# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2019

####################################################################### 
# 
# 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_DMA-1
_database_code_depnum_ccdc_archive 'CCDC 1946814'
loop_
_audit_author_name
_audit_author_address
'Pavel Abramov'
;Nikolaev Institute of Inorganic Chemistry SB RAS
Russia
;
_audit_update_record             
;
2019-09-05 deposited with the CCDC.	2019-09-26 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT971_DMA-1               
;
PROBLEM: Check Calcd Resid. Dens.  0.81A   From W11             3.77 eA-3
RESPONSE: Residual electronic density without any chemical sense
;
_vrf_PLAT201_DMA-1               
;
PROBLEM: Isotropic non-H Atoms in Main Residue(s) .......          7 Report
RESPONSE: Disordered cations with small occupancies, As and some O-ligands of POM refined isotropically due to high absorption
;
_vrf_PLAT306_DMA-1               
;
PROBLEM: Isolated Oxygen Atom (H-atoms Missing ?) .......       O11W Check
RESPONSE: H-atoms of water molecules were not localized
;
_vrf_PLAT430_DMA-1               
;
PROBLEM: Short Inter D...A Contact  O1W      ..O11W     .       2.79 Ang.
RESPONSE: H-bond
;
_vrf_PLAT971_DMA-1_2             
;
PROBLEM: Check Calcd Resid. Dens.  0.78A   From W9              3.25 eA-3
RESPONSE: Residual electronic density without any chemical sense.
;
# Added during the CSD deposition process: Wednesday 04 September 2019 01:05 PM
# end Validation Reply Form

#complex 1 ((CH3)2NH2)7[As2W17{Ru(NO)}O61].4.5H2O (analytical data)
#{Ru(NO)}-group is fully disordered over 18 positions
_audit_creation_method           SHELXL-2017/1
_shelx_SHELXL_version_number     2017/1
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C10.40 H40.80 As2 N5.20 O66 Ru0 W18'
_chemical_formula_weight         4754.02

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'
As As 0.0499 2.0058 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ru Ru -1.2594 0.8363 '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           14
_space_group_name_H-M_alt        'P 21/n'
_space_group_name_Hall           '-P 2yn'

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

_cell_length_a                   22.9019(4)
_cell_length_b                   13.94647(19)
_cell_length_c                   24.2943(4)
_cell_angle_alpha                90
_cell_angle_beta                 113.566(2)
_cell_angle_gamma                90
_cell_volume                     7112.4(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    130(2)
_cell_measurement_reflns_used    16382
_cell_measurement_theta_min      2.2850
_cell_measurement_theta_max      29.4350

_exptl_crystal_description       plate
_exptl_crystal_colour            red
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    4.440
_exptl_crystal_F_000             8262
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.222
_exptl_crystal_size_mid          0.153
_exptl_crystal_size_min          0.067
_exptl_absorpt_coefficient_mu    30.011
_shelx_estimated_absorpt_T_min   0.057
_shelx_estimated_absorpt_T_max   0.238
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_correction_T_min  0.966
_exptl_absorpt_correction_T_max  0.988

loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
1 -20 -1 0.0997
-1 20 1 0.0971
16 -2 20 0.0627
29 2 -26 0.0497
-29 -2 25 0.0153
-16 3 -20 0.0852
8 0 -34 0.0745

_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      130(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'sealed X-ray tube'
_diffrn_measurement_device_type  'New Xcalibur, AtlasS2'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 10.6168
_diffrn_reflns_number            39135
_diffrn_reflns_av_unetI/netI     0.0598
_diffrn_reflns_av_R_equivalents  0.0428
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_theta_min         1.940
_diffrn_reflns_theta_max         26.021
_diffrn_reflns_theta_full        25.500
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measured_fraction_theta_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_point_group_measured_fraction_full 0.993
_reflns_number_total             13888
_reflns_number_gt                10986
_reflns_threshold_expression     >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       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_structure_solution    'SHELXS-2014 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_molecular_graphics    'ShelXle (Hübschle, 2011)'
_computing_publication_material  'CIFTAB-2014 (Sheldrick, 2014)'
_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)+(0.0440P)²+40.0442P] 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         13888
_refine_ls_number_parameters     829
_refine_ls_number_restraints     19
_refine_ls_R_factor_all          0.0603
_refine_ls_R_factor_gt           0.0420
_refine_ls_wR_factor_ref         0.0995
_refine_ls_wR_factor_gt          0.0922
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_restrained_S_all      1.045
_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
C1 C 0.1125(14) 0.217(2) 0.7891(13) 0.065(8) Uiso 0.7 1 d . . P . .
H1A H 0.087696 0.260275 0.802965 0.098 Uiso 0.7 1 calc R U P . .
H1B H 0.094439 0.152070 0.784368 0.098 Uiso 0.7 1 calc R U P . .
H1C H 0.111252 0.239196 0.750373 0.098 Uiso 0.7 1 calc R U P . .
C2 C 0.1997(15) 0.303(2) 0.8511(14) 0.068(9) Uiso 0.7 1 d . . P . .
H2A H 0.190669 0.344100 0.815771 0.103 Uiso 0.7 1 calc R U P . .
H2B H 0.245712 0.301926 0.875131 0.103 Uiso 0.7 1 calc R U P . .
H2C H 0.177888 0.329015 0.875314 0.103 Uiso 0.7 1 calc R U P . .
C6 C 0.6319(7) 0.6527(9) 0.5853(6) 0.024(3) Uiso 1 1 d . . . . .
H6A H 0.677858 0.651553 0.595399 0.036 Uiso 1 1 calc R U . . .
H6B H 0.624508 0.668428 0.621340 0.036 Uiso 1 1 calc R U . . .
H6C H 0.611729 0.701295 0.554384 0.036 Uiso 1 1 calc R U . . .
C7 C 0.6371(7) 0.5071(9) 0.5282(6) 0.022(3) Uiso 1 1 d . . . . .
H7A H 0.634915 0.547654 0.494516 0.033 Uiso 1 1 calc R U . . .
H7B H 0.616572 0.445354 0.512884 0.033 Uiso 1 1 calc R U . . .
H7C H 0.681810 0.496320 0.554956 0.033 Uiso 1 1 calc R U . . .
C8 C 0.8868(7) 0.3169(10) 0.7037(6) 0.026(3) Uiso 1 1 d . . . . .
H8A H 0.928961 0.328239 0.703582 0.039 Uiso 1 1 calc R U . . .
H8B H 0.854040 0.344003 0.667185 0.039 Uiso 1 1 calc R U . . .
H8C H 0.879788 0.247720 0.704983 0.039 Uiso 1 1 calc R U . . .
C9 C 0.9267(7) 0.3169(10) 0.8128(6) 0.025(3) Uiso 1 1 d . . . . .
H9A H 0.919880 0.247423 0.810017 0.038 Uiso 1 1 calc R U . . .
H9B H 0.918123 0.342108 0.846536 0.038 Uiso 1 1 calc R U . . .
H9C H 0.970841 0.330981 0.819251 0.038 Uiso 1 1 calc R U . . .
C11 C 0.0565(18) 0.251(2) 0.6073(16) 0.046(9) Uiso 0.5 1 d . . P . .
H11A H 0.010810 0.252056 0.581660 0.069 Uiso 0.5 1 calc R U P . .
H11B H 0.074534 0.314895 0.608162 0.069 Uiso 0.5 1 calc R U P . .
H11C H 0.062605 0.232196 0.648153 0.069 Uiso 0.5 1 calc R U P . .
C12 C 0.062(2) 0.102(3) 0.5416(19) 0.087(15) Uiso 0.5 1 d D . P . .
H12A H 0.019938 0.087170 0.540675 0.130 Uiso 0.5 1 calc R U P . .
H12B H 0.089465 0.045001 0.554874 0.130 Uiso 0.5 1 calc R U P . .
H12C H 0.058175 0.120290 0.501364 0.130 Uiso 0.5 1 calc R U P . .
N1 N 0.6038(6) 0.5554(7) 0.5621(5) 0.022(3) Uiso 1 1 d . . . . .
H1D H 0.606317 0.517841 0.593593 0.026 Uiso 1 1 calc R U . . .
H1E H 0.561832 0.562469 0.537656 0.026 Uiso 1 1 calc R U . . .
N2 N 0.8831(6) 0.3626(8) 0.7565(5) 0.029(3) Uiso 1 1 d . . . . .
H2D H 0.842470 0.358749 0.754007 0.034 Uiso 1 1 calc R U . . .
H2E H 0.893309 0.425805 0.757064 0.034 Uiso 1 1 calc R U . . .
N4 N 0.1790(9) 0.2147(12) 0.8334(8) 0.032(4) Uiso 0.7 1 d . . P . .
H4A H 0.181741 0.179100 0.865700 0.038 Uiso 0.7 1 calc R U P . .
H4B H 0.204078 0.186753 0.816788 0.038 Uiso 0.7 1 calc R U P . .
N8 N 0.0898(14) 0.1788(19) 0.5824(12) 0.044(7) Uiso 0.5 1 d D . P . .
H8D H 0.110854 0.214836 0.564915 0.053 Uiso 0.5 1 calc R U P . .
H8E H 0.120458 0.151268 0.615194 0.053 Uiso 0.5 1 calc R U P . .
O1 O 0.2290(4) 0.1664(7) 0.6583(4) 0.022(2) Uani 1 1 d . . . . .
O2 O 0.1876(5) 0.3131(7) 0.7126(4) 0.030(2) Uani 1 1 d . U . . .
O61 O 0.2702(5) 0.1682(7) 0.7782(4) 0.024(2) Uani 1 1 d . . . . .
O62 O 0.5000(4) 0.5396(6) 0.7335(4) 0.017(2) Uani 1 1 d . . . . .
O63 O 0.5318(4) 0.0540(6) 0.6694(4) 0.021(2) Uani 1 1 d . . . . .
O64 O 0.7305(4) 0.3452(6) 0.6305(4) 0.017(2) Uani 1 1 d . . . . .
O1W O 0.3193(9) 0.6781(12) 0.5500(8) 0.066(5) Uiso 0.8 1 d . . P . .
O65 O 0.6885(4) 0.6626(6) 0.7488(4) 0.020(2) Uani 1 1 d . . . . .
O66 O 0.5449(5) 0.6465(6) 0.8419(4) 0.022(2) Uani 1 1 d . . . . .
O3 O 0.8199(4) 0.3478(6) 0.8772(4) 0.017(2) Uani 1 1 d . . . . .
O5 O 0.3207(5) 0.0015(7) 0.8473(4) 0.024(2) Uani 1 1 d . . . . .
O5W O 0.3672(15) 0.372(2) 0.9697(13) 0.076(9) Uiso 0.5 1 d . . P . .
O6W O 0.6220(14) 0.7705(19) 0.9486(12) 0.088(8) Uiso 0.6 1 d . . P . .
O9 O 0.4124(4) 0.0173(6) 0.7964(4) 0.021(2) Uani 1 1 d . . . . .
O8W O 0.7058(11) -0.0866(15) 0.9652(10) 0.078(7) Uiso 0.7 1 d . . P . .
O10 O 0.2893(6) 0.0168(8) 0.7221(5) 0.033(3) Uani 1 1 d . . . . .
O11 O 0.4687(4) 0.6432(6) 0.6248(4) 0.019(2) Uani 1 1 d . . . . .
O12 O 0.5249(4) -0.0755(6) 0.8570(4) 0.021(2) Uani 1 1 d . . . . .
O11W O 0.3975(6) -0.2099(9) 0.5126(6) 0.058(4) Uani 1 1 d . . . . .
O13 O 0.6741(4) 0.3356(6) 0.9743(4) 0.024(2) Uani 1 1 d . . . . .
O14 O 0.6938(4) 0.4902(5) 0.6898(4) 0.0119(18) Uiso 1 1 d . . . . .
O15 O 0.5193(4) 0.3700(6) 0.6762(4) 0.012(2) Uani 1 1 d . . . . .
O16 O 0.4795(4) -0.0449(6) 0.7333(4) 0.019(2) Uani 1 1 d . . . . .
O17 O 0.4089(4) 0.4806(6) 0.6344(4) 0.017(2) Uani 1 1 d . . . . .
O18 O 0.5819(4) 0.5497(6) 0.6835(4) 0.014(2) Uani 1 1 d . . . . .
O19 O 0.5858(4) 0.2127(6) 0.7422(4) 0.017(2) Uani 1 1 d . . . . .
O20 O 0.4013(4) 0.2912(6) 0.6677(4) 0.017(2) Uani 1 1 d . . . . .
O21 O 0.3746(4) 0.4521(6) 0.7266(4) 0.020(2) Uani 1 1 d . . . . .
O22 O 0.5442(4) 0.2117(6) 0.6146(4) 0.017(2) Uani 1 1 d . . . . .
O23 O 0.3207(4) 0.3428(6) 0.7797(4) 0.020(2) Uani 1 1 d . . . . .
O24 O 0.3179(5) 0.3516(6) 0.5714(4) 0.021(2) Uani 1 1 d . . . . .
O25 O 0.5105(4) 0.3284(6) 0.5114(4) 0.021(2) Uani 1 1 d . . . . .
O26 O 0.4944(4) 0.4677(6) 0.5823(4) 0.016(2) Uani 1 1 d . . . . .
O27 O 0.6048(4) 0.3715(5) 0.6182(3) 0.0108(18) Uani 1 1 d . U . . .
O28 O 0.7569(4) 0.3428(6) 0.7520(4) 0.0156(19) Uani 1 1 d . U . . .
O29 O 0.7374(4) 0.4916(6) 0.8105(4) 0.0142(19) Uiso 1 1 d . . . . .
O30 O 0.6221(4) 0.5503(5) 0.7985(3) 0.0112(18) Uiso 1 1 d . . . . .
O31 O 0.6457(4) 0.3800(6) 0.7450(4) 0.015(2) Uani 1 1 d . . . . .
O32 O 0.6659(4) 0.2237(6) 0.6796(4) 0.015(2) Uani 1 1 d . . . . .
O33 O 0.5629(4) 0.3723(6) 0.7998(4) 0.019(2) Uani 1 1 d . . . . .
O34 O 0.4759(4) 0.4803(6) 0.8267(4) 0.019(2) Uani 1 1 d . . . . .
O35 O 0.7151(4) 0.2249(6) 0.8188(4) 0.016(2) Uani 1 1 d . . . . .
O36 O 0.6032(4) 0.4720(6) 0.8921(4) 0.022(2) Uani 1 1 d . . . . .
O37 O 0.6954(4) 0.3743(6) 0.8729(3) 0.013(2) Uani 1 1 d . . . . .
O38 O 0.7097(4) 0.0530(6) 0.8727(4) 0.021(2) Uani 1 1 d . . . . .
O39 O 0.6360(4) 0.2145(6) 0.8696(4) 0.019(2) Uani 1 1 d . . . . .
O40 O 0.5508(4) 0.2999(6) 0.9018(4) 0.018(2) Uani 1 1 d . . . . .
O41 O 0.4297(4) 0.3503(6) 0.8815(4) 0.021(2) Uani 1 1 d . . . . .
O42 O 0.3627(5) 0.5172(6) 0.8336(4) 0.025(2) Uani 1 1 d . . . . .
O43 O 0.3932(5) 0.1665(6) 0.8523(4) 0.024(2) Uani 1 1 d . . . . .
O44 O 0.4463(4) 0.2904(6) 0.7931(4) 0.019(2) Uani 1 1 d . . . . .
O45 O 0.3229(4) 0.2043(7) 0.4970(4) 0.021(2) Uani 1 1 d . . . . .
O46 O 0.2311(5) -0.0029(7) 0.5959(4) 0.024(2) Uani 1 1 d . . . . .
O47 O 0.4310(4) 0.2999(5) 0.5674(3) 0.0093(17) Uiso 1 1 d . . . . .
O48 O 0.4164(4) 0.1272(6) 0.6042(4) 0.018(2) Uani 1 1 d . . . . .
O49 O 0.4369(5) -0.0726(6) 0.6088(4) 0.022(2) Uani 1 1 d . . . . .
O50 O 0.6224(4) 0.0521(6) 0.6236(4) 0.020(2) Uani 1 1 d . . . . .
O51 O 0.6550(4) 0.0726(6) 0.7470(4) 0.016(2) Uani 1 1 d . . . . .
O52 O 0.4913(5) 0.2019(7) 0.9608(4) 0.025(2) Uani 1 1 d . . . . .
O53 O 0.5813(5) 0.0544(6) 0.8096(4) 0.023(2) Uani 1 1 d . . . . .
O54 O 0.3467(4) 0.1762(6) 0.7251(4) 0.016(2) Uiso 1 1 d . . . . .
O55 O 0.3630(4) 0.0178(6) 0.6586(4) 0.018(2) Uani 1 1 d . . . . .
O56 O 0.3028(4) 0.1646(6) 0.5982(4) 0.015(2) Uani 1 1 d . . . . .
O57 O 0.2791(4) 0.3420(6) 0.6623(4) 0.019(2) Uani 1 1 d . . . . .
O58 O 0.2853(4) 0.5191(6) 0.6139(4) 0.024(2) Uani 1 1 d . . . . .
O59 O 0.4658(4) 0.1330(6) 0.7326(4) 0.014(2) Uani 1 1 d . . . . .
O60 O 0.5079(4) 0.1258(6) 0.8607(4) 0.021(2) Uani 1 1 d . . . . .
As1 As 0.57577(6) 0.33295(8) 0.74070(5) 0.0090(3) Uiso 1 1 d . . . . .
As2 As 0.41683(6) 0.22497(8) 0.72948(5) 0.0112(3) Uiso 1 1 d . . . . .
W1 W 0.49166(3) 0.53175(4) 0.65262(2) 0.01469(13) Uani 1 1 d . . . . .
W1A W 0.25951(3) 0.26770(4) 0.71783(3) 0.01766(14) Uani 0.94 1 d . . P . .
W1B W 0.3023(7) 0.2150(10) 0.7950(6) 0.047(3) Uiso 0.06 1 d . . P . .
W3 W 0.66605(2) 0.54606(3) 0.74742(2) 0.01261(13) Uani 1 1 d . . . . .
W2A W 0.33783(3) 0.07536(4) 0.79880(2) 0.01475(14) Uani 0.94 1 d . . P . .
W2B W 0.2456(7) 0.2294(10) 0.6437(6) 0.051(3) Uiso 0.06 1 d . . P . .
W4 W 0.68929(3) 0.35399(3) 0.67457(2) 0.01225(12) Uani 1 1 d . . . . .
W3A W 0.28351(3) 0.07228(4) 0.64809(2) 0.01516(14) Uani 0.94 1 d . . P . .
W3B W 0.3177(10) 0.0251(13) 0.7132(8) 0.054(5) Uiso 0.06 1 d . . P . .
W5 W 0.74372(2) 0.35271(3) 0.82615(2) 0.01194(12) Uani 1 1 d . . . . .
W6 W 0.60455(3) 0.12599(3) 0.67094(2) 0.01402(13) Uani 1 1 d . . . . .
W7 W 0.65595(3) 0.12736(4) 0.82201(2) 0.01517(13) Uani 1 1 d . . . . .
W8 W 0.62908(3) 0.34104(4) 0.89913(2) 0.01437(13) Uani 1 1 d . . . . .
W9 W 0.51402(3) 0.33348(3) 0.58282(2) 0.01197(12) Uani 1 1 d . . . . .
W10 W 0.35745(3) 0.23141(4) 0.57114(2) 0.01421(13) Uani 1 1 d . . . . .
W11 W 0.33719(3) 0.42666(4) 0.64352(2) 0.01660(13) Uani 1 1 d . . . . .
W12 W 0.39419(3) 0.42411(4) 0.80898(2) 0.01885(14) Uani 1 1 d . . . . .
W13 W 0.44721(3) 0.02285(4) 0.65715(2) 0.01564(13) Uani 1 1 d . . . . .
W14 W 0.50020(3) 0.01974(4) 0.80882(2) 0.01646(13) Uani 1 1 d . . . . .
W15 W 0.47504(3) 0.23152(4) 0.88809(2) 0.01587(13) Uani 1 1 d . . . . .
W17 W 0.54812(3) 0.53230(4) 0.81779(2) 0.01494(13) Uani 1 1 d . . . . .
C11A C 0.343(2) -0.111(3) 0.9915(18) 0.080(12) Uiso 0.6 1 d . . P A 1
H11D H 0.341260 -0.154457 0.959219 0.120 Uiso 0.6 1 calc R U P A 1
H11E H 0.303415 -0.118692 0.998326 0.120 Uiso 0.6 1 calc R U P A 1
H11F H 0.379444 -0.126794 1.028369 0.120 Uiso 0.6 1 calc R U P A 1
C14 C 0.4129(10) 0.0152(14) 0.9896(9) 0.015(5) Uiso 0.6 1 d . . P A 1
H14A H 0.438383 -0.043155 1.003814 0.022 Uiso 0.6 1 calc R U P A 1
H14B H 0.426484 0.063263 1.021722 0.022 Uiso 0.6 1 calc R U P A 1
H14C H 0.419072 0.040545 0.954678 0.022 Uiso 0.6 1 calc R U P A 1
N7 N 0.3479(10) -0.0064(14) 0.9732(9) 0.029(5) Uiso 0.6 1 d . . P A 1
H7D H 0.326167 0.000857 0.932914 0.035 Uiso 0.6 1 calc R U P A 1
H7E H 0.330912 0.034068 0.992232 0.035 Uiso 0.6 1 calc R U P A 1
O12W O 0.3324(13) -0.1899(17) 0.9485(11) 0.031(6) Uiso 0.4 1 d . . P B 2
N6 N 0.466(2) -0.043(3) 0.5050(18) 0.055(11) Uiso 0.4 1 d . . P C -1
C10 C 0.5295(11) -0.0731(16) 0.5125(10) 0.049(6) Uiso 0.8 1 d . . P C -1
H10A H 0.538086 -0.051307 0.478093 0.073 Uiso 0.8 1 calc R U P C -1
H10B H 0.531978 -0.143204 0.514884 0.073 Uiso 0.8 1 calc R U P C -1
H10C H 0.561081 -0.045453 0.549474 0.073 Uiso 0.8 1 calc R U P C -1
N3 N 0.7114(12) 0.0924(16) 0.5696(10) 0.042(6) Uiso 0.6 1 d . . P D 3
H3A H 0.675063 0.127562 0.558481 0.050 Uiso 0.6 1 calc R U P D 3
H3B H 0.718337 0.063790 0.605383 0.050 Uiso 0.6 1 calc R U P D 3
C3A C 0.7617(12) 0.1520(18) 0.5764(11) 0.085(8) Uiso 0.6 1 d . . P D 3
H3A1 H 0.797864 0.113687 0.577048 0.127 Uiso 0.6 1 calc R U P D 3
H3A2 H 0.774201 0.187424 0.614274 0.127 Uiso 0.6 1 calc R U P D 3
H3A3 H 0.748978 0.197351 0.542867 0.127 Uiso 0.6 1 calc R U P D 3
C4A C 0.7032(11) 0.0149(15) 0.5220(10) 0.068(6) Uiso 0.6 1 d . . P D 3
H4A1 H 0.664042 0.027258 0.486483 0.103 Uiso 0.6 1 calc R U P D 3
H4A2 H 0.700504 -0.048285 0.538514 0.103 Uiso 0.6 1 calc R U P D 3
H4A3 H 0.739775 0.016389 0.510779 0.103 Uiso 0.6 1 calc R U P D 3
N5 N 0.7692(18) 0.069(2) 0.5698(15) 0.041(9) Uiso 0.4 1 d . . P E 4
H5A H 0.782371 0.038675 0.606075 0.049 Uiso 0.4 1 calc R U P E 4
H5B H 0.800500 0.061882 0.555989 0.049 Uiso 0.4 1 calc R U P E 4
C3B C 0.7617(12) 0.1520(18) 0.5764(11) 0.085(8) Uiso 0.4 1 d . . P E 4
H3B1 H 0.742558 0.183216 0.537103 0.127 Uiso 0.4 1 calc R U P E 4
H3B2 H 0.803029 0.181694 0.599998 0.127 Uiso 0.4 1 calc R U P E 4
H3B3 H 0.733529 0.159431 0.597669 0.127 Uiso 0.4 1 calc R U P E 4
C4B C 0.7032(11) 0.0149(15) 0.5220(10) 0.068(6) Uiso 0.4 1 d . . P E 4
H4B1 H 0.678098 -0.008056 0.543936 0.103 Uiso 0.4 1 calc R U P E 4
H4B2 H 0.714859 -0.039500 0.502978 0.103 Uiso 0.4 1 calc R U P E 4
H4B3 H 0.677891 0.060787 0.491158 0.103 Uiso 0.4 1 calc R U P E 4


