 O8 K1 103.0(5) 2_656 5_666 ?
W6 O8 K1 103.0(5) 2_656 5_666 ?
W6 O9 Sm1 154.5(5) . . ?
W6 O9 K1 97.2(4) . . ?
Sm1 O9 K1 100.6(4) . . ?
W3 O12 W6 147.4(5) . . ?
W5 O13 Sm2 176.9(6) . . ?
W1 O14 W4 154.7(6) 2_656 . ?
W4 O15 W6 123.6(5) . . ?
W1 O16 W3 124.2(5) . . ?
W4 O17 Ti1 124.4(5) . 2_656 ?
W4 O17 W5 124.4(5) . 2_656 ?
W1 O18 W2 150.2(6) . 2_656 ?
W2 O19 W4 151.0(6) . . ?
W3 O20 W5 147.1(6) . . ?
C1 O21 Sm1 150.8(14) . . ?
C7 O23 Sm2 161.4(16) . . ?
O21 C1 O22 125.2(17) . . ?
O21 C1 C2 117.2(16) . . ?
O22 C1 C2 117.4(16) . . ?
C3 C2 C6 118.8(17) . . ?
C3 C2 C1 119.9(16) . . ?
C6 C2 C1 121.3(16) . . ?
N1 C3 C2 117.4(18) . . ?
N1 C4 C5 117.8(18) . . ?
C4 C5 C6 120.0(18) . . ?
C5 C6 C2 118.9(17) . . ?
O23 C7 O24 124(2) . . ?
O23 C7 C8 120.1(18) . . ?
O24 C7 C8 116(2) . . ?
C9 C8 C12 115(2) . . ?
C9 C8 C7 121.6(18) . . ?
C12 C8 C7 123.4(18) . . ?
N2 C9 C8 122.1(19) . . ?
N2 C10 C11 117(2) . . ?
C12 C11 C10 120.0(19) . . ?
C11 C12 C8 122(2) . . ?
C3 N1 C4 126.9(17) . . ?
C9 N2 C10 124.1(18) . . ?
Sm1 O3W K1 102.8(6) . . ?

_refine_diff_density_max         6.541
_refine_diff_density_min         -3.918
_refine_diff_density_rms         0.441

_shelxl_version_number           2014-3

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_11
_database_code_depnum_ccdc_archive 'CCDC 1818609'
_audit_update_record             
;
2018-06-07 deposited with the CCDC.
2018-06-08 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C21 H49.50 K N3.50 Nd2 O62 P W11'
_chemical_formula_weight         3723.93

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'
Nd Nd -0.1943 3.0179 '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'
K K 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   13.0716(6)
_cell_length_b                   14.3465(7)
_cell_length_c                   21.2358(11)
_cell_angle_alpha                84.449(3)
_cell_angle_beta                 89.313(3)
_cell_angle_gamma                84.531(3)
_cell_volume                     3945.7(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    37497
_cell_measurement_theta_min      1.565
_cell_measurement_theta_max      25.00

_exptl_crystal_description       'block '
_exptl_crystal_colour            'light purple'
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    3.134
_exptl_crystal_F_000             3327
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.11
_exptl_absorpt_coefficient_mu    17.428
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.054
_exptl_absorpt_correction_T_max  0.147
_exptl_absorpt_process_details   'SADABS; Sheldrick, 1996'

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'Bruker Smart Apex CCD'
_diffrn_measurement_method       ω-2θ
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            37497
_diffrn_reflns_av_unetI/netI     0.1135
_diffrn_reflns_av_R_equivalents  0.0813
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         1.565
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measured_fraction_theta_full 0.970
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_Laue_measured_fraction_full 0.970
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_point_group_measured_fraction_full 0.970
_reflns_number_total             13851
_reflns_number_gt                8867
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
During the refinement, the command 'omit -3 50' was used to omit the weak reflections above 50 degree.
 In the structure, there are two disordered cationic groups [Nd(2)(H2O)6] and [Nd(2a)(H2O)6] with
 50% site-occupancies for each.Some O atoms on the polyoxoanions, C, N and O atoms on the organic ligands, and coordinated water molecules
are retrained with the command 'isor', which leds to a  restraint value of 276. Rint after the absorption
 correction process is 0.0813, which indicates that the absorption correction process is effective.
 In the final refinement,'squeeze' command was used to deal with the water molecules of solvation.The highest
 residual peak is close to W(6) with the distance of 0.77 A, indicative an featureless peak. The largest residual peak
is mainly due to the series termination errors. The deepest hole is  close to the heavy metal center W(4). 
;

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXS-2014 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
;
 ?
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1290P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         13851
_refine_ls_number_parameters     884
_refine_ls_number_restraints     276
_refine_ls_R_factor_all          0.1144
_refine_ls_R_factor_gt           0.0808
_refine_ls_wR_factor_ref         0.2449
_refine_ls_wR_factor_gt          0.2179
_refine_ls_goodness_of_fit_ref   1.098
_refine_ls_restrained_S_all      1.101
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000

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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
W1 W 1.43481(8) 0.14490(10) 0.18225(6) 0.0652(4) Uani 1 1 d . . . . .
W2 W 1.29223(6) 0.00626(7) 0.30769(5) 0.0408(3) Uani 1 1 d . . . . .
W3 W 1.34243(9) 0.37109(10) 0.13278(5) 0.0680(4) Uani 1 1 d . . . . .
W4 W 1.34439(8) 0.43250(8) 0.29794(5) 0.0524(3) Uani 1 1 d . . . . .
W5 W 0.97878(8) 0.29484(8) 0.16530(5) 0.0503(3) Uani 1 1 d . . . . .
W6 W 1.21382(9) 0.18648(11) 0.09537(5) 0.0700(4) Uani 1 1 d . U . . .
W7 W 1.43546(7) 0.20634(8) 0.34555(5) 0.0461(3) Uani 1 1 d . . . . .
W8 W 1.21167(6) 0.29891(6) 0.41320(4) 0.0333(2) Uani 1 1 d . . . . .
W9 W 1.10429(8) 0.47744(8) 0.20403(5) 0.0532(3) Uani 1 1 d . . . . .
W10 W 1.07341(7) 0.04948(7) 0.22419(4) 0.0421(3) Uani 1 1 d . . . . .
W11 W 0.97683(7) 0.34158(6) 0.32109(4) 0.0367(3) Uani 1 1 d . . . . .
Nd1 Nd 1.04331(8) 0.07267(7) 0.40890(5) 0.0279(3) Uani 1 1 d . . . . .
Nd2 Nd 0.8470(3) -0.1232(5) 0.1848(3) 0.071(2) Uani 0.5 1 d . . P A 1
O3W O 0.709(4) -0.166(3) 0.249(2) 0.103(15) Uani 0.5 1 d . U P A 1
H3WA H 0.7139 -0.2193 0.2711 0.124 Uiso 0.5 1 d R U P A 1
H3WB H 0.6539 -0.1297 0.2504 0.124 Uiso 0.5 1 d R U P A 1
O1W O 0.9110(16) -0.0898(16) 0.0818(11) 0.090(6) Uani 0.5 1 d . U P A 1
O2W O 0.8953(13) -0.1104(12) 0.2969(8) 0.057(4) Uani 0.5 1 d . U P A 1
O6W O 0.706(3) -0.131(3) 0.1108(17) 0.170(13) Uani 0.5 1 d . U P A 1
O5W O 0.875(3) -0.300(3) 0.255(2) 0.217(18) Uani 0.5 1 d . U P A 1
O7W O 0.776(3) -0.254(3) 0.122(2) 0.206(16) Uani 0.5 1 d . U P A 1
Nd2A Nd 0.8912(5) -0.1395(4) 0.1814(3) 0.0830(17) Uani 0.5 1 d . U P A 2
O4W O 1.041(4) -0.217(4) 0.186(3) 0.131(19) Uani 0.5 1 d . U P A 2
H4WA H 1.0570 -0.2586 0.1612 0.157 Uiso 0.5 1 d R U P A 2
H4WB H 1.0844 -0.2051 0.2133 0.157 Uiso 0.5 1 d R U P A 2
O1X O 0.9110(16) -0.0898(16) 0.0818(11) 0.090(6) Uani 0.5 1 d . U P A 2
O2X O 0.8953(13) -0.1104(12) 0.2969(8) 0.057(4) Uani 0.5 1 d . U P A 2
O6X O 0.706(3) -0.131(3) 0.1108(17) 0.170(13) Uani 0.5 1 d . U P A 2
O5X O 0.875(3) -0.300(3) 0.255(2) 0.217(18) Uani 0.5 1 d . U P A 2
O7X O 0.776(3) -0.254(3) 0.122(2) 0.206(16) Uani 0.5 1 d . U P A 2
P1 P 1.2072(4) 0.2410(4) 0.2541(2) 0.0294(13) Uani 1 1 d . . . . .
O1 O 1.1800(9) 0.1406(10) 0.2744(6) 0.032(3) Uani 1 1 d . . . . .
O2 O 1.2715(12) 0.2400(12) 0.1925(7) 0.055(5) Uani 1 1 d . . . . .
O3 O 1.2692(11) 0.2773(11) 0.3041(7) 0.047(4) Uani 1 1 d . . . . .
O4 O 1.1100(11) 0.3086(11) 0.2409(7) 0.046(4) Uani 1 1 d . . . . .
O5 O 1.1616(13) 0.0933(14) 0.1463(8) 0.064(5) Uani 1 1 d . . . . .
O6 O 1.0094(13) -0.0240(12) 0.1839(8) 0.060(5) Uani 1 1 d . U . . .
O7 O 1.3558(14) 0.1281(14) 0.1123(9) 0.071(5) Uani 1 1 d . U . . .
O8 O 1.0940(10) 0.3649(9) 0.3706(7) 0.034(3) Uani 1 1 d . . . . .
O9 O 1.5465(13) 0.0883(14) 0.1583(9) 0.075(6) Uani 1 1 d . U . . .
O10 O 0.9134(11) 0.3252(11) 0.2412(7) 0.047(4) Uani 1 1 d . . . . .
O11 O 1.3564(12) 0.2433(10) 0.4149(7) 0.043(4) Uani 1 1 d . . . . .
O12 O 0.9852(10) 0.2235(9) 0.3482(6) 0.033(3) Uani 1 1 d . . . . .
O13 O 1.0173(9) 0.0369(10) 0.3009(7) 0.035(3) Uani 1 1 d . . . . .
O14 O 1.0135(13) 0.4256(12) 0.1539(8) 0.060(5) Uani 1 1 d . U . . .
O15 O 1.2131(14) 0.4809(12) 0.2628(9) 0.067(6) Uani 1 1 d . . . . .
O16 O 1.1940(12) 0.3283(10) 0.4886(7) 0.046(4) Uani 1 1 d . . . . .
O17 O 1.1636(10) 0.1893(10) 0.4148(6) 0.036(4) Uani 1 1 d . . . . .
O18 O 0.9948(11) 0.1695(11) 0.1993(7) 0.044(4) Uani 1 1 d . . . . .
O19 O 1.0934(12) 0.2629(14) 0.1116(8) 0.065(5) Uani 1 1 d . . . . .
O20 O 1.0856(15) 0.5928(12) 0.1783(9) 0.071(6) Uani 1 1 d . . . . .
O21 O 1.4490(10) 0.3391(11) 0.3257(8) 0.048(4) Uani 1 1 d . . . . .
O22 O 1.3741(10) 0.0914(11) 0.3462(7) 0.039(4) Uani 1 1 d . . . . .
O23 O 1.4028(15) 0.5344(15) 0.3029(8) 0.084(7) Uani 1 1 d . . . . .
O24 O 1.2811(11) 0.4163(10) 0.3768(8) 0.049(4) Uani 1 1 d . . . . .
O25 O 1.1973(11) -0.0266(13) 0.2488(7) 0.052(4) Uani 1 1 d . . . . .
O26 O 1.3726(11) -0.0933(12) 0.3185(7) 0.050(4) Uani 1 1 d . . . . .
O27 O 1.2125(15) 0.4321(14) 0.1479(8) 0.076(6) Uani 1 1 d . . . . .
O28 O 1.0134(13) 0.4639(11) 0.2705(8) 0.058(5) Uani 1 1 d . . . . .
O29 O 0.8783(14) 0.3004(14) 0.1136(9) 0.073(5) Uani 1 1 d . U . . .
O30 O 1.4706(12) 0.1942(13) 0.2578(8) 0.060(5) Uani 1 1 d . . . . .
O31 O 1.2765(15) 0.3107(14) 0.0760(9) 0.076(6) Uani 1 1 d . U . . .
O32 O 1.2083(10) -0.0032(11) 0.3734(7) 0.044(4) Uani 1 1 d . . . . .
O33 O 0.8770(12) 0.3888(10) 0.3627(8) 0.050(5) Uani 1 1 d . . . . .
O34 O 1.5457(12) 0.1693(12) 0.3841(8) 0.053(4) Uani 1 1 d . . . . .
O35 O 1.3993(16) 0.4526(16) 0.0819(11) 0.095(7) Uani 1 1 d . U . . .
O36 O 1.3684(11) 0.0562(14) 0.2285(8) 0.062(5) Uani 1 1 d . . . . .
O37 O 1.1921(15) 0.1555(16) 0.0229(10) 0.088(7) Uani 1 1 d . U . . .
O38 O 1.4475(12) 0.2710(15) 0.1458(10) 0.078(6) Uani 1 1 d . . . . .
O39 O 1.3803(14) 0.4064(15) 0.2148(9) 0.076(6) Uani 1 1 d . . . . .
O40 O 0.9659(11) 0.1737(9) 0.4873(8) 0.041(4) Uani 1 1 d . . . . .
O41 O 0.9661(11) 0.1003(9) 0.5848(6) 0.033(3) Uani 1 1 d . . . . .
O42 O 0.8595(9) 0.0516(10) 0.3954(7) 0.033(3) Uani 1 1 d . . . . .
O43 O 0.8683(9) -0.0123(10) 0.4944(6) 0.034(3) Uani 1 1 d . . . . .
O44 O 0.746(3) 0.142(3) 0.100(2) 0.177(14) Uani 1 1 d . U . . .
O45 O 0.7937(17) 0.021(2) 0.1817(11) 0.096(7) Uani 1 1 d . . . . .
C1 C 0.9538(16) 0.1695(17) 0.5451(13) 0.047(6) Uani 1 1 d . . . . .
C2 C 0.9303(15) 0.2635(17) 0.5728(10) 0.040(6) Uani 1 1 d . . . . .
C3 C 0.930(2) 0.3478(18) 0.5362(14) 0.069(8) Uani 1 1 d . . . . .
H3A H 0.9414 0.3488 0.4928 0.083 Uiso 1 1 calc R U . . .
C4 C 0.914(2) 0.4320(16) 0.5642(16) 0.074(10) Uani 1 1 d . . . . .
H4A H 0.9180 0.4893 0.5403 0.089 Uiso 1 1 calc R U . . .
C5 C 0.886(2) 0.351(2) 0.6588(16) 0.074(8) Uani 1 1 d . U . . .
H5A H 0.8697 0.3527 0.7014 0.088 Uiso 1 1 calc R U . . .
C6 C 0.904(2) 0.2646(18) 0.6363(14) 0.072(9) Uani 1 1 d . . . . .
H6A H 0.8992 0.2093 0.6624 0.086 Uiso 1 1 calc R U . . .
C7 C 0.8203(15) 0.0062(13) 0.4427(11) 0.032(5) Uani 1 1 d . U . . .
C8 C 0.7167(14) -0.0266(13) 0.4361(9) 0.028(4) Uani 1 1 d . U . . .
C9 C 0.6635(17) -0.0671(17) 0.4880(13) 0.051(7) Uani 1 1 d . . . . .
H9A H 0.6917 -0.0752 0.5284 0.062 Uiso 1 1 calc R U . . .
C10 C 0.5684(17) -0.0943(16) 0.4766(12) 0.047(6) Uani 1 1 d . U . . .
H10A H 0.5298 -0.1174 0.5107 0.056 Uiso 1 1 calc R U . . .
C11 C 0.5787(16) -0.0585(16) 0.3691(12) 0.046(6) Uani 1 1 d . U . . .
H11A H 0.5509 -0.0591 0.3291 0.055 Uiso 1 1 calc R U . . .
C12 C 0.6734(15) -0.0251(14) 0.3772(11) 0.036(5) Uani 1 1 d . U . . .
H12A H 0.7086 -0.0010 0.3419 0.043 Uiso 1 1 calc R U . . .
C13 C 0.769(3) 0.101(3) 0.1603(19) 0.086(10) Uani 1 1 d . U . . .
C14 C 0.741(2) 0.1721(19) 0.2055(15) 0.063(7) Uani 1 1 d . U . . .
C15 C 0.685(3) 0.259(3) 0.185(2) 0.120(14) Uani 1 1 d . U . . .
H15A H 0.6710 0.2760 0.1425 0.144 Uiso 1 1 calc R U . . .
C16 C 0.654(2) 0.314(2) 0.2294(16) 0.070(8) Uani 1 1 d . U . . .
H16A H 0.6079 0.3660 0.2171 0.084 Uiso 1 1 calc R U . . .
C17 C 0.739(2) 0.220(2) 0.3066(16) 0.071(8) Uani 1 1 d . U . . .
H17A H 0.7559 0.2086 0.3493 0.086 Uiso 1 1 calc R U . . .
C18 C 0.7721(17) 0.1537(16) 0.2680(11) 0.042(5) Uani 1 1 d . U . . .
H18A H 0.8131 0.0994 0.2823 0.051 Uiso 1 1 calc R U . . .
N1 N 0.891(2) 0.4291(17) 0.6245(11) 0.075(7) Uani 1 1 d . . . . .
H1A H 0.8800 0.4810 0.6418 0.090 Uiso 1 1 calc R U . . .
N2 N 0.5298(13) -0.0892(11) 0.4200(9) 0.039(4) Uani 1 1 d . U . . .
H2A H 0.4694 -0.1068 0.4159 0.047 Uiso 1 1 calc R U . . .
N3 N 0.681(2) 0.304(2) 0.2858(16) 0.095(9) Uani 1 1 d . U . . .
H3B H 0.6652 0.3468 0.3109 0.114 Uiso 1 1 calc R U . . .
K1 K 0.8483(3) 0.1884(3) 0.0121(2) 0.0313(10) Uani 1 1 d . . . . .
C19 C 0.290(4) 0.599(4) -0.040(3) 0.056(13) Uani 0.5 1 d . U P . .
C20 C 0.220(3) 0.522(2) -0.0466(19) 0.027(8) Uani 0.5 1 d . U P . .
C21 C 0.140(3) 0.510(3) 0.012(2) 0.046(11) Uani 0.5 1 d . U P . .
H21A H 0.1325 0.5444 0.0473 0.055 Uiso 0.5 1 calc R U P . .
C22 C 0.086(6) 0.440(5) -0.002(4) 0.09(2) Uani 0.5 1 d . U P . .
H22A H 0.0299 0.4342 0.0247 0.111 Uiso 0.5 1 calc R U P . .
C23 C 0.163(5) 0.410(5) -0.096(4) 0.10(2) Uani 0.5 1 d . U P . .
H23A H 0.1643 0.3718 -0.1291 0.116 Uiso 0.5 1 calc R U P . .
C24 C 0.215(4) 0.474(4) -0.101(3) 0.059(14) Uani 0.5 1 d . U P . .
H24A H 0.2494 0.4913 -0.1384 0.071 Uiso 0.5 1 calc R U P . .
N4 N 0.092(4) 0.386(4) -0.038(3) 0.090(16) Uani 0.5 1 d . U P . .
H4B H 0.0596 0.3363 -0.0334 0.108 Uiso 0.5 1 calc R U P . .
O46 O 0.283(4) 0.675(4) -0.020(3) 0.110(16) Uani 0.5 1 d . U P . .
O47 O 0.383(5) 0.573(5) -0.053(3) 0.15(2) Uani 0.5 1 d . U P . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
W1 O9 1.698(17) . ?
W1 O36 1.813(18) . ?
W1 O7 1.87(2) . ?
W1 O30 1.896(17) . ?
W1 O38 1.92(2) . ?
W1 O2 2.441(17) . ?
W2 O26 1.689(16) . ?
W2 O32 1.767(14) . ?
W2 O25 1.894(15) . ?
W2 O22 1.941(14) . ?
W2 O36 2.048(17) . ?
W2 O1 2.364(14) . ?
W3 O35 1.729(18) . ?
W3 O31 1.82(2) . ?
W3 O27 1.87(2) . ?
W3 O38 1.89(2) . ?
W3 O39 1.94(2) . ?
W3 O2 2.419(15) . ?
W4 O23 1.725(17) . ?
W4 O24 1.864(15) . ?
W4 O21 1.878(15) . ?
W4 O39 1.88(2) . ?
W4 O15 1.920(19) . ?
W4 O3 2.509(15) . ?
W5 O29 1.713(19) . ?
W5 O18 1.865(15) . ?
W5 O10 1.884(15) . ?
W5 O19 1.920(17) . ?
W5 O14 1.964(16) . ?
W5 O4 2.399(16) . ?
W6 O37 1.68(2) . ?
W6 O5 1.816(18) . ?
W6 O19 1.879(19) . ?
W6 O7 1.985(19) . ?
W6 O31 2.036(19) . ?
W6 O2 2.423(17) . ?
W7 O34 1.681(17) . ?
W7 O11 1.878(15) . ?
W7 O22 1.900(14) . ?
W7 O30 1.933(17) . ?
W7 O21 1.935(14) . ?
W7 O3 2.447(16) . ?
W8 O16 1.702(15) . ?
W8 O17 1.745(13) . ?
W8 O8 1.916(14) . ?
W8 O11 1.981(15) . ?
W8 O24 2.069(12) . ?
W8 O3 2.467(15) . ?
W9 O20 1.688(16) . ?
W9 O28 1.842(17) . ?
W9 O14 1.856(19) . ?
W9 O15 1.91(2) . ?
W9 O27 1.94(2) . ?
W9 O4 2.466(15) . ?
W10 O6 1.703(17) . ?
W10 O13 1.779(13) . ?
W10 O25 1.913(16) . ?
W10 O18 1.950(16) . ?
W10 O5 2.087(16) . ?
W10 O1 2.333(13) . ?
W11 O33 1.692(14) . ?
W11 O12 1.730(12) . ?
W11 O8 1.940(14) . ?
W11 O10 1.941(16) . ?
W11 O28 2.061(14) . ?
W11 O4 2.466(14) . ?
Nd1 O43 2.414(14) 2_756 ?
Nd1 O17 2.416(13) . ?
Nd1 O13 2.432(14) . ?
Nd1 O40 2.458(15) . ?
Nd1 O32 2.465(14) . ?
Nd1 O12 2.467(13) . ?
Nd1 O42 2.474(12) . ?
Nd1 O41 2.487(13) 2_756 ?
Nd2 O45 2.12(3) . ?
Nd2 O1W 2.35(2) . ?
Nd2 O3W 2.34(4) . ?
Nd2 O6W 2.45(4) . ?
Nd2 O2W 2.499(18) . ?
Nd2 O6 2.665(18) . ?
Nd2 O7W 2.65(4) . ?
Nd2 O5W 2.81(4) . ?
O3W H3WA 0.8501 . ?
O3W H3WB 0.8500 . ?
Nd2A O4W 2.16(5) . ?
Nd2A O6 2.376(18) . ?
Nd2A O45 2.53(3) . ?
O4W H4WA 0.8501 . ?
O4W H4WB 0.8500 . ?
P1 O3 1.504(17) . ?
P1 O1 1.537(14) . ?
P1 O4 1.535(16) . ?
P1 O2 1.546(16) . ?
O29 K1 2.86(2) . ?
O40 C1 1.23(3) . ?
O41 C1 1.24(3) . ?
O41 Nd1 2.487(13) 2_756 ?
O42 C7 1.27(2) . ?
O43 C7 1.26(2) . ?
O43 Nd1 2.414(14) 2_756 ?
O44 C13 1.39(5) . ?
O44 K1 2.35(4) . ?
O45 C13 1.20(4) . ?
C1 C2 1.53(3) . ?
C2 C3 1.37(3) . ?
C2 C6 1.39(3) . ?
C3 C4 1.39(4) . ?
C3 H3A 0.9300 . ?
C4 N1 1.31(3) . ?
C4 H4A 0.9300 . ?
C5 N1 1.29(3) . ?
C5 C6 1.36(4) . ?
C5 H5A 0.9300 . ?
C6 H6A 0.9300 . ?
C7 C8 1.49(3) . ?
C8 C12 1.38(3) . ?
C8 C9 1.40(3) . ?
C9 C10 1.37(3) . ?
C9 H9A 0.9300 . ?
C10 N2 1.30(3) . ?
C10 H10A 0.9300 . ?
C11 N2 1.31(3) . ?
C11 C12 1.39(3) . ?
C11 H11A 0.9300 . ?
C12 H12A 0.9300 . ?
C13 C14 1.49(4) . ?
C14 C18 1.39(4) . ?
C14 C15 1.41(5) . ?
C15 C16 1.33(5) . ?
C15 H15A 0.9300 . ?
C16 N3 1.24(4) . ?
C16 H16A 0.9300 . ?
C17 C18 1.35(4) . ?
C17 N3 1.40(4) . ?
C17 H17A 0.9300 . ?
C18 H18A 0.9300 . ?
N1 H1A 0.8600 . ?
N2 H2A 0.8600 . ?
N3 H3B 0.8600 . ?
K1 O46 2.50(5) 2_665 ?
C19 O46 1.21(6) . ?
C19 O47 1.28(7) . ?
C19 C20 1.51(6) . ?
C20 C24 1.41(7) . ?
C20 C21 1.63(6) . ?
C21 C22 1.33(8) . ?
C21 H21A 0.9300 . ?
C22 N4 1.14(8) . ?
C22 H22A 0.9300 . ?
C23 C24 1.19(8) . ?
C23 N4 1.57(8) . ?
C23 H23A 0.9300 . ?
C24 H24A 0.9300 . ?
N4 H4B 0.8600 . ?
O46 K1 2.50(5) 2_665 ?

