# Electronic Supplementary Material (ESI) for RSC Advances.
# This journal is © The Royal Society of Chemistry 2020

####################################################################### 
# 
# 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_shelx
_database_code_depnum_ccdc_archive 'CCDC 1998540'
loop_
_audit_author_name
_audit_author_address
'Laura Bereczki'
;Research Centre for Natural Sciences
Hungary
;
_audit_update_record             
;
2020-12-17 deposited with the CCDC.	2020-12-28 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT214_shelx               
;
PROBLEM: Atom O5W       (Anion/Solvent) ADP max/min Ratio        6.1 prolat
RESPONSE: O5W oxygen might be split into two but this wouldn?t really improve the structure and it wouldn?t give more accurate information concerning the position of that water molecule.
;
_vrf_PLAT971_shelx               
;
PROBLEM: Check Calcd Resid. Dens.  0.81A   From W6              6.52 eA-3
RESPONSE: In the structure, relatively large residual electron density can be found mainly next to the large tungsten atoms that give level A alerts when checking the cif files. In the structures, no void volumes can be found. These residual electron densities correspond to the imperfect fitting of the structure model in some very high electron density areas. Generally, large residual electron density is characteristic of polytungstate crystal structures.
;
# Added during the CSD deposition process: Thursday 17 December 2020 12:47 PM
# end Validation Reply Form


_audit_creation_method           SHELXL-2018/3
_chemical_name_systematic        
;
decakis(dimethylammonium) dihydrododecatungstate(10-).10 hydrate
;
_chemical_name_common            
;
dimethylammonium paratungstate B.10 hydrate
;
_chemical_melting_point          ?
_chemical_formula_moiety         'O42 W12, 2(C2 N), 8(C2 H8 N), 10(O)'
_chemical_formula_sum            'C20 H64 N10 O52 W12'
_chemical_formula_weight         3483.01

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
W W -0.8490 6.8722 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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                   11.4037(5)
_cell_length_b                   13.7428(7)
_cell_length_c                   13.9665(8)
_cell_angle_alpha                63.686(4)
_cell_angle_beta                 79.005(6)
_cell_angle_gamma                69.227(5)
_cell_volume                     1832.99(18)
_cell_formula_units_Z            1
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    68858
_cell_measurement_theta_min      3.000
_cell_measurement_theta_max      30.525

_exptl_crystal_description       needle
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    3.155
_exptl_crystal_F_000             1558
_exptl_transmission_factor_min   0.01640
_exptl_transmission_factor_max   0.20650
_exptl_crystal_size_max          0.51
_exptl_crystal_size_mid          0.42
_exptl_crystal_size_min          0.21
_exptl_absorpt_coefficient_mu    18.841
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_correction_T_max  0.207
_exptl_absorpt_correction_T_min  0.015
_exptl_absorpt_process_details   
;
 T.Higashi, Numerical Absorption Correction, NUMABS, 2002
;
_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71075
_diffrn_radiation_type           MoK\a
_diffrn_source                   'Sealed Tube'
_diffrn_measurement_device_type  RAXIS-RAPID
_diffrn_measurement_method       dtprofit.ref
_diffrn_detector_area_resol_mean 10.0000
_diffrn_reflns_number            77800
_diffrn_reflns_av_unetI/netI     0.0509
_diffrn_reflns_av_R_equivalents  0.1174
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         2.999
_diffrn_reflns_theta_max         30.507
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             11156
_reflns_number_gt                10975
_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.
;

_computing_data_collection       
;
RAPID-AUTO (Rigaku Corp., Tokyo, Japan, 2015)
;
_computing_cell_refinement       
;
RAPID-AUTO (Rigaku Corp., Tokyo, Japan, 2015)
;
_computing_data_reduction        
;
RAPID-AUTO (Rigaku Corp., Tokyo, Japan, 2015)
;
_computing_structure_solution    
;
L. Palatinus, G. Chapuis 2007 J. Appl. Cryst., Vol. 40, pp. 786-790.
;
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    
;
Spek, A.L. (2003). J.Appl.Cryst. 36,7-13.
;
_computing_publication_material  
;
C. F. Macrae, J. Appl. Cryst., 41, 466-470, 2008
;
_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)+(0.0298P)²+121.0632P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     iterative
_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         11156
_refine_ls_number_parameters     441
_refine_ls_number_restraints     355
_refine_ls_R_factor_all          0.0832
_refine_ls_R_factor_gt           0.0813
_refine_ls_wR_factor_ref         0.1732
_refine_ls_wR_factor_gt          0.1724
_refine_ls_goodness_of_fit_ref   1.392
_refine_ls_restrained_S_all      1.375
_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 1.07058(5) 0.05802(5) 0.14711(5) 0.01159(11) Uani 1 1 d . U . . .
W2 W 1.17858(5) 0.19883(5) -0.09871(5) 0.01201(12) Uani 1 1 d . U . . .
W3 W 0.81962(6) -0.08048(5) 0.28963(5) 0.01476(12) Uani 1 1 d . U . . .
W4 W 0.73290(6) 0.20154(5) 0.19734(5) 0.01622(13) Uani 1 1 d . U . . .
W5 W 0.84728(5) 0.33077(5) -0.04302(5) 0.01496(12) Uani 1 1 d . U . . .
W6 W 1.26518(5) -0.08571(5) 0.00457(5) 0.01116(11) Uani 1 1 d . U . . .
O1 O 0.9932(10) -0.0504(9) 0.1948(8) 0.0129(9) Uani 1 1 d . U . . .
O2 O 1.0979(10) 0.0652(10) 0.2607(9) 0.0176(15) Uani 1 1 d . U . . .
O3 O 0.9196(10) 0.1823(9) 0.1003(9) 0.0142(9) Uani 1 1 d . U . . .
O4 O 1.1532(9) 0.1800(9) 0.0430(9) 0.0129(7) Uani 1 1 d . U . . .
O5 O 0.9992(10) 0.2895(9) -0.1180(9) 0.0148(8) Uani 1 1 d . U . . .
O6 O 1.2490(10) 0.3053(9) -0.1572(10) 0.0174(15) Uani 1 1 d . U . . .
O7 O 1.1546(10) 0.1812(9) -0.2239(9) 0.0135(9) Uani 1 1 d . U . . .
O8 O 1.3133(9) 0.0673(9) -0.0678(9) 0.0129(9) Uani 1 1 d . U . . .
O9 O 1.0895(9) 0.0558(8) -0.0197(8) 0.0105(7) Uani 1 1 d . U . . .
O10 O 1.2317(9) -0.0451(8) 0.1289(8) 0.0121(8) Uani 1 1 d . U . . .
O11 O 0.8107(10) 0.1906(9) -0.0664(9) 0.0157(15) Uani 1 1 d . U . . .
O12 O 1.4223(10) -0.1627(10) 0.0299(10) 0.021(2) Uani 1 1 d . U . . .
O13 O 0.7478(10) 0.0634(9) 0.1371(9) 0.0154(11) Uani 1 1 d . U . . .
O14 O 0.9128(11) -0.1761(10) 0.3979(10) 0.0217(19) Uani 1 1 d . U . . .
O15 O 0.6677(11) -0.0782(10) 0.3442(10) 0.0200(18) Uani 1 1 d . U . . .
O16 O 0.8170(10) 0.0582(9) 0.3000(9) 0.0154(7) Uani 1 1 d . U . . .
O17 O 0.5764(11) 0.2116(11) 0.2411(11) 0.0238(17) Uani 1 1 d . U . . .
O18 O 0.7711(11) 0.2831(10) 0.2470(10) 0.0196(16) Uani 1 1 d . U . . .
O19 O 0.7014(10) 0.3080(9) 0.0523(9) 0.0156(8) Uani 1 1 d . U . . .
O20 O 0.8812(11) 0.4154(9) 0.0031(10) 0.0184(15) Uani 1 1 d . U . . .
O21 O 0.7523(10) 0.4316(9) -0.1509(10) 0.0181(15) Uani 1 1 d . U . . .
N5 N 0.498(6) -0.042(5) 0.542(5) 0.075(8) Uani 0.5 1 d . U P . .
C9 C 0.571(4) 0.061(3) 0.504(3) 0.075(8) Uani 1 1 d . U . . .
N6 N 1.050(5) 0.011(4) 0.513(4) 0.057(6) Uani 0.5 1 d . U P . .
C10 C 0.936(3) 0.099(2) 0.484(3) 0.058(6) Uani 1 1 d . U . . .
N1 N 0.5478(15) 0.0400(13) 0.8299(13) 0.026(3) Uani 1 1 d . U . . .
H1A H 0.479699 0.043519 0.873268 0.031 Uiso 1 1 d R U . . .
H1B H 0.610968 0.032789 0.863918 0.031 Uiso 1 1 d R U . . .
C1 C 0.5783(18) -0.0643(15) 0.8078(15) 0.026(3) Uani 1 1 d . U . . .
H1C H 0.508494 -0.059647 0.775258 0.039 Uiso 1 1 calc R U . . .
H1D H 0.594863 -0.131223 0.873678 0.039 Uiso 1 1 calc R U . . .
H1E H 0.651110 -0.068349 0.760318 0.039 Uiso 1 1 calc R U . . .
C2 C 0.526(2) 0.1460(17) 0.7342(18) 0.034(4) Uani 1 1 d . U . . .
H2A H 0.594322 0.139179 0.683055 0.051 Uiso 1 1 calc R U . . .
H2B H 0.520222 0.207249 0.752403 0.051 Uiso 1 1 calc R U . . .
H2C H 0.449077 0.161488 0.704037 0.051 Uiso 1 1 calc R U . . .
N2 N 0.1041(19) 0.6848(15) 0.3114(16) 0.039(4) Uani 1 1 d . U . . .
H2D H 0.041213 0.740067 0.322598 0.046 Uiso 1 1 d R U . . .
H2E H 0.104283 0.698207 0.242888 0.046 Uiso 1 1 d R U . . .
C3 C 0.078(2) 0.578(2) 0.3757(19) 0.044(5) Uani 1 1 d . U . . .
H3C H 0.123706 0.523511 0.345502 0.066 Uiso 1 1 calc R U . . .
H3D H -0.010011 0.589370 0.377099 0.066 Uiso 1 1 calc R U . . .
H3E H 0.104243 0.549032 0.447239 0.066 Uiso 1 1 calc R U . . .
C4 C 0.222(2) 0.6924(19) 0.330(2) 0.045(6) Uani 1 1 d . U . . .
H4C H 0.223687 0.679169 0.403350 0.067 Uiso 1 1 calc R U . . .
H4D H 0.229356 0.766991 0.284398 0.067 Uiso 1 1 calc R U . . .
H4E H 0.291734 0.636043 0.314348 0.067 Uiso 1 1 calc R U . . .
N3 N 0.4995(17) 0.6110(15) 0.0923(14) 0.032(3) Uani 1 1 d . U . . .
H3A H 0.469947 0.684154 0.081563 0.038 Uiso 1 1 d R U . . .
H3B H 0.435546 0.589724 0.089463 0.038 Uiso 1 1 d R U . . .
C5 C 0.550(2) 0.5445(18) 0.1967(17) 0.033(3) Uani 1 1 d . U . . .
H5A H 0.584081 0.465643 0.208146 0.050 Uiso 1 1 calc R U . . .
H5B H 0.484803 0.552737 0.249797 0.050 Uiso 1 1 calc R U . . .
H5C H 0.615412 0.570525 0.202066 0.050 Uiso 1 1 calc R U . . .
C6 C 0.596(2) 0.598(2) 0.0030(18) 0.038(4) Uani 1 1 d . U . . .
H6A H 0.664749 0.622054 0.004976 0.058 Uiso 1 1 calc R U . . .
H6B H 0.557303 0.645074 -0.064777 0.058 Uiso 1 1 calc R U . . .
H6C H 0.626097 0.520047 0.012677 0.058 Uiso 1 1 calc R U . . .
N4 N 0.0084(17) 0.3399(15) 0.196(2) 0.045(5) Uani 1 1 d . U . . .
H4A H 0.009359 0.279986 0.257888 0.054 Uiso 1 1 d R U . . .
H4B H -0.032591 0.335076 0.150818 0.054 Uiso 1 1 d R U . . .
C7 C -0.063(3) 0.441(2) 0.213(2) 0.056(8) Uani 1 1 d . U . . .
H7A H -0.103348 0.419352 0.283288 0.083 Uiso 1 1 calc R U . . .
H7B H -0.125962 0.487568 0.160515 0.083 Uiso 1 1 calc R U . . .
H7C H -0.008527 0.482509 0.207500 0.083 Uiso 1 1 calc R U . . .
C8 C 0.135(2) 0.329(2) 0.156(3) 0.047(6) Uani 1 1 d . U . . .
H8A H 0.136484 0.391894 0.087617 0.071 Uiso 1 1 calc R U . . .
H8B H 0.171389 0.258814 0.147615 0.071 Uiso 1 1 calc R U . . .
H8C H 0.182450 0.330672 0.204873 0.071 Uiso 1 1 calc R U . . .
O1W O 0.3580(15) 0.3518(13) 0.3001(11) 0.040(4) Uani 1 1 d . . . . .
O2W O 0.442(2) 0.372(2) 0.4690(18) 0.072(7) Uani 1 1 d . . . . .
O3W O 0.2676(18) 0.4459(15) 0.6114(13) 0.048(4) Uani 1 1 d . . . . .
O4W O 0.6935(16) 0.3508(15) 0.4204(13) 0.044(4) Uani 1 1 d . . . . .
O5W O 0.204(7) 0.211(4) 0.400(2) 0.24(4) Uani 1 1 d . . . . .


