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

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
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data_rot
_database_code_depnum_ccdc_archive 'CCDC 1569737'
_audit_update_record             
;
2018-07-03 deposited with the CCDC.
2018-10-09 downloaded from the CCDC.
;
_audit_creation_date             2017-08-09
_audit_creation_method           
;
Olex2 1.2
(compiled 2017.07.20 svn.r3457 for OlexSys, GUI svn.r5370)
;
_chemical_name_systematic        ?
_chemical_name_common            '(2, 3-DAP)-tri-manganese-18-tungstoantimonate'
_chemical_formula_moiety         
'H12 K4 Mn3 O74.5 Sb2 W19, 5.6(H2 O), 4(C12 H11 N4)'
_chemical_formula_sum            'C48 H67.20 K4 Mn3 N16 O80.10 Sb2 W19'
_chemical_formula_weight         6207.84
_exptl_crystal_recrystallization_method 
'Evaporation from aqueous buffer solution'
_chemical_melting_point          ?
_exptl_crystal_description       plate
_exptl_crystal_colour            'clear dark red'
_diffrn_ambient_temperature      200
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'
K K 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Mn Mn 0.3368 0.7283 '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'

_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.
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
_chemical_absolute_configuration ?
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   12.116(2)
_cell_length_b                   14.374(3)
_cell_length_c                   21.414(4)
_cell_angle_alpha                108.55(3)
_cell_angle_beta                 91.90(3)
_cell_angle_gamma                99.07(3)
_cell_volume                     3477.6(14)
_cell_formula_units_Z            1
_cell_measurement_reflns_used    ?
_cell_measurement_temperature    200
_cell_measurement_theta_max      ?
_cell_measurement_theta_min      ?
_shelx_estimated_absorpt_T_max   0.493
_shelx_estimated_absorpt_T_min   0.493
_exptl_absorpt_coefficient_mu    16.489
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details   ?
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    2.964
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_F_000             2767
_exptl_crystal_preparation       ?
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0688
_diffrn_reflns_av_unetI/netI     0.0980
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            37980
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.064
_diffrn_reflns_theta_min         2.075
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device_type  'Nonius Kappa'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'sealed x-ray tube'
_diffrn_source_type              'Incoatec IuS'
_diffrn_special_details          
'85 sec/frame ** 2 degree/frame ** 404 frames ** 35 mm distance to detector **'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                12262
_reflns_number_total             20123
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       ?
_computing_data_collection       ?
_computing_data_reduction        ?
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'SIR2004 (Burla et al., 2007)'
_refine_diff_density_max         3.181
_refine_diff_density_min         -2.688
_refine_diff_density_rms         0.337
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.017
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     800
_refine_ls_number_reflns         20123
_refine_ls_number_restraints     25
_refine_ls_R_factor_all          0.1026
_refine_ls_R_factor_gt           0.0553
_refine_ls_restrained_S_all      1.025
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0702P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1289
_refine_ls_wR_factor_ref         0.1451
_refine_special_details          
;_olex2_refinement_description
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups, All N(H,H) groups
 At 1.5 times of:
  All O(H,H) groups
2. Restrained distances
 H8B-H7B
 2.2 with sigma of 0.02
 H38A_$1-H37A
 2.2 with sigma of 0.02
 H3SB-O6
 2 with sigma of 0.02
 O12_$2-H2SA
 2.6 with sigma of 0.09
 O9_$2-H2SB
 2 with sigma of 0.04
 O3S_$3-H1SA
 2 with sigma of 0.1
 H1SB-O2S
 2.3 with sigma of 0.1
3. Uiso/Uaniso restraints and constraints
Uanis(Mn2) ∼ Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(K1) ∼ Ueq, Uanis(K2) ∼ Ueq: with sigma of 0.001 and sigma for
terminal atoms of 0.002
4. Others
 Fixed Sof: O22(0.5) O32(0.75) Mn2(0.5) W10(0.5) O1S(0.8) H1SA(0.8) H1SB(0.8)
5.a Free rotating group:
 O1S(H1SA,H1SB), O2S(H2SA,H2SB), O3S(H3SA,H3SB)
5.b Rotating group:
 O36(H36A,H36B), O37(H37A,H37B), O38(H38A,H38B)
5.c Aromatic/amide H refined with riding coordinates:
 N2(H2), C2(H2A), C3(H3), C4(H4), C5(H5), C8(H8), C11(H11), N6(H6), C14(H14),
 C15(H15), C16(H16), C17(H17), C20(H20), C23(H23)
5.d X=CH2 refined with riding coordinates:
 N3(H3A,H3B), N7(H7A,H7B), N8(H8A,H8B), N0AA(H0AA,H0AB)

_smtbx_masks_special_details      
loop_
  _smtbx_masks_void_nr
  _smtbx_masks_void_average_x
  _smtbx_masks_void_average_y
  _smtbx_masks_void_average_z
  _smtbx_masks_void_volume
  _smtbx_masks_void_count_electrons
  _smtbx_masks_void_content
 1 -0.507 0.000 0.500 696.8 100.6 ?
 2 0.471 0.299 0.968 10.5 3.5 ?
 3 0.529 0.701 0.032 10.5 2.7 ?,SQUEEZE
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
W1 W 0.47570(4) 0.43853(4) 0.17918(2) 0.03153(12) Uani 1 1 d . . . . .
W2 W 0.43511(4) 0.18310(4) 0.19290(2) 0.03077(12) Uani 1 1 d . . . . .
W3 W 0.40223(4) 0.15123(4) 0.33804(2) 0.03133(12) Uani 1 1 d . . . . .
W4 W 0.20419(3) 0.23319(4) 0.27183(2) 0.03093(12) Uani 1 1 d . . . . .
W5 W 0.24546(4) 0.48435(4) 0.25796(2) 0.03094(12) Uani 1 1 d . . . . .
W6 W 0.48908(4) 0.63783(4) 0.31279(2) 0.03237(12) Uani 1 1 d . . . . .
W7 W 0.72123(4) 0.49839(4) 0.29886(2) 0.03159(12) Uani 1 1 d . . . . .
W8 W 0.68092(4) 0.26920(4) 0.31320(2) 0.03096(12) Uani 1 1 d . . . . .
W9 W 0.69569(4) 0.47286(4) 0.45119(2) 0.03679(13) Uani 1 1 d . . . . .
Sb1 Sb 0.43494(5) 0.41613(5) 0.36031(3) 0.02348(16) Uani 1 1 d . . . . .
Mn11 Mn 0.90158(13) 0.56774(15) 0.60783(8) 0.0359(4) Uani 1 1 d . . . . .
K1 K 0.6748(2) 0.25149(19) 0.45936(12) 0.0329(5) Uani 1 1 d . U . . .
K2 K 0.75136(16) 0.68696(16) 0.43370(10) 0.0193(4) Uani 1 1 d . U . . .
O1 O 0.3906(5) 0.2774(5) 0.2968(3) 0.0254(16) Uani 1 1 d . . . . .
O2 O 0.5977(5) 0.4127(5) 0.3529(3) 0.0207(15) Uani 1 1 d . . . . .
O2AA O 0.7665(6) 0.1814(6) 0.2919(4) 0.042(2) Uani 1 1 d . . . . .
O3 O 0.4239(5) 0.4721(5) 0.2869(3) 0.0236(15) Uani 1 1 d . . . . .
O4 O 0.4406(6) 0.3025(6) 0.1715(3) 0.0311(18) Uani 1 1 d . . . . .
O5 O 0.3286(5) 0.4534(6) 0.1739(4) 0.0307(18) Uani 1 1 d . . . . .
O6 O 0.5183(6) 0.5813(6) 0.2197(4) 0.0351(18) Uani 1 1 d D . . . .
O7 O 0.6201(6) 0.4406(6) 0.2238(4) 0.0364(19) Uani 1 1 d . . . . .
O8 O 0.4322(6) 0.0959(6) 0.2454(4) 0.0364(19) Uani 1 1 d . . . . .
O9 O 0.2779(5) 0.1631(5) 0.1903(3) 0.0275(16) Uani 1 1 d D . . . .
O10 O 0.5861(6) 0.2361(6) 0.2353(3) 0.0354(19) Uani 1 1 d . . . . .
O11 O 0.5662(6) 0.2059(6) 0.3495(4) 0.0318(18) Uani 1 1 d . . . . .
O12 O 0.2483(6) 0.1296(6) 0.3062(4) 0.042(2) Uani 1 1 d D . . . .
O13 O 0.2168(6) 0.3419(6) 0.2379(4) 0.0325(18) Uani 1 1 d . . . . .
O14 O 0.3363(6) 0.6196(6) 0.2819(4) 0.041(2) Uani 1 1 d . . . . .
O15 O 0.6364(6) 0.6018(6) 0.3279(4) 0.0354(19) Uani 1 1 d . . . . .
O16 O 0.4612(7) 0.6381(6) 0.3973(4) 0.042(2) Uani 1 1 d . . . . .
O17 O 0.7856(6) 0.5336(6) 0.3910(4) 0.0359(19) Uani 1 1 d . . . . .
O18 O 0.7685(6) 0.3715(6) 0.2844(4) 0.0343(18) Uani 1 1 d . . . . .
O19 O 0.7517(6) 0.3447(6) 0.4009(4) 0.0334(18) Uani 1 1 d . . . . .
O20 O 0.6207(6) 0.5773(6) 0.4694(4) 0.039(2) Uani 1 1 d . . . . .
O21 O 0.5878(6) 0.3934(7) 0.4787(4) 0.041(2) Uani 1 1 d . . . . .
O22 O 0.6576(13) 0.7671(11) 0.4603(8) 0.035(4) Uiso 0.5 1 d . . P A .
O23 O 0.5121(6) 0.4310(7) 0.1011(4) 0.042(2) Uani 1 1 d . . . . .
O24 O 0.4591(7) 0.1018(6) 0.1181(4) 0.045(2) Uani 1 1 d . . . . .
O25 O 0.4035(8) 0.0457(7) 0.3606(5) 0.059(3) Uani 1 1 d . . . . .
O26 O 0.0688(6) 0.1743(6) 0.2375(4) 0.043(2) Uani 1 1 d . . . . .
O27 O 0.1258(6) 0.5002(6) 0.2186(4) 0.041(2) Uani 1 1 d . . . . .
O28 O 0.5293(8) 0.7642(7) 0.3225(5) 0.057(3) Uani 1 1 d . . . . .
O29 O 0.8332(6) 0.5554(7) 0.2698(4) 0.047(2) Uani 1 1 d . . . . .
O31 O 0.8025(6) 0.5111(6) 0.5154(4) 0.039(2) Uani 1 1 d . . . . .
O32 O 0.5615(12) 0.2036(11) 0.4913(6) 0.066(4) Uani 0.75 1 d . . P . .
O33 O 0.3916(6) 0.2502(7) 0.4169(4) 0.043(2) Uani 1 1 d . . . . .
O34 O 0.1842(6) 0.3115(6) 0.3536(4) 0.0362(19) Uani 1 1 d . . . . .
O35 O 0.2141(6) 0.5037(6) 0.3424(4) 0.0353(19) Uani 1 1 d . . . . .
O36 O 1.0149(6) 0.6358(7) 0.6987(4) 0.051(3) Uani 1 1 d . . . . .
H36A H 1.006072 0.700497 0.721915 0.077 Uiso 1 1 d GR . . . .
H36B H 1.089248 0.645684 0.689671 0.077 Uiso 1 1 d GR . . . .
O37 O 0.9880(7) 0.4390(7) 0.5792(4) 0.047(2) Uani 1 1 d . . . . .
H37A H 0.948008 0.380300 0.586275 0.070 Uiso 1 1 d DGR . . . .
H37B H 1.056626 0.448277 0.605970 0.070 Uiso 1 1 d GR . . . .
O38 O 1.0253(7) 0.6460(7) 0.5612(4) 0.047(2) Uani 1 1 d . . . . .
H38A H 1.008771 0.629116 0.514901 0.070 Uiso 1 1 d DGR . . . .
H38B H 1.097003 0.627810 0.562382 0.070 Uiso 1 1 d GR . . . .
Mn2 Mn 0.5624(3) 0.6832(3) 0.48393(19) 0.0115(8) Uani 0.5 1 d . U P A 1
W10 W 0.52089(13) 0.69623(11) 0.49293(7) 0.0468(3) Uani 0.5 1 d . . P A 2
O1S O 0.5560(12) 0.1191(9) -0.1340(8) 0.075(4) Uani 0.8 1 d . . P . .
H1SA H 0.554318 0.179260 -0.130989 0.112 Uiso 0.8 1 d DG . P . .
H1SB H 0.614375 0.106387 -0.153633 0.112 Uiso 0.8 1 d DG . P . .
O2S O 0.7916(11) 0.0497(8) -0.1538(6) 0.084(4) Uani 1 1 d D . . . .
H2SA H 0.817027 0.042324 -0.192326 0.126 Uiso 1 1 d DG . . . .
H2SB H 0.779439 -0.010171 -0.151201 0.126 Uiso 1 1 d DG . . . .
O3S O 0.4204(10) 0.6731(9) 0.1357(6) 0.070(3) Uani 1 1 d D . . . .
H3SA H 0.350271 0.671840 0.143345 0.105 Uiso 1 1 d G . . . .
H3SB H 0.445242 0.639123 0.158503 0.105 Uiso 1 1 d DG . . . .
N1 N 0.9237(9) 0.0851(7) -0.0307(5) 0.040(3) Uani 1 1 d . . . . .
N2 N 1.0139(8) 0.1527(7) 0.1000(5) 0.036(2) Uani 1 1 d . . . . .
H2 H 1.042148 0.172873 0.141450 0.043 Uiso 1 1 calc R . . . .
N3 N 0.6683(9) 0.0088(9) 0.1619(5) 0.055(3) Uani 1 1 d . . . . .
H3A H 0.695041 0.030811 0.203711 0.066 Uiso 1 1 calc R . . . .
H3B H 0.599915 -0.025880 0.150321 0.066 Uiso 1 1 calc R . . . .
C1 C 1.0315(9) 0.1373(8) -0.0146(6) 0.032(3) Uani 1 1 d . . . . .
C2 C 1.0992(11) 0.1588(10) -0.0620(6) 0.044(3) Uani 1 1 d . . . . .
H2A H 1.069835 0.137417 -0.106984 0.053 Uiso 1 1 calc R . . . .
C3 C 1.2043(10) 0.2089(8) -0.0447(7) 0.040(3) Uani 1 1 d . . . . .
H3 H 1.247938 0.221569 -0.078131 0.048 Uiso 1 1 calc R . . . .
C4 C 1.2533(10) 0.2439(9) 0.0216(6) 0.037(3) Uani 1 1 d . . . . .
H4 H 1.328590 0.278638 0.031862 0.045 Uiso 1 1 calc R . . . .
C5 C 1.1918(10) 0.2274(9) 0.0702(6) 0.039(3) Uani 1 1 d . . . . .
H5 H 1.223185 0.251887 0.114844 0.047 Uiso 1 1 calc R . . . .
C6 C 1.0794(10) 0.1730(8) 0.0536(6) 0.036(3) Uani 1 1 d . . . . .
C7 C 0.9087(10) 0.1036(8) 0.0847(6) 0.035(3) Uani 1 1 d . . . . .
C8 C 0.8419(10) 0.0835(9) 0.1324(5) 0.036(3) Uani 1 1 d . . . . .
H8 H 0.870075 0.107184 0.177612 0.043 Uiso 1 1 calc R . . . .
C9 C 0.7350(10) 0.0291(10) 0.1136(7) 0.048(3) Uani 1 1 d . . . . .
C10 C 0.6875(9) -0.0079(8) 0.0455(6) 0.030(2) Uani 1 1 d . . . . .
C11 C 0.7517(11) 0.0150(9) -0.0008(6) 0.045(3) Uani 1 1 d . . . . .
H11 H 0.720617 -0.004074 -0.045292 0.054 Uiso 1 1 calc R . . . .
C12 C 0.8638(10) 0.0668(8) 0.0166(6) 0.033(3) Uani 1 1 d . . . . .
N5 N 0.9200(7) 0.3369(7) -0.0368(4) 0.030(2) Uani 1 1 d . . . . .
N6 N 1.0300(7) 0.4050(7) 0.0879(5) 0.033(2) Uani 1 1 d . . . . .
H6 H 1.065377 0.425164 0.127714 0.039 Uiso 1 1 calc R . . . .
N7 N 1.2465(9) 0.4536(8) -0.1271(5) 0.045(3) Uani 1 1 d . . . . .
H7A H 1.211181 0.430080 -0.166977 0.054 Uiso 1 1 calc R . . . .
H7B H 1.317049 0.483570 -0.121208 0.054 Uiso 1 1 calc DR . . . .
N8 N 1.3605(7) 0.5277(8) 0.0038(5) 0.041(3) Uani 1 1 d . . . . .
H8A H 1.394508 0.550576 0.044022 0.049 Uiso 1 1 calc R . . . .
H8B H 1.396888 0.535434 -0.029642 0.049 Uiso 1 1 calc DR . . . .
C13 C 0.8676(9) 0.3233(8) 0.0147(5) 0.029(2) Uani 1 1 d . . . . .
C14 C 0.7539(9) 0.2723(9) 0.0076(6) 0.036(3) Uani 1 1 d . . . . .
H14 H 0.715636 0.245763 -0.035417 0.043 Uiso 1 1 calc R . . . .
C15 C 0.6992(10) 0.2601(8) 0.0579(6) 0.034(3) Uani 1 1 d . . . . .
H15 H 0.622607 0.228682 0.051167 0.041 Uiso 1 1 calc R . . . .
C16 C 0.7572(10) 0.2949(10) 0.1221(7) 0.048(3) Uani 1 1 d . . . . .
H16 H 0.719822 0.283703 0.158060 0.057 Uiso 1 1 calc R . . . .
C17 C 0.8644(10) 0.3435(8) 0.1328(6) 0.032(3) Uani 1 1 d . . . . .
H17 H 0.901319 0.368087 0.176255 0.039 Uiso 1 1 calc R . . . .
C18 C 0.9220(9) 0.3578(8) 0.0789(5) 0.027(2) Uani 1 1 d . . . . .
C19 C 1.0859(8) 0.4222(8) 0.0374(5) 0.025(2) Uani 1 1 d . . . . .
C20 C 1.1962(9) 0.4696(9) 0.0477(6) 0.032(3) Uani 1 1 d . . . . .
H20 H 1.233791 0.494236 0.090929 0.039 Uiso 1 1 calc R . . . .
C21 C 1.2528(9) 0.4810(9) -0.0067(6) 0.032(3) Uani 1 1 d . . . . .
C22 C 1.1907(9) 0.4436(8) -0.0732(5) 0.028(2) Uani 1 1 d . . . . .
C23 C 1.0836(9) 0.3984(8) -0.0811(6) 0.031(3) Uani 1 1 d . . . . .
H23 H 1.044760 0.374738 -0.123988 0.037 Uiso 1 1 calc R . . . .
C24 C 1.0263(9) 0.3848(8) -0.0270(5) 0.028(2) Uani 1 1 d . . . . .
N0AA N 0.5844(8) -0.0633(8) 0.0289(5) 0.045(3) Uani 1 1 d . . . . .
H0AA H 0.556238 -0.085897 -0.012614 0.054 Uiso 1 1 calc R . . . .
H0AB H 0.544822 -0.076983 0.059639 0.054 Uiso 1 1 calc R . . . .


_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
W10b K1 2.732(3) 2_666 ?
MN2a K1 3.312(4) 2_666 ?
W1 O3 2.330(7) . ?
W1 O4 1.887(8) . ?
W1 O5 1.832(7) . ?
W1 O6 1.932(8) . ?
W1 O7 1.957(7) . ?
W10b O21 1.945(8) 2_666 ?
MN2a O21 2.279(8) 2_666 ?
W1 O23 1.717(7) . ?
MN2a O32 2.336(15) 2_666 ?
W10b O32 1.830(15) 2_666 ?
W10b O33 2.027(8) 2_666 ?
MN2a O33 2.049(9) 2_666 ?
W2 O1 2.339(7) . ?
W2 O4 1.904(8) . ?
W2 O8 1.929(8) . ?
W2 O9 1.877(6) . ?
W2 O10 1.939(7) . ?
W2 O24 1.721(8) . ?
W3 K1 3.909(3) . ?
W3 O1 2.276(7) . ?
W3 O8 1.958(8) . ?
W3 O11 1.994(7) . ?
W3 O12 1.907(7) . ?
W3 O25 1.735(9) . ?
W3 O33 1.853(9) . ?
W4 O1 2.245(6) . ?
W4 O9 2.031(7) . ?
W4 O12 1.992(8) . ?
W4 O13 1.909(8) . ?
W4 O26 1.742(7) . ?
W4 O34 1.803(7) . ?
W5 O3 2.277(6) . ?
W5 O5 2.050(7) . ?
W5 O13 1.925(8) . ?
W5 O14 1.977(8) . ?
W5 O27 1.735(7) . ?
W5 O35 1.803(7) . ?
W6 O3 2.267(7) . ?
W6 O6 1.967(8) . ?
W6 O14 1.894(7) . ?
W6 O15 1.980(7) . ?
W6 O16 1.850(8) . ?
W6 O28 1.747(9) . ?
W7 O2 2.353(6) . ?
W7 O7 1.864(7) . ?
W7 O15 1.894(8) . ?
W7 O17 1.973(7) . ?
W7 O18 1.932(8) . ?
W7 O29 1.712(7) . ?
W8 O2 2.365(7) . ?
W8 O2AA 1.719(8) . ?
W8 O10 1.878(7) . ?
W8 O11 1.868(8) . ?
W8 O18 1.949(8) . ?
W8 O19 1.935(7) . ?
W9 O2 2.222(6) . ?
W9 O17 2.030(7) . ?
W9 O19 2.047(8) . ?
W9 O20 1.820(8) . ?
W9 O21 1.835(8) . ?
W9 O31 1.745(7) . ?
Sb1 O1 2.000(7) . ?
Sb1 O2 1.990(6) . ?
Sb1 O3 1.992(7) . ?
Mn11 O31 2.128(7) . ?
Mn11 O34 2.119(8) 2_666 ?
Mn11 O35 2.121(8) 2_666 ?
Mn11 O36 2.194(8) . ?
Mn11 O37 2.197(9) . ?
Mn11 O38 2.189(9) . ?
K1 O11 2.497(7) . ?
K1 O19 2.232(8) . ?
K1 O21 2.369(9) . ?
K1 O32 1.700(14) . ?
K1 Mn2 3.312(4) 2_666 ?
K1 W10 2.732(3) 2_666 ?
K2 O15 2.461(8) . ?
K2 O17 2.213(9) . ?
K2 O20 2.374(9) . ?
K2 O22 1.726(15) . ?
K2 Mn2 2.562(4) . ?
K2 W10 3.109(3) . ?
O16 Mn2 2.050(9) . ?
O16 W10 2.010(8) . ?
O20 Mn2 1.722(9) . ?
O20 W10 2.187(8) . ?
O21 Mn2 2.279(8) 2_666 ?
O21 W10 1.945(8) 2_666 ?
O22 Mn2 1.740(16) . ?
O22 W10 2.066(15) . ?
O32 Mn2 2.336(15) 2_666 ?
O32 W10 1.830(15) 2_666 ?
O33 Mn2 2.049(9) 2_666 ?
O33 W10 2.027(8) 2_666 ?
O34 Mn11 2.119(8) 2_666 ?
O35 Mn11 2.121(8) 2_666 ?
N1 C1 1.372(14) . ?
N1 C12 1.334(15) . ?
N2 C6 1.366(15) . ?
N2 C7 1.330(14) . ?
N3 C9 1.408(17) . ?
C1 C2 1.405(16) . ?
C1 C6 1.451(16) . ?
C2 C3 1.337(17) . ?
C3 C4 1.420(17) . ?
C4 C5 1.360(17) . ?
C5 C6 1.431(16) . ?
C7 C8 1.397(17) . ?
C7 C12 1.438(15) . ?
C8 C9 1.377(16) . ?
C9 C10 1.448(16) . ?
C10 C11 1.369(18) . ?
C10 N0AA 1.341(14) . ?
C11 C12 1.417(16) . ?
N5 C13 1.343(13) . ?
N5 C24 1.336(13) . ?
N6 C18 1.353(13) . ?
N6 C19 1.362(13) . ?
N7 C22 1.391(13) . ?
N8 C21 1.347(14) . ?
C13 C14 1.434(15) . ?
C13 C18 1.405(15) . ?
C14 C15 1.327(16) . ?
C15 C16 1.421(18) . ?
C16 C17 1.350(17) . ?
C17 C18 1.421(15) . ?
C19 C20 1.377(15) . ?
C19 C24 1.433(14) . ?
C20 C21 1.412(15) . ?
C21 C22 1.481(15) . ?
C22 C23 1.337(15) . ?
C23 C24 1.420(15) . ?