_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
C1 N4 1.47(3) . ?
C1 H1A 0.9800 . ?
C1 H1B 0.9800 . ?
C1 H1C 0.9800 . ?
C2 N4 1.33(3) . ?
C2 H2A 0.9800 . ?
C2 H2B 0.9800 . ?
C2 H2C 0.9800 . ?
C6 N1 1.512(16) . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?
C7 N1 1.490(19) . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
C8 N2 1.466(19) . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 N2 1.476(16) . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C11 N8 1.53(5) . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C12 N8 1.426(19) . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
N1 H1D 0.9100 . ?
N1 H1E 0.9100 . ?
N2 H2D 0.9100 . ?
N2 H2E 0.9100 . ?
N4 H4A 0.9100 . ?
N4 H4B 0.9100 . ?
N8 H8D 0.9100 . ?
N8 H8E 0.9100 . ?
O1 W2B 1.074(16) . ?
O1 W3A 1.895(10) . ?
O1 W1A 1.942(9) . ?
O2 W1A 1.721(11) . ?
O61 W1B 0.945(15) . ?
O61 W2A 1.926(10) . ?
O61 W1A 1.961(10) . ?
O62 W1 1.898(9) . ?
O62 W17 1.902(8) . ?
O63 W13 1.889(10) . ?
O63 W6 1.933(10) . ?
O64 W4 1.692(10) . ?
O65 W3 1.701(8) . ?
O66 W17 1.709(8) . ?
O3 W5 1.691(8) . ?
O5 W2A 1.724(10) . ?
O9 W14 1.911(10) . ?
O9 W2A 1.911(10) . ?
O9 W3B 2.30(2) . ?
O10 W3B 0.77(2) . ?
O10 W3A 1.912(13) . ?
O10 W2A 1.929(10) . ?
O11 W1 1.692(8) . ?
O12 W14 1.711(9) . ?
O13 W8 1.703(9) . ?
O14 W3 1.920(9) . ?
O14 W4 1.930(8) . ?
O15 As1 1.665(8) . ?
O15 W9 2.281(9) . ?
O15 W1 2.352(8) . ?
O16 W14 1.925(9) . ?
O16 W13 1.942(8) . ?
O17 W11 1.898(9) . ?
O17 W1 1.904(9) . ?
O18 W1 1.911(8) . ?
O18 W3 1.934(8) . ?
O19 As1 1.692(8) . ?
O19 W6 2.289(9) . ?
O19 W7 2.294(8) . ?
O20 As2 1.674(9) . ?
O20 W10 2.308(8) . ?
O20 W11 2.320(9) . ?
O21 W11 1.885(9) . ?
O21 W12 1.908(9) . ?
O22 W9 1.879(8) . ?
O22 W6 1.924(8) . ?
O23 W1B 1.903(17) . ?
O23 W1A 1.907(9) . ?
O23 W12 1.916(9) . ?
O24 W10 1.907(9) . ?
O24 W11 1.934(9) . ?
O25 W9 1.707(9) . ?
O26 W9 1.923(8) . ?
O26 W1 1.951(9) . ?
O27 W4 1.887(8) . ?
O27 W9 1.978(8) . ?
O28 W4 1.906(8) . ?
O28 W5 1.947(9) . ?
O29 W3 1.895(8) . ?
O29 W5 1.968(8) . ?
O30 W3 1.885(9) . ?
O30 W17 1.947(9) . ?
O31 As1 1.696(9) . ?
O31 W4 2.328(10) . ?
O31 W5 2.352(8) . ?
O31 W3 2.358(8) . ?
O32 W6 1.907(9) . ?
O32 W4 1.912(8) . ?
O33 As1 1.669(10) . ?
O33 W8 2.321(8) . ?
O33 W17 2.325(8) . ?
O34 W17 1.896(10) . ?
O34 W12 1.913(9) . ?
O35 W5 1.882(8) . ?
O35 W7 1.944(9) . ?
O36 W8 1.906(9) . ?
O36 W17 1.934(9) . ?
O37 W5 1.902(9) . ?
O37 W8 1.922(9) . ?
O38 W7 1.701(8) . ?
O39 W7 1.855(9) . ?
O39 W8 1.936(8) . ?
O40 W15 1.890(9) . ?
O40 W8 1.907(10) . ?
O41 W12 1.918(9) . ?
O41 W15 1.928(9) . ?
O42 W12 1.706(10) . ?
O43 W2A 1.896(9) . ?
O43 W15 1.947(9) . ?
O43 W1B 2.101(17) . ?
O44 As2 1.686(9) . ?
O44 W15 2.284(9) . ?
O44 W12 2.328(9) . ?
O45 W10 1.696(9) . ?
O46 W3A 1.712(9) . ?
O47 W9 1.845(9) . ?
O47 W10 1.971(9) . ?
O48 W13 1.883(8) . ?
O48 W10 1.927(8) . ?
O49 W13 1.728(8) . ?
O50 W6 1.710(9) . ?
O51 W6 1.896(8) . ?
O51 W7 1.969(9) . ?
O52 W15 1.705(9) . ?
O53 W7 1.906(10) . ?
O53 W14 1.912(10) . ?
O54 As2 1.707(10) . ?
O54 W3B 2.19(2) . ?
O54 W1A 2.316(9) . ?
O54 W2A 2.348(9) . ?
O54 W3A 2.353(8) . ?
O54 W1B 2.365(18) . ?
O54 W2B 2.482(16) . ?
O55 W3A 1.894(9) . ?
O55 W13 1.944(10) . ?
O55 W3B 1.99(2) . ?
O56 W10 1.877(9) . ?
O56 W3A 1.937(9) . ?
O56 W2B 2.217(19) . ?
O57 W2B 1.726(17) . ?
O57 W1A 1.892(9) . ?
O57 W11 1.964(9) . ?
O58 W11 1.705(8) . ?
O59 As2 1.685(8) . ?
O59 W13 2.298(8) . ?
O59 W14 2.318(8) . ?
O60 W15 1.893(9) . ?
O60 W14 1.906(9) . ?
W1A W2B 1.780(15) . ?
W1A W1B 1.883(13) . ?
W1B W2A 2.099(14) . ?
W2A W3B 2.065(19) . ?
W2B W3A 2.344(14) . ?
W2B O12W 2.51(3) 2_556 ?
W3A W3B 1.598(18) . ?
C11A N7 1.55(4) . ?
C11A H11D 0.9800 . ?
C11A H11E 0.9800 . ?
C11A H11F 0.9800 . ?
C14 N7 1.41(3) . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
N7 H7D 0.9100 . ?
N7 H7E 0.9100 . ?
N6 C10 1.45(5) . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
N3 C3A 1.38(3) . ?
N3 C4A 1.54(3) . ?
N3 H3A 0.9100 . ?
N3 H3B 0.9100 . ?
C3A H3A1 0.9800 . ?
C3A H3A2 0.9800 . ?
C3A H3A3 0.9800 . ?
C4A H4A1 0.9800 . ?
C4A H4A2 0.9800 . ?
C4A H4A3 0.9800 . ?
N5 C3B 1.20(4) . ?
N5 C4B 1.67(4) . ?
N5 H5A 0.9100 . ?
N5 H5B 0.9100 . ?
C3B H3B1 0.9800 . ?
C3B H3B2 0.9800 . ?
C3B H3B3 0.9800 . ?
C4B H4B1 0.9800 . ?
C4B H4B2 0.9800 . ?
C4B H4B3 0.9800 . ?