_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 O2 1.724(11) . ?
W1 O1 1.808(11) . ?
W1 O3 1.914(10) . ?
W1 O10 1.935(10) . ?
W1 O4 2.062(11) . ?
W1 O9 2.312(10) . ?
W2 O6 1.725(11) . ?
W2 O8 1.845(10) . ?
W2 O4 1.857(11) . ?
W2 O7 1.948(11) . ?
W2 O5 1.979(10) . ?
W2 O9 2.276(10) . ?
W3 O14 1.733(12) . ?
W3 O15 1.750(11) . ?
W3 O7 1.892(10) 2_755 ?
W3 O16 1.963(10) . ?
W3 O13 2.214(11) . ?
W3 O1 2.222(10) . ?
W4 O17 1.750(12) . ?
W4 O18 1.755(11) . ?
W4 O16 1.880(11) . ?
W4 O19 1.910(12) . ?
W4 O3 2.293(10) . ?
W4 O13 2.339(10) . ?
W5 O20 1.731(11) . ?
W5 O21 1.752(11) . ?
W5 O5 1.886(10) . ?
W5 O19 1.948(11) . ?
W5 O3 2.160(11) . ?
W5 O11 2.274(11) . ?
W6 O12 1.738(11) . ?
W6 O11 1.752(11) 2_755 ?
W6 O13 1.890(11) 2_755 ?
W6 O10 1.981(10) . ?
W6 O8 2.114(10) . ?
W6 O9 2.195(9) . ?
N5 N5 1.24(12) 2_656 ?
N5 C9 1.26(7) 2_656 ?
N5 C9 1.73(8) . ?
N6 C10 1.41(6) . ?
N6 N6 1.44(9) 2_756 ?
N6 C10 1.45(5) 2_756 ?
N1 C2 1.45(2) . ?
N1 C1 1.51(2) . ?
N1 H1A 0.8900 . ?
N1 H1B 0.8900 . ?
C1 H1C 0.9600 . ?
C1 H1D 0.9600 . ?
C1 H1E 0.9600 . ?
C2 H2A 0.9600 . ?
C2 H2B 0.9600 . ?
C2 H2C 0.9600 . ?
N2 C3 1.45(3) . ?
N2 C4 1.47(3) . ?
N2 H2D 0.8900 . ?
N2 H2E 0.8900 . ?
C3 H3C 0.9600 . ?
C3 H3D 0.9600 . ?
C3 H3E 0.9600 . ?
C4 H4C 0.9600 . ?
C4 H4D 0.9600 . ?
C4 H4E 0.9600 . ?
N3 C5 1.44(3) . ?
N3 C6 1.52(3) . ?
N3 H3A 0.8900 . ?
N3 H3B 0.8900 . ?
C5 H5A 0.9600 . ?
C5 H5B 0.9600 . ?
C5 H5C 0.9600 . ?
C6 H6A 0.9600 . ?
C6 H6B 0.9600 . ?
C6 H6C 0.9600 . ?
N4 C8 1.43(3) . ?
N4 C7 1.44(3) . ?
N4 H4A 0.8899 . ?
N4 H4B 0.8900 . ?
C7 H7A 0.9600 . ?
C7 H7B 0.9600 . ?
C7 H7C 0.9600 . ?
C8 H8A 0.9600 . ?
C8 H8B 0.9600 . ?
C8 H8C 0.9600 . ?

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
O2 W1 O1 105.0(5) . . ?
O2 W1 O3 101.6(5) . . ?
O1 W1 O3 94.3(5) . . ?
O2 W1 O10 99.2(5) . . ?
O1 W1 O10 93.0(4) . . ?
O3 W1 O10 155.4(4) . . ?
O2 W1 O4 95.1(5) . . ?
O1 W1 O4 159.9(4) . . ?
O3 W1 O4 82.6(4) . . ?
O10 W1 O4 82.6(4) . . ?
O2 W1 O9 163.6(4) . . ?
O1 W1 O9 88.0(4) . . ?
O3 W1 O9 87.0(4) . . ?
O10 W1 O9 69.8(4) . . ?
O4 W1 O9 72.1(4) . . ?
O6 W2 O8 103.1(5) . . ?
O6 W2 O4 103.1(5) . . ?
O8 W2 O4 92.6(5) . . ?
O6 W2 O7 100.8(5) . . ?
O8 W2 O7 88.0(4) . . ?
O4 W2 O7 155.3(4) . . ?
O6 W2 O5 101.1(5) . . ?
O8 W2 O5 155.2(4) . . ?
O4 W2 O5 87.4(4) . . ?
O7 W2 O5 81.9(4) . . ?
O6 W2 O9 178.8(5) . . ?
O8 W2 O9 75.8(4) . . ?
O4 W2 O9 76.5(4) . . ?
O7 W2 O9 79.7(4) . . ?
O5 W2 O9 80.1(4) . . ?
O14 W3 O15 102.9(6) . . ?
O14 W3 O7 97.2(5) . 2_755 ?
O15 W3 O7 99.3(5) . 2_755 ?
O14 W3 O16 96.3(5) . . ?
O15 W3 O16 95.9(5) . . ?
O7 W3 O16 156.9(5) 2_755 . ?
O14 W3 O13 162.8(5) . . ?
O15 W3 O13 92.1(5) . . ?
O7 W3 O13 88.5(4) 2_755 . ?
O16 W3 O13 73.6(4) . . ?
O14 W3 O1 87.9(5) . . ?
O15 W3 O1 168.5(5) . . ?
O7 W3 O1 82.9(4) 2_755 . ?
O16 W3 O1 78.9(4) . . ?
O13 W3 O1 76.7(4) . . ?
O17 W4 O18 103.7(6) . . ?
O17 W4 O16 101.1(6) . . ?
O18 W4 O16 96.4(5) . . ?
O17 W4 O19 97.2(5) . . ?
O18 W4 O19 100.5(5) . . ?
O16 W4 O19 151.3(4) . . ?
O17 W4 O3 163.1(5) . . ?
O18 W4 O3 91.3(5) . . ?
O16 W4 O3 84.8(4) . . ?
O19 W4 O3 71.9(4) . . ?
O17 W4 O13 91.8(5) . . ?
O18 W4 O13 162.4(5) . . ?
O16 W4 O13 72.1(4) . . ?
O19 W4 O13 85.5(4) . . ?
O3 W4 O13 74.8(4) . . ?
O20 W5 O21 102.5(5) . . ?
O20 W5 O5 100.4(5) . . ?
O21 W5 O5 99.8(5) . . ?
O20 W5 O19 96.6(5) . . ?
O21 W5 O19 91.8(5) . . ?
O5 W5 O19 156.7(4) . . ?
O20 W5 O3 90.1(5) . . ?
O21 W5 O3 162.3(5) . . ?
O5 W5 O3 89.9(4) . . ?
O19 W5 O3 74.3(4) . . ?
O20 W5 O11 167.5(5) . . ?
O21 W5 O11 88.8(5) . . ?
O5 W5 O11 82.5(4) . . ?
O19 W5 O11 77.6(4) . . ?
O3 W5 O11 77.7(4) . . ?
O12 W6 O11 103.4(5) . 2_755 ?
O12 W6 O13 103.2(5) . 2_755 ?
O11 W6 O13 96.2(5) 2_755 2_755 ?
O12 W6 O10 95.4(5) . . ?
O11 W6 O10 93.2(5) 2_755 . ?
O13 W6 O10 156.6(4) 2_755 . ?
O12 W6 O8 89.6(5) . . ?
O11 W6 O8 166.3(4) 2_755 . ?
O13 W6 O8 84.9(4) 2_755 . ?
O10 W6 O8 81.0(4) . . ?
O12 W6 O9 159.2(5) . . ?
O11 W6 O9 93.7(4) 2_755 . ?
O13 W6 O9 86.4(4) 2_755 . ?
O10 W6 O9 71.6(4) . . ?
O8 W6 O9 72.7(4) . . ?
W1 O1 W3 137.2(5) . . ?
W1 O3 W5 139.0(6) . . ?
W1 O3 W4 125.5(5) . . ?
W5 O3 W4 95.2(4) . . ?
W2 O4 W1 117.5(5) . . ?
W5 O5 W2 143.1(6) . . ?
W3 O7 W2 147.0(6) 2_755 . ?
W2 O8 W6 114.9(5) . . ?
W6 O9 W2 96.6(4) . . ?
W6 O9 W1 97.5(4) . . ?
W2 O9 W1 93.9(4) . . ?
W1 O10 W6 119.8(5) . . ?
W6 O11 W5 141.5(6) 2_755 . ?
W6 O13 W3 137.7(5) 2_755 . ?
W6 O13 W4 127.4(5) 2_755 . ?
W3 O13 W4 93.5(4) . . ?
W4 O16 W3 119.3(6) . . ?
W4 O19 W5 116.9(5) . . ?
N5 N5 C9 88(7) 2_656 2_656 ?
N5 N5 C9 47(5) 2_656 . ?
C9 N5 C9 134(5) 2_656 . ?
N5 C9 N5 46(5) 2_656 . ?
C10 N6 N6 61(4) . 2_756 ?
C10 N6 C10 120(3) . 2_756 ?
N6 N6 C10 58(3) 2_756 2_756 ?
N6 C10 N6 60(3) . 2_756 ?
C2 N1 C1 113.7(15) . . ?
C2 N1 H1A 108.9 . . ?
C1 N1 H1A 108.8 . . ?
C2 N1 H1B 108.8 . . ?
C1 N1 H1B 108.8 . . ?
H1A N1 H1B 107.7 . . ?
N1 C1 H1C 109.5 . . ?
N1 C1 H1D 109.5 . . ?
H1C C1 H1D 109.5 . . ?
N1 C1 H1E 109.5 . . ?
H1C C1 H1E 109.5 . . ?
H1D C1 H1E 109.5 . . ?
N1 C2 H2A 109.5 . . ?
N1 C2 H2B 109.5 . . ?
H2A C2 H2B 109.5 . . ?
N1 C2 H2C 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
C3 N2 C4 116.4(18) . . ?
C3 N2 H2D 108.3 . . ?
C4 N2 H2D 108.3 . . ?
C3 N2 H2E 108.2 . . ?
C4 N2 H2E 108.1 . . ?
H2D N2 H2E 107.3 . . ?
N2 C3 H3C 109.5 . . ?
N2 C3 H3D 109.5 . . ?
H3C C3 H3D 109.5 . . ?
N2 C3 H3E 109.5 . . ?
H3C C3 H3E 109.5 . . ?
H3D C3 H3E 109.5 . . ?
N2 C4 H4C 109.5 . . ?
N2 C4 H4D 109.5 . . ?
H4C C4 H4D 109.5 . . ?
N2 C4 H4E 109.5 . . ?
H4C C4 H4E 109.5 . . ?
H4D C4 H4E 109.5 . . ?
C5 N3 C6 113.0(17) . . ?
C5 N3 H3A 109.0 . . ?
C6 N3 H3A 109.0 . . ?
C5 N3 H3B 108.9 . . ?
C6 N3 H3B 108.9 . . ?
H3A N3 H3B 107.8 . . ?
N3 C5 H5A 109.5 . . ?
N3 C5 H5B 109.5 . . ?
H5A C5 H5B 109.5 . . ?
N3 C5 H5C 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
N3 C6 H6A 109.5 . . ?
N3 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
N3 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
C8 N4 C7 118.3(18) . . ?
C8 N4 H4A 107.7 . . ?
C7 N4 H4A 107.7 . . ?
C8 N4 H4B 107.8 . . ?
C7 N4 H4B 107.8 . . ?
H4A N4 H4B 107.1 . . ?
N4 C7 H7A 109.5 . . ?
N4 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
N4 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
N4 C8 H8A 109.5 . . ?
N4 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
N4 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?

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 W1 O1 W3 58.8(9) . . . . ?
O3 W1 O1 W3 -44.4(8) . . . . ?
O10 W1 O1 W3 159.1(8) . . . . ?
O4 W1 O1 W3 -124.4(11) . . . . ?
O9 W1 O1 W3 -131.3(8) . . . . ?
O6 W2 O4 W1 -179.6(5) . . . . ?
O8 W2 O4 W1 -75.5(6) . . . . ?
O7 W2 O4 W1 15.4(13) . . . . ?
O5 W2 O4 W1 79.7(6) . . . . ?
O9 W2 O4 W1 -0.8(5) . . . . ?
O20 W5 O5 W2 68.6(11) . . . . ?
O21 W5 O5 W2 173.4(10) . . . . ?
O19 W5 O5 W2 -67.9(17) . . . . ?
O3 W5 O5 W2 -21.5(10) . . . . ?
O11 W5 O5 W2 -99.1(10) . . . . ?
O6 W2 O8 W6 -179.3(6) . . . . ?
O4 W2 O8 W6 76.7(6) . . . . ?
O7 W2 O8 W6 -78.7(6) . . . . ?
O5 W2 O8 W6 -12.9(14) . . . . ?
O9 W2 O8 W6 1.3(5) . . . . ?
O17 W4 O16 W3 77.1(7) . . . . ?
O18 W4 O16 W3 -177.5(6) . . . . ?
O19 W4 O16 W3 -51.6(12) . . . . ?
O3 W4 O16 W3 -86.8(6) . . . . ?
O13 W4 O16 W3 -11.1(5) . . . . ?
C9 N5 C9 N5 -0.001(16) 2_656 . . 2_656 ?
C10 N6 C10 N6 -0.002(9) 2_756 . . 2_756 ?