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
_geom_angle_publ_flag
O9 W1 O36 105.7(9) . . ?
O9 W1 O7 97.3(9) . . ?
O36 W1 O7 89.1(8) . . ?
O9 W1 O30 104.0(9) . . ?
O36 W1 O30 89.8(7) . . ?
O7 W1 O30 158.2(8) . . ?
O9 W1 O38 101.3(8) . . ?
O36 W1 O38 153.0(7) . . ?
O7 W1 O38 88.0(9) . . ?
O30 W1 O38 83.2(8) . . ?
O9 W1 O2 167.5(8) . . ?
O36 W1 O2 82.8(6) . . ?
O7 W1 O2 73.4(7) . . ?
O30 W1 O2 84.8(7) . . ?
O38 W1 O2 70.6(6) . . ?
O26 W2 O32 103.2(7) . . ?
O26 W2 O25 101.8(7) . . ?
O32 W2 O25 95.2(7) . . ?
O26 W2 O22 99.3(7) . . ?
O32 W2 O22 93.0(6) . . ?
O25 W2 O22 155.0(7) . . ?
O26 W2 O36 93.3(7) . . ?
O32 W2 O36 163.2(7) . . ?
O25 W2 O36 84.1(6) . . ?
O22 W2 O36 81.3(6) . . ?
O26 W2 O1 170.4(6) . . ?
O32 W2 O1 84.0(6) . . ?
O25 W2 O1 70.9(6) . . ?
O22 W2 O1 86.5(6) . . ?
O36 W2 O1 79.9(6) . . ?
O35 W3 O31 100.1(10) . . ?
O35 W3 O27 103.3(9) . . ?
O31 W3 O27 85.3(8) . . ?
O35 W3 O38 103.0(9) . . ?
O31 W3 O38 92.4(9) . . ?
O27 W3 O38 153.6(7) . . ?
O35 W3 O39 101.6(9) . . ?
O31 W3 O39 157.9(7) . . ?
O27 W3 O39 86.0(9) . . ?
O38 W3 O39 86.4(9) . . ?
O35 W3 O2 171.2(9) . . ?
O31 W3 O2 73.6(6) . . ?
O27 W3 O2 82.6(6) . . ?
O38 W3 O2 71.5(7) . . ?
O39 W3 O2 85.1(7) . . ?
O23 W4 O24 102.2(8) . . ?
O23 W4 O21 102.2(9) . . ?
O24 W4 O21 89.5(7) . . ?
O23 W4 O39 100.7(8) . . ?
O24 W4 O39 157.0(7) . . ?
O21 W4 O39 87.2(8) . . ?
O23 W4 O15 101.6(9) . . ?
O24 W4 O15 88.5(7) . . ?
O21 W4 O15 156.0(7) . . ?
O39 W4 O15 85.5(9) . . ?
O23 W4 O3 172.8(7) . . ?
O24 W4 O3 73.1(6) . . ?
O21 W4 O3 72.7(6) . . ?
O39 W4 O3 84.2(7) . . ?
O15 W4 O3 83.8(6) . . ?
O29 W5 O18 104.5(8) . . ?
O29 W5 O10 102.9(8) . . ?
O18 W5 O10 88.3(6) . . ?
O29 W5 O19 101.3(8) . . ?
O18 W5 O19 86.4(7) . . ?
O10 W5 O19 155.7(7) . . ?
O29 W5 O14 100.6(8) . . ?
O18 W5 O14 154.9(7) . . ?
O10 W5 O14 86.9(7) . . ?
O19 W5 O14 87.9(7) . . ?
O29 W5 O4 172.0(8) . . ?
O18 W5 O4 82.0(6) . . ?
O10 W5 O4 72.2(6) . . ?
O19 W5 O4 83.6(6) . . ?
O14 W5 O4 73.1(6) . . ?
O37 W6 O5 102.3(9) . . ?
O37 W6 O19 102.5(9) . . ?
O5 W6 O19 87.4(8) . . ?
O37 W6 O7 102.0(9) . . ?
O5 W6 O7 90.8(8) . . ?
O19 W6 O7 155.3(8) . . ?
O37 W6 O31 102.4(9) . . ?
O5 W6 O31 155.1(8) . . ?
O19 W6 O31 84.5(7) . . ?
O7 W6 O31 86.9(8) . . ?
O37 W6 O2 170.5(7) . . ?
O5 W6 O2 85.4(6) . . ?
O19 W6 O2 83.2(7) . . ?
O7 W6 O2 72.0(7) . . ?
O31 W6 O2 70.2(7) . . ?
O34 W7 O11 98.4(7) . . ?
O34 W7 O22 100.7(7) . . ?
O11 W7 O22 92.4(6) . . ?
O34 W7 O30 103.6(7) . . ?
O11 W7 O30 157.7(7) . . ?
O22 W7 O30 87.7(6) . . ?
O34 W7 O21 102.1(7) . . ?
O11 W7 O21 85.5(6) . . ?
O22 W7 O21 157.1(6) . . ?
O30 W7 O21 85.8(7) . . ?
O34 W7 O3 170.3(7) . . ?
O11 W7 O3 72.9(6) . . ?
O22 W7 O3 84.2(6) . . ?
O30 W7 O3 84.9(6) . . ?
O21 W7 O3 73.4(6) . . ?
O16 W8 O17 103.8(6) . . ?
O16 W8 O8 102.3(7) . . ?
O17 W8 O8 94.0(6) . . ?
O16 W8 O11 102.1(7) . . ?
O17 W8 O11 92.9(6) . . ?
O8 W8 O11 152.2(6) . . ?
O16 W8 O24 98.0(6) . . ?
O17 W8 O24 158.2(6) . . ?
O8 W8 O24 82.5(6) . . ?
O11 W8 O24 81.2(6) . . ?
O16 W8 O3 167.5(6) . . ?
O17 W8 O3 87.2(6) . . ?
O8 W8 O3 82.6(6) . . ?
O11 W8 O3 70.9(6) . . ?
O24 W8 O3 71.0(6) . . ?
O20 W9 O28 103.8(8) . . ?
O20 W9 O14 102.0(9) . . ?
O28 W9 O14 88.8(7) . . ?
O20 W9 O15 99.6(9) . . ?
O28 W9 O15 89.7(7) . . ?
O14 W9 O15 158.1(7) . . ?
O20 W9 O27 102.2(8) . . ?
O28 W9 O27 153.9(7) . . ?
O14 W9 O27 86.9(8) . . ?
O15 W9 O27 84.9(8) . . ?
O20 W9 O4 173.4(8) . . ?
O28 W9 O4 72.0(6) . . ?
O14 W9 O4 73.1(6) . . ?
O15 W9 O4 85.6(6) . . ?
O27 W9 O4 82.1(6) . . ?
O6 W10 O13 102.6(7) . . ?
O6 W10 O25 102.6(8) . . ?
O13 W10 O25 94.1(6) . . ?
O6 W10 O18 100.6(7) . . ?
O13 W10 O18 94.2(6) . . ?
O25 W10 O18 153.0(7) . . ?
O6 W10 O5 94.2(8) . . ?
O13 W10 O5 163.2(6) . . ?
O25 W10 O5 83.2(7) . . ?
O18 W10 O5 81.4(7) . . ?
O6 W10 O1 172.8(7) . . ?
O13 W10 O1 82.1(5) . . ?
O25 W10 O1 71.4(6) . . ?
O18 W10 O1 84.4(6) . . ?
O5 W10 O1 81.4(6) . . ?
O33 W11 O12 103.4(6) . . ?
O33 W11 O8 102.1(8) . . ?
O12 W11 O8 93.1(6) . . ?
O33 W11 O10 102.5(8) . . ?
O12 W11 O10 94.8(7) . . ?
O8 W11 O10 151.5(6) . . ?
O33 W11 O28 97.7(7) . . ?
O12 W11 O28 158.8(7) . . ?
O8 W11 O28 81.5(6) . . ?
O10 W11 O28 81.3(7) . . ?
O33 W11 O4 165.1(6) . . ?
O12 W11 O4 90.2(6) . . ?
O8 W11 O4 82.9(6) . . ?
O10 W11 O4 69.8(5) . . ?
O28 W11 O4 68.9(6) . . ?
O43 Nd1 O17 79.7(4) 2_756 . ?
O43 Nd1 O13 142.1(5) 2_756 . ?
O17 Nd1 O13 112.3(4) . . ?
O43 Nd1 O40 76.5(5) 2_756 . ?
O17 Nd1 O40 76.2(5) . . ?
O13 Nd1 O40 140.3(5) . . ?
O43 Nd1 O32 75.6(5) 2_756 . ?
O17 Nd1 O32 75.3(5) . . ?
O13 Nd1 O32 73.4(5) . . ?
O40 Nd1 O32 143.0(5) . . ?
O43 Nd1 O12 140.5(5) 2_756 . ?
O17 Nd1 O12 67.7(4) . . ?
O13 Nd1 O12 73.8(5) . . ?
O40 Nd1 O12 74.6(5) . . ?
O32 Nd1 O12 114.8(5) . . ?
O43 Nd1 O42 120.6(4) 2_756 . ?
O17 Nd1 O42 143.6(5) . . ?
O13 Nd1 O42 71.6(4) . . ?
O40 Nd1 O42 79.8(5) . . ?
O32 Nd1 O42 136.0(5) . . ?
O12 Nd1 O42 79.8(4) . . ?
O43 Nd1 O41 75.4(5) 2_756 2_756 ?
O17 Nd1 O41 141.9(5) . 2_756 ?
O13 Nd1 O41 74.3(5) . 2_756 ?
O40 Nd1 O41 123.9(4) . 2_756 ?
O32 Nd1 O41 70.9(5) . 2_756 ?
O12 Nd1 O41 143.9(5) . 2_756 ?
O42 Nd1 O41 74.5(4) . 2_756 ?
O45 Nd2 O1W 86.9(9) . . ?
O45 Nd2 O3W 91.9(14) . . ?
O1W Nd2 O3W 147.6(13) . . ?
O45 Nd2 O6W 84.6(11) . . ?
O1W Nd2 O6W 72.5(9) . . ?
O3W Nd2 O6W 75.2(14) . . ?
O45 Nd2 O2W 86.2(8) . . ?
O1W Nd2 O2W 139.4(6) . . ?
O3W Nd2 O2W 72.6(12) . . ?
O6W Nd2 O2W 146.1(9) . . ?
O45 Nd2 O6 71.6(7) . . ?
O1W Nd2 O6 68.0(6) . . ?
O3W Nd2 O6 141.6(12) . . ?
O6W Nd2 O6 134.4(9) . . ?
O2W Nd2 O6 71.9(5) . . ?
O45 Nd2 O7W 128.1(12) . . ?
O1W Nd2 O7W 77.0(10) . . ?
O3W Nd2 O7W 78.5(14) . . ?
O6W Nd2 O7W 43.5(12) . . ?
O2W Nd2 O7W 135.6(10) . . ?
O6 Nd2 O7W 139.0(10) . . ?
O45 Nd2 O5W 148.3(12) . . ?
O1W Nd2 O5W 124.5(11) . . ?
O3W Nd2 O5W 63.9(16) . . ?
O6W Nd2 O5W 106.6(13) . . ?
O2W Nd2 O5W 67.8(10) . . ?
O6 Nd2 O5W 114.1(10) . . ?
O7W Nd2 O5W 69.5(13) . . ?
Nd2 O3W H3WA 119.3 . . ?
Nd2 O3W H3WB 120.7 . . ?
H3WA O3W H3WB 120.0 . . ?
O4W Nd2A O6 74.6(16) . . ?
O4W Nd2A O45 145.0(16) . . ?
O6 Nd2A O45 70.5(7) . . ?
Nd2A O4W H4WA 120.2 . . ?
Nd2A O4W H4WB 119.8 . . ?
H4WA O4W H4WB 120.0 . . ?
O3 P1 O1 111.2(8) . . ?
O3 P1 O4 108.8(9) . . ?
O1 P1 O4 111.1(7) . . ?
O3 P1 O2 108.7(8) . . ?
O1 P1 O2 108.8(9) . . ?
O4 P1 O2 108.2(9) . . ?
P1 O1 W10 128.8(8) . . ?
P1 O1 W2 128.2(7) . . ?
W10 O1 W2 91.3(5) . . ?
P1 O2 W3 127.9(10) . . ?
P1 O2 W6 124.2(8) . . ?
W3 O2 W6 90.2(5) . . ?
P1 O2 W1 124.2(9) . . ?
W3 O2 W1 89.5(5) . . ?
W6 O2 W1 89.3(6) . . ?
P1 O3 W7 126.1(9) . . ?
P1 O3 W8 125.6(7) . . ?
W7 O3 W8 89.2(5) . . ?
P1 O3 W4 127.0(8) . . ?
W7 O3 W4 86.9(5) . . ?
W8 O3 W4 89.6(5) . . ?
P1 O4 W5 126.5(9) . . ?
P1 O4 W9 126.2(8) . . ?
W5 O4 W9 88.4(5) . . ?
P1 O4 W11 123.7(8) . . ?
W5 O4 W11 89.9(5) . . ?
W9 O4 W11 90.8(5) . . ?
W6 O5 W10 150.4(11) . . ?
W10 O6 Nd2A 150.8(10) . . ?
W10 O6 Nd2 145.1(9) . . ?
W1 O7 W6 125.2(10) . . ?
W8 O8 W11 140.5(7) . . ?
W5 O10 W11 128.0(8) . . ?
W7 O11 W8 126.8(8) . . ?
W11 O12 Nd1 160.4(8) . . ?
W10 O13 Nd1 141.4(6) . . ?
W9 O14 W5 125.2(9) . . ?
W9 O15 W4 151.0(12) . . ?
W8 O17 Nd1 160.1(8) . . ?
W5 O18 W10 154.4(8) . . ?
W6 O19 W5 150.4(10) . . ?
W4 O21 W7 126.8(8) . . ?
W7 O22 W2 152.1(8) . . ?
W4 O24 W8 126.1(9) . . ?
W2 O25 W10 123.8(9) . . ?
W3 O27 W9 152.2(10) . . ?
W9 O28 W11 128.2(10) . . ?
W5 O29 K1 129.9(10) . . ?
W1 O30 W7 145.8(8) . . ?
W3 O31 W6 125.4(10) . . ?
W2 O32 Nd1 138.8(8) . . ?
W1 O36 W2 152.8(10) . . ?
W3 O38 W1 127.8(8) . . ?
W4 O39 W3 150.2(10) . . ?
C1 O40 Nd1 137.8(15) . . ?
C1 O41 Nd1 138.8(15) . 2_756 ?
C7 O42 Nd1 113.7(12) . . ?
C7 O43 Nd1 171.1(14) . 2_756 ?
C13 O44 K1 134(3) . . ?
C13 O45 Nd2 160(3) . . ?
C13 O45 Nd2A 154(2) . . ?
O40 C1 O41 129(2) . . ?
O40 C1 C2 116(2) . . ?
O41 C1 C2 115(2) . . ?
C3 C2 C6 118(2) . . ?
C3 C2 C1 122(2) . . ?
C6 C2 C1 120(2) . . ?
C2 C3 C4 120(3) . . ?
C2 C3 H3A 120.0 . . ?
C4 C3 H3A 120.0 . . ?
N1 C4 C3 119(2) . . ?
N1 C4 H4A 120.5 . . ?
C3 C4 H4A 120.5 . . ?
N1 C5 C6 124(3) . . ?
N1 C5 H5A 118.1 . . ?
C6 C5 H5A 118.1 . . ?
C5 C6 C2 117(2) . . ?
C5 C6 H6A 121.5 . . ?
C2 C6 H6A 121.5 . . ?
O43 C7 O42 121.2(18) . . ?
O43 C7 C8 119.9(17) . . ?
O42 C7 C8 118.9(19) . . ?
C12 C8 C9 117.4(18) . . ?
C12 C8 C7 120.3(17) . . ?
C9 C8 C7 122.1(19) . . ?
C10 C9 C8 117(2) . . ?
C10 C9 H9A 121.4 . . ?
C8 C9 H9A 121.4 . . ?
N2 C10 C9 123(2) . . ?
N2 C10 H10A 118.7 . . ?
C9 C10 H10A 118.7 . . ?
N2 C11 C12 118(2) . . ?