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
N4 C1 H1A 109.5 . . ?
N4 C1 H1B 109.5 . . ?
H1A C1 H1B 109.5 . . ?
N4 C1 H1C 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
N4 C2 H2A 109.5 . . ?
N4 C2 H2B 109.5 . . ?
H2A C2 H2B 109.5 . . ?
N4 C2 H2C 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
N1 C6 H6A 109.5 . . ?
N1 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
N1 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
N1 C7 H7A 109.5 . . ?
N1 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
N1 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
N2 C8 H8A 109.5 . . ?
N2 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
N2 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
N2 C9 H9A 109.5 . . ?
N2 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
N2 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
N8 C11 H11A 109.5 . . ?
N8 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
N8 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
N8 C12 H12A 109.5 . . ?
N8 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
N8 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C7 N1 C6 112.1(12) . . ?
C7 N1 H1D 109.2 . . ?
C6 N1 H1D 109.2 . . ?
C7 N1 H1E 109.2 . . ?
C6 N1 H1E 109.2 . . ?
H1D N1 H1E 107.9 . . ?
C8 N2 C9 111.7(11) . . ?
C8 N2 H2D 109.3 . . ?
C9 N2 H2D 109.3 . . ?
C8 N2 H2E 109.3 . . ?
C9 N2 H2E 109.3 . . ?
H2D N2 H2E 107.9 . . ?
C2 N4 C1 110(2) . . ?
C2 N4 H4A 109.6 . . ?
C1 N4 H4A 109.6 . . ?
C2 N4 H4B 109.6 . . ?
C1 N4 H4B 109.6 . . ?
H4A N4 H4B 108.1 . . ?
C12 N8 C11 128(3) . . ?
C12 N8 H8D 105.3 . . ?
C11 N8 H8D 105.3 . . ?
C12 N8 H8E 105.3 . . ?
C11 N8 H8E 105.3 . . ?
H8D N8 H8E 106.0 . . ?
W2B O1 W3A 100.6(11) . . ?
W2B O1 W1A 65.1(9) . . ?
W3A O1 W1A 122.8(5) . . ?
W1B O61 W2A 86.9(11) . . ?
W1B O61 W1A 71.2(10) . . ?
W2A O61 W1A 121.2(6) . . ?
W1 O62 W17 152.5(6) . . ?
W13 O63 W6 160.7(5) . . ?
W14 O9 W2A 152.2(5) . . ?
W14 O9 W3B 134.4(7) . . ?
W2A O9 W3B 57.8(6) . . ?
W3B O10 W3A 54.9(17) . . ?
W3B O10 W2A 89.0(18) . . ?
W3A O10 W2A 122.2(6) . . ?
W3 O14 W4 122.1(5) . . ?
As1 O15 W9 125.4(5) . . ?
As1 O15 W1 124.0(4) . . ?
W9 O15 W1 94.0(3) . . ?
W14 O16 W13 122.4(4) . . ?
W11 O17 W1 161.6(5) . . ?
W1 O18 W3 152.3(5) . . ?
As1 O19 W6 124.9(5) . . ?
As1 O19 W7 125.2(4) . . ?
W6 O19 W7 94.9(3) . . ?
As2 O20 W10 124.2(4) . . ?
As2 O20 W11 124.2(5) . . ?
W10 O20 W11 93.6(3) . . ?
W11 O21 W12 154.2(5) . . ?
W9 O22 W6 153.6(5) . . ?
W1B O23 W1A 59.3(5) . . ?
W1B O23 W12 135.4(6) . . ?
W1A O23 W12 151.4(6) . . ?
W10 O24 W11 122.8(4) . . ?
W9 O26 W1 122.0(4) . . ?
W4 O27 W9 151.1(5) . . ?
W4 O28 W5 122.8(5) . . ?
W3 O29 W5 121.6(4) . . ?
W3 O30 W17 154.1(4) . . ?
As1 O31 W4 124.5(4) . . ?
As1 O31 W5 123.4(5) . . ?
W4 O31 W5 92.6(3) . . ?
As1 O31 W3 123.7(4) . . ?
W4 O31 W3 91.9(3) . . ?
W5 O31 W3 91.5(3) . . ?
W6 O32 W4 152.3(5) . . ?
As1 O33 W8 124.5(4) . . ?
As1 O33 W17 124.5(5) . . ?
W8 O33 W17 93.9(3) . . ?
W17 O34 W12 161.9(5) . . ?
W5 O35 W7 151.7(6) . . ?
W8 O36 W17 124.3(5) . . ?
W5 O37 W8 152.3(4) . . ?
W7 O39 W8 154.9(6) . . ?
W15 O40 W8 162.8(5) . . ?
W12 O41 W15 123.6(5) . . ?
W2A O43 W15 151.6(6) . . ?
W2A O43 W1B 63.1(5) . . ?
W15 O43 W1B 131.9(6) . . ?
As2 O44 W15 125.5(4) . . ?
As2 O44 W12 122.8(4) . . ?
W15 O44 W12 94.6(4) . . ?
W9 O47 W10 160.8(4) . . ?
W13 O48 W10 151.2(6) . . ?
W6 O51 W7 121.8(4) . . ?
W7 O53 W14 160.5(6) . . ?
As2 O54 W3B 128.2(7) . . ?
As2 O54 W1A 123.1(4) . . ?
W3B O54 W1A 108.2(7) . . ?
As2 O54 W2A 123.9(4) . . ?
W3B O54 W2A 54.0(5) . . ?
W1A O54 W2A 93.1(4) . . ?
As2 O54 W3A 124.0(5) . . ?
W3B O54 W3A 41.0(5) . . ?
W1A O54 W3A 92.3(3) . . ?
W2A O54 W3A 91.4(3) . . ?
As2 O54 W1B 121.9(6) . . ?
W3B O54 W1B 96.9(7) . . ?
W1A O54 W1B 47.4(4) . . ?
W2A O54 W1B 52.9(4) . . ?
W3A O54 W1B 114.0(5) . . ?
As2 O54 W2B 119.0(6) . . ?
W3B O54 W2B 92.6(7) . . ?
W1A O54 W2B 43.4(4) . . ?
W2A O54 W2B 116.7(6) . . ?
W3A O54 W2B 57.9(4) . . ?
W1B O54 W2B 88.4(6) . . ?
W3A O55 W13 152.9(5) . . ?
W3A O55 W3B 48.6(6) . . ?
W13 O55 W3B 142.9(7) . . ?
W10 O56 W3A 154.2(5) . . ?
W10 O56 W2B 125.5(6) . . ?
W3A O56 W2B 68.3(5) . . ?
W2B O57 W1A 58.7(6) . . ?
W2B O57 W11 139.2(8) . . ?
W1A O57 W11 150.5(5) . . ?
As2 O59 W13 124.4(4) . . ?
As2 O59 W14 124.2(5) . . ?
W13 O59 W14 94.4(3) . . ?
W15 O60 W14 153.2(5) . . ?
O15 As1 O33 111.7(4) . . ?
O15 As1 O19 112.1(4) . . ?
O33 As1 O19 112.1(4) . . ?
O15 As1 O31 107.3(4) . . ?
O33 As1 O31 107.9(4) . . ?
O19 As1 O31 105.4(4) . . ?
O20 As2 O59 111.1(5) . . ?
O20 As2 O44 112.8(4) . . ?
O59 As2 O44 110.8(4) . . ?
O20 As2 O54 107.9(4) . . ?
O59 As2 O54 107.0(4) . . ?
O44 As2 O54 107.1(5) . . ?
O11 W1 O62 104.3(4) . . ?
O11 W1 O17 97.5(4) . . ?
O62 W1 O17 86.6(4) . . ?
O11 W1 O18 98.7(4) . . ?
O62 W1 O18 86.6(4) . . ?
O17 W1 O18 163.6(3) . . ?
O11 W1 O26 100.7(4) . . ?
O62 W1 O26 155.1(3) . . ?
O17 W1 O26 90.2(4) . . ?
O18 W1 O26 89.7(4) . . ?
O11 W1 O15 171.4(4) . . ?
O62 W1 O15 84.1(3) . . ?
O17 W1 O15 81.0(3) . . ?
O18 W1 O15 83.5(3) . . ?
O26 W1 O15 71.0(3) . . ?
O2 W1A W2B 104.9(6) . . ?
O2 W1A W1B 108.5(6) . . ?
W2B W1A W1B 134.5(6) . . ?
O2 W1A O57 103.8(4) . . ?
W2B W1A O57 56.0(6) . . ?
W1B W1A O57 138.3(6) . . ?
O2 W1A O23 103.6(4) . . ?
W2B W1A O23 137.7(6) . . ?
W1B W1A O23 60.3(5) . . ?
O57 W1A O23 87.3(4) . . ?
O2 W1A O1 99.4(4) . . ?
W2B W1A O1 33.2(5) . . ?
W1B W1A O1 110.3(5) . . ?
O57 W1A O1 89.1(4) . . ?
O23 W1A O1 156.9(4) . . ?
O2 W1A O61 98.3(5) . . ?
W2B W1A O61 117.5(5) . . ?
W1B W1A O61 28.4(5) . . ?
O57 W1A O61 157.8(4) . . ?
O23 W1A O61 88.1(4) . . ?
O1 W1A O61 86.7(4) . . ?
O2 W1A O54 168.1(4) . . ?
W2B W1A O54 73.3(5) . . ?
W1B W1A O54 67.6(5) . . ?
O57 W1A O54 85.0(4) . . ?
O23 W1A O54 84.4(4) . . ?
O1 W1A O54 72.5(3) . . ?
O61 W1A O54 73.0(4) . . ?
O61 W1B W1A 80.4(10) . . ?
O61 W1B O23 139.2(13) . . ?
W1A W1B O23 60.5(5) . . ?
O61 W1B W2A 66.4(10) . . ?
W1A W1B W2A 116.3(7) . . ?
O23 W1B W2A 140.0(9) . . ?
O61 W1B O43 117.2(12) . . ?
W1A W1B O43 140.2(9) . . ?
O23 W1B O43 101.1(8) . . ?
W2A W1B O43 53.7(4) . . ?
O61 W1B O54 90.8(12) . . ?
W1A W1B O54 64.9(5) . . ?
O23 W1B O54 83.2(7) . . ?
W2A W1B O54 63.1(5) . . ?
O43 W1B O54 78.7(6) . . ?
O65 W3 O30 101.2(4) . . ?
O65 W3 O29 102.2(4) . . ?
O30 W3 O29 89.7(4) . . ?
O65 W3 O14 102.5(4) . . ?
O30 W3 O14 155.8(3) . . ?
O29 W3 O14 89.8(4) . . ?
O65 W3 O18 100.8(4) . . ?
O30 W3 O18 84.5(4) . . ?
O29 W3 O18 157.0(3) . . ?
O14 W3 O18 86.5(4) . . ?
O65 W3 O31 173.7(4) . . ?
O30 W3 O31 84.0(3) . . ?
O29 W3 O31 74.0(3) . . ?
O14 W3 O31 72.7(3) . . ?
O18 W3 O31 83.2(3) . . ?
O5 W2A O43 101.8(4) . . ?
O5 W2A O9 102.6(4) . . ?
O43 W2A O9 86.8(4) . . ?
O5 W2A O61 101.6(5) . . ?
O43 W2A O61 88.6(4) . . ?
O9 W2A O61 155.9(4) . . ?
O5 W2A O10 101.9(5) . . ?
O43 W2A O10 156.3(5) . . ?
O9 W2A O10 88.2(5) . . ?
O61 W2A O10 86.6(5) . . ?
O5 W2A W3B 117.8(6) . . ?
O43 W2A W3B 137.5(6) . . ?
O9 W2A W3B 70.6(6) . . ?
O61 W2A W3B 97.7(6) . . ?
O10 W2A W3B 22.0(5) . . ?
O5 W2A W1B 113.2(5) . . ?
O43 W2A W1B 63.2(5) . . ?
O9 W2A W1B 136.7(5) . . ?
O61 W2A W1B 26.7(4) . . ?
O10 W2A W1B 106.7(5) . . ?
W3B W2A W1B 110.1(6) . . ?
O5 W2A O54 172.5(4) . . ?
O43 W2A O54 83.3(3) . . ?
O9 W2A O54 83.1(4) . . ?
O61 W2A O54 72.8(4) . . ?
O10 W2A O54 73.1(4) . . ?
W3B W2A O54 59.2(6) . . ?
W1B W2A O54 64.0(5) . . ?
O1 W2B O57 147.0(14) . . ?
O1 W2B W1A 81.7(11) . . ?
O57 W2B W1A 65.3(6) . . ?
O1 W2B O56 100.9(11) . . ?
O57 W2B O56 102.3(9) . . ?
W1A W2B O56 136.4(8) . . ?
O1 W2B W3A 52.6(9) . . ?
O57 W2B W3A 136.2(9) . . ?
W1A W2B W3A 108.8(6) . . ?
O56 W2B W3A 50.2(4) . . ?
O1 W2B O54 80.4(9) . . ?
O57 W2B O54 83.6(6) . . ?
W1A W2B O54 63.3(5) . . ?
O56 W2B O54 74.1(5) . . ?
W3A W2B O54 58.3(4) . . ?
O1 W2B O12W 116.2(12) . 2_556 ?
O57 W2B O12W 84.8(8) . 2_556 ?
W1A W2B O12W 123.0(9) . 2_556 ?
O56 W2B O12W 95.2(9) . 2_556 ?
W3A W2B O12W 125.4(8) . 2_556 ?
O54 W2B O12W 162.1(10) . 2_556 ?
O64 W4 O27 102.7(4) . . ?
O64 W4 O28 100.3(4) . . ?
O27 W4 O28 156.9(4) . . ?
O64 W4 O32 102.3(4) . . ?
O27 W4 O32 86.4(3) . . ?
O28 W4 O32 89.8(3) . . ?
O64 W4 O14 101.1(4) . . ?
O27 W4 O14 88.4(3) . . ?
O28 W4 O14 86.1(3) . . ?
O32 W4 O14 156.6(4) . . ?
O64 W4 O31 171.2(3) . . ?
O27 W4 O31 84.0(3) . . ?
O28 W4 O31 72.9(4) . . ?
O32 W4 O31 83.5(4) . . ?
O14 W4 O31 73.2(3) . . ?
W3B W3A O46 113.6(7) . . ?
W3B W3A O55 68.7(8) . . ?
O46 W3A O55 101.9(4) . . ?
W3B W3A O1 104.1(8) . . ?
O46 W3A O1 102.5(4) . . ?
O55 W3A O1 155.3(4) . . ?
W3B W3A O10 23.3(7) . . ?
O46 W3A O10 102.2(5) . . ?
O55 W3A O10 90.5(5) . . ?
O1 W3A O10 87.6(5) . . ?
W3B W3A O56 138.4(8) . . ?
O46 W3A O56 102.3(4) . . ?
O55 W3A O56 84.4(4) . . ?
O1 W3A O56 87.1(4) . . ?
O10 W3A O56 155.5(4) . . ?
W3B W3A W2B 117.1(8) . . ?
O46 W3A W2B 113.7(5) . . ?
O55 W3A W2B 134.4(5) . . ?
O1 W3A W2B 26.8(5) . . ?
O10 W3A W2B 107.8(5) . . ?
O56 W3A W2B 61.5(5) . . ?
W3B W3A O54 64.2(7) . . ?
O46 W3A O54 173.1(4) . . ?
O55 W3A O54 83.5(3) . . ?
O1 W3A O54 72.4(4) . . ?
O10 W3A O54 73.3(4) . . ?
O56 W3A O54 82.3(3) . . ?
W2B W3A O54 63.8(4) . . ?
O10 W3B W3A 102(2) . . ?
O10 W3B O55 155(2) . . ?
W3A W3B O55 62.7(7) . . ?
O10 W3B W2A 69.0(17) . . ?
W3A W3B W2A 132.9(11) . . ?
O55 W3B W2A 136.3(11) . . ?
O10 W3B O54 111(2) . . ?
W3A W3B O54 74.8(7) . . ?
O55 W3B O54 85.8(8) . . ?
W2A W3B O54 66.8(6) . . ?
O10 W3B O9 110(2) . . ?
W3A W3B O9 143.6(12) . . ?
O55 W3B O9 91.3(9) . . ?
W2A W3B O9 51.6(5) . . ?
O54 W3B O9 78.4(7) . . ?
O3 W5 O35 104.4(4) . . ?
O3 W5 O37 104.2(4) . . ?
O35 W5 O37 86.7(4) . . ?
O3 W5 O28 100.3(4) . . ?
O35 W5 O28 91.2(4) . . ?
O37 W5 O28 155.1(3) . . ?
O3 W5 O29 99.0(4) . . ?
O35 W5 O29 156.6(3) . . ?
O37 W5 O29 86.8(4) . . ?
O28 W5 O29 85.3(4) . . ?
O3 W5 O31 168.7(4) . . ?
O35 W5 O31 84.0(3) . . ?
O37 W5 O31 83.5(3) . . ?
O28 W5 O31 71.6(3) . . ?
O29 W5 O31 72.9(3) . . ?
O50 W6 O51 101.6(4) . . ?
O50 W6 O32 98.2(4) . . ?
O51 W6 O32 92.2(4) . . ?
O50 W6 O22 101.1(4) . . ?
O51 W6 O22 157.2(4) . . ?
O32 W6 O22 85.5(4) . . ?
O50 W6 O63 96.3(4) . . ?
O51 W6 O63 90.0(4) . . ?
O32 W6 O63 164.6(4) . . ?
O22 W6 O63 86.6(4) . . ?
O50 W6 O19 173.7(3) . . ?
O51 W6 O19 72.3(3) . . ?
O32 W6 O19 83.8(4) . . ?
O22 W6 O19 84.9(3) . . ?
O63 W6 O19 82.4(4) . . ?
O38 W7 O39 103.7(4) . . ?
O38 W7 O53 97.6(4) . . ?
O39 W7 O53 91.1(4) . . ?
O38 W7 O35 98.1(4) . . ?
O39 W7 O35 85.2(4) . . ?
O53 W7 O35 164.3(3) . . ?
O38 W7 O51 99.8(4) . . ?
O39 W7 O51 156.4(4) . . ?
O53 W7 O51 88.3(4) . . ?
O35 W7 O51 89.1(4) . . ?
O38 W7 O19 170.8(4) . . ?
O39 W7 O19 85.6(3) . . ?
O53 W7 O19 82.1(3) . . ?
O35 W7 O19 82.4(3) . . ?
O51 W7 O19 71.0(3) . . ?
O13 W8 O36 99.9(4) . . ?
O13 W8 O40 97.2(4) . . ?
O36 W8 O40 91.6(4) . . ?
O13 W8 O37 98.4(4) . . ?
O36 W8 O37 89.9(4) . . ?
O40 W8 O37 163.9(3) . . ?
O13 W8 O39 104.6(4) . . ?
O36 W8 O39 155.4(4) . . ?
O40 W8 O39 87.5(4) . . ?
O37 W8 O39 84.5(4) . . ?
O13 W8 O33 170.9(4) . . ?
O36 W8 O33 71.2(3) . . ?
O40 W8 O33 81.9(4) . . ?
O37 W8 O33 83.4(3) . . ?
O39 W8 O33 84.4(3) . . ?
O25 W9 O47 99.1(4) . . ?
O25 W9 O22 103.9(4) . . ?
O47 W9 O22 92.0(4) . . ?
O25 W9 O26 96.8(4) . . ?
O47 W9 O26 91.5(4) . . ?
O22 W9 O26 158.2(4) . . ?
O25 W9 O27 93.9(4) . . ?
O47 W9 O27 167.1(3) . . ?
O22 W9 O27 85.1(3) . . ?
O26 W9 O27 86.8(3) . . ?
O25 W9 O15 169.5(4) . . ?
O47 W9 O15 84.2(3) . . ?
O22 W9 O15 85.9(3) . . ?
O26 W9 O15 73.1(3) . . ?
O27 W9 O15 83.0(3) . . ?
O45 W10 O56 99.7(4) . . ?
O45 W10 O24 100.3(4) . . ?
O56 W10 O24 93.0(4) . . ?
O45 W10 O48 103.1(4) . . ?
O56 W10 O48 86.2(4) . . ?
O24 W10 O48 156.4(4) . . ?
O45 W10 O47 96.0(4) . . ?
O56 W10 O47 163.5(3) . . ?
O24 W10 O47 89.4(4) . . ?
O48 W10 O47 85.2(4) . . ?
O45 W10 O20 171.7(4) . . ?
O56 W10 O20 84.4(3) . . ?
O24 W10 O20 72.1(3) . . ?
O48 W10 O20 84.4(3) . . ?
O47 W10 O20 80.7(3) . . ?
O58 W11 O21 104.6(4) . . ?
O58 W11 O17 98.1(4) . . ?
O21 W11 O17 90.3(4) . . ?
O58 W11 O24 99.1(4) . . ?
O21 W11 O24 156.0(4) . . ?
O17 W11 O24 90.2(4) . . ?
O58 W11 O57 97.5(4) . . ?
O21 W11 O57 85.7(4) . . ?
O17 W11 O57 164.4(3) . . ?
O24 W11 O57 87.4(4) . . ?
O58 W11 O20 170.5(4) . . ?
O21 W11 O20 84.9(3) . . ?
O17 W11 O20 82.1(3) . . ?
O24 W11 O20 71.4(3) . . ?
O57 W11 O20 82.6(4) . . ?
O42 W12 O21 104.9(4) . . ?
O42 W12 O34 97.0(4) . . ?
O21 W12 O34 87.2(4) . . ?
O42 W12 O23 98.5(4) . . ?
O21 W12 O23 85.9(4) . . ?
O34 W12 O23 164.2(4) . . ?
O42 W12 O41 99.8(4) . . ?
O21 W12 O41 155.3(4) . . ?
O34 W12 O41 89.8(4) . . ?
O23 W12 O41 90.6(4) . . ?
O42 W12 O44 170.0(4) . . ?
O21 W12 O44 84.9(3) . . ?
O34 W12 O44 81.1(3) . . ?
O23 W12 O44 84.1(4) . . ?
O41 W12 O44 70.4(4) . . ?
O49 W13 O48 102.6(4) . . ?
O49 W13 O63 97.9(4) . . ?
O48 W13 O63 90.7(4) . . ?
O49 W13 O16 99.7(4) . . ?
O48 W13 O16 157.4(4) . . ?
O63 W13 O16 89.2(4) . . ?
O49 W13 O55 96.8(4) . . ?
O48 W13 O55 86.4(4) . . ?
O63 W13 O55 165.3(4) . . ?
O16 W13 O55 88.1(4) . . ?
O49 W13 O59 171.4(4) . . ?
O48 W13 O59 85.9(3) . . ?
O63 W13 O59 82.5(4) . . ?
O16 W13 O59 71.7(3) . . ?
O55 W13 O59 83.0(3) . . ?
O12 W14 O60 103.4(4) . . ?
O12 W14 O9 97.7(4) . . ?
O60 W14 O9 86.1(4) . . ?
O12 W14 O53 97.8(4) . . ?
O60 W14 O53 87.9(4) . . ?
O9 W14 O53 164.4(4) . . ?
O12 W14 O16 100.2(4) . . ?
O60 W14 O16 156.4(4) . . ?
O9 W14 O16 89.9(4) . . ?
O53 W14 O16 89.8(4) . . ?
O12 W14 O59 171.7(4) . . ?
O60 W14 O59 84.9(3) . . ?
O9 W14 O59 83.5(4) . . ?
O53 W14 O59 81.6(3) . . ?
O16 W14 O59 71.5(3) . . ?
O52 W15 O40 97.8(4) . . ?
O52 W15 O60 102.9(4) . . ?
O40 W15 O60 89.4(4) . . ?
O52 W15 O41 100.5(4) . . ?
O40 W15 O41 90.4(4) . . ?
O60 W15 O41 156.5(4) . . ?
O52 W15 O43 97.0(4) . . ?
O40 W15 O43 165.1(4) . . ?
O60 W15 O43 85.8(4) . . ?
O41 W15 O43 88.4(4) . . ?
O52 W15 O44 171.7(4) . . ?
O40 W15 O44 82.5(3) . . ?
O60 W15 O44 85.4(4) . . ?
O41 W15 O44 71.3(4) . . ?
O43 W15 O44 83.1(3) . . ?
O66 W17 O34 99.1(4) . . ?
O66 W17 O62 103.5(4) . . ?
O34 W17 O62 89.3(4) . . ?
O66 W17 O36 100.8(4) . . ?
O34 W17 O36 90.0(4) . . ?
O62 W17 O36 155.5(4) . . ?
O66 W17 O30 97.1(4) . . ?
O34 W17 O30 163.7(3) . . ?
O62 W17 O30 85.3(4) . . ?
O36 W17 O30 88.6(4) . . ?
O66 W17 O33 171.4(4) . . ?
O34 W17 O33 81.6(4) . . ?
O62 W17 O33 85.1(3) . . ?
O36 W17 O33 70.6(3) . . ?
O30 W17 O33 82.6(3) . . ?
N7 C11A H11D 109.5 . . ?
N7 C11A H11E 109.5 . . ?
H11D C11A H11E 109.5 . . ?
N7 C11A H11F 109.5 . . ?
H11D C11A H11F 109.5 . . ?
H11E C11A H11F 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 . . ?
C14 N7 C11A 109(2) . . ?
C14 N7 H7D 110.0 . . ?
C11A N7 H7D 110.0 . . ?
C14 N7 H7E 110.0 . . ?
C11A N7 H7E 110.0 . . ?
H7D N7 H7E 108.4 . . ?
N6 C10 H10A 109.5 . . ?
N6 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
N6 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C3A N3 C4A 111(2) . . ?
C3A N3 H3A 109.4 . . ?
C4A N3 H3A 109.4 . . ?
C3A N3 H3B 109.4 . . ?
C4A N3 H3B 109.4 . . ?
H3A N3 H3B 108.0 . . ?
N3 C3A H3A1 109.5 . . ?
N3 C3A H3A2 109.5 . . ?
H3A1 C3A H3A2 109.5 . . ?
N3 C3A H3A3 109.5 . . ?
H3A1 C3A H3A3 109.5 . . ?
H3A2 C3A H3A3 109.5 . . ?
N3 C4A H4A1 109.5 . . ?
N3 C4A H4A2 109.5 . . ?
H4A1 C4A H4A2 109.5 . . ?
N3 C4A H4A3 109.5 . . ?
H4A1 C4A H4A3 109.5 . . ?
H4A2 C4A H4A3 109.5 . . ?
C3B N5 C4B 113(3) . . ?
C3B N5 H5A 109.0 . . ?
C4B N5 H5A 109.0 . . ?
C3B N5 H5B 109.0 . . ?
C4B N5 H5B 109.0 . . ?
H5A N5 H5B 107.8 . . ?
N5 C3B H3B1 109.5 . . ?
N5 C3B H3B2 109.5 . . ?
H3B1 C3B H3B2 109.5 . . ?
N5 C3B H3B3 109.5 . . ?
H3B1 C3B H3B3 109.5 . . ?
H3B2 C3B H3B3 109.5 . . ?
N5 C4B H4B1 109.5 . . ?
N5 C4B H4B2 109.5 . . ?
H4B1 C4B H4B2 109.5 . . ?
N5 C4B H4B3 109.5 . . ?
H4B1 C4B H4B3 109.5 . . ?
H4B2 C4B H4B3 109.5 . . ?