_refine_diff_density_max         6.140
_refine_diff_density_min         -5.441
_refine_diff_density_rms         0.571

####################################################################### 
# 
# 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_shelx_CCDC1
_database_code_depnum_ccdc_archive 'CCDC 1998541'
loop_
_audit_author_name
_audit_author_address
'Laura Bereczki'
;Research Centre for Natural Sciences
Hungary
;
_audit_update_record             
;
2020-12-17 deposited with the CCDC.	2020-12-28 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT971_shelx               
;
PROBLEM: Check Calcd Resid. Dens.  0.95A   From W11             4.61 eA-3
RESPONSE: Relatively large residual electron density can be found mainly next to the large tungsten atoms that give level A alerts when checking the cif files. In the structures, no void volumes can be found. These residual electron densities correspond to the imperfect fitting of the structure model in some very high electron density areas. Generally large residual electron density is characteristic of polytungstate crystal structures.
;
# Added during the CSD deposition process: Thursday 17 December 2020 12:58 PM
# end Validation Reply Form


_audit_creation_method           SHELXL-2018/3
_chemical_name_systematic        
;
decakis(dimethylammonium) dihydrododecatungstate(10-).11 hydrate
;
_chemical_name_common            
;
dimethylammonium paratungstate B.11 hydrate
;
_chemical_melting_point          ?
_chemical_formula_moiety         'O42 W12, 10(C2 H8 N), 11(O)'
_chemical_formula_sum            'C20 H80 N10 O53 W12'
_chemical_formula_weight         3515.14

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
W W -0.8490 6.8722 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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                   13.5917(3)
_cell_length_b                   16.6057(4)
_cell_length_c                   18.6449(4)
_cell_angle_alpha                90.344(6)
_cell_angle_beta                 105.743(7)
_cell_angle_gamma                112.051(8)
_cell_volume                     3726.5(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    153(2)
_cell_measurement_reflns_used    149683
_cell_measurement_theta_min      3.015
_cell_measurement_theta_max      30.490

_exptl_crystal_description       platelet
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    3.133
_exptl_crystal_F_000             3164
_exptl_transmission_factor_min   0.998108
_exptl_transmission_factor_max   0.999224
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.15
_exptl_absorpt_coefficient_mu    18.538
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_correction_T_max  0.999
_exptl_absorpt_correction_T_min  0.998
_exptl_absorpt_process_details   
;
  NUMABS, Numerical Absorption correction Program (T.Higashi, 2011)
;
_diffrn_ambient_temperature      153(2)
_diffrn_radiation_wavelength     0.71075
_diffrn_radiation_type           MoK\a
_diffrn_source                   'Sealed Tube'
_diffrn_measurement_device_type  RAXIS-RAPID
_diffrn_measurement_method       dtprofit.ref
_diffrn_detector_area_resol_mean 10.0000
_diffrn_reflns_number            199047
_diffrn_reflns_av_unetI/netI     0.1079
_diffrn_reflns_av_R_equivalents  0.1837
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_theta_min         3.015
_diffrn_reflns_theta_max         30.491
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             22666
_reflns_number_gt                17352
_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.
;

_computing_data_collection       
;
RAPID-AUTO (Rigaku Corp., Tokyo, Japan, 2015)
;
_computing_cell_refinement       
;
RAPID-AUTO (Rigaku Corp., Tokyo, Japan, 2015)
;
_computing_data_reduction        
;
RAPID-AUTO (Rigaku Corp., Tokyo, Japan, 2015)
;
_computing_structure_solution    
;
L. Palatinus, G. Chapuis 2007 J. Appl. Cryst., Vol. 40, pp. 786-790.
;
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    
;
Spek, A.L. (2003). J.Appl.Cryst. 36,7-13.
;
_computing_publication_material  
;
C. F. Macrae, J. Appl. Cryst., 41, 466-470, 2008
;
_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)+(0.0571P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     iterative
_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         22666
_refine_ls_number_parameters     876
_refine_ls_number_restraints     663
_refine_ls_R_factor_all          0.1038
_refine_ls_R_factor_gt           0.0687
_refine_ls_wR_factor_ref         0.1505
_refine_ls_wR_factor_gt          0.1387
_refine_ls_goodness_of_fit_ref   1.142
_refine_ls_restrained_S_all      1.129
_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 -0.10875(5) 0.05925(3) 0.16737(3) 0.01551(11) Uani 1 1 d . U . . .
W2 W 0.15794(5) 0.11621(3) 0.25254(3) 0.01707(12) Uani 1 1 d . U . . .
W3 W 0.30513(5) 0.07999(3) 0.15006(3) 0.01616(11) Uani 1 1 d . U . . .
W4 W -0.17021(5) 0.12645(3) -0.02215(3) 0.01477(11) Uani 1 1 d . U . . .
W5 W 0.10183(5) 0.17863(3) 0.05904(3) 0.01339(11) Uani 1 1 d . U . . .
W6 W 0.01478(5) -0.09630(3) 0.12359(3) 0.01303(11) Uani 1 1 d . U . . .
O1 O -0.2202(8) -0.0219(6) 0.1874(5) 0.0205(13) Uani 1 1 d . U . . .
O2 O -0.1035(9) 0.1552(6) 0.2120(5) 0.0214(15) Uani 1 1 d . U . . .
O3 O 0.0129(8) 0.0474(5) 0.2477(4) 0.0168(7) Uani 1 1 d . U . . .
O4 O 0.1696(9) 0.2149(6) 0.2954(5) 0.0245(16) Uani 1 1 d . U . . .
O5 O 0.2191(9) 0.0709(6) 0.3267(5) 0.0228(15) Uani 1 1 d . U . . .
O6 O 0.2776(8) 0.1636(6) 0.2095(5) 0.0179(6) Uani 1 1 d . U . . .
O7 O 0.4124(8) 0.1617(6) 0.1262(5) 0.0214(14) Uani 1 1 d . U . . .
O8 O 0.3757(8) 0.0407(6) 0.2261(5) 0.0231(15) Uani 1 1 d . U . . .
O9 O 0.2714(8) -0.0089(5) 0.0747(5) 0.0168(9) Uani 1 1 d . U . . .
O10 O -0.1829(8) 0.0693(5) 0.0673(4) 0.0157(7) Uani 1 1 d . U . . .
O11 O -0.2637(9) 0.1765(6) -0.0317(5) 0.0224(17) Uani 1 1 d . U . . .
O12 O -0.0402(8) 0.2105(5) 0.0360(4) 0.0157(7) Uani 1 1 d . U . . .
O13 O 0.0501(8) 0.1326(5) 0.1419(4) 0.0150(7) Uani 1 1 d . U . . .
O14 O 0.1927(8) 0.2830(6) 0.0987(5) 0.0180(13) Uani 1 1 d . U . . .
O15 O 0.1870(8) 0.1183(5) 0.0620(4) 0.0154(7) Uani 1 1 d . U . . .
O16 O 0.0881(8) 0.1954(5) -0.0466(4) 0.0142(9) Uani 1 1 d . U . . .
O17 O -0.0450(7) 0.0637(5) -0.0139(4) 0.0127(8) Uani 1 1 d . U . . .
O18 O -0.1291(8) 0.1481(5) -0.1089(4) 0.0152(9) Uani 1 1 d . U . . .
O19 O 0.1452(8) 0.0052(5) 0.1671(4) 0.0153(7) Uani 1 1 d . U . . .
O20 O -0.0810(8) -0.0434(5) 0.1094(4) 0.0145(8) Uani 1 1 d . U . . .
O21 O -0.0021(9) -0.1517(6) 0.2002(5) 0.0199(19) Uani 1 1 d . U . . .
W7 W 0.88124(5) 0.60609(3) 0.44583(3) 0.01381(11) Uani 1 1 d . U . . .
W8 W 1.15308(5) 0.72975(3) 0.49593(3) 0.01626(11) Uani 1 1 d . U . . .
W9 W 0.67762(5) 0.37716(3) 0.38656(3) 0.01770(12) Uani 1 1 d . U . . .
W10 W 0.78020(5) 0.47847(4) 0.25583(3) 0.01958(12) Uani 1 1 d . U . . .
W11 W 1.04854(5) 0.60022(3) 0.30989(3) 0.01708(12) Uani 1 1 d . U . . .
W12 W 1.04093(5) 0.62086(3) 0.62288(3) 0.01408(11) Uani 1 1 d . U . . .
O22 O 0.8079(8) 0.4917(5) 0.4582(4) 0.0163(9) Uani 1 1 d . U . . .
O23 O 0.7751(8) 0.6416(6) 0.4153(5) 0.0214(14) Uani 1 1 d . U . . .
O24 O 0.9058(8) 0.5786(5) 0.3546(4) 0.0142(7) Uani 1 1 d . U . . .
O25 O 1.0076(8) 0.7244(5) 0.4510(5) 0.0170(7) Uani 1 1 d . U . . .
O26 O 1.1403(8) 0.6708(5) 0.4028(5) 0.0176(7) Uani 1 1 d . U . . .
O27 O 1.2320(9) 0.8385(6) 0.4876(5) 0.0240(15) Uani 1 1 d . U . . .
O28 O 1.2646(8) 0.6855(5) 0.5388(5) 0.0171(9) Uani 1 1 d . U . . .
O29 O 0.5854(9) 0.3973(6) 0.4266(5) 0.0258(17) Uani 1 1 d . U . . .
O30 O 0.5880(9) 0.2864(6) 0.3192(5) 0.0282(19) Uani 1 1 d . U . . .
O31 O 0.6832(8) 0.4620(6) 0.3153(5) 0.0194(7) Uani 1 1 d . U . . .
O32 O 0.7087(9) 0.3820(7) 0.1940(5) 0.0270(16) Uani 1 1 d . U . . .
O33 O 0.7465(9) 0.5583(7) 0.2044(5) 0.0268(17) Uani 1 1 d . U . . .
O34 O 0.9222(8) 0.5024(6) 0.2451(5) 0.0186(7) Uani 1 1 d . U . . .
O35 O 1.0184(9) 0.6812(6) 0.2593(5) 0.0249(16) Uani 1 1 d . U . . .
O36 O 1.1502(9) 0.5881(6) 0.2765(5) 0.0258(15) Uani 1 1 d . U . . .
O37 O 1.0490(8) 0.4907(5) 0.3766(5) 0.0178(15) Uani 1 1 d . U . . .
O38 O 1.0467(8) 0.6754(6) 0.7038(5) 0.0188(17) Uani 1 1 d . U . . .
O39 O 1.1335(8) 0.7380(5) 0.5892(5) 0.0170(8) Uani 1 1 d . U . . .
O40 O 0.9196(8) 0.6429(5) 0.5528(4) 0.0147(7) Uani 1 1 d . U . . .
O41 O 1.0422(7) 0.5927(5) 0.5062(4) 0.0126(7) Uani 1 1 d . U . . .
O42 O 0.8221(8) 0.3922(5) 0.3476(4) 0.0158(10) Uani 1 1 d . U . . .
N1 N 0.2880(19) 0.5119(17) 0.4228(10) 0.106(6) Uani 1 1 d . U . . .
H1A H 0.218411 0.497576 0.394238 0.127 Uiso 1 1 d R U . . .
H1B H 0.289341 0.521206 0.470209 0.127 Uiso 1 1 d R U . . .
C1 C 0.361(2) 0.597(2) 0.4016(13) 0.106(6) Uani 1 1 d . U . . .
H1C H 0.354444 0.589863 0.349194 0.160 Uiso 1 1 calc R U . . .
H1D H 0.436800 0.612248 0.430686 0.160 Uiso 1 1 calc R U . . .
H1E H 0.337396 0.642571 0.411548 0.160 Uiso 1 1 calc R U . . .
C2 C 0.318(2) 0.438(2) 0.4158(13) 0.106(6) Uani 1 1 d . U . . .
H2C H 0.390972 0.450113 0.448937 0.159 Uiso 1 1 calc R U . . .
H2D H 0.317011 0.426514 0.364976 0.159 Uiso 1 1 calc R U . . .
H2E H 0.265443 0.386838 0.428817 0.159 Uiso 1 1 calc R U . . .
N2 N 0.0146(12) 0.3239(8) 0.1668(7) 0.031(3) Uani 1 1 d . U . . .
H2A H 0.019166 0.286665 0.134622 0.037 Uiso 1 1 d R U . . .
H2B H -0.019204 0.292825 0.198292 0.037 Uiso 1 1 d R U . . .
C3 C -0.054(2) 0.3690(14) 0.1248(10) 0.069(6) Uani 1 1 d . U . . .
H3A H -0.020545 0.399912 0.088603 0.104 Uiso 1 1 calc R U . . .
H3B H -0.058967 0.409748 0.159036 0.104 Uiso 1 1 calc R U . . .
H3C H -0.127156 0.326715 0.099454 0.104 Uiso 1 1 calc R U . . .
C4 C 0.1265(17) 0.3832(12) 0.2095(12) 0.055(5) Uani 1 1 d . U . . .
H4A H 0.122525 0.428081 0.239842 0.083 Uiso 1 1 calc R U . . .
H4B H 0.167962 0.409398 0.175512 0.083 Uiso 1 1 calc R U . . .
H4C H 0.162788 0.350990 0.241247 0.083 Uiso 1 1 calc R U . . .
N3 N 0.8986(14) 0.6462(9) 0.0989(7) 0.040(3) Uani 1 1 d . U . . .
H3D H 0.909444 0.701257 0.091120 0.048 Uiso 1 1 d R U . . .
H3E H 0.899184 0.641647 0.146570 0.048 Uiso 1 1 d R U . . .
C5 C 0.993(2) 0.6293(13) 0.0889(11) 0.060(5) Uani 1 1 d . U . . .
H5C H 0.981122 0.569262 0.094812 0.090 Uiso 1 1 calc R U . . .
H5D H 1.059989 0.666843 0.125854 0.090 Uiso 1 1 calc R U . . .
H5E H 0.999231 0.640645 0.039621 0.090 Uiso 1 1 calc R U . . .
C6 C 0.7852(19) 0.5879(11) 0.0498(9) 0.054(4) Uani 1 1 d . U . . .
H6A H 0.780006 0.597045 -0.001694 0.081 Uiso 1 1 calc R U . . .
H6B H 0.729961 0.601606 0.063986 0.081 Uiso 1 1 calc R U . . .
H6C H 0.773194 0.527857 0.055585 0.081 Uiso 1 1 calc R U . . .
N4 N 0.4379(12) 0.3320(8) 0.1983(6) 0.030(3) Uani 1 1 d . U . . .
H4D H 0.380416 0.280531 0.186532 0.036 Uiso 1 1 d R U . . .
H4E H 0.497806 0.323391 0.224382 0.036 Uiso 1 1 d R U . . .
C7 C 0.4154(15) 0.3944(12) 0.2455(9) 0.040(4) Uani 1 1 d . U . . .
H7A H 0.337365 0.382171 0.230318 0.060 Uiso 1 1 calc R U . . .
H7B H 0.455893 0.453639 0.238343 0.060 Uiso 1 1 calc R U . . .
H7C H 0.438866 0.386939 0.297500 0.060 Uiso 1 1 calc R U . . .
C8 C 0.4556(16) 0.3692(11) 0.1303(9) 0.038(4) Uani 1 1 d . U . . .
H8A H 0.529799 0.413004 0.141486 0.057 Uiso 1 1 calc R U . . .
H8B H 0.403247 0.395409 0.110879 0.057 Uiso 1 1 calc R U . . .
H8C H 0.445596 0.323868 0.093502 0.057 Uiso 1 1 calc R U . . .
N5 N 0.6525(14) 0.8702(10) 0.0325(8) 0.047(3) Uani 1 1 d . U . . .
H5A H 0.717781 0.915235 0.048773 0.056 Uiso 1 1 d R U . . .
H5B H 0.639851 0.856285 -0.016297 0.056 Uiso 1 1 d R U . . .
C9 C 0.6600(17) 0.7953(12) 0.0719(9) 0.047(3) Uani 1 1 d . U . . .
H9C H 0.670488 0.808466 0.124333 0.071 Uiso 1 1 calc R U . . .
H9D H 0.721788 0.784020 0.065895 0.071 Uiso 1 1 calc R U . . .
H9E H 0.592691 0.744553 0.051293 0.071 Uiso 1 1 calc R U . . .
C10 C 0.5668(17) 0.8976(12) 0.0418(9) 0.047(3) Uani 1 1 d . U . . .
H10C H 0.495893 0.849496 0.024685 0.071 Uiso 1 1 calc R U . . .
H10D H 0.565738 0.945232 0.013089 0.071 Uiso 1 1 calc R U . . .
H10E H 0.582103 0.916367 0.093925 0.071 Uiso 1 1 calc R U . . .
N6 N 0.2324(19) 0.8331(15) 0.2524(10) 0.087(4) Uani 1 1 d . U . . .
H6D H 0.164723 0.790668 0.240336 0.104 Uiso 1 1 d R U . . .
H6E H 0.232463 0.867768 0.216226 0.104 Uiso 1 1 d R U . . .
C11 C 0.244(2) 0.8803(18) 0.3151(12) 0.086(4) Uani 1 1 d . U . . .
H11A H 0.309582 0.883685 0.353128 0.130 Uiso 1 1 calc R U . . .
H11B H 0.180186 0.852884 0.332452 0.130 Uiso 1 1 calc R U . . .
H11C H 0.250308 0.938274 0.304387 0.130 Uiso 1 1 calc R U . . .
C12 C 0.302(2) 0.7949(19) 0.2481(12) 0.087(4) Uani 1 1 d . U . . .
H12A H 0.372749 0.824898 0.285364 0.131 Uiso 1 1 calc R U . . .
H12B H 0.312864 0.797707 0.199112 0.131 Uiso 1 1 calc R U . . .
H12C H 0.271856 0.734770 0.256721 0.131 Uiso 1 1 calc R U . . .
N7 N 0.4540(15) 0.1517(10) 0.3805(8) 0.054(4) Uani 1 1 d . U . . .
H7D H 0.492712 0.190229 0.355268 0.064 Uiso 1 1 d R U . . .
H7E H 0.385822 0.122269 0.349908 0.064 Uiso 1 1 d R U . . .
C13 C 0.448(2) 0.1976(18) 0.4463(14) 0.095(9) Uani 1 1 d . U . . .
H13A H 0.518918 0.217499 0.484267 0.142 Uiso 1 1 calc R U . . .
H13B H 0.392113 0.158251 0.465790 0.142 Uiso 1 1 calc R U . . .
H13C H 0.430283 0.246882 0.431649 0.142 Uiso 1 1 calc R U . . .
C14 C 0.5073(17) 0.0915(15) 0.4066(10) 0.061(5) Uani 1 1 d . U . . .
H14A H 0.561263 0.115534 0.454708 0.091 Uiso 1 1 calc R U . . .
H14B H 0.543587 0.082874 0.371336 0.091 Uiso 1 1 calc R U . . .
H14C H 0.452351 0.036390 0.410786 0.091 Uiso 1 1 calc R U . . .
N8 N 0.0682(12) 0.2021(7) 0.6761(6) 0.028(3) Uani 1 1 d . U . . .
H8D H 0.029173 0.203879 0.707001 0.033 Uiso 1 1 d R U . . .
H8E H 0.058353 0.237129 0.641361 0.033 Uiso 1 1 d R U . . .
C15 C 0.1900(18) 0.2363(14) 0.7200(11) 0.059(5) Uani 1 1 d . U . . .
H15A H 0.201661 0.198293 0.757117 0.088 Uiso 1 1 calc R U . . .
H15B H 0.212560 0.294125 0.744358 0.088 Uiso 1 1 calc R U . . .
H15C H 0.233113 0.238033 0.686467 0.088 Uiso 1 1 calc R U . . .
C16 C 0.026(2) 0.1133(11) 0.6397(9) 0.051(5) Uani 1 1 d . U . . .
H16A H 0.061017 0.112081 0.601830 0.077 Uiso 1 1 calc R U . . .
H16B H -0.053173 0.093389 0.616804 0.077 Uiso 1 1 calc R U . . .
H16C H 0.040660 0.075741 0.676224 0.077 Uiso 1 1 calc R U . . .
N9 N 0.0170(13) 0.1739(8) 0.3903(7) 0.036(3) Uani 1 1 d . U . . .
H9A H 0.007086 0.221124 0.403887 0.044 Uiso 1 1 d R U . . .
H9B H 0.027396 0.178885 0.345146 0.044 Uiso 1 1 d R U . . .
C17 C 0.1141(17) 0.1714(11) 0.4426(9) 0.042(4) Uani 1 1 d . U . . .
H17A H 0.125817 0.120984 0.428023 0.063 Uiso 1 1 calc R U . . .
H17B H 0.104608 0.168202 0.491826 0.063 Uiso 1 1 calc R U . . .
H17C H 0.177284 0.223453 0.443139 0.063 Uiso 1 1 calc R U . . .
C18 C -0.0859(18) 0.0943(12) 0.3851(10) 0.049(4) Uani 1 1 d . U . . .
H18A H -0.099925 0.090200 0.432949 0.074 Uiso 1 1 calc R U . . .
H18B H -0.075719 0.043014 0.370732 0.074 Uiso 1 1 calc R U . . .
H18C H -0.147907 0.098719 0.348148 0.074 Uiso 1 1 calc R U . . .
N10 N 0.7150(13) 0.2086(8) 0.2209(8) 0.041(3) Uani 1 1 d . U . . .
H10A H 0.704987 0.256753 0.231525 0.050 Uiso 1 1 d R U . . .
H10B H 0.787767 0.221443 0.234805 0.050 Uiso 1 1 d R U . . .
C19 C 0.667(2) 0.1795(15) 0.1351(9) 0.063(6) Uani 1 1 d . U . . .
H19A H 0.589191 0.169191 0.119425 0.095 Uiso 1 1 calc R U . . .
H19B H 0.675649 0.126716 0.123624 0.095 Uiso 1 1 calc R U . . .
H19C H 0.705434 0.224751 0.109081 0.095 Uiso 1 1 calc R U . . .
C20 C 0.664(2) 0.1425(13) 0.2623(9) 0.060(6) Uani 1 1 d . U . . .
H20A H 0.667440 0.088567 0.247071 0.090 Uiso 1 1 calc R U . . .
H20B H 0.587596 0.134498 0.253024 0.090 Uiso 1 1 calc R U . . .
H20C H 0.702000 0.159626 0.314940 0.090 Uiso 1 1 calc R U . . .
O1W O 0.2254(12) 0.6431(8) 0.0429(7) 0.052(4) Uani 1 1 d . . . . .
O2W O 0.481(2) 0.5579(13) 0.0356(10) 0.118(8) Uani 1 1 d . . . . .
O3W O 0.2879(13) 0.5923(9) 0.1844(7) 0.057(4) Uani 1 1 d . . . . .
O4W O 0.3794(12) 0.2867(9) 0.5894(7) 0.055(4) Uani 1 1 d . . . . .
O5W O 0.5096(12) 0.7079(9) 0.2616(8) 0.059(4) Uani 1 1 d . . . . .
O6W O 0.2686(13) 0.1096(8) 0.5908(7) 0.054(4) Uani 1 1 d . . . . .
O7W O 0.3768(12) 0.1083(9) 0.7430(7) 0.049(3) Uani 1 1 d . . . . .
O8W O 0.2614(14) 0.0090(8) 0.4710(7) 0.060(4) Uani 1 1 d . . . . .
O9W O 0.571(2) 0.6065(14) 0.1795(11) 0.133(10) Uani 1 1 d . . . . .
O10W O 0.6287(12) 0.3476(8) 0.0375(6) 0.049(3) Uani 1 1 d . . . . .
O11W O 0.450(2) 0.931(2) 0.1725(15) 0.187(14) Uani 1 1 d . . . . .