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
W10b K1 W3 62.44(6) 2_666 . ?
O4 W1 O3 86.5(3) . . ?
MN2a K1 W3 62.22(8) 2_666 . ?
MN2a O20 W9 173.6(6) . . ?
MN2a O20 K2 75.5(3) . . ?
W10b O20 K2 85.9(3) . . ?
MN2a O21 K1 90.9(3) 2_666 . ?
W10b O21 K1 77.9(3) 2_666 . ?
K1 W10b K2 166.06(9) 2_666 . ?
K2 MN2a K1 161.45(17) . 2_666 ?
O4 W1 O6 159.6(3) . . ?
O4 W1 O7 86.9(3) . . ?
O5 W1 O3 74.9(3) . . ?
O5 W1 O4 94.1(3) . . ?
O5 W1 O6 89.2(3) . . ?
O5 W1 O7 155.8(3) . . ?
O6 W1 O3 74.9(3) . . ?
O6 W1 O7 82.0(3) . . ?
O7 W1 O3 81.1(3) . . ?
O23 W1 O3 171.8(4) . . ?
O23 W1 O4 101.4(4) . . ?
O23 W1 O5 102.0(4) . . ?
O23 W1 O6 97.6(4) . . ?
O23 W1 O7 101.5(3) . . ?
O4 W2 O1 85.2(3) . . ?
O4 W2 O8 159.7(3) . . ?
O4 W2 O10 87.6(3) . . ?
O8 W2 O1 75.3(3) . . ?
O8 W2 O10 84.1(3) . . ?
O9 W2 O1 73.2(3) . . ?
O9 W2 O4 91.9(3) . . ?
O9 W2 O8 87.8(3) . . ?
O9 W2 O10 154.4(3) . . ?
O10 W2 O1 81.3(3) . . ?
O24 W2 O1 173.3(3) . . ?
O24 W2 O4 100.7(4) . . ?
O24 W2 O8 99.2(4) . . ?
O24 W2 O9 103.2(4) . . ?
O24 W2 O10 102.0(3) . . ?
O1 W3 K1 103.27(17) . . ?
O8 W3 K1 113.2(2) . . ?
O8 W3 O1 76.2(3) . . ?
O8 W3 O11 82.6(3) . . ?
O11 W3 K1 33.4(2) . . ?
O11 W3 O1 83.5(3) . . ?
O12 W3 K1 159.6(3) . . ?
O12 W3 O1 75.6(3) . . ?
O12 W3 O8 86.6(3) . . ?
O12 W3 O11 158.3(3) . . ?
O25 W3 K1 82.5(3) . . ?
O25 W3 O1 173.3(4) . . ?
O25 W3 O8 98.5(4) . . ?
O25 W3 O11 100.0(4) . . ?
O25 W3 O12 100.2(4) . . ?
O25 W3 O33 104.1(4) . . ?
O33 W3 K1 64.0(2) . . ?
O33 W3 O1 81.7(3) . . ?
O33 W3 O8 156.5(4) . . ?
O33 W3 O11 86.9(3) . . ?
O33 W3 O12 95.9(4) . . ?
O9 W4 O1 72.8(3) . . ?
O12 W4 O1 74.8(3) . . ?
O12 W4 O9 84.3(3) . . ?
O13 W4 O1 85.9(3) . . ?
O13 W4 O9 85.6(3) . . ?
O13 W4 O12 160.1(3) . . ?
O26 W4 O1 165.9(3) . . ?
O26 W4 O9 94.0(3) . . ?
O26 W4 O12 99.5(4) . . ?
O26 W4 O13 98.3(3) . . ?
O26 W4 O34 104.0(4) . . ?
O34 W4 O1 89.2(3) . . ?
O34 W4 O9 162.0(3) . . ?
O34 W4 O12 92.0(4) . . ?
O34 W4 O13 92.4(4) . . ?
O5 W5 O3 72.3(3) . . ?
O13 W5 O3 84.1(3) . . ?
O13 W5 O5 84.3(3) . . ?
O13 W5 O14 157.0(3) . . ?
O14 W5 O3 73.1(3) . . ?
O14 W5 O5 85.4(3) . . ?
O27 W5 O3 164.9(3) . . ?
O27 W5 O5 93.7(3) . . ?
O27 W5 O13 100.4(4) . . ?
O27 W5 O14 100.8(4) . . ?
O27 W5 O35 105.0(4) . . ?
O35 W5 O3 89.1(3) . . ?
O35 W5 O5 161.2(3) . . ?
O35 W5 O13 91.5(3) . . ?
O35 W5 O14 91.7(4) . . ?
O6 W6 O3 75.8(3) . . ?
O6 W6 O15 82.1(3) . . ?
O14 W6 O3 74.8(3) . . ?
O14 W6 O6 86.9(4) . . ?
O14 W6 O15 158.3(3) . . ?
O15 W6 O3 84.3(3) . . ?
O16 W6 O3 82.6(3) . . ?
O16 W6 O6 156.9(3) . . ?
O16 W6 O14 95.4(4) . . ?
O16 W6 O15 87.7(3) . . ?
O28 W6 O3 172.1(3) . . ?
O28 W6 O6 98.7(4) . . ?
O28 W6 O14 99.4(4) . . ?
O28 W6 O15 100.7(4) . . ?
O28 W6 O16 103.6(4) . . ?
O7 W7 O2 87.3(3) . . ?
O7 W7 O15 88.8(3) . . ?
O7 W7 O17 159.5(3) . . ?
O7 W7 O18 89.4(3) . . ?
O15 W7 O2 85.6(3) . . ?
O15 W7 O17 88.5(3) . . ?
O15 W7 O18 159.9(3) . . ?
O17 W7 O2 72.2(3) . . ?
O18 W7 O2 74.4(3) . . ?
O18 W7 O17 86.2(3) . . ?
O29 W7 O2 167.5(3) . . ?
O29 W7 O7 102.8(4) . . ?
O29 W7 O15 101.8(4) . . ?
O29 W7 O17 97.7(4) . . ?
O29 W7 O18 98.0(4) . . ?
O2AA W8 O2 168.2(3) . . ?
O2AA W8 O10 102.2(4) . . ?
O2AA W8 O11 101.5(4) . . ?
O2AA W8 O18 98.6(4) . . ?
O2AA W8 O19 98.4(4) . . ?
O10 W8 O2 86.7(3) . . ?
O10 W8 O18 87.2(3) . . ?
O10 W8 O19 159.1(3) . . ?
O11 W8 O2 86.2(3) . . ?
O11 W8 O10 89.2(3) . . ?
O11 W8 O18 159.9(3) . . ?
O11 W8 O19 90.3(3) . . ?
O16 MN2a K1 79.6(2) . 2_666 ?
O16 W10b K1 96.4(2) . 2_666 ?
O16 MN2a K2 97.6(3) . . ?
O18 W8 O2 73.8(3) . . ?
O19 W8 O2 72.5(3) . . ?
O19 W8 O18 86.2(3) . . ?
O17 W9 O2 74.1(3) . . ?
O17 W9 O19 85.1(3) . . ?
O19 W9 O2 73.7(3) . . ?
O20 W9 O2 87.4(3) . . ?
O20 W9 O17 87.8(4) . . ?
O20 W9 O19 161.1(3) . . ?
O20 W9 O21 94.4(4) . . ?
O21 W9 O2 86.6(3) . . ?
O21 W9 O17 160.6(3) . . ?
O21 W9 O19 86.7(4) . . ?
O31 W9 O2 164.4(3) . . ?
O31 W9 O17 95.0(3) . . ?
O31 W9 O19 94.6(3) . . ?
O31 W9 O20 103.5(4) . . ?
O31 W9 O21 103.2(4) . . ?
O2 Sb1 O1 92.4(3) . . ?
O2 Sb1 O3 92.7(3) . . ?
O3 Sb1 O1 90.8(3) . . ?
O31 Mn11 O36 174.2(4) . . ?
O31 Mn11 O37 90.4(3) . . ?
O31 Mn11 O38 87.8(3) . . ?
O34 Mn11 O31 94.3(3) 2_666 . ?
O34 Mn11 O35 83.3(3) 2_666 2_666 ?
O34 Mn11 O36 85.5(3) 2_666 . ?
O34 Mn11 O37 173.1(3) 2_666 . ?
O34 Mn11 O38 95.9(3) 2_666 . ?
O35 Mn11 O31 94.9(3) 2_666 . ?
O35 Mn11 O36 90.9(3) 2_666 . ?
O35 Mn11 O37 91.2(3) 2_666 . ?
O35 Mn11 O38 177.2(3) 2_666 . ?
O36 Mn11 O37 90.4(3) . . ?
O38 Mn11 O36 86.4(3) . . ?
O38 Mn11 O37 89.4(3) . . ?
O11 K1 W3 26.06(18) . . ?
O11 K1 Mn2 83.1(2) . 2_666 ?
O11 K1 W10 83.55(19) . 2_666 ?
O19 K1 W3 92.45(19) . . ?
O16 W10b K2 82.8(2) . . ?
O16 W10b O20 85.2(3) . . ?
O16 MN2a O21 83.9(3) . 2_666 ?
O16 W10b O22 86.0(5) . . ?
O16 MN2a O32 78.4(4) . 2_666 ?
O16 W10b O33 169.5(3) . 2_666 ?
O19 K1 O11 69.3(3) . . ?
O19 K1 O21 70.8(3) . . ?
O19 K1 Mn2 112.0(2) . 2_666 ?
O19 K1 W10 112.7(2) . 2_666 ?
O21 K1 W3 76.8(2) . . ?
O21 K1 O11 80.9(3) . . ?
O21 K1 Mn2 43.5(2) . 2_666 ?
O21 K1 W10 44.11(19) . 2_666 ?
O32 K1 W3 65.3(4) . . ?
O32 K1 O11 91.2(4) . . ?
O32 K1 O19 150.8(5) . . ?
O32 K1 O21 85.2(5) . . ?
O32 K1 Mn2 41.7(5) . 2_666 ?
O32 K1 W10 41.1(5) . 2_666 ?
O15 K2 Mn2 84.4(2) . . ?
O15 K2 W10 84.15(18) . . ?
O17 K2 O15 70.3(3) . . ?
O17 K2 O20 71.2(3) . . ?
O17 K2 Mn2 110.2(2) . . ?
O17 K2 W10 113.7(2) . . ?
O20 K2 O15 81.9(3) . . ?
O20 K2 Mn2 40.6(2) . . ?
O20 K2 W10 44.54(19) . . ?
O22 K2 O15 91.3(6) . . ?
O22 K2 O17 150.0(6) . . ?
O22 K2 O20 83.2(5) . . ?
O22 K2 Mn2 42.5(5) . . ?
O22 K2 W10 38.7(5) . . ?
W3 O1 W2 91.7(3) . . ?
W4 O1 W2 94.7(2) . . ?
W4 O1 W3 93.7(3) . . ?
Sb1 O1 W2 138.0(3) . . ?
Sb1 O1 W3 116.5(3) . . ?
Sb1 O1 W4 112.5(3) . . ?
W7 O2 W8 91.0(2) . . ?
W9 O2 W7 96.5(2) . . ?
W9 O2 W8 96.0(2) . . ?
Sb1 O2 W7 127.2(3) . . ?
Sb1 O2 W8 126.8(3) . . ?
Sb1 O2 W9 111.9(3) . . ?
W5 O3 W1 93.4(2) . . ?
W6 O3 W1 92.5(2) . . ?
W6 O3 W5 93.9(3) . . ?
Sb1 O3 W1 137.8(3) . . ?
Sb1 O3 W5 113.6(3) . . ?
Sb1 O3 W6 116.0(3) . . ?
W1 O4 W2 159.9(4) . . ?
W1 O5 W5 119.4(4) . . ?
W1 O6 W6 116.8(4) . . ?
W7 O7 W1 147.3(5) . . ?
W2 O8 W3 116.8(4) . . ?
W2 O9 W4 119.3(3) . . ?
W8 O10 W2 146.2(4) . . ?
W3 O11 K1 120.6(4) . . ?
W8 O11 W3 143.4(4) . . ?
W8 O11 K1 94.1(3) . . ?
W3 O12 W4 115.6(4) . . ?
W4 O13 W5 146.7(4) . . ?
W6 O14 W5 118.1(4) . . ?
W6 O15 K2 120.2(4) . . ?
W7 O15 W6 142.6(4) . . ?
W7 O15 K2 95.0(3) . . ?
W6 O16 Mn2 132.3(4) . . ?
W6 O16 W10 143.9(5) . . ?
W7 O17 W9 117.1(4) . . ?
W7 O17 K2 101.0(3) . . ?
W9 O17 K2 97.3(3) . . ?
W7 O18 W8 120.3(4) . . ?
W8 O19 W9 117.8(3) . . ?
W8 O19 K1 101.0(3) . . ?
W9 O19 K1 97.2(3) . . ?
W9 O20 K2 98.1(3) . . ?
W9 O20 W10 176.1(5) . . ?
W9 O21 K1 98.9(3) . . ?
W9 O21 Mn2 170.2(5) . 2_666 ?
W9 O21 W10 176.8(5) . 2_666 ?
K2 O22 Mn2 95.3(7) . . ?
K2 O22 W10 109.9(7) . . ?
W9 O31 Mn11 166.4(5) . . ?
K1 O32 Mn2 109.3(7) . 2_666 ?
K1 O32 W10 101.3(7) . 2_666 ?
W3 O33 Mn2 149.5(5) . 2_666 ?
W3 O33 W10 135.1(4) . 2_666 ?
W4 O34 Mn11 135.1(4) . 2_666 ?
W5 O35 Mn11 136.4(4) . 2_666 ?
C12 N1 C1 119.6(10) . . ?
C7 N2 C6 122.3(11) . . ?
N1 C1 C2 122.5(11) . . ?
N1 C1 C6 120.1(11) . . ?
C2 C1 C6 117.5(11) . . ?
C3 C2 C1 120.9(12) . . ?
C2 C3 C4 122.7(12) . . ?
C5 C4 C3 119.5(12) . . ?
C4 C5 C6 119.5(12) . . ?
N2 C6 C1 117.8(11) . . ?
N2 C6 C5 122.4(11) . . ?
C5 C6 C1 119.9(11) . . ?
N2 C7 C8 122.0(11) . . ?
N2 C7 C12 119.0(11) . . ?
C8 C7 C12 118.9(11) . . ?
O20 MN2a K1 134.6(3) . 2_666 ?
O20 W10b K1 144.3(2) . 2_666 ?
O20 MN2a K2 63.8(3) . . ?
O20 W10b K2 49.6(2) . . ?
O20 MN2a O16 97.4(4) . . ?
C9 C8 C7 119.8(11) . . ?
N3 C9 C10 118.2(11) . . ?
C8 C9 N3 119.4(12) . . ?
C8 C9 C10 122.4(13) . . ?
C11 C10 C9 117.7(11) . . ?
N0AA C10 C9 120.5(11) . . ?
N0AA C10 C11 121.8(11) . . ?
C10 C11 C12 121.1(11) . . ?
N1 C12 C7 121.2(11) . . ?
N1 C12 C11 118.8(11) . . ?
C11 C12 C7 120.0(11) . . ?
C24 N5 C13 119.5(10) . . ?
C18 N6 C19 122.3(10) . . ?
N5 C13 C14 122.3(10) . . ?
N5 C13 C18 121.6(10) . . ?
C18 C13 C14 116.1(10) . . ?
C15 C14 C13 123.6(12) . . ?
C14 C15 C16 118.8(12) . . ?
C17 C16 C15 121.1(12) . . ?
C16 C17 C18 119.7(11) . . ?
N6 C18 C13 118.2(10) . . ?
N6 C18 C17 121.2(10) . . ?
C13 C18 C17 120.6(10) . . ?
N6 C19 C20 121.2(10) . . ?
N6 C19 C24 116.9(9) . . ?
C20 C19 C24 121.9(10) . . ?
C19 C20 C21 119.3(11) . . ?
N8 C21 C20 118.9(10) . . ?
N8 C21 C22 122.1(9) . . ?
C20 C21 C22 118.9(10) . . ?
N7 C22 C21 119.1(10) . . ?
C23 C22 N7 120.8(10) . . ?
C23 C22 C21 120.0(9) . . ?
C22 C23 C24 121.6(11) . . ?
N5 C24 C19 121.4(10) . . ?
N5 C24 C23 120.3(10) . . ?
C23 C24 C19 118.3(10) . . ?
O20 MN2a O21 89.0(4) . 2_666 ?
O20 MN2a O22 105.9(6) . . ?
O20 MN2a O32 163.3(5) . 2_666 ?
O20 MN2a O33 100.0(4) . 2_666 ?
O21 MN2a K1 45.7(2) 2_666 2_666 ?
O21 W10b K1 58.0(3) 2_666 2_666 ?
O21 W10b K2 135.9(3) 2_666 . ?
O21 MN2a K2 152.8(3) 2_666 . ?
O21 W10b O16 94.3(3) 2_666 . ?
O21 W10b O20 86.3(4) 2_666 . ?
O21 W10b O22 167.3(5) 2_666 . ?
O21 MN2a O32 74.6(4) 2_666 2_666 ?
O21 W10b O33 91.9(3) 2_666 2_666 ?
O22 MN2a K1 119.4(5) . 2_666 ?
O22 W10b K1 134.7(4) . 2_666 ?
O22 W10b K2 31.5(4) . . ?
O22 MN2a K2 42.1(5) . . ?
O22 MN2a O16 94.0(6) . . ?
O22 W10b O20 81.0(5) . . ?
O22 MN2a O21 165.1(6) . 2_666 ?
O22 MN2a O32 90.5(6) . 2_666 ?
O22 MN2a O33 94.7(6) . 2_666 ?
O32 W10b K1 37.6(4) 2_666 2_666 ?
O32 MN2a K1 29.0(4) 2_666 2_666 ?
O32 MN2a K2 132.5(4) 2_666 . ?
O32 W10b K2 128.5(5) 2_666 . ?
O32 W10b O16 92.7(4) 2_666 . ?
O32 W10b O20 177.2(4) 2_666 . ?
O32 W10b O21 95.6(5) 2_666 2_666 ?
O32 W10b O22 97.1(6) 2_666 . ?
O32 W10b O33 95.1(4) 2_666 2_666 ?
O33 MN2a K1 78.1(2) 2_666 2_666 ?
O33 W10b K1 94.1(2) 2_666 2_666 ?
O33 W10b K2 86.8(2) 2_666 . ?
O33 MN2a K2 102.8(3) 2_666 . ?
O33 MN2a O16 157.5(4) 2_666 . ?
O33 W10b O20 86.8(3) 2_666 . ?
O33 MN2a O21 82.4(3) 2_666 2_666 ?
O33 W10b O22 86.1(5) 2_666 . ?
O33 MN2a O32 80.8(4) 2_666 2_666 ?



####################################################################### 
# 
# 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_et046_0m_a
_database_code_depnum_ccdc_archive 'CCDC 1569739'
_audit_update_record             
;
2018-07-03 deposited with the CCDC.
2018-10-09 downloaded from the CCDC.
;
_audit_creation_date             2017-08-16
_audit_creation_method           
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5375)
;
_chemical_name_systematic        ?
_chemical_name_common            '(2, 3-DAP)-di-zinc-18-tungstoantimonate'
_chemical_formula_moiety         
'H12 Na5 O83 Sb2 W19.89 Zn2.11, 4(C12 H10.25 N4)'
_chemical_formula_sum            'C48 H53 N16 Na5 O83 Sb2 W19.89 Zn2.11'
_chemical_formula_weight         6335.22
_exptl_crystal_recrystallization_method 'Evaporation from water buffer'
_chemical_melting_point          ?
_exptl_crystal_description       plate