_refine_diff_density_max         3.792
_refine_diff_density_min         -3.275
_refine_diff_density_rms         0.444

_diffrn_radiation_probe          x-ray
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            AtlasS2

####################################################################### 
# 
# 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_CsNaK
_database_code_depnum_ccdc_archive 'CCDC 1946816'
loop_
_audit_author_name
_audit_author_address
'Pavel Abramov'
;Nikolaev Institute of Inorganic Chemistry SB RAS
Russia
;
_audit_update_record             
;
2019-09-05 deposited with the CCDC.	2019-09-26 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT971_CsNaK               
;
PROBLEM: Check Calcd Resid. Dens.  0.88A   From O3              4.46 eA-3
RESPONSE: Residual electronic density without any chemical sense
;
_vrf_PLAT973_CsNaK               
;
PROBLEM: Check Calcd Positive Resid. Density on        W5       2.90 eA-3
RESPONSE: Residual electronic density without any chemical sense
;
_vrf_PLAT975_CsNaK               
;
PROBLEM: Check Calcd Resid. Dens.  0.88A   From O3              4.46 eA-3
RESPONSE: Residual electronic density without any chemical sense
;
_vrf_PLAT971_CsNaK_2             
;
PROBLEM: Check Calcd Resid. Dens.  0.75A   From Cs5             3.47 eA-3
RESPONSE: Residual electronic density without any chemical sense
;
_vrf_PLAT972_CsNaK               
;
PROBLEM: Check Calcd Resid. Dens.  0.89A   From W2             -2.86 eA-3
RESPONSE: Residual electronic density without any chemical sense
;
_vrf_PLAT975_CsNaK_2             
;
PROBLEM: Check Calcd Resid. Dens.  0.72A   From O2W             1.93 eA-3
RESPONSE: Residual electronic density without any chemical sense
;
# Added during the CSD deposition process: Wednesday 04 September 2019 01:05 PM
# end Validation Reply Form

#complex Cs6KNa3[SbW17{Ru(NO)}O59]*12H2O (analytical data)
_audit_creation_method           SHELXL-2017/1
_shelx_SHELXL_version_number     2017/1
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'Cs5.37 O65.60 Ru Sb W17'
_chemical_formula_weight         5111.88

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ru Ru -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Sb Sb -0.5866 1.5461 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cs Cs -0.3680 2.1192 '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      orthorhombic
_space_group_IT_number           58
_space_group_name_H-M_alt        'P n n m'
_space_group_name_Hall           '-P 2 2n'

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

_cell_length_a                   12.5497(4)
_cell_length_b                   18.5385(7)
_cell_length_c                   15.6808(5)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     3648.2(2)
_cell_formula_units_Z            2
_cell_measurement_temperature    130(2)
_cell_measurement_reflns_used    5206
_cell_measurement_theta_min      2.3430
_cell_measurement_theta_max      28.6850

_exptl_crystal_description       block
_exptl_crystal_colour            red
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    4.654
_exptl_crystal_F_000             4347
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.333
_exptl_crystal_size_mid          0.131
_exptl_crystal_size_min          0.096
_exptl_absorpt_coefficient_mu    29.978
_shelx_estimated_absorpt_T_min   0.036
_shelx_estimated_absorpt_T_max   0.161
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_correction_T_min  0.955
_exptl_absorpt_correction_T_max  0.986

loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-3 -16 17 0.0597
2 12 -19 0.0222
-2 -18 -16 0.0078
0 16 18 0.0723
17 -5 -6 0.1428
-15 -9 -10 0.0754

_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      130(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'sealed X-ray tube'
_diffrn_measurement_device_type  'New Xcalibur, AtlasS2'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 10.6168
_diffrn_reflns_number            13707
_diffrn_reflns_av_unetI/netI     0.0468
_diffrn_reflns_av_R_equivalents  0.0468
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         1.960
_diffrn_reflns_theta_max         25.677
_diffrn_reflns_theta_full        25.500
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measured_fraction_theta_full 0.986
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_Laue_measured_fraction_full 0.986
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_point_group_measured_fraction_full 0.986
_reflns_number_total             3553
_reflns_number_gt                2920
_reflns_threshold_expression     >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       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_structure_solution    'SHELXS-2014 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_molecular_graphics    'ShelXle (Hübschle, 2011)'
_computing_publication_material  'CIFTAB-2014 (Sheldrick, 2014)'
_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)+(0.0990P)²+106.1746P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   .
_refine_ls_hydrogen_treatment    undef
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         3553
_refine_ls_number_parameters     233
_refine_ls_number_restraints     6
_refine_ls_R_factor_all          0.0688
_refine_ls_R_factor_gt           0.0549
_refine_ls_wR_factor_ref         0.1641
_refine_ls_wR_factor_gt          0.1550
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_restrained_S_all      1.064
_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
O1 O 0.1738(11) 0.2453(8) 0.6534(9) 0.037(3) Uani 1 1 d . . . . .
O19 O 0.5924(19) 0.3762(15) 1.000000 0.050(6) Uiso 1 2 d S . P . .
O2 O 0.2183(14) 0.3158(11) 0.500000 0.027(4) Uani 1 2 d S T P . .
O3 O 0.1630(10) 0.3921(8) 0.6350(9) 0.032(3) Uani 1 1 d . . . . .
O4 O 0.3333(11) 0.3346(8) 0.7202(9) 0.036(3) Uani 1 1 d . U . . .
O5 O 0.4532(13) 0.4165(9) 0.8323(9) 0.043(4) Uani 1 1 d . . . . .
O6 O 0.2966(11) 0.4767(8) 0.7265(9) 0.033(3) Uani 1 1 d . . . . .
O7 O 0.500000 0.500000 0.6885(12) 0.031(4) Uani 1 2 d S T P . .
O8 O 0.5370(10) 0.3584(7) 0.6822(8) 0.026(3) Uani 1 1 d . . . . .
O9 O 0.3780(10) 0.2578(7) 0.4169(8) 0.027(3) Uani 1 1 d . . . . .
O10 O 0.4680(18) 0.1376(12) 0.500000 0.044(5) Uani 1 2 d S T P . .
O11 O 0.5887(11) 0.2420(9) 0.5875(10) 0.038(4) Uani 1 1 d . . . . .
O12 O 0.7516(11) 0.3103(10) 0.6752(10) 0.044(4) Uani 1 1 d . . . . .
O13 O 0.7277(14) 0.3230(12) 0.500000 0.035(5) Uani 1 2 d S T P . .
O14 O 0.6800(10) 0.4376(7) 0.5929(8) 0.025(3) Uani 1 1 d . . . . .
O15 O 0.8850(10) 0.4605(8) 0.6553(10) 0.038(4) Uani 1 1 d . . . . .
O16 O 0.8115(13) 0.5186(10) 0.500000 0.024(4) Uani 1 2 d S T P . .
O17 O 0.6432(9) 0.5863(8) 0.5900(8) 0.026(3) Uani 1 1 d . . . . .
O18 O 0.4690(13) 0.6475(10) 0.500000 0.024(4) Uani 1 2 d S T P . .
O1W O 0.535(2) 0.3338(16) 1.000000 0.058(7) Uiso 1 2 d S . P . .
O2W O 0.291(3) 0.354(2) 1.000000 0.076(11) Uiso 0.8 2 d S . P . .
Sb1 Sb 0.5417(2) 0.55184(18) 0.500000 0.0138(6) Uiso 0.5 2 d S . P . .
Cs1 Cs 0.47310(15) 0.18171(16) 0.75620(17) 0.0746(9) Uani 0.8 1 d . . P . .
Cs2 Cs 0.9733(4) 0.3710(4) 0.500000 0.0715(16) Uani 0.5 2 d S T P . .
Cs3 Cs 0.500000 0.500000 1.000000 0.035(5) Uiso 0.12 4 d S . P . .
Cs4 Cs 0.5584(14) 0.4925(11) 1.000000 0.034(4) Uiso 0.1 2 d S . P . .
Cs5 Cs 0.5216(19) 0.0971(14) 0.6993(16) 0.054(6) Uiso 0.07 1 d . . P . .
Cs6 Cs 0.2418(16) 0.5951(7) 0.8497(9) 0.070(5) Uani 0.12 1 d . . P . .
Cs7 Cs 0.373(3) -0.003(3) 0.500000 0.032(9) Uiso 0.04 2 d S . P . .
W1 W 0.25567(6) 0.31148(5) 0.61803(5) 0.0240(2) Uani 1 1 d . . . . .
W2 W 0.48067(9) 0.23114(6) 0.500000 0.0280(3) Uani 1 2 d S T P . .
W3 W 0.65128(6) 0.33577(5) 0.60541(5) 0.0299(3) Uani 1 1 d . . . . .
W4 W 0.42410(7) 0.41648(5) 0.72469(5) 0.0276(3) Uani 0.87 1 d . . P . .
Ru4 Ru 0.42410(7) 0.41648(5) 0.72469(5) 0.0276(3) Uani 0.13 1 d . . P . .
W5 W 0.77912(6) 0.51170(5) 0.61954(5) 0.0255(2) Uani 0.88 1 d . . P . .
Ru5 Ru 0.77912(6) 0.51170(5) 0.61954(5) 0.0255(2) Uani 0.12 1 d . . 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
O1 W1 1.693(14) . ?
O1 Cs6 2.98(2) 3_546 ?
O1 Cs1 3.191(16) 4_456 ?
O19 O1W 1.07(3) . ?
O19 Cs4 2.20(3) . ?
O19 Cs3 2.57(3) . ?
O19 Cs4 3.08(3) 5_667 ?
O19 Cs6 3.19(2) 5_667 ?
O19 Cs6 3.19(2) 2_665 ?
O2 W1 1.911(5) 6_556 ?
O2 W1 1.911(5) . ?
O2 Cs2 3.240(19) 1_455 ?
O3 W1 1.912(14) . ?
O3 W5 1.942(14) 2_665 ?
O3 Cs5 3.15(3) 4_456 ?
O3 Cs2 3.209(14) 1_455 ?
O3 Cs1 3.234(13) 4_456 ?
O4 W4 1.899(15) . ?
O4 W1 1.924(14) . ?
O4 Cs1 3.381(15) . ?
O5 W4 1.726(14) . ?
O5 Cs3 3.107(15) . ?
O5 Cs4 3.127(19) 5_667 ?
O5 Cs4 3.262(19) . ?
O6 W5 1.939(14) 2_665 ?
O6 W4 1.951(14) . ?
O6 Cs6 3.005(18) . ?
O7 W4 1.904(6) 2_665 ?
O7 W4 1.904(6) . ?
O8 W4 1.900(14) . ?
O8 W3 1.919(13) . ?
O8 Cs1 3.566(13) . ?
O9 W2 1.898(13) . ?
O9 W1 1.910(13) 6_556 ?
O9 Cs1 3.283(13) 6_556 ?
O9 Cs6 3.530(19) 8_655 ?
O10 W2 1.74(2) . ?
O10 Cs7 2.87(5) . ?
O10 Cs7 3.19(5) 5_656 ?
O10 Cs5 3.28(3) 6_556 ?
O10 Cs5 3.28(3) . ?
O10 Cs6 3.62(2) 8_655 ?
O10 Cs6 3.62(2) 3_546 ?
O11 W3 1.929(15) . ?
O11 W2 1.939(14) . ?
O11 Cs1 3.217(15) . ?
O11 Cs5 3.32(3) . ?
O12 W3 1.734(14) . ?
O12 Cs1 2.984(14) 4_556 ?
O12 Cs6 3.25(2) 2_665 ?
O13 W3 1.926(9) 6_556 ?
O13 W3 1.926(9) . ?
O13 Cs2 3.208(18) . ?
O14 W5 1.900(13) . ?
O14 W3 1.932(14) . ?
O15 W5 1.727(14) . ?
O15 Cs5 3.05(3) 4_556 ?
O15 Cs2 3.148(17) . ?
O15 Cs1 3.177(15) 4_556 ?
O15 Cs6 3.59(2) 2_665 ?
O15 Cs5 3.60(3) 3_656 ?
O16 W5 1.922(4) . ?
O16 W5 1.922(4) 6_556 ?
O16 Cs2 3.388(19) 5_766 ?
O16 Cs2 3.407(18) . ?
O17 Sb1 2.006(12) . ?
O17 W5 2.244(13) . ?
O17 W4 2.274(12) 2_665 ?
O17 W1 2.323(13) 2_665 ?
O18 Sb1 1.994(18) . ?
O18 W3 2.260(11) 5_666 ?
O18 W3 2.260(11) 2_665 ?
O18 W2 2.337(19) 5_666 ?
O1W Cs4 2.96(4) . ?
O1W Cs3 3.11(3) . ?
O1W Cs4 3.42(3) 5_667 ?
O2W Cs7 3.35(6) 3_556 ?
O2W Cs4 3.41(4) 5_667 ?
O2W Cs3 3.77(4) . ?
Sb1 Sb1 2.188(6) 5_666 ?
Cs1 Cs5 1.91(3) . ?
Cs1 Cs6 3.551(19) 3_546 ?
Cs1 Cs2 3.946(3) 7_566 ?
Cs1 W1 4.060(2) 4_556 ?
Cs2 W5 4.032(5) . ?
Cs3 Cs4 0.746(18) . ?
Cs3 Cs4 0.746(18) 5_667 ?
Cs4 Cs4 1.49(4) 5_667 ?
Cs4 Cs6 3.81(2) 5_667 ?
Cs5 Cs6 3.39(3) 3_546 ?
Cs5 Cs5 3.64(5) 2_655 ?
Cs5 Cs7 3.81(4) 5_656 ?
Cs5 W2 4.03(3) . ?
Cs5 Cs7 4.09(4) . ?
Cs5 W5 4.10(2) 3_646 ?
Cs6 Cs7 3.31(4) 3_556 ?
Cs6 W1 4.042(12) 3_556 ?
Cs7 Cs7 3.19(9) 5_656 ?