_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 O1 1.741(9) . ?
W1 O2 1.761(8) . ?
W1 O10 1.907(8) . ?
W1 O3 1.979(9) . ?
W1 O20 2.213(8) . ?
W1 O13 2.227(9) . ?
W2 O5 1.740(9) . ?
W2 O4 1.753(8) . ?
W2 O3 1.847(10) . ?
W2 O6 1.914(9) . ?
W2 O13 2.268(8) . ?
W2 O19 2.353(8) . ?
W3 O7 1.742(9) . ?
W3 O8 1.761(9) . ?
W3 O9 1.866(8) . ?
W3 O6 1.973(8) . ?
W3 O19 2.173(9) . ?
W3 O15 2.243(8) . ?
W4 O11 1.734(9) . ?
W4 O12 1.827(9) . ?
W4 O18 1.846(8) . ?
W4 O10 1.940(8) . ?
W4 O9 1.973(9) 2 ?
W4 O17 2.278(8) . ?
W5 O14 1.720(9) . ?
W5 O15 1.783(8) . ?
W5 O13 1.915(8) . ?
W5 O16 1.959(8) . ?
W5 O12 2.124(9) . ?
W5 O17 2.260(8) . ?
W6 O21 1.725(8) . ?
W6 O20 1.792(8) . ?
W6 O19 1.898(9) . ?
W6 O16 1.969(8) 2 ?
W6 O18 2.112(8) 2 ?
W6 O17 2.225(8) 2 ?
W7 O23 1.717(9) . ?
W7 O22 1.834(8) . ?
W7 O24 1.905(8) . ?
W7 O40 1.951(8) . ?
W7 O25 2.048(9) . ?
W7 O41 2.266(9) . ?
W8 O27 1.755(9) . ?
W8 O39 1.840(8) . ?
W8 O25 1.894(9) . ?
W8 O28 1.914(9) . ?
W8 O26 1.922(8) . ?
W8 O41 2.252(8) . ?
W9 O29 1.750(10) . ?
W9 O30 1.762(9) . ?
W9 O28 1.916(8) 2_766 ?
W9 O31 1.936(9) . ?
W9 O22 2.167(9) . ?
W9 O42 2.204(9) . ?
W10 O32 1.744(9) . ?
W10 O33 1.766(9) . ?
W10 O34 1.886(10) . ?
W10 O31 1.889(9) . ?
W10 O24 2.279(9) . ?
W10 O42 2.327(8) . ?
W11 O36 1.736(10) . ?
W11 O35 1.757(9) . ?
W11 O26 1.906(9) . ?
W11 O34 1.950(9) . ?
W11 O37 2.210(8) . ?
W11 O24 2.223(9) . ?
W12 O38 1.723(8) . ?
W12 O37 1.798(9) 2_766 ?
W12 O42 1.888(9) 2_766 ?
W12 O40 1.962(9) . ?
W12 O39 2.090(9) . ?
W12 O41 2.229(8) . ?
N1 C2 1.45(4) . ?
N1 C1 1.52(3) . ?
N1 H1A 0.8901 . ?
N1 H1B 0.8899 . ?
C1 H1C 0.9600 . ?
C1 H1D 0.9600 . ?
C1 H1E 0.9600 . ?
C2 H2C 0.9600 . ?
C2 H2D 0.9600 . ?
C2 H2E 0.9600 . ?
N2 C4 1.46(2) . ?
N2 C3 1.48(2) . ?
N2 H2A 0.8899 . ?
N2 H2B 0.8901 . ?
C3 H3A 0.9600 . ?
C3 H3B 0.9600 . ?
C3 H3C 0.9600 . ?
C4 H4A 0.9600 . ?
C4 H4B 0.9600 . ?
C4 H4C 0.9600 . ?
N3 C5 1.47(2) . ?
N3 C6 1.50(2) . ?
N3 H3D 0.8900 . ?
N3 H3E 0.8900 . ?
C5 H5C 0.9600 . ?
C5 H5D 0.9600 . ?
C5 H5E 0.9600 . ?
C6 H6A 0.9600 . ?
C6 H6B 0.9600 . ?
C6 H6C 0.9600 . ?
N4 C8 1.454(18) . ?
N4 C7 1.522(18) . ?
N4 H4D 0.8900 . ?
N4 H4E 0.8900 . ?
C7 H7A 0.9600 . ?
C7 H7B 0.9600 . ?
C7 H7C 0.9600 . ?
C8 H8A 0.9600 . ?
C8 H8B 0.9600 . ?
C8 H8C 0.9600 . ?
N5 C10 1.45(2) . ?
N5 C9 1.47(2) . ?
N5 H5A 0.8900 . ?
N5 H5B 0.8900 . ?
C9 H9C 0.9600 . ?
C9 H9D 0.9600 . ?
C9 H9E 0.9600 . ?
C10 H10C 0.9600 . ?
C10 H10D 0.9600 . ?
C10 H10E 0.9600 . ?
N6 C11 1.34(2) . ?
N6 C12 1.35(3) . ?
N6 H6D 0.8899 . ?
N6 H6E 0.8901 . ?
C11 H11A 0.9600 . ?
C11 H11B 0.9600 . ?
C11 H11C 0.9600 . ?
C12 H12A 0.9600 . ?
C12 H12B 0.9600 . ?
C12 H12C 0.9600 . ?
N7 C14 1.46(3) . ?
N7 C13 1.47(2) . ?
N7 H7D 0.8900 . ?
N7 H7E 0.8899 . ?
C13 H13A 0.9600 . ?
C13 H13B 0.9600 . ?
C13 H13C 0.9600 . ?
C14 H14A 0.9600 . ?
C14 H14B 0.9600 . ?
C14 H14C 0.9600 . ?
N8 C16 1.450(19) . ?
N8 C15 1.51(2) . ?
N8 H8D 0.8901 . ?
N8 H8E 0.8901 . ?
C15 H15A 0.9600 . ?
C15 H15B 0.9600 . ?
C15 H15C 0.9600 . ?
C16 H16A 0.9600 . ?
C16 H16B 0.9600 . ?
C16 H16C 0.9600 . ?
N9 C17 1.43(2) . ?
N9 C18 1.50(2) . ?
N9 H9A 0.8900 . ?
N9 H9B 0.8900 . ?
C17 H17A 0.9600 . ?
C17 H17B 0.9600 . ?
C17 H17C 0.9600 . ?
C18 H18A 0.9600 . ?
C18 H18B 0.9600 . ?
C18 H18C 0.9600 . ?
N10 C20 1.42(2) . ?
N10 C19 1.55(2) . ?
N10 H10A 0.8900 . ?
N10 H10B 0.8901 . ?
C19 H19A 0.9600 . ?
C19 H19B 0.9600 . ?
C19 H19C 0.9600 . ?
C20 H20A 0.9600 . ?
C20 H20B 0.9600 . ?
C20 H20C 0.9600 . ?