_exptl_crystal_colour            'clear red'
_diffrn_ambient_temperature      200.0
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'
Na Na 0.0362 0.0249 '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'
Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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.
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
_chemical_absolute_configuration ?
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   12.6796(7)
_cell_length_b                   14.1057(7)
_cell_length_c                   20.5025(11)
_cell_angle_alpha                92.665(3)
_cell_angle_beta                 93.300(3)
_cell_angle_gamma                115.147(3)
_cell_volume                     3303.7(3)
_cell_formula_units_Z            1
_cell_measurement_reflns_used    9979
_cell_measurement_temperature    200.0
_cell_measurement_theta_max      30.522
_cell_measurement_theta_min      2.559
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    18.120
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.4500
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. 
wR2(int) was 0.1163 before and 0.0645 after correction. 
The Ratio of minimum to maximum transmission is 0.6031. 
The λ/2 correction factor is Not present.
;
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    3.184
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_F_000             2809
_exptl_crystal_preparation       ?
_exptl_crystal_size_max          0.125
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.01
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0519
_diffrn_reflns_av_unetI/netI     0.0431
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            65919
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.348
_diffrn_reflns_theta_min         2.115
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker X8 APEX'
_diffrn_measurement_method       ?
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'sealed x-ray tube'
_diffrn_source_type              'Incoatec IuS'
_diffrn_special_details          
'80 sec/frame ** 2 degree/frame ** 623 frames ** 40 mm distance to detector **'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                10072
_reflns_number_total             12045
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_refine_diff_density_max         3.724
_refine_diff_density_min         -1.822
_refine_diff_density_rms         0.322
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.018
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     798
_refine_ls_number_reflns         12045
_refine_ls_number_restraints     37
_refine_ls_R_factor_all          0.0519
_refine_ls_R_factor_gt           0.0403
_refine_ls_restrained_S_all      1.018
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0329P)²+128.4466P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0915
_refine_ls_wR_factor_ref         0.0956
_refine_special_details          
;1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups, All N(H,H) groups
 At 1.5 times of:
  All O(H,H) groups
2. Restrained distances
 O1AA-N6_$1
 3.1 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
Uanis(Na1) ∼ Ueq, Uanis(Na3) ∼ Ueq, Uanis(Na2) ∼ Ueq: with sigma of
0.05 and sigma for terminal atoms of 0.1
Uanis(O21) ∼ Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(O6AA) ∼ Ueq: with sigma of 0.5 and sigma for terminal atoms of 1
Uanis(O5AA) ∼ Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(O2) = Uanis(O3) = Uanis(O1)
Uanis(Zn10) = Uanis(W10)
Uanis(W11) = Uanis(Zn11)
Uanis(Zn11) = Uanis(W11)
4. Others
 Sof(Zn10)=1-FVAR(1)
 Sof(W10)=FVAR(1)
 Sof(Zn11)=1-FVAR(2)
 Sof(W11)=FVAR(2)
 Fixed Sof: Na1(0.75) Na2(0.75) H1(0.25) H6(0.25) O5AA(0.75) O6AA(0.75)
5.a Riding coordinates:
 O36(H36A,H36B), O37(H37), O37(H37A), O38(H38A,H38B)
5.b Aromatic/amide H refined with riding coordinates:
 N1(H1), C2(H2), C3(H3), C4(H4), C5(H5), C8(H8), C11(H11), N6(H6), C14(H14),
 C15(H15), C16(H16), C17(H17), C20(H20), C23(H23)
5.c X=CH2 refined with riding coordinates:
 N3(H3A,H3B), N4(H4A,H4B), N7(H7A,H7B), N8(H8A,H8B),SQUEEZE
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     heavy
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
W1 W 0.53236(4) 0.64990(4) 0.31070(2) 0.01310(11) Uani 1 1 d . . . . .
W2 W 0.61797(4) 0.42855(4) 0.30494(2) 0.01316(11) Uani 1 1 d . . . . .
W3 W 0.65726(4) 0.33588(4) 0.16330(2) 0.01341(11) Uani 1 1 d . . . . .
W4 W 0.84436(4) 0.57839(4) 0.22006(2) 0.01419(12) Uani 1 1 d . . . . .
W5 W 0.75702(4) 0.79322(4) 0.22547(2) 0.01437(12) Uani 1 1 d . . . . .
W6 W 0.48626(4) 0.75011(4) 0.17586(2) 0.01353(12) Uani 1 1 d . . . . .
W7 W 0.27680(4) 0.48124(4) 0.19842(2) 0.01463(12) Uani 1 1 d . . . . .
W8 W 0.35550(4) 0.28454(4) 0.19380(2) 0.01512(12) Uani 1 1 d . . . . .
W9 W 0.31321(4) 0.38395(4) 0.05202(2) 0.01616(12) Uani 1 1 d . . . . .
Sb1 Sb 0.58135(7) 0.54846(6) 0.13452(4) 0.00967(16) Uani 1 1 d . . . . .
Na1 Na 0.3608(6) 0.1777(5) 0.0587(3) 0.0183(14) Uani 0.75 1 d . U P A 1
Na2 Na 0.9568(6) 0.3762(7) 0.2113(4) 0.0338(19) Uani 0.75 1 d . U P B 1
Na3 Na 0.7853(4) 0.4484(4) -0.0633(2) 0.0145(10) Uani 1 1 d . U . A 1
O1 O 0.5847(7) 0.6534(6) 0.2052(4) 0.0114(10) Uani 1 1 d . . . . .
O2 O 0.6486(7) 0.4869(6) 0.2014(4) 0.0114(10) Uani 1 1 d . . . . .
O3 O 0.4172(7) 0.4474(6) 0.1481(4) 0.0114(10) Uani 1 1 d . . . . .
O0AA O 0.5961(7) 0.5534(7) 0.3240(4) 0.0172(19) Uani 1 1 d . . . . .
O1AA O 0.6809(7) 0.7640(7) 0.3126(4) 0.0150(18) Uani 1 1 d D . . . .
O2AA O 0.4707(7) 0.7412(7) 0.2680(4) 0.0169(19) Uani 1 1 d . . . . .
O7 O 0.3908(7) 0.5378(7) 0.2717(4) 0.0165(19) Uani 1 1 d . . . . .
O8 O 0.6400(7) 0.3208(7) 0.2565(4) 0.0161(18) Uani 1 1 d . . . . .
O9 O 0.7820(7) 0.5132(7) 0.3055(4) 0.0182(19) Uani 1 1 d . . . . .
O10 O 0.4598(7) 0.3614(7) 0.2696(4) 0.0147(18) Uani 1 1 d . . . . .
O11 O 0.8142(7) 0.4337(7) 0.1870(4) 0.0177(19) Uani 1 1 d . . . . .
O12 O 0.4862(7) 0.2756(7) 0.1602(4) 0.0176(19) Uani 1 1 d . . . . .
O13 O 0.8144(7) 0.6931(6) 0.2506(4) 0.0154(18) Uani 1 1 d . . . . .
O14 O 0.6459(8) 0.8502(7) 0.1982(4) 0.022(2) Uani 1 1 d . . . . .
O15 O 0.3481(7) 0.6175(7) 0.1662(4) 0.0180(19) Uani 1 1 d . . . . .
O16 O 0.2554(7) 0.3448(6) 0.2237(4) 0.0158(18) Uani 1 1 d . . . . .
O17 O 0.6441(7) 0.3880(7) 0.0830(4) 0.0191(19) Uani 1 1 d . . . . .
O18 O 0.8458(7) 0.6150(7) 0.1372(4) 0.0185(19) Uani 1 1 d . . . . .
O19 O 0.7892(8) 0.7807(7) 0.1429(4) 0.023(2) Uani 1 1 d . . . . .
O20 O 0.2754(7) 0.2605(7) 0.1092(4) 0.0156(18) Uani 1 1 d . . . . .
O21 O 0.2114(7) 0.4193(6) 0.1121(4) 0.0139(18) Uani 1 1 d . U . . .
O22 O 0.4331(8) 0.3582(7) 0.0254(4) 0.024(2) Uani 1 1 d . . . . .
O23 O 0.4917(8) 0.6645(7) 0.3872(4) 0.021(2) Uani 1 1 d . . . . .
O24 O 0.6104(8) 0.3846(7) 0.3813(4) 0.021(2) Uani 1 1 d . . . . .
O25 O 0.6802(9) 0.2271(7) 0.1424(5) 0.025(2) Uani 1 1 d . . . C 1
O26 O 0.9904(7) 0.6200(7) 0.2456(5) 0.023(2) Uani 1 1 d . . . . .
O27 O 0.8699(8) 0.9115(7) 0.2584(4) 0.022(2) Uani 1 1 d . . . . .
O28 O 0.4272(8) 0.8373(7) 0.1607(4) 0.023(2) Uani 1 1 d . . . . .
O29 O 0.1567(8) 0.4870(7) 0.2300(4) 0.022(2) Uani 1 1 d . . . . .
O30 O 0.2854(8) 0.1605(7) 0.2218(5) 0.025(2) Uani 1 1 d . . . . .
O31 O 0.2005(8) 0.3154(7) -0.0092(4) 0.020(2) Uani 1 1 d . . . . .
O32 O 0.3703(8) 0.5184(7) 0.0299(4) 0.020(2) Uani 1 1 d . . . . .
O33 O 0.4821(7) 0.2868(7) -0.0919(4) 0.0174(19) Uani 1 1 d . . . . .
O34 O 0.4936(9) 0.1904(8) 0.0197(5) 0.034(2) Uani 1 1 d . . . . .
O35 O 0.6992(9) 0.3214(8) -0.0315(5) 0.030(2) Uani 1 1 d . . . . .
O36 O 1.0330(10) 0.7129(10) 0.0533(6) 0.046(3) Uani 1 1 d . . . . .
H36A H 1.040277 0.730758 0.013165 0.069 Uiso 1 1 d R . . D 1
H36B H 1.000357 0.644518 0.049405 0.069 Uiso 1 1 d R . . D 1
O37 O 0.9692(11) 0.8914(9) 0.0463(6) 0.049(3) Uani 1 1 d . . . . .
H37 H 0.980341 0.946444 0.071865 0.073 Uiso 1 1 d R . . E 1
H37A H 0.913501 0.888944 0.018415 0.073 Uiso 1 1 d R . . F 2
O38 O 1.0343(10) 0.8340(9) 0.1709(6) 0.045(3) Uani 1 1 d . . . . .
H38A H 0.997948 0.830276 0.206115 0.067 Uiso 1 1 d R . . G 2
H38B H 1.067568 0.900676 0.165045 0.067 Uiso 1 1 d R . . G 2
W10 W 0.56752(9) 0.32224(8) -0.00583(5) 0.0186(3) Uani 0.782(5) 1 d . . P A 1
W11 W 0.920(3) 0.752(3) 0.0974(15) 0.0166(17) Uani 0.164(5) 1 d . . P H 1
Zn10 Zn 0.5383(12) 0.3256(11) 0.0033(6) 0.0186(3) Uani 0.218(5) 1 d . . P A 2
Zn11 Zn 0.9125(14) 0.7628(13) 0.0914(8) 0.0166(17) Uani 0.836(5) 1 d . . P H 2
N1 N 0.0208(9) 0.3719(8) 0.4324(5) 0.016(2) Uani 1 1 d . . . . .
H1 H -0.010871 0.366304 0.392210 0.019 Uiso 0.25 1 calc R . P . .
N2 N 0.1230(9) 0.3959(8) 0.5584(5) 0.015(2) Uani 1 1 d . . . . .
N3 N -0.2295(10) 0.3705(10) 0.6428(6) 0.028(3) Uani 1 1 d . . . . .
H3A H -0.198651 0.378713 0.683446 0.034 Uiso 1 1 calc R . . . .
H3B H -0.302157 0.361685 0.635089 0.034 Uiso 1 1 calc R . . . .
N4 N -0.3330(9) 0.3419(9) 0.5152(5) 0.021(2) Uani 1 1 d . . . . .
H4A H -0.366836 0.331539 0.475148 0.025 Uiso 1 1 calc R . . . .
H4B H -0.372629 0.341951 0.549037 0.025 Uiso 1 1 calc R . . . .
C1 C 0.1337(11) 0.3826(10) 0.4426(6) 0.017(3) Uani 1 1 d . . . . .
C2 C 0.1967(11) 0.3827(10) 0.3902(6) 0.019(3) Uani 1 1 d . . . . .
H2 H 0.161550 0.377114 0.347186 0.023 Uiso 1 1 calc R . . . .
C3 C 0.3081(13) 0.3905(11) 0.3978(7) 0.031(4) Uani 1 1 d . . . . .
H3 H 0.349517 0.388864 0.360946 0.037 Uiso 1 1 calc R . . . .
C4 C 0.3594(11) 0.4012(10) 0.4625(7) 0.022(3) Uani 1 1 d . . . . .
H4 H 0.436978 0.407556 0.468957 0.027 Uiso 1 1 calc R . . . .
C5 C 0.3005(11) 0.4025(10) 0.5158(7) 0.021(3) Uani 1 1 d . . . . .
H5 H 0.336160 0.408975 0.558828 0.025 Uiso 1 1 calc R . . . .
C6 C 0.1849(11) 0.3942(10) 0.5061(6) 0.018(3) Uani 1 1 d . . . . .
C7 C 0.0109(11) 0.3840(9) 0.5503(6) 0.015(3) Uani 1 1 d . . . . .
C8 C -0.0531(11) 0.3847(10) 0.6022(6) 0.019(3) Uani 1 1 d . . . . .
H8 H -0.017753 0.394677 0.645679 0.023 Uiso 1 1 calc R . . . .
C9 C -0.1657(11) 0.3713(10) 0.5928(6) 0.017(3) Uani 1 1 d . . . . .
C10 C -0.2207(11) 0.3576(10) 0.5247(7) 0.018(3) Uani 1 1 d . . . . .
C11 C -0.1557(11) 0.3581(10) 0.4730(6) 0.018(3) Uani 1 1 d . . . . .
H11 H -0.189622 0.350208 0.429439 0.022 Uiso 1 1 calc R . . . .
C12 C -0.0407(11) 0.3700(9) 0.4835(6) 0.015(3) Uani 1 1 d . . . . .
N5 N 0.0357(10) 0.1212(8) 0.4510(5) 0.021(2) Uani 1 1 d . . . . .
N6 N 0.1595(10) 0.1525(9) 0.5724(6) 0.025(3) Uani 1 1 d D . . . .
H6 H 0.199224 0.162836 0.610722 0.030 Uiso 0.25 1 calc R . P . .
N7 N -0.1647(12) 0.1513(10) 0.6767(6) 0.035(3) Uani 1 1 d . . . . .
H7A H -0.125061 0.162890 0.715138 0.042 Uiso 1 1 calc R . . . .
H7B H -0.237185 0.144348 0.674103 0.042 Uiso 1 1 calc R . . . .
N8 N -0.2924(10) 0.1134(9) 0.5546(6) 0.025(3) Uani 1 1 d . . . . .
H8A H -0.333079 0.101367 0.516424 0.030 Uiso 1 1 calc R . . . .
H8B H -0.324114 0.118532 0.590865 0.030 Uiso 1 1 calc R . . . .
C13 C 0.1481(12) 0.1285(10) 0.4558(7) 0.024(3) Uani 1 1 d . . . . .
C14 C 0.2023(13) 0.1234(11) 0.3984(7) 0.030(3) Uani 1 1 d . . . . .
H14 H 0.161791 0.114460 0.356446 0.036 Uiso 1 1 calc R . . . .
C15 C 0.3148(13) 0.1315(12) 0.4038(9) 0.039(4) Uani 1 1 d . . . . .
H15 H 0.350961 0.128596 0.364871 0.046 Uiso 1 1 calc R . . . .
C16 C 0.3764(14) 0.1435(12) 0.4631(9) 0.037(4) Uani 1 1 d . . . . .
H16 H 0.453803 0.148898 0.464885 0.045 Uiso 1 1 calc R . . . .
C17 C 0.3249(12) 0.1477(11) 0.5210(7) 0.027(3) Uani 1 1 d . . . . .
H17 H 0.364989 0.152462 0.562432 0.032 Uiso 1 1 calc R . . . .
C18 C 0.2119(12) 0.1449(10) 0.5165(7) 0.021(3) Uani 1 1 d . . . . .
C19 C 0.0506(12) 0.1449(9) 0.5704(7) 0.020(3) Uani 1 1 d . . . . .
C20 C -0.0014(11) 0.1550(9) 0.6268(6) 0.018(3) Uani 1 1 d . . . . .
H20 H 0.041608 0.169483 0.668395 0.021 Uiso 1 1 calc R . . . .
C21 C -0.1152(13) 0.1441(10) 0.6225(7) 0.023(3) Uani 1 1 d . . . . .
C22 C -0.1818(12) 0.1241(10) 0.5575(6) 0.020(3) Uani 1 1 d . . . . .
C23 C -0.1284(11) 0.1169(9) 0.5026(6) 0.018(3) Uani 1 1 d . . . . .
H23 H -0.171357 0.104241 0.461120 0.021 Uiso 1 1 calc R . . . .
C24 C -0.0128(11) 0.1273(10) 0.5048(6) 0.017(3) Uani 1 1 d . . . . .
O3AA O 0.8983(10) 0.3696(9) 0.3131(5) 0.041(3) Uani 1 1 d . . . . .
O4AA O 0.8913(10) 0.4878(10) 0.0347(6) 0.049(3) Uani 1 1 d . . . . .
O5AA O 0.9664(14) 0.3532(14) 0.1020(9) 0.055(4) Uani 0.75 1 d . U P . .
O6AA O 0.2140(18) 0.0406(14) 0.0716(10) 0.078(7) Uani 0.75 1 d . U P . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
NA2a W7 3.712(7) 1_655 ?
NA3a W7 3.155(4) 2_665 ?
NA3a W9 3.114(5) 2_665 ?
W1 O1 2.295(8) . ?
W1 O0AA 1.877(9) . ?
W1 O1AA 1.884(8) . ?
W1 O2AA 1.979(8) . ?
W1 O7 1.915(8) . ?
NA2a O11 2.314(11) . ?
NA1a O12 2.501(11) . ?
NA3a O15 2.500(9) 2_665 ?
NA1a O20 2.168(11) . ?
NA3a O21 2.144(9) 2_665 ?
NA1a O22 2.458(11) . ?
W1 O23 1.708(9) . ?
NA2a O29 2.341(12) 1_655 ?
W11a O31 2.19(3) 2_665 ?
ZN11b O31 2.077(18) 2_665 ?
NA3a O32 2.342(10) 2_665 ?
W10a O32 2.135(9) 2_665 ?
ZN10b O32 2.170(16) 2_665 ?
NA1a O34 1.849(13) . ?
NA3a O35 1.832(11) . ?
NA1a W10 2.981(6) . ?
NA3a W10 2.927(5) . ?
NA2a O3AA 2.248(13) . ?
NA3a O4AA 2.258(13) . ?
NA2a O5AA 2.27(2) . ?
NA1a O6AA 2.078(19) . ?
W2 O2 2.306(8) . ?
W2 O0AA 1.922(9) . ?
W2 O8 1.904(8) . ?
W2 O9 1.907(8) . ?
W2 O10 1.898(8) . ?
W2 O24 1.704(8) . ?
W3 Na2 3.660(7) . ?
W3 O2 2.284(8) . ?
W3 O8 1.948(8) . ?
W3 O11 1.896(8) . ?
W3 O12 1.961(8) . ?
W3 O17 1.860(9) . ?
W3 O25 1.720(9) . ?
W4 Na2 3.692(8) . ?
W4 O2 2.257(8) . ?
W4 O9 2.056(9) . ?
W4 O11 1.987(9) . ?
W4 O13 1.899(9) . ?
W4 O18 1.798(8) . ?
W4 O26 1.727(9) . ?
W5 O1 2.235(8) . ?
W5 O1AA 2.055(9) . ?
W5 O13 1.921(8) . ?
W5 O14 1.964(9) . ?
W5 O19 1.782(9) . ?
W5 O27 1.745(9) . ?
W6 O1 2.284(8) . ?
W6 O2AA 1.914(8) . ?
W6 O14 1.924(9) . ?
W6 O15 1.936(9) . ?
W6 O28 1.721(8) . ?
W6 O33 1.890(9) 2_665 ?
W7 Na2 3.712(7) 1_455 ?
W7 Na3 3.155(4) 2_665 ?
W7 O3 2.313(8) . ?
W7 O7 1.909(8) . ?
W7 O15 1.912(9) . ?
W7 O16 1.926(8) . ?
W7 O21 1.912(8) . ?
W7 O29 1.720(9) . ?
W8 Na1 3.109(6) . ?
W8 O3 2.350(8) . ?
W8 O10 1.930(8) . ?
W8 O12 1.880(9) . ?
W8 O16 1.916(9) . ?
W8 O20 1.898(8) . ?
W8 O30 1.735(9) . ?
W9 Na1 3.220(7) . ?
W9 Na3 3.114(5) 2_665 ?
W9 O3 2.226(8) . ?
W9 O20 2.046(8) . ?
W9 O21 2.026(8) . ?
W9 O22 1.812(9) . ?
W9 O31 1.749(8) . ?
W9 O32 1.811(9) . ?
Sb1 O1 2.009(8) . ?
Sb1 O2 1.992(8) . ?
Sb1 O3 2.006(8) . ?
O15 Na3 2.500(9) 2_665 ?
O17 W10 1.999(9) . ?
O17 Zn10 1.965(16) . ?
O18 W11 1.99(3) . ?
O18 Zn11 2.172(16) . ?
O19 W11 2.12(4) . ?
O19 Zn11 2.03(2) . ?
O21 Na3 2.144(9) 2_665 ?
O22 W10 2.099(9) . ?
O22 Zn10 1.664(16) . ?
O29 Na2 2.341(12) 1_455 ?
O31 W11 2.19(3) 2_665 ?
O31 Zn11 2.077(18) 2_665 ?
O32 Na3 2.342(10) 2_665 ?
O32 W10 2.135(9) 2_665 ?
O32 Zn10 2.170(16) 2_665 ?
O33 W6 1.890(9) 2_665 ?
O33 W10 1.942(8) . ?
O33 Zn10 2.005(15) . ?
O34 W10 1.810(11) . ?
O34 Zn10 1.799(17) . ?
O35 W10 1.784(11) . ?
O35 Zn10 2.223(17) . ?
O36 W11 1.99(4) . ?
O36 Zn11 2.11(2) . ?
O37 W11 2.14(3) . ?
O37 Zn11 1.946(18) . ?
O38 W11 1.97(3) . ?
O38 Zn11 2.071(19) . ?
N1 C1 1.377(16) . ?
N1 C12 1.337(16) . ?
N2 C6 1.369(16) . ?
N2 C7 1.358(16) . ?
N3 C9 1.339(16) . ?
N4 C10 1.345(16) . ?
C1 C2 1.374(18) . ?
C1 C6 1.392(18) . ?
C2 C3 1.37(2) . ?
C3 C4 1.416(19) . ?
C4 C5 1.362(19) . ?
C5 C6 1.420(18) . ?
C7 C8 1.379(18) . ?
C7 C12 1.450(16) . ?
C8 C9 1.359(18) . ?
C9 C10 1.491(17) . ?
C10 C11 1.377(18) . ?
C11 C12 1.397(18) . ?
N5 C13 1.382(18) . ?
N5 C24 1.310(17) . ?
N6 C18 1.379(18) . ?
N6 C19 1.337(18) . ?
N7 C21 1.327(18) . ?
N8 C22 1.342(17) . ?
C13 C14 1.41(2) . ?
C13 C18 1.397(19) . ?
C14 C15 1.38(2) . ?
C15 C16 1.37(2) . ?
C16 C17 1.40(2) . ?
C17 C18 1.414(19) . ?
C19 C20 1.395(19) . ?
C19 C24 1.480(17) . ?
C20 C21 1.38(2) . ?
C21 C22 1.483(18) . ?
C22 C23 1.367(19) . ?
C23 C24 1.408(18) . ?

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
O0AA W1 O1 87.4(3) . . ?
O0AA W1 O1AA 92.8(4) . . ?
O0AA W1 O2AA 162.1(3) . . ?
W10a NA3a W7 108.68(14) . 2_665 ?
W10a NA1a W8 108.76(19) . . ?
W10a NA1a W9 78.08(15) . . ?
O0AA W1 O7 89.6(4) . . ?
O1AA W1 O1 74.6(3) . . ?
O1AA W1 O2AA 86.5(3) . . ?
O1AA W1 O7 156.6(4) . . ?
O2AA W1 O1 75.2(3) . . ?
O7 W1 O1 82.3(3) . . ?
O7 W1 O2AA 84.2(3) . . ?
O23 W1 O1 171.3(4) . . ?
O23 W1 O0AA 100.9(4) . . ?
O23 W1 O1AA 102.1(4) . . ?
O23 W1 O2AA 96.7(4) . . ?
W10a NA3a W9 81.47(12) . 2_665 ?
NA3a W10a Na1 172.80(16) . . ?
O25a W3 Na2 67.8(4) . . ?
O25a W3 O2 172.0(4) . . ?
O25a W3 O8 100.0(4) . . ?
O25a W3 O11 99.1(4) . . ?
O25a W3 O12 101.7(4) . . ?
O25a W3 O17 103.5(4) . . ?
NA3a W7 Na2 83.29(14) 2_665 1_455 ?
NA3a W9 Na1 166.13(15) 2_665 . ?
ZN10b O22 W9 175.6(8) . . ?
W10a O22 Na1 81.3(3) . . ?
W10a O32 Na3 81.5(3) 2_665 2_665 ?
W10a O34 Na1 109.1(6) . . ?
W10a O35 Na3 108.1(5) . . ?
W3 NA2a W4 53.88(10) . . ?
W3 NA2a W7 155.8(2) . 1_655 ?
W4 NA2a W7 114.4(2) . 1_655 ?
W8 NA1a W9 64.90(13) . . ?
W9 NA3a W7 65.24(9) 2_665 2_665 ?
O23 W1 O7 100.2(4) . . ?
O0AA W2 O2 84.4(3) . . ?
O8 W2 O2 76.0(3) . . ?
O8 W2 O0AA 160.2(3) . . ?
O8 W2 O9 87.9(4) . . ?
O9 W2 O2 74.0(3) . . ?
O9 W2 O0AA 89.3(4) . . ?
O10 W2 O2 82.9(3) . . ?
O10 W2 O0AA 88.4(4) . . ?
O10 W2 O8 86.5(4) . . ?
O10 W2 O9 156.8(3) . . ?
O24 W2 O2 173.4(4) . . ?
O11 NA2a W3 26.5(2) . . ?
O11 NA2a W4 28.3(2) . . ?
O11 NA2a W7 135.5(4) . 1_655 ?
O24 W2 O0AA 99.6(4) . . ?
O11 NA2a O29 124.2(5) . 1_655 ?
O12 NA1a W8 37.2(2) . . ?
O24 W2 O8 100.2(4) . . ?
O24 W2 O9 100.6(4) . . ?
O24 W2 O10 102.5(4) . . ?
O2 W3 Na2 104.8(2) . . ?
O8 W3 Na2 82.9(3) . . ?
O8 W3 O2 75.8(3) . . ?
O8 W3 O12 81.4(4) . . ?
O11 W3 Na2 33.0(3) . . ?
O11 W3 O2 74.2(3) . . ?
O11 W3 O8 87.3(4) . . ?
O11 W3 O12 157.7(4) . . ?
O12 W3 Na2 159.2(3) . . ?
O12 W3 O2 84.4(3) . . ?
O17 W3 Na2 112.4(3) . . ?
O17 W3 O2 81.7(3) . . ?
O17 W3 O8 155.5(4) . . ?
O17 W3 O11 95.8(4) . . ?
O17 W3 O12 87.0(4) . . ?
O2 W4 Na2 104.4(2) . . ?
O9 W4 Na2 83.5(3) . . ?
O9 W4 O2 72.5(3) . . ?
O11 W4 Na2 33.6(3) . . ?
O11 W4 O2 73.2(3) . . ?
O11 W4 O9 85.7(4) . . ?
O13 W4 Na2 161.9(3) . . ?
O13 W4 O2 86.5(3) . . ?
O13 W4 O9 86.1(4) . . ?
O13 W4 O11 159.6(3) . . ?
O18 W4 Na2 103.2(3) . . ?
O18 W4 O2 87.8(3) . . ?
O18 W4 O9 160.2(4) . . ?
O18 W4 O11 89.9(4) . . ?
O18 W4 O13 91.5(4) . . ?
O26 W4 Na2 63.8(3) . . ?
O26 W4 O2 164.7(4) . . ?
O26 W4 O9 95.7(4) . . ?
O26 W4 O11 96.8(4) . . ?
O26 W4 O13 102.6(4) . . ?
O26 W4 O18 104.0(4) . . ?
O1AA W5 O1 73.0(3) . . ?
O13 W5 O1 84.9(3) . . ?
O13 W5 O1AA 83.8(3) . . ?
O13 W5 O14 159.5(4) . . ?
O14 W5 O1 74.8(3) . . ?
O14 W5 O1AA 87.9(4) . . ?
O19 W5 O1 90.3(4) . . ?
O19 W5 O1AA 162.9(4) . . ?
O19 W5 O13 91.2(4) . . ?
O19 W5 O14 91.4(4) . . ?
O27 W5 O1 163.5(4) . . ?
O27 W5 O1AA 92.6(4) . . ?
O27 W5 O13 101.9(4) . . ?
O27 W5 O14 97.1(4) . . ?
O27 W5 O19 104.4(4) . . ?
O2AA W6 O1 76.6(3) . . ?
O2AA W6 O14 87.2(4) . . ?
O2AA W6 O15 85.2(4) . . ?
O14 W6 O1 74.3(3) . . ?
O14 W6 O15 159.7(3) . . ?
O15 W6 O1 85.6(3) . . ?
O28 W6 O1 171.9(4) . . ?
O28 W6 O2AA 99.9(4) . . ?
O28 W6 O14 98.3(4) . . ?
O28 W6 O15 101.5(4) . . ?
O28 W6 O33 103.4(4) . 2_665 ?
O33 W6 O1 80.7(3) 2_665 . ?
O33 W6 O2AA 156.4(4) 2_665 . ?
O33 W6 O14 93.0(4) 2_665 . ?
O33 W6 O15 86.6(4) 2_665 . ?
O3 W7 Na2 142.6(2) . 1_455 ?
O3 W7 Na3 87.7(2) . 2_665 ?
O7 W7 Na2 123.8(3) . 1_455 ?
O7 W7 Na3 138.7(3) . 2_665 ?
O7 W7 O3 85.6(3) . . ?
O7 W7 O15 86.4(4) . . ?
O7 W7 O16 86.5(4) . . ?
O7 W7 O21 158.4(4) . . ?
O15 W7 Na2 115.4(3) . 1_455 ?
O15 W7 Na3 52.4(3) . 2_665 ?
O15 W7 O3 86.1(3) . . ?
O15 W7 O16 160.3(4) . . ?
O16 W7 Na2 83.7(3) . 1_455 ?
O16 W7 Na3 130.6(3) . 2_665 ?
O16 W7 O3 75.0(3) . . ?
O21 W7 Na2 76.5(3) . 1_455 ?
O21 W7 Na3 41.7(3) . 2_665 ?
O21 W7 O3 72.8(3) . . ?
O21 W7 O15 90.9(4) . . ?
O21 W7 O16 88.9(3) . . ?
O29 W7 Na2 28.2(3) . 1_455 ?
O29 W7 Na3 90.8(3) . 2_665 ?
O29 W7 O3 170.8(4) . . ?
O29 W7 O7 101.4(4) . . ?
O29 W7 O15 100.2(4) . . ?
O29 W7 O16 99.3(4) . . ?
O29 W7 O21 100.2(4) . . ?
O3 W8 Na1 90.2(2) . . ?
O10 W8 Na1 139.7(3) . . ?
O10 W8 O3 86.2(3) . . ?
O12 W8 Na1 53.5(3) . . ?
O12 W8 O3 86.6(3) . . ?
O12 W8 O10 86.2(4) . . ?
O12 W8 O16 159.7(4) . . ?
O12 W8 O20 92.5(4) . . ?
O16 W8 Na1 131.6(3) . . ?
O16 W8 O3 74.3(3) . . ?
O16 W8 O10 85.7(3) . . ?
O20 W8 Na1 43.4(3) . . ?
O20 W8 O3 72.4(3) . . ?
O20 W8 O10 158.6(4) . . ?
O20 W8 O16 88.3(4) . . ?
O30 W8 Na1 88.5(3) . . ?
O30 W8 O3 169.8(4) . . ?
O30 W8 O10 101.3(4) . . ?
O30 W8 O12 100.7(4) . . ?
O30 W8 O16 99.2(4) . . ?
O30 W8 O20 99.9(4) . . ?
O3 W9 Na1 89.6(2) . . ?
O3 W9 Na3 90.2(2) . 2_665 ?
O20 W9 Na1 41.6(3) . . ?
O20 W9 Na3 125.7(3) . 2_665 ?
O20 W9 O3 72.7(3) . . ?
O21 W9 Na1 124.1(3) . . ?
O21 W9 Na3 43.2(2) . 2_665 ?
O21 W9 O3 72.8(3) . . ?
O21 W9 O20 82.6(3) . . ?
O22 W9 Na1 49.3(3) . . ?
O22 W9 Na3 144.5(3) . 2_665 ?
O22 W9 O3 87.8(4) . . ?
O22 W9 O20 87.3(4) . . ?
O22 W9 O21 160.0(4) . . ?
O31 W9 Na1 88.5(3) . . ?
O31 W9 Na3 87.8(3) . 2_665 ?
O31 W9 O3 163.8(4) . . ?
O31 W9 O20 95.5(4) . . ?
O31 W9 O21 95.1(4) . . ?
O31 W9 O22 103.0(4) . . ?
O31 W9 O32 103.6(4) . . ?
O32 W9 Na1 145.4(3) . . ?
O32 W9 Na3 48.4(3) . 2_665 ?
O32 W9 O3 86.9(3) . . ?
O32 W9 O20 159.2(4) . . ?
O32 W9 O21 87.5(4) . . ?
O32 W9 O22 96.2(4) . . ?
O2 Sb1 O1 88.4(3) . . ?
O2 Sb1 O3 92.2(3) . . ?
O3 Sb1 O1 93.0(3) . . ?
W5 O1 W1 95.6(3) . . ?
W5 O1 W6 94.2(3) . . ?
W6 O1 W1 92.1(3) . . ?
Sb1 O1 W1 136.7(4) . . ?
Sb1 O1 W5 114.5(4) . . ?
Sb1 O1 W6 114.6(3) . . ?
W3 O2 W2 91.2(3) . . ?
W4 O2 W2 96.0(3) . . ?
W4 O2 W3 94.4(3) . . ?
Sb1 O2 W2 139.9(4) . . ?
Sb1 O2 W3 113.5(3) . . ?
Sb1 O2 W4 112.1(4) . . ?
W7 O3 W8 90.9(3) . . ?
W9 O3 W7 96.2(3) . . ?
W9 O3 W8 95.8(3) . . ?
Sb1 O3 W7 128.2(4) . . ?
Sb1 O3 W8 127.6(4) . . ?
Sb1 O3 W9 110.3(3) . . ?
W1 O0AA W2 155.8(5) . . ?
W1 O1AA W5 116.8(4) . . ?
W6 O2AA W1 115.7(4) . . ?
W7 O7 W1 148.5(5) . . ?
W2 O8 W3 116.7(4) . . ?
W2 O9 W4 117.6(4) . . ?
W2 O10 W8 145.3(5) . . ?
W3 O11 W4 118.2(4) . . ?
W3 O11 Na2 120.5(5) . . ?
W4 O11 Na2 118.1(4) . . ?
W3 O12 Na1 121.4(4) . . ?
W8 O12 W3 146.4(5) . . ?
W8 O12 Na1 89.3(4) . . ?
W4 O13 W5 144.8(5) . . ?
W6 O14 W5 116.7(4) . . ?
W6 O15 Na3 123.3(4) . 2_665 ?
W7 O15 W6 144.0(5) . . ?
W7 O15 Na3 90.3(3) . 2_665 ?
W8 O16 W7 119.8(4) . . ?
W3 O17 W10 134.3(5) . . ?
W3 O17 Zn10 132.5(6) . . ?
W4 O18 W11 133.0(11) . . ?
W4 O18 Zn11 134.9(7) . . ?
W5 O19 W11 134.9(9) . . ?
W5 O19 Zn11 140.2(6) . . ?
W8 O20 W9 118.9(4) . . ?
W8 O20 Na1 99.5(4) . . ?
W9 O20 Na1 99.6(4) . . ?
W7 O21 W9 118.2(4) . . ?
W7 O21 Na3 101.9(4) . 2_665 ?
W9 O21 Na3 96.6(4) . 2_665 ?
W9 O22 Na1 96.7(4) . . ?
W9 O22 W10 177.8(5) . . ?
W7 O29 Na2 131.5(5) . 1_455 ?
W9 O31 W11 169.9(10) . 2_665 ?
W9 O31 Zn11 171.0(7) . 2_665 ?
W9 O32 Na3 96.3(4) . 2_665 ?
W9 O32 W10 177.8(5) . 2_665 ?
W9 O32 Zn10 170.4(6) . 2_665 ?
W6 O33 W10 134.2(5) 2_665 . ?
W6 O33 Zn10 147.0(6) 2_665 . ?
C12 N1 C1 119.9(10) . . ?
C7 N2 C6 121.8(10) . . ?
N1 C1 C6 120.1(12) . . ?
C2 C1 N1 120.2(12) . . ?
C2 C1 C6 119.7(12) . . ?
C3 C2 C1 122.5(13) . . ?
C2 C3 C4 117.6(14) . . ?
C5 C4 C3 121.8(13) . . ?
C4 C5 C6 119.0(13) . . ?
N2 C6 C1 119.8(12) . . ?
N2 C6 C5 120.8(12) . . ?
C1 C6 C5 119.4(12) . . ?
N2 C7 C8 122.7(11) . . ?
N2 C7 C12 117.0(11) . . ?
C8 C7 C12 120.3(11) . . ?
C9 C8 C7 121.5(11) . . ?
N3 C9 C8 122.2(12) . . ?
O12 NA1a W9 83.0(3) . . ?
O12 NA1a W10 82.2(3) . . ?
O15 NA3a W7 37.3(2) 2_665 2_665 ?
O15 NA3a W9 84.5(2) 2_665 2_665 ?
O15 NA3a W10 81.2(2) 2_665 . ?
O17 W10a Na1 88.4(3) . . ?
O17 W10a Na3 89.6(3) . . ?
O17 W10a O22 82.9(4) . . ?
O17 W10a O32 83.4(3) . 2_665 ?
O17 ZN10b O32 83.3(6) . 2_665 ?
O17 ZN10b O33 160.3(8) . . ?
O17 ZN10b O35 80.9(6) . . ?
O18 W11a O19 82.8(13) . . ?
O18 W11a O31 89.8(13) . 2_665 ?
O18 W11a O37 169.8(17) . . ?
O19 ZN11b O18 80.6(7) . . ?
O19 ZN11b O31 95.3(7) . 2_665 ?
O19 W11a O31 89.6(12) . 2_665 ?
O19 ZN11b O36 165.4(8) . . ?
O19 W11a O37 91.8(12) . . ?
O19 ZN11b O38 89.4(8) . . ?
O20 NA1a W8 37.0(2) . . ?
O20 NA1a W9 38.8(2) . . ?
O20 NA1a O12 71.2(3) . . ?
O20 NA1a O22 70.1(4) . . ?
O20 NA1a W10 112.3(3) . . ?
O21 NA3a W7 36.4(2) 2_665 2_665 ?
O21 NA3a W9 40.3(2) 2_665 2_665 ?
O21 NA3a O15 71.4(3) 2_665 2_665 ?
O21 NA3a O32 72.5(3) 2_665 2_665 ?
O21 NA3a W10 115.9(3) 2_665 . ?
O21 NA3a O4AA 115.3(4) 2_665 . ?
O22 NA1a W8 82.9(3) . . ?
O22 NA1a W9 34.0(2) . . ?
O22 W10a Na1 54.6(3) . . ?
O22 W10a Na3 131.9(3) . . ?
O22 NA1a O12 80.2(3) . . ?
O22 ZN10b O17 96.5(7) . . ?
O22 W10a O32 79.7(4) . 2_665 ?
O22 ZN10b O32 89.0(7) . 2_665 ?
O22 ZN10b O33 97.5(7) . . ?
O22 ZN10b O34 106.8(9) . . ?
O22 ZN10b O35 166.5(9) . . ?
O22 NA1a W10 44.1(2) . . ?
O29 NA2a W3 150.4(4) 1_655 . ?
O29 NA2a W4 98.4(3) 1_655 . ?
O29 NA2a W7 20.3(2) 1_655 1_655 ?
O31 ZN11b O18 88.2(7) 2_665 . ?
O31 ZN11b O36 87.6(8) 2_665 . ?
O32 NA3a W7 83.3(2) 2_665 2_665 ?
O32 NA3a W9 35.3(2) 2_665 2_665 ?
O32 W10a Na1 134.2(3) 2_665 . ?
O32 W10a Na3 52.3(3) 2_665 . ?
O32 NA3a O15 81.0(3) 2_665 2_665 ?
O32 ZN10b O35 77.6(6) 2_665 . ?
O32 NA3a W10 46.2(2) 2_665 . ?
O33 W10a Na1 92.9(3) . . ?
O33 W10a Na3 90.7(3) . . ?
O33 W10a O17 165.9(4) . . ?
O33 W10a O22 86.4(4) . . ?
O33 W10a O32 85.6(3) . 2_665 ?
O33 ZN10b O32 83.2(6) . 2_665 ?
O33 ZN10b O35 82.2(6) . . ?
O34 NA1a W8 125.9(4) . . ?
O34 NA1a W9 113.0(4) . . ?
O34 W10a Na1 35.9(4) . . ?
O34 W10a Na3 137.6(4) . . ?
O34 NA1a O12 89.3(4) . . ?
O34 W10a O17 95.4(4) . . ?
O34 ZN10b O17 97.0(7) . . ?
O34 NA1a O20 145.7(5) . . ?
O34 W10a O22 90.4(4) . . ?
O34 NA1a O22 79.1(4) . . ?
O34 W10a O32 170.1(4) . 2_665 ?
O34 ZN10b O32 164.0(9) . 2_665 ?
O34 W10a O33 93.9(4) . . ?
O34 ZN10b O33 92.1(7) . . ?
O34 ZN10b O35 86.7(7) . . ?
O34 NA1a W10 35.0(3) . . ?
O34 NA1a O6AA 127.8(7) . . ?
O35 NA3a W7 124.5(3) . 2_665 ?
O35 NA3a W9 116.8(4) . 2_665 ?
O35 W10a Na1 136.7(3) . . ?
O35 W10a Na3 36.5(3) . . ?
O35 NA3a O15 87.5(4) . 2_665 ?
O35 W10a O17 92.0(4) . . ?
O35 NA3a O21 148.5(4) . 2_665 ?
O35 W10a O22 167.7(4) . . ?
O35 W10a O32 88.7(4) . 2_665 ?
O35 NA3a O32 81.5(4) . 2_665 ?
O35 W10a O33 96.6(4) . . ?
O35 W10a O34 101.2(5) . . ?
O35 NA3a W10 35.4(3) . . ?
O35 NA3a O4AA 85.1(5) . . ?
O36 W11a O18 93.4(14) . . ?
O36 ZN11b O18 85.3(7) . . ?
O36 W11a O19 175.3(19) . . ?
O36 W11a O31 87.6(14) . 2_665 ?
O36 W11a O37 91.5(14) . . ?
O37 ZN11b O18 177.2(11) . . ?
O37 ZN11b O19 100.5(8) . . ?
O37 W11a O31 81.5(10) . 2_665 ?
O37 ZN11b O31 89.2(7) . 2_665 ?
O37 ZN11b O36 93.8(9) . . ?
O37 ZN11b O38 92.2(8) . . ?
O38 W11a O18 99.0(13) . . ?
O38 ZN11b O18 90.4(6) . . ?
O38 W11a O19 89.7(14) . . ?
O38 W11a O31 171.0(16) . 2_665 ?
O38 ZN11b O31 174.8(10) . 2_665 ?
O38 ZN11b O36 87.3(7) . . ?
O38 W11a O36 93.6(14) . . ?
O38 W11a O37 89.6(14) . . ?
N3 C9 C10 118.5(12) . . ?
C8 C9 C10 119.3(11) . . ?
N4 C10 C9 119.4(12) . . ?
N4 C10 C11 121.8(12) . . ?
C11 C10 C9 118.7(11) . . ?
C10 C11 C12 121.3(11) . . ?
N1 C12 C7 121.3(11) . . ?
N1 C12 C11 119.8(11) . . ?
C11 C12 C7 118.8(12) . . ?
C24 N5 C13 118.9(11) . . ?
C19 N6 C18 122.4(12) . . ?
N5 C13 C14 119.7(13) . . ?
N5 C13 C18 121.6(13) . . ?
C18 C13 C14 118.7(13) . . ?
C15 C14 C13 119.2(14) . . ?
C16 C15 C14 122.5(15) . . ?
C15 C16 C17 119.7(14) . . ?
C16 C17 C18 118.7(13) . . ?
N6 C18 C13 118.4(12) . . ?
N6 C18 C17 120.5(12) . . ?
C13 C18 C17 121.0(13) . . ?
N6 C19 C20 122.4(12) . . ?
N6 C19 C24 116.9(12) . . ?
C20 C19 C24 120.8(12) . . ?
C21 C20 C19 120.3(12) . . ?
N7 C21 C20 119.7(13) . . ?
N7 C21 C22 120.2(13) . . ?
C20 C21 C22 120.0(13) . . ?
N8 C22 C21 118.9(12) . . ?
N8 C22 C23 122.3(12) . . ?
C23 C22 C21 118.8(12) . . ?
C22 C23 C24 123.0(12) . . ?
N5 C24 C19 121.9(12) . . ?
N5 C24 C23 121.2(11) . . ?
C23 C24 C19 117.0(12) . . ?
O3AA NA2a W3 83.4(3) . . ?
O3AA NA2a W4 76.7(4) . . ?
O3AA NA2a W7 116.4(4) . 1_655 ?
O3AA NA2a O11 84.2(4) . . ?
O3AA NA2a O29 101.7(5) . 1_655 ?
O3AA NA2a O5AA 165.1(6) . . ?
O4AA NA3a W7 150.0(4) . 2_665 ?
O4AA NA3a W9 98.6(3) . 2_665 ?
O4AA NA3a O15 172.6(4) . 2_665 ?
O4AA NA3a O32 97.7(4) . 2_665 ?
O4AA NA3a W10 92.6(3) . . ?
O5AA NA2a W3 84.0(4) . . ?
O5AA NA2a W4 101.9(5) . . ?
O5AA NA2a W7 77.9(4) . 1_655 ?
O5AA NA2a O11 88.0(5) . . ?
O5AA NA2a O29 93.2(6) . 1_655 ?
O6AA NA1a W8 93.5(5) . . ?
O6AA NA1a W9 114.6(7) . . ?
O6AA NA1a O12 116.4(7) . . ?
O6AA NA1a O20 86.6(6) . . ?
O6AA NA1a O22 145.8(8) . . ?
O6AA NA1a W10 157.7(5) . . ?