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
W1 O1 Cs6 117.1(8) . 3_546 ?
W1 O1 Cs1 108.5(7) . 4_456 ?
Cs6 O1 Cs1 133.2(6) 3_546 4_456 ?
O1W O19 Cs4 126(2) . . ?
O1W O19 Cs3 111(2) . . ?
Cs4 O19 Cs3 15.6(5) . . ?
O1W O19 Cs4 99(2) . 5_667 ?
Cs4 O19 Cs4 26.7(8) . 5_667 ?
Cs3 O19 Cs4 11.1(4) . 5_667 ?
O1W O19 Cs6 124.4(11) . 5_667 ?
Cs4 O19 Cs6 87.9(8) . 5_667 ?
Cs3 O19 Cs6 98.4(7) . 5_667 ?
Cs4 O19 Cs6 105.6(7) 5_667 5_667 ?
O1W O19 Cs6 124.4(11) . 2_665 ?
Cs4 O19 Cs6 87.9(8) . 2_665 ?
Cs3 O19 Cs6 98.4(7) . 2_665 ?
Cs4 O19 Cs6 105.6(7) 5_667 2_665 ?
Cs6 O19 Cs6 95.3(9) 5_667 2_665 ?
W1 O2 W1 151.2(10) 6_556 . ?
W1 O2 Cs2 104.2(5) 6_556 1_455 ?
W1 O2 Cs2 104.2(5) . 1_455 ?
W1 O3 W5 118.2(6) . 2_665 ?
W1 O3 Cs5 120.5(8) . 4_456 ?
W5 O3 Cs5 104.8(7) 2_665 4_456 ?
W1 O3 Cs2 105.3(6) . 1_455 ?
W5 O3 Cs2 107.9(6) 2_665 1_455 ?
Cs5 O3 Cs2 97.7(6) 4_456 1_455 ?
W1 O3 Cs1 101.0(5) . 4_456 ?
W5 O3 Cs1 136.9(6) 2_665 4_456 ?
Cs5 O3 Cs1 34.7(5) 4_456 4_456 ?
Cs2 O3 Cs1 75.5(3) 1_455 4_456 ?
W4 O4 W1 120.8(8) . . ?
W4 O4 Cs1 110.6(6) . . ?
W1 O4 Cs1 102.4(6) . . ?
W4 O5 Cs3 150.2(8) . . ?
W4 O5 Cs4 144.3(9) . 5_667 ?
Cs3 O5 Cs4 13.7(3) . 5_667 ?
W4 O5 Cs4 150.9(8) . . ?
Cs3 O5 Cs4 13.2(3) . . ?
Cs4 O5 Cs4 26.9(6) 5_667 . ?
W5 O6 W4 116.9(7) 2_665 . ?
W5 O6 Cs6 111.3(7) 2_665 . ?
W4 O6 Cs6 128.0(7) . . ?
W4 O7 W4 145.3(11) 2_665 . ?
W4 O8 W3 154.3(7) . . ?
W4 O8 Cs1 103.8(4) . . ?
W3 O8 Cs1 99.9(5) . . ?
W2 O9 W1 151.4(8) . 6_556 ?
W2 O9 Cs1 102.1(5) . 6_556 ?
W1 O9 Cs1 106.2(5) 6_556 6_556 ?
W2 O9 Cs6 105.8(6) . 8_655 ?
W1 O9 Cs6 91.0(5) 6_556 8_655 ?
Cs1 O9 Cs6 62.7(4) 6_556 8_655 ?
W2 O10 Cs7 160.7(15) . . ?
W2 O10 Cs7 136.0(14) . 5_656 ?
Cs7 O10 Cs7 63.3(15) . 5_656 ?
W2 O10 Cs5 102.1(6) . 6_556 ?
Cs7 O10 Cs5 82.9(6) . 6_556 ?
Cs7 O10 Cs5 72.1(6) 5_656 6_556 ?
W2 O10 Cs5 102.1(6) . . ?
Cs7 O10 Cs5 82.9(6) . . ?
Cs7 O10 Cs5 72.1(6) 5_656 . ?
Cs5 O10 Cs5 144.2(11) 6_556 . ?
W2 O10 Cs6 106.4(7) . 8_655 ?
Cs7 O10 Cs6 60.0(7) . 8_655 ?
Cs7 O10 Cs6 106.6(8) 5_656 8_655 ?
Cs5 O10 Cs6 58.7(5) 6_556 8_655 ?
Cs5 O10 Cs6 136.0(8) . 8_655 ?
W2 O10 Cs6 106.4(7) . 3_546 ?
Cs7 O10 Cs6 60.0(7) . 3_546 ?
Cs7 O10 Cs6 106.6(8) 5_656 3_546 ?
Cs5 O10 Cs6 136.0(8) 6_556 3_546 ?
Cs5 O10 Cs6 58.7(5) . 3_546 ?
Cs6 O10 Cs6 81.2(8) 8_655 3_546 ?
W3 O11 W2 118.7(8) . . ?
W3 O11 Cs1 112.1(6) . . ?
W2 O11 Cs1 103.3(5) . . ?
W3 O11 Cs5 139.2(8) . . ?
W2 O11 Cs5 96.5(7) . . ?
Cs1 O11 Cs5 33.9(5) . . ?
W3 O12 Cs1 152.9(8) . 4_556 ?
W3 O12 Cs6 113.7(8) . 2_665 ?
Cs1 O12 Cs6 69.3(5) 4_556 2_665 ?
W3 O13 W3 118.3(9) 6_556 . ?
W3 O13 Cs2 116.4(5) 6_556 . ?
W3 O13 Cs2 116.4(5) . . ?
W5 O14 W3 143.8(7) . . ?
W5 O15 Cs5 150.3(9) . 4_556 ?
W5 O15 Cs2 108.0(7) . . ?
Cs5 O15 Cs2 101.3(6) 4_556 . ?
W5 O15 Cs1 150.0(7) . 4_556 ?
Cs5 O15 Cs1 35.6(5) 4_556 4_556 ?
Cs2 O15 Cs1 77.2(4) . 4_556 ?
W5 O15 Cs6 95.3(6) . 2_665 ?
Cs5 O15 Cs6 60.9(6) 4_556 2_665 ?
Cs2 O15 Cs6 131.4(5) . 2_665 ?
Cs1 O15 Cs6 62.9(4) 4_556 2_665 ?
W5 O15 Cs5 94.0(7) . 3_656 ?
Cs5 O15 Cs5 65.8(9) 4_556 3_656 ?
Cs2 O15 Cs5 138.2(6) . 3_656 ?
Cs1 O15 Cs5 101.2(6) 4_556 3_656 ?
Cs6 O15 Cs5 79.0(6) 2_665 3_656 ?
W5 O16 W5 154.4(10) . 6_556 ?
W5 O16 Cs2 102.0(5) . 5_766 ?
W5 O16 Cs2 102.0(5) 6_556 5_766 ?
W5 O16 Cs2 94.2(5) . . ?
W5 O16 Cs2 94.2(5) 6_556 . ?
Cs2 O16 Cs2 90.6(4) 5_766 . ?
Sb1 O17 W5 115.6(7) . . ?
Sb1 O17 W4 114.3(5) . 2_665 ?
W5 O17 W4 94.4(5) . 2_665 ?
Sb1 O17 W1 137.7(7) . 2_665 ?
W5 O17 W1 92.8(4) . 2_665 ?
W4 O17 W1 92.6(5) 2_665 2_665 ?
Sb1 O18 W3 115.3(6) . 5_666 ?
Sb1 O18 W3 115.3(6) . 2_665 ?
W3 O18 W3 94.0(6) 5_666 2_665 ?
Sb1 O18 W2 137.1(8) . 5_666 ?
W3 O18 W2 92.8(6) 5_666 5_666 ?
W3 O18 W2 92.8(6) 2_665 5_666 ?
O19 O1W Cs4 36.9(19) . . ?
O19 O1W Cs3 50.7(19) . . ?
Cs4 O1W Cs3 13.8(4) . . ?
O19 O1W Cs4 63(2) . 5_667 ?
Cs4 O1W Cs4 25.7(7) . 5_667 ?
Cs3 O1W Cs4 11.9(3) . 5_667 ?
Cs7 O2W Cs4 71.5(12) 3_556 5_667 ?
Cs7 O2W Cs3 82.0(12) 3_556 . ?
Cs4 O2W Cs3 10.5(3) 5_667 . ?
O18 Sb1 O17 90.4(6) . 6_556 ?
O18 Sb1 O17 90.4(6) . . ?
O17 Sb1 O17 89.5(7) 6_556 . ?
O18 Sb1 Sb1 124.2(6) . 5_666 ?
O17 Sb1 Sb1 125.7(4) 6_556 5_666 ?
O17 Sb1 Sb1 125.7(4) . 5_666 ?
Cs5 Cs1 O12 120.5(8) . 4_456 ?
Cs5 Cs1 O15 68.4(8) . 4_456 ?
O12 Cs1 O15 63.9(4) 4_456 4_456 ?
Cs5 Cs1 O1 107.7(8) . 4_556 ?
O12 Cs1 O1 123.6(4) 4_456 4_556 ?
O15 Cs1 O1 115.6(4) 4_456 4_556 ?
Cs5 Cs1 O11 75.9(8) . . ?
O12 Cs1 O11 134.4(4) 4_456 . ?
O15 Cs1 O11 143.5(4) 4_456 . ?
O1 Cs1 O11 82.1(4) 4_556 . ?
Cs5 Cs1 O3 70.3(8) . 4_556 ?
O12 Cs1 O3 121.2(4) 4_456 4_556 ?
O15 Cs1 O3 71.0(3) 4_456 4_556 ?
O1 Cs1 O3 50.5(4) 4_556 4_556 ?
O11 Cs1 O3 104.4(4) . 4_556 ?
Cs5 Cs1 O9 94.7(8) . 6_556 ?
O12 Cs1 O9 86.4(4) 4_456 6_556 ?
O15 Cs1 O9 126.2(4) 4_456 6_556 ?
O1 Cs1 O9 118.2(4) 4_556 6_556 ?
O11 Cs1 O9 48.3(3) . 6_556 ?
O3 Cs1 O9 152.3(3) 4_556 6_556 ?
Cs5 Cs1 O4 141.1(8) . . ?
O12 Cs1 O4 62.3(4) 4_456 . ?
O15 Cs1 O4 126.0(3) 4_456 . ?
O1 Cs1 O4 97.4(4) 4_556 . ?
O11 Cs1 O4 78.8(4) . . ?
O3 Cs1 O4 145.6(4) 4_556 . ?
O9 Cs1 O4 46.6(4) 6_556 . ?
Cs5 Cs1 Cs6 69.6(8) . 3_546 ?
O12 Cs1 Cs6 58.9(4) 4_456 3_546 ?
O15 Cs1 Cs6 64.2(3) 4_456 3_546 ?
O1 Cs1 Cs6 177.3(4) 4_556 3_546 ?
O11 Cs1 Cs6 96.6(3) . 3_546 ?
O3 Cs1 Cs6 128.0(3) 4_556 3_546 ?
O9 Cs1 Cs6 62.0(3) 6_556 3_546 ?
O4 Cs1 Cs6 84.6(3) . 3_546 ?
Cs5 Cs1 O8 122.1(8) . . ?
O12 Cs1 O8 106.3(4) 4_456 . ?
O15 Cs1 O8 169.2(4) 4_456 . ?
O1 Cs1 O8 65.0(3) 4_556 . ?
O11 Cs1 O8 46.5(4) . . ?
O3 Cs1 O8 113.2(3) 4_556 . ?
O9 Cs1 O8 54.4(3) 6_556 . ?
O4 Cs1 O8 45.0(3) . . ?
Cs6 Cs1 O8 115.7(3) 3_546 . ?
Cs5 Cs1 Cs2 104.5(8) . 7_566 ?
O12 Cs1 Cs2 70.4(3) 4_456 7_566 ?
O15 Cs1 Cs2 51.1(3) 4_456 7_566 ?
O1 Cs1 Cs2 71.0(3) 4_556 7_566 ?
O11 Cs1 Cs2 151.9(3) . 7_566 ?
O3 Cs1 Cs2 51.9(3) 4_556 7_566 ?
O9 Cs1 Cs2 155.2(3) 6_556 7_566 ?
O4 Cs1 Cs2 111.7(3) . 7_566 ?
Cs6 Cs1 Cs2 110.0(2) 3_546 7_566 ?
O8 Cs1 Cs2 122.9(2) . 7_566 ?
Cs5 Cs1 W1 88.5(7) . 4_556 ?
O12 Cs1 W1 129.6(3) 4_456 4_556 ?
O15 Cs1 W1 96.8(3) 4_456 4_556 ?
O1 Cs1 W1 23.3(3) 4_556 4_556 ?
O11 Cs1 W1 89.7(2) . 4_556 ?
O3 Cs1 W1 27.5(2) 4_556 4_556 ?
O9 Cs1 W1 134.9(2) 6_556 4_556 ?
O4 Cs1 W1 120.5(3) . 4_556 ?
Cs6 Cs1 W1 154.8(2) 3_546 4_556 ?
O8 Cs1 W1 86.2(2) . 4_556 ?
Cs2 Cs1 W1 62.38(8) 7_566 4_556 ?
O15 Cs2 O15 101.4(6) 6_556 . ?
O15 Cs2 O13 78.9(4) 6_556 . ?
O15 Cs2 O13 78.9(4) . . ?
O15 Cs2 O3 135.0(4) 6_556 1_655 ?
O15 Cs2 O3 71.7(4) . 1_655 ?
O13 Cs2 O3 138.3(3) . 1_655 ?
O15 Cs2 O3 71.7(4) 6_556 6_656 ?
O15 Cs2 O3 135.0(4) . 6_656 ?
O13 Cs2 O3 138.3(3) . 6_656 ?
O3 Cs2 O3 82.6(5) 1_655 6_656 ?
O15 Cs2 O2 120.0(3) 6_556 1_655 ?
O15 Cs2 O2 120.0(3) . 1_655 ?
O13 Cs2 O2 145.5(6) . 1_655 ?
O3 Cs2 O2 48.3(3) 1_655 1_655 ?
O3 Cs2 O2 48.3(3) 6_656 1_655 ?
O15 Cs2 O16 87.8(3) 6_556 5_766 ?
O15 Cs2 O16 87.8(3) . 5_766 ?
O13 Cs2 O16 159.0(5) . 5_766 ?
O3 Cs2 O16 48.4(3) 1_655 5_766 ?
O3 Cs2 O16 48.4(3) 6_656 5_766 ?
O2 Cs2 O16 55.6(5) 1_655 5_766 ?
O15 Cs2 O16 50.7(3) 6_556 . ?
O15 Cs2 O16 50.7(3) . . ?
O13 Cs2 O16 69.5(5) . . ?
O3 Cs2 O16 110.2(4) 1_655 . ?
O3 Cs2 O16 110.2(4) 6_656 . ?
O2 Cs2 O16 145.0(5) 1_655 . ?
O16 Cs2 O16 89.4(4) 5_766 . ?
O15 Cs2 Cs1 51.7(3) 6_556 7_665 ?
O15 Cs2 Cs1 151.6(3) . 7_665 ?
O13 Cs2 Cs1 86.02(13) . 7_665 ?
O3 Cs2 Cs1 132.0(3) 1_655 7_665 ?
O3 Cs2 Cs1 52.5(3) 6_656 7_665 ?
O2 Cs2 Cs1 85.55(12) 1_655 7_665 ?
O16 Cs2 Cs1 98.64(10) 5_766 7_665 ?
O16 Cs2 Cs1 101.45(10) . 7_665 ?
O15 Cs2 Cs1 151.6(3) 6_556 4_556 ?
O15 Cs2 Cs1 51.7(3) . 4_556 ?
O13 Cs2 Cs1 86.02(13) . 4_556 ?
O3 Cs2 Cs1 52.5(3) 1_655 4_556 ?
O3 Cs2 Cs1 132.0(3) 6_656 4_556 ?
O2 Cs2 Cs1 85.55(12) 1_655 4_556 ?
O16 Cs2 Cs1 98.64(10) 5_766 4_556 ?
O16 Cs2 Cs1 101.45(10) . 4_556 ?
Cs1 Cs2 Cs1 151.3(2) 7_665 4_556 ?
O15 Cs2 W5 78.8(3) 6_556 . ?
O15 Cs2 W5 24.0(3) . . ?
O13 Cs2 W5 66.3(4) . . ?
O3 Cs2 W5 93.6(3) 1_655 . ?
O3 Cs2 W5 132.6(3) 6_656 . ?
O2 Cs2 W5 141.1(3) 1_655 . ?
O16 Cs2 W5 95.2(3) 5_766 . ?
O16 Cs2 W5 28.39(7) . . ?
Cs1 Cs2 W5 127.61(12) 7_665 . ?
Cs1 Cs2 W5 73.11(6) 4_556 . ?
Cs4 Cs3 Cs4 179.996(10) . 5_667 ?
Cs4 Cs3 O19 52.5(16) . . ?
Cs4 Cs3 O19 127.5(16) 5_667 . ?
Cs4 Cs3 O19 127.5(16) . 5_667 ?
Cs4 Cs3 O19 52.5(16) 5_667 5_667 ?
O19 Cs3 O19 180.0 . 5_667 ?
Cs4 Cs3 O5 84.6(9) . 5_667 ?
Cs4 Cs3 O5 95.4(9) 5_667 5_667 ?
O19 Cs3 O5 111.0(4) . 5_667 ?
O19 Cs3 O5 69.0(4) 5_667 5_667 ?
Cs4 Cs3 O5 95.4(9) . 6_557 ?
Cs4 Cs3 O5 84.6(9) 5_667 6_557 ?
O19 Cs3 O5 69.0(4) . 6_557 ?
O19 Cs3 O5 111.0(4) 5_667 6_557 ?
O5 Cs3 O5 64.4(6) 5_667 6_557 ?
