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

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

data_Na1Ni5_1
_audit_block_doi                 10.5517/ccdc.csd.cc204qqm
_database_code_depnum_ccdc_archive 'CCDC 1851590'
loop_
_citation_id
_citation_doi
_citation_year
1 10.1039/C8CC07884J 2019
loop_
_audit_author_name
_audit_author_address
'Lubin Ni'
;School of Chemistry and Chemical Engineering, Yangzhou University
China
;
_audit_update_record             
;
2018-10-02 deposited with the CCDC.	2020-02-05 downloaded from the CCDC.
;

_publ_intended_journal           Chem.Commun

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C25 N10 Na1.70 Ni5.30 O82 Sb2 W18'
_chemical_formula_weight         5655.40

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'
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'
Ni Ni 0.3393 1.1124 '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'

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

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

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

_cell_length_a                   22.4271(14)
_cell_length_b                   22.3391(14)
_cell_length_c                   25.7151(15)
_cell_angle_alpha                90
_cell_angle_beta                 114.014(2)
_cell_angle_gamma                90
_cell_volume                     11768.2(13)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    9899
_cell_measurement_theta_min      2.2709
_cell_measurement_theta_max      27.5398

_exptl_crystal_description       bluk
_exptl_crystal_colour            orange
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    3.192
_exptl_crystal_F_000             9908
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.09
_exptl_absorpt_coefficient_mu    18.885
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.729
_exptl_absorpt_correction_T_max  0.788
_exptl_absorpt_process_details   
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET)
(compiled Nov  6 2009,16:24:50)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   
;
 ?
;
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  graphite
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            55150
_diffrn_reflns_av_unetI/netI     0.0365
_diffrn_reflns_av_R_equivalents  0.0380
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_theta_min         1.809
_diffrn_reflns_theta_max         27.103
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measured_fraction_theta_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_point_group_measured_fraction_full 0.991
_reflns_number_total             12881
_reflns_number_gt                10150
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 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.
;