####################################################################### 
# 
# 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_mo_eltacd6_p-1_a_final
_database_code_depnum_ccdc_archive 'CCDC 1849600'
_audit_update_record             
;
2018-06-15 deposited with the CCDC.
2018-10-09 downloaded from the CCDC.
;
_audit_creation_date             2018-06-15
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2016/4
_chemical_name_systematic        
'Di-cadmium-di-manganese octadecatungstoantimonate'
_chemical_name_common            Krebs-Cadmium-tungstoantimonate
_chemical_formula_moiety         
'Cd2 Cl Mn2 Na6 O89.5 Sb2 W18, 4(H2 O), 2(C4 H12 N)'
_chemical_formula_sum            'C8 H32 Cd2 Cl Mn2 N2 Na6 O93.50 Sb2 W18'
_chemical_formula_weight         5713.22
_exptl_crystal_recrystallization_method 'Evaporation of aqueous buffer solution'
_chemical_melting_point          ?
_exptl_crystal_description       block
_exptl_crystal_colour            orange
_diffrn_ambient_temperature      101.85
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'
Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Mn Mn 0.3368 0.7283 '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'
Na Na 0.0362 0.0249 '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'

_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.
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   12.3753(7)
_cell_length_b                   13.6520(8)
_cell_length_c                   17.0910(10)
_cell_angle_alpha                70.120(2)
_cell_angle_beta                 83.879(2)
_cell_angle_gamma                65.614(2)
_cell_volume                     2471.2(3)
_cell_formula_units_Z            1
_cell_measurement_reflns_used    9965
_cell_measurement_temperature    102(2)
_cell_measurement_theta_max      30.119
_cell_measurement_theta_min      2.54
_shelx_estimated_absorpt_T_max   0.456
_shelx_estimated_absorpt_T_min   0.036
_exptl_absorpt_coefficient_mu    22.216
_exptl_absorpt_correction_T_max  0.0082
_exptl_absorpt_correction_T_min  0.0003
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. 
wR2(int) was 0.1194 before and 0.0588 after correction. 
The Ratio of minimum to maximum transmission is 0.0366. 
The λ/2 correction factor is Not present.
;
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    3.839
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_F_000             2505
_exptl_crystal_size_max          0.451
_exptl_crystal_size_mid          0.136
_exptl_crystal_size_min          0.042
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0434
_diffrn_reflns_av_unetI/netI     0.0366
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            42040
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.350
_diffrn_reflns_theta_min         2.249
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Bruker D8 Venture'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'sealed x-ray tube'
_diffrn_source_type              'Incoatec IuS'
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                7844
_reflns_number_total             8983
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_collection       'APEX 3'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    ?
_refine_diff_density_max         3.967
_refine_diff_density_min         -1.826
_refine_diff_density_rms         0.656
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.109
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     675
_refine_ls_number_reflns         8983
_refine_ls_number_restraints     75
_refine_ls_R_factor_all          0.0713
_refine_ls_R_factor_gt           0.0652
_refine_ls_restrained_S_all      1.109
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1280P)²+11.0744P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1693
_refine_ls_wR_factor_ref         0.1780
_refine_special_details          
;_olex2_refinement_description

1. Fixed Uiso
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
2. Restrained distances
 H1SA-O15
 2 with sigma of 0.02
 O9-H1SB
 1.8 with sigma of 0.02
 H1B-H3B
 2.1 with sigma of 0.15
 Cd1-O51 ∼ Cd1-O24 ∼ Cd1-O37
 with sigma of 0.02
 Cd1-O51 ∼ Cd1-O37 ∼ Cd1-O24
 with sigma of 0.02
 N01N-C79 ∼ N01N-C6 ∼ N01N-C1 ∼ N01N-C5 ∼ N01N-C4 ∼ N01N-C3
∼ N01N-C2
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(O51) ∼ Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(W8) ∼ Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(O29) ∼ Ueq: with sigma of 0.0001 and sigma for terminal atoms of
0.0002
Uanis(O30) ∼ Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(O48) ∼ Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(W1) ∼ Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O32) ∼ Ueq, Uanis(O31) ∼ Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(O47) = Uanis(O46)
Uanis(Na3) = Uanis(Na4)
Uanis(O36) = Uanis(O38) = Uanis(O37)
Uanis(C2) = Uanis(C3)
Uanis(C4) = Uanis(C5)
Uanis(C6) = Uanis(C79)
4. Others
 Sof(C79)=Sof(H79A)=Sof(H79B)=Sof(H79C)=Sof(C2)=Sof(H2A)=Sof(H2B)=Sof(H2C)=
 Sof(C4)=Sof(H4A)=Sof(H4B)=Sof(H4C)=1-FVAR(1)
 Sof(C3)=Sof(H3A)=Sof(H3B)=Sof(H3C)=Sof(C5)=Sof(H5A)=Sof(H5B)=Sof(H5C)=Sof(C6)=
 Sof(H6A)=Sof(H6B)=Sof(H6C)=FVAR(1)
 Fixed Sof: O38(0.5) Cl1(0.5) Na4(0.5) O29(0.4) O32(0.5) O37(0.5) O46(0.8)
 O49(0.75) Na3(0.5) O28(0.6) O30(0.75) O31(0.5) O36(0.5) O47(0.2) O48(0.25)
 O51(0.5)
5.a Free rotating group:
 O1S(H1SA,H1SB), O2S(H2SA,H2SB)
5.b Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C3(H3A,H3B,H3C), C5(H5A,H5B,H5C), C79(H79A,H79B,H79C),
 C2(H2A,H2B,H2C), C4(H4A,H4B,H4C), C6(H6A,H6B,H6C)
_smtbx_masks_special_details       
loop_
  _smtbx_masks_void_nr
  _smtbx_masks_void_average_x
  _smtbx_masks_void_average_y
  _smtbx_masks_void_average_z
  _smtbx_masks_void_volume
  _smtbx_masks_void_count_electrons
  _smtbx_masks_void_content
 1 0.208 0.076 0.367 10.9 6.8 ?
 2 0.500 0.000 0.000 103.9 49.3 ?
 3 0.792 -0.076 0.633 10.9 6.8 ?,SQUEEZE
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
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
W2 W 0.25274(6) 0.66630(6) 0.62655(4) 0.04697(18) Uani 1 1 d . . . . .
W3 W 0.06648(6) 0.69305(6) 0.78636(4) 0.05095(19) Uani 1 1 d . . . . .
W9 W 0.34148(6) 0.52555(5) 1.11307(4) 0.04669(18) Uani 1 1 d . . . . .
Sb1 Sb 0.35667(9) 0.64765(8) 0.84810(6) 0.0426(2) Uani 1 1 d . . . . .
Cd1 Cd 0.54212(12) 0.68807(10) 1.00860(7) 0.0540(3) Uani 1 1 d D . . . .
Mn1 Mn 0.0514(2) 0.7473(2) 0.98523(14) 0.0511(5) Uani 1 1 d . . . . .
Na1 Na 0.1769(6) 0.7120(5) 0.3909(4) 0.0515(14) Uani 1 1 d . . . . .
Na2 Na -0.0098(6) 0.6493(5) 0.3220(4) 0.0505(13) Uani 1 1 d . . . . .
O1 O 0.3141(9) 0.8083(8) 0.7757(6) 0.046(2) Uani 1 1 d . . . . .
O2 O 0.2641(9) 0.6301(9) 0.7690(6) 0.046(2) Uani 1 1 d . . . . .
O3 O 0.5093(9) 0.5944(9) 0.7912(6) 0.044(2) Uani 1 1 d . . . . .
O4 O 0.6357(9) 0.5862(9) 0.6587(7) 0.048(2) Uani 1 1 d . . . . .
O5 O 0.4706(9) 0.7935(9) 0.6434(6) 0.049(2) Uani 1 1 d . . . . .
O6 O 0.2535(11) 0.8111(10) 0.6140(7) 0.052(2) Uani 1 1 d . . . . .
O7 O 0.4193(9) 0.5997(10) 0.6386(7) 0.049(2) Uani 1 1 d . . . . .
O8 O 0.2611(11) 0.5127(10) 0.6761(7) 0.053(3) Uani 1 1 d . . . . .
O9 O 0.0727(10) 0.8383(9) 0.7601(7) 0.050(2) Uani 1 1 d D . . . .
O10 O 0.1619(11) 0.9888(9) 0.6754(6) 0.056(3) Uani 1 1 d . . . . .
O11 O 0.3806(12) 0.9713(9) 0.6918(7) 0.056(3) Uani 1 1 d . . . . .
O12 O 0.5526(10) 0.7909(9) 0.7791(7) 0.050(2) Uani 1 1 d . . . . .
O13 O 0.4541(10) 0.4168(9) 0.7692(6) 0.046(2) Uani 1 1 d . . . . .
O14 O 0.1239(11) 0.5277(11) 0.8033(8) 0.061(3) Uani 1 1 d . . . . .
O15 O 0.0950(10) 0.7164(11) 0.6616(7) 0.054(3) Uani 1 1 d D . . . .
O16 O 0.2434(12) 0.9846(10) 0.8188(8) 0.063(3) Uani 1 1 d . . . . .
O17 O 0.7213(10) 0.5787(11) 0.7978(7) 0.055(3) Uani 1 1 d . . . . .
O18 O 0.6725(9) 0.4026(9) 0.7959(7) 0.049(2) Uani 1 1 d . . . . .
O19 O 0.6246(10) 0.3949(10) 0.6463(7) 0.052(2) Uani 1 1 d . . . . .
O20 O 0.3254(12) 0.4294(10) 0.9028(7) 0.057(3) Uani 1 1 d . . . . .
O21 O 0.2898(12) 0.3123(11) 0.8113(9) 0.065(3) Uani 1 1 d . . . . .
O22 O 0.0893(11) 0.6616(11) 0.8949(7) 0.057(3) Uani 1 1 d . . . . .
O23 O -0.0851(10) 0.7297(12) 0.7731(9) 0.065(3) Uani 1 1 d . . . . .
O24 O 0.4406(10) 0.5921(11) 1.0624(7) 0.057(3) Uani 1 1 d D . . . .
O25 O 0.2030(10) 0.6228(10) 1.0638(7) 0.054(3) Uani 1 1 d . . . . .
O26 O 0.3882(11) 0.4195(10) 1.0608(7) 0.056(3) Uani 1 1 d . . . . .
O27 O 0.1532(11) 0.8313(10) 0.9036(7) 0.054(3) Uani 1 1 d . . . . .
O33 O 0.0007(12) 1.0415(11) 0.7973(8) 0.066(3) Uani 1 1 d . . . . .
O34 O 0.2304(11) 0.6826(10) 0.5240(7) 0.055(3) Uani 1 1 d . . . . .
O35 O 0.7115(11) 0.7547(11) 0.6508(7) 0.059(3) Uani 1 1 d . . . . .
O38 O 0.875(3) 0.561(3) 0.987(2) 0.090(6) Uani 0.5 1 d . . P . .
O39 O 0.4190(11) 0.7928(10) 0.9156(7) 0.055(3) Uani 1 1 d . . . . .
O40 O 0.4648(12) 0.9875(10) 0.8304(8) 0.061(3) Uani 1 1 d . . . . .
O41 O 0.3036(12) 1.0032(11) 0.5350(8) 0.063(3) Uani 1 1 d . . . . .
O42 O 0.1732(18) 0.8980(13) 0.3300(11) 0.098(6) Uani 1 1 d . . . . .
O43 O 0.1241(9) 0.7297(9) 0.2576(7) 0.050(2) Uani 1 1 d . . . . .
O44 O -0.0345(10) 0.7733(10) 0.4031(7) 0.053(3) Uani 1 1 d . . . . .
O45 O 0.1571(10) 0.5298(10) 0.4195(7) 0.051(2) Uani 1 1 d . . . . .
O50 O 0.0437(11) 0.5382(10) 0.2309(7) 0.056(3) Uani 1 1 d . . . . .
W4 W 0.13266(6) 0.92576(5) 0.79824(4) 0.05132(19) Uani 1 1 d . . . A 1
W5 W 0.41042(6) 0.89882(5) 0.81161(4) 0.04979(19) Uani 1 1 d . . . B 1
W7 W 0.55843(6) 0.48128(6) 0.70683(4) 0.04705(18) Uani 1 1 d . . . C 1
W8 W 0.28801(6) 0.44440(5) 0.79699(4) 0.04702(18) Uani 1 1 d . U . D 1
Cl1 Cl 0.3783(8) 0.7465(8) 1.1347(6) 0.0596(19) Uani 0.5 1 d . . P E 1
Na4 Na 0.743(3) 0.704(3) 0.864(2) 0.059(5) Uani 0.5 1 d . . P B 1
O29 O -0.060(5) 0.659(4) 1.067(4) 0.060(4) Uani 0.4 1 d . U P F 1
O32 O 0.045(5) 0.870(4) 1.053(3) 0.105(14) Uani 0.5 1 d . U P F 1
O37 O 0.652(4) 0.780(4) 0.974(3) 0.090(6) Uani 0.5 1 d D . P B 1
O46 O -0.1068(14) 0.5300(11) 0.4057(9) 0.043(3) Uani 0.8 1 d . . P G 1
O49 O -0.1411(15) 0.7878(15) 0.2050(12) 0.057(4) Uani 0.75 1 d . . P G 1
W1 W 0.31131(6) 0.91099(5) 0.63514(4) 0.04975(19) Uani 1 1 d . U . H 2
W6 W 0.61362(6) 0.69931(6) 0.70918(4) 0.04799(18) Uani 1 1 d . . . B 2
Na3 Na 0.706(3) 0.696(3) 0.882(2) 0.059(5) Uani 0.5 1 d . . P B 2
O28 O -0.047(4) 0.670(6) 1.072(3) 0.15(2) Uani 0.6 1 d . . P F 2
O30 O -0.1197(19) 0.8832(18) 0.9226(13) 0.079(5) Uani 0.75 1 d . U P F 2
O31 O -0.001(2) 0.848(2) 1.0695(16) 0.046(5) Uani 0.5 1 d . U P F 2
O36 O 0.633(4) 0.758(4) 0.959(3) 0.090(6) Uani 0.5 1 d . . P B 2
O47 O -0.075(7) 0.485(5) 0.415(5) 0.043(3) Uani 0.2 1 d . . P G 2
O48 O -0.165(6) 0.779(5) 0.255(4) 0.066(13) Uani 0.25 1 d . U P G 2
O51 O 0.4474(19) 0.7855(18) 1.0857(13) 0.055(5) Uani 0.5 1 d D U P E 2
O1S O 0.0217(13) 0.9333(13) 0.6084(9) 0.075(4) Uani 1 1 d . . . . .
H1SA H 0.084160 0.874749 0.604321 0.112 Uiso 1 1 d DG . . . .
H1SB H -0.001398 0.919085 0.659371 0.112 Uiso 1 1 d DG . . . .
O2S O -0.0657(11) 0.6922(11) 0.5745(6) 0.052(3) Uani 1 1 d . . . . .
H2SA H -0.002906 0.668224 0.605775 0.079 Uiso 1 1 d G . . . .
H2SB H -0.123077 0.694637 0.609160 0.079 Uiso 1 1 d G . . . .
N01N N 0.5541(13) 0.7613(12) 0.4125(9) 0.063(4) Uani 1 1 d D . . . .
C1 C 0.561(2) 0.646(2) 0.4578(14) 0.087(7) Uani 1 1 d D . . . .
H1A H 0.552208 0.635647 0.517398 0.131 Uiso 1 1 calc GR . . . .
H1B H 0.638271 0.589739 0.449328 0.131 Uiso 1 1 calc DGR . . . .
H1C H 0.497546 0.634824 0.436995 0.131 Uiso 1 1 calc GR . . . .
C3 C 0.679(3) 0.744(5) 0.397(4) 0.080(9) Uani 0.37(3) 1 d D . P I 1
H3A H 0.704846 0.713874 0.350355 0.119 Uiso 0.37(3) 1 calc GR . P I 1
H3B H 0.728053 0.689111 0.446902 0.119 Uiso 0.37(3) 1 calc DGR . P I 1
H3C H 0.686336 0.816266 0.383132 0.119 Uiso 0.37(3) 1 calc GR . P I 1
C5 C 0.513(6) 0.798(5) 0.325(2) 0.083(9) Uani 0.37(3) 1 d D . P I 1
H5A H 0.578656 0.798801 0.288536 0.125 Uiso 0.37(3) 1 calc GR . P I 1
H5B H 0.448867 0.874568 0.310857 0.125 Uiso 0.37(3) 1 calc GR . P I 1
H5C H 0.482414 0.744940 0.319038 0.125 Uiso 0.37(3) 1 calc GR . P I 1
C79 C 0.450(3) 0.841(5) 0.441(3) 0.108(14) Uani 0.63(3) 1 d D . P I 1
H79A H 0.406957 0.799487 0.479881 0.163 Uiso 0.63(3) 1 calc GR . P I 1
H79B H 0.397028 0.897943 0.393302 0.163 Uiso 0.63(3) 1 calc GR . P I 1
H79C H 0.475559 0.879825 0.469657 0.163 Uiso 0.63(3) 1 calc GR . P I 1
C2 C 0.653(3) 0.767(3) 0.449(2) 0.080(9) Uani 0.63(3) 1 d D . P I 2
H2A H 0.662616 0.723189 0.508677 0.119 Uiso 0.63(3) 1 calc GR . P I 2
H2B H 0.635487 0.846519 0.441761 0.119 Uiso 0.63(3) 1 calc GR . P I 2
H2C H 0.726155 0.735117 0.421382 0.119 Uiso 0.63(3) 1 calc GR . P I 2
C4 C 0.611(4) 0.759(3) 0.3329(17) 0.083(9) Uani 0.63(3) 1 d D . P I 2
H4A H 0.695777 0.711122 0.343073 0.125 Uiso 0.63(3) 1 calc GR . P I 2
H4B H 0.599528 0.836713 0.298172 0.125 Uiso 0.63(3) 1 calc GR . P I 2
H4C H 0.574632 0.728349 0.304131 0.125 Uiso 0.63(3) 1 calc GR . P I 2
C6 C 0.445(6) 0.866(6) 0.392(6) 0.108(14) Uani 0.37(3) 1 d D . P I 2
H6A H 0.465465 0.932562 0.372985 0.163 Uiso 0.37(3) 1 calc GR . P I 2
H6B H 0.396869 0.868117 0.441166 0.163 Uiso 0.37(3) 1 calc GR . P I 2
H6C H 0.399137 0.868565 0.347250 0.163 Uiso 0.37(3) 1 calc GR . P I 2