N2 C11 H11A 121.2 . . ?
C12 C11 H11A 121.2 . . ?
C8 C12 C11 121.8(19) . . ?
C8 C12 H12A 119.1 . . ?
C11 C12 H12A 119.1 . . ?
O45 C13 O44 133(4) . . ?
O45 C13 C14 118(3) . . ?
O44 C13 C14 108(3) . . ?
C18 C14 C15 120(3) . . ?
C18 C14 C13 119(3) . . ?
C15 C14 C13 121(4) . . ?
C16 C15 C14 117(4) . . ?
C16 C15 H15A 121.6 . . ?
C14 C15 H15A 121.6 . . ?
N3 C16 C15 126(4) . . ?
N3 C16 H16A 116.9 . . ?
C15 C16 H16A 116.9 . . ?
C18 C17 N3 123(3) . . ?
C18 C17 H17A 118.3 . . ?
N3 C17 H17A 118.3 . . ?
C17 C18 C14 116(3) . . ?
C17 C18 H18A 122.2 . . ?
C14 C18 H18A 122.2 . . ?
C5 N1 C4 122(3) . . ?
C5 N1 H1A 119.2 . . ?
C4 N1 H1A 119.2 . . ?
C10 N2 C11 123.1(18) . . ?
C10 N2 H2A 118.5 . . ?
C11 N2 H2A 118.5 . . ?
C16 N3 C17 117(3) . . ?
C16 N3 H3B 121.5 . . ?
C17 N3 H3B 121.5 . . ?
O44 K1 O46 75.8(15) . 2_665 ?
O44 K1 O29 70.0(10) . . ?
O46 K1 O29 65.1(13) 2_665 . ?
O46 C19 O47 111(6) . . ?
O46 C19 C20 137(5) . . ?
O47 C19 C20 112(5) . . ?
C24 C20 C19 124(4) . . ?
C24 C20 C21 123(4) . . ?
C19 C20 C21 113(4) . . ?
C22 C21 C20 104(5) . . ?
C22 C21 H21A 128.1 . . ?
C20 C21 H21A 128.1 . . ?
N4 C22 C21 137(8) . . ?
N4 C22 H22A 111.5 . . ?
C21 C22 H22A 111.5 . . ?
C24 C23 N4 125(7) . . ?
C24 C23 H23A 117.7 . . ?
N4 C23 H23A 117.7 . . ?
C23 C24 C20 115(6) . . ?
C23 C24 H24A 122.4 . . ?
C20 C24 H24A 122.4 . . ?
C22 N4 C23 114(6) . . ?
C22 N4 H4B 122.9 . . ?
C23 N4 H4B 122.9 . . ?
C19 O46 K1 138(5) . 2_665 ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O3 P1 O1 W10 173.5(8) . . . . ?
O4 P1 O1 W10 52.2(12) . . . . ?
O2 P1 O1 W10 -66.8(11) . . . . ?
O3 P1 O1 W2 -54.4(12) . . . . ?
O4 P1 O1 W2 -175.7(9) . . . . ?
O2 P1 O1 W2 65.3(11) . . . . ?
O3 P1 O2 W3 -58.5(13) . . . . ?
O1 P1 O2 W3 -179.8(9) . . . . ?
O4 P1 O2 W3 59.4(13) . . . . ?
O3 P1 O2 W6 179.1(10) . . . . ?
O1 P1 O2 W6 57.9(12) . . . . ?
O4 P1 O2 W6 -63.0(12) . . . . ?
O3 P1 O2 W1 62.6(12) . . . . ?
O1 P1 O2 W1 -58.6(12) . . . . ?
O4 P1 O2 W1 -179.4(9) . . . . ?
O1 P1 O3 W7 59.1(11) . . . . ?
O4 P1 O3 W7 -178.2(8) . . . . ?
O2 P1 O3 W7 -60.6(11) . . . . ?
O1 P1 O3 W8 -61.1(12) . . . . ?
O4 P1 O3 W8 61.6(11) . . . . ?
O2 P1 O3 W8 179.2(10) . . . . ?
O1 P1 O3 W4 177.0(8) . . . . ?
O4 P1 O3 W4 -60.3(11) . . . . ?
O2 P1 O3 W4 57.2(12) . . . . ?
O3 P1 O4 W5 178.9(8) . . . . ?
O1 P1 O4 W5 -58.4(11) . . . . ?
O2 P1 O4 W5 61.0(11) . . . . ?
O3 P1 O4 W9 59.0(12) . . . . ?
O1 P1 O4 W9 -178.3(9) . . . . ?
O2 P1 O4 W9 -58.9(13) . . . . ?
O3 P1 O4 W11 -61.7(11) . . . . ?
O1 P1 O4 W11 61.1(12) . . . . ?
O2 P1 O4 W11 -179.6(9) . . . . ?
O37 W6 O5 W10 -135(2) . . . . ?
O19 W6 O5 W10 -32(2) . . . . ?
O7 W6 O5 W10 123(2) . . . . ?
O31 W6 O5 W10 38(3) . . . . ?
O2 W6 O5 W10 50.9(19) . . . . ?
O13 W10 O6 Nd2A -6(2) . . . . ?
O25 W10 O6 Nd2A 91(2) . . . . ?
O18 W10 O6 Nd2A -103(2) . . . . ?
O5 W10 O6 Nd2A 175(2) . . . . ?
O13 W10 O6 Nd2 14.4(18) . . . . ?
O25 W10 O6 Nd2 111.6(16) . . . . ?
O18 W10 O6 Nd2 -82.4(17) . . . . ?
O5 W10 O6 Nd2 -164.5(16) . . . . ?
O9 W1 O7 W6 -172.5(12) . . . . ?
O36 W1 O7 W6 81.8(12) . . . . ?
O30 W1 O7 W6 -5(3) . . . . ?
O38 W1 O7 W6 -71.3(12) . . . . ?
O2 W1 O7 W6 -1.0(10) . . . . ?
O29 W5 O10 W11 -175.7(11) . . . . ?
O18 W5 O10 W11 79.8(10) . . . . ?
O19 W5 O10 W11 2(2) . . . . ?
O14 W5 O10 W11 -75.6(11) . . . . ?
O4 W5 O10 W11 -2.3(9) . . . . ?
O34 W7 O11 W8 179.1(9) . . . . ?
O22 W7 O11 W8 -79.7(9) . . . . ?
O30 W7 O11 W8 10(2) . . . . ?
O21 W7 O11 W8 77.5(9) . . . . ?
O3 W7 O11 W8 3.6(7) . . . . ?
O33 W11 O12 Nd1 -99(2) . . . . ?
O8 W11 O12 Nd1 5(2) . . . . ?
O10 W11 O12 Nd1 157(2) . . . . ?
O28 W11 O12 Nd1 79(3) . . . . ?
O4 W11 O12 Nd1 88(2) . . . . ?
O6 W10 O13 Nd1 166.7(12) . . . . ?
O25 W10 O13 Nd1 62.8(12) . . . . ?
O18 W10 O13 Nd1 -91.4(12) . . . . ?
O5 W10 O13 Nd1 -17(3) . . . . ?
O1 W10 O13 Nd1 -7.7(11) . . . . ?
O20 W9 O14 W5 -171.0(11) . . . . ?
O28 W9 O14 W5 -67.1(11) . . . . ?
O15 W9 O14 W5 19(3) . . . . ?
O27 W9 O14 W5 87.1(11) . . . . ?
O4 W9 O14 W5 4.4(9) . . . . ?
O16 W8 O17 Nd1 88(2) . . . . ?
O8 W8 O17 Nd1 -16(2) . . . . ?
O11 W8 O17 Nd1 -169(2) . . . . ?
O24 W8 O17 Nd1 -96(3) . . . . ?
O3 W8 O17 Nd1 -98(2) . . . . ?
O29 W5 O18 W10 131(2) . . . . ?
O10 W5 O18 W10 -126(2) . . . . ?
O19 W5 O18 W10 31(2) . . . . ?
O14 W5 O18 W10 -47(3) . . . . ?
O4 W5 O18 W10 -53.3(19) . . . . ?
O37 W6 O19 W5 129(2) . . . . ?
O5 W6 O19 W5 27(2) . . . . ?
O7 W6 O19 W5 -60(3) . . . . ?
O31 W6 O19 W5 -130(2) . . . . ?
O2 W6 O19 W5 -59(2) . . . . ?
O23 W4 O21 W7 169.9(11) . . . . ?
O24 W4 O21 W7 67.6(11) . . . . ?
O39 W4 O21 W7 -89.7(11) . . . . ?
O15 W4 O21 W7 -17(2) . . . . ?
O3 W4 O21 W7 -4.9(9) . . . . ?
O23 W4 O24 W8 -170.7(11) . . . . ?
O21 W4 O24 W8 -68.4(10) . . . . ?
O39 W4 O24 W8 13(3) . . . . ?
O15 W4 O24 W8 87.7(10) . . . . ?
O3 W4 O24 W8 3.7(8) . . . . ?
O26 W2 O25 W10 171.3(9) . . . . ?
O32 W2 O25 W10 66.6(11) . . . . ?
O22 W2 O25 W10 -42.0(18) . . . . ?
O36 W2 O25 W10 -96.5(11) . . . . ?
O1 W2 O25 W10 -15.2(8) . . . . ?
O35 W3 O27 W9 -127(2) . . . . ?
O31 W3 O27 W9 134(2) . . . . ?
O38 W3 O27 W9 48(3) . . . . ?
O39 W3 O27 W9 -26(2) . . . . ?
O2 W3 O27 W9 60(2) . . . . ?
O20 W9 O28 W11 172.5(11) . . . . ?
O14 W9 O28 W11 70.5(11) . . . . ?
O15 W9 O28 W11 -87.7(11) . . . . ?
O27 W9 O28 W11 -10(2) . . . . ?
O4 W9 O28 W11 -2.2(9) . . . . ?
O18 W5 O29 K1 -52.8(11) . . . . ?
O10 W5 O29 K1 -144.4(10) . . . . ?
O19 W5 O29 K1 36.4(12) . . . . ?
O14 W5 O29 K1 126.4(10) . . . . ?
O9 W1 O30 W7 -130.3(19) . . . . ?
O36 W1 O30 W7 -24.2(19) . . . . ?
O7 W1 O30 W7 63(3) . . . . ?
O38 W1 O30 W7 130(2) . . . . ?
O2 W1 O30 W7 58.6(19) . . . . ?
O35 W3 O31 W6 166.8(12) . . . . ?
O27 W3 O31 W6 -90.6(11) . . . . ?
O38 W3 O31 W6 63.1(12) . . . . ?
O39 W3 O31 W6 -23(3) . . . . ?
O2 W3 O31 W6 -6.9(10) . . . . ?
O26 W2 O32 Nd1 -167.1(12) . . . . ?
O25 W2 O32 Nd1 -63.7(13) . . . . ?
O22 W2 O32 Nd1 92.7(12) . . . . ?
O36 W2 O32 Nd1 23(3) . . . . ?
O1 W2 O32 Nd1 6.5(11) . . . . ?
O9 W1 O36 W2 130(2) . . . . ?
O7 W1 O36 W2 -133(2) . . . . ?
O30 W1 O36 W2 25(2) . . . . ?
O38 W1 O36 W2 -49(3) . . . . ?
O2 W1 O36 W2 -60(2) . . . . ?
O35 W3 O38 W1 -165.9(15) . . . . ?
O31 W3 O38 W1 -64.9(15) . . . . ?
O27 W3 O38 W1 19(3) . . . . ?
O39 W3 O38 W1 93.0(14) . . . . ?
O2 W3 O38 W1 6.9(12) . . . . ?
O23 W4 O39 W3 -134(2) . . . . ?
O24 W4 O39 W3 42(4) . . . . ?
O21 W4 O39 W3 124(2) . . . . ?
O15 W4 O39 W3 -33(2) . . . . ?
O3 W4 O39 W3 51(2) . . . . ?
Nd1 O40 C1 O41 -12(4) . . . . ?
Nd1 O40 C1 C2 161.1(13) . . . . ?
Nd1 O41 C1 O40 -29(4) 2_756 . . . ?
Nd1 O41 C1 C2 157.7(14) 2_756 . . . ?
O40 C1 C2 C3 -5(3) . . . . ?
O41 C1 C2 C3 170(2) . . . . ?
O40 C1 C2 C6 173(2) . . . . ?
O41 C1 C2 C6 -13(3) . . . . ?
C6 C2 C3 C4 6(4) . . . . ?
C1 C2 C3 C4 -177(2) . . . . ?
C2 C3 C4 N1 -4(5) . . . . ?
N1 C5 C6 C2 1(5) . . . . ?
C3 C2 C6 C5 -4(4) . . . . ?
C1 C2 C6 C5 178(2) . . . . ?
Nd1 O42 C7 O43 10(2) . . . . ?
Nd1 O42 C7 C8 -168.8(13) . . . . ?
O43 C7 C8 C12 -165.9(19) . . . . ?
O42 C7 C8 C12 13(3) . . . . ?
O43 C7 C8 C9 9(3) . . . . ?
O42 C7 C8 C9 -172.3(19) . . . . ?
C12 C8 C9 C10 -6(3) . . . . ?
C7 C8 C9 C10 180(2) . . . . ?
C8 C9 C10 N2 4(4) . . . . ?
C9 C8 C12 C11 3(3) . . . . ?
C7 C8 C12 C11 177(2) . . . . ?
N2 C11 C12 C8 2(3) . . . . ?
Nd2 O45 C13 O44 15(11) . . . . ?
Nd2A O45 C13 O44 40(9) . . . . ?
Nd2 O45 C13 C14 -176(5) . . . . ?
Nd2A O45 C13 C14 -150(4) . . . . ?
K1 O44 C13 O45 -79(6) . . . . ?
K1 O44 C13 C14 110(4) . . . . ?
O45 C13 C14 C18 19(4) . . . . ?
O44 C13 C14 C18 -169(3) . . . . ?
O45 C13 C14 C15 -163(3) . . . . ?
O44 C13 C14 C15 9(4) . . . . ?
C18 C14 C15 C16 -8(5) . . . . ?
C13 C14 C15 C16 173(3) . . . . ?
C14 C15 C16 N3 11(6) . . . . ?
N3 C17 C18 C14 -3(4) . . . . ?
C15 C14 C18 C17 5(4) . . . . ?
C13 C14 C18 C17 -177(2) . . . . ?
C6 C5 N1 C4 1(5) . . . . ?
C3 C4 N1 C5 1(5) . . . . ?
C9 C10 N2 C11 1(4) . . . . ?
C12 C11 N2 C10 -4(3) . . . . ?
C15 C16 N3 C17 -9(5) . . . . ?
C18 C17 N3 C16 5(4) . . . . ?
O46 C19 C20 C24 138(7) . . . . ?
O47 C19 C20 C24 -53(7) . . . . ?
O46 C19 C20 C21 -34(9) . . . . ?
O47 C19 C20 C21 135(5) . . . . ?
C24 C20 C21 C22 8(6) . . . . ?
C19 C20 C21 C22 -180(5) . . . . ?
C20 C21 C22 N4 10(12) . . . . ?
N4 C23 C24 C20 8(10) . . . . ?
C19 C20 C24 C23 174(6) . . . . ?
C21 C20 C24 C23 -15(8) . . . . ?
C21 C22 N4 C23 -18(13) . . . . ?
C24 C23 N4 C22 7(10) . . . . ?
O47 C19 O46 K1 155(5) . . . 2_665 ?
C20 C19 O46 K1 -36(11) . . . 2_665 ?