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and
 goodness of fit S are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The threshold expression of
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
 not relevant to the choice of reflections for refinement.  R-factors based
 on F² are statistically about twice as large as those based on F, and R-
 factors based on ALL data will be even larger.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0327P)²+636.8115P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   .
_refine_ls_hydrogen_treatment    undef
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_extinction_coef       0.000107(7)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         12881
_refine_ls_number_parameters     589
_refine_ls_number_restraints     20
_refine_ls_R_factor_all          0.0705
_refine_ls_R_factor_gt           0.0517
_refine_ls_wR_factor_ref         0.1241
_refine_ls_wR_factor_gt          0.1123
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_restrained_S_all      1.066
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
W1 W 0.77689(3) 0.60925(3) 0.40185(3) 0.05874(18) Uani 1 1 d . . . . .
W2 W 0.79653(3) 0.46553(3) 0.33797(3) 0.06273(19) Uani 1 1 d . . . . .
W3 W 0.75584(3) 0.46477(3) 0.46393(3) 0.06194(19) Uani 1 1 d . . . . .
W4 W 0.60755(3) 0.51011(2) 0.44904(2) 0.04033(14) Uani 1 1 d . . . . .
W5 W 0.62574(3) 0.37913(2) 0.39304(2) 0.04394(14) Uani 1 1 d . . . . .
W6 W 0.66705(3) 0.37884(2) 0.26599(2) 0.04406(14) Uani 1 1 d . . . . .
W7 W 0.37258(3) 0.65371(2) 0.11467(2) 0.04161(14) Uani 1 1 d . . . . .
W8 W 0.33388(3) 0.65233(2) 0.22676(2) 0.04169(14) Uani 1 1 d . . . . .
W9 W 0.31373(3) 0.50832(2) 0.29008(2) 0.04305(14) Uani 1 1 d . . . . .
Sb1 Sb 0.61385(9) 0.51317(9) 0.31184(8) 0.0283(4) Uani 0.8 1 d . . P A 2
Sb2 Sb 0.6278(3) 0.5144(4) 0.3196(3) 0.0196(16) Uiso 0.2 1 d . . P A 1
Ni1 Ni 0.5000 0.38132(9) 0.2500 0.0334(4) Uani 1 2 d S T P . .
Ni2 Ni 0.46789(8) 0.43626(7) 0.35298(7) 0.0382(3) Uiso 1 1 d D . . . .
Ni3 Ni 0.47130(7) 0.58050(6) 0.33556(6) 0.0304(3) Uani 1 1 d . . . . .
Ni4 Ni 0.5000 0.6718(2) 0.2500 0.0470(10) Uani 0.3 2 d S T P B 1
Na1 Na 0.9244(5) 0.3768(6) 0.3195(6) 0.071(4) Uani 0.5 1 d . . P . .
Na2 Na 0.5000 0.6718(2) 0.2500 0.0470(10) Uani 0.7 2 d S T P B 2
O1 O 0.8532(6) 0.6376(7) 0.4428(6) 0.090(4) Uani 1 1 d . . . . .
O2 O 0.7559(5) 0.6568(5) 0.3353(5) 0.062(3) Uani 1 1 d . . . . .
O3 O 0.7235(5) 0.6570(5) 0.4272(4) 0.062(3) Uani 1 1 d . . . . .
O4 O 0.7713(5) 0.5451(6) 0.4497(4) 0.070(3) Uani 1 1 d . . . . .
O5 O 0.8009(4) 0.5458(5) 0.3620(5) 0.066(3) Uani 1 1 d . . . . .
O6 O 0.7775(5) 0.4918(5) 0.2609(5) 0.066(3) Uani 1 1 d . . . . .