Cs4 Cs3 O5 84.6(9) . 2_665 ?
Cs4 Cs3 O5 95.4(9) 5_667 2_665 ?
O19 Cs3 O5 111.0(4) . 2_665 ?
O19 Cs3 O5 69.0(4) 5_667 2_665 ?
O5 Cs3 O5 115.6(6) 5_667 2_665 ?
O5 Cs3 O5 180.0 6_557 2_665 ?
Cs4 Cs3 O5 95.4(9) . . ?
Cs4 Cs3 O5 84.6(9) 5_667 . ?
O19 Cs3 O5 69.0(4) . . ?
O19 Cs3 O5 111.0(4) 5_667 . ?
O5 Cs3 O5 180.0 5_667 . ?
O5 Cs3 O5 115.6(6) 6_557 . ?
O5 Cs3 O5 64.4(6) 2_665 . ?
Cs4 Cs3 O1W 108.7(16) . 5_667 ?
Cs4 Cs3 O1W 71.3(16) 5_667 5_667 ?
O19 Cs3 O1W 161.2(7) . 5_667 ?
O19 Cs3 O1W 18.8(7) 5_667 5_667 ?
O5 Cs3 O1W 62.2(3) 5_667 5_667 ?
O5 Cs3 O1W 117.8(3) 6_557 5_667 ?
O5 Cs3 O1W 62.2(3) 2_665 5_667 ?
O5 Cs3 O1W 117.8(3) . 5_667 ?
Cs4 Cs3 O1W 71.3(16) . . ?
Cs4 Cs3 O1W 108.7(16) 5_667 . ?
O19 Cs3 O1W 18.8(7) . . ?
O19 Cs3 O1W 161.2(7) 5_667 . ?
O5 Cs3 O1W 117.8(3) 5_667 . ?
O5 Cs3 O1W 62.2(3) 6_557 . ?
O5 Cs3 O1W 117.8(3) 2_665 . ?
O5 Cs3 O1W 62.2(3) . . ?
O1W Cs3 O1W 180.0 5_667 . ?
Cs4 Cs3 O2W 56.6(17) . 5_667 ?
Cs4 Cs3 O2W 123.4(17) 5_667 5_667 ?
O19 Cs3 O2W 109.1(8) . 5_667 ?
O19 Cs3 O2W 70.9(8) 5_667 5_667 ?
O5 Cs3 O2W 60.7(3) 5_667 5_667 ?
O5 Cs3 O2W 119.3(3) 6_557 5_667 ?
O5 Cs3 O2W 60.7(3) 2_665 5_667 ?
O5 Cs3 O2W 119.3(3) . 5_667 ?
O1W Cs3 O2W 52.1(8) 5_667 5_667 ?
O1W Cs3 O2W 127.9(8) . 5_667 ?
Cs4 Cs3 O2W 123.4(17) . . ?
Cs4 Cs3 O2W 56.6(17) 5_667 . ?
O19 Cs3 O2W 70.9(8) . . ?
O19 Cs3 O2W 109.1(8) 5_667 . ?
O5 Cs3 O2W 119.3(3) 5_667 . ?
O5 Cs3 O2W 60.7(3) 6_557 . ?
O5 Cs3 O2W 119.3(3) 2_665 . ?
O5 Cs3 O2W 60.7(3) . . ?
O1W Cs3 O2W 127.9(8) 5_667 . ?
O1W Cs3 O2W 52.1(8) . . ?
O2W Cs3 O2W 180.0 5_667 . ?
Cs3 Cs4 Cs4 0.002(6) . 5_667 ?
Cs3 Cs4 O19 111.9(19) . . ?
Cs4 Cs4 O19 111.9(19) 5_667 . ?
Cs3 Cs4 O1W 94.9(17) . . ?
Cs4 Cs4 O1W 94.9(17) 5_667 . ?
O19 Cs4 O1W 17.0(8) . . ?
Cs3 Cs4 O19 41.4(14) . 5_667 ?
Cs4 Cs4 O19 41.4(14) 5_667 5_667 ?
O19 Cs4 O19 153.3(8) . 5_667 ?
O1W Cs4 O19 136.3(9) . 5_667 ?
Cs3 Cs4 O5 81.6(9) . 5_667 ?
Cs4 Cs4 O5 81.6(9) 5_667 5_667 ?
O19 Cs4 O5 122.5(4) . 5_667 ?
O1W Cs4 O5 122.1(4) . 5_667 ?
O19 Cs4 O5 63.0(5) 5_667 5_667 ?
Cs3 Cs4 O5 81.6(9) . 2_665 ?
Cs4 Cs4 O5 81.6(9) 5_667 2_665 ?
O19 Cs4 O5 122.5(4) . 2_665 ?
O1W Cs4 O5 122.1(4) . 2_665 ?
O19 Cs4 O5 63.0(5) 5_667 2_665 ?
O5 Cs4 O5 114.5(9) 5_667 2_665 ?
Cs3 Cs4 O5 71.5(8) . 6_557 ?
Cs4 Cs4 O5 71.5(8) 5_667 6_557 ?
O19 Cs4 O5 69.8(6) . 6_557 ?
O1W Cs4 O5 61.9(5) . 6_557 ?
O19 Cs4 O5 95.3(6) 5_667 6_557 ?
O5 Cs4 O5 62.3(6) 5_667 6_557 ?
O5 Cs4 O5 153.1(6) 2_665 6_557 ?
Cs3 Cs4 O5 71.5(8) . . ?
Cs4 Cs4 O5 71.5(8) 5_667 . ?
O19 Cs4 O5 69.8(6) . . ?
O1W Cs4 O5 61.9(5) . . ?
O19 Cs4 O5 95.3(6) 5_667 . ?
O5 Cs4 O5 153.1(6) 5_667 . ?
O5 Cs4 O5 62.3(6) 2_665 . ?
O5 Cs4 O5 107.4(8) 6_557 . ?
Cs3 Cs4 O2W 112.9(18) . 5_667 ?
Cs4 Cs4 O2W 112.9(18) 5_667 5_667 ?
O19 Cs4 O2W 135.2(12) . 5_667 ?
O1W Cs4 O2W 152.2(10) . 5_667 ?
O19 Cs4 O2W 71.4(9) 5_667 5_667 ?
O5 Cs4 O2W 65.0(5) 5_667 5_667 ?
O5 Cs4 O2W 65.0(5) 2_665 5_667 ?
O5 Cs4 O2W 125.7(4) 6_557 5_667 ?
O5 Cs4 O2W 125.7(4) . 5_667 ?
Cs3 Cs4 O1W 59.4(15) . 5_667 ?
Cs4 Cs4 O1W 59.4(15) 5_667 5_667 ?
O19 Cs4 O1W 171.3(11) . 5_667 ?
O1W Cs4 O1W 154.3(7) . 5_667 ?
O19 Cs4 O1W 17.9(6) 5_667 5_667 ?
O5 Cs4 O1W 58.5(4) 5_667 5_667 ?
O5 Cs4 O1W 58.5(4) 2_665 5_667 ?
O5 Cs4 O1W 105.5(6) 6_557 5_667 ?
O5 Cs4 O1W 105.5(6) . 5_667 ?
O2W Cs4 O1W 53.5(9) 5_667 5_667 ?
Cs3 Cs4 Cs6 136.6(8) . 5_667 ?
Cs4 Cs4 Cs6 136.6(8) 5_667 5_667 ?
O19 Cs4 Cs6 56.8(6) . 5_667 ?
O1W Cs4 Cs6 69.0(5) . 5_667 ?
O19 Cs4 Cs6 137.9(4) 5_667 5_667 ?
O5 Cs4 Cs6 74.9(4) 5_667 5_667 ?
O5 Cs4 Cs6 141.4(7) 2_665 5_667 ?
O5 Cs4 Cs6 65.3(4) 6_557 5_667 ?
O5 Cs4 Cs6 125.5(7) . 5_667 ?
O2W Cs4 Cs6 89.5(7) 5_667 5_667 ?
O1W Cs4 Cs6 128.8(5) 5_667 5_667 ?
Cs1 Cs5 O15 76.0(8) . 4_456 ?
Cs1 Cs5 O3 75.0(8) . 4_556 ?
O15 Cs5 O3 73.9(7) 4_456 4_556 ?
Cs1 Cs5 O10 101.1(10) . . ?
O15 Cs5 O10 132.6(9) 4_456 . ?
O3 Cs5 O10 152.3(10) 4_556 . ?
Cs1 Cs5 O11 70.2(8) . . ?
O15 Cs5 O11 145.3(10) 4_456 . ?
O3 Cs5 O11 104.0(8) 4_556 . ?
O10 Cs5 O11 50.5(6) . . ?
Cs1 Cs5 Cs6 78.7(8) . 3_546 ?
O15 Cs5 Cs6 67.5(6) 4_456 3_546 ?
O3 Cs5 Cs6 137.3(9) 4_556 3_546 ?
O10 Cs5 Cs6 65.6(6) . 3_546 ?
O11 Cs5 Cs6 97.8(7) . 3_546 ?
Cs1 Cs5 O15 112.7(10) . 3_646 ?
O15 Cs5 O15 57.5(6) 4_456 3_646 ?
O3 Cs5 O15 48.7(5) 4_556 3_646 ?
O10 Cs5 O15 146.1(9) . 3_646 ?
O11 Cs5 O15 145.2(8) . 3_646 ?
Cs6 Cs5 O15 116.9(8) 3_546 3_646 ?
Cs1 Cs5 Cs5 140.1(11) . 2_655 ?
O15 Cs5 Cs5 64.5(6) 4_456 2_655 ?
O3 Cs5 Cs5 98.5(7) 4_556 2_655 ?
O10 Cs5 Cs5 101.3(6) . 2_655 ?
O11 Cs5 Cs5 147.0(6) . 2_655 ?
Cs6 Cs5 Cs5 81.0(8) 3_546 2_655 ?
O15 Cs5 Cs5 49.7(5) 3_646 2_655 ?
Cs1 Cs5 Cs7 150.5(13) . 5_656 ?
O15 Cs5 Cs7 130.5(11) 4_456 5_656 ?
O3 Cs5 Cs7 120.6(9) 4_556 5_656 ?
O10 Cs5 Cs7 52.8(8) . 5_656 ?
O11 Cs5 Cs7 81.2(9) . 5_656 ?
Cs6 Cs5 Cs7 98.5(9) 3_546 5_656 ?
O15 Cs5 Cs7 94.9(9) 3_646 5_656 ?
Cs5 Cs5 Cs7 66.5(8) 2_655 5_656 ?
Cs1 Cs5 W2 79.3(8) . . ?
O15 Cs5 W2 136.5(8) 4_456 . ?
O3 Cs5 W2 132.2(8) 4_556 . ?
O10 Cs5 W2 25.0(4) . . ?
O11 Cs5 W2 28.6(3) . . ?
Cs6 Cs5 W2 72.9(5) 3_546 . ?
O15 Cs5 W2 165.1(8) 3_646 . ?
Cs5 Cs5 W2 126.3(4) 2_655 . ?
Cs7 Cs5 W2 71.9(8) 5_656 . ?
Cs1 Cs5 Cs7 126.0(12) . . ?
O15 Cs5 Cs7 98.9(9) 4_456 . ?
O3 Cs5 Cs7 156.3(11) 4_556 . ?
O10 Cs5 Cs7 44.2(8) . . ?
O11 Cs5 Cs7 94.7(8) . . ?
Cs6 Cs5 Cs7 51.5(7) 3_546 . ?
O15 Cs5 Cs7 108.2(9) 3_646 . ?
Cs5 Cs5 Cs7 58.8(7) 2_655 . ?
Cs7 Cs5 Cs7 47.5(12) 5_656 . ?
W2 Cs5 Cs7 68.3(7) . . ?
Cs1 Cs5 W5 100.8(9) . 3_646 ?
O15 Cs5 W5 71.9(6) 4_456 3_646 ?
O3 Cs5 W5 27.2(3) 4_556 3_646 ?
O10 Cs5 W5 150.7(8) . 3_646 ?
O11 Cs5 W5 121.6(7) . 3_646 ?
Cs6 Cs5 W5 138.3(8) 3_546 3_646 ?
O15 Cs5 W5 24.8(3) 3_646 3_646 ?
Cs5 Cs5 W5 73.1(6) 2_655 3_646 ?
Cs7 Cs5 W5 100.4(8) 5_656 3_646 ?
W2 Cs5 W5 148.6(7) . 3_646 ?
Cs7 Cs5 W5 129.2(9) . 3_646 ?
O1 Cs6 O6 126.2(6) 3_556 . ?
O1 Cs6 O19 68.0(6) 3_556 5_667 ?
O6 Cs6 O19 116.6(8) . 5_667 ?
O1 Cs6 O12 58.2(5) 3_556 2_665 ?
O6 Cs6 O12 81.2(5) . 2_665 ?
O19 Cs6 O12 121.1(7) 5_667 2_665 ?
O1 Cs6 Cs7 133.0(8) 3_556 3_556 ?
O6 Cs6 Cs7 98.9(8) . 3_556 ?
O19 Cs6 Cs7 81.3(8) 5_667 3_556 ?
O12 Cs6 Cs7 155.2(10) 2_665 3_556 ?
O1 Cs6 Cs5 109.4(7) 3_556 3_556 ?
O6 Cs6 Cs5 94.9(7) . 3_556 ?
O19 Cs6 Cs5 143.2(7) 5_667 3_556 ?
O12 Cs6 Cs5 80.1(6) 2_665 3_556 ?
Cs7 Cs6 Cs5 75.1(9) 3_556 3_556 ?
O1 Cs6 O9 50.1(4) 3_556 8_666 ?
O6 Cs6 O9 156.0(7) . 8_666 ?
O19 Cs6 O9 85.1(6) 5_667 8_666 ?
O12 Cs6 O9 78.5(5) 2_665 8_666 ?
Cs7 Cs6 O9 94.2(9) 3_556 8_666 ?
Cs5 Cs6 O9 69.1(6) 3_556 8_666 ?
O1 Cs6 Cs1 80.8(4) 3_556 3_556 ?
O6 Cs6 Cs1 101.7(5) . 3_556 ?
O19 Cs6 Cs1 140.0(6) 5_667 3_556 ?
O12 Cs6 Cs1 51.8(4) 2_665 3_556 ?
Cs7 Cs6 Cs1 104.6(9) 3_556 3_556 ?
Cs5 Cs6 Cs1 31.7(5) 3_556 3_556 ?
O9 Cs6 Cs1 55.2(3) 8_666 3_556 ?
O1 Cs6 O15 114.3(5) 3_556 2_665 ?
O6 Cs6 O15 49.1(4) . 2_665 ?
O19 Cs6 O15 164.8(7) 5_667 2_665 ?
O12 Cs6 O15 56.7(4) 2_665 2_665 ?
Cs7 Cs6 O15 104.7(8) 3_556 2_665 ?
Cs5 Cs6 O15 51.6(6) 3_556 2_665 ?
O9 Cs6 O15 108.0(6) 8_666 2_665 ?
Cs1 Cs6 O15 52.8(3) 3_556 2_665 ?
O1 Cs6 O10 93.8(6) 3_556 3_556 ?
O6 Cs6 O10 138.1(7) . 3_556 ?
O19 Cs6 O10 87.6(5) 5_667 3_556 ?
O12 Cs6 O10 116.7(6) 2_665 3_556 ?
Cs7 Cs6 O10 48.8(9) 3_556 3_556 ?
Cs5 Cs6 O10 55.7(6) 3_556 3_556 ?
O9 Cs6 O10 46.4(4) 8_666 3_556 ?
Cs1 Cs6 O10 69.7(4) 3_556 3_556 ?
O15 Cs6 O10 107.0(6) 2_665 3_556 ?
O1 Cs6 Cs4 100.1(6) 3_556 5_667 ?
O6 Cs6 Cs4 86.3(5) . 5_667 ?
O19 Cs6 Cs4 35.3(6) 5_667 5_667 ?
O12 Cs6 Cs4 137.3(7) 2_665 5_667 ?
Cs7 Cs6 Cs4 67.0(8) 3_556 5_667 ?
Cs5 Cs6 Cs4 141.9(7) 3_556 5_667 ?
O9 Cs6 Cs4 117.4(5) 8_666 5_667 ?
Cs1 Cs6 Cs4 169.5(5) 3_556 5_667 ?
O15 Cs6 Cs4 134.0(5) 2_665 5_667 ?
O10 Cs6 Cs4 99.7(4) 3_556 5_667 ?
O1 Cs6 W1 21.9(3) 3_556 3_556 ?
O6 Cs6 W1 143.5(5) . 3_556 ?
O19 Cs6 W1 74.8(6) 5_667 3_556 ?
O12 Cs6 W1 64.5(4) 2_665 3_556 ?
Cs7 Cs6 W1 117.5(8) 3_556 3_556 ?
Cs5 Cs6 W1 91.5(6) 3_556 3_556 ?
O9 Cs6 W1 28.2(2) 8_666 3_556 ?
Cs1 Cs6 W1 67.4(2) 3_556 3_556 ?
O15 Cs6 W1 113.2(5) 2_665 3_556 ?
O10 Cs6 W1 73.1(4) 3_556 3_556 ?
Cs4 Cs6 W1 110.0(5) 5_667 3_556 ?
O10 Cs7 O10 116.7(15) . 5_656 ?
O10 Cs7 Cs7 63.2(16) . 5_656 ?
O10 Cs7 Cs7 53.5(14) 5_656 5_656 ?
O10 Cs7 Cs6 71.2(10) . 3_546 ?
O10 Cs7 Cs6 134.6(6) 5_656 3_546 ?
Cs7 Cs7 Cs6 114.3(15) 5_656 3_546 ?
O10 Cs7 Cs6 71.2(10) . 8_655 ?
O10 Cs7 Cs6 134.6(6) 5_656 8_655 ?
Cs7 Cs7 Cs6 114.3(15) 5_656 8_655 ?
Cs6 Cs7 Cs6 90.7(13) 3_546 8_655 ?
O10 Cs7 O2W 166.6(19) . 3_546 ?
O10 Cs7 O2W 76.7(14) 5_656 3_546 ?
Cs7 Cs7 O2W 130(2) 5_656 3_546 ?
Cs6 Cs7 O2W 99.7(11) 3_546 3_546 ?