_refine_diff_density_max         3.945
_refine_diff_density_min         -4.547
_refine_diff_density_rms         0.461

_shelxl_version_number           2014-3


# SQUEEZE RESULTS (Version = 230318)
# Note: Data are Listed for all Voids in the P1 Unit Cell
# i.e. Centre of Gravity, Solvent Accessible Volume,
# Recovered number of Electrons in the Void and
# Details about the Squeezed Material
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.065 0.482 0.546 1396 629 ' '
_platon_squeeze_void_probe_radius 1.20
_platon_squeeze_details          ?
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_5
_database_code_depnum_ccdc_archive 'CCDC 1818608'
_audit_update_record             
;
2018-06-07 deposited with the CCDC.
2018-06-08 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C18 H45 Ce2 N3 O59.50 P W11'
_chemical_formula_weight         3589.13

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'
Ce Ce -0.2486 2.6331 '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'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   13.0263(13)
_cell_length_b                   14.3304(14)
_cell_length_c                   21.410(2)
_cell_angle_alpha                96.253(2)
_cell_angle_beta                 91.877(2)
_cell_angle_gamma                95.276(2)
_cell_volume                     3952.4(7)
_cell_formula_units_Z            2
_cell_measurement_temperature    200(2)
_cell_measurement_reflns_used    20170
_cell_measurement_theta_min      1.805
_cell_measurement_theta_max      25.00

_exptl_crystal_description       'block '
_exptl_crystal_colour            'orange yellow'
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    3.016
_exptl_crystal_F_000             3190
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.03
_exptl_absorpt_coefficient_mu    17.176
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.443
_exptl_absorpt_correction_T_max  0.597
_exptl_absorpt_process_details   'SADABS; Sheldrick, 1996'

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      200(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'Bruker Smart Apex CCD'
_diffrn_measurement_method       ω-2θ
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            20170
_diffrn_reflns_av_unetI/netI     0.0562
_diffrn_reflns_av_R_equivalents  0.0264
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         1.805
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.980
_diffrn_measured_fraction_theta_full 0.953
_diffrn_reflns_Laue_measured_fraction_max 0.980
_diffrn_reflns_Laue_measured_fraction_full 0.953
_diffrn_reflns_point_group_measured_fraction_max 0.980
_diffrn_reflns_point_group_measured_fraction_full 0.953
_reflns_number_total             13625
_reflns_number_gt                10386
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
During the refinement, the command 'omit -3 50' was used to omit the weak reflections above 50 degree.
 Some O atoms on the polyoxoanions, C and N atoms on the organic ligands, and coordinated water molecules
are retrained with the command 'isor'. Ce(2) and O6W are structually restrained  with the command 'DELU'. 
All these restrained refinement led to a  restraint value of 122. Rint after the absorption correction
 process is 0.0264, which indicates that the absorption correction process is effective.In the final refinement,
'squeeze' command was used to deal with the water molecules of solvation.The highest residual peak is 
close to W(3) with the distance of 0.88 A, indicative an featureless peak.
The deepest hole is  close to the heavy metal center Ce(2). And, the Ce(2) freely refines to an occupancy 
of  around 90%, indicating the general disorder around this area.
;

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXS-2014 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
;
 Refined as a 2-component perfect inversion twin.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0716P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         13625
_refine_ls_number_parameters     793
_refine_ls_number_restraints     122
_refine_ls_R_factor_all          0.0588
_refine_ls_R_factor_gt           0.0451
_refine_ls_wR_factor_ref         0.1265
_refine_ls_wR_factor_gt          0.1204
_refine_ls_goodness_of_fit_ref   1.020
_refine_ls_restrained_S_all      1.024
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000

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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
W1 W 1.04097(5) 0.30433(4) 0.33368(3) 0.03544(15) Uani 1 1 d . . . . .
W2 W 0.67835(5) 0.37803(4) 0.36634(3) 0.04161(17) Uani 1 1 d . . . . .
W3 W 0.66044(5) 0.43486(4) 0.20235(3) 0.03533(15) Uani 1 1 d . . . . .
W4 W 0.81365(5) 0.19457(4) 0.40313(3) 0.04231(17) Uani 1 1 d . . . . .
W5 W 0.56969(4) 0.20550(4) 0.15543(3) 0.03076(14) Uani 1 1 d . . . . .
W6 W 0.94763(4) 0.05636(4) 0.27607(2) 0.02766(13) Uani 1 1 d . . . . .
W7 W 0.90798(5) 0.48570(4) 0.29511(3) 0.03838(16) Uani 1 1 d . . . . .
W8 W 0.58379(5) 0.14879(4) 0.31742(3) 0.03965(16) Uani 1 1 d . . . . .
W9 W 0.78675(4) 0.29927(3) 0.08713(2) 0.02619(13) Uani 1 1 d . . . . .
W10 W 1.02903(4) 0.34763(3) 0.17803(2) 0.02844(14) Uani 1 1 d . . . . .
W11 W 0.72058(4) 0.00868(3) 0.19275(2) 0.02537(13) Uani 1 1 d . . . . .
Ce1 Ce 0.96244(5) 0.07442(5) 0.09050(3) 0.02278(16) Uani 1 1 d . . . . .
Ce2 Ce 1.16853(8) -0.12199(9) 0.32090(6) 0.0692(3) Uani 1 1 d . U . . .
P1 P 0.8048(2) 0.2451(2) 0.24492(14) 0.0203(7) Uani 1 1 d . . . . .
O1 O 0.7362(7) 0.2794(6) 0.1947(4) 0.036(2) Uani 1 1 d . . . . .
O2 O 0.8324(7) 0.1435(6) 0.2252(4) 0.037(2) Uani 1 1 d . . . . .
O3 O 0.7472(8) 0.2467(6) 0.3086(4) 0.042(3) Uani 1 1 d . . . . .
O4 O 0.9039(7) 0.3145(6) 0.2575(4) 0.035(2) Uani 1 1 d . . . . .
O5 O 0.6239(9) 0.4599(8) 0.4148(5) 0.063(3) Uani 1 1 d . . . . .
O6 O 0.8408(9) 0.1626(8) 0.4776(5) 0.057(3) Uani 1 1 d . . . . .
O7 O 0.5969(8) 0.5327(7) 0.1944(5) 0.050(3) Uani 1 1 d . . . . .
O8 O 0.5748(8) 0.2783(6) 0.3570(5) 0.048(3) Uani 1 1 d . . . . .
O9 O 1.1477(8) 0.3118(7) 0.3831(4) 0.047(3) Uani 1 1 d . . . . .
O10 O 1.1252(7) 0.3983(7) 0.1357(5) 0.049(3) Uani 1 1 d . . . . .
O11 O 0.9329(9) 0.6029(7) 0.3217(5) 0.057(3) Uani 1 1 d . . . . .
O12 O 0.9340(8) 0.2750(6) 0.3883(4) 0.048(3) Uani 1 1 d . . . . .
O13 O 0.7508(10) 0.3149(7) 0.4232(5) 0.060(3) Uani 1 1 d . . . . .
O14 O 0.6479(7) 0.0566(6) 0.2703(4) 0.041(2) Uani 1 1 d . . . . .
O15 O 0.6339(8) 0.4088(7) 0.2864(5) 0.052(3) Uani 1 1 d . . . . .
O16 O 0.6353(7) 0.0943(6) 0.1550(4) 0.037(2) Uani 1 1 d . . . . .
O17 O 0.4541(7) 0.1680(7) 0.1160(5) 0.041(2) Uani 1 1 d . . . . .
O18 O 1.1019(7) 0.3339(7) 0.2569(5) 0.043(2) Uani 1 1 d . . . . .
O19 O 0.7184(7) 0.4161(6) 0.1244(5) 0.042(2) Uani 1 1 d . . . . .
O20 O 0.8075(8) 0.4411(7) 0.3516(4) 0.045(3) Uani 1 1 d . . . . .
O21 O 0.7951(7) 0.4855(6) 0.2375(4) 0.040(2) Uani 1 1 d . . . . .
O22 O 0.9960(6) 0.0402(6) 0.2002(4) 0.032(2) Uani 1 1 d . . . . .
O23 O 0.6413(7) -0.0955(6) 0.1809(4) 0.039(2) Uani 1 1 d . . . . .
O24 O 0.5528(7) 0.3384(7) 0.1749(5) 0.046(3) Uani 1 1 d . . . . .
O25 O 0.7935(8) 0.3298(7) 0.0121(4) 0.044(3) Uani 1 1 d . . . . .
O26 O 1.0260(7) 0.1742(6) 0.3004(4) 0.039(2) Uani 1 1 d . . . . .
O27 O 0.5446(7) 0.1957(6) 0.2418(4) 0.038(2) Uani 1 1 d . . . . .
O28 O 0.7978(6) 0.0000(6) 0.1268(4) 0.034(2) Uani 1 1 d . . . . .
O29 O 0.8605(8) 0.1013(6) 0.3508(4) 0.042(2) Uani 1 1 d . . . . .
O30 O 1.0220(7) 0.2261(6) 0.1526(4) 0.036(2) Uani 1 1 d . . . . .
O31 O 0.9089(7) 0.3666(6) 0.1281(4) 0.033(2) Uani 1 1 d . . . . .
O32 O 0.9947(8) 0.4719(6) 0.2279(5) 0.044(3) Uani 1 1 d . . . . .
O33 O 0.4726(8) 0.0884(7) 0.3386(5) 0.050(3) Uani 1 1 d . . . . .
O34 O 0.8221(6) -0.0238(6) 0.2515(4) 0.034(2) Uani 1 1 d . . . . .
O35 O 0.8363(6) 0.1887(5) 0.0847(4) 0.030(2) Uani 1 1 d . . . . .
O36 O 1.0081(8) 0.4317(6) 0.3451(4) 0.042(2) Uani 1 1 d . . . . .
O37 O 0.6448(6) 0.2416(6) 0.0860(4) 0.030(2) Uani 1 1 d . . . . .
O38 O 0.6744(8) 0.1366(7) 0.3900(5) 0.051(3) Uani 1 1 d . . . . .
O39 O 1.0159(8) -0.0188(6) 0.3148(4) 0.045(3) Uani 1 1 d . . . . .
O40 O 0.8661(6) 0.0094(6) -0.0065(4) 0.0269(19) Uani 1 1 d . U . . .
O41 O 0.8454(6) -0.0561(6) -0.1057(4) 0.033(2) Uani 1 1 d . . . . .
O42 O 1.0357(7) 0.1770(6) 0.0133(4) 0.034(2) Uani 1 1 d . . . . .
O43 O 1.0245(7) 0.1005(6) -0.0837(4) 0.033(2) Uani 1 1 d . . . . .
O44 O 1.2320(16) 0.0401(16) 0.3171(11) 0.156(8) Uani 1 1 d . U . . .
O45 O 1.2845(15) 0.1640(14) 0.4126(10) 0.139(7) Uani 1 1 d . . . . .
C1 C 0.8206(10) -0.0074(8) -0.0573(7) 0.031(3) Uani 1 1 d . . . . .
C2 C 0.7086(9) 0.0296(8) -0.0657(6) 0.025(3) Uani 1 1 d . . . . .
C3 C 0.6615(11) 0.0660(11) -0.0121(7) 0.047(4) Uani 1 1 d . . . . .
H3A H 0.6929 0.0679 0.0277 0.056 Uiso 1 1 calc R U . . .
C4 C 0.5678(11) 0.0986(9) -0.0205(8) 0.045(4) Uani 1 1 d . . . . .
H4A H 0.5339 0.1244 0.0139 0.053 Uiso 1 1 calc R U . . .
C5 C 0.5703(10) 0.0619(11) -0.1287(7) 0.046(4) Uani 1 1 d . . . . .
H5A H 0.5375 0.0629 -0.1678 0.055 Uiso 1 1 calc R U . . .
C6 C 0.6628(10) 0.0282(10) -0.1253(6) 0.035(3) Uani 1 1 d . U . . .
H6A H 0.6947 0.0051 -0.1612 0.042 Uiso 1 1 calc R U . . .
C7 C 1.0396(10) 0.1697(8) -0.0449(6) 0.027(3) Uani 1 1 d . U . . .
C8 C 1.0652(10) 0.2639(9) -0.0748(7) 0.034(3) Uani 1 1 d . . . . .
C9 C 1.0661(15) 0.3484(10) -0.0362(8) 0.067(6) Uani 1 1 d . . . . .
H9A H 1.0524 0.3495 0.0062 0.080 Uiso 1 1 calc R U . . .
C10 C 1.0886(17) 0.4327(11) -0.0639(9) 0.078(6) Uani 1 1 d . . . . .
H10A H 1.0909 0.4903 -0.0390 0.093 Uiso 1 1 calc R U . . .
C11 C 1.1163(17) 0.3446(11) -0.1627(8) 0.073(6) Uani 1 1 d . . . . .
H11A H 1.1369 0.3427 -0.2040 0.088 Uiso 1 1 calc R U . . .
C12 C 1.0925(14) 0.2643(10) -0.1332(9) 0.059(5) Uani 1 1 d . . . . .
H12A H 1.0961 0.2063 -0.1567 0.071 Uiso 1 1 calc R U . . .
C13 C 1.260(3) 0.129(3) 0.3489(15) 0.161(13) Uani 1 1 d D U . . .
C14 C 1.2801(12) 0.1863(9) 0.2987(7) 0.134(10) Uani 1 1 d DG U . . .
C15 C 1.2484(9) 0.1644(8) 0.2358(7) 0.072(5) Uani 1 1 d G U . . .
H15A H 1.2099 0.1074 0.2225 0.087 Uiso 1 1 calc R U . . .
C16 C 1.2741(10) 0.2278(11) 0.1928(5) 0.116(9) Uani 1 1 d G U . . .
H16A H 1.2529 0.2132 0.1507 0.139 Uiso 1 1 calc R U . . .
N3 N 1.3316(11) 0.3131(9) 0.2127(7) 0.108(7) Uani 1 1 d G U . . .
H3B H 1.3475 0.3523 0.1861 0.130 Uiso 1 1 calc R U . . .
C17 C 1.3634(9) 0.3349(8) 0.2756(7) 0.073(5) Uani 1 1 d G U . . .
H17A H 1.4018 0.3919 0.2890 0.087 Uiso 1 1 calc R U . . .
C18 C 1.3376(11) 0.2715(11) 0.3187(5) 0.084(6) Uani 1 1 d G U . . .
H18A H 1.3589 0.2861 0.3608 0.100 Uiso 1 1 calc R U . . .
N1 N 0.5254(8) 0.0934(8) -0.0778(6) 0.040(3) Uani 1 1 d . . . . .
H1A H 0.4648 0.1118 -0.0820 0.048 Uiso 1 1 calc R U . . .
N2 N 1.1062(12) 0.4314(9) -0.1232(6) 0.062(4) Uani 1 1 d . . . . .
H2A H 1.1120 0.4838 -0.1395 0.074 Uiso 1 1 calc R U . . .
O1W O 1.1304(7) -0.1054(8) 0.2074(5) 0.054(3) Uani 1 1 d . U . . .
H1WA H 1.1465 -0.0481 0.1917 0.065 Uiso 1 1 d R U . . .
H1WB H 1.0989 -0.1567 0.1812 0.065 Uiso 1 1 d R U . . .
O2W O 1.3406(19) -0.0758(18) 0.2873(12) 0.209(11) Uani 1 1 d . U . . .
H2WA H 1.3693 -0.1122 0.2607 0.251 Uiso 1 1 d R U . . .
H2WB H 1.3720 -0.0230 0.3022 0.251 Uiso 1 1 d R U . . .
O3W O 1.0033(16) -0.2175(12) 0.3093(11) 0.164(8) Uani 1 1 d . U . . .
H3WA H 0.9431 -0.1913 0.2990 0.197 Uiso 1 1 d R U . . .
H3WB H 1.0014 -0.2815 0.3134 0.197 Uiso 1 1 d R U . . .
O4W O 1.1073(13) -0.0810(12) 0.4201(8) 0.132(7) Uani 1 1 d . U . . .
H4WA H 1.1161 -0.0191 0.4391 0.159 Uiso 1 1 d R U . . .
H4WB H 1.0733 -0.1279 0.4407 0.159 Uiso 1 1 d R U . . .
O5W O 1.3261(18) -0.1042(19) 0.3904(12) 0.212(11) Uani 1 1 d . U . . .
H5WA H 1.3632 -0.0451 0.3950 0.255 Uiso 1 1 d R U . . .
H5WB H 1.3518 -0.1539 0.4085 0.255 Uiso 1 1 d R U . . .
O6W O 1.220(4) -0.250(2) 0.3835(15) 0.119(14) Uani 0.55(5) 1 d . U P A 1
H6WA H 1.2765 -0.2408 0.4120 0.143 Uiso 0.55(5) 1 d R U P A 1
H6WB H 1.1821 -0.3085 0.3763 0.143 Uiso 0.55(5) 1 d R U P A 1
O6WA O 1.141(4) -0.260(2) 0.3919(17) 0.087(14) Uani 0.45(5) 1 d . U P A 2
H6WC H 1.1585 -0.2490 0.4347 0.105 Uiso 0.45(5) 1 d R U P A 2
H6WD H 1.1128 -0.3197 0.3746 0.105 Uiso 0.45(5) 1 d R U P A 2
O7W O 1.291(3) -0.221(3) 0.2547(17) 0.143(14) Uani 0.5 1 d . U P A 5
H7WA H 1.2496 -0.2670 0.2377 0.171 Uiso 0.5 1 d R U P A 5
H7WB H 1.3557 -0.2239 0.2527 0.171 Uiso 0.5 1 d R U P A 5
O7WA O 1.129(3) -0.301(3) 0.2507(19) 0.146(14) Uani 0.5 1 d . U P A 6
H7WC H 1.1728 -0.3251 0.2270 0.175 Uiso 0.5 1 d R U P A 6
H7WD H 1.0702 -0.3303 0.2539 0.175 Uiso 0.5 1 d R U P A 6