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
O1 W1 O2 102.5(4) . . ?
O1 W1 O10 98.5(4) . . ?
O2 W1 O10 98.2(4) . . ?
O1 W1 O3 98.3(4) . . ?
O2 W1 O3 95.8(4) . . ?
O10 W1 O3 155.3(4) . . ?
O1 W1 O20 89.2(4) . . ?
O2 W1 O20 168.0(4) . . ?
O10 W1 O20 82.4(3) . . ?
O3 W1 O20 79.8(3) . . ?
O1 W1 O13 163.9(4) . . ?
O2 W1 O13 91.5(4) . . ?
O10 W1 O13 87.1(3) . . ?
O3 W1 O13 72.2(3) . . ?
O20 W1 O13 76.6(3) . . ?
O5 W2 O4 103.6(4) . . ?
O5 W2 O3 96.0(4) . . ?
O4 W2 O3 99.6(4) . . ?
O5 W2 O6 99.9(4) . . ?
O4 W2 O6 97.8(4) . . ?
O3 W2 O6 152.9(4) . . ?
O5 W2 O13 162.9(4) . . ?
O4 W2 O13 91.7(4) . . ?
O3 W2 O13 73.6(3) . . ?
O6 W2 O13 85.3(3) . . ?
O5 W2 O19 90.0(4) . . ?
O4 W2 O19 164.5(4) . . ?
O3 W2 O19 86.2(3) . . ?
O6 W2 O19 72.1(3) . . ?
O13 W2 O19 76.0(3) . . ?
O7 W3 O8 103.3(5) . . ?
O7 W3 O9 98.8(4) . . ?
O8 W3 O9 98.8(4) . . ?
O7 W3 O6 93.5(4) . . ?
O8 W3 O6 97.2(4) . . ?
O9 W3 O6 157.0(4) . . ?
O7 W3 O19 162.0(4) . . ?
O8 W3 O19 92.2(4) . . ?
O9 W3 O19 87.7(4) . . ?
O6 W3 O19 75.2(3) . . ?
O7 W3 O15 87.2(4) . . ?
O8 W3 O15 168.8(4) . . ?
O9 W3 O15 83.2(3) . . ?
O6 W3 O15 78.1(3) . . ?
O19 W3 O15 76.9(3) . . ?
O11 W4 O12 102.9(4) . . ?
O11 W4 O18 101.7(4) . . ?
O12 W4 O18 92.9(4) . . ?
O11 W4 O10 102.1(4) . . ?
O12 W4 O10 87.7(4) . . ?
O18 W4 O10 155.4(3) . . ?
O11 W4 O9 100.1(4) . 2 ?
O12 W4 O9 156.6(4) . 2 ?
O18 W4 O9 86.2(4) . 2 ?
O10 W4 O9 83.6(3) . 2 ?
O11 W4 O17 177.5(4) . . ?
O12 W4 O17 76.8(3) . . ?
O18 W4 O17 75.8(3) . . ?
O10 W4 O17 80.4(3) . . ?
O9 W4 O17 80.3(3) 2 . ?
O14 W5 O15 105.2(4) . . ?
O14 W5 O13 101.0(4) . . ?
O15 W5 O13 96.1(4) . . ?
O14 W5 O16 98.4(4) . . ?
O15 W5 O16 93.0(4) . . ?
O13 W5 O16 155.5(4) . . ?
O14 W5 O12 93.7(4) . . ?
O15 W5 O12 161.0(4) . . ?
O13 W5 O12 81.6(3) . . ?
O16 W5 O12 82.5(3) . . ?
O14 W5 O17 162.8(4) . . ?
O15 W5 O17 89.2(3) . . ?
O13 W5 O17 86.4(3) . . ?
O16 W5 O17 71.1(3) . . ?
O12 W5 O17 71.8(3) . . ?
O21 W6 O20 104.7(4) . . ?
O21 W6 O19 102.1(4) . . ?
O20 W6 O19 96.5(4) . . ?
O21 W6 O16 96.4(4) . 2 ?
O20 W6 O16 93.1(4) . 2 ?
O19 W6 O16 156.1(4) . 2 ?
O21 W6 O18 91.7(4) . 2 ?
O20 W6 O18 163.3(3) . 2 ?
O19 W6 O18 83.3(4) . 2 ?
O16 W6 O18 81.2(4) 2 2 ?
O21 W6 O17 161.0(3) . 2 ?
O20 W6 O17 91.0(3) . 2 ?
O19 W6 O17 86.3(3) . 2 ?
O16 W6 O17 71.7(3) 2 2 ?
O18 W6 O17 72.2(3) 2 2 ?
W2 O3 W1 118.7(4) . . ?
W2 O6 W3 116.9(4) . . ?
W3 O9 W4 147.9(5) . 2 ?
W1 O10 W4 146.6(5) . . ?
W4 O12 W5 116.0(4) . . ?
W5 O13 W1 139.7(5) . . ?
W5 O13 W2 125.2(5) . . ?
W1 O13 W2 94.2(3) . . ?
W5 O15 W3 137.2(4) . . ?
W5 O16 W6 118.2(4) . 2 ?
W6 O17 W5 97.5(3) 2 . ?
W6 O17 W4 96.2(3) 2 . ?
W5 O17 W4 95.3(3) . . ?
W4 O18 W6 115.7(4) . 2 ?
W6 O19 W3 139.9(4) . . ?
W6 O19 W2 124.7(4) . . ?
W3 O19 W2 94.0(3) . . ?
W6 O20 W1 139.4(5) . . ?
O23 W7 O22 102.7(5) . . ?
O23 W7 O24 102.6(4) . . ?
O22 W7 O24 94.8(4) . . ?
O23 W7 O40 97.9(4) . . ?
O22 W7 O40 91.4(4) . . ?
O24 W7 O40 156.7(4) . . ?
O23 W7 O25 96.2(4) . . ?
O22 W7 O25 160.7(4) . . ?
O24 W7 O25 84.6(4) . . ?
O40 W7 O25 82.2(4) . . ?
O23 W7 O41 165.0(4) . . ?
O22 W7 O41 87.8(4) . . ?
O24 W7 O41 86.9(3) . . ?
O40 W7 O41 70.9(3) . . ?
O25 W7 O41 72.9(3) . . ?
O27 W8 O39 102.9(4) . . ?
O27 W8 O25 100.5(4) . . ?
O39 W8 O25 89.6(4) . . ?
O27 W8 O28 102.7(4) . . ?
O39 W8 O28 88.6(4) . . ?
O25 W8 O28 156.6(4) . . ?
O27 W8 O26 101.2(4) . . ?
O39 W8 O26 155.9(4) . . ?
O25 W8 O26 87.2(4) . . ?
O28 W8 O26 84.9(4) . . ?
O27 W8 O41 176.2(4) . . ?
O39 W8 O41 75.8(3) . . ?
O25 W8 O41 76.0(3) . . ?
O28 W8 O41 80.9(3) . . ?
O26 W8 O41 80.3(3) . . ?
O29 W9 O30 102.0(5) . . ?
O29 W9 O28 99.7(4) . 2_766 ?
O30 W9 O28 97.4(4) . 2_766 ?
O29 W9 O31 97.4(4) . . ?
O30 W9 O31 94.6(4) . . ?
O28 W9 O31 156.5(4) 2_766 . ?
O29 W9 O22 87.4(4) . . ?
O30 W9 O22 170.0(4) . . ?
O28 W9 O22 83.9(3) 2_766 . ?
O31 W9 O22 80.9(3) . . ?
O29 W9 O42 163.4(4) . . ?
O30 W9 O42 93.1(4) . . ?
O28 W9 O42 84.9(3) 2_766 . ?
O31 W9 O42 74.3(4) . . ?
O22 W9 O42 77.2(3) . . ?
O32 W10 O33 104.3(4) . . ?
O32 W10 O34 97.4(4) . . ?
O33 W10 O34 99.9(4) . . ?
O32 W10 O31 99.9(5) . . ?
O33 W10 O31 97.4(4) . . ?
O34 W10 O31 151.6(4) . . ?
O32 W10 O24 161.2(4) . . ?
O33 W10 O24 93.4(4) . . ?
O34 W10 O24 73.0(3) . . ?
O31 W10 O24 83.7(4) . . ?
O32 W10 O42 86.8(4) . . ?
O33 W10 O42 166.2(4) . . ?
O34 W10 O42 86.5(3) . . ?
O31 W10 O42 72.2(3) . . ?
O24 W10 O42 76.6(3) . . ?
O36 W11 O35 103.1(5) . . ?
O36 W11 O26 99.4(4) . . ?
O35 W11 O26 98.8(4) . . ?
O36 W11 O34 97.2(4) . . ?
O35 W11 O34 95.0(4) . . ?
O26 W11 O34 155.4(4) . . ?
O36 W11 O37 88.9(4) . . ?
O35 W11 O37 167.1(4) . . ?
O26 W11 O37 83.7(3) . . ?
O34 W11 O37 78.6(3) . . ?
O36 W11 O24 165.0(4) . . ?
O35 W11 O24 89.5(4) . . ?
O26 W11 O24 86.6(4) . . ?
O34 W11 O24 73.2(3) . . ?
O37 W11 O24 78.0(3) . . ?
O38 W12 O37 104.4(4) . 2_766 ?
O38 W12 O42 101.0(4) . 2_766 ?
O37 W12 O42 98.3(4) 2_766 2_766 ?
O38 W12 O40 98.7(4) . . ?
O37 W12 O40 91.6(4) 2_766 . ?
O42 W12 O40 154.9(3) 2_766 . ?
O38 W12 O39 91.4(4) . . ?
O37 W12 O39 163.3(3) 2_766 . ?
O42 W12 O39 83.6(4) 2_766 . ?
O40 W12 O39 80.6(4) . . ?
O38 W12 O41 161.5(4) . . ?
O37 W12 O41 91.8(3) 2_766 . ?
O42 W12 O41 85.1(3) 2_766 . ?
O40 W12 O41 71.5(3) . . ?
O39 W12 O41 71.7(3) . . ?
W7 O22 W9 135.5(4) . . ?
W7 O24 W11 138.3(5) . . ?
W7 O24 W10 126.7(5) . . ?
W11 O24 W10 94.0(3) . . ?
W8 O25 W7 115.7(4) . . ?
W11 O26 W8 149.2(6) . . ?
W8 O28 W9 149.0(5) . 2_766 ?
W10 O31 W9 118.8(5) . . ?
W10 O34 W11 118.3(4) . . ?
W12 O37 W11 138.4(5) 2_766 . ?
W8 O39 W12 116.1(4) . . ?
W7 O40 W12 119.1(4) . . ?
W12 O41 W8 96.3(3) . . ?
W12 O41 W7 97.2(3) . . ?
W8 O41 W7 95.3(3) . . ?
W12 O42 W9 141.6(4) 2_766 . ?
W12 O42 W10 123.4(4) 2_766 . ?
W9 O42 W10 93.2(3) . . ?
C2 N1 C1 116(2) . . ?
C2 N1 H1A 108.2 . . ?
C1 N1 H1A 108.3 . . ?
C2 N1 H1B 108.3 . . ?
C1 N1 H1B 108.2 . . ?
H1A N1 H1B 107.4 . . ?
N1 C1 H1C 109.5 . . ?
N1 C1 H1D 109.5 . . ?
H1C C1 H1D 109.5 . . ?
N1 C1 H1E 109.5 . . ?
H1C C1 H1E 109.5 . . ?
H1D C1 H1E 109.5 . . ?
N1 C2 H2C 109.5 . . ?
N1 C2 H2D 109.5 . . ?
H2C C2 H2D 109.5 . . ?
N1 C2 H2E 109.5 . . ?
H2C C2 H2E 109.5 . . ?
H2D C2 H2E 109.5 . . ?
C4 N2 C3 113.6(15) . . ?
C4 N2 H2A 108.9 . . ?
C3 N2 H2A 108.8 . . ?
C4 N2 H2B 108.8 . . ?
C3 N2 H2B 108.8 . . ?
H2A N2 H2B 107.7 . . ?
N2 C3 H3A 109.5 . . ?
N2 C3 H3B 109.5 . . ?
H3A C3 H3B 109.5 . . ?
N2 C3 H3C 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?
N2 C4 H4A 109.5 . . ?
N2 C4 H4B 109.5 . . ?
H4A C4 H4B 109.5 . . ?
N2 C4 H4C 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
C5 N3 C6 116.7(14) . . ?
C5 N3 H3D 108.2 . . ?
C6 N3 H3D 108.1 . . ?
C5 N3 H3E 108.1 . . ?
C6 N3 H3E 108.1 . . ?
H3D N3 H3E 107.3 . . ?
N3 C5 H5C 109.5 . . ?
N3 C5 H5D 109.5 . . ?
H5C C5 H5D 109.5 . . ?
N3 C5 H5E 109.5 . . ?
H5C C5 H5E 109.5 . . ?
H5D C5 H5E 109.5 . . ?
N3 C6 H6A 109.5 . . ?
N3 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
N3 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
C8 N4 C7 109.2(12) . . ?
C8 N4 H4D 109.9 . . ?
C7 N4 H4D 109.9 . . ?
C8 N4 H4E 109.8 . . ?
C7 N4 H4E 109.8 . . ?
H4D N4 H4E 108.3 . . ?
N4 C7 H7A 109.5 . . ?
N4 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
N4 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
N4 C8 H8A 109.5 . . ?
N4 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
N4 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C10 N5 C9 114.7(15) . . ?
C10 N5 H5A 108.6 . . ?
C9 N5 H5A 108.6 . . ?
C10 N5 H5B 108.6 . . ?
C9 N5 H5B 108.6 . . ?
H5A N5 H5B 107.6 . . ?
N5 C9 H9C 109.5 . . ?
N5 C9 H9D 109.5 . . ?
H9C C9 H9D 109.5 . . ?
N5 C9 H9E 109.5 . . ?
H9C C9 H9E 109.5 . . ?
H9D C9 H9E 109.5 . . ?
N5 C10 H10C 109.5 . . ?
N5 C10 H10D 109.5 . . ?
H10C C10 H10D 109.5 . . ?
N5 C10 H10E 109.5 . . ?
H10C C10 H10E 109.5 . . ?
H10D C10 H10E 109.5 . . ?
C11 N6 C12 123(2) . . ?
C11 N6 H6D 106.6 . . ?
C12 N6 H6D 106.6 . . ?
C11 N6 H6E 106.6 . . ?
C12 N6 H6E 106.7 . . ?
H6D N6 H6E 106.5 . . ?
N6 C11 H11A 109.5 . . ?
N6 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
N6 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
N6 C12 H12A 109.5 . . ?
N6 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
N6 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C14 N7 C13 108.5(18) . . ?
C14 N7 H7D 110.0 . . ?
C13 N7 H7D 110.1 . . ?
C14 N7 H7E 109.9 . . ?
C13 N7 H7E 109.9 . . ?
H7D N7 H7E 108.4 . . ?
N7 C13 H13A 109.5 . . ?
N7 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
N7 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
N7 C14 H14A 109.5 . . ?
N7 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
N7 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C16 N8 C15 113.4(15) . . ?
C16 N8 H8D 108.9 . . ?
C15 N8 H8D 109.0 . . ?
C16 N8 H8E 108.9 . . ?
C15 N8 H8E 108.9 . . ?
H8D N8 H8E 107.7 . . ?
N8 C15 H15A 109.5 . . ?
N8 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
N8 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
N8 C16 H16A 109.5 . . ?
N8 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
N8 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C17 N9 C18 113.1(13) . . ?
C17 N9 H9A 108.9 . . ?
C18 N9 H9A 109.0 . . ?
C17 N9 H9B 108.9 . . ?
C18 N9 H9B 109.0 . . ?
H9A N9 H9B 107.8 . . ?
N9 C17 H17A 109.5 . . ?
N9 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
N9 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
N9 C18 H18A 109.5 . . ?
N9 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
N9 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C20 N10 C19 111.8(14) . . ?
C20 N10 H10A 109.2 . . ?
C19 N10 H10A 109.3 . . ?
C20 N10 H10B 109.2 . . ?
C19 N10 H10B 109.3 . . ?
H10A N10 H10B 107.9 . . ?
N10 C19 H19A 109.5 . . ?
N10 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
N10 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
N10 C20 H20A 109.5 . . ?
N10 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
N10 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?