O7 O 0.7614(5) 0.3878(5) 0.3077(5) 0.068(3) Uani 1 1 d . . . . .
O8 O 0.6854(4) 0.4764(4) 0.2951(4) 0.0407(19) Uani 1 1 d . . . . .
O9 O 0.7856(5) 0.4434(6) 0.4055(5) 0.074(3) Uani 1 1 d . . . . .
O10 O 0.8776(6) 0.4489(8) 0.3582(7) 0.108(5) Uani 1 1 d . . . . .
O11 O 0.6700(4) 0.5863(4) 0.3418(3) 0.0368(18) Uani 1 1 d . . . . .
O12 O 0.6536(4) 0.4769(4) 0.3898(3) 0.0378(18) Uani 1 1 d . . . . .
O13 O 0.6989(5) 0.4924(5) 0.4974(4) 0.061(3) Uani 1 1 d . . . . .
O14 O 0.7149(5) 0.3882(5) 0.4504(4) 0.066(3) Uani 1 1 d . . . . .
O16 O 0.6317(5) 0.5874(4) 0.4356(4) 0.051(2) Uani 1 1 d . . . . .
O17 O 0.5805(5) 0.5237(4) 0.5013(4) 0.056(3) Uani 1 1 d . . . . .
O18 O 0.5964(5) 0.4226(4) 0.4439(3) 0.045(2) Uani 1 1 d . . . . .
O19 O 0.6119(6) 0.3077(4) 0.4103(4) 0.063(3) Uani 1 1 d . . . . .
O20 O 0.6612(5) 0.3655(4) 0.3379(4) 0.053(2) Uani 1 1 d . . . . .
O21 O 0.6665(6) 0.3069(4) 0.2424(5) 0.070(3) Uani 1 1 d . . . . .
O22 O 0.5798(4) 0.4006(4) 0.2364(4) 0.043(2) Uani 1 1 d . . . . .
O23 O 0.5466(4) 0.3998(4) 0.3325(4) 0.044(2) Uani 1 1 d . . . . .
O24 O 0.5313(4) 0.5150(4) 0.3811(3) 0.0392(19) Uani 1 1 d . . . . .
O25 O 0.4172(4) 0.6265(4) 0.2659(3) 0.0390(18) Uani 1 1 d . . . . .
O26 O 0.4035(4) 0.5151(4) 0.3136(4) 0.043(2) Uani 1 1 d . . . . .
O27 O 0.4527(4) 0.6267(4) 0.1632(4) 0.0402(19) Uani 1 1 d . . . . .
O28 O 0.3889(6) 0.7121(4) 0.0792(4) 0.064(3) Uani 1 1 d . . . . .
O29 O 0.3605(5) 0.6971(4) 0.1749(4) 0.047(2) Uani 1 1 d . . . . .
O30 O 0.3253(6) 0.7116(4) 0.2663(5) 0.065(3) Uani 1 1 d . . . . .
O31 O 0.3039(5) 0.5868(4) 0.2584(4) 0.051(2) Uani 1 1 d . . . . .
O32 O 0.3019(6) 0.5205(5) 0.3513(5) 0.066(3) Uani 1 1 d . . . . .
O33 O 0.3238(5) 0.4220(4) 0.2961(4) 0.051(2) Uani 1 1 d . . . . .
O34 O 0.8628(14) 0.3093(13) 0.3367(13) 0.091(8) Uiso 0.5 1 d . . P C 1
O34A O 0.8611(19) 0.3250(19) 0.2975(18) 0.134(13) Uiso 0.5 1 d . . P C 2
O35 O 0.9865(10) 0.4606(12) 0.4020(14) 0.100(10) Uani 0.5 1 d . . P C 1
O35A O 0.879(2) 0.438(2) 0.236(2) 0.172(17) Uiso 0.5 1 d . . P C 2
O36 O 0.8257(6) 0.4490(7) 0.5238(6) 0.093(4) Uani 1 1 d . . . . .
N1 N 0.4531(6) 0.6210(5) 0.3970(4) 0.042(2) Uani 1 1 d . . . . .
N2 N 0.4341(8) 0.6298(6) 0.4722(5) 0.068(4) Uani 1 1 d . . . . .
N3 N 0.5095(11) 0.2576(7) 0.2105(10) 0.113(7) Uani 1 1 d . . . . .
C1 C 0.4391(8) 0.5923(6) 0.4348(6) 0.053(4) Uani 1 1 d . . . . .
C2 C 0.4470(13) 0.6851(9) 0.4583(9) 0.094(7) Uani 1 1 d . . . . .
C3 C 0.4570(9) 0.6802(6) 0.4098(7) 0.063(4) Uani 1 1 d . . . . .
C4 C 0.5000 0.2932(7) 0.2500 0.031(3) Uiso 1 2 d S . P D 1
C5 C 0.5063(13) 0.1994(6) 0.2272(10) 0.097(7) Uani 1 1 d . . . . .
O37 O 0.4374(14) 0.3892(13) 0.4227(11) 0.198(11) Uani 1 1 d D . . . .
O38 O 0.897(5) 0.357(5) 0.456(4) 0.35(5) Uiso 0.5 1 d . . P E 1