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
W1 O9 1.706(10) . ?
W1 O12 1.896(9) . ?
W1 O36 1.905(9) . ?
W1 O26 1.913(8) . ?
W1 O18 1.921(10) . ?
W1 O4 2.404(9) . ?
W2 O5 1.700(10) . ?
W2 O8 1.862(9) . ?
W2 O13 1.874(11) . ?
W2 O20 1.888(9) . ?
W2 O15 1.899(11) . ?
W2 O3 2.398(8) . ?
W3 O7 1.713(10) . ?
W3 O19 1.857(10) . ?
W3 O24 1.906(10) . ?
W3 O15 1.913(10) . ?
W3 O21 1.932(9) . ?
W3 O1 2.509(9) . ?
W4 O6 1.741(10) . ?
W4 O29 1.813(10) . ?
W4 O12 1.914(9) . ?
W4 O38 1.923(10) . ?
W4 O13 1.988(10) . ?
W4 O3 2.396(10) . ?
W5 O17 1.713(9) . ?
W5 O16 1.875(9) . ?
W5 O37 1.898(9) . ?
W5 O27 1.907(9) . ?
W5 O24 1.939(9) . ?
W5 O1 2.408(9) . ?
W6 O39 1.720(10) . ?
W6 O22 1.760(9) . ?
W6 O26 1.902(8) . ?
W6 O34 1.933(8) . ?
W6 O29 2.071(10) . ?
W6 O2 2.353(10) . ?
W7 O11 1.712(9) . ?
W7 O32 1.863(9) . ?
W7 O21 1.887(10) . ?
W7 O20 1.924(9) . ?
W7 O36 1.929(10) . ?
W7 O4 2.493(8) . ?
W8 O33 1.717(9) . ?
W8 O14 1.851(9) . ?
W8 O27 1.892(9) . ?
W8 O38 1.953(11) . ?
W8 O8 1.970(9) . ?
W8 O3 2.464(9) . ?
W9 O25 1.714(9) . ?
W9 O35 1.762(8) . ?
W9 O31 1.917(9) . ?
W9 O37 1.953(8) . ?
W9 O19 2.065(9) . ?
W9 O1 2.455(9) . ?
W10 O10 1.723(9) . ?
W10 O30 1.760(8) . ?
W10 O31 1.923(9) . ?
W10 O18 1.947(9) . ?
W10 O32 2.067(9) . ?
W10 O4 2.447(9) . ?
W11 O23 1.725(9) . ?
W11 O28 1.760(8) . ?
W11 O34 1.918(8) . ?
W11 O16 1.950(9) . ?
W11 O14 2.024(9) . ?
W11 O2 2.337(8) . ?
Ce1 O35 2.433(8) . ?
Ce1 O40 2.440(8) . ?
Ce1 O30 2.467(8) . ?
Ce1 O22 2.485(9) . ?
Ce1 O42 2.486(9) . ?
Ce1 O28 2.492(8) . ?
Ce1 O43 2.516(8) 2_755 ?
Ce1 O41 2.554(8) 2_755 ?
Ce2 O4W 2.327(19) . ?
Ce2 O44 2.40(2) . ?
Ce2 O2W 2.43(2) . ?
Ce2 O3W 2.432(19) . ?
Ce2 O5W 2.47(2) . ?
Ce2 O1W 2.505(10) . ?
Ce2 O6W 2.51(3) . ?
Ce2 O7W 2.59(4) . ?
Ce2 O39 2.593(10) . ?
Ce2 O6WA 2.63(3) . ?
Ce2 O7WA 2.82(4) . ?
P1 O1 1.526(9) . ?
P1 O2 1.549(9) . ?
P1 O4 1.553(9) . ?
P1 O3 1.575(8) . ?
O40 C1 1.211(16) . ?
O41 C1 1.253(15) . ?
O41 Ce1 2.554(8) 2_755 ?
O42 C7 1.241(15) . ?
O43 C7 1.220(14) . ?
O43 Ce1 2.516(8) 2_755 ?
O44 C13 1.38(4) . ?
O45 C13 1.42(4) . ?
C1 C2 1.608(17) . ?
C2 C6 1.389(17) . ?
C2 C3 1.392(17) . ?
C3 C4 1.360(19) . ?
C4 N1 1.322(19) . ?
C5 N1 1.309(18) . ?
C5 C6 1.341(18) . ?
C7 C8 1.569(17) . ?
C8 C12 1.31(2) . ?
C8 C9 1.389(18) . ?
C9 C10 1.41(2) . ?
C10 N2 1.29(2) . ?
C11 C12 1.39(2) . ?
C11 N2 1.45(2) . ?
C13 C14 1.442(10) . ?
C14 C15 1.3900 . ?
C14 C18 1.3900 . ?
C15 C16 1.3900 . ?
C16 N3 1.3900 . ?
N3 C17 1.3900 . ?
C17 C18 1.3900 . ?

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
_geom_angle_publ_flag
O9 W1 O12 101.5(5) . . ?
O9 W1 O36 100.3(4) . . ?
O12 W1 O36 87.8(4) . . ?
O9 W1 O26 102.8(4) . . ?
O12 W1 O26 87.5(4) . . ?
O36 W1 O26 157.0(4) . . ?
O9 W1 O18 101.2(4) . . ?
O12 W1 O18 157.3(4) . . ?
O36 W1 O18 86.9(4) . . ?
O26 W1 O18 88.8(4) . . ?
O9 W1 O4 171.1(4) . . ?
O12 W1 O4 85.4(4) . . ?
O36 W1 O4 74.2(3) . . ?
O26 W1 O4 82.9(4) . . ?
O18 W1 O4 71.9(3) . . ?
O5 W2 O8 101.8(5) . . ?
O5 W2 O13 102.4(5) . . ?
O8 W2 O13 89.7(5) . . ?
O5 W2 O20 102.8(5) . . ?
O8 W2 O20 155.4(4) . . ?
O13 W2 O20 86.1(5) . . ?
O5 W2 O15 100.8(5) . . ?
O8 W2 O15 87.8(4) . . ?
O13 W2 O15 156.6(5) . . ?
O20 W2 O15 86.5(4) . . ?
O5 W2 O3 171.7(5) . . ?
O8 W2 O3 72.7(4) . . ?
O13 W2 O3 71.7(4) . . ?
O20 W2 O3 83.0(4) . . ?
O15 W2 O3 85.4(4) . . ?
O7 W3 O19 101.4(5) . . ?
O7 W3 O24 99.9(5) . . ?
O19 W3 O24 89.6(4) . . ?
O7 W3 O15 103.5(5) . . ?
O19 W3 O15 155.2(4) . . ?
O24 W3 O15 87.3(4) . . ?
O7 W3 O21 104.1(4) . . ?
O19 W3 O21 88.4(4) . . ?
O24 W3 O21 155.9(4) . . ?
O15 W3 O21 84.5(4) . . ?
O7 W3 O1 169.2(4) . . ?
O19 W3 O1 71.9(3) . . ?
O24 W3 O1 72.0(4) . . ?
O15 W3 O1 83.7(4) . . ?
O21 W3 O1 84.5(3) . . ?
O6 W4 O29 103.4(5) . . ?
O6 W4 O12 102.9(5) . . ?
O29 W4 O12 89.1(4) . . ?
O6 W4 O38 99.1(5) . . ?
O29 W4 O38 91.0(4) . . ?
O12 W4 O38 157.3(4) . . ?
O6 W4 O13 102.1(5) . . ?
O29 W4 O13 154.4(4) . . ?
O12 W4 O13 84.3(5) . . ?
O38 W4 O13 86.0(5) . . ?
O6 W4 O3 169.5(4) . . ?
O29 W4 O3 84.7(4) . . ?
O12 W4 O3 83.7(4) . . ?
O38 W4 O3 73.8(4) . . ?
O13 W4 O3 70.0(4) . . ?
O17 W5 O16 103.0(4) . . ?
O17 W5 O37 98.2(4) . . ?
O16 W5 O37 91.4(4) . . ?
O17 W5 O27 105.1(4) . . ?
O16 W5 O27 87.4(4) . . ?
O37 W5 O27 156.3(4) . . ?
O17 W5 O24 100.0(4) . . ?
O16 W5 O24 157.0(4) . . ?
O37 W5 O24 86.1(4) . . ?
O27 W5 O24 85.8(4) . . ?
O17 W5 O1 168.4(4) . . ?
O16 W5 O1 83.4(4) . . ?
O37 W5 O1 71.8(3) . . ?
O27 W5 O1 84.6(4) . . ?
O24 W5 O1 74.0(4) . . ?
O39 W6 O22 101.3(4) . . ?
O39 W6 O26 101.5(4) . . ?
O22 W6 O26 95.4(4) . . ?
O39 W6 O34 100.7(4) . . ?
O22 W6 O34 92.9(4) . . ?
O26 W6 O34 154.3(4) . . ?
O39 W6 O29 96.9(4) . . ?
O22 W6 O29 161.7(4) . . ?
O26 W6 O29 82.5(4) . . ?
O34 W6 O29 82.0(4) . . ?
O39 W6 O2 171.4(4) . . ?
O22 W6 O2 82.1(4) . . ?
O26 W6 O2 85.9(4) . . ?
O34 W6 O2 71.1(3) . . ?
O29 W6 O2 79.6(4) . . ?
O11 W7 O32 102.4(4) . . ?
O11 W7 O21 102.4(5) . . ?
O32 W7 O21 89.4(4) . . ?
O11 W7 O20 103.3(4) . . ?
O32 W7 O20 154.3(4) . . ?
O21 W7 O20 85.8(4) . . ?
O11 W7 O36 101.0(5) . . ?
O32 W7 O36 88.2(4) . . ?
O21 W7 O36 156.5(4) . . ?
O20 W7 O36 86.3(4) . . ?
O11 W7 O4 170.3(4) . . ?
O32 W7 O4 71.6(3) . . ?
O21 W7 O4 85.4(3) . . ?
O20 W7 O4 82.8(4) . . ?
O36 W7 O4 71.7(3) . . ?
O33 W8 O14 103.2(4) . . ?
O33 W8 O27 103.9(5) . . ?
O14 W8 O27 88.8(4) . . ?
O33 W8 O38 99.8(5) . . ?
O14 W8 O38 89.9(4) . . ?
O27 W8 O38 155.9(4) . . ?
O33 W8 O8 103.4(4) . . ?
O14 W8 O8 153.4(4) . . ?
O27 W8 O8 85.3(4) . . ?
O38 W8 O8 85.1(4) . . ?
O33 W8 O3 169.0(4) . . ?
O14 W8 O3 84.1(3) . . ?
O27 W8 O3 84.2(4) . . ?
O38 W8 O3 71.7(3) . . ?
O8 W8 O3 69.6(3) . . ?
O25 W9 O35 105.5(4) . . ?
O25 W9 O31 102.5(4) . . ?
O35 W9 O31 93.9(4) . . ?
O25 W9 O37 101.1(4) . . ?
O35 W9 O37 91.9(4) . . ?
O31 W9 O37 153.1(4) . . ?
O25 W9 O19 96.5(4) . . ?
O35 W9 O19 157.9(4) . . ?
O31 W9 O19 83.1(4) . . ?
O37 W9 O19 81.7(4) . . ?
O25 W9 O1 164.6(4) . . ?
O35 W9 O1 87.7(4) . . ?
O31 W9 O1 84.1(3) . . ?
O37 W9 O1 69.9(3) . . ?
O19 W9 O1 70.2(3) . . ?
O10 W10 O30 105.1(5) . . ?
O10 W10 O31 100.7(4) . . ?
O30 W10 O31 93.6(4) . . ?
O10 W10 O18 102.3(5) . . ?
O30 W10 O18 93.1(4) . . ?
O31 W10 O18 153.4(4) . . ?
O10 W10 O32 96.1(4) . . ?
O30 W10 O32 158.9(4) . . ?
O31 W10 O32 82.4(4) . . ?
O18 W10 O32 82.1(4) . . ?
O10 W10 O4 164.5(4) . . ?
O30 W10 O4 89.3(4) . . ?
O31 W10 O4 83.9(3) . . ?
O18 W10 O4 70.5(4) . . ?
O32 W10 O4 69.7(3) . . ?
O23 W11 O28 102.2(4) . . ?
O23 W11 O34 100.6(4) . . ?
O28 W11 O34 96.2(4) . . ?
O23 W11 O16 101.1(4) . . ?
O28 W11 O16 91.7(4) . . ?
O34 W11 O16 154.7(4) . . ?
O23 W11 O14 93.2(4) . . ?
O28 W11 O14 164.1(4) . . ?
O34 W11 O14 84.8(4) . . ?
O16 W11 O14 81.2(4) . . ?
O23 W11 O2 170.8(4) . . ?
O28 W11 O2 83.9(4) . . ?
O34 W11 O2 71.7(3) . . ?
O16 W11 O2 85.4(4) . . ?
O14 W11 O2 81.3(3) . . ?
O35 Ce1 O40 79.5(3) . . ?
O35 Ce1 O30 68.5(3) . . ?
O40 Ce1 O30 141.5(3) . . ?
O35 Ce1 O22 111.8(3) . . ?
O40 Ce1 O22 141.4(3) . . ?
O30 Ce1 O22 73.1(3) . . ?
O35 Ce1 O42 77.1(3) . . ?
O40 Ce1 O42 77.8(3) . . ?
O30 Ce1 O42 74.7(3) . . ?
O22 Ce1 O42 139.8(3) . . ?
O35 Ce1 O28 73.5(3) . . ?
O40 Ce1 O28 75.9(3) . . ?
O30 Ce1 O28 113.0(3) . . ?
O22 Ce1 O28 72.8(3) . . ?
O42 Ce1 O28 143.4(3) . . ?
O35 Ce1 O43 141.4(3) . 2_755 ?
O40 Ce1 O43 75.1(3) . 2_755 ?
O30 Ce1 O43 143.2(3) . 2_755 ?
O22 Ce1 O43 74.3(3) . 2_755 ?
O42 Ce1 O43 124.0(3) . 2_755 ?
O28 Ce1 O43 72.4(3) . 2_755 ?
O35 Ce1 O41 144.1(3) . 2_755 ?
O40 Ce1 O41 121.2(3) . 2_755 ?
O30 Ce1 O41 79.3(3) . 2_755 ?
O22 Ce1 O41 71.7(3) . 2_755 ?
O42 Ce1 O41 79.3(3) . 2_755 ?
O28 Ce1 O41 136.5(3) . 2_755 ?
O43 Ce1 O41 74.6(3) 2_755 2_755 ?
O4W Ce2 O44 89.3(7) . . ?
O4W Ce2 O2W 125.4(7) . . ?
O44 Ce2 O2W 57.6(8) . . ?
O4W Ce2 O3W 81.1(7) . . ?
O44 Ce2 O3W 137.7(7) . . ?
O2W Ce2 O3W 152.8(8) . . ?
O4W Ce2 O5W 76.7(7) . . ?
O44 Ce2 O5W 77.4(8) . . ?
O2W Ce2 O5W 55.9(9) . . ?
O3W Ce2 O5W 138.1(8) . . ?
O4W Ce2 O1W 140.6(4) . . ?
O44 Ce2 O1W 79.4(6) . . ?
O2W Ce2 O1W 79.3(7) . . ?
O3W Ce2 O1W 82.4(6) . . ?
O5W Ce2 O1W 135.2(7) . . ?
O4W Ce2 O6W 76.2(9) . . ?
O44 Ce2 O6W 134.2(13) . . ?
O2W Ce2 O6W 96.2(14) . . ?
O3W Ce2 O6W 83.4(13) . . ?
O5W Ce2 O6W 57.1(13) . . ?
O1W Ce2 O6W 136.6(9) . . ?
O4W Ce2 O7W 146.7(9) . . ?
O44 Ce2 O7W 106.0(11) . . ?
O2W Ce2 O7W 50.8(10) . . ?
O3W Ce2 O7W 104.2(10) . . ?
O5W Ce2 O7W 78.1(10) . . ?
O1W Ce2 O7W 72.3(8) . . ?
O4W Ce2 O39 68.7(4) . . ?
O44 Ce2 O39 69.7(6) . . ?
O2W Ce2 O39 123.5(7) . . ?
O3W Ce2 O39 68.4(5) . . ?
O5W Ce2 O39 131.7(6) . . ?
O1W Ce2 O39 72.0(3) . . ?
O6W Ce2 O39 137.4(12) . . ?
O7W Ce2 O39 144.2(8) . . ?
O4W Ce2 O6WA 64.4(10) . . ?
O44 Ce2 O6WA 145.9(9) . . ?
O2W Ce2 O6WA 119.5(13) . . ?
O3W Ce2 O6WA 62.7(11) . . ?
O5W Ce2 O6WA 75.7(12) . . ?
O1W Ce2 O6WA 134.7(8) . . ?
O39 Ce2 O6WA 115.3(11) . . ?
O4W Ce2 O7WA 125.0(9) . . ?
O44 Ce2 O7WA 145.0(10) . . ?
O2W Ce2 O7WA 100.1(10) . . ?
O3W Ce2 O7WA 54.2(10) . . ?
O5W Ce2 O7WA 114.3(10) . . ?
O1W Ce2 O7WA 69.4(7) . . ?
O39 Ce2 O7WA 113.0(8) . . ?
O1 P1 O2 111.5(5) . . ?
O1 P1 O4 109.1(5) . . ?
O2 P1 O4 110.8(5) . . ?
O1 P1 O3 109.5(5) . . ?
O2 P1 O3 108.9(5) . . ?
O4 P1 O3 106.9(5) . . ?
P1 O1 W5 125.9(5) . . ?
P1 O1 W9 124.7(5) . . ?
W5 O1 W9 90.6(3) . . ?
P1 O1 W3 126.0(5) . . ?
W5 O1 W3 88.1(3) . . ?
W9 O1 W3 90.2(3) . . ?
P1 O2 W11 128.2(5) . . ?
P1 O2 W6 128.4(5) . . ?
W11 O2 W6 92.2(3) . . ?
P1 O3 W4 124.8(5) . . ?
P1 O3 W2 127.9(5) . . ?
W4 O3 W2 91.8(3) . . ?
P1 O3 W8 121.6(5) . . ?
W4 O3 W8 89.8(3) . . ?
W2 O3 W8 90.0(3) . . ?
P1 O4 W1 126.0(5) . . ?
P1 O4 W10 124.3(5) . . ?
W1 O4 W10 90.9(3) . . ?
P1 O4 W7 125.3(5) . . ?
W1 O4 W7 88.3(3) . . ?
W10 O4 W7 91.1(3) . . ?
W2 O8 W8 127.6(5) . . ?
W1 O12 W4 147.7(5) . . ?
W2 O13 W4 126.1(5) . . ?
W8 O14 W11 151.8(5) . . ?
W2 O15 W3 151.5(6) . . ?
W5 O16 W11 153.5(5) . . ?
W1 O18 W10 126.7(5) . . ?
W3 O19 W9 127.5(5) . . ?
W2 O20 W7 150.9(6) . . ?
W7 O21 W3 151.6(5) . . ?
W6 O22 Ce1 141.9(4) . . ?
W3 O24 W5 125.6(5) . . ?
W6 O26 W1 153.2(6) . . ?
W8 O27 W5 147.9(5) . . ?
W11 O28 Ce1 139.3(5) . . ?
W4 O29 W6 151.0(5) . . ?
W10 O30 Ce1 158.5(5) . . ?
W9 O31 W10 141.3(5) . . ?
W7 O32 W10 127.5(5) . . ?
W11 O34 W6 122.6(5) . . ?
W9 O35 Ce1 158.9(4) . . ?
W1 O36 W7 125.7(5) . . ?
W5 O37 W9 127.6(5) . . ?
W4 O38 W8 124.6(5) . . ?
W6 O39 Ce2 150.4(5) . . ?
C1 O40 Ce1 168.9(8) . . ?
C1 O41 Ce1 106.4(8) . 2_755 ?
C7 O42 Ce1 134.9(8) . . ?
C7 O43 Ce1 138.8(8) . 2_755 ?
C13 O44 Ce2 148.5(17) . . ?
O40 C1 O41 128.9(12) . . ?
O40 C1 C2 118.6(11) . . ?
O41 C1 C2 112.4(12) . . ?
C6 C2 C3 121.5(12) . . ?
C6 C2 C1 120.3(11) . . ?
C3 C2 C1 118.2(11) . . ?
C4 C3 C2 117.2(14) . . ?
N1 C4 C3 119.4(13) . . ?
N1 C5 C6 121.1(14) . . ?
C5 C6 C2 116.9(13) . . ?
O43 C7 O42 130.3(12) . . ?
O43 C7 C8 113.4(12) . . ?
O42 C7 C8 116.3(10) . . ?
C12 C8 C9 119.8(13) . . ?
C12 C8 C7 121.9(13) . . ?
C9 C8 C7 118.0(13) . . ?
C8 C9 C10 117.4(15) . . ?
N2 C10 C9 121.4(16) . . ?
C12 C11 N2 113.5(15) . . ?
C8 C12 C11 125.1(15) . . ?
O44 C13 O45 134.9(18) . . ?
O44 C13 C14 103(3) . . ?
O45 C13 C14 121(3) . . ?
C15 C14 C18 120.0 . . ?
C15 C14 C13 127(2) . . ?
C18 C14 C13 113(2) . . ?
C14 C15 C16 120.0 . . ?
C15 C16 N3 120.0 . . ?
C17 N3 C16 120.0 . . ?
N3 C17 C18 120.0 . . ?
C17 C18 C14 120.0 . . ?
C5 N1 C4 123.9(12) . . ?
C10 N2 C11 122.0(13) . . ?