Cs6 Cs7 O2W 99.7(11) 8_655 3_546 ?
O10 Cs7 Cs5 105.7(10) . 5_656 ?
O10 Cs7 Cs5 55.1(7) 5_656 5_656 ?
Cs7 Cs7 Cs5 70.8(10) 5_656 5_656 ?
Cs6 Cs7 Cs5 170.3(12) 3_546 5_656 ?
Cs6 Cs7 Cs5 79.6(5) 8_655 5_656 ?
O2W Cs7 Cs5 81.6(10) 3_546 5_656 ?
O10 Cs7 Cs5 105.7(10) . 2_655 ?
O10 Cs7 Cs5 55.1(7) 5_656 2_655 ?
Cs7 Cs7 Cs5 70.8(10) 5_656 2_655 ?
Cs6 Cs7 Cs5 79.6(5) 3_546 2_655 ?
Cs6 Cs7 Cs5 170.3(12) 8_655 2_655 ?
O2W Cs7 Cs5 81.6(10) 3_546 2_655 ?
Cs5 Cs7 Cs5 110.1(14) 5_656 2_655 ?
O10 Cs7 Cs4 111.6(15) . 7_565 ?
O10 Cs7 Cs4 131.7(15) 5_656 7_565 ?
Cs7 Cs7 Cs4 175(2) 5_656 7_565 ?
Cs6 Cs7 Cs4 62.5(8) 3_546 7_565 ?
Cs6 Cs7 Cs4 62.5(8) 8_655 7_565 ?
O2W Cs7 Cs4 55.0(10) 3_546 7_565 ?
Cs5 Cs7 Cs4 111.7(9) 5_656 7_565 ?
Cs5 Cs7 Cs4 111.7(9) 2_655 7_565 ?
O10 Cs7 Cs5 52.8(7) . . ?
O10 Cs7 Cs5 94.0(9) 5_656 . ?
Cs7 Cs7 Cs5 61.7(10) 5_656 . ?
Cs6 Cs7 Cs5 53.4(6) 3_546 . ?
Cs6 Cs7 Cs5 119.4(14) 8_655 . ?
O2W Cs7 Cs5 129.8(6) 3_546 . ?
Cs5 Cs7 Cs5 132.5(12) 5_656 . ?
Cs5 Cs7 Cs5 54.7(8) 2_655 . ?
Cs4 Cs7 Cs5 115.6(9) 7_565 . ?
O10 Cs7 Cs5 52.8(7) . 6_556 ?
O10 Cs7 Cs5 94.0(9) 5_656 6_556 ?
Cs7 Cs7 Cs5 61.7(10) 5_656 6_556 ?
Cs6 Cs7 Cs5 119.4(14) 3_546 6_556 ?
Cs6 Cs7 Cs5 53.4(6) 8_655 6_556 ?
O2W Cs7 Cs5 129.8(6) 3_546 6_556 ?
Cs5 Cs7 Cs5 54.7(8) 5_656 6_556 ?
Cs5 Cs7 Cs5 132.5(12) 2_655 6_556 ?
Cs4 Cs7 Cs5 115.6(9) 7_565 6_556 ?
Cs5 Cs7 Cs5 99.7(12) . 6_556 ?
O10 Cs7 Cs3 113.8(14) . 3_546 ?
O10 Cs7 Cs3 129.6(14) 5_656 3_546 ?
Cs7 Cs7 Cs3 177(2) 5_656 3_546 ?
Cs6 Cs7 Cs3 63.8(8) 3_546 3_546 ?
Cs6 Cs7 Cs3 63.8(8) 8_655 3_546 ?
O2W Cs7 Cs3 52.8(9) 3_546 3_546 ?
Cs5 Cs7 Cs3 110.7(8) 5_656 3_546 ?
Cs5 Cs7 Cs3 110.7(8) 2_655 3_546 ?
Cs4 Cs7 Cs3 2.1(3) 7_565 3_546 ?
Cs5 Cs7 Cs3 116.8(8) . 3_546 ?
Cs5 Cs7 Cs3 116.8(8) 6_556 3_546 ?
O1 W1 O9 101.8(7) . 6_556 ?
O1 W1 O2 101.5(7) . . ?
O9 W1 O2 86.6(7) 6_556 . ?
O1 W1 O3 98.7(7) . . ?
O9 W1 O3 159.4(6) 6_556 . ?
O2 W1 O3 87.3(7) . . ?
O1 W1 O4 101.3(7) . . ?
O9 W1 O4 87.0(6) 6_556 . ?
O2 W1 O4 157.2(7) . . ?
O3 W1 O4 91.0(6) . . ?
O1 W1 O17 169.9(6) . 2_665 ?
O9 W1 O17 86.1(5) 6_556 2_665 ?
O2 W1 O17 85.2(6) . 2_665 ?
O3 W1 O17 73.8(5) . 2_665 ?
O4 W1 O17 72.5(5) . 2_665 ?
O1 W1 Cs6 41.0(6) . 3_546 ?
O9 W1 Cs6 60.8(5) 6_556 3_546 ?
O2 W1 Cs6 99.5(7) . 3_546 ?
O3 W1 Cs6 139.7(5) . 3_546 ?
O4 W1 Cs6 96.5(5) . 3_546 ?
O17 W1 Cs6 146.0(4) 2_665 3_546 ?
O1 W1 Cs1 48.2(5) . 4_456 ?
O9 W1 Cs1 149.1(4) 6_556 4_456 ?
O2 W1 Cs1 104.8(5) . 4_456 ?
O3 W1 Cs1 51.4(4) . 4_456 ?
O4 W1 Cs1 91.7(4) . 4_456 ?
O17 W1 Cs1 122.9(3) 2_665 4_456 ?
Cs6 W1 Cs1 88.7(3) 3_546 4_456 ?
O1 W1 Cs2 79.7(5) . 1_455 ?
O9 W1 Cs2 134.2(4) 6_556 1_455 ?
O2 W1 Cs2 49.2(5) . 1_455 ?
O3 W1 Cs2 48.3(4) . 1_455 ?
O4 W1 Cs2 138.1(4) . 1_455 ?
O17 W1 Cs2 99.5(3) 2_665 1_455 ?
Cs6 W1 Cs2 109.1(3) 3_546 1_455 ?
Cs1 W1 Cs2 57.47(5) 4_456 1_455 ?
O1 W1 Cs1 79.2(5) . . ?
O9 W1 Cs1 48.1(4) 6_556 . ?
O2 W1 Cs1 132.7(6) . . ?
O3 W1 Cs1 139.9(4) . . ?
O4 W1 Cs1 51.3(5) . . ?
O17 W1 Cs1 102.0(3) 2_665 . ?
Cs6 W1 Cs1 50.8(3) 3_546 . ?
Cs1 W1 Cs1 109.39(3) 4_456 . ?
Cs2 W1 Cs1 158.47(9) 1_455 . ?
O1 W1 Cs5 70.4(6) . 4_456 ?
O9 W1 Cs5 156.3(5) 6_556 4_456 ?
O2 W1 Cs5 116.5(6) . 4_456 ?
O3 W1 Cs5 37.7(5) . 4_456 ?
O4 W1 Cs5 73.3(5) . 4_456 ?
O17 W1 Cs5 99.9(5) 2_665 4_456 ?
Cs6 W1 Cs5 107.7(4) 3_546 4_456 ?
Cs1 W1 Cs5 25.4(3) 4_456 4_456 ?
Cs2 W1 Cs5 67.7(3) 1_455 4_456 ?
Cs1 W1 Cs5 108.2(3) . 4_456 ?
O10 W2 O9 101.4(7) . 6_556 ?
O10 W2 O9 101.4(7) . . ?
O9 W2 O9 86.7(8) 6_556 . ?
O10 W2 O11 99.6(7) . 6_556 ?
O9 W2 O11 159.0(6) 6_556 6_556 ?
O9 W2 O11 87.8(6) . 6_556 ?
O10 W2 O11 99.6(7) . . ?
O9 W2 O11 87.8(6) 6_556 . ?
O9 W2 O11 159.0(6) . . ?
O11 W2 O11 90.0(9) 6_556 . ?
O10 W2 O18 169.6(9) . 5_666 ?
O9 W2 O18 86.2(5) 6_556 5_666 ?
O9 W2 O18 86.2(5) . 5_666 ?
O11 W2 O18 73.2(5) 6_556 5_666 ?
O11 W2 O18 73.2(5) . 5_666 ?
O10 W2 Cs5 52.9(4) . 6_556 ?
O9 W2 Cs5 141.3(5) 6_556 6_556 ?
O9 W2 Cs5 73.4(5) . 6_556 ?
O11 W2 Cs5 54.9(6) 6_556 6_556 ?
O11 W2 Cs5 121.6(6) . 6_556 ?
O18 W2 Cs5 124.0(4) 5_666 6_556 ?
O10 W2 Cs5 52.9(4) . . ?
O9 W2 Cs5 73.4(5) 6_556 . ?
O9 W2 Cs5 141.3(5) . . ?
O11 W2 Cs5 121.6(6) 6_556 . ?
O11 W2 Cs5 54.9(6) . . ?
O18 W2 Cs5 124.0(4) 5_666 . ?
Cs5 W2 Cs5 101.8(7) 6_556 . ?
O10 W2 Cs1 77.09(5) . 6_556 ?
O9 W2 Cs1 135.3(4) 6_556 6_556 ?
O9 W2 Cs1 51.2(4) . 6_556 ?
O11 W2 Cs1 49.4(4) 6_556 6_556 ?
O11 W2 Cs1 136.8(5) . 6_556 ?
O18 W2 Cs1 102.72(5) 5_666 6_556 ?
Cs5 W2 Cs1 27.0(4) 6_556 6_556 ?
Cs5 W2 Cs1 128.5(4) . 6_556 ?
O10 W2 Cs1 77.09(5) . . ?
O9 W2 Cs1 51.2(4) 6_556 . ?
O9 W2 Cs1 135.3(4) . . ?
O11 W2 Cs1 136.8(5) 6_556 . ?
O11 W2 Cs1 49.4(4) . . ?
O18 W2 Cs1 102.72(5) 5_666 . ?
Cs5 W2 Cs1 128.5(4) 6_556 . ?
Cs5 W2 Cs1 27.0(4) . . ?
Cs1 W2 Cs1 154.17(10) 6_556 . ?
O10 W2 Cs6 51.5(6) . 8_655 ?
O9 W2 Cs6 94.9(5) 6_556 8_655 ?
O9 W2 Cs6 49.9(4) . 8_655 ?
O11 W2 Cs6 97.1(5) 6_556 8_655 ?
O11 W2 Cs6 150.9(5) . 8_655 ?
O18 W2 Cs6 135.8(3) 5_666 8_655 ?
Cs5 W2 Cs6 47.0(4) 6_556 8_655 ?
Cs5 W2 Cs6 98.1(4) . 8_655 ?
Cs1 W2 Cs6 48.8(2) 6_556 8_655 ?
Cs1 W2 Cs6 112.1(2) . 8_655 ?
O10 W2 Cs6 51.5(6) . 3_546 ?
O9 W2 Cs6 49.9(4) 6_556 3_546 ?
O9 W2 Cs6 94.9(5) . 3_546 ?
O11 W2 Cs6 150.9(5) 6_556 3_546 ?
O11 W2 Cs6 97.1(5) . 3_546 ?
O18 W2 Cs6 135.8(3) 5_666 3_546 ?
Cs5 W2 Cs6 98.1(4) 6_556 3_546 ?
Cs5 W2 Cs6 47.0(4) . 3_546 ?
Cs1 W2 Cs6 112.1(2) 6_556 3_546 ?
Cs1 W2 Cs6 48.8(2) . 3_546 ?
Cs6 W2 Cs6 64.1(4) 8_655 3_546 ?
O12 W3 O8 101.9(7) . . ?
O12 W3 O13 98.4(7) . . ?
O8 W3 O13 159.7(6) . . ?
O12 W3 O11 98.1(7) . . ?
O8 W3 O11 89.1(6) . . ?
O13 W3 O11 88.1(8) . . ?
O12 W3 O14 101.2(7) . . ?
O8 W3 O14 89.4(5) . . ?
O13 W3 O14 86.6(8) . . ?
O11 W3 O14 160.4(6) . . ?
O12 W3 O18 169.8(7) . 5_666 ?
O8 W3 O18 86.0(5) . 5_666 ?
O13 W3 O18 73.9(6) . 5_666 ?
O11 W3 O18 75.2(6) . 5_666 ?
O14 W3 O18 85.2(6) . 5_666 ?
O12 W3 Cs6 44.4(6) . 2_665 ?
O8 W3 Cs6 66.7(5) . 2_665 ?
O13 W3 Cs6 130.7(6) . 2_665 ?
O11 W3 Cs6 122.1(5) . 2_665 ?
O14 W3 Cs6 74.8(4) . 2_665 ?
O18 W3 Cs6 145.8(5) 5_666 2_665 ?
O12 W3 Cs1 81.4(5) . . ?
O8 W3 Cs1 54.2(4) . . ?
O13 W3 Cs1 130.2(7) . . ?
O11 W3 Cs1 43.5(5) . . ?
O14 W3 Cs1 142.8(4) . . ?
O18 W3 Cs1 98.3(4) 5_666 . ?
Cs6 W3 Cs1 82.5(2) 2_665 . ?
O12 W3 Cs2 67.2(5) . . ?
O8 W3 Cs2 152.5(4) . . ?
O13 W3 Cs2 40.6(5) . . ?
O11 W3 Cs2 116.8(5) . . ?
O14 W3 Cs2 69.3(4) . . ?
O18 W3 Cs2 108.5(3) 5_666 . ?
Cs6 W3 Cs2 90.2(3) 2_665 . ?
Cs1 W3 Cs2 140.79(8) . . ?
O5 W4 O4 99.4(7) . . ?
O5 W4 O8 100.7(7) . . ?
O4 W4 O8 89.0(6) . . ?
O5 W4 O7 100.7(8) . . ?
O4 W4 O7 159.9(7) . . ?
O8 W4 O7 89.0(4) . . ?
O5 W4 O6 99.2(7) . . ?
O4 W4 O6 88.0(6) . . ?
O8 W4 O6 160.2(5) . . ?
O7 W4 O6 87.1(4) . . ?
O5 W4 O17 170.4(6) . 2_665 ?
O4 W4 O17 74.0(6) . 2_665 ?
O8 W4 O17 86.5(5) . 2_665 ?
O7 W4 O17 85.8(6) . 2_665 ?
O6 W4 O17 73.9(5) . 2_665 ?
O5 W4 Cs1 82.1(6) . . ?
O4 W4 Cs1 45.7(4) . . ?
O8 W4 Cs1 51.5(4) . . ?
O7 W4 Cs1 139.79(11) . . ?
O6 W4 Cs1 132.5(4) . . ?
O17 W4 Cs1 97.6(4) 2_665 . ?
O5 W4 Cs6 71.3(6) . . ?
O4 W4 Cs6 107.5(5) . . ?
O8 W4 Cs6 162.5(4) . . ?
O7 W4 Cs6 77.6(3) . . ?
O6 W4 Cs6 31.9(4) . . ?
O17 W4 Cs6 103.5(4) 2_665 . ?
Cs1 W4 Cs6 138.59(18) . . ?
O15 W5 O14 100.2(6) . . ?
O15 W5 O16 101.0(7) . . ?
O14 W5 O16 88.4(7) . . ?
O15 W5 O6 99.1(7) . 2_665 ?
O14 W5 O6 87.1(6) . 2_665 ?
O16 W5 O6 159.9(6) . 2_665 ?
O15 W5 O3 100.2(6) . 2_665 ?
O14 W5 O3 159.6(6) . 2_665 ?
O16 W5 O3 89.0(7) . 2_665 ?
O6 W5 O3 88.5(6) 2_665 2_665 ?
O15 W5 O17 172.2(6) . . ?
O14 W5 O17 84.4(5) . . ?
O16 W5 O17 85.4(6) . . ?
O6 W5 O17 74.8(5) 2_665 . ?
O3 W5 O17 75.2(5) 2_665 . ?
O15 W5 Cs2 47.9(5) . . ?
O14 W5 Cs2 80.0(4) . . ?
O16 W5 Cs2 57.4(5) . . ?
O6 W5 Cs2 140.3(4) 2_665 . ?
O3 W5 Cs2 115.2(4) 2_665 . ?
O17 W5 Cs2 139.7(3) . . ?
O15 W5 Cs5 61.2(6) . 3_656 ?
O14 W5 Cs5 146.1(5) . 3_656 ?
O16 W5 Cs5 121.4(6) . 3_656 ?
O6 W5 Cs5 70.0(5) 2_665 3_656 ?
O3 W5 Cs5 48.0(6) 2_665 3_656 ?
O17 W5 Cs5 111.6(5) . 3_656 ?
Cs2 W5 Cs5 101.7(4) . 3_656 ?
O15 W5 Cs6 60.1(6) . 2_665 ?
O14 W5 Cs6 78.7(4) . 2_665 ?
O16 W5 Cs6 154.0(6) . 2_665 ?
O6 W5 Cs6 42.7(5) 2_665 2_665 ?
O3 W5 Cs6 110.8(5) 2_665 2_665 ?
O17 W5 Cs6 115.3(4) . 2_665 ?
Cs2 W5 Cs6 97.7(2) . 2_665 ?
Cs5 W5 Cs6 67.6(4) 3_656 2_665 ?
O15 W5 Cs2 82.0(5) . 5_766 ?
O14 W5 Cs2 139.1(4) . 5_766 ?
O16 W5 Cs2 51.6(5) . 5_766 ?
O6 W5 Cs2 133.3(4) 2_665 5_766 ?
O3 W5 Cs2 46.2(4) 2_665 5_766 ?
O17 W5 Cs2 98.7(3) . 5_766 ?
Cs2 W5 Cs2 71.48(15) . 5_766 ?
Cs5 W5 Cs2 70.2(4) 3_656 5_766 ?
Cs6 W5 Cs2 132.9(3) 2_665 5_766 ?