_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
NA4a W9 3.58(3) 2_667 ?
NA3b W9 3.28(3) 2_667 ?
W2 O2 2.321(10) . ?
W2 O6 1.918(11) . ?
W2 O7 1.880(10) . ?
W2 O8 1.938(12) . ?
W2 O15 1.887(11) . ?
NA4a O23 2.57(2) 1_655 ?
NA4a O26 2.73(2) 2_667 ?
NA3b O26 2.24(3) 2_667 ?
W2 O34 1.727(10) . ?
NA4a O37 2.41(6) . ?
W6b Na3 3.25(4) . ?
NA3b O36 1.78(5) . ?
W3 O2 2.257(10) . ?
W3 O9 1.912(10) . ?
W3 O14 1.989(13) . ?
W3 O15 2.060(11) . ?
W3 O22 1.782(12) . ?
W3 O23 1.749(12) . ?
W9 O3 2.257(11) 2_667 ?
W9 O17 2.034(12) 2_667 ?
W9 O18 2.062(11) 2_667 ?
W9 O24 1.799(11) . ?
W9 O25 1.754(11) . ?
W9 O26 1.819(12) . ?
W9 Na4 3.58(3) 2_667 ?
W9 Na3 3.28(3) 2_667 ?
Sb1 O1 1.990(10) . ?
Sb1 O2 1.994(10) . ?
Sb1 O3 1.999(10) . ?
Cd1 O20 2.064(13) 2_667 ?
Cd1 O24 2.106(11) . ?
Cd1 O26 2.055(12) 2_667 ?
Cd1 O39 2.016(11) . ?
Cd1 Cl1 2.880(9) . ?
Cd1 Na4 3.33(2) . ?
Cd1 O37 2.125(18) . ?
Cd1 Na3 2.81(2) . ?
Cd1 O36 1.74(3) . ?
Cd1 O51 2.111(16) . ?
Mn1 O22 2.143(13) . ?
Mn1 O25 2.136(11) . ?
Mn1 O27 2.140(12) . ?
Mn1 O29 2.27(6) . ?
Mn1 O32 2.31(4) . ?
Mn1 O28 2.10(4) . ?
Mn1 O30 2.23(2) . ?
Mn1 O31 2.19(3) . ?
Na1 Na2 3.218(9) . ?
Na1 O19 2.429(13) 2_666 ?
Na1 O34 2.294(12) . ?
Na1 O42 2.377(16) . ?
Na1 O43 2.341(13) . ?
Na1 O44 2.405(13) . ?
Na1 O45 2.477(13) . ?
Na2 O43 2.335(12) . ?
Na2 O44 2.443(13) . ?
Na2 O45 2.410(13) . ?
Na2 O50 2.391(13) . ?
Na2 O46 2.410(16) . ?
Na2 O49 2.409(19) . ?
Na2 O47 2.64(7) . ?
Na2 O48 2.10(6) . ?
O1 W4 2.241(10) . ?
O1 W5 2.283(10) . ?
O1 W1 2.329(10) . ?
O2 W8 2.308(11) . ?
O3 W9 2.257(10) 2_667 ?
O3 W7 2.321(10) . ?
O3 W6 2.336(10) . ?
O4 W7 1.950(10) . ?
O4 W6 1.927(11) . ?
O5 W1 1.942(11) . ?
O5 W6 1.901(10) . ?
O6 W1 1.923(11) . ?
O7 W7 1.945(10) . ?
O8 W8 1.956(11) . ?
O9 W4 1.939(10) . ?
O10 W4 2.036(11) . ?
O10 W1 1.904(12) . ?
O11 W5 1.948(11) . ?
O11 W1 1.911(12) . ?
O12 W5 1.946(11) . ?
O12 Na4 2.52(4) . ?
O12 W6 1.898(10) . ?
O12 Na3 2.34(4) . ?
O13 W7 1.894(10) . ?
O13 W8 1.966(10) . ?
O14 W8 1.887(13) . ?
O16 W4 1.962(13) . ?
O16 W5 1.924(14) . ?
O17 W9 2.033(12) 2_667 ?
O17 Na4 2.46(4) . ?
O17 W6 1.924(11) . ?
O17 Na3 2.43(4) . ?
O18 W9 2.062(11) 2_667 ?
O18 W7 1.887(11) . ?
O19 Na1 2.429(13) 2_666 ?
O19 W7 1.727(10) . ?
O20 Cd1 2.064(12) 2_667 ?
O20 W8 1.837(11) . ?
O21 W8 1.726(11) . ?
O23 Na4 2.57(2) 1_455 ?
O26 Cd1 2.055(12) 2_667 ?
O26 Na4 2.73(2) 2_667 ?
O26 Na3 2.24(3) 2_667 ?
O27 W4 1.794(11) . ?
O33 W4 1.739(14) . ?
O35 W6 1.737(12) . ?
O38 Na4 2.48(5) . ?
O38 Na3 2.53(6) . ?
O39 W5 1.851(11) . ?
O40 W5 1.733(11) . ?
O41 W1 1.730(13) . ?
N01N C1 1.472(18) . ?
N01N C3 1.47(2) . ?
N01N C5 1.47(2) . ?
N01N C79 1.47(2) . ?
N01N C2 1.472(19) . ?
N01N C4 1.467(19) . ?
N01N C6 1.47(2) . ?

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
W6b NA3b W9 62.7(6) . 2_667 ?
O6 W2 O2 86.3(4) . . ?
O37a NA4a W9 106.6(8) . 2_667 ?
O36b NA3b W9 114.5(14) . 2_667 ?
O36b NA3b Cd1 36.5(11) . . ?
O37a NA4a Cd1 39.5(5) . . ?
O36b NA3b O12 100(2) . . ?
O37a NA4a O12 94.5(16) . . ?
O36b NA3b O17 149.8(16) . . ?
O37a NA4a O17 137.2(10) . . ?
O37a NA4a O23 129.2(14) . 1_655 ?
O36b NA3b O26 82.7(13) . 2_667 ?
O37a NA4a O26 77.1(8) . 2_667 ?
O36b NA3b O38 88(2) . . ?
O6 W2 O8 161.6(4) . . ?
O7 W2 O2 83.2(4) . . ?
O7 W2 O6 89.8(5) . . ?
O7 W2 O8 86.1(5) . . ?
O7 W2 O15 156.5(5) . . ?
O8 W2 O2 75.4(4) . . ?
O15 W2 O2 73.4(4) . . ?
O15 W2 O6 89.8(5) . . ?
O15 W2 O8 87.0(5) . . ?
O34 W2 O2 171.4(5) . . ?
O34 W2 O6 100.4(5) . . ?
O34 W2 O7 102.0(5) . . ?
O34 W2 O8 98.0(5) . . ?
O34 W2 O15 101.2(5) . . ?
O9 W3 O2 84.6(4) . . ?
O9 W3 O14 158.3(5) . . ?
O37a NA4a O38 77.9(17) . . ?
O36b NA3b W6 133(2) . . ?
O36b Cd1 O20 91.1(16) . 2_667 ?
O36b Cd1 O24 174.5(14) . . ?
O36b Cd1 O26 89.3(14) . 2_667 ?
O36b Cd1 O39 88.8(16) . . ?
O37a Cd1 Cl1 113.3(12) . . ?
O37a Cd1 Na4 46.2(14) . . ?
CL1a Cd1 Na4 159.0(6) . . ?
O36b Cd1 Na3 37.4(15) . . ?
O51b Cd1 Na3 137.9(10) . . ?
O36b Cd1 O51 100.9(15) . . ?
O28b Mn1 O22 103.1(17) . . ?
O28b Mn1 O25 85.9(16) . . ?
O28b Mn1 O27 175.5(16) . . ?
O29a Mn1 O32 101.4(18) . . ?
O31b Mn1 O30 80.0(8) . . ?
O28b Mn1 O30 88.2(17) . . ?
O28b Mn1 O31 77.8(19) . . ?
O49a Na2 Na1 119.2(5) . . ?
O46a Na2 Na1 125.4(4) . . ?
O48b Na2 Na1 120.4(14) . . ?
O47b Na2 Na1 121.7(16) . . ?
O48b Na2 O43 98.3(18) . . ?
O48b Na2 O44 86.2(16) . . ?
O46a Na2 O44 101.8(5) . . ?
O49a Na2 O44 98.6(6) . . ?
O48b Na2 O45 166.3(16) . . ?
O49a Na2 O45 165.4(6) . . ?
O48b Na2 O50 96.6(17) . . ?
O49a Na2 O46 108.1(6) . . ?
O48b Na2 O47 105(2) . . ?
W4a O1 W5 94.7(4) . . ?
O9 W3 O15 84.3(4) . . ?
O14 W3 O2 73.7(4) . . ?
O14 W3 O15 87.3(5) . . ?
O15 W3 O2 71.9(4) . . ?
O22 W3 O2 90.7(5) . . ?
O22 W3 O9 92.1(5) . . ?
O22 W3 O14 90.0(6) . . ?
O22 W3 O15 162.5(5) . . ?
O23 W3 O2 162.5(5) . . ?
O23 W3 O9 102.3(6) . . ?
O23 W3 O14 98.0(6) . . ?
O23 W3 O15 92.6(5) . . ?
O23 W3 O22 104.9(6) . . ?
O3 W9 Na4 89.4(7) 2_667 2_667 ?
O3 W9 Na3 87.7(7) 2_667 2_667 ?
O17 W9 O3 72.9(4) 2_667 2_667 ?
O17 W9 O18 83.2(5) 2_667 2_667 ?
O17 W9 Na4 41.4(6) 2_667 2_667 ?
O17 W9 Na3 47.7(6) 2_667 2_667 ?
O18 W9 O3 72.0(4) 2_667 2_667 ?
O18 W9 Na4 124.6(6) 2_667 2_667 ?
O18 W9 Na3 130.8(6) 2_667 2_667 ?
O24 W9 O3 86.4(5) . 2_667 ?
O24 W9 O17 159.0(5) . 2_667 ?
O24 W9 O18 87.3(5) . 2_667 ?
O24 W9 O26 96.5(6) . . ?
O24 W9 Na4 144.5(6) . 2_667 ?
O24 W9 Na3 136.8(6) . 2_667 ?
O25 W9 O3 163.8(5) . 2_667 ?
O25 W9 O17 96.0(5) . 2_667 ?
O25 W9 O18 95.5(5) . 2_667 ?
O25 W9 O24 103.5(5) . . ?
O25 W9 O26 102.6(5) . . ?
O25 W9 Na4 89.6(7) . 2_667 ?
O25 W9 Na3 93.3(8) . 2_667 ?
O26 W9 O3 88.6(4) . 2_667 ?
O26 W9 O17 86.5(5) . 2_667 ?
O26 W9 O18 160.0(5) . 2_667 ?
O26 W9 Na4 48.2(6) . 2_667 ?
O26 W9 Na3 40.6(6) . 2_667 ?
O1 Sb1 O2 88.8(4) . . ?
O1 Sb1 O3 91.9(4) . . ?
O2 Sb1 O3 93.7(4) . . ?
O20 Cd1 O24 87.9(5) 2_667 . ?
O20 Cd1 Cl1 91.7(4) 2_667 . ?
O20 Cd1 Na4 90.6(7) 2_667 . ?
O20 Cd1 O37 85.1(14) 2_667 . ?
O20 Cd1 Na3 92.2(9) 2_667 . ?
O20 Cd1 O51 94.9(7) 2_667 . ?
O24 Cd1 Cl1 60.7(4) . . ?
O24 Cd1 Na4 140.2(7) . . ?
O24 Cd1 O37 170.8(14) . . ?
O24 Cd1 Na3 137.3(8) . . ?
O24 Cd1 O51 84.5(7) . . ?
O26 Cd1 O20 86.9(5) 2_667 2_667 ?
O26 Cd1 O24 85.3(5) 2_667 . ?
O26 Cd1 Cl1 145.9(4) 2_667 . ?
O26 Cd1 Na4 55.0(7) 2_667 . ?
O26 Cd1 O37 100.5(13) 2_667 . ?
O26 Cd1 Na3 52.1(8) 2_667 . ?
O26 Cd1 O51 169.5(7) 2_667 . ?
O39 Cd1 O20 174.6(5) . 2_667 ?
O39 Cd1 O24 91.6(5) . . ?
O39 Cd1 O26 87.7(5) . 2_667 ?
O39 Cd1 Cl1 92.8(4) . . ?
O39 Cd1 Na4 86.3(7) . . ?
O39 Cd1 O37 95.9(14) . . ?
O39 Cd1 Na3 84.5(9) . . ?
O39 Cd1 O51 90.4(7) . . ?
O22 Mn1 O29 97.0(13) . . ?
O22 Mn1 O32 161.6(14) . . ?
O22 Mn1 O30 94.6(6) . . ?
O22 Mn1 O31 174.5(7) . . ?
O25 Mn1 O22 94.1(5) . . ?
O25 Mn1 O27 92.8(5) . . ?
O25 Mn1 O29 88.8(14) . . ?
O25 Mn1 O32 87.3(13) . . ?
O25 Mn1 O30 170.4(6) . . ?
W8a O2 W2 91.7(4) . . ?
W6b O5 W1 146.5(6) . . ?
W5a O12 Na4 119.6(9) . . ?
W6b O12 Na3 99.8(10) . . ?
W7a O13 W8 145.5(6) . . ?
W8a O14 W3 118.3(6) . . ?
W5a O16 W4 117.8(6) . . ?
W6b O17 W9 118.5(5) . 2_667 ?
W6b O17 Na3 95.9(10) . . ?
W7a O18 W9 118.6(5) . 2_667 ?
W7a O19 Na1 138.5(6) . 2_666 ?
W8a O20 Cd1 135.0(7) . 2_667 ?
W4a O27 Mn1 134.8(7) . . ?
W5a O39 Cd1 137.3(7) . . ?
C4b N01N C1 107(2) . . ?
C3a N01N C1 103(3) . . ?
C79a N01N C1 108(3) . . ?
C2b N01N C1 104.2(17) . . ?
C79a N01N C5 98(3) . . ?
C3a N01N C5 98(4) . . ?
C3a N01N C79 137(4) . . ?
C4b N01N C2 94(3) . . ?
C4b N01N C6 105(4) . . ?
C2b N01N C6 115(4) . . ?
Cd1 NA3b W9 78.2(5) . 2_667 ?
Cd1 NA4a W9 67.8(4) . 2_667 ?
Cd1 O37a Na4 94.3(14) . . ?
Cd1 NA3b W6 112.9(9) . . ?
Cd1 O36b Na3 106.2(19) . . ?
O3 W6b Na3 87.2(4) . . ?
O4 W7a O3 75.1(4) . . ?
O4 W6b O3 75.1(4) . . ?
O4 W6b Na3 135.3(7) . . ?
O5 W1b O1 82.1(4) . . ?
O5 W6b O3 86.4(4) . . ?
O5 W6b O4 88.2(5) . . ?
O5 W6b O17 159.3(5) . . ?
O5 W6b Na3 132.0(7) . . ?
O6 W1b O1 86.3(4) . . ?
O6 W1b O5 88.0(5) . . ?
O7 W7a O3 85.5(4) . . ?
O7 W7a O4 86.0(5) . . ?
O8 W8a O2 75.4(4) . . ?
O8 W8a O13 83.0(5) . . ?
O9 W4a O1 86.4(4) . . ?
O9 W4a O10 83.7(5) . . ?
O9 W4a O16 159.7(5) . . ?
O10 W1b O1 73.6(4) . . ?
O10 W4a O1 73.3(4) . . ?
O10 W1b O5 155.7(4) . . ?
O10 W1b O6 91.2(5) . . ?
O10 W1b O11 88.1(5) . . ?
O11 W5a O1 75.5(4) . . ?
O11 W1b O1 75.0(4) . . ?
O11 W1b O5 84.8(5) . . ?
O11 W1b O6 160.7(5) . . ?
O12 NA4a W9 74.0(8) . 2_667 ?
O12 NA3b W9 82.3(10) . 2_667 ?
O12 NA4a Cd1 77.1(7) . . ?
O12 NA3b Cd1 91.3(9) . . ?
O12 W5a O1 85.0(4) . . ?
O12 W6b O3 85.1(4) . . ?
O12 W6b O4 159.9(5) . . ?
O12 W6b O5 86.9(5) . . ?
O12 W5a O11 83.2(5) . . ?
O12 W6b O17 90.5(5) . . ?
O12 NA3b O17 69.2(11) . . ?
O12 NA4a O23 111.4(12) . 1_655 ?
O12 NA4a O26 72.3(8) . 2_667 ?
O12 NA3b O38 169.1(18) . . ?
O12 NA3b W6 35.1(6) . . ?
O12 W6b Na3 45.1(7) . . ?
O13 W8a O2 84.7(4) . . ?
O13 W7a O3 87.1(4) . . ?
O13 W7a O4 161.2(5) . . ?
O13 W7a O7 86.6(5) . . ?
O14 W8a O2 74.3(4) . . ?
O14 W8a O8 86.1(5) . . ?
O14 W8a O13 158.2(5) . . ?
O16 W5a O1 73.6(4) . . ?
O16 W4a O1 73.9(5) . . ?
O16 W4a O10 85.8(5) . . ?
O16 W5a O11 85.1(6) . . ?
O16 W5a O12 157.5(5) . . ?
O17 NA4a W9 33.2(4) . 2_667 ?
O17 NA3b W9 38.1(5) . 2_667 ?
O17 NA3b Cd1 113.8(10) . . ?
O17 NA4a Cd1 97.8(7) . . ?
O17 W6b O3 72.9(4) . . ?
O17 W6b O4 87.3(5) . . ?
O17 NA4a O12 66.1(10) . . ?
O17 NA4a O23 93.6(11) . 1_655 ?
O17 NA4a O26 61.0(8) . 2_667 ?
O17 NA3b O38 100.3(16) . . ?
O17 NA4a O38 100.8(15) . . ?
O17 NA3b W6 36.0(6) . . ?
O17 W6b Na3 48.1(8) . . ?
O18 W7a O3 73.6(4) . . ?
O18 W7a O4 89.3(5) . . ?
O18 W7a O7 159.1(5) . . ?
O18 W7a O13 91.4(5) . . ?
O19 W7a O3 168.0(5) . . ?
O19 W7a O4 96.6(5) . . ?
O19 W7a O7 102.7(5) . . ?
O19 W7a O13 101.9(5) . . ?
O19 W7a O18 98.1(5) . . ?
O20 W8a O2 83.3(4) . . ?
O20 W8a O8 157.6(5) . . ?
O20 W8a O13 88.5(5) . . ?
O20 W8a O14 94.7(6) . . ?
O21 W8a O2 173.1(5) . . ?
O21 W8a O8 100.3(6) . . ?
O21 W8a O13 100.4(5) . . ?
O21 W8a O14 100.1(6) . . ?
O21 W8a O20 101.5(6) . . ?
O23 NA4a W9 121.9(12) 1_655 2_667 ?
O23 NA4a Cd1 168.0(14) 1_655 . ?
O23 NA4a O26 151.2(16) 1_655 2_667 ?
O25 Mn1 O31 91.4(7) . . ?
O26 NA3b W9 31.9(6) 2_667 2_667 ?
O26 NA4a W9 29.8(4) 2_667 2_667 ?
O26 NA4a Cd1 38.0(4) 2_667 . ?
O26 NA3b Cd1 46.3(5) 2_667 . ?
O26 NA3b O12 85.1(11) 2_667 . ?
O26 NA3b O17 68.7(10) 2_667 . ?
O26 NA3b O38 88.2(13) 2_667 . ?
O26 NA3b W6 82.7(10) 2_667 . ?
O27 Mn1 O22 81.3(5) . . ?
O27 Mn1 O29 177.8(15) . . ?
O27 Mn1 O32 80.2(14) . . ?
O27 Mn1 O30 92.6(6) . . ?
O27 Mn1 O31 98.0(8) . . ?
O19 Na1 Na2 108.9(3) 2_666 . ?
O19 Na1 O45 82.5(4) 2_666 . ?
O34 Na1 Na2 131.2(4) . . ?
O34 Na1 O19 95.5(5) . 2_666 ?
O34 Na1 O42 97.3(5) . . ?
O34 Na1 O43 176.3(5) . . ?
O34 Na1 O44 99.7(5) . . ?
O34 Na1 O45 97.2(5) . . ?
O42 Na1 Na2 119.0(4) . . ?
O42 Na1 O19 98.5(7) . 2_666 ?
O42 Na1 O44 95.6(6) . . ?
O42 Na1 O45 165.4(5) . . ?
O43 Na1 Na2 46.4(3) . . ?
O43 Na1 O19 83.4(4) . 2_666 ?
O43 Na1 O42 86.3(5) . . ?
O43 Na1 O44 80.4(4) . . ?
O43 Na1 O45 79.2(4) . . ?
O44 Na1 Na2 48.9(3) . . ?
O44 Na1 O19 157.8(5) . 2_666 ?
O44 Na1 O45 79.5(4) . . ?
O45 Na1 Na2 47.9(3) . . ?
O27 W4a O1 87.3(5) . . ?
O27 W4a O9 92.6(5) . . ?
O27 W4a O10 160.4(5) . . ?
O27 W4a O16 91.4(5) . . ?
O33 W4a O1 166.2(5) . . ?
O33 W4a O9 99.8(6) . . ?
O33 W4a O10 95.0(5) . . ?
O33 W4a O16 98.4(6) . . ?
O33 W4a O27 104.6(6) . . ?
O35 W6b O3 170.1(5) . . ?
O35 W6b O4 98.6(5) . . ?
O35 W6b O5 101.2(5) . . ?
O35 W6b O12 101.4(5) . . ?
O35 W6b O17 99.4(6) . . ?
O35 W6b Na3 92.3(5) . . ?
O38 NA3b W9 87.5(12) . 2_667 ?
O38 NA4a W9 81.7(10) . 2_667 ?
O38 NA4a Cd1 79.8(10) . . ?
O38 NA3b Cd1 90.3(12) . . ?
O38 NA4a O12 151.3(11) . . ?
O38 NA4a O23 94.2(13) . 1_655 ?
O38 NA4a O26 79.0(10) . 2_667 ?
O38 NA3b W6 135.4(16) . . ?
O39 W5a O1 82.5(5) . . ?
O39 W5a O11 157.6(5) . . ?
O39 W5a O12 91.2(5) . . ?
O39 W5a O16 92.4(6) . . ?
O40 W5a O1 170.8(5) . . ?
O40 W5a O11 98.7(5) . . ?
O40 W5a O12 101.6(6) . . ?
O40 W5a O16 99.1(6) . . ?
O40 W5a O39 103.6(5) . . ?
O41 W1b O1 172.2(5) . . ?
O41 W1b O5 102.5(5) . . ?
O41 W1b O6 100.0(5) . . ?
O41 W1b O10 101.6(5) . . ?
O41 W1b O11 99.0(5) . . ?
O43 Na2 Na1 46.6(3) . . ?
O43 Na2 O44 79.8(4) . . ?
O43 Na2 O45 80.8(4) . . ?
O43 Na2 O50 89.6(4) . . ?
O43 Na2 O46 166.6(5) . . ?
O43 Na2 O49 84.7(5) . . ?
O43 Na2 O47 155.9(16) . . ?
O44 Na2 Na1 47.9(3) . . ?
O44 Na2 O47 107.5(16) . . ?
O45 Na2 Na1 49.7(3) . . ?
O45 Na2 O44 80.1(4) . . ?
O45 Na2 O46 86.4(5) . . ?
O45 Na2 O47 78.0(16) . . ?
O50 Na2 Na1 122.8(4) . . ?
O50 Na2 O44 169.3(5) . . ?
O50 Na2 O45 97.1(4) . . ?
O50 Na2 O46 88.3(5) . . ?
O50 Na2 O49 81.4(6) . . ?
O50 Na2 O47 81.9(16) . . ?
Sb1 O1 W4 112.8(5) . . ?
Sb1 O1 W5 114.4(5) . . ?
Sb1 O1 W1 138.8(5) . . ?
W3 O2 W2 95.9(4) . . ?
W3 O2 W8 93.6(4) . . ?
Sb1 O2 W2 137.3(5) . . ?
Sb1 O2 W3 115.3(5) . . ?
Sb1 O2 W8 113.3(5) . . ?
W9 O3 W7 95.8(4) 2_667 . ?
W9 O3 W6 95.5(4) 2_667 . ?
Sb1 O3 W9 109.8(4) . 2_667 ?
Sb1 O3 W7 127.1(5) . . ?
Sb1 O3 W6 129.1(5) . . ?
W2 O6 W1 154.9(7) . . ?
W2 O7 W7 146.7(6) . . ?
W2 O8 W8 117.0(5) . . ?
W3 O9 W4 144.1(7) . . ?
W2 O15 W3 118.8(6) . . ?
W9 O17 Na4 105.4(7) 2_667 . ?
W9 O17 Na3 94.2(7) 2_667 . ?
W3 O22 Mn1 139.8(7) . . ?
W3 O23 Na4 137.7(11) . 1_455 ?
W9 O24 Cd1 172.4(8) . . ?
W9 O25 Mn1 170.1(7) . . ?
W9 O26 Cd1 171.0(7) . 2_667 ?
W9 O26 Na4 102.0(9) . 2_667 ?
W9 O26 Na3 107.5(10) . 2_667 ?
Cd1 O26 Na4 87.0(8) 2_667 2_667 ?
Cd1 O26 Na3 81.5(10) 2_667 2_667 ?
W2 O34 Na1 173.1(7) . . ?
Na2 O43 Na1 87.0(4) . . ?
Na1 O44 Na2 83.2(4) . . ?
Na2 O45 Na1 82.4(4) . . ?
C1 N01N C5 111(3) . . ?
C1 N01N C6 126(5) . . ?




_symmetry_cell_setting           triclinic
_symmetry_space_group_name_h-m   ?
_symmetry_int_tables_number      2
_chemical_absolute_configuration ?