_refine_diff_density_max         3.116
_refine_diff_density_min         -2.876
_refine_diff_density_rms         0.285

_shelxl_version_number           2014-3


# SQUEEZE RESULTS (Version = 230318)
# Note: Data are Listed for all Voids in the P1 Unit Cell
# i.e. Centre of Gravity, Solvent Accessible Volume,
# Recovered number of Electrons in the Void and
# Details about the Squeezed Material
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.075 0.477 0.548 1395 566 ' '
_platon_squeeze_void_probe_radius 1.20
_platon_squeeze_details          ?


####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_4
_database_code_depnum_ccdc_archive 'CCDC 1818607'
_audit_update_record             
;
2018-06-07 deposited with the CCDC.
2018-06-08 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C18 H59 La2 N3 O66.50 P W11'
_chemical_formula_weight         3712.71

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'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   13.0114(5)
_cell_length_b                   14.3598(6)
_cell_length_c                   21.4373(8)
_cell_angle_alpha                96.428(2)
_cell_angle_beta                 91.620(2)
_cell_angle_gamma                95.623(2)
_cell_volume                     3957.9(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    27811
_cell_measurement_theta_min      1.630
_cell_measurement_theta_max      24.999

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    3.115
_exptl_crystal_F_000             3325
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_exptl_absorpt_coefficient_mu    17.094
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.058
_exptl_absorpt_correction_T_max  0.181
_exptl_absorpt_process_details   'SADABS; Sheldrick, 1996'

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'Bruker Smart Apex CCD'
_diffrn_measurement_method       ω-2θ
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            27811
_diffrn_reflns_av_unetI/netI     0.0871
_diffrn_reflns_av_R_equivalents  0.0564
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_theta_min         1.630
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measured_fraction_theta_full 0.965
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_Laue_measured_fraction_full 0.965
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_point_group_measured_fraction_full 0.965
_reflns_number_total             13825
_reflns_number_gt                10400
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
During the refinement, the command 'omit -3 50' was used to omit the weak reflections above 50 degree.
 Some O atoms on the polyoxoanions, C and N atoms on the organic ligands, and coordinated water molecules
are retrained with the command 'isor', which leds to a  restraint value of 180. Rint after the absorption 
correction process is 0.0564, which indicates that the absorption correction process is effective.
In the final refinement,'squeeze' command was used to deal with the water molecules of solvation.
The highest residual peak is close to W(3) with the distance of 0.86 A, indicative an featureless peak.
The deepest hole is  close to the heavy metal center La(2). And, the La(2) freely refines to an occupancy 
of  around 90%, indicating the general disorder around this area.
;

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXS-2014 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
;
 ?
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0721P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         13825
_refine_ls_number_parameters     782
_refine_ls_number_restraints     180
_refine_ls_R_factor_all          0.0715
_refine_ls_R_factor_gt           0.0550
_refine_ls_wR_factor_ref         0.1497
_refine_ls_wR_factor_gt          0.1414
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_restrained_S_all      1.058
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000

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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
W1 W 0.58246(5) 0.14814(5) 0.31756(3) 0.03266(18) Uani 1 1 d . . . . .
W2 W 0.90827(6) 0.48500(5) 0.29570(3) 0.03133(18) Uani 1 1 d . . . . .
W3 W 0.66129(5) 0.43378(5) 0.20301(3) 0.02868(17) Uani 1 1 d . . . . .
W4 W 0.71914(4) 0.00848(4) 0.19286(3) 0.01971(15) Uani 1 1 d . . . . .
W5 W 0.67728(6) 0.37711(5) 0.36673(3) 0.03375(18) Uani 1 1 d . . . . .
W6 W 0.94603(5) 0.05682(4) 0.27622(3) 0.02180(15) Uani 1 1 d . . . . .
W7 W 0.81181(6) 0.19453(5) 0.40319(3) 0.03512(19) Uani 1 1 d . . . . .
W8 W 1.04023(5) 0.30451(5) 0.33391(3) 0.02869(17) Uani 1 1 d . . . . .
W9 W 1.03000(5) 0.34808(4) 0.17880(3) 0.02252(15) Uani 1 1 d . . . . .
W10 W 0.78788(5) 0.29918(4) 0.08783(3) 0.02040(15) Uani 1 1 d . . . . .
W11 W 0.56974(5) 0.20482(5) 0.15603(3) 0.02424(16) Uani 1 1 d . . . . .
P1 P 0.8052(2) 0.2445(2) 0.24563(15) 0.0131(7) Uani 1 1 d . . . . .
La1 La 0.96345(6) 0.07418(6) 0.09020(4) 0.01724(19) Uani 1 1 d . . . . .
La2 La 1.16573(9) -0.12045(10) 0.32219(6) 0.0579(4) Uani 1 1 d . . . . .
O1 O 0.8320(7) 0.1440(7) 0.2247(5) 0.027(2) Uani 1 1 d . . . . .
O2 O 0.7366(8) 0.2777(7) 0.1953(5) 0.029(2) Uani 1 1 d . . . . .
O3 O 0.9034(8) 0.3149(7) 0.2577(4) 0.028(2) Uani 1 1 d . . . . .
O4 O 0.7439(9) 0.2442(8) 0.3078(4) 0.036(3) Uani 1 1 d . . . . .
O5 O 0.9949(8) 0.0410(7) 0.2006(5) 0.030(2) Uani 1 1 d . . . . .
O6 O 0.7955(8) 0.3281(8) 0.0134(5) 0.037(3) Uani 1 1 d . . . . .
O7 O 0.8078(8) 0.4423(9) 0.3530(5) 0.040(3) Uani 1 1 d . . . . .
O8 O 0.5989(10) 0.5325(8) 0.1978(6) 0.046(3) Uani 1 1 d . . . . .
O9 O 0.5426(8) 0.1945(8) 0.2403(5) 0.038(3) Uani 1 1 d . . . . .
O10 O 1.0231(7) 0.2280(7) 0.1538(4) 0.024(2) Uani 1 1 d . . . . .
O11 O 0.8344(7) 0.1897(6) 0.0849(4) 0.025(2) Uani 1 1 d . . . . .
O12 O 1.0998(8) 0.3348(8) 0.2581(5) 0.036(3) Uani 1 1 d . . . . .
O13 O 0.9105(8) 0.3651(7) 0.1299(4) 0.027(2) Uani 1 1 d . . . . .
O14 O 0.6341(8) 0.0944(7) 0.1557(4) 0.026(2) Uani 1 1 d . . . . .
O15 O 1.0231(8) 0.1742(7) 0.3005(5) 0.030(3) Uani 1 1 d . . . . .
O16 O 0.5551(8) 0.3376(8) 0.1745(5) 0.037(3) Uani 1 1 d . . . . .
O17 O 0.7981(8) -0.0006(8) 0.1269(4) 0.031(3) Uani 1 1 d . . . . .
O18 O 1.0074(8) 0.4321(8) 0.3456(5) 0.039(3) Uani 1 1 d . . . . .
O19 O 0.6411(8) -0.0967(7) 0.1822(5) 0.033(3) Uani 1 1 d . . . . .
O20 O 0.4566(8) 0.1688(8) 0.1180(5) 0.031(3) Uani 1 1 d . . . . .
O21 O 0.9318(8) 0.2762(8) 0.3875(4) 0.033(3) Uani 1 1 d . . . . .
O22 O 0.8603(8) 0.1028(8) 0.3504(5) 0.035(3) Uani 1 1 d . . . . .
O23 O 1.1448(9) 0.3111(8) 0.3839(5) 0.044(3) Uani 1 1 d . . . . .
O24 O 0.6712(10) 0.1357(8) 0.3905(6) 0.048(3) Uani 1 1 d . . . . .
O25 O 0.6475(8) 0.0610(8) 0.2721(5) 0.039(3) Uani 1 1 d . . . . .
O26 O 0.7496(10) 0.3130(8) 0.4237(5) 0.044(3) Uani 1 1 d . . . . .
O27 O 1.1301(8) 0.3984(8) 0.1376(6) 0.042(3) Uani 1 1 d . . . . .
O28 O 0.5730(8) 0.2768(8) 0.3589(5) 0.036(3) Uani 1 1 d . . . . .
O29 O 0.6214(10) 0.4591(10) 0.4165(6) 0.061(4) Uani 1 1 d . . . . .
O30 O 0.6333(8) 0.4076(7) 0.2883(5) 0.036(3) Uani 1 1 d . . . . .
O31 O 0.8358(9) 0.1651(9) 0.4766(5) 0.047(3) Uani 1 1 d . . . . .
O32 O 0.8209(8) -0.0250(8) 0.2502(5) 0.032(3) Uani 1 1 d . . . . .
O33 O 0.7980(9) 0.4853(7) 0.2371(5) 0.036(3) Uani 1 1 d . . . . .
O34 O 0.9956(8) 0.4721(7) 0.2306(5) 0.037(3) Uani 1 1 d . . . . .
O35 O 0.4698(9) 0.0880(9) 0.3378(5) 0.046(3) Uani 1 1 d . . . . .
O36 O 1.0129(8) -0.0173(7) 0.3154(4) 0.031(3) Uani 1 1 d . U . . .
O37 O 0.6465(8) 0.2408(7) 0.0867(5) 0.029(2) Uani 1 1 d . . . . .
O38 O 0.9324(9) 0.6035(8) 0.3209(6) 0.048(3) Uani 1 1 d . . . . .
O39 O 0.7205(8) 0.4148(7) 0.1236(5) 0.029(2) Uani 1 1 d . . . . .
O40 O 0.8670(7) 0.0080(7) -0.0085(4) 0.024(2) Uani 1 1 d . . . . .
O41 O 0.8447(7) -0.0542(8) -0.1068(4) 0.029(3) Uani 1 1 d . . . . .
O42 O 0.9732(7) -0.1020(7) 0.0828(5) 0.026(2) Uani 1 1 d . . . . .
O43 O 0.9624(8) -0.1799(7) -0.0131(4) 0.028(2) Uani 1 1 d . . . . .
O44 O 1.2257(15) 0.0489(15) 0.3243(11) 0.120(7) Uani 1 1 d . U . . .
O45 O 1.2853(16) 0.1674(16) 0.4117(12) 0.131(8) Uani 1 1 d . . . . .
N1 N 0.5245(10) 0.0947(9) -0.0777(7) 0.039(4) Uani 1 1 d . . . . .
H1A H 0.4652 0.1151 -0.0826 0.046 Uiso 1 1 calc R U . . .
N2 N 0.8980(11) -0.4325(10) 0.1241(7) 0.042(4) Uani 1 1 d . U . . .
H2A H 0.8923 -0.4845 0.1406 0.050 Uiso 1 1 calc R U . . .
C1 C 0.8182(10) -0.0083(10) -0.0598(7) 0.022(3) Uani 1 1 d . U . . .
C2 C 0.7116(11) 0.0286(11) -0.0651(6) 0.024(3) Uani 1 1 d . U . . .
C3 C 0.6612(11) 0.0654(11) -0.0117(7) 0.030(4) Uani 1 1 d . U . . .
H3A H 0.6919 0.0683 0.0283 0.036 Uiso 1 1 calc R U . . .
C4 C 0.5662(12) 0.0967(11) -0.0199(8) 0.033(4) Uani 1 1 d . U . . .
H4A H 0.5308 0.1193 0.0147 0.039 Uiso 1 1 calc R U . . .
C5 C 0.5731(12) 0.0618(11) -0.1272(8) 0.035(4) Uani 1 1 d . U . . .
H5A H 0.5415 0.0624 -0.1666 0.042 Uiso 1 1 calc R U . . .
C6 C 0.6619(12) 0.0288(11) -0.1245(7) 0.033(4) Uani 1 1 d . U . . .
H6A H 0.6924 0.0057 -0.1610 0.039 Uiso 1 1 calc R U . . .
C7 C 0.9596(11) -0.1729(11) 0.0453(7) 0.025(3) Uani 1 1 d . U . . .
C8 C 0.9344(12) -0.2661(11) 0.0742(8) 0.032(4) Uani 1 1 d . U . . .
C9 C 0.9347(15) -0.3503(14) 0.0365(10) 0.055(5) Uani 1 1 d . U . . .
H9A H 0.9467 -0.3519 -0.0061 0.066 Uiso 1 1 calc R U . . .
C10 C 0.9166(15) -0.4326(15) 0.0644(10) 0.060(6) Uani 1 1 d . U . . .
H10A H 0.9176 -0.4901 0.0397 0.072 Uiso 1 1 calc R U . . .
C11 C 0.8876(16) -0.3491(16) 0.1601(11) 0.065(6) Uani 1 1 d . U . . .
H11A H 0.8659 -0.3491 0.2011 0.079 Uiso 1 1 calc R U . . .
C12 C 0.9095(14) -0.2657(13) 0.1354(9) 0.049(5) Uani 1 1 d . U . . .
H12A H 0.9074 -0.2088 0.1606 0.059 Uiso 1 1 calc R U . . .
C13 C 1.253(3) 0.123(3) 0.352(2) 0.129(13) Uani 1 1 d . U . . .
C14 C 1.2819(13) 0.1891(11) 0.3031(7) 0.111(10) Uani 1 1 d G U . . .
C15 C 1.3398(12) 0.2751(12) 0.3206(5) 0.093(8) Uani 1 1 d G U . . .
H15A H 1.3620 0.2922 0.3623 0.111 Uiso 1 1 calc R U . . .
C16 C 1.3645(10) 0.3356(9) 0.2757(8) 0.070(6) Uani 1 1 d G U . . .
H16A H 1.4033 0.3932 0.2874 0.084 Uiso 1 1 calc R U . . .
N3 N 1.3314(10) 0.3100(10) 0.2134(7) 0.077(6) Uani 1 1 d G U . . .
H3B H 1.3467 0.3475 0.1856 0.093 Uiso 1 1 calc R U . . .
C17 C 1.2735(10) 0.2240(11) 0.1959(5) 0.074(7) Uani 1 1 d G U . . .
H17A H 1.2513 0.2069 0.1542 0.089 Uiso 1 1 calc R U . . .
C18 C 1.2487(10) 0.1635(8) 0.2408(8) 0.065(6) Uani 1 1 d G U . . .
H18A H 1.2100 0.1060 0.2291 0.077 Uiso 1 1 calc R U . . .
O1W O 1.318(2) -0.106(2) 0.3970(13) 0.202(12) Uani 1 1 d . U . . .
H1WA H 1.3515 -0.1530 0.4003 0.242 Uiso 1 1 d R U . . .
H1WB H 1.3362 -0.0537 0.4194 0.242 Uiso 1 1 d R U . . .
O2W O 1.3419(18) -0.0852(19) 0.2834(12) 0.173(10) Uani 1 1 d . U . . .
H2WA H 1.3752 -0.1320 0.2612 0.208 Uiso 1 1 d R U . . .
H2WB H 1.3741 -0.0241 0.2910 0.208 Uiso 1 1 d R U . . .
O3W O 0.9982(15) -0.2169(13) 0.3052(11) 0.130(7) Uani 1 1 d . U . . .
H3WA H 0.9937 -0.2697 0.2824 0.156 Uiso 1 1 d R U . . .
H3WB H 0.9447 -0.1973 0.3220 0.156 Uiso 1 1 d R U . . .
O4W O 1.0944(14) -0.0719(13) 0.4258(8) 0.109(6) Uani 1 1 d . U . . .
H4WA H 1.0515 -0.1097 0.4421 0.130 Uiso 1 1 d R U . . .
H4WB H 1.1129 -0.0175 0.4449 0.130 Uiso 1 1 d R U . . .
O5W O 1.246(3) -0.247(3) 0.2644(16) 0.142(13) Uani 0.6 1 d . U P A 1
H5WA H 1.2011 -0.2994 0.2487 0.171 Uiso 0.6 1 d R U P A 1
H5WB H 1.3165 -0.2466 0.2581 0.171 Uiso 0.6 1 d R U P A 1
O5WA O 1.117(3) -0.297(3) 0.251(2) 0.116(17) Uani 0.4 1 d . U P A 2
H5WC H 1.1144 -0.3472 0.2689 0.139 Uiso 0.4 1 d R U P A 2
H5WD H 1.1049 -0.3007 0.2115 0.139 Uiso 0.4 1 d R U P A 2
O6W O 1.162(3) -0.263(2) 0.3907(14) 0.232(15) Uani 1 1 d . U . . .
H6WA H 1.2192 -0.2862 0.3965 0.279 Uiso 1 1 d R U . . .
H6WB H 1.1249 -0.2818 0.4198 0.279 Uiso 1 1 d R U . . .
O7W O 1.1294(8) -0.1064(9) 0.2068(5) 0.046(3) Uani 1 1 d . U . . .
H7WA H 1.1406 -0.1334 0.1707 0.055 Uiso 1 1 d R U . . .
H7WB H 1.0882 -0.0662 0.1997 0.055 Uiso 1 1 d R U . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
W1 O35 1.718(12) . ?
W1 O25 1.792(12) . ?
W1 O9 1.930(11) . ?
W1 O24 1.953(12) . ?
W1 O28 1.975(11) . ?
W1 O4 2.425(12) . ?
W2 O38 1.722(11) . ?
W2 O34 1.829(11) . ?
W2 O33 1.881(10) . ?
W2 O18 1.918(11) . ?
W2 O7 1.922(11) . ?
W2 O3 2.481(10) . ?
W3 O8 1.714(11) . ?
W3 O16 1.892(12) . ?
W3 O39 1.891(10) . ?
W3 O30 1.944(11) . ?
W3 O33 1.947(11) . ?
W3 O2 2.523(10) . ?
W4 O19 1.724(10) . ?
W4 O17 1.772(9) . ?
W4 O32 1.912(10) . ?
W4 O14 1.955(9) . ?
W4 O25 2.065(11) . ?
W4 O1 2.344(10) . ?
W5 O29 1.727(12) . ?
W5 O28 1.869(10) . ?
W5 O30 1.873(11) . ?
W5 O26 1.892(11) . ?
W5 O7 1.905(11) . ?
W5 O4 2.415(10) . ?
W6 O36 1.713(9) . ?
W6 O5 1.758(10) . ?
W6 O15 1.886(10) . ?
W6 O32 1.941(10) . ?
W6 O22 2.054(10) . ?
W6 O1 2.359(9) . ?
W7 O31 1.702(11) . ?
W7 O22 1.812(11) . ?
W7 O21 1.920(11) . ?
W7 O24 1.937(12) . ?
W7 O26 1.966(12) . ?
W7 O4 2.412(10) . ?
W8 O23 1.697(11) . ?
W8 O21 1.886(10) . ?
W8 O12 1.897(11) . ?
W8 O18 1.913(11) . ?
W8 O15 1.917(10) . ?
W8 O3 2.410(9) . ?
W9 O27 1.738(10) . ?
W9 O10 1.740(9) . ?
W9 O13 1.902(10) . ?
W9 O12 1.941(10) . ?
W9 O34 2.085(11) . ?
W9 O3 2.446(10) . ?
W10 O6 1.696(10) . ?
W10 O11 1.734(9) . ?
W10 O13 1.920(10) . ?
W10 O37 1.944(10) . ?
W10 O39 2.037(10) . ?
W10 O2 2.460(10) . ?
W11 O20 1.669(10) . ?
W11 O14 1.863(9) . ?
W11 O9 1.869(11) . ?
W11 O37 1.904(9) . ?
W11 O16 1.932(12) . ?
W11 O2 2.402(11) . ?
P1 O2 1.528(11) . ?
P1 O1 1.540(11) . ?
P1 O3 1.546(11) . ?
P1 O4 1.573(10) . ?
La1 O40 2.474(9) . ?
La1 O11 2.482(9) . ?
La1 O5 2.496(10) . ?
La1 O17 2.497(10) . ?
La1 O10 2.504(9) . ?
La1 O43 2.517(10) 2_755 ?
La1 O42 2.533(10) . ?
La1 O41 2.559(9) 2_755 ?
La2 O5W 2.42(4) . ?
La2 O44 2.47(2) . ?
La2 O2W 2.48(2) . ?
La2 O3W 2.461(19) . ?
La2 O1W 2.49(2) . ?
La2 O4W 2.485(19) . ?
La2 O7W 2.539(11) . ?
La2 O36 2.604(10) . ?
La2 O6W 2.65(3) . ?
La2 O5WA 2.82(5) . ?
O40 C1 1.242(16) . ?
O41 C1 1.217(17) . ?
O41 La1 2.559(9) 2_755 ?
O42 C7 1.220(17) . ?
O43 C7 1.246(17) . ?
O43 La1 2.517(10) 2_755 ?
O44 C13 1.17(4) . ?
O45 C13 1.41(4) . ?
N1 C5 1.32(2) . ?
N1 C4 1.33(2) . ?
N1 H1A 0.8600 . ?
N2 C10 1.31(2) . ?
N2 C11 1.37(3) . ?
N2 H2A 0.8600 . ?
C1 C2 1.539(19) . ?
C2 C3 1.41(2) . ?
C2 C6 1.41(2) . ?
C3 C4 1.37(2) . ?
C3 H3A 0.9300 . ?
C4 H4A 0.9300 . ?
C5 C6 1.29(2) . ?
C5 H5A 0.9300 . ?
C6 H6A 0.9300 . ?
C7 C8 1.55(2) . ?
C8 C12 1.36(2) . ?
C8 C9 1.38(2) . ?
C9 C10 1.39(3) . ?
C9 H9A 0.9300 . ?
C10 H10A 0.9300 . ?
C11 C12 1.37(3) . ?
C11 H11A 0.9300 . ?
C12 H12A 0.9300 . ?
C13 C14 1.51(4) . ?
C14 C15 1.3900 . ?
C14 C18 1.3900 . ?
C15 C16 1.3900 . ?
C15 H15A 0.9300 . ?
C16 N3 1.3900 . ?
C16 H16A 0.9300 . ?
N3 C17 1.3900 . ?
N3 H3B 0.8600 . ?
C17 C18 1.3900 . ?
C17 H17A 0.9300 . ?
C18 H18A 0.9300 . ?
O1W H1WA 0.8499 . ?
O1W H1WB 0.8499 . ?
O2W H2WA 0.9301 . ?
O2W H2WB 0.9300 . ?
O3W H3WA 0.8500 . ?
O3W H3WB 0.8499 . ?
O4W H4WA 0.8500 . ?
O4W H4WB 0.8500 . ?
O5W H5WA 0.9300 . ?
O5W H5WB 0.9300 . ?
O5WA H5WC 0.8499 . ?
O5WA H5WD 0.8501 . ?
O6W H6WA 0.8502 . ?
O6W H6WB 0.8502 . ?
O7W H7WA 0.8496 . ?
O7W H7WB 0.8491 . ?