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
O5 W2 O3 W1 -176.4(5) . . . . ?
O4 W2 O3 W1 78.8(5) . . . . ?
O6 W2 O3 W1 -50.4(10) . . . . ?
O13 W2 O3 W1 -10.2(4) . . . . ?
O19 W2 O3 W1 -86.8(4) . . . . ?
O7 W3 O9 W4 -170.4(9) . . . 2 ?
O8 W3 O9 W4 84.5(9) . . . 2 ?
O6 W3 O9 W4 -48.8(14) . . . 2 ?
O19 W3 O9 W4 -7.3(9) . . . 2 ?
O15 W3 O9 W4 -84.4(9) . . . 2 ?
O11 W4 O12 W5 -177.8(4) . . . . ?
O18 W4 O12 W5 -75.0(4) . . . . ?
O10 W4 O12 W5 80.3(4) . . . . ?
O9 W4 O12 W5 12.3(11) 2 . . . ?
O17 W4 O12 W5 -0.3(4) . . . . ?
O14 W5 O15 W3 61.8(7) . . . . ?
O13 W5 O15 W3 -41.4(7) . . . . ?
O16 W5 O15 W3 161.3(7) . . . . ?
O12 W5 O15 W3 -123.2(9) . . . . ?
O17 W5 O15 W3 -127.7(7) . . . . ?
O11 W4 O18 W6 -179.0(5) . . . 2 ?
O12 W4 O18 W6 77.2(5) . . . 2 ?
O10 W4 O18 W6 -13.8(12) . . . 2 ?
O9 W4 O18 W6 -79.4(5) 2 . . 2 ?
O17 W4 O18 W6 1.6(4) . . . 2 ?
O21 W6 O19 W3 129.8(7) . . . . ?
O20 W6 O19 W3 -123.6(7) . . . . ?
O16 W6 O19 W3 -10.4(13) 2 . . . ?
O18 W6 O19 W3 39.5(6) 2 . . . ?
O17 W6 O19 W3 -33.0(6) 2 . . . ?
O21 W6 O19 W2 -67.1(5) . . . . ?
O20 W6 O19 W2 39.4(5) . . . . ?
O16 W6 O19 W2 152.7(6) 2 . . . ?
O18 W6 O19 W2 -157.4(5) 2 . . . ?
O17 W6 O19 W2 130.1(5) 2 . . . ?
O21 W6 O20 W1 64.9(8) . . . . ?
O19 W6 O20 W1 -39.5(7) . . . . ?
O16 W6 O20 W1 162.4(7) 2 . . . ?
O18 W6 O20 W1 -128.0(11) 2 . . . ?
O17 W6 O20 W1 -125.9(7) 2 . . . ?
O23 W7 O22 W9 58.2(7) . . . . ?
O24 W7 O22 W9 -45.9(7) . . . . ?
O40 W7 O22 W9 156.6(7) . . . . ?
O25 W7 O22 W9 -133.2(9) . . . . ?
O41 W7 O22 W9 -132.6(7) . . . . ?
O27 W8 O25 W7 179.3(4) . . . . ?
O39 W8 O25 W7 -77.7(5) . . . . ?
O28 W8 O25 W7 7.9(11) . . . . ?
O26 W8 O25 W7 78.4(4) . . . . ?
O41 W8 O25 W7 -2.3(4) . . . . ?
O32 W10 O31 W9 73.1(6) . . . . ?
O33 W10 O31 W9 179.1(5) . . . . ?
O34 W10 O31 W9 -53.5(10) . . . . ?
O24 W10 O31 W9 -88.3(5) . . . . ?
O42 W10 O31 W9 -10.3(4) . . . . ?
O32 W10 O34 W11 -173.8(5) . . . . ?
O33 W10 O34 W11 80.2(5) . . . . ?
O31 W10 O34 W11 -46.7(10) . . . . ?
O24 W10 O34 W11 -10.4(4) . . . . ?
O42 W10 O34 W11 -87.5(5) . . . . ?
O27 W8 O39 W12 179.7(5) . . . . ?
O25 W8 O39 W12 79.0(5) . . . . ?
O28 W8 O39 W12 -77.6(5) . . . . ?
O26 W8 O39 W12 -3.3(13) . . . . ?
O41 W8 O39 W12 3.3(4) . . . . ?

_refine_diff_density_max         4.215
_refine_diff_density_min         -4.202
_refine_diff_density_rms         0.478

####################################################################### 
# 
# 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_shelx_CCDC2
_database_code_depnum_ccdc_archive 'CCDC 1998542'
loop_
_audit_author_name
_audit_author_address
'Laura Bereczki'
;Research Centre for Natural Sciences
Hungary
;
_audit_update_record             
;
2020-12-17 deposited with the CCDC.	2020-12-28 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT971_shelx               
;
PROBLEM: Check Calcd Resid. Dens.  2.36A   From C2              4.65 eA-3
RESPONSE: Relatively large residual electron density can be found in the structure mainly next to the large tungsten atoms that give level A alerts when checking the cif files. In the structure, no void volumes can be found. These residual electron densities correspond to the imperfect fitting of the structure model in some very high electron density areas. Generally, large residual electron density is characteristic of polytungstate crystal structures.
;
# Added during the CSD deposition process: Thursday 17 December 2020 01:05 PM
# end Validation Reply Form


_audit_creation_method           SHELXL-2018/3
_chemical_name_systematic        
;
decakis(dimethylammonium) dihydrododecatungstate(10-).10 hydrate
;
_chemical_name_common            
;
dimethylammonium paratungstate B.10 hydrate
;
_chemical_melting_point          ?
_chemical_formula_moiety         'O42 W12, 10(C2 H8 N), 10(O)'
_chemical_formula_sum            'C20 H80 N10 O52 W12'
_chemical_formula_weight         3499.14

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
W W -0.8490 6.8722 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 2/c'
_space_group_name_Hall           '-C 2yc'

_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+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'

_cell_length_a                   14.7682(3)
_cell_length_b                   24.7368(4)
_cell_length_c                   21.1511(4)
_cell_angle_alpha                90
_cell_angle_beta                 108.924(8)
_cell_angle_gamma                90
_cell_volume                     7309.2(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    143(2)
_cell_measurement_reflns_used    228980
_cell_measurement_theta_min      3.040
_cell_measurement_theta_max      30.575

_exptl_crystal_description       prism
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    3.180
_exptl_crystal_F_000             6296
_exptl_transmission_factor_min   0.157571
_exptl_transmission_factor_max   0.340433
_exptl_crystal_size_max          0.70
_exptl_crystal_size_mid          0.55
_exptl_crystal_size_min          0.46
_exptl_absorpt_coefficient_mu    18.900
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_correction_T_min  0.158
_exptl_absorpt_correction_T_max  0.340
_exptl_absorpt_process_details   
;
  NUMABS, Numerical Absorption correction Program (T.Higashi, 2011)
;
_diffrn_ambient_temperature      143(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'Sealed Tube'
_diffrn_measurement_device_type  RAXIS-RAPID
_diffrn_measurement_method       dtprofit.ref
_diffrn_detector_area_resol_mean 10.0000
_diffrn_reflns_number            307689
_diffrn_reflns_av_unetI/netI     0.0336
_diffrn_reflns_av_R_equivalents  0.1595
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_k_min       -35
_diffrn_reflns_limit_k_max       35
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_theta_min         3.041
_diffrn_reflns_theta_max         30.508
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             11149
_reflns_number_gt                10769
_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.
;