####################################################################### 
# 
# 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_elta076_p-1
_database_code_depnum_ccdc_archive 'CCDC 1569738'
_audit_update_record             
;
2018-07-03 deposited with the CCDC.
2018-10-09 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT307_elta076_p-1         
;
PROBLEM: Isolated Metal Atom found in Structure (Unusual)        W1B Check
RESPONSE: High residual electron density due to disorder
;
_audit_creation_date             2017-08-17
_audit_creation_method           
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5375)
;
_chemical_name_systematic        ?
_chemical_name_common            Hexa-zinc-18-tungstoantimonate
_chemical_formula_moiety         
'O72 Sb2 W17.5 Zn6, 14(H2 O), 4(C12 H11 N4), 8.6(O), 2(C4 H12 N), 0.5(C24 H1'

_chemical_formula_sum            'C68 H109 N22 O94 Sb2 W18 Zn6'
_chemical_formula_weight         6683.79
_exptl_crystal_recrystallization_method 'Evaporation in aqueous solution'
_chemical_melting_point          ?
_exptl_crystal_description       plate

_exptl_crystal_colour            'clear red'
_diffrn_ambient_temperature      100.0
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'
Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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.
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
_chemical_absolute_configuration ?
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   12.4792(8)
_cell_length_b                   17.4813(13)
_cell_length_c                   17.6938(11)
_cell_angle_alpha                94.425(4)
_cell_angle_beta                 109.140(3)
_cell_angle_gamma                104.946(4)
_cell_volume                     3467.5(4)
_cell_formula_units_Z            1
_cell_measurement_reflns_used    9883
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      29.240
_cell_measurement_theta_min      2.344
_shelx_estimated_absorpt_T_max   0.639
_shelx_estimated_absorpt_T_min   0.208
_exptl_absorpt_coefficient_mu    16.367
_exptl_absorpt_correction_T_max  0.7460
_exptl_absorpt_correction_T_min  0.4281
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.1584 before and 0.0624 after correction.
The Ratio of minimum to maximum transmission is 0.5739.
The λ/2 correction factor is 0.0015.
;
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    3.201
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_F_000             3037
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.03
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0849
_diffrn_reflns_av_unetI/netI     0.0714
_diffrn_reflns_Laue_measured_fraction_full 0.986
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            56012
_diffrn_reflns_point_group_measured_fraction_full 0.986
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.350
_diffrn_reflns_theta_min         2.344
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device_type  'Bruker X8 APEX'
_diffrn_measurement_method       ?
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'sealed x-ray tube'
_diffrn_source_type              'Incoatec IuS'
_diffrn_special_details          ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                9612
_reflns_number_total             12509
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT v7.68A (Bruker, 2009)'
_computing_data_collection       'APEX 2 v2011.2-0'
_computing_data_reduction        'SAINT v7.68A (Bruker, 2009)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    ?
_refine_diff_density_max         2.096
_refine_diff_density_min         -1.887
_refine_diff_density_rms         0.327
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     973
_refine_ls_number_reflns         12509
_refine_ls_number_restraints     108
_refine_ls_R_factor_all          0.0683
_refine_ls_R_factor_gt           0.0449
_refine_ls_restrained_S_all      1.325
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0432P)²+53.8347P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1007
_refine_ls_wR_factor_ref         0.1124
_refine_special_details          
;1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups, All N(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
2. Restrained distances
 H1D-O31
 2 with sigma of 0.05
 H8BA-H37A
 2.2 with sigma of 0.04
 H8BA-H39C
 2.2 with sigma of 0.04
 H38C-H8BA
 2.2 with sigma of 0.04
 H3-H2C
 2.2 with sigma of 0.04
 H5C-H9AA
 2.2 with sigma of 0.05
 H4B-H2B_$2
 2.2 with sigma of 0.05
 H4B-O25_$3
 1.89 with sigma of 0.04
 C29-C28 ∼ C29-C30 ∼ C30-C25 ∼ C25-C26 ∼ C27-C26 ∼ C27-C28
 with sigma of 0.02
 N10-C28 ∼ N9-C27
 with sigma of 0.02
 W1-W1B ∼ W2-W2B ∼ W3-W3B ∼ W1B-W3B
 with sigma of 0.02
 W8-W9 ∼ W8B-W9B ∼ W9-W4 ∼ W9B-W4B ∼ W4-W5 ∼ W4B-W5B ∼
W7B-W8B ∼ W5-W6 ∼ W6-W7
 ∼ W7-W8 ∼ W6-W1B ∼ W6-W1
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(O16) ∼ Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C10) ∼ Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O29) ∼ Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(C31) = Uanis(C32) = Uanis(C33) = Uanis(C34) = Uanis(C35) = Uanis(C29) =
Uanis(C28) = Uanis(C27) = Uanis(C26) = Uanis(C25) = Uanis(C30) = Uanis(C36)
Uanis(N12) = Uanis(N11) = Uanis(N9) = Uanis(N10)
Uanis(O6) = Uanis(O14) = Uanis(O23) = Uanis(O11) = Uanis(O18)
4. Others
 Fixed Sof: W1(0.96) W2(0.96) W3(0.96) W4(0.96) W5(0.96) W8(0.96) W9(0.96)
 O37A(0.47) O3(0.5) O0AA(0.5) O3DA(0.5) O6BA(0.5) C31(0.5) C32(0.5) C33(0.5)
 H33(0.5) C34(0.5) H34(0.5) C35(0.5) H35(0.5) O4A(0.5) N9(0.5) H9A(0.5)
 H9B(0.5) N10(0.5) H10A(0.5) H10B(0.5) N11(0.5) N12(0.5) C25(0.5) C26(0.5)
 H26(0.5) C27(0.5) C28(0.5) C29(0.5) H29(0.5) C30(0.5) C36(0.5) O37B(0.33)
 W3B(0.03) W1B(0.02) W2B(0.03) W8B(0.03) W5B(0.03) W4B(0.03) W9B(0.03) W7B(0.03)
5.a Free rotating group:
 O1(H1C,H1D), O2(H2C,H2D), O4(H4A,H4B), O5(H5C,H5D), O9AA(H9AA,H9AB), O0A(H0AA,
 H0AB), O8BA(H8BA,H8BB)
5.b Aromatic/amide H refined with riding coordinates:
 N3(H3), C2(H2), C5(H5), C8(H8), C9(H9), C10(H10), C11(H11), N7(H7), C14(H14),
 C17(H17), C20(H20), C21(H21), C22(H22), C23(H23), C33(H33), C34(H34), C35(H35),
  C26(H26), C29(H29)
5.c X=CH2 refined with riding coordinates:
 N1(H1A,H1B), N2(H2A,H2B), N5(H5A,H5B), N6(H6A,H6B), N9(H9A,H9B), N10(H10A,H10B)
5.d Idealised Me refined as rotating group:
 C37(H37A,H37B,H37C), C38(H38A,H38B,H38C), C39(H39A,H39B,H39C), C40(H40A,H40B,
 H40C),SQUEEZE
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
W1 W 0.15795(5) -0.26479(3) -0.28995(3) 0.01479(13) Uani 0.96 1 d D . P A 1
W2 W 0.36158(5) -0.12538(3) -0.36428(3) 0.01674(13) Uani 0.96 1 d D . P A 1
W3 W 0.10612(5) -0.07280(3) -0.33802(3) 0.01715(14) Uani 0.96 1 d D . P A 1
W4 W 0.10617(5) -0.02142(4) -0.15347(4) 0.02083(15) Uani 0.96 1 d D . P A 1
W5 W 0.15562(5) -0.21613(4) -0.10513(4) 0.01868(14) Uani 0.96 1 d D . P A 1
W6 W 0.38510(5) -0.26643(3) -0.12620(3) 0.01968(14) Uani 1 1 d D . . . .
W7 W 0.59297(5) -0.12895(4) -0.20330(4) 0.02335(15) Uani 1 1 d D . . A 1
W8 W 0.55151(5) 0.04576(4) -0.24592(4) 0.02196(15) Uani 0.96 1 d D . P A 1
W9 W 0.29369(6) 0.10115(4) -0.22074(4) 0.02218(15) Uani 0.96 1 d D . P A 1
Sb1 Sb 0.37943(7) -0.06360(5) -0.13877(5) 0.01464(19) Uani 1 1 d . . . A 1
Zn1 Zn 0.42546(13) -0.16116(9) 0.06153(9) 0.0176(3) Uani 1 1 d . . . A 1
Zn2 Zn 0.64611(12) -0.11962(9) 0.00940(9) 0.0181(3) Uani 1 1 d . . . A 1
Zn3 Zn 0.72364(13) 0.04093(9) -0.04822(9) 0.0193(3) Uani 1 1 d . . . A 1
O1 O 0.9055(11) -0.1596(8) -0.0556(7) 0.046(3) Uani 1 1 d . . . . .
H1C H 0.967878 -0.157752 -0.068032 0.069 Uiso 1 1 d G . . . .
H1D H 0.848235 -0.156159 -0.098124 0.069 Uiso 1 1 d DG . . . .
O2 O 0.8236(9) -0.2531(7) -0.2888(7) 0.035(3) Uani 1 1 d . . . B 1
H2C H 0.867021 -0.251568 -0.318791 0.052 Uiso 1 1 d DG . . B 1
H2D H 0.863327 -0.259008 -0.240187 0.052 Uiso 1 1 d G . . B 1
O3AA O 0.2829(7) -0.1774(5) -0.1715(5) 0.0171(19) Uani 1 1 d . . . A 1
O2AA O 0.4402(7) -0.0721(6) -0.2282(5) 0.020(2) Uani 1 1 d . . . A 1
O4AA O 0.2471(8) -0.0311(6) -0.2074(5) 0.022(2) Uani 1 1 d . . . A 1
O5AA O 0.2710(8) -0.2172(6) -0.3343(6) 0.027(2) Uani 1 1 d . . . A 1
O6AA O 0.0888(7) -0.1804(6) -0.3187(5) 0.023(2) Uani 1 1 d . . . A 1
O6 O 0.0770(7) -0.2800(5) -0.2156(5) 0.0192(9) Uani 1 1 d . . . A 1
O7 O 0.2641(7) -0.3186(5) -0.2327(5) 0.0163(19) Uani 1 1 d . . . A 1
O8 O 0.2375(8) -0.0797(6) -0.3694(5) 0.021(2) Uani 1 1 d . . . A 1
O9 O 0.4992(8) -0.1601(5) -0.3184(5) 0.019(2) Uani 1 1 d . . . A 1
O10 O 0.4622(8) -0.0193(6) -0.3543(6) 0.023(2) Uani 1 1 d . . . A 1
O11 O 0.0212(7) -0.0601(5) -0.2697(5) 0.0192(9) Uani 1 1 d . . . A 1
O12 O 0.1699(7) 0.0419(5) -0.3234(5) 0.019(2) Uani 1 1 d . . . A 1
O13 O 0.0932(7) -0.1325(5) -0.1433(5) 0.020(2) Uani 1 1 d . . . A 1
O14 O 0.2551(7) -0.2877(5) -0.0862(5) 0.0192(9) Uani 1 1 d . . . A 1
O15 O 0.4873(8) -0.2183(6) -0.1818(5) 0.021(2) Uani 1 1 d . . . A 1
O16 O 0.6519(8) -0.0223(5) -0.2299(5) 0.020(2) Uani 1 1 d . U . A 1
O17 O 0.4138(8) 0.0829(6) -0.2571(6) 0.025(2) Uani 1 1 d . . . A 1
O18 O 0.1598(7) 0.0826(5) -0.1788(5) 0.0192(9) Uani 1 1 d . . . A 1
O19 O 0.2711(7) -0.1444(5) -0.0164(5) 0.0151(19) Uani 1 1 d . . . A 1
O20 O 0.4710(7) -0.1846(5) -0.0385(5) 0.0162(19) Uani 1 1 d . . . A 1
O21 O 0.6374(7) -0.0774(5) -0.0961(5) 0.019(2) Uani 1 1 d . . . A 1
O22 O 0.5947(7) 0.0740(5) -0.1343(5) 0.020(2) Uani 1 1 d . . . A 1
O23 O 0.6075(7) -0.1149(5) 0.1136(5) 0.0192(9) Uani 1 1 d . . . A 1
O24 O 0.7657(7) -0.0064(5) 0.0546(5) 0.018(2) Uani 1 1 d . . . A 1
O25 O 0.0642(8) -0.3418(5) -0.3685(5) 0.022(2) Uani 1 1 d D . . A 1
O26 O 0.3258(8) -0.1605(5) -0.4669(5) 0.023(2) Uani 1 1 d . . . A 1
O27 O -0.0034(8) -0.0886(6) -0.4323(6) 0.029(2) Uani 1 1 d . . . A 1
O28 O -0.0118(8) -0.0124(6) -0.1255(6) 0.026(2) Uani 1 1 d . . . A 1
O29 O 0.0494(9) -0.2662(6) -0.0689(6) 0.032(2) Uani 1 1 d . U . A 1
O30 O 0.4341(8) -0.3464(6) -0.0988(6) 0.024(2) Uani 1 1 d . . . C 1
O31 O 0.7094(8) -0.1652(6) -0.2031(6) 0.027(2) Uani 1 1 d D . . A 1
O32 O 0.6366(9) 0.1255(6) -0.2720(6) 0.031(2) Uani 1 1 d . . . A 1
O33 O 0.2980(9) 0.1965(6) -0.2370(6) 0.031(2) Uani 1 1 d . . . A 1
O34 O 0.3932(8) -0.2610(6) 0.1066(6) 0.027(2) Uani 1 1 d . . . A 1
O35 O 0.7315(8) -0.1990(6) 0.0027(6) 0.031(2) Uani 1 1 d . . . A 1
O36 O 0.8741(9) 0.0745(7) -0.0709(7) 0.036(3) Uani 1 1 d . . . A 1
N1 N 0.9521(10) -0.5137(8) -0.4155(7) 0.026(3) Uani 1 1 d . . . . .
H1A H 1.004756 -0.465619 -0.398355 0.031 Uiso 1 1 calc R . . . .
H1B H 0.971918 -0.554775 -0.432356 0.031 Uiso 1 1 calc R . . . .
N2 N 0.7867(11) -0.6645(7) -0.4687(7) 0.030(3) Uani 1 1 d . . . . .
H2A H 0.733191 -0.712143 -0.487336 0.036 Uiso 1 1 calc R . . . .
H2B H 0.859484 -0.657905 -0.467735 0.036 Uiso 1 1 calc DR . . . .
N3 N 0.6619(10) -0.4071(7) -0.3660(6) 0.022(3) Uani 1 1 d . . . . .
H3 H 0.715179 -0.359319 -0.347828 0.026 Uiso 1 1 calc DR . . . .
N4 N 0.4982(9) -0.5570(7) -0.4186(6) 0.022(3) Uani 1 1 d . . . . .
C1 C 0.6954(11) -0.4690(8) -0.3909(7) 0.016(3) Uani 1 1 d . . . . .
C2 C 0.8104(12) -0.4594(8) -0.3892(8) 0.021(3) Uani 1 1 d . . . . .
H2 H 0.868163 -0.407972 -0.369611 0.025 Uiso 1 1 calc R . . . .
C3 C 0.8417(11) -0.5242(8) -0.4158(8) 0.019(3) Uani 1 1 d . . . . .
C4 C 0.7572(12) -0.6021(9) -0.4420(8) 0.022(3) Uani 1 1 d . . . . .
C5 C 0.6431(10) -0.6118(8) -0.4434(7) 0.016(3) Uani 1 1 d . . . . .
H5 H 0.586642 -0.663746 -0.462756 0.019 Uiso 1 1 calc R . . . .
C6 C 0.6069(11) -0.5474(8) -0.4170(8) 0.019(3) Uani 1 1 d . . . . .
C7 C 0.4678(13) -0.4929(8) -0.3951(8) 0.024(3) Uani 1 1 d . . . . .
C8 C 0.3510(12) -0.5040(9) -0.3940(8) 0.025(3) Uani 1 1 d . . . . .
H8 H 0.294316 -0.555897 -0.411951 0.029 Uiso 1 1 calc R . . . .
C9 C 0.3209(14) -0.4414(9) -0.3678(9) 0.028(3) Uani 1 1 d . . . . .
H9 H 0.244371 -0.449903 -0.364477 0.034 Uiso 1 1 calc R . . . .
C10 C 0.4035(12) -0.3613(9) -0.3448(8) 0.025(3) Uani 1 1 d . U . . .
H10 H 0.379695 -0.316590 -0.330373 0.030 Uiso 1 1 calc R . . . .
C11 C 0.5163(12) -0.3505(9) -0.3438(7) 0.020(3) Uani 1 1 d . . . . .
H11 H 0.572256 -0.298222 -0.326582 0.024 Uiso 1 1 calc R . . . .
C12 C 0.5495(11) -0.4148(9) -0.3677(8) 0.021(3) Uani 1 1 d . . . . .
O4 O 0.9647(10) 0.6371(7) 0.4652(6) 0.036(3) Uani 1 1 d . . . . .
H4A H 0.926553 0.669352 0.442065 0.055 Uiso 1 1 d G . . . .
H4B H 0.997929 0.654957 0.517215 0.055 Uiso 1 1 d DG . . . .
O5 O 0.9777(11) 0.8769(8) 0.4056(8) 0.052(3) Uani 1 1 d . . . . .
H5C H 0.974972 0.828368 0.387957 0.077 Uiso 1 1 d DG . . . .
H5D H 0.995235 0.883787 0.457878 0.077 Uiso 1 1 d G . . . .
O9AA O 1.1406(12) 0.8193(9) 0.3608(9) 0.066(4) Uani 1 1 d . . . . .
H9AA H 1.145859 0.805198 0.407780 0.099 Uiso 1 1 d DG . . . .
H9AB H 1.209050 0.827034 0.355005 0.099 Uiso 1 1 d G . . . .
O0A O 0.5803(9) 0.2734(6) 0.7362(7) 0.031(2) Uani 1 1 d . . . . .
H0AA H 0.625261 0.321380 0.738527 0.047 Uiso 1 1 d G . . . .
H0AB H 0.614859 0.238044 0.727733 0.047 Uiso 1 1 d G . . . .
O8BA O 0.3835(10) 0.2880(7) 0.6086(7) 0.046(3) Uani 1 1 d . . . . .
H8BA H 0.343913 0.256834 0.561430 0.069 Uiso 1 1 d DG . . . .
H8BB H 0.422530 0.262185 0.641973 0.069 Uiso 1 1 d G . . . .
O37A O 0.332(2) 0.3686(15) -0.2185(16) 0.039(6) Uiso 0.47 1 d . . P D 1
O3 O 0.441(3) 0.4058(16) -0.0430(16) 0.051(7) Uiso 0.5 1 d . . P E 1
N13 N 0.3248(12) 0.0890(8) 0.4755(8) 0.036(3) Uani 1 1 d . . . . .
C37 C 0.4559(15) 0.1314(16) 0.5260(14) 0.079(8) Uani 1 1 d . . . . .
H37A H 0.463628 0.182756 0.556875 0.119 Uiso 1 1 calc DGR . . . .
H37B H 0.500994 0.141136 0.489776 0.119 Uiso 1 1 calc GR . . . .
H37C H 0.487020 0.097297 0.563644 0.119 Uiso 1 1 calc GR . . . .
C38 C 0.2600(13) 0.0785(10) 0.5344(9) 0.036(4) Uani 1 1 d . . . . .
H38A H 0.287832 0.042140 0.570363 0.054 Uiso 1 1 calc GR . . . .
H38B H 0.174353 0.055622 0.504122 0.054 Uiso 1 1 calc GR . . . .
H38C H 0.275752 0.130865 0.566975 0.054 Uiso 1 1 calc DGR . . . .
C39 C 0.2813(15) 0.1407(11) 0.4200(10) 0.044(5) Uani 1 1 d . . . . .
H39A H 0.195204 0.128721 0.405777 0.067 Uiso 1 1 calc GR . . . .
H39B H 0.298732 0.130970 0.370650 0.067 Uiso 1 1 calc GR . . . .
H39C H 0.320677 0.197111 0.446302 0.067 Uiso 1 1 calc DGR . . . .
C40 C 0.311(3) 0.0091(14) 0.4321(16) 0.098(10) Uani 1 1 d . . . . .
H40A H 0.345156 -0.022525 0.471340 0.148 Uiso 1 1 calc GR . . . .
H40B H 0.351638 0.015972 0.393177 0.148 Uiso 1 1 calc GR . . . .
H40C H 0.225976 -0.018905 0.402926 0.148 Uiso 1 1 calc GR . . . .
N5 N 1.2016(10) 0.4846(7) 0.7802(8) 0.029(3) Uani 1 1 d . . . . .
H5A H 1.254741 0.532358 0.798863 0.035 Uiso 1 1 calc R . . . .
H5B H 1.221477 0.443641 0.763024 0.035 Uiso 1 1 calc R . . . .
N6 N 1.0398(10) 0.3336(7) 0.7187(7) 0.025(3) Uani 1 1 d . . . . .
H6A H 0.989704 0.284824 0.699585 0.030 Uiso 1 1 calc R . . . .
H6B H 1.113061 0.343669 0.719553 0.030 Uiso 1 1 calc R . . . .
N7 N 0.9028(9) 0.5816(7) 0.8281(7) 0.021(3) Uani 1 1 d . . . . .
H7 H 0.953045 0.630454 0.845099 0.025 Uiso 1 1 calc R . . . .
N8 N 0.7455(9) 0.4278(7) 0.7731(7) 0.024(3) Uani 1 1 d . . . . .
C13 C 0.9411(11) 0.5218(8) 0.8036(8) 0.019(3) Uani 1 1 d . . . . .
C14 C 1.0566(12) 0.5345(9) 0.8032(8) 0.026(3) Uani 1 1 d . . . . .
H14 H 1.111578 0.587070 0.821315 0.031 Uiso 1 1 calc R . . . .
C15 C 1.0902(12) 0.4742(9) 0.7779(8) 0.022(3) Uani 1 1 d . . . . .
C16 C 1.0049(11) 0.3920(8) 0.7462(8) 0.017(3) Uani 1 1 d . . . . .
C17 C 0.8941(12) 0.3812(9) 0.7468(8) 0.025(3) Uani 1 1 d . . . . .
H17 H 0.839487 0.328603 0.727558 0.029 Uiso 1 1 calc R . . . .
C18 C 0.8542(11) 0.4412(8) 0.7735(7) 0.019(3) Uani 1 1 d . . . . .
C19 C 0.7107(12) 0.4895(9) 0.7997(8) 0.024(3) Uani 1 1 d . . . . .
C20 C 0.5930(13) 0.4760(10) 0.7980(9) 0.030(4) Uani 1 1 d . . . . .
H20 H 0.537820 0.423610 0.778497 0.036 Uiso 1 1 calc R . . . .
C21 C 0.5581(12) 0.5385(9) 0.8244(9) 0.028(4) Uani 1 1 d . . . . .
H21 H 0.479811 0.529069 0.824758 0.034 Uiso 1 1 calc R . . . .
C22 C 0.6398(13) 0.6166(9) 0.8509(9) 0.031(4) Uani 1 1 d . . . . .
H22 H 0.614684 0.659592 0.867881 0.037 Uiso 1 1 calc R . . . .
C23 C 0.7534(13) 0.6323(10) 0.8530(9) 0.031(4) Uani 1 1 d . . . . .
H23 H 0.806800 0.685328 0.871402 0.037 Uiso 1 1 calc R . . . .
C24 C 0.7902(11) 0.5700(9) 0.8280(8) 0.025(3) Uani 1 1 d . . . . .
O0AA O 0.509(3) 0.4294(17) -0.0247(16) 0.054(7) Uiso 0.5 1 d . . P F 2
O3DA O 1.120(3) 0.8086(19) 0.1707(19) 0.078(9) Uiso 0.5 1 d . . P G -2
O6BA O 0.880(2) 0.7718(15) 0.1497(15) 0.046(6) Uani 0.5 1 d . . P H -2
C31 C 0.963(3) 0.496(2) 0.000(2) 0.028(2) Uani 0.5 1 d . . P I 2
C32 C 0.979(3) 0.577(2) 0.033(2) 0.028(2) Uani 0.5 1 d . . P I 2
C33 C 0.883(3) 0.597(2) 0.0446(19) 0.028(2) Uani 0.5 1 d . . P I 2
H33 H 0.892544 0.649952 0.068160 0.034 Uiso 0.5 1 calc R . P I 2
C34 C 0.770(3) 0.5373(18) 0.0211(17) 0.028(2) Uani 0.5 1 d . . P I 2
H34 H 0.704849 0.552246 0.026954 0.034 Uiso 0.5 1 calc R . P I 2
C35 C 0.754(3) 0.460(2) -0.0091(18) 0.028(2) Uani 0.5 1 d . . P I 2
H35 H 0.678717 0.421285 -0.021536 0.034 Uiso 0.5 1 calc R . P I 2
O4A O 0.7293(18) 0.4064(13) -0.0130(12) 0.030(5) Uiso 0.5 1 d . . P J -1
N9 N 1.023(2) 0.8267(15) 0.1738(15) 0.033(3) Uani 0.5 1 d D . P K -1
H9A H 1.093786 0.862911 0.190721 0.040 Uiso 0.5 1 calc R . P K -1
H9B H 0.964265 0.837932 0.184254 0.040 Uiso 0.5 1 calc R . P K -1
N10 N 0.798(2) 0.7185(18) 0.1173(16) 0.033(3) Uani 0.5 1 d D . P K -1
H10A H 0.727887 0.682156 0.102957 0.040 Uiso 0.5 1 calc R . P K -1
H10B H 0.809592 0.767050 0.142521 0.040 Uiso 0.5 1 calc R . P K -1
N11 N 0.946(2) 0.5258(19) 0.0119(17) 0.033(3) Uani 0.5 1 d . . P K -1
N12 N 1.170(2) 0.6359(16) 0.0577(16) 0.033(3) Uani 0.5 1 d . . P K -1
C25 C 1.078(2) 0.6562(14) 0.0712(16) 0.028(2) Uani 0.5 1 d D . P K -1
C26 C 1.099(2) 0.7338(16) 0.1141(16) 0.028(2) Uani 0.5 1 d D . P K -1
H26 H 1.175586 0.772408 0.130971 0.034 Uiso 0.5 1 calc R . P K -1
C27 C 1.0058(18) 0.7533(15) 0.1316(16) 0.028(2) Uani 0.5 1 d D . P K -1
C28 C 0.8884(19) 0.6996(14) 0.1006(16) 0.028(2) Uani 0.5 1 d D . P K -1
C29 C 0.870(3) 0.6220(17) 0.0603(19) 0.028(2) Uani 0.5 1 d D . P K -1
H29 H 0.792646 0.584085 0.041981 0.034 Uiso 0.5 1 calc R . P K -1
C30 C 0.964(2) 0.5997(18) 0.0468(19) 0.028(2) Uani 0.5 1 d D . P K -1
C36 C 1.151(3) 0.5620(19) 0.0225(18) 0.028(2) Uani 0.5 1 d . . P L 2
O37B O 0.326(2) 0.3617(17) -0.1767(18) 0.021(6) Uiso 0.33 1 d . . P M 2
W3B W 0.005(2) -0.1948(17) -0.2625(16) 0.050(6) Uiso 0.03 1 d D . P N 2
W1B W 0.194(6) -0.265(4) -0.320(2) 0.09(2) Uiso 0.02 1 d D . P O 2
W2B W 0.176(4) -0.068(2) -0.364(2) 0.071(9) Uiso 0.03 1 d D . P P 2
W8B W 0.472(2) 0.0298(14) -0.2556(15) 0.043(6) Uiso 0.03 1 d D . P Q 2
W5B W 0.143(2) -0.2178(13) -0.0686(16) 0.030(6) Uiso 0.03 1 d D . P R 2
W4B W 0.083(3) -0.0413(14) -0.1185(19) 0.055(8) Uiso 0.03 1 d D . P S 2
W9B W 0.247(2) 0.0867(17) -0.2116(18) 0.043(8) Uiso 0.03 1 d D . P T 2
W7B W 0.508(3) -0.1587(15) -0.2151(18) 0.058(7) Uiso 0.03 1 d D . P A 2
O1AA O 0.8294(10) 0.7191(7) 0.3785(7) 0.046(3) Uani 1 1 d . . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
O24a W4 1.867(8) 2_655 ?
O23a W9 1.848(9) 2_655 ?
O22a Zn1 2.037(8) 2_655 ?
ZN3a Zn1 3.121(2) 2_655 ?
ZN1a Zn2 3.114(2) . ?
ZN1a Zn3 3.121(2) 2_655 ?
O19a Zn3 2.038(8) 2_655 ?
ZN2a Zn3 3.089(2) . ?
W1a O3AA 2.301(9) . ?
SB1a O3AA 1.968(9) . ?
W5a O3AA 2.270(8) . ?
W8a O2AA 2.276(9) . ?
W7a O2AA 2.306(8) . ?
W2a O2AA 2.294(9) . ?
SB1a O2AA 1.976(8) . ?
W3a O4AA 2.320(9) . ?
W4a O4AA 2.294(8) . ?
W9a O4AA 2.285(9) . ?
SB1a O4AA 1.949(9) . ?
W2a O5AA 1.930(11) . ?
W1a O5AA 1.876(10) . ?
W3a O6AA 1.907(10) . ?
W1a O6AA 1.915(9) . ?
W1a O6 1.900(8) . ?
W5a O6 1.967(9) . ?
W1a O7 1.891(9) . ?
W3a O8 1.924(9) . ?
W2a O8 1.898(9) . ?
W7a O9 1.937(9) . ?
W2a O9 1.917(9) . ?
W2a O10 1.910(9) . ?
W8a O10 1.955(9) . ?
W4a O11 1.949(9) . ?
W3a O11 1.884(8) . ?
W9a O12 1.950(9) . ?
W3a O12 1.920(8) . ?
W5a O13 1.897(9) . ?
W4a O13 1.934(9) . ?
W5a O14 1.952(8) . ?
W7a O15 1.919(9) . ?
W7a O16 1.973(9) . ?
W8a O16 1.911(9) . ?
W9a O17 1.901(9) . ?
W8a O17 1.945(9) . ?
W4a O18 1.911(9) . ?
W9a O18 2.004(8) . ?
ZN3a O19 2.038(8) 2_655 ?
W5a O19 1.842(9) . ?
ZN1a O19 2.076(8) . ?
ZN1a O20 2.072(8) . ?
ZN2a O20 2.035(8) . ?
ZN2a O21 2.041(9) . ?
W7a O21 1.872(9) . ?
ZN3a O21 2.034(9) . ?
ZN1a O22 2.037(8) 2_655 ?
W8a O22 1.857(9) . ?
ZN3a O22 2.062(9) . ?
W9a O23 1.848(9) 2_655 ?
ZN2a O23 2.054(8) . ?
ZN1a O23 2.057(8) . ?
ZN3a O24 2.025(9) . ?
W4a O24 1.867(8) 2_655 ?
ZN2a O24 2.058(9) . ?
W1a O25 1.716(9) . ?
W2a O26 1.741(9) . ?
W3a O27 1.723(10) . ?
W4a O28 1.739(8) . ?
W5a O29 1.726(9) . ?
W7a O31 1.728(8) . ?
W8a O32 1.715(10) . ?
W9a O33 1.703(10) . ?
ZN1a O34 1.977(10) . ?
ZN2a O35 1.974(9) . ?
ZN3a O36 1.998(9) . ?
C36b C31 1.42(4) 2_765 ?
C32b C31 1.78(5) 2_765 ?
C31b C32 1.43(5) . ?
C31b C32 1.78(5) 2_765 ?
C32b C33 1.40(4) . ?
C33b C34 1.42(4) . ?
C36b C35 1.43(4) 2_765 ?
C34b C35 1.34(4) . ?
C35b C36 1.43(4) 2_765 ?
C31b C36 1.42(4) 2_765 ?
W6 O3AA 2.288(8) . ?
W6 O7 1.955(8) . ?
W6 O14 1.938(8) . ?
W6 O15 1.923(9) . ?
W6 O20 1.838(9) . ?
W6 O30 1.708(9) . ?
W6 W7B 2.99(3) . ?
N1 C3 1.340(16) . ?
N2 C4 1.338(17) . ?
N3 C1 1.350(15) . ?
N3 C12 1.363(16) . ?
N4 C6 1.314(16) . ?
N4 C7 1.349(17) . ?
C1 C2 1.392(17) . ?
C1 C6 1.449(18) . ?
C2 C3 1.386(18) . ?
C3 C4 1.421(19) . ?
C4 C5 1.382(17) . ?
C5 C6 1.417(17) . ?
C7 C8 1.426(19) . ?
C7 C12 1.41(2) . ?
C8 C9 1.343(19) . ?
C9 C10 1.44(2) . ?
C10 C11 1.366(18) . ?
C11 C12 1.378(18) . ?
N13 C37 1.53(2) . ?
N13 C38 1.510(18) . ?
N13 C39 1.45(2) . ?
N13 C40 1.48(3) . ?
N5 C15 1.341(17) . ?
N6 C16 1.327(16) . ?
N7 C13 1.354(16) . ?
N7 C24 1.366(16) . ?
N8 C18 1.314(16) . ?
N8 C19 1.367(17) . ?
C13 C14 1.402(18) . ?
C13 C18 1.471(19) . ?
C14 C15 1.329(18) . ?
C15 C16 1.486(19) . ?
C16 C17 1.350(18) . ?
C17 C18 1.384(18) . ?
C19 C20 1.416(19) . ?
C19 C24 1.44(2) . ?
C20 C21 1.380(19) . ?
C21 C22 1.41(2) . ?
C22 C23 1.36(2) . ?
C23 C24 1.380(19) . ?
N9 C27 1.36(3) . ?
N10 C28 1.37(2) . ?
N11 C30 1.32(4) . ?
N12 C25 1.37(3) . ?
C25 C26 1.419(18) . ?
C25 C30 1.416(18) . ?
C26 C27 1.414(17) . ?
C27 C28 1.418(18) . ?
C28 C29 1.408(18) . ?
C29 C30 1.414(18) . ?