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
_geom_angle_publ_flag
O35 W1 O25 104.6(5) . . ?
O35 W1 O9 102.8(5) . . ?
O25 W1 O9 88.5(5) . . ?
O35 W1 O24 99.9(5) . . ?
O25 W1 O24 89.5(5) . . ?
O9 W1 O24 156.9(5) . . ?
O35 W1 O28 102.6(5) . . ?
O25 W1 O28 152.8(5) . . ?
O9 W1 O28 86.8(5) . . ?
O24 W1 O28 84.5(5) . . ?
O35 W1 O4 170.1(4) . . ?
O25 W1 O4 82.3(4) . . ?
O9 W1 O4 84.2(4) . . ?
O24 W1 O4 72.8(4) . . ?
O28 W1 O4 70.5(4) . . ?
O38 W2 O34 101.4(5) . . ?
O38 W2 O33 100.9(5) . . ?
O34 W2 O33 89.1(5) . . ?
O38 W2 O18 102.1(5) . . ?
O34 W2 O18 87.7(5) . . ?
O33 W2 O18 157.0(5) . . ?
O38 W2 O7 102.9(5) . . ?
O34 W2 O7 155.6(5) . . ?
O33 W2 O7 87.5(5) . . ?
O18 W2 O7 86.2(5) . . ?
O38 W2 O3 171.0(5) . . ?
O34 W2 O3 71.8(4) . . ?
O33 W2 O3 85.3(4) . . ?
O18 W2 O3 72.1(4) . . ?
O7 W2 O3 83.8(4) . . ?
O8 W3 O16 101.1(5) . . ?
O8 W3 O39 102.8(5) . . ?
O16 W3 O39 88.6(4) . . ?
O8 W3 O30 101.7(5) . . ?
O16 W3 O30 88.0(4) . . ?
O39 W3 O30 155.4(4) . . ?
O8 W3 O33 103.0(5) . . ?
O16 W3 O33 155.8(4) . . ?
O39 W3 O33 87.7(4) . . ?
O30 W3 O33 85.5(5) . . ?
O8 W3 O2 171.0(5) . . ?
O16 W3 O2 71.6(4) . . ?
O39 W3 O2 72.1(4) . . ?
O30 W3 O2 83.7(4) . . ?
O33 W3 O2 84.5(4) . . ?
O19 W4 O17 102.4(5) . . ?
O19 W4 O32 98.9(5) . . ?
O17 W4 O32 94.9(4) . . ?
O19 W4 O14 102.6(5) . . ?
O17 W4 O14 92.5(4) . . ?
O32 W4 O14 155.2(4) . . ?
O19 W4 O25 94.8(5) . . ?
O17 W4 O25 162.5(5) . . ?
O32 W4 O25 85.6(4) . . ?
O14 W4 O25 80.5(4) . . ?
O19 W4 O1 170.0(4) . . ?
O17 W4 O1 83.5(4) . . ?
O32 W4 O1 72.4(4) . . ?
O14 W4 O1 85.0(4) . . ?
O25 W4 O1 79.9(4) . . ?
O29 W5 O28 100.8(6) . . ?
O29 W5 O30 101.0(5) . . ?
O28 W5 O30 88.8(5) . . ?
O29 W5 O26 102.2(5) . . ?
O28 W5 O26 88.6(5) . . ?
O30 W5 O26 156.7(5) . . ?
O29 W5 O7 102.4(6) . . ?
O28 W5 O7 156.8(5) . . ?
O30 W5 O7 87.1(5) . . ?
O26 W5 O7 86.3(5) . . ?
O29 W5 O4 170.7(5) . . ?
O28 W5 O4 72.3(4) . . ?
O30 W5 O4 85.3(4) . . ?
O26 W5 O4 71.9(4) . . ?
O7 W5 O4 84.6(5) . . ?
O36 W6 O5 102.0(5) . . ?
O36 W6 O15 101.7(5) . . ?
O5 W6 O15 95.4(4) . . ?
O36 W6 O32 100.6(5) . . ?
O5 W6 O32 92.0(4) . . ?
O15 W6 O32 154.4(4) . . ?
O36 W6 O22 96.5(5) . . ?
O5 W6 O22 161.5(4) . . ?
O15 W6 O22 81.5(4) . . ?
O32 W6 O22 83.7(4) . . ?
O36 W6 O1 171.5(4) . . ?
O5 W6 O1 81.6(4) . . ?
O15 W6 O1 85.4(4) . . ?
O32 W6 O1 71.5(4) . . ?
O22 W6 O1 79.9(4) . . ?
O31 W7 O22 105.0(5) . . ?
O31 W7 O21 104.1(5) . . ?
O22 W7 O21 88.3(4) . . ?
O31 W7 O24 98.2(5) . . ?
O22 W7 O24 91.9(5) . . ?
O21 W7 O24 156.8(5) . . ?
O31 W7 O26 100.5(5) . . ?
O22 W7 O26 154.4(4) . . ?
O21 W7 O26 84.0(5) . . ?
O24 W7 O26 85.9(5) . . ?
O31 W7 O4 168.1(5) . . ?
O22 W7 O4 84.0(4) . . ?
O21 W7 O4 83.6(4) . . ?
O24 W7 O4 73.3(4) . . ?
O26 W7 O4 70.9(4) . . ?
O23 W8 O21 101.2(5) . . ?
O23 W8 O12 102.7(5) . . ?
O21 W8 O12 156.0(4) . . ?
O23 W8 O18 100.6(5) . . ?
O21 W8 O18 87.1(5) . . ?
O12 W8 O18 86.3(5) . . ?
O23 W8 O15 103.0(5) . . ?
O21 W8 O15 87.3(5) . . ?
O12 W8 O15 89.5(5) . . ?
O18 W8 O15 156.3(4) . . ?
O23 W8 O3 171.9(5) . . ?
O21 W8 O3 84.7(4) . . ?
O12 W8 O3 71.3(4) . . ?
O18 W8 O3 73.9(4) . . ?
O15 W8 O3 82.7(4) . . ?
O27 W9 O10 104.8(5) . . ?
O27 W9 O13 102.8(5) . . ?
O10 W9 O13 93.4(4) . . ?
O27 W9 O12 101.8(5) . . ?
O10 W9 O12 93.0(4) . . ?
O13 W9 O12 152.0(4) . . ?
O27 W9 O34 96.9(5) . . ?
O10 W9 O34 158.2(4) . . ?
O13 W9 O34 83.3(4) . . ?
O12 W9 O34 80.7(5) . . ?
O27 W9 O3 164.2(5) . . ?
O10 W9 O3 89.2(4) . . ?
O13 W9 O3 83.1(4) . . ?
O12 W9 O3 69.8(4) . . ?
O34 W9 O3 69.0(4) . . ?
O6 W10 O11 104.8(5) . . ?
O6 W10 O13 103.6(5) . . ?
O11 W10 O13 94.1(4) . . ?
O6 W10 O37 101.2(5) . . ?
O11 W10 O37 90.7(4) . . ?
O13 W10 O37 152.6(4) . . ?
O6 W10 O39 96.4(5) . . ?
O11 W10 O39 158.6(4) . . ?
O13 W10 O39 83.7(4) . . ?
O37 W10 O39 82.1(4) . . ?
O6 W10 O2 165.4(4) . . ?
O11 W10 O2 87.1(4) . . ?
O13 W10 O2 83.6(4) . . ?
O37 W10 O2 69.7(4) . . ?
O39 W10 O2 71.5(4) . . ?
O20 W11 O14 103.4(5) . . ?
O20 W11 O9 104.0(5) . . ?
O14 W11 O9 87.3(4) . . ?
O20 W11 O37 98.7(5) . . ?
O14 W11 O37 91.4(4) . . ?
O9 W11 O37 156.9(5) . . ?
O20 W11 O16 99.9(5) . . ?
O14 W11 O16 156.7(4) . . ?
O9 W11 O16 86.9(5) . . ?
O37 W11 O16 85.3(4) . . ?
O20 W11 O2 168.7(4) . . ?
O14 W11 O2 83.1(4) . . ?
O9 W11 O2 85.3(4) . . ?
O37 W11 O2 71.7(4) . . ?
O16 W11 O2 73.9(4) . . ?
O2 P1 O1 110.1(5) . . ?
O2 P1 O3 108.6(6) . . ?
O1 P1 O3 111.6(5) . . ?
O2 P1 O4 108.3(6) . . ?
O1 P1 O4 109.1(6) . . ?
O3 P1 O4 109.0(6) . . ?
O40 La1 O11 79.7(3) . . ?
O40 La1 O5 141.6(3) . . ?
O11 La1 O5 111.0(3) . . ?
O40 La1 O17 76.4(3) . . ?
O11 La1 O17 73.3(3) . . ?
O5 La1 O17 72.3(3) . . ?
O40 La1 O10 141.5(3) . . ?
O11 La1 O10 68.4(3) . . ?
O5 La1 O10 72.7(3) . . ?
O17 La1 O10 112.4(3) . . ?
O40 La1 O43 77.9(3) . 2_755 ?
O11 La1 O43 76.8(3) . 2_755 ?
O5 La1 O43 139.7(3) . 2_755 ?
O17 La1 O43 143.4(3) . 2_755 ?
O10 La1 O43 74.4(3) . 2_755 ?
O40 La1 O42 74.6(3) . . ?
O11 La1 O42 140.3(3) . . ?
O5 La1 O42 74.9(3) . . ?
O17 La1 O42 71.6(3) . . ?
O10 La1 O42 143.8(3) . . ?
O43 La1 O42 125.1(3) 2_755 . ?
O40 La1 O41 121.2(3) . 2_755 ?
O11 La1 O41 145.0(3) . 2_755 ?
O5 La1 O41 71.3(3) . 2_755 ?
O17 La1 O41 135.3(3) . 2_755 ?
O10 La1 O41 79.9(3) . 2_755 ?
O43 La1 O41 80.8(3) 2_755 2_755 ?
O42 La1 O41 74.7(3) . 2_755 ?
O5W La2 O44 124.5(12) . . ?
O5W La2 O2W 61.6(12) . . ?
O44 La2 O2W 64.6(8) . . ?
O5W La2 O3W 88.9(11) . . ?
O44 La2 O3W 135.5(6) . . ?
O2W La2 O3W 146.7(9) . . ?
O5W La2 O1W 86.2(10) . . ?
O44 La2 O1W 79.1(8) . . ?
O2W La2 O1W 60.6(9) . . ?
O3W La2 O1W 137.3(9) . . ?
O5W La2 O4W 142.4(10) . . ?
O44 La2 O4W 84.6(7) . . ?
O2W La2 O4W 129.9(8) . . ?
O3W La2 O4W 82.7(7) . . ?
O1W La2 O4W 76.0(8) . . ?
O5W La2 O7W 74.1(8) . . ?
O44 La2 O7W 82.4(6) . . ?
O2W La2 O7W 77.5(7) . . ?
O3W La2 O7W 79.9(6) . . ?
O1W La2 O7W 138.1(8) . . ?
O4W La2 O7W 138.9(4) . . ?
O5W La2 O36 142.2(8) . . ?
O44 La2 O36 67.7(5) . . ?
O2W La2 O36 126.1(7) . . ?
O3W La2 O36 68.1(5) . . ?
O1W La2 O36 131.2(7) . . ?
O4W La2 O36 66.4(4) . . ?
O7W La2 O36 72.6(3) . . ?
O5W La2 O6W 71.5(11) . . ?
O44 La2 O6W 142.6(8) . . ?
O2W La2 O6W 110.2(10) . . ?
O3W La2 O6W 70.3(8) . . ?
O1W La2 O6W 67.9(10) . . ?
O4W La2 O6W 71.2(8) . . ?
O7W La2 O6W 134.3(7) . . ?
O36 La2 O6W 122.9(8) . . ?
O44 La2 O5WA 148.2(12) . . ?
O2W La2 O5WA 97.6(11) . . ?
O3W La2 O5WA 50.9(11) . . ?
O1W La2 O5WA 116.4(12) . . ?
O4W La2 O5WA 125.0(11) . . ?
O7W La2 O5WA 67.6(11) . . ?
O36 La2 O5WA 110.5(10) . . ?
O6W La2 O5WA 66.8(12) . . ?
P1 O1 W4 128.4(5) . . ?
P1 O1 W6 127.4(6) . . ?
W4 O1 W6 91.8(4) . . ?
P1 O2 W11 126.6(6) . . ?
P1 O2 W10 125.0(5) . . ?
W11 O2 W10 90.6(3) . . ?
P1 O2 W3 125.6(6) . . ?
W11 O2 W3 87.8(3) . . ?
W10 O2 W3 89.6(3) . . ?
P1 O3 W8 125.0(6) . . ?
P1 O3 W9 124.7(5) . . ?
W8 O3 W9 90.7(3) . . ?
P1 O3 W2 126.0(5) . . ?
W8 O3 W2 88.3(3) . . ?
W9 O3 W2 91.2(4) . . ?
P1 O4 W7 123.4(6) . . ?
P1 O4 W5 127.1(6) . . ?
W7 O4 W5 90.9(3) . . ?
P1 O4 W1 124.1(6) . . ?
W7 O4 W1 90.2(4) . . ?
W5 O4 W1 90.4(4) . . ?
W6 O5 La1 142.5(5) . . ?
W5 O7 W2 149.5(6) . . ?
W11 O9 W1 147.6(6) . . ?
W9 O10 La1 158.2(5) . . ?
W10 O11 La1 157.7(5) . . ?
W8 O12 W9 128.2(6) . . ?
W9 O13 W10 142.9(5) . . ?
W11 O14 W4 154.0(6) . . ?
W6 O15 W8 154.4(6) . . ?
W3 O16 W11 126.5(5) . . ?
W4 O17 La1 139.6(6) . . ?
W8 O18 W2 125.6(6) . . ?
W8 O21 W7 148.0(6) . . ?
W7 O22 W6 152.6(6) . . ?
W7 O24 W1 123.6(6) . . ?
W1 O25 W4 153.4(6) . . ?
W5 O26 W7 126.1(5) . . ?
W5 O28 W1 126.7(6) . . ?
W5 O30 W3 151.0(6) . . ?
W4 O32 W6 122.5(5) . . ?
W2 O33 W3 149.9(6) . . ?
W2 O34 W9 128.0(6) . . ?
W6 O36 La2 150.2(6) . . ?
W11 O37 W10 127.9(5) . . ?
W3 O39 W10 126.7(5) . . ?
C1 O40 La1 168.5(9) . . ?
C1 O41 La1 107.3(9) . 2_755 ?
C7 O42 La1 141.2(9) . . ?
C7 O43 La1 134.2(10) . 2_755 ?
C13 O44 La2 151(3) . . ?
C5 N1 C4 120.7(14) . . ?
C5 N1 H1A 119.6 . . ?
C4 N1 H1A 119.6 . . ?
C10 N2 C11 119.7(17) . . ?
C10 N2 H2A 120.1 . . ?
C11 N2 H2A 120.1 . . ?
O41 C1 O40 126.3(13) . . ?
O41 C1 C2 115.6(13) . . ?
O40 C1 C2 118.1(12) . . ?
C3 C2 C6 117.7(13) . . ?
C3 C2 C1 121.8(12) . . ?
C6 C2 C1 120.4(13) . . ?
C4 C3 C2 118.6(14) . . ?
C4 C3 H3A 120.7 . . ?
C2 C3 H3A 120.7 . . ?