_computing_data_collection       
;
RAPID-AUTO (Rigaku Corp., Tokyo, Japan, 2015)
;
_computing_cell_refinement       
;
RAPID-AUTO (Rigaku Corp., Tokyo, Japan, 2015)
;
_computing_data_reduction        
;
RAPID-AUTO (Rigaku Corp., Tokyo, Japan, 2015)
;
_computing_structure_solution    
;
L. Palatinus, G. Chapuis 2007 J. Appl. Cryst., Vol. 40, pp. 786-790.
;
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    
;
Spek, A.L. (2003). J.Appl.Cryst. 36,7-13.
;
_computing_publication_material  
;
C. F. Macrae, J. Appl. Cryst., 41, 466-470, 2008
;
_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)+891.2659P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     iterative
_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         11149
_refine_ls_number_parameters     435
_refine_ls_number_restraints     345
_refine_ls_R_factor_all          0.0825
_refine_ls_R_factor_gt           0.0796
_refine_ls_wR_factor_ref         0.1455
_refine_ls_wR_factor_gt          0.1446
_refine_ls_goodness_of_fit_ref   1.498
_refine_ls_restrained_S_all      1.477
_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 0.500000 0.13666(3) 0.250000 0.01097(14) Uani 1 2 d S TU P . .
W2 W 0.39032(4) 0.20920(2) 0.33393(3) 0.01016(11) Uani 1 1 d . U . . .
W3 W 0.36382(4) 0.25826(2) 0.16152(3) 0.00929(10) Uani 1 1 d . U . . .
W4 W 0.52415(4) 0.32779(2) 0.42509(2) 0.01030(10) Uani 1 1 d . U . . .
W5 W 0.35989(4) 0.39477(2) 0.16249(3) 0.00982(11) Uani 1 1 d . U . . .
W6 W 0.39057(4) 0.44346(2) 0.33605(3) 0.01184(11) Uani 1 1 d . U . . .
W7 W 0.500000 0.51257(3) 0.250000 0.01394(15) Uani 1 2 d S TU P . .
O1 O 0.4548(8) 0.0923(4) 0.1831(5) 0.0152(17) Uani 1 1 d . U . . .
O2 O 0.3836(7) 0.1559(4) 0.2631(5) 0.0109(6) Uani 1 1 d . U . . .
O3 O 0.4193(7) 0.1610(4) 0.3977(5) 0.0113(14) Uani 1 1 d . U . . .
O4 O 0.2650(7) 0.2138(4) 0.3136(5) 0.0141(14) Uani 1 1 d . U . . .
O5 O 0.4256(7) 0.2712(4) 0.3840(5) 0.0111(9) Uani 1 1 d . U . . .
O6 O 0.3685(7) 0.2633(4) 0.2465(5) 0.0101(7) Uani 1 1 d . U . . .
O7 O 0.2683(7) 0.2159(4) 0.1262(5) 0.0140(14) Uani 1 1 d . U . . .
O8 O 0.4690(7) 0.2097(4) 0.1783(5) 0.0094(8) Uani 1 1 d . U . . .
O9 O 0.3867(7) 0.2730(4) 0.0723(5) 0.0111(13) Uani 1 1 d . U . . .
O10 O 0.4674(6) 0.3260(4) 0.1802(4) 0.0094(10) Uani 1 1 d . U . . .
O11 O 0.2926(7) 0.3268(4) 0.1386(5) 0.0102(7) Uani 1 1 d . U . . .
O12 O 0.2676(8) 0.4389(4) 0.1253(5) 0.0167(16) Uani 1 1 d . U . . .
O13 O 0.4668(7) 0.4403(4) 0.1804(5) 0.0116(8) Uani 1 1 d . U . . .
O14 O 0.6118(7) 0.3810(4) 0.4270(5) 0.0110(9) Uani 1 1 d . U . . .
O15 O 0.5192(7) 0.3270(4) 0.5052(5) 0.0142(16) Uani 1 1 d . U . . .
O16 O 0.4200(7) 0.3765(4) 0.3809(5) 0.0110(7) Uani 1 1 d . U . . .
O17 O 0.3604(7) 0.3907(4) 0.2478(5) 0.0110(8) Uani 1 1 d . U . . .
O18 O 0.2701(8) 0.4456(4) 0.3278(5) 0.0154(14) Uani 1 1 d . U . . .
O19 O 0.4412(8) 0.4852(4) 0.4058(5) 0.0163(16) Uani 1 1 d . U . . .
O20 O 0.3847(8) 0.4959(4) 0.2668(5) 0.0137(6) Uani 1 1 d . U . . .
O21 O 0.5526(8) 0.5566(4) 0.3170(5) 0.0140(17) Uani 1 1 d . U . . .
N1 N 0.2248(12) 0.3235(7) 0.2943(8) 0.031(3) Uani 1 1 d . U . . .
H1A H 0.277571 0.341650 0.296138 0.037 Uiso 1 1 d R U . . .
H1B H 0.235619 0.288658 0.288748 0.037 Uiso 1 1 d R U . . .
C1 C 0.2069(16) 0.3302(9) 0.3595(10) 0.036(4) Uani 1 1 d . U . . .
H1C H 0.195787 0.367643 0.366245 0.054 Uiso 1 1 calc R U . . .
H1D H 0.261704 0.317776 0.395191 0.054 Uiso 1 1 calc R U . . .
H1E H 0.151784 0.309393 0.359052 0.054 Uiso 1 1 calc R U . . .
C2 C 0.1474(17) 0.3420(10) 0.2364(11) 0.044(5) Uani 1 1 d . U . . .
H2C H 0.097412 0.315333 0.224428 0.066 Uiso 1 1 calc R U . . .
H2D H 0.171093 0.347333 0.199585 0.066 Uiso 1 1 calc R U . . .
H2E H 0.122544 0.375433 0.246775 0.066 Uiso 1 1 calc R U . . .
N2 N 0.1578(10) 0.3141(5) 0.0136(7) 0.020(2) Uani 1 1 d . U . . .
H2A H 0.155281 0.285785 -0.012869 0.024 Uiso 1 1 d R U . . .
H2B H 0.213971 0.313205 0.046101 0.024 Uiso 1 1 d R U . . .
C3 C 0.0822(14) 0.3093(8) 0.0428(9) 0.031(4) Uani 1 1 d . U . . .
H3C H 0.087628 0.337981 0.074346 0.047 Uiso 1 1 calc R U . . .
H3D H 0.087530 0.275088 0.065205 0.047 Uiso 1 1 calc R U . . .
H3E H 0.021196 0.311498 0.008225 0.047 Uiso 1 1 calc R U . . .
C4 C 0.1523(14) 0.3647(7) -0.0262(9) 0.029(4) Uani 1 1 d . U . . .
H4C H 0.090553 0.367024 -0.059915 0.043 Uiso 1 1 calc R U . . .
H4D H 0.201108 0.364046 -0.047104 0.043 Uiso 1 1 calc R U . . .
H4E H 0.161730 0.395477 0.002850 0.043 Uiso 1 1 calc R U . . .
N3 N 0.1805(13) 0.1429(7) 0.1865(9) 0.032(3) Uani 1 1 d . U . . .
H3A H 0.205755 0.130862 0.228192 0.039 Uiso 1 1 d R U . . .
H3B H 0.218635 0.168872 0.180532 0.039 Uiso 1 1 d R U . . .
C5 C 0.0887(15) 0.1660(9) 0.1792(11) 0.035(3) Uani 1 1 d . U . . .
H5C H 0.062265 0.181128 0.135255 0.053 Uiso 1 1 calc R U . . .
H5D H 0.095651 0.193854 0.211993 0.053 Uiso 1 1 calc R U . . .
H5E H 0.046674 0.138383 0.185467 0.053 Uiso 1 1 calc R U . . .
C6 C 0.1802(15) 0.0982(8) 0.1404(10) 0.033(3) Uani 1 1 d . U . . .
H6A H 0.147692 0.067646 0.150898 0.050 Uiso 1 1 calc R U . . .
H6B H 0.244934 0.088431 0.145035 0.050 Uiso 1 1 calc R U . . .
H6C H 0.147811 0.109542 0.095314 0.050 Uiso 1 1 calc R U . . .
N4 N 0.3894(9) 0.0493(5) 0.3554(6) 0.017(2) Uani 1 1 d . U . . .
H4A H 0.338937 0.070086 0.352347 0.020 Uiso 1 1 d R U . . .
H4B H 0.435028 0.070386 0.349867 0.020 Uiso 1 1 d R U . . .
C7 C 0.3620(14) 0.0090(7) 0.3014(9) 0.027(3) Uani 1 1 d . U . . .
H7A H 0.417644 -0.010902 0.301116 0.040 Uiso 1 1 calc R U . . .
H7B H 0.334856 0.027062 0.259302 0.040 Uiso 1 1 calc R U . . .
H7C H 0.315702 -0.015339 0.308578 0.040 Uiso 1 1 calc R U . . .
C8 C 0.4241(15) 0.0254(8) 0.4231(9) 0.032(4) Uani 1 1 d . U . . .
H8A H 0.373625 0.004837 0.430927 0.048 Uiso 1 1 calc R U . . .
H8B H 0.443862 0.053670 0.455752 0.048 Uiso 1 1 calc R U . . .
H8C H 0.477487 0.002037 0.426574 0.048 Uiso 1 1 calc R U . . .
N5 N 0.1267(13) 0.0206(7) 0.4545(9) 0.034(3) Uani 1 1 d . U . . .
H5A H 0.070201 0.005602 0.449917 0.040 Uiso 1 1 d R U . . .
H5B H 0.137631 0.017062 0.415697 0.040 Uiso 1 1 d R U . . .
C9 C 0.1989(15) -0.0083(8) 0.5048(10) 0.032(3) Uani 1 1 d . U . . .
H9A H 0.259359 0.009702 0.513494 0.048 Uiso 1 1 calc R U . . .
H9B H 0.203586 -0.044431 0.489538 0.048 Uiso 1 1 calc R U . . .
H9C H 0.182370 -0.009588 0.545038 0.048 Uiso 1 1 calc R U . . .
C10 C 0.1211(19) 0.0786(9) 0.4688(12) 0.041(5) Uani 1 1 d . U . . .
H10A H 0.100320 0.082868 0.507011 0.062 Uiso 1 1 calc R U . . .
H10B H 0.076333 0.095992 0.430821 0.062 Uiso 1 1 calc R U . . .
H10C H 0.183124 0.094822 0.477731 0.062 Uiso 1 1 calc R U . . .
O1W O 0.3218(9) 0.1769(6) 0.4920(6) 0.029(3) Uani 1 1 d . . . . .
O2W O 0.4509(16) 0.0954(8) 0.5781(12) 0.070(6) Uani 1 1 d . . . . .
O3W O 0.2166(10) 0.1058(6) 0.3282(8) 0.037(3) Uani 1 1 d . . . . .
O4W O 0.3880(11) 0.0131(6) 0.6434(9) 0.041(4) Uani 1 1 d . . . . .
O5W O 0.1308(12) 0.2195(7) 0.4559(9) 0.048(4) Uani 1 1 d . . . . .


_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 O1 1.743(10) . ?
W1 O1 1.743(10) 2_655 ?
W1 O2 1.889(10) . ?
W1 O2 1.890(10) 2_655 ?
W1 O8 2.307(10) 2_655 ?
W1 O8 2.307(10) . ?
W2 O3 1.746(10) . ?
W2 O4 1.763(10) . ?
W2 O5 1.842(10) . ?
W2 O2 1.973(10) . ?
W2 O8 2.175(10) 2_655 ?
W2 O6 2.219(10) . ?
W3 O7 1.721(10) . ?
W3 O6 1.782(9) . ?
W3 O8 1.904(10) . ?
W3 O11 1.971(10) . ?
W3 O9 2.054(10) . ?
W3 O10 2.215(10) . ?
W4 O15 1.719(9) . ?
W4 O14 1.836(10) . ?
W4 O9 1.878(10) 2_655 ?
W4 O16 1.939(10) . ?
W4 O5 2.002(10) . ?
W4 O10 2.271(9) 2_655 ?
W5 O12 1.723(10) . ?
W5 O17 1.806(10) . ?
W5 O13 1.876(10) . ?
W5 O11 1.935(10) . ?
W5 O14 2.095(10) 2_655 ?
W5 O10 2.274(10) . ?
W6 O18 1.731(11) . ?
W6 O19 1.756(10) . ?
W6 O16 1.888(10) . ?
W6 O20 1.938(10) . ?
W6 O17 2.201(10) . ?
W6 O13 2.245(10) 2_655 ?
W7 O21 1.756(10) 2_655 ?
W7 O21 1.756(10) . ?
W7 O20 1.894(11) . ?
W7 O20 1.894(11) 2_655 ?
W7 O13 2.265(10) . ?
W7 O13 2.265(10) 2_655 ?
N1 C2 1.45(3) . ?
N1 C1 1.50(2) . ?
N1 H1A 0.8900 . ?
N1 H1B 0.8900 . ?
C1 H1C 0.9600 . ?
C1 H1D 0.9600 . ?
C1 H1E 0.9600 . ?
C2 H2C 0.9600 . ?
C2 H2D 0.9600 . ?
C2 H2E 0.9600 . ?
N2 C3 1.45(2) . ?
N2 C4 1.49(2) . ?
N2 H2A 0.8901 . ?
N2 H2B 0.8901 . ?
C3 H3C 0.9600 . ?
C3 H3D 0.9600 . ?
C3 H3E 0.9600 . ?
C4 H4C 0.9600 . ?
C4 H4D 0.9600 . ?
C4 H4E 0.9600 . ?
N3 C5 1.43(3) . ?
N3 C6 1.47(3) . ?
N3 H3A 0.8900 . ?
N3 H3B 0.8902 . ?
C5 H5C 0.9600 . ?
C5 H5D 0.9600 . ?
C5 H5E 0.9600 . ?
C6 H6A 0.9600 . ?
C6 H6B 0.9600 . ?
C6 H6C 0.9600 . ?
N4 C7 1.47(2) . ?
N4 C8 1.48(2) . ?
N4 H4A 0.8899 . ?
N4 H4B 0.8900 . ?
C7 H7A 0.9600 . ?
C7 H7B 0.9600 . ?
C7 H7C 0.9600 . ?
C8 H8A 0.9600 . ?
C8 H8B 0.9600 . ?
C8 H8C 0.9600 . ?
N5 C9 1.43(3) . ?
N5 C10 1.47(3) . ?
N5 H5A 0.8900 . ?
N5 H5B 0.8900 . ?
C9 H9A 0.9600 . ?
C9 H9B 0.9600 . ?
C9 H9C 0.9600 . ?
C10 H10A 0.9600 . ?
C10 H10B 0.9600 . ?
C10 H10C 0.9600 . ?