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
SB1a O3AAa W1 137.6(4) . . ?
W5a O3AAa W1 93.4(3) . . ?
C1 N3 C12 123.2(12) . . ?
W3a O6AAa W1 149.6(5) . . ?
SB1a O2AAa W2 136.7(4) . . ?
W1a O5AAa W2 151.7(5) . . ?
W8a O2AAa W2 93.5(3) . . ?
C6 N4 C7 119.8(12) . . ?
W2a O8a W3 150.2(5) . . ?
N3 C1 C2 122.1(12) . . ?
W4a O4AAa W3 92.0(3) . . ?
SB1a O4AAa W3 137.4(4) . . ?
N3 C1 C6 116.9(11) . . ?
C2 C1 C6 121.0(11) . . ?
C3 C2 C1 120.7(13) . . ?
N1 C3 C2 120.0(13) . . ?
N1 C3 C4 120.0(12) . . ?
C2 C3 C4 120.0(12) . . ?
N2 C4 C3 120.1(12) . . ?
N2 C4 C5 120.4(13) . . ?
C5 C4 C3 119.3(12) . . ?
C4 C5 C6 122.7(12) . . ?
W9a O4AAa W3 93.2(3) . . ?
W9a O4AAa W4 93.5(3) . . ?
SB1a O4AAa W4 116.0(4) . . ?
W5a O13a W4 153.2(5) . . ?
W3a O11a W4 119.9(4) . . ?
N4 C6 C1 121.3(11) . . ?
N4 C6 C5 122.4(13) . . ?
C5 C6 C1 116.2(11) . . ?
N4 C7 C8 119.7(13) . . ?
N4 C7 C12 122.3(13) . . ?
C12 C7 C8 118.0(12) . . ?
C9 C8 C7 120.4(14) . . ?
C8 C9 C10 120.6(13) . . ?
C11 C10 C9 119.3(13) . . ?
C10 C11 C12 120.4(14) . . ?
N3 C12 C7 116.5(12) . . ?
N3 C12 C11 122.3(13) . . ?
C11 C12 C7 121.1(12) . . ?
C38 N13 C37 106.8(14) . . ?
C39 N13 C37 108.2(14) . . ?
SB1a O3AAa W5 114.7(4) . . ?
W1a O6a W5 118.7(4) . . ?
SB1a O3AAa W6 114.7(4) . . ?
W7a O15a W6 153.3(5) . . ?
C39 N13 C38 109.9(12) . . ?
W1a O7a W6 120.1(4) . . ?
W5a O3AAa W6 93.7(3) . . ?
W2a O2AAa W7 93.3(3) . . ?
SB1a O2AAa W7 115.0(4) . . ?
W8a O2AAa W7 93.2(3) . . ?
W8a O16a W7 118.0(4) . . ?
W2a O9a W7 120.4(4) . . ?
W9a O17a W8 152.7(5) . . ?
W2a O10a W8 118.9(5) . . ?
SB1a O2AAa W8 115.6(4) . . ?
W3a O12a W9 119.8(4) . . ?
W4a O18a W9 116.7(4) . . ?
SB1a O4AAa W9 114.8(4) . . ?
O23a ZN2a Zn1 40.8(2) . . ?
O22a ZN3a Zn1 40.1(2) . 2_655 ?
W9a O23a Zn1 129.6(5) 2_655 . ?
W8a O22a Zn1 134.1(5) . 2_655 ?
ZN2a O20a Zn1 98.6(4) . . ?
O35a ZN2a Zn1 120.9(3) . . ?
ZN3a ZN2a Zn1 120.89(6) . . ?
O21a ZN2a Zn1 120.9(2) . . ?
O36a ZN3a Zn1 118.0(3) . 2_655 ?
ZN2a O23a Zn1 98.5(4) . . ?
O24a ZN2a Zn1 117.4(2) . . ?
O21a ZN3a Zn1 118.8(2) . 2_655 ?
O24a ZN3a Zn1 118.2(2) . 2_655 ?
ZN2a ZN3a Zn1 120.07(6) . 2_655 ?
ZN3a O19a Zn1 98.7(4) 2_655 . ?
O20a ZN2a Zn1 41.1(2) . . ?
W5a O19a Zn1 127.3(4) . . ?
O19a ZN3a Zn1 41.1(2) 2_655 2_655 ?
W4a O24a Zn2 124.4(5) 2_655 . ?
O22a ZN3a Zn2 117.7(3) . . ?
O36a ZN3a Zn2 121.8(3) . . ?
O24a ZN3a Zn2 41.2(2) . . ?
O19a ZN1a Zn2 116.7(2) . . ?
W7a O21a Zn2 132.6(5) . . ?
O34a ZN1a Zn2 117.2(3) . . ?
ZN3a O24a Zn2 98.3(4) . . ?
O23a ZN1a Zn2 40.7(2) . . ?
O20a ZN1a Zn2 40.3(2) . . ?
W9a O23a Zn2 129.9(4) 2_655 . ?
O22a ZN1a Zn2 118.3(3) 2_655 . ?
ZN3a O21a Zn2 98.6(4) . . ?
O19a ZN3a Zn2 118.8(2) 2_655 . ?
O21a ZN3a Zn2 40.8(3) . . ?
O20a ZN2a Zn3 117.9(2) . . ?
O22a ZN1a Zn3 40.7(2) 2_655 2_655 ?
O23a ZN1a Zn3 117.7(3) . 2_655 ?
O20a ZN1a Zn3 115.3(2) . 2_655 ?
O24a ZN2a Zn3 40.4(2) . . ?
ZN1a O22a Zn3 99.2(4) 2_655 . ?
O23a ZN2a Zn3 117.5(3) . . ?
O34a ZN1a Zn3 123.8(3) . 2_655 ?
ZN2a ZN1a Zn3 118.99(6) . 2_655 ?
O21a ZN2a Zn3 40.6(2) . . ?
O35a ZN2a Zn3 118.0(3) . . ?
W8a O22a Zn3 124.8(4) . . ?
W4a O24a Zn3 135.2(5) 2_655 . ?
W7a O21a Zn3 127.9(5) . . ?
O19a ZN1a Zn3 40.2(2) . 2_655 ?
W5a O19a Zn3 133.0(4) . 2_655 ?
O4AAa SB1a O3AA 90.9(4) . . ?
O5AAa W1a O3AA 85.7(3) . . ?
O7a W1a O3AA 73.8(3) . . ?
O6a W1a O3AA 74.2(3) . . ?
O19a W5a O3AA 85.9(3) . . ?
O13a W5a O3AA 86.0(3) . . ?
O6a W5a O3AA 73.7(3) . . ?
O6AAa W1a O3AA 86.6(3) . . ?
O29a W5a O3AA 167.0(4) . . ?
O14a W5a O3AA 74.3(3) . . ?
O25a W1a O3AA 170.6(4) . . ?
O9a W2a O2AA 73.5(3) . . ?
O10a W2a O2AA 74.0(4) . . ?
O4AAa SB1a O2AA 91.3(3) . . ?
O9a W7a O2AA 72.9(3) . . ?
O22a W8a O2AA 83.7(4) . . ?
O15a W7a O2AA 85.7(3) . . ?
O26a W2a O2AA 170.6(4) . . ?
O17a W8a O2AA 85.5(3) . . ?
O8a W2a O2AA 86.2(3) . . ?
O16a W7a O2AA 73.4(3) . . ?
O32a W8a O2AA 170.9(4) . . ?
O10a W8a O2AA 73.6(3) . . ?
O21a W7a O2AA 83.9(3) . . ?
O31a W7a O2AA 168.1(4) . . ?
O16a W8a O2AA 75.2(3) . . ?
O3AAa SB1a O2AA 91.3(4) . . ?
C39 N13 C40 112.1(16) . . ?
C40 N13 C37 110.2(17) . . ?
C40 N13 C38 109.4(13) . . ?
C13 N7 C24 123.5(12) . . ?
C18 N8 C19 120.2(13) . . ?
N7 C13 C14 123.0(13) . . ?
N7 C13 C18 117.1(11) . . ?
C14 C13 C18 119.9(12) . . ?
C15 C14 C13 121.0(14) . . ?
N5 C15 C16 117.3(12) . . ?
C14 C15 N5 121.9(14) . . ?
C14 C15 C16 120.8(13) . . ?
N6 C16 C15 119.5(12) . . ?
N6 C16 C17 123.4(13) . . ?
C17 C16 C15 117.1(12) . . ?
C16 C17 C18 124.8(14) . . ?
N8 C18 C13 121.0(12) . . ?
N8 C18 C17 122.7(13) . . ?
C17 C18 C13 116.3(12) . . ?
N8 C19 C20 120.6(13) . . ?
N8 C19 C24 121.7(12) . . ?
C20 C19 C24 117.7(12) . . ?
C21 C20 C19 120.4(14) . . ?
C20 C21 C22 119.3(13) . . ?
C23 C22 C21 122.2(14) . . ?
C22 C23 C24 119.1(15) . . ?
N7 C24 C19 116.5(12) . . ?
N7 C24 C23 122.2(13) . . ?
C23 C24 C19 121.3(13) . . ?
N12 C25 C26 120(2) . . ?
N12 C25 C30 121(2) . . ?
C30 C25 C26 119(2) . . ?
C27 C26 C25 120(2) . . ?
N9 C27 C26 121(2) . . ?
N9 C27 C28 117.5(19) . . ?
C26 C27 C28 121.3(19) . . ?
N10 C28 C27 121(2) . . ?
N10 C28 C29 120(2) . . ?
C29 C28 C27 118(2) . . ?
C28 C29 C30 121(2) . . ?
N11 C30 C25 120(2) . . ?
N11 C30 C29 120(2) . . ?
C29 C30 C25 120(2) . . ?
O5AAa W2a O2AA 85.7(3) . . ?
O6AAa W3a O4AA 87.2(3) . . ?
O27a W3a O4AA 170.3(4) . . ?
O12a W3a O4AA 73.4(4) . . ?
O8a W3a O4AA 85.0(3) . . ?
O13a W4a O4AA 84.2(3) . . ?
O24a W4a O4AA 83.8(3) 2_655 . ?
O18a W4a O4AA 75.5(3) . . ?
O17a W9a O4AA 87.2(4) . . ?
O33a W9a O4AA 168.3(4) . . ?
O11a W4a O4AA 73.8(3) . . ?
O28a W4a O4AA 172.3(4) . . ?
O11a W3a O4AA 74.3(3) . . ?
O23a W9a O4AA 82.6(4) 2_655 . ?
O12a W9a O4AA 73.6(3) . . ?
O18a W9a O4AA 74.1(3) . . ?
O8a W2a O5AA 86.8(4) . . ?
O10a W2a O5AA 159.3(4) . . ?
O9a W2a O5AA 88.1(4) . . ?
O26a W2a O5AA 100.9(4) . . ?
O25a W1a O5AA 100.6(4) . . ?
O25a W1a O6AA 100.7(4) . . ?
O7a W1a O6AA 160.1(4) . . ?
O11a W3a O6AA 88.5(4) . . ?
O6a W1a O6AA 87.2(4) . . ?
O27a W3a O6AA 101.2(4) . . ?
O5AAa W1a O6AA 86.9(4) . . ?
O25a W1a O6 100.0(4) . . ?
O19a W5a O6 159.6(3) . . ?
O14a W5a O6 85.4(4) . . ?
O29a W5a O6 95.0(4) . . ?
O5AAa W1a O6 159.3(4) . . ?
O7a W1a O6 90.4(4) . . ?
O13a W5a O6 89.3(4) . . ?
O5AAa W1a O7 88.4(4) . . ?
O25a W1a O7 99.2(4) . . ?
O6AAa W3a O8 87.4(4) . . ?
O26a W2a O8 100.7(4) . . ?
O11a W3a O8 159.0(4) . . ?
O27a W3a O8 100.2(4) . . ?
O12a W3a O8 87.0(4) . . ?
O8a W2a O9 159.4(4) . . ?
O26a W2a O9 99.8(4) . . ?
O21a W7a O9 156.8(4) . . ?
O10a W2a O9 89.8(4) . . ?
O15a W7a O9 90.0(4) . . ?
O31a W7a O9 98.2(4) . . ?
O16a W8a O10 87.3(4) . . ?
O8a W2a O10 87.9(4) . . ?
O22a W8a O10 157.0(4) . . ?
O32a W8a O10 98.7(4) . . ?
O17a W8a O10 87.5(4) . . ?
O26a W2a O10 99.8(4) . . ?
O18a W4a O11 87.6(4) . . ?
O27a W3a O11 100.8(4) . . ?
O28a W4a O11 99.3(4) . . ?
O13a W4a O11 86.8(4) . . ?
O24a W4a O11 157.2(3) 2_655 . ?
O6AAa W3a O12 160.1(4) . . ?
O27a W3a O12 98.6(4) . . ?
O11a W3a O12 90.0(4) . . ?
O33a W9a O12 98.9(4) . . ?
O23a W9a O12 156.0(4) 2_655 . ?
O17a W9a O12 91.1(4) . . ?
O29a W5a O13 100.6(4) . . ?
O18a W4a O13 159.7(3) . . ?
O24a W4a O13 87.0(4) 2_655 . ?
O19a W5a O13 90.5(4) . . ?
O28a W4a O13 99.0(4) . . ?
O29a W5a O14 98.8(4) . . ?
O13a W5a O14 160.3(4) . . ?
O19a W5a O14 87.9(4) . . ?
O31a W7a O15 102.5(4) . . ?
O21a W7a O15 89.0(4) . . ?
O15a W7a O16 159.1(3) . . ?
O21a W7a O16 87.7(4) . . ?
O32a W8a O16 99.9(4) . . ?
O9a W7a O16 85.0(4) . . ?
O31a W7a O16 98.3(4) . . ?
O22a W8a O16 90.6(4) . . ?
O32a W8a O17 99.2(4) . . ?
O22a W8a O17 87.0(4) . . ?
O16a W8a O17 160.7(4) . . ?
O33a W9a O17 102.1(4) . . ?
O23a W9a O17 90.9(4) 2_655 . ?
O28a W4a O18 101.2(4) . . ?
O23a W9a O18 86.2(4) 2_655 . ?
O12a W9a O18 84.3(3) . . ?
O33a W9a O18 96.6(4) . . ?
O24a W4a O18 90.7(4) 2_655 . ?
O17a W9a O18 161.2(4) . . ?
O24a ZN3a O19 90.4(3) . 2_655 ?
O23a ZN1a O19 145.2(4) . . ?
O20a ZN1a O19 88.5(3) . . ?
O36a ZN3a O19 102.0(4) . 2_655 ?
O21a ZN3a O19 148.2(3) . 2_655 ?
O34a ZN1a O19 112.2(4) . . ?
O22a ZN1a O19 79.6(3) 2_655 . ?
O29a W5a O19 105.0(4) . . ?
O22a ZN1a O20 144.5(4) 2_655 . ?
O34a ZN1a O20 108.6(4) . . ?
O35a ZN2a O20 104.6(4) . . ?
O23a ZN1a O20 80.1(3) . . ?
O31a W7a O21 104.6(4) . . ?
O24a ZN3a O21 80.5(4) . . ?
O35a ZN2a O21 100.1(4) . . ?
O20a ZN2a O21 91.6(3) . . ?
O36a ZN3a O21 109.8(4) . . ?
O34a ZN1a O22 106.9(4) . 2_655 ?
O36a ZN3a O22 108.3(4) . . ?
O21a ZN3a O22 90.8(4) . . ?
O24a ZN3a O22 146.3(3) . . ?
O19a ZN3a O22 79.9(3) 2_655 . ?
O32a W8a O22 104.2(4) . . ?
O35a ZN2a O23 111.8(4) . . ?
O34a ZN1a O23 102.5(4) . . ?
O33a W9a O23 104.1(4) . 2_655 ?
O22a ZN1a O23 90.9(3) 2_655 . ?
O20a ZN2a O23 81.0(3) . . ?
O21a ZN2a O23 148.1(3) . . ?
O36a ZN3a O24 105.3(4) . . ?
O23a ZN2a O24 89.0(3) . . ?
O35a ZN2a O24 109.8(4) . . ?
O20a ZN2a O24 145.4(3) . . ?
O21a ZN2a O24 79.6(3) . . ?
O28a W4a O24 103.3(4) . 2_655 ?
C33b C32b C31 149(3) . 2_765 ?
C31b C32b C31 30(2) . 2_765 ?
C33b C32b C31 119(3) . . ?
C32b C31b C32 150(2) . 2_765 ?
C36b C31b C32 119(3) 2_765 . ?
C36b C31b C32 91(3) 2_765 2_765 ?
C35b C34b C33 122(3) . . ?
C32b C33b C34 120(3) . . ?
C31b C36b C35 120(3) 2_765 2_765 ?
C34b C35b C36 120(3) . 2_765 ?
O14a W6 O3AA 74.1(3) . . ?
O15a W6 O3AA 85.7(3) . . ?
O20a W6 O3AA 83.3(3) . . ?
O7a W6 O3AA 73.0(3) . . ?
O30a W6 O3AA 168.7(4) . . ?
O14a W6 O7 85.9(3) . . ?
O15a W6 O7 87.8(4) . . ?
O20a W6 O7 156.3(4) . . ?
O30a W6 O7 98.9(4) . . ?
O20a W6 O14 88.8(4) . . ?
O15a W6 O14 159.8(4) . . ?
O30a W6 O14 97.8(4) . . ?
O20a W6 O15 89.3(4) . . ?
O30a W6 O15 102.1(4) . . ?
O30a W6 O20 104.7(4) . . ?
W6 O3AAa W1 93.1(3) . . ?
W6 O14a W5 117.5(5) . . ?
W6 O20a Zn1 126.1(4) . . ?
W6 O20a Zn2 132.4(4) . . ?



loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O25a W1a O5AAa W2a 126.0(11) . . . . ?
O7a W1a O5AAa W2a -135.0(11) . . . . ?
O6a W1a O5AAa W2a -47.9(18) . . . . ?
O6AAa W1a O5AAa W2a 25.7(11) . . . . ?
O3AAa W1a O5AAa W2a -61.1(11) . . . . ?
O25a W1a O6a W5a 171.9(5) . . . . ?
O5AAa W1a O6a W5a -14.2(14) . . . . ?
O7a W1a O6a W5a 72.5(5) . . . . ?
O6AAa W1a O6a W5a -87.7(5) . . . . ?
O3AAa W1a O6a W5a -0.5(4) . . . . ?
O25a W1a O7a W6 -172.4(5) . . . . ?
O5AAa W1a O7a W6 87.2(5) . . . . ?
O6a W1a O7a W6 -72.2(5) . . . . ?
O6AAa W1a O7a W6 10.7(13) . . . . ?
O3AAa W1a O7a W6 1.2(4) . . . . ?
O26a W2a O8a W3a 123.8(10) . . . . ?
O10a W2a O8a W3a -136.6(11) . . . . ?
O9a W2a O8a W3a -52.6(18) . . . . ?
O5AAa W2a O8a W3a 23.3(10) . . . . ?
O2AAa W2a O8a W3a -62.5(10) . . . . ?
O27a W3a O11a W4a -169.2(5) . . . . ?
O6AAa W3a O11a W4a 89.8(5) . . . . ?
O12a W3a O11a W4a -70.4(5) . . . . ?
O8a W3a O11a W4a 11.3(14) . . . . ?
O4AAa W3a O11a W4a 2.3(5) . . . . ?
O29a W5a O13a W4a 132.7(11) . . . . ?
O19a W5a O13a W4a 27.3(11) . . . . ?
O14a W5a O13a W4a -58.0(17) . . . . ?
O6a W5a O13a W4a -132.3(11) . . . . ?
O3AAa W5a O13a W4a -58.6(11) . . . . ?
O29a W5a O19a ZN3a -71.5(7) . . . 2_655 ?
O13a W5a O19a ZN3a 29.6(6) . . . 2_655 ?
O14a W5a O19a ZN3a -170.0(6) . . . 2_655 ?
O6a W5a O19a ZN3a 119.1(9) . . . 2_655 ?
O3AAa W5a O19a ZN3a 115.6(6) . . . 2_655 ?
O29a W5a O19a ZN1a 94.5(6) . . . . ?
O13a W5a O19a ZN1a -164.4(5) . . . . ?
O14a W5a O19a ZN1a -4.1(5) . . . . ?
O6a W5a O19a ZN1a -74.9(12) . . . . ?
O3AAa W5a O19a ZN1a -78.5(5) . . . . ?
O30a W6 O20a ZN2a 68.8(7) . . . . ?
O15a W6 O20a ZN2a -33.5(6) . . . . ?
O14a W6 O20a ZN2a 166.6(6) . . . . ?
O7a W6 O20a ZN2a -116.5(8) . . . . ?
O3AAa W6 O20a ZN2a -119.3(6) . . . . ?
O30a W6 O20a ZN1a -87.7(6) . . . . ?
O15a W6 O20a ZN1a 169.9(5) . . . . ?
O14a W6 O20a ZN1a 10.1(5) . . . . ?
O7a W6 O20a ZN1a 87.0(10) . . . . ?
O3AAa W6 O20a ZN1a 84.2(5) . . . . ?
O31a W7a O21a ZN3a 93.4(6) . . . . ?
O15a W7a O21a ZN3a -163.9(6) . . . . ?
O9a W7a O21a ZN3a -76.2(11) . . . . ?
O16a W7a O21a ZN3a -4.6(5) . . . . ?
O2AAa W7a O21a ZN3a -78.1(5) . . . . ?
O31a W7a O21a ZN2a -73.0(7) . . . . ?
O15a W7a O21a ZN2a 29.6(6) . . . . ?
O9a W7a O21a ZN2a 117.3(9) . . . . ?
O16a W7a O21a ZN2a -171.0(6) . . . . ?
O2AAa W7a O21a ZN2a 115.4(6) . . . . ?
O32a W8a O22a ZN1a 66.7(7) . . . 2_655 ?
O16a W8a O22a ZN1a 167.1(7) . . . 2_655 ?
O17a W8a O22a ZN1a -32.0(7) . . . 2_655 ?
O10a W8a O22a ZN1a -108.5(10) . . . 2_655 ?
O2AAa W8a O22a ZN1a -117.8(6) . . . 2_655 ?
O32a W8a O22a ZN3a -94.0(6) . . . . ?
O16a W8a O22a ZN3a 6.4(6) . . . . ?
O17a W8a O22a ZN3a 167.2(6) . . . . ?
O10a W8a O22a ZN3a 90.8(10) . . . . ?
O2AAa W8a O22a ZN3a 81.4(5) . . . . ?
C12 N3 C1 C2 179.4(12) . . . . ?
C12 N3 C1 C6 -2.7(18) . . . . ?
N3 C1 C2 C3 -179.5(12) . . . . ?
C6 C1 C2 C3 2.8(19) . . . . ?
C1 C2 C3 N1 178.5(12) . . . . ?
C1 C2 C3 C4 -2.6(19) . . . . ?
N1 C3 C4 N2 -2(2) . . . . ?
C2 C3 C4 N2 179.1(12) . . . . ?
N1 C3 C4 C5 -178.9(12) . . . . ?
C2 C3 C4 C5 2.3(19) . . . . ?
N2 C4 C5 C6 -179.0(12) . . . . ?
C3 C4 C5 C6 -2.1(19) . . . . ?
C7 N4 C6 C5 -177.9(12) . . . . ?
C7 N4 C6 C1 -0.4(19) . . . . ?
C4 C5 C6 N4 179.8(12) . . . . ?
C4 C5 C6 C1 2.2(18) . . . . ?
N3 C1 C6 N4 2.0(19) . . . . ?
C2 C1 C6 N4 179.9(12) . . . . ?
N3 C1 C6 C5 179.7(11) . . . . ?
C2 C1 C6 C5 -2.5(18) . . . . ?
C6 N4 C7 C12 -0.6(19) . . . . ?
C6 N4 C7 C8 -177.7(12) . . . . ?
N4 C7 C8 C9 177.4(12) . . . . ?
C12 C7 C8 C9 0(2) . . . . ?
C7 C8 C9 C10 4(2) . . . . ?
C8 C9 C10 C11 -5(2) . . . . ?
C9 C10 C11 C12 2.6(19) . . . . ?
C1 N3 C12 C11 -178.5(12) . . . . ?
C1 N3 C12 C7 1.8(18) . . . . ?
C10 C11 C12 N3 -178.5(12) . . . . ?
C10 C11 C12 C7 1.2(19) . . . . ?
N4 C7 C12 N3 -0.1(19) . . . . ?
C8 C7 C12 N3 177.1(12) . . . . ?
N4 C7 C12 C11 -179.8(12) . . . . ?
C8 C7 C12 C11 -2.6(19) . . . . ?
C24 N7 C13 C14 179.3(13) . . . . ?
C24 N7 C13 C18 1.6(19) . . . . ?
N7 C13 C14 C15 -179.3(13) . . . . ?
C18 C13 C14 C15 -2(2) . . . . ?
C13 C14 C15 N5 -177.2(13) . . . . ?
C13 C14 C15 C16 2(2) . . . . ?
C14 C15 C16 N6 177.7(12) . . . . ?
N5 C15 C16 N6 -2.7(18) . . . . ?
C14 C15 C16 C17 -2.0(19) . . . . ?
N5 C15 C16 C17 177.6(12) . . . . ?
N6 C16 C17 C18 -178.6(13) . . . . ?
C15 C16 C17 C18 1(2) . . . . ?
C19 N8 C18 C17 -179.6(12) . . . . ?
C19 N8 C18 C13 1.2(19) . . . . ?
C16 C17 C18 N8 -179.8(13) . . . . ?
C16 C17 C18 C13 -1(2) . . . . ?
N7 C13 C18 N8 -2.2(19) . . . . ?
C14 C13 C18 N8 -179.9(12) . . . . ?
N7 C13 C18 C17 178.5(11) . . . . ?
C14 C13 C18 C17 0.8(18) . . . . ?
C18 N8 C19 C20 178.7(13) . . . . ?
C18 N8 C19 C24 0(2) . . . . ?
N8 C19 C20 C21 -179.7(13) . . . . ?
C24 C19 C20 C21 -1(2) . . . . ?
C19 C20 C21 C22 2(2) . . . . ?
C20 C21 C22 C23 -1(2) . . . . ?
C21 C22 C23 C24 0(2) . . . . ?
C13 N7 C24 C23 -179.7(13) . . . . ?
C13 N7 C24 C19 -0.2(19) . . . . ?
C22 C23 C24 N7 179.7(14) . . . . ?
C22 C23 C24 C19 0(2) . . . . ?
N8 C19 C24 N7 -1(2) . . . . ?
C20 C19 C24 N7 -179.3(12) . . . . ?
N8 C19 C24 C23 178.6(13) . . . . ?
C20 C19 C24 C23 0(2) . . . . ?
C36b C31b C32b C33b 2(5) 2_765 . . . ?
C32b C31b C32b C33b 179(4) 2_765 . . . ?
C36b C31b C32b C31b -177(7) 2_765 . . 2_765 ?
C32b C31b C32b C31b 0.003(6) 2_765 . . 2_765 ?
C31b C32b C33b C34b -2(4) . . . . ?
C31b C32b C33b C34b -1(7) 2_765 . . . ?
C32b C33b C34b C35b 3(4) . . . . ?
C33b C34b C35b C36b -4(4) . . . 2_765 ?
N12 C25 C26 C27 -177(2) . . . . ?
C30 C25 C26 C27 0(4) . . . . ?
C25 C26 C27 N9 179(3) . . . . ?
C25 C26 C27 C28 -6(4) . . . . ?
N9 C27 C28 N10 -5(4) . . . . ?
C26 C27 C28 N10 -180(3) . . . . ?
N9 C27 C28 C29 -177(3) . . . . ?
C26 C27 C28 C29 8(4) . . . . ?
N10 C28 C29 C30 -176(3) . . . . ?
C27 C28 C29 C30 -4(4) . . . . ?
C28 C29 C30 N11 177(3) . . . . ?
C28 C29 C30 C25 -2(4) . . . . ?
N12 C25 C30 N11 1(4) . . . . ?
C26 C25 C30 N11 -175(3) . . . . ?
N12 C25 C30 C29 -179(3) . . . . ?
C26 C25 C30 C29 4(4) . . . . ?