_refine_diff_density_max         4.450
_refine_diff_density_min         -2.609
_refine_diff_density_rms         0.523

_diffrn_radiation_probe          x-ray
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            AtlasS2

####################################################################### 
# 
# 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_DMA2
_database_code_depnum_ccdc_archive 'CCDC 1946815'
loop_
_audit_author_name
_audit_author_address
'Pavel Abramov'
;Nikolaev Institute of Inorganic Chemistry SB RAS
Russia
;
_audit_update_record             
;
2019-09-05 deposited with the CCDC.	2019-09-26 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT430_DMA2                
;
PROBLEM: Short Inter D...A Contact  O2W      ..O2W      .       2.71 Ang.
RESPONSE: H-bond
;
# Added during the CSD deposition process: Wednesday 04 September 2019 01:05 PM
# end Validation Reply Form

#complex ((CH3)2NH2)10[SbW17{Ru(NO)}O59].11H2O (analytical data)
#NO ligand was not localized
_audit_creation_method           SHELXL-2017/1
_shelx_SHELXL_version_number     2017/1
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C8 H24 N4 O62 Ru1.02 Sb W16.98'
_chemical_formula_weight         4514.94

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'
Sb Sb -0.5866 1.5461 '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'
Ru Ru -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      trigonal
_space_group_IT_number           166
_space_group_name_H-M_alt        'R -3 m'
_space_group_name_Hall           '-R 3 2'

_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'
'-y, x-y, z'
'-x+y, -x, z'
'y, x, -z'
'x-y, -y, -z'
'-x, -x+y, -z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'y+2/3, x+1/3, -z+1/3'
'x-y+2/3, -y+1/3, -z+1/3'
'-x+2/3, -x+y+1/3, -z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'y+1/3, x+2/3, -z+2/3'
'x-y+1/3, -y+2/3, -z+2/3'
'-x+1/3, -x+y+2/3, -z+2/3'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-y, -x, z'
'-x+y, y, z'
'x, x-y, z'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-y+2/3, -x+1/3, z+1/3'
'-x+y+2/3, y+1/3, z+1/3'
'x+2/3, x-y+1/3, z+1/3'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'
'-y+1/3, -x+2/3, z+2/3'
'-x+y+1/3, y+2/3, z+2/3'
'x+1/3, x-y+2/3, z+2/3'

_cell_length_a                   21.1706(14)
_cell_length_b                   21.1706(14)
_cell_length_c                   15.680(2)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     6086.0(11)
_cell_formula_units_Z            3
_cell_measurement_temperature    130(2)
_cell_measurement_reflns_used    2159
_cell_measurement_theta_min      2.5390
_cell_measurement_theta_max      28.2410

_exptl_crystal_description       polyhedra
_exptl_crystal_colour            red
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    3.696
_exptl_crystal_F_000             5845
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.273
_exptl_crystal_size_mid          0.227
_exptl_crystal_size_min          0.157
_exptl_absorpt_coefficient_mu    24.556
_shelx_estimated_absorpt_T_min   0.057
_shelx_estimated_absorpt_T_max   0.113
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_correction_T_min  0.965
_exptl_absorpt_correction_T_max  0.974

loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
6 14 -16 0.0641
4 0 22 0.0532
-8 -7 -19 0.0969
-18 -6 12 0.0974
2 -27 1 0.1439
-27 23 -6 0.1258
-19 28 7 0.1022
6 20 9 0.1143
29 -13 3 0.0608
26 -25 -3 0.1112

_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      130(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'sealed X-ray tube'
_diffrn_measurement_device_type  'New Xcalibur, AtlasS2'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 10.6168
_diffrn_reflns_number            5031
_diffrn_reflns_av_unetI/netI     0.0314
_diffrn_reflns_av_R_equivalents  0.0323
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         2.574
_diffrn_reflns_theta_max         25.670
_diffrn_reflns_theta_full        25.500
_diffrn_measured_fraction_theta_max 0.966
_diffrn_measured_fraction_theta_full 0.967
_diffrn_reflns_Laue_measured_fraction_max 0.966
_diffrn_reflns_Laue_measured_fraction_full 0.967
_diffrn_reflns_point_group_measured_fraction_max 0.966
_diffrn_reflns_point_group_measured_fraction_full 0.967
_reflns_number_total             1353
_reflns_number_gt                1079
_reflns_threshold_expression     >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       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_structure_solution    'SHELXS-2014 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_molecular_graphics    'ShelXle (Hübschle, 2011)'
_computing_publication_material  'CIFTAB-2014 (Sheldrick, 2014)'
_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)+(0.0415P)²+364.2240P] 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         1353
_refine_ls_number_parameters     92
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0579
_refine_ls_R_factor_gt           0.0418
_refine_ls_wR_factor_ref         0.1102
_refine_ls_wR_factor_gt          0.1046
_refine_ls_goodness_of_fit_ref   1.099
_refine_ls_restrained_S_all      1.099
_refine_ls_shift/su_max          0.000
_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
N1 N 0.755(2) 0.8774(12) 0.664(3) 0.094(12) Uiso 0.6 2 d S . P . .
C3 C 0.6948(19) 0.8474(10) 0.710(2) 0.051(9) Uiso 0.6 2 d S . P A .
H3A H 0.695129 0.883821 0.748644 0.076 Uiso 0.3 1 calc R U P . .
H3B H 0.691957 0.806811 0.742938 0.076 Uiso 0.3 1 calc R U P . .
H3C H 0.652441 0.829131 0.671842 0.076 Uiso 0.6 2 calc R U P . .
O1 O 0.3749(4) 0.6251(4) 0.3681(10) 0.053(4) Uani 1 2 d S T P . .
O2 O 0.4864(8) 0.7432(4) 0.2782(10) 0.067(4) Uani 1 2 d S T P . .
N2 N 0.666667 0.833333 0.333333 0.13(11) Uiso 0.1332 4 d S . P . .
O3 O 0.5090(6) 0.6903(6) 0.4299(7) 0.059(3) Uani 1 1 d . . . . .
O4 O 0.4233(7) 0.7116(3) 0.5246(9) 0.043(3) Uani 1 2 d S T P . .
O5 O 0.4225(3) 0.5775(3) 0.5323(10) 0.050(3) Uani 1 2 d S T P . .
O6 O 0.5564(7) 0.7782(3) 0.5661(9) 0.049(4) Uani 1 2 d S T P . .
O7 O 0.5738(5) 0.6573(6) 0.5605(7) 0.060(3) Uani 1 1 d . . . . .
O8 O 0.4728(6) 0.666667 0.666667 0.044(3) Uani 1 2 d S T P . .
O1W O 0.333333 0.666667 0.166667 0.06(2) Uiso 0.4 12 d S . P . .
O2W O 0.736(5) 0.730(5) 0.414(5) 0.06(2) Uiso 0.1333 1 d . . P . .
Sb1 Sb 0.333333 0.666667 0.5938(3) 0.0383(11) Uani 0.5 6 d S T P . .
W1 W 0.44984(5) 0.72492(2) 0.37793(7) 0.0542(3) Uani 1 2 d S T P . .
W2 W 0.50315(3) 0.67364(3) 0.55095(5) 0.0487(3) Uani 0.915 1 d . . P . .
Ru2 Ru 0.50315(3) 0.67364(3) 0.55095(5) 0.0487(3) Uani 0.085 1 d . . P . .
C2 C 0.759(5) 0.901(5) 0.582(5) 0.05(2) Uiso 0.15 1 d . . P A -1
H2A H 0.731317 0.859216 0.544671 0.069 Uiso 0.15 1 calc R U P A -1
H2B H 0.810587 0.926998 0.564200 0.069 Uiso 0.15 1 calc R U P A -1
H2C H 0.739657 0.934192 0.579055 0.069 Uiso 0.15 1 calc R U P A -1
C5 C 0.662(4) 0.780(4) 0.378(4) 0.059(19) Uiso 0.2168 1 d . . P B -1
H5A H 0.706566 0.797371 0.411890 0.088 Uiso 0.2168 1 calc R U P B -1
H5B H 0.655547 0.740689 0.340568 0.088 Uiso 0.2168 1 calc R U P B -1
H5C H 0.619937 0.762577 0.416800 0.088 Uiso 0.2168 1 calc R U P B -1


_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
N1 C3 1.31(5) . ?
N1 C2 1.36(8) . ?
C3 H3A 0.9800 . ?
C3 H3B 0.9800 . ?
C3 H3C 0.9800 . ?
C3 H3A 0.9800 24_565 ?
C3 H3B 0.9800 24_565 ?
C3 H3C 0.9800 24_565 ?
O1 W1 1.912(4) . ?
O1 W1 1.912(4) 3_565 ?
O2 W1 1.701(15) . ?
N2 C5 1.29(7) . ?
O3 W1 1.920(11) . ?
O3 W2 1.923(11) . ?
O4 Sb1 1.975(13) . ?
O4 W2 2.245(8) 24_565 ?
O4 W2 2.245(8) . ?
O4 W1 2.350(14) . ?
O5 W2 1.915(3) . ?
O5 W2 1.915(3) 22_665 ?
O6 W2 1.931(6) 24_565 ?
O6 W2 1.931(6) . ?
O7 W2 1.702(10) . ?
O8 W2 1.906(4) 11_566 ?
O8 W2 1.906(4) . ?
Sb1 Sb1 2.284(10) 25_566 ?
C2 H2A 0.9800 . ?
C2 H2B 0.9800 . ?
C2 H2C 0.9800 . ?
C5 H5A 0.9800 . ?
C5 H5B 0.9800 . ?
C5 H5C 0.9800 . ?

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
C3 N1 C2 124(5) . . ?
N1 C3 H3A 109.5 . . ?
N1 C3 H3B 109.5 . . ?
H3A C3 H3B 109.5 . . ?
N1 C3 H3C 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?
N1 C3 H3A 109.5(14) . 24_565 ?
H3A C3 H3A 103.1 . 24_565 ?
H3B C3 H3A 7.2 . 24_565 ?
H3C C3 H3A 115.6 . 24_565 ?
N1 C3 H3B 109.5(11) . 24_565 ?
H3A C3 H3B 7.2 . 24_565 ?
H3B C3 H3B 115.6 . 24_565 ?
H3C C3 H3B 103.1 . 24_565 ?
H3A C3 H3B 109.5 24_565 24_565 ?
N1 C3 H3C 109(2) . 24_565 ?
H3A C3 H3C 115.6 . 24_565 ?
H3B C3 H3C 103.1 . 24_565 ?
H3C C3 H3C 7.2 . 24_565 ?
H3A C3 H3C 109.5 24_565 24_565 ?
H3B C3 H3C 109.5 24_565 24_565 ?
W1 O1 W1 150.8(8) . 3_565 ?
W1 O3 W2 119.7(5) . . ?
Sb1 O4 W2 116.3(5) . 24_565 ?
Sb1 O4 W2 116.3(5) . . ?
W2 O4 W2 94.6(5) 24_565 . ?
Sb1 O4 W1 135.3(6) . . ?
W2 O4 W1 92.6(4) 24_565 . ?
W2 O4 W1 92.6(4) . . ?
W2 O5 W2 155.4(8) . 22_665 ?
W2 O6 W2 117.4(6) 24_565 . ?
W2 O8 W2 145.3(7) 11_566 . ?
O4 Sb1 O4 92.6(6) 3_565 . ?
O4 Sb1 O4 92.6(6) 3_565 2_665 ?
O4 Sb1 O4 92.6(6) . 2_665 ?
O4 Sb1 Sb1 123.4(4) 3_565 25_566 ?
O4 Sb1 Sb1 123.4(4) . 25_566 ?
O4 Sb1 Sb1 123.4(4) 2_665 25_566 ?
O2 W1 O1 102.1(6) . 2_665 ?
O2 W1 O1 102.1(6) . . ?
O1 W1 O1 87.4(8) 2_665 . ?
O2 W1 O3 99.7(5) . 24_565 ?
O1 W1 O3 87.2(5) 2_665 24_565 ?
O1 W1 O3 158.3(6) . 24_565 ?
O2 W1 O3 99.7(5) . . ?
O1 W1 O3 158.3(6) 2_665 . ?
O1 W1 O3 87.2(5) . . ?
O3 W1 O3 90.1(6) 24_565 . ?
O2 W1 O4 168.8(6) . . ?
O1 W1 O4 86.0(5) 2_665 . ?
O1 W1 O4 86.0(5) . . ?
O3 W1 O4 72.6(4) 24_565 . ?
O3 W1 O4 72.6(4) . . ?
O7 W2 O8 101.4(5) . . ?
O7 W2 O5 101.8(5) . . ?
O8 W2 O5 88.6(5) . . ?
O7 W2 O3 98.2(5) . . ?
O8 W2 O3 160.4(5) . . ?
O5 W2 O3 89.2(5) . . ?
O7 W2 O6 98.8(5) . . ?
O8 W2 O6 87.3(4) . . ?
O5 W2 O6 159.4(5) . . ?
O3 W2 O6 87.9(5) . . ?
O7 W2 O4 170.1(5) . . ?
O8 W2 O4 85.3(5) . . ?
O5 W2 O4 85.5(4) . . ?
O3 W2 O4 75.1(5) . . ?
O6 W2 O4 74.0(4) . . ?
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 . . ?
N2 C5 H5A 109.5 . . ?
N2 C5 H5B 109.5 . . ?
H5A C5 H5B 109.5 . . ?
N2 C5 H5C 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?

_refine_diff_density_max         1.675
_refine_diff_density_min         -2.406
_refine_diff_density_rms         0.276

_diffrn_radiation_probe          x-ray
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            AtlasS2