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
O1 W1 O1 102.0(7) . 2_655 ?
O1 W1 O2 98.7(5) . . ?
O1 W1 O2 99.6(5) 2_655 . ?
O1 W1 O2 99.6(5) . 2_655 ?
O1 W1 O2 98.7(5) 2_655 2_655 ?
O2 W1 O2 150.8(6) . 2_655 ?
O1 W1 O8 165.5(4) . 2_655 ?
O1 W1 O8 91.0(4) 2_655 2_655 ?
O2 W1 O8 72.6(4) . 2_655 ?
O2 W1 O8 84.4(4) 2_655 2_655 ?
O1 W1 O8 91.0(4) . . ?
O1 W1 O8 165.5(4) 2_655 . ?
O2 W1 O8 84.4(4) . . ?
O2 W1 O8 72.6(4) 2_655 . ?
O8 W1 O8 76.9(5) 2_655 . ?
O3 W2 O4 102.0(5) . . ?
O3 W2 O5 99.9(4) . . ?
O4 W2 O5 99.5(5) . . ?
O3 W2 O2 94.0(4) . . ?
O4 W2 O2 93.9(4) . . ?
O5 W2 O2 158.2(4) . . ?
O3 W2 O8 95.3(4) . 2_655 ?
O4 W2 O8 159.7(4) . 2_655 ?
O5 W2 O8 87.7(4) . 2_655 ?
O2 W2 O8 74.2(4) . 2_655 ?
O3 W2 O6 171.2(4) . . ?
O4 W2 O6 84.3(4) . . ?
O5 W2 O6 85.1(4) . . ?
O2 W2 O6 79.2(4) . . ?
O8 W2 O6 77.5(3) 2_655 . ?
O7 W3 O6 103.8(5) . . ?
O7 W3 O8 101.6(5) . . ?
O6 W3 O8 95.4(4) . . ?
O7 W3 O11 96.9(4) . . ?
O6 W3 O11 91.8(4) . . ?
O8 W3 O11 157.9(4) . . ?
O7 W3 O9 93.7(4) . . ?
O6 W3 O9 161.9(4) . . ?
O8 W3 O9 85.2(4) . . ?
O11 W3 O9 81.6(4) . . ?
O7 W3 O10 163.5(4) . . ?
O6 W3 O10 88.2(4) . . ?
O8 W3 O10 88.2(4) . . ?
O11 W3 O10 71.1(4) . . ?
O9 W3 O10 73.7(4) . . ?
O15 W4 O14 104.0(5) . . ?
O15 W4 O9 102.5(5) . 2_655 ?
O14 W4 O9 91.9(4) . 2_655 ?
O15 W4 O16 101.6(5) . . ?
O14 W4 O16 90.5(4) . . ?
O9 W4 O16 154.4(4) 2_655 . ?
O15 W4 O5 99.3(4) . . ?
O14 W4 O5 156.6(4) . . ?
O9 W4 O5 85.0(4) 2_655 . ?
O16 W4 O5 82.8(4) . . ?
O15 W4 O10 178.1(4) . 2_655 ?
O14 W4 O10 76.9(4) . 2_655 ?
O9 W4 O10 75.7(4) 2_655 2_655 ?
O16 W4 O10 80.1(4) . 2_655 ?
O5 W4 O10 79.9(4) . 2_655 ?
O12 W5 O17 103.7(5) . . ?
O12 W5 O13 101.6(5) . . ?
O17 W5 O13 95.8(4) . . ?
O12 W5 O11 99.7(5) . . ?
O17 W5 O11 92.7(4) . . ?
O13 W5 O11 154.4(4) . . ?
O12 W5 O14 92.9(5) . 2_655 ?
O17 W5 O14 163.2(4) . 2_655 ?
O13 W5 O14 83.1(4) . 2_655 ?
O11 W5 O14 81.9(4) . 2_655 ?
O12 W5 O10 162.8(4) . . ?
O17 W5 O10 91.0(4) . . ?
O13 W5 O10 85.4(4) . . ?
O11 W5 O10 70.4(4) . . ?
O14 W5 O10 72.1(3) 2_655 . ?
O18 W6 O19 102.2(5) . . ?
O18 W6 O16 98.0(5) . . ?
O19 W6 O16 97.3(5) . . ?
O18 W6 O20 96.3(5) . . ?
O19 W6 O20 98.2(5) . . ?
O16 W6 O20 156.1(4) . . ?
O18 W6 O17 90.8(4) . . ?
O19 W6 O17 167.0(4) . . ?
O16 W6 O17 81.7(4) . . ?
O20 W6 O17 79.0(4) . . ?
O18 W6 O13 166.1(4) . 2_655 ?
O19 W6 O13 89.1(4) . 2_655 ?
O16 W6 O13 88.5(4) . 2_655 ?
O20 W6 O13 73.7(4) . 2_655 ?
O17 W6 O13 77.9(4) . 2_655 ?
O21 W7 O21 103.4(7) 2_655 . ?
O21 W7 O20 95.6(5) 2_655 . ?
O21 W7 O20 99.9(5) . . ?
O21 W7 O20 99.9(5) 2_655 2_655 ?
O21 W7 O20 95.6(5) . 2_655 ?
O20 W7 O20 154.9(6) . 2_655 ?
O21 W7 O13 91.1(4) 2_655 . ?
O21 W7 O13 163.6(4) . . ?
O20 W7 O13 86.1(4) . . ?
O20 W7 O13 74.0(4) 2_655 . ?
O21 W7 O13 163.6(4) 2_655 2_655 ?
O21 W7 O13 91.1(4) . 2_655 ?
O20 W7 O13 74.0(4) . 2_655 ?
O20 W7 O13 86.1(4) 2_655 2_655 ?
O13 W7 O13 75.8(5) . 2_655 ?
W1 O2 W2 117.1(5) . . ?
W2 O5 W4 149.6(6) . . ?
W3 O6 W2 138.3(5) . . ?
W3 O8 W2 137.3(5) . 2_655 ?
W3 O8 W1 126.4(5) . . ?
W2 O8 W1 94.6(4) 2_655 . ?
W4 O9 W3 115.1(5) 2_655 . ?
W3 O10 W4 95.4(3) . 2_655 ?
W3 O10 W5 97.6(3) . . ?
W4 O10 W5 94.7(3) 2_655 . ?
W5 O11 W3 119.7(5) . . ?
W5 O13 W6 139.5(5) . 2_655 ?
W5 O13 W7 126.6(5) . . ?
W6 O13 W7 93.3(4) 2_655 . ?
W4 O14 W5 116.3(5) . 2_655 ?
W6 O16 W4 143.6(6) . . ?
W5 O17 W6 138.4(5) . . ?
W7 O20 W6 117.7(5) . . ?
C2 N1 C1 114.7(17) . . ?
C2 N1 H1A 108.5 . . ?
C1 N1 H1A 108.5 . . ?
C2 N1 H1B 108.7 . . ?
C1 N1 H1B 108.7 . . ?
H1A N1 H1B 107.6 . . ?
N1 C1 H1C 109.5 . . ?
N1 C1 H1D 109.5 . . ?
H1C C1 H1D 109.5 . . ?
N1 C1 H1E 109.5 . . ?
H1C C1 H1E 109.5 . . ?
H1D C1 H1E 109.5 . . ?
N1 C2 H2C 109.5 . . ?
N1 C2 H2D 109.5 . . ?
H2C C2 H2D 109.5 . . ?
N1 C2 H2E 109.5 . . ?
H2C C2 H2E 109.5 . . ?
H2D C2 H2E 109.5 . . ?
C3 N2 C4 113.7(14) . . ?
C3 N2 H2A 108.8 . . ?
C4 N2 H2A 108.8 . . ?
C3 N2 H2B 108.8 . . ?
C4 N2 H2B 108.9 . . ?
H2A N2 H2B 107.7 . . ?
N2 C3 H3C 109.5 . . ?
N2 C3 H3D 109.5 . . ?
H3C C3 H3D 109.5 . . ?
N2 C3 H3E 109.5 . . ?
H3C C3 H3E 109.5 . . ?
H3D C3 H3E 109.5 . . ?
N2 C4 H4C 109.5 . . ?
N2 C4 H4D 109.5 . . ?
H4C C4 H4D 109.5 . . ?
N2 C4 H4E 109.5 . . ?
H4C C4 H4E 109.5 . . ?
H4D C4 H4E 109.5 . . ?
C5 N3 C6 115.4(17) . . ?
C5 N3 H3A 108.5 . . ?
C6 N3 H3A 108.5 . . ?
C5 N3 H3B 108.4 . . ?
C6 N3 H3B 108.4 . . ?
H3A N3 H3B 107.5 . . ?
N3 C5 H5C 109.5 . . ?
N3 C5 H5D 109.5 . . ?
H5C C5 H5D 109.5 . . ?
N3 C5 H5E 109.5 . . ?
H5C C5 H5E 109.5 . . ?
H5D C5 H5E 109.5 . . ?
N3 C6 H6A 109.5 . . ?
N3 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
N3 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
C7 N4 C8 113.7(14) . . ?
C7 N4 H4A 108.8 . . ?
C8 N4 H4A 108.8 . . ?
C7 N4 H4B 108.9 . . ?
C8 N4 H4B 108.8 . . ?
H4A N4 H4B 107.7 . . ?
N4 C7 H7A 109.5 . . ?
N4 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
N4 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
N4 C8 H8A 109.5 . . ?
N4 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
N4 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C9 N5 C10 114.4(17) . . ?
C9 N5 H5A 108.6 . . ?
C10 N5 H5A 108.4 . . ?
C9 N5 H5B 108.8 . . ?
C10 N5 H5B 108.9 . . ?
H5A N5 H5B 107.6 . . ?
N5 C9 H9A 109.5 . . ?
N5 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
N5 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
N5 C10 H10A 109.5 . . ?
N5 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
N5 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?

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 W1 O2 W2 -178.2(6) . . . . ?
O1 W1 O2 W2 77.9(6) 2_655 . . . ?
O2 W1 O2 W2 -50.1(4) 2_655 . . . ?
O8 W1 O2 W2 -10.1(4) 2_655 . . . ?
O8 W1 O2 W2 -88.1(5) . . . . ?
O3 W2 O5 W4 93.8(11) . . . . ?
O4 W2 O5 W4 -162.2(11) . . . . ?
O2 W2 O5 W4 -35.0(19) . . . . ?
O8 W2 O5 W4 -1.2(11) 2_655 . . . ?
O6 W2 O5 W4 -78.9(11) . . . . ?
O7 W3 O6 W2 61.7(8) . . . . ?
O8 W3 O6 W2 -41.7(8) . . . . ?
O11 W3 O6 W2 159.3(8) . . . . ?
O9 W3 O6 W2 -132.6(12) . . . . ?
O10 W3 O6 W2 -129.7(8) . . . . ?
O12 W5 O13 W6 -128.6(8) . . . 2_655 ?
O17 W5 O13 W6 126.1(8) . . . 2_655 ?
O11 W5 O13 W6 17.2(15) . . . 2_655 ?
O14 W5 O13 W6 -37.0(7) 2_655 . . 2_655 ?
O10 W5 O13 W6 35.5(7) . . . 2_655 ?
O12 W5 O13 W7 63.5(7) . . . . ?
O17 W5 O13 W7 -41.8(6) . . . . ?
O11 W5 O13 W7 -150.7(7) . . . . ?
O14 W5 O13 W7 155.1(6) 2_655 . . . ?
O10 W5 O13 W7 -132.4(6) . . . . ?
O15 W4 O14 W5 179.5(5) . . . 2_655 ?
O9 W4 O14 W5 76.1(5) 2_655 . . 2_655 ?
O16 W4 O14 W5 -78.4(5) . . . 2_655 ?
O5 W4 O14 W5 -5.7(14) . . . 2_655 ?
O10 W4 O14 W5 1.3(5) 2_655 . . 2_655 ?
O18 W6 O16 W4 -173.9(9) . . . . ?
O19 W6 O16 W4 -70.4(10) . . . . ?
O20 W6 O16 W4 59.9(15) . . . . ?
O17 W6 O16 W4 96.5(9) . . . . ?
O13 W6 O16 W4 18.5(9) 2_655 . . . ?
O12 W5 O17 W6 -66.9(9) . . . . ?
O13 W5 O17 W6 36.6(8) . . . . ?
O11 W5 O17 W6 -167.5(8) . . . . ?
O14 W5 O17 W6 121.9(13) 2_655 . . . ?
O10 W5 O17 W6 122.1(8) . . . . ?
O21 W7 O20 W6 176.9(6) 2_655 . . . ?
O21 W7 O20 W6 -78.4(6) . . . . ?
O20 W7 O20 W6 48.9(5) 2_655 . . . ?
O13 W7 O20 W6 86.2(6) . . . . ?
O13 W7 O20 W6 9.8(5) 2_655 . . . ?

_refine_diff_density_max         4.292
_refine_diff_density_min         -5.371
_refine_diff_density_rms         0.451