####################################################################### 
# 
# 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_elta076_c2m
_database_code_depnum_ccdc_archive 'CCDC 1576366'
_audit_update_record             
;
2018-07-03 deposited with the CCDC.
2018-10-09 downloaded from the CCDC.
;
_audit_creation_date             2017-08-17
_audit_creation_method           
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5375)
;
_chemical_name_common            (TMA)4Hexa-zinc-18-tungstoantimonate
_chemical_name_systematic        ?
_chemical_formula_moiety         'O72 Sb2 W18 Zn6, 4(C4 H12 N)'
_chemical_formula_sum            'C16 H48 N4 O72 Sb2 W18 Zn6'
_chemical_formula_weight         5393.60
_chemical_melting_point          ?
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'
Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           12
_space_group_name_H-M_alt        'C 1 2/m 1'
_space_group_name_Hall           '-C 2y'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z'
'-x, -y, -z'
'x, -y, z'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z'

_cell_length_a                   14.5029(12)
_cell_length_b                   23.1699(12)
_cell_length_c                   18.1162(11)
_cell_angle_alpha                90
_cell_angle_beta                 95.440(4)
_cell_angle_gamma                90
_cell_volume                     6060.2(7)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    9097
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      29.994
_cell_measurement_theta_min      2.697
_shelx_estimated_absorpt_T_max   0.094
_shelx_estimated_absorpt_T_min   0.071
_exptl_absorpt_coefficient_mu    18.674
_exptl_absorpt_correction_T_max  0.7460
_exptl_absorpt_correction_T_min  0.1335
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction. 
wR2(int) was 0.1811 before and 0.1090 after correction. 
The Ratio of minimum to maximum transmission is 0.1790. 
The λ/2 correction factor is 0.0015.
;

_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.956
_exptl_crystal_density_meas      .
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             4724
_exptl_crystal_preparation       ?
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.24
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.2444
_diffrn_reflns_av_unetI/netI     0.0693
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            151418
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.876
_diffrn_reflns_theta_min         2.083
_diffrn_ambient_temperature      100.0
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_diffrn_special_details          ?
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                6705
_reflns_number_total             7386
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT v7.68A (Bruker, 2009)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT v7.68A (Bruker, 2009)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'XS (Sheldrick, 2008)'
_refine_diff_density_max         3.336
_refine_diff_density_min         -6.817
_refine_diff_density_rms         0.681
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.069
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     284
_refine_ls_number_reflns         7386
_refine_ls_number_restraints     108
_refine_ls_R_factor_all          0.0783
_refine_ls_R_factor_gt           0.0753
_refine_ls_restrained_S_all      1.134
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1346P)²+178.2807P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1982
_refine_ls_wR_factor_ref         0.2026
_refine_special_details          
;_olex2_refinement_description

1. Fixed Uiso
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(O2) ∼ Ueq, Uanis(O14) ∼ Ueq, Uanis(O17) ∼ Ueq, Uanis(O5)
∼ Ueq, Uanis(O16) ∼ Ueq: with sigma of 0.001 and sigma for terminal
atoms of 0.002
Uanis(C4) ∼ Ueq: with sigma of 0.03 and sigma for terminal atoms of 0.06
Uanis(O12) ∼ Ueq, Uanis(O4) ∼ Ueq, Uanis(O8) ∼ Ueq, Uanis(O15)
∼ Ueq, Uanis(O9) ∼ Ueq, Uanis(O13) ∼ Ueq, Uanis(O1) ∼ Ueq,
Uanis(O6) ∼ Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(Zn2) ∼ Ueq: with sigma of 0.002 and sigma for terminal atoms of 0.001
Uanis(W1) ∼ Ueq, Uanis(W2) ∼ Ueq, Uanis(Sb1) ∼ Ueq: with sigma of
0.001 and sigma for terminal atoms of 0.0005
3.a Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C2(H2A,H2B,H2C), C3(H3A,H3B,H3C), C4(H4A,H4B,H4C)

_smtbx_masks_special_details      ?
loop_
  _smtbx_masks_void_nr
  _smtbx_masks_void_average_x
  _smtbx_masks_void_average_y
  _smtbx_masks_void_average_z
  _smtbx_masks_void_volume
  _smtbx_masks_void_count_electrons
  _smtbx_masks_void_content
 1 -0.333 -0.954 -0.892 2435.6 2817.8 ?,SQUEEZE
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
W1 W 0.92746(3) 0.58013(2) 0.17485(2) 0.01822(16) Uani 1 1 d . U . . .
W2 W 0.72114(5) 0.500000 0.22312(3) 0.01882(18) Uani 1 2 d S TU P . .
W3 W 0.72471(4) 0.57143(3) 0.38385(3) 0.02744(17) Uani 1 1 d . . . . .
W4 W 0.93242(4) 0.65292(2) 0.33441(2) 0.02429(17) Uani 1 1 d . . . . .
W5 W 1.11855(3) 0.58094(2) 0.29202(2) 0.01623(15) Uani 1 1 d . . . . .
Sb1 Sb 0.94188(7) 0.500000 0.37120(5) 0.0129(2) Uani 1 2 d S TU P . .
Zn1 Zn 1.19907(13) 0.500000 0.45252(9) 0.0157(4) Uani 1 2 d S T P . .
Zn2 Zn 1.10105(9) 0.38276(5) 0.47865(7) 0.0159(3) Uani 1 1 d . U . . .
O1 O 0.9661(5) 0.5622(3) 0.2991(4) 0.0141(15) Uani 1 1 d . U . . .
O2 O 0.8098(8) 0.500000 0.3343(6) 0.017(2) Uani 1 2 d S TU P . .
O3 O 0.8109(6) 0.6233(4) 0.3434(4) 0.0206(17) Uani 1 1 d . . . . .
O4 O 0.9071(7) 0.6496(4) 0.2261(5) 0.0237(18) Uani 1 1 d . U . . .
O5 O 0.8040(6) 0.5562(4) 0.1923(5) 0.0199(17) Uani 1 1 d . U . . .
O6 O 0.6688(6) 0.5572(4) 0.2825(5) 0.0221(17) Uani 1 1 d . U . . .
O7 O 0.9112(7) 0.6049(5) 0.0854(5) 0.033(2) Uani 1 1 d . . . . .
O8 O 0.6378(9) 0.500000 0.1514(7) 0.027(3) Uani 1 2 d S TU P . .
O9 O 0.6456(7) 0.6210(4) 0.4118(5) 0.0269(19) Uani 1 1 d . U . . .
O9AA O 1.0629(6) 0.6536(3) 0.3142(4) 0.0204(17) Uani 1 1 d . . . . .
O10 O 0.9152(7) 0.7262(4) 0.3462(5) 0.029(2) Uani 1 1 d . . . . .
O11 O 1.2270(6) 0.6071(4) 0.2767(5) 0.0217(17) Uani 1 1 d . . . . .
O12 O 1.0579(6) 0.5921(4) 0.1929(5) 0.0196(16) Uani 1 1 d . U . . .
O13 O 1.1298(8) 0.500000 0.2705(6) 0.014(2) Uani 1 2 d S TU P . .
O14 O 0.9486(8) 0.500000 0.1593(6) 0.017(2) Uani 1 2 d S TU P . .
O15 O 0.6626(9) 0.500000 0.4086(6) 0.021(2) Uani 1 2 d S TU P . .
O16 O 0.8087(6) 0.5618(3) 0.4670(4) 0.0161(15) Uani 1 1 d . U . . .
O17 O 0.9704(6) 0.6267(3) 0.4286(5) 0.0178(16) Uani 1 1 d . U . . .
O18 O 1.3250(8) 0.500000 0.4173(7) 0.021(2) Uani 1 2 d S T P . .
O19 O 1.1754(6) 0.3107(4) 0.4774(5) 0.0225(18) Uani 1 1 d . . . . .
O20 O 1.1302(6) 0.5624(4) 0.3924(4) 0.0202(17) Uani 1 1 d . . . . .
N1 N 0.6393(11) 0.2771(6) 0.1974(8) 0.043(3) Uani 1 1 d . . . . .
C1 C 0.566(2) 0.2468(10) 0.1537(11) 0.076(8) Uani 1 1 d . . . . .
H1A H 0.509639 0.270599 0.149602 0.114 Uiso 1 1 calc GR . . . .
H1B H 0.553326 0.210192 0.177867 0.114 Uiso 1 1 calc GR . . . .
H1C H 0.584638 0.239242 0.104083 0.114 Uiso 1 1 calc GR . . . .
C2 C 0.716(2) 0.2424(10) 0.1854(15) 0.086(9) Uani 1 1 d . . . . .
H2A H 0.694166 0.204525 0.167010 0.129 Uiso 1 1 calc GR . . . .
H2B H 0.755032 0.237692 0.232055 0.129 Uiso 1 1 calc GR . . . .
H2C H 0.751593 0.260861 0.148620 0.129 Uiso 1 1 calc GR . . . .
C3 C 0.6573(17) 0.3331(9) 0.1568(10) 0.061(6) Uani 1 1 d . . . . .
H3A H 0.628252 0.330922 0.105811 0.092 Uiso 1 1 calc GR . . . .
H3B H 0.724213 0.338656 0.156188 0.092 Uiso 1 1 calc GR . . . .
H3C H 0.631060 0.365545 0.182429 0.092 Uiso 1 1 calc GR . . . .
C4 C 0.627(2) 0.2865(13) 0.2737(13) 0.112(12) Uani 1 1 d . U . . .
H4A H 0.685246 0.300140 0.299693 0.168 Uiso 1 1 calc GR . . . .
H4B H 0.608511 0.250326 0.296041 0.168 Uiso 1 1 calc GR . . . .
H4C H 0.578650 0.315641 0.277684 0.168 Uiso 1 1 calc GR . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
W1 O1 2.306(7) . ?
W1 O4 1.895(9) . ?
W1 O5 1.929(9) . ?
W1 O7 1.715(9) . ?
W1 O12 1.909(8) . ?
W1 O14 1.907(3) . ?
W2 O2 2.285(11) . ?
W2 O5 1.891(9) 6_565 ?
W2 O5 1.892(9) . ?
W2 O6 1.910(9) 6_565 ?
W2 O6 1.910(9) . ?
W2 O8 1.689(12) . ?
W3 O2 2.297(8) . ?
W3 O3 1.928(9) . ?
W3 O6 1.964(9) . ?
W3 O9 1.732(9) . ?
W3 O15 1.956(7) . ?
W3 O16 1.858(8) . ?
W4 O1 2.263(8) . ?
W4 O3 1.912(9) . ?
W4 O4 1.964(9) . ?
W4 O9AA 1.961(9) . ?
W4 O10 1.732(9) . ?
W4 O17 1.846(8) . ?
W5 O1 2.269(8) . ?
W5 O9AA 1.925(8) . ?
W5 O11 1.732(9) . ?
W5 O12 1.941(8) . ?
W5 O13 1.925(2) . ?
W5 O20 1.861(8) . ?
Sb1 O1 1.999(8) . ?
Sb1 O1 1.999(8) 6_565 ?
Sb1 O2 1.968(11) . ?
Zn1 Zn2 3.1227(16) 6_565 ?
Zn1 Zn2 3.1227(16) . ?
Zn1 O16 2.054(8) 5_766 ?
Zn1 O16 2.054(8) 2_756 ?
Zn1 O18 1.991(11) . ?
Zn1 O20 2.017(9) 6_565 ?
Zn1 O20 2.017(9) . ?
Zn2 Zn2 3.102(3) 2_756 ?
Zn2 O16 2.023(8) 5_766 ?
Zn2 O17 2.033(8) 6_565 ?
Zn2 O17 2.068(9) 5_766 ?
Zn2 O19 1.989(8) . ?
Zn2 O20 2.087(9) 6_565 ?
O2 W3 2.297(8) 6_565 ?
O13 W5 1.925(2) 6_565 ?
O14 W1 1.907(3) 6_565 ?
O15 W3 1.956(7) 6_565 ?
O16 Zn1 2.054(8) 5_766 ?
O16 Zn2 2.023(8) 5_766 ?
O17 Zn2 2.033(8) 6_565 ?
O17 Zn2 2.068(9) 5_766 ?
O20 Zn2 2.086(9) 6_565 ?
N1 C1 1.45(2) . ?
N1 C2 1.40(3) . ?
N1 C3 1.52(2) . ?
N1 C4 1.43(3) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O4 W1 O1 73.1(3) . . ?
O4 W1 O5 88.5(4) . . ?
O4 W1 O12 89.5(4) . . ?
O4 W1 O14 159.1(4) . . ?
O5 W1 O1 86.1(3) . . ?
O7 W1 O1 169.2(4) . . ?
O7 W1 O4 99.5(5) . . ?
O7 W1 O5 101.8(4) . . ?
O7 W1 O12 99.1(4) . . ?
O7 W1 O14 101.3(5) . . ?
O12 W1 O1 73.4(3) . . ?
O12 W1 O5 159.0(3) . . ?
O14 W1 O1 86.7(4) . . ?
O14 W1 O5 84.7(4) . . ?
O14 W1 O12 89.8(4) . . ?
O5 W2 O2 86.6(3) . . ?
O5 W2 O2 86.6(3) 6_565 . ?
O5 W2 O5 86.9(5) 6_565 . ?
O5 W2 O6 160.4(4) 6_565 . ?
O5 W2 O6 89.2(4) 6_565 6_565 ?
O5 W2 O6 89.2(4) . . ?
O5 W2 O6 160.4(4) . 6_565 ?
O6 W2 O2 74.0(3) . . ?
O6 W2 O2 74.0(3) 6_565 . ?
O6 W2 O6 88.0(5) 6_565 . ?
O8 W2 O2 168.6(5) . . ?
O8 W2 O5 101.6(4) . 6_565 ?
O8 W2 O5 101.6(4) . . ?
O8 W2 O6 98.0(4) . 6_565 ?
O8 W2 O6 98.0(4) . . ?
O3 W3 O2 84.8(3) . . ?
O3 W3 O6 88.5(4) . . ?
O3 W3 O15 160.6(4) . . ?
O6 W3 O2 72.8(4) . . ?
O9 W3 O2 170.7(4) . . ?
O9 W3 O3 99.8(4) . . ?
O9 W3 O6 99.1(4) . . ?
O9 W3 O15 99.3(5) . . ?
O9 W3 O16 104.1(4) . . ?
O15 W3 O2 75.9(4) . . ?
O15 W3 O6 85.1(4) . . ?
O16 W3 O2 84.0(4) . . ?
O16 W3 O3 89.1(4) . . ?
O16 W3 O6 156.7(4) . . ?
O16 W3 O15 89.6(4) . . ?
O3 W4 O1 85.2(3) . . ?
O3 W4 O4 89.1(4) . . ?
O3 W4 O9AA 158.7(3) . . ?
O4 W4 O1 72.9(3) . . ?
O9AA W4 O1 73.5(3) . . ?
O9AA W4 O4 84.6(4) . . ?
O10 W4 O1 169.2(4) . . ?
O10 W4 O3 101.3(4) . . ?
O10 W4 O4 98.4(4) . . ?
O10 W4 O9AA 99.7(4) . . ?
O10 W4 O17 104.0(4) . . ?
O17 W4 O1 84.4(3) . . ?
O17 W4 O3 90.0(3) . . ?
O17 W4 O4 157.3(4) . . ?
O17 W4 O9AA 88.1(4) . . ?
O9AA W5 O1 74.0(3) . . ?
O9AA W5 O12 85.1(4) . . ?
O9AA W5 O13 159.8(4) . . ?
O11 W5 O1 168.6(3) . . ?
O11 W5 O9AA 97.6(4) . . ?
O11 W5 O12 98.3(4) . . ?
O11 W5 O13 102.3(4) . . ?
O11 W5 O20 103.8(4) . . ?
O12 W5 O1 73.7(3) . . ?
O13 W5 O1 85.8(4) . . ?
O13 W5 O12 89.0(4) . . ?
O20 W5 O1 84.2(3) . . ?
O20 W5 O9AA 89.9(4) . . ?
O20 W5 O12 157.9(4) . . ?
O20 W5 O13 88.4(4) . . ?
O1 Sb1 O1 92.4(4) 6_565 . ?
O2 Sb1 O1 90.2(3) . . ?
O2 Sb1 O1 90.2(3) . 6_565 ?
Zn2 Zn1 Zn2 120.89(7) . 6_565 ?
O16 Zn1 Zn2 39.6(2) 2_756 6_565 ?
O16 Zn1 Zn2 116.2(2) 2_756 . ?
O16 Zn1 Zn2 116.2(2) 5_766 6_565 ?
O16 Zn1 Zn2 39.6(2) 5_766 . ?
O16 Zn1 O16 88.3(4) 2_756 5_766 ?
O18 Zn1 Zn2 119.55(4) . 6_565 ?
O18 Zn1 Zn2 119.55(4) . . ?
O18 Zn1 O16 109.9(3) . 5_766 ?
O18 Zn1 O16 109.9(3) . 2_756 ?
O18 Zn1 O20 104.5(3) . . ?
O18 Zn1 O20 104.5(3) . 6_565 ?
O20 Zn1 Zn2 119.8(3) 6_565 6_565 ?
O20 Zn1 Zn2 41.3(2) 6_565 . ?
O20 Zn1 Zn2 41.3(2) . 6_565 ?
O20 Zn1 Zn2 119.8(3) . . ?
O20 Zn1 O16 80.0(3) . 2_756 ?
O20 Zn1 O16 80.0(3) 6_565 5_766 ?
O20 Zn1 O16 145.6(3) 6_565 2_756 ?
O20 Zn1 O16 145.6(3) . 5_766 ?
O20 Zn1 O20 91.6(5) . 6_565 ?
Zn2 Zn2 Zn1 119.50(4) 2_756 . ?
O16 Zn2 Zn1 40.4(2) 5_766 . ?
O16 Zn2 Zn2 117.5(2) 5_766 2_756 ?
O16 Zn2 O17 91.3(3) 5_766 5_766 ?
O16 Zn2 O17 144.9(3) 5_766 6_565 ?
O16 Zn2 O20 79.1(3) 5_766 6_565 ?
O17 Zn2 Zn1 116.4(2) 6_565 . ?
O17 Zn2 Zn1 119.1(2) 5_766 . ?
O17 Zn2 Zn2 40.4(2) 5_766 2_756 ?
O17 Zn2 Zn2 41.3(2) 6_565 2_756 ?
O17 Zn2 O17 80.4(4) 6_565 5_766 ?
O17 Zn2 O20 88.8(3) 6_565 6_565 ?
O17 Zn2 O20 145.6(3) 5_766 6_565 ?
O19 Zn2 Zn1 118.3(3) . . ?
O19 Zn2 Zn2 121.9(3) . 2_756 ?
O19 Zn2 O16 102.3(4) . 5_766 ?
O19 Zn2 O17 103.5(3) . 5_766 ?
O19 Zn2 O17 112.8(4) . 6_565 ?
O19 Zn2 O20 110.7(3) . 6_565 ?
O20 Zn2 Zn1 39.6(2) 6_565 . ?
O20 Zn2 Zn2 116.7(2) 6_565 2_756 ?
W4 O1 W1 94.0(3) . . ?
W4 O1 W5 94.4(3) . . ?
W5 O1 W1 93.3(3) . . ?
Sb1 O1 W1 136.6(4) . . ?
Sb1 O1 W4 115.4(4) . . ?
Sb1 O1 W5 114.0(3) . . ?
W2 O2 W3 93.8(4) . 6_565 ?
W2 O2 W3 93.8(4) . . ?
W3 O2 W3 92.2(4) 6_565 . ?
Sb1 O2 W2 138.4(6) . . ?
Sb1 O2 W3 114.1(4) . . ?
Sb1 O2 W3 114.1(4) . 6_565 ?
W4 O3 W3 153.2(5) . . ?
W1 O4 W4 120.0(4) . . ?
W2 O5 W1 150.7(5) . . ?
W2 O6 W3 119.4(5) . . ?
W5 O9AA W4 117.6(4) . . ?
W1 O12 W5 119.6(4) . . ?
W5 O13 W5 153.8(6) . 6_565 ?
W1 O14 W1 153.6(7) . 6_565 ?
W3 O15 W3 115.5(6) 6_565 . ?
W3 O16 Zn1 125.7(4) . 5_766 ?
W3 O16 Zn2 131.5(4) . 5_766 ?
Zn2 O16 Zn1 100.0(3) 5_766 5_766 ?
W4 O17 Zn2 129.2(5) . 6_565 ?
W4 O17 Zn2 131.1(4) . 5_766 ?
Zn2 O17 Zn2 98.3(3) 6_565 5_766 ?
W5 O20 Zn1 133.4(5) . . ?
W5 O20 Zn2 125.8(5) . 6_565 ?
Zn1 O20 Zn2 99.1(3) . 6_565 ?
C1 N1 C3 107.4(14) . . ?
C2 N1 C1 101(2) . . ?
C2 N1 C3 103.8(17) . . ?
C2 N1 C4 114(2) . . ?
C4 N1 C1 116.7(18) . . ?
C4 N1 C3 112.3(16) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O1 W1 O4 W4 0.3(4) . . . . ?
O1 W4 O17 Zn2 80.3(5) . . . 6_565 ?
O1 W4 O17 Zn2 -116.4(5) . . . 5_766 ?
O1 W5 O20 Zn1 117.8(6) . . . . ?
O1 W5 O20 Zn2 -80.4(5) . . . 6_565 ?
O2 W2 O5 W1 58.3(10) . . . . ?
O2 W3 O16 Zn1 -83.2(5) . . . 5_766 ?
O2 W3 O16 Zn2 119.9(6) . . . 5_766 ?
O3 W3 O16 Zn1 -168.0(5) . . . 5_766 ?
O3 W3 O16 Zn2 35.0(6) . . . 5_766 ?
O3 W4 O17 Zn2 -31.2(6) . . . 5_766 ?
O3 W4 O17 Zn2 165.5(5) . . . 6_565 ?
O4 W4 O17 Zn2 77.8(11) . . . 6_565 ?
O4 W4 O17 Zn2 -118.9(10) . . . 5_766 ?
O5 W1 O4 W4 86.6(5) . . . . ?
O5 W2 O5 W1 -28.4(12) 6_565 . . . ?
O6 W2 O5 W1 50.6(17) 6_565 . . . ?
O6 W2 O5 W1 132.3(10) . . . . ?
O6 W3 O16 Zn1 -83.9(10) . . . 5_766 ?
O6 W3 O16 Zn2 119.2(8) . . . 5_766 ?
O7 W1 O4 W4 -171.6(6) . . . . ?
O8 W2 O5 W1 -129.7(10) . . . . ?
O9 W3 O16 Zn1 92.1(6) . . . 5_766 ?
O9 W3 O16 Zn2 -64.8(7) . . . 5_766 ?
O9AA W4 O17 Zn2 170.0(5) . . . 5_766 ?
O9AA W4 O17 Zn2 6.7(5) . . . 6_565 ?
O9AA W5 O20 Zn1 -168.2(7) . . . . ?
O9AA W5 O20 Zn2 -6.5(5) . . . 6_565 ?
O10 W4 O17 Zn2 70.5(6) . . . 5_766 ?
O10 W4 O17 Zn2 -92.9(6) . . . 6_565 ?
O11 W5 O20 Zn1 -70.4(7) . . . . ?
O11 W5 O20 Zn2 91.4(6) . . . 6_565 ?
O12 W1 O4 W4 -72.5(5) . . . . ?
O12 W5 O20 Zn1 115.2(10) . . . . ?
O12 W5 O20 Zn2 -83.0(11) . . . 6_565 ?
O13 W5 O20 Zn1 31.9(7) . . . . ?
O13 W5 O20 Zn2 -166.4(6) . . . 6_565 ?
O14 W1 O4 W4 15.6(15) . . . . ?
O15 W3 O16 Zn1 -7.4(6) . . . 5_766 ?
O15 W3 O16 Zn2 -164.3(6) . . . 5_766 ?