N1 C4 C3 120.0(15) . . ?
N1 C4 H4A 120.0 . . ?
C3 C4 H4A 120.0 . . ?
C6 C5 N1 124.2(16) . . ?
C6 C5 H5A 117.9 . . ?
N1 C5 H5A 117.9 . . ?
C5 C6 C2 118.7(15) . . ?
C5 C6 H6A 120.7 . . ?
C2 C6 H6A 120.7 . . ?
O42 C7 O43 128.5(15) . . ?
O42 C7 C8 115.6(13) . . ?
O43 C7 C8 115.9(14) . . ?
C12 C8 C9 120.0(17) . . ?
C12 C8 C7 120.9(15) . . ?
C9 C8 C7 119.1(15) . . ?
C8 C9 C10 117.7(19) . . ?
C8 C9 H9A 121.1 . . ?
C10 C9 H9A 121.1 . . ?
N2 C10 C9 122(2) . . ?
N2 C10 H10A 118.8 . . ?
C9 C10 H10A 118.8 . . ?
N2 C11 C12 119.6(19) . . ?
N2 C11 H11A 120.2 . . ?
C12 C11 H11A 120.2 . . ?
C8 C12 C11 120.0(19) . . ?
C8 C12 H12A 120.0 . . ?
C11 C12 H12A 120.0 . . ?
O44 C13 O45 142(4) . . ?
O44 C13 C14 107(3) . . ?
O45 C13 C14 109(3) . . ?
C15 C14 C18 120.0 . . ?
C15 C14 C13 121(2) . . ?
C18 C14 C13 119(2) . . ?
C14 C15 C16 120.0 . . ?
C14 C15 H15A 120.0 . . ?
C16 C15 H15A 120.0 . . ?
N3 C16 C15 120.0 . . ?
N3 C16 H16A 120.0 . . ?
C15 C16 H16A 120.0 . . ?
C17 N3 C16 120.0 . . ?
C17 N3 H3B 120.0 . . ?
C16 N3 H3B 120.0 . . ?
N3 C17 C18 120.0 . . ?
N3 C17 H17A 120.0 . . ?
C18 C17 H17A 120.0 . . ?
C17 C18 C14 120.0 . . ?
C17 C18 H18A 120.0 . . ?
C14 C18 H18A 120.0 . . ?
La2 O1W H1WA 119.8 . . ?
La2 O1W H1WB 120.2 . . ?
H1WA O1W H1WB 120.0 . . ?
La2 O2W H2WA 120.9 . . ?
La2 O2W H2WB 119.1 . . ?
H2WA O2W H2WB 120.0 . . ?
La2 O3W H3WA 120.1 . . ?
La2 O3W H3WB 119.9 . . ?
H3WA O3W H3WB 120.0 . . ?
La2 O4W H4WA 120.1 . . ?
La2 O4W H4WB 119.9 . . ?
H4WA O4W H4WB 120.0 . . ?
La2 O5W H5WA 115.3 . . ?
La2 O5W H5WB 124.7 . . ?
H5WA O5W H5WB 120.0 . . ?
La2 O5WA H5WC 119.9 . . ?
La2 O5WA H5WD 120.1 . . ?
H5WC O5WA H5WD 120.0 . . ?
La2 O6W H6WA 116.8 . . ?
La2 O6W H6WB 134.8 . . ?
H6WA O6W H6WB 104.2 . . ?
La2 O7W H7WA 140.3 . . ?
La2 O7W H7WB 114.9 . . ?
H7WA O7W H7WB 104.4 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O2 P1 O1 W4 -54.7(8) . . . . ?
O3 P1 O1 W4 -175.4(6) . . . . ?
O4 P1 O1 W4 64.0(8) . . . . ?
O2 P1 O1 W6 174.3(6) . . . . ?
O3 P1 O1 W6 53.6(8) . . . . ?
O4 P1 O1 W6 -67.0(8) . . . . ?
O1 P1 O2 W11 59.6(8) . . . . ?
O3 P1 O2 W11 -177.9(6) . . . . ?
O4 P1 O2 W11 -59.6(8) . . . . ?
O1 P1 O2 W10 -62.9(8) . . . . ?
O3 P1 O2 W10 59.6(8) . . . . ?
O4 P1 O2 W10 177.9(6) . . . . ?
O1 P1 O2 W3 177.7(6) . . . . ?
O3 P1 O2 W3 -59.7(7) . . . . ?
O4 P1 O2 W3 58.6(8) . . . . ?
O2 P1 O3 W8 178.2(5) . . . . ?
O1 P1 O3 W8 -60.1(8) . . . . ?
O4 P1 O3 W8 60.4(7) . . . . ?
O2 P1 O3 W9 -61.7(7) . . . . ?
O1 P1 O3 W9 60.0(8) . . . . ?
O4 P1 O3 W9 -179.5(6) . . . . ?
O2 P1 O3 W2 60.7(7) . . . . ?
O1 P1 O3 W2 -177.7(6) . . . . ?
O4 P1 O3 W2 -57.2(8) . . . . ?
O2 P1 O4 W7 178.5(6) . . . . ?
O1 P1 O4 W7 58.7(8) . . . . ?
O3 P1 O4 W7 -63.5(8) . . . . ?
O2 P1 O4 W5 -60.0(8) . . . . ?
O1 P1 O4 W5 -179.9(6) . . . . ?
O3 P1 O4 W5 58.0(8) . . . . ?
O2 P1 O4 W1 61.6(8) . . . . ?
O1 P1 O4 W1 -58.3(8) . . . . ?
O3 P1 O4 W1 179.6(6) . . . . ?
O36 W6 O5 La1 167.3(8) . . . . ?
O15 W6 O5 La1 -89.4(9) . . . . ?
O32 W6 O5 La1 66.1(9) . . . . ?
O22 W6 O5 La1 -10(2) . . . . ?
O1 W6 O5 La1 -4.9(8) . . . . ?
O20 W11 O9 W1 129.4(12) . . . . ?
O14 W11 O9 W1 26.3(13) . . . . ?
O37 W11 O9 W1 -61(2) . . . . ?
O16 W11 O9 W1 -131.2(13) . . . . ?
O2 W11 O9 W1 -57.1(13) . . . . ?
O27 W9 O10 La1 -94.0(14) . . . . ?
O13 W9 O10 La1 10.2(14) . . . . ?
O12 W9 O10 La1 163.0(14) . . . . ?
O34 W9 O10 La1 90.6(18) . . . . ?
O3 W9 O10 La1 93.3(14) . . . . ?
O6 W10 O11 La1 89.4(14) . . . . ?
O13 W10 O11 La1 -15.8(14) . . . . ?
O37 W10 O11 La1 -168.8(14) . . . . ?
O39 W10 O11 La1 -99.1(18) . . . . ?
O2 W10 O11 La1 -99.2(14) . . . . ?
O23 W8 O12 W9 -176.9(7) . . . . ?
O21 W8 O12 W9 -2.4(16) . . . . ?
O18 W8 O12 W9 -76.8(8) . . . . ?
O15 W8 O12 W9 79.9(7) . . . . ?
O3 W8 O12 W9 -2.5(6) . . . . ?
O20 W11 O14 W4 -141.5(13) . . . . ?
O9 W11 O14 W4 -37.7(13) . . . . ?
O37 W11 O14 W4 119.2(13) . . . . ?
O16 W11 O14 W4 38(2) . . . . ?
O2 W11 O14 W4 47.9(13) . . . . ?
O36 W6 O15 W8 -127.4(13) . . . . ?
O5 W6 O15 W8 129.1(13) . . . . ?
O32 W6 O15 W8 23(2) . . . . ?
O22 W6 O15 W8 -32.5(13) . . . . ?
O1 W6 O15 W8 48.0(13) . . . . ?
O8 W3 O16 W11 171.2(7) . . . . ?
O39 W3 O16 W11 68.4(7) . . . . ?
O30 W3 O16 W11 -87.3(7) . . . . ?
O33 W3 O16 W11 -12.8(15) . . . . ?
O2 W3 O16 W11 -3.2(6) . . . . ?
O19 W4 O17 La1 -163.3(8) . . . . ?
O32 W4 O17 La1 -63.0(8) . . . . ?
O14 W4 O17 La1 93.3(8) . . . . ?
O25 W4 O17 La1 28(2) . . . . ?
O1 W4 O17 La1 8.6(8) . . . . ?
O23 W8 O21 W7 -126.0(12) . . . . ?
O12 W8 O21 W7 59.4(19) . . . . ?
O18 W8 O21 W7 133.7(12) . . . . ?
O15 W8 O21 W7 -23.3(12) . . . . ?
O3 W8 O21 W7 59.6(12) . . . . ?
O31 W7 O22 W6 -129.9(13) . . . . ?
O21 W7 O22 W6 -25.7(13) . . . . ?
O24 W7 O22 W6 131.1(13) . . . . ?
O26 W7 O22 W6 47(2) . . . . ?
O4 W7 O22 W6 58.0(13) . . . . ?
O35 W1 O25 W4 125.6(14) . . . . ?
O9 W1 O25 W4 22.7(14) . . . . ?
O24 W1 O25 W4 -134.3(14) . . . . ?
O28 W1 O25 W4 -57.5(19) . . . . ?
O4 W1 O25 W4 -61.6(14) . . . . ?
O29 W5 O26 W7 168.0(8) . . . . ?
O28 W5 O26 W7 67.3(8) . . . . ?
O30 W5 O26 W7 -16.4(18) . . . . ?
O7 W5 O26 W7 -90.1(8) . . . . ?
O4 W5 O26 W7 -4.6(7) . . . . ?
O29 W5 O28 W1 -171.8(7) . . . . ?
O30 W5 O28 W1 87.3(7) . . . . ?
O26 W5 O28 W1 -69.6(7) . . . . ?
O7 W5 O28 W1 7.6(17) . . . . ?
O4 W5 O28 W1 1.8(6) . . . . ?
O29 W5 O30 W3 132.6(13) . . . . ?
O28 W5 O30 W3 -126.6(13) . . . . ?
O26 W5 O30 W3 -43(2) . . . . ?
O7 W5 O30 W3 30.5(13) . . . . ?
O4 W5 O30 W3 -54.3(12) . . . . ?
O38 W2 O33 W3 -132.9(12) . . . . ?
O34 W2 O33 W3 125.6(12) . . . . ?
O18 W2 O33 W3 44(2) . . . . ?
O7 W2 O33 W3 -30.2(12) . . . . ?
O3 W2 O33 W3 53.8(12) . . . . ?
O38 W2 O34 W9 172.4(7) . . . . ?
O33 W2 O34 W9 -86.7(7) . . . . ?
O18 W2 O34 W9 70.6(7) . . . . ?
O7 W2 O34 W9 -4.9(16) . . . . ?
O3 W2 O34 W9 -1.4(6) . . . . ?
O5 W6 O36 La2 15.0(12) . . . . ?
O15 W6 O36 La2 -83.2(11) . . . . ?
O32 W6 O36 La2 109.4(11) . . . . ?
O22 W6 O36 La2 -165.9(11) . . . . ?
O8 W3 O39 W10 -169.4(7) . . . . ?
O16 W3 O39 W10 -68.3(7) . . . . ?
O30 W3 O39 W10 14.0(15) . . . . ?
O33 W3 O39 W10 87.8(7) . . . . ?
O2 W3 O39 W10 2.8(6) . . . . ?
La1 O41 C1 O40 -14.4(18) 2_755 . . . ?
La1 O41 C1 C2 168.3(9) 2_755 . . . ?
La1 O40 C1 O41 121(4) . . . . ?
La1 O40 C1 C2 -62(5) . . . . ?
O41 C1 C2 C3 166.5(15) . . . . ?
O40 C1 C2 C3 -11(2) . . . . ?
O41 C1 C2 C6 -15(2) . . . . ?
O40 C1 C2 C6 167.4(14) . . . . ?
C6 C2 C3 C4 2(2) . . . . ?
C1 C2 C3 C4 -179.8(14) . . . . ?
C5 N1 C4 C3 1(2) . . . . ?
C2 C3 C4 N1 -2(2) . . . . ?
C4 N1 C5 C6 1(3) . . . . ?
N1 C5 C6 C2 -1(3) . . . . ?
C3 C2 C6 C5 0(2) . . . . ?
C1 C2 C6 C5 -178.9(14) . . . . ?
La1 O42 C7 O43 24(3) . . . . ?
La1 O42 C7 C8 -155.3(10) . . . . ?
La1 O43 C7 O42 18(2) 2_755 . . . ?
La1 O43 C7 C8 -162.5(9) 2_755 . . . ?
O42 C7 C8 C12 12(2) . . . . ?
O43 C7 C8 C12 -167.1(15) . . . . ?
O42 C7 C8 C9 -169.4(15) . . . . ?
O43 C7 C8 C9 11(2) . . . . ?
C12 C8 C9 C10 -5(3) . . . . ?
C7 C8 C9 C10 177.1(16) . . . . ?
C11 N2 C10 C9 5(3) . . . . ?
C8 C9 C10 N2 1(3) . . . . ?
C10 N2 C11 C12 -8(3) . . . . ?
C9 C8 C12 C11 2(3) . . . . ?
C7 C8 C12 C11 -179.9(16) . . . . ?
N2 C11 C12 C8 5(3) . . . . ?
La2 O44 C13 O45 12(10) . . . . ?
La2 O44 C13 C14 176(3) . . . . ?
O44 C13 C14 C15 -165(2) . . . . ?
O45 C13 C14 C15 5(3) . . . . ?
O44 C13 C14 C18 16(4) . . . . ?
O45 C13 C14 C18 -173.9(17) . . . . ?
C18 C14 C15 C16 0.0 . . . . ?
C13 C14 C15 C16 -179(2) . . . . ?
C14 C15 C16 N3 0.0 . . . . ?
C15 C16 N3 C17 0.0 . . . . ?
C16 N3 C17 C18 0.0 . . . . ?
N3 C17 C18 C14 0.0 . . . . ?
C15 C14 C18 C17 0.0 . . . . ?
C13 C14 C18 C17 179(2) . . . . ?

_refine_diff_density_max         3.822
_refine_diff_density_min         -3.053
_refine_diff_density_rms         0.364

_shelxl_version_number           2014-3


# SQUEEZE RESULTS (Version = 230318)
# Note: Data are Listed for all Voids in the P1 Unit Cell
# i.e. Centre of Gravity, Solvent Accessible Volume,
# Recovered number of Electrons in the Void and
# Details about the Squeezed Material
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.065 0.482 0.546 1396 629 ' '
_platon_squeeze_void_probe_radius 1.20
_platon_squeeze_details          ?