O38A O 0.836(2) 0.319(2) 0.440(2) 0.161(16) Uiso 0.5 1 d . . P F 2
O39 O 0.5676(15) 0.2032(15) 0.4439(13) 0.224(12) Uiso 1 1 d . . . . .
O40 O 0.4368(15) 0.8020(14) 0.0375(13) 0.217(12) Uiso 1 1 d . . . . .
O41 O 0.8668(17) 0.5927(16) 0.2761(15) 0.241(14) Uiso 1 1 d . . . . .
O42 O 0.6411(8) 0.2057(10) 0.1763(9) 0.153(8) Uani 1 1 d . . . . .
N4 N 0.2605(16) 0.3416(15) 0.4033(14) 0.201(14) Uiso 1 1 d D . . . .
C6 C 0.2658(19) 0.4111(15) 0.4095(16) 0.179(15) Uiso 1 1 d D . . . .
C7 C 0.2339(19) 0.3271(18) 0.3387(15) 0.194(16) Uiso 1 1 d D . . . .
C8 C 0.338(2) 0.321(3) 0.430(3) 0.44(5) Uiso 1 1 d D . . . .
C9 C 0.230(3) 0.311(3) 0.437(3) 0.42(5) Uiso 1 1 d D . . . .
N5 N 0.7267(12) 0.1841(11) 0.3816(10) 0.134(8) Uiso 1 1 d D . . . .
C11 C 0.743(2) 0.207(2) 0.4436(15) 0.25(2) Uiso 1 1 d D . . . .
C12 C 0.734(4) 0.1177(18) 0.380(3) 0.48(6) Uiso 1 1 d D . . . .
C13 C 0.773(3) 0.219(3) 0.357(3) 0.47(6) Uiso 1 1 d D . . . .
C14 C 0.6589(19) 0.211(2) 0.3419(17) 0.208(18) Uiso 1 1 d D . . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
W1 O1 1.725(11) . ?
W1 O2 1.904(11) . ?
W1 O3 1.904(12) . ?
W1 O4 1.926(11) . ?
W1 O5 1.950(12) . ?
W1 O11 2.319(8) . ?
W2 O10 1.716(11) . ?
W2 O5 1.886(12) . ?
W2 O9 1.915(11) . ?
W2 O7 1.935(13) . ?
W2 O6 1.941(12) . ?
W2 O8 2.291(8) . ?
W2 Na1 3.674(12) . ?
W3 O36 1.728(11) . ?
W3 O4 1.891(12) . ?
W3 O14 1.905(12) . ?
W3 O13 1.910(12) . ?
W3 O9 1.935(11) . ?
W3 O12 2.324(8) . ?
W4 O17 1.711(9) . ?
W4 O16 1.882(9) . ?
W4 O24 1.887(8) . ?
W4 O13 1.956(10) . ?
W4 O18 1.967(9) . ?
W4 O12 2.285(8) . ?
W5 O19 1.718(9) . ?
W5 O23 1.881(9) . ?
W5 O20 1.912(9) . ?
W5 O18 1.946(9) . ?
W5 O14 1.953(11) . ?
W5 O12 2.282(8) . ?
W6 O21 1.716(10) . ?
W6 O22 1.852(9) . ?
W6 O20 1.929(9) . ?
W6 O33 1.945(9) 2_655 ?
W6 O7 1.954(11) . ?
W6 O8 2.287(9) . ?
W7 O28 1.714(10) . ?
W7 O27 1.824(8) . ?
W7 O29 1.937(8) . ?
W7 O16 1.944(9) 2_655 ?
W7 O3 1.980(10) 2_655 ?
W7 O11 2.303(8) 2_655 ?
W7 Na2 3.5136(8) . ?
W8 O30 1.726(9) . ?
W8 O25 1.819(8) . ?
W8 O31 1.923(9) . ?
W8 O29 1.945(9) . ?
W8 O2 2.000(10) 2_655 ?
W8 O11 2.274(8) 2_655 ?
W8 Na2 3.5517(8) . ?
W9 O32 1.721(10) . ?
W9 O26 1.858(9) . ?
W9 O31 1.909(10) . ?
W9 O33 1.941(9) . ?
W9 O6 1.964(11) 2_655 ?
W9 O8 2.310(8) 2_655 ?
Sb1 O8 2.000(9) . ?
Sb1 O12 2.004(8) . ?
Sb1 O11 2.014(8) . ?
Sb2 O11 1.833(11) . ?
Sb2 O12 1.857(11) . ?
Sb2 O8 1.858(12) . ?
Ni1 C4 1.969(16) . ?
Ni1 O23 1.989(8) . ?
Ni1 O23 1.989(8) 2_655 ?
Ni1 O22 2.005(8) 2_655 ?
Ni1 O22 2.005(8) . ?
Ni2 O24 2.191(8) . ?
Ni2 O23 2.196(9) . ?
Ni2 O26 2.240(9) . ?
Ni2 O22 2.249(9) 2_655 ?
Ni2 O37 2.40(2) . ?
Ni3 O27 1.982(8) 2_655 ?
Ni3 O25 1.991(8) . ?
Ni3 N1 2.001(9) . ?
Ni3 O24 2.010(8) . ?
Ni3 O26 2.016(8) . ?
Ni3 Na2 3.250(3) . ?
Ni4 O27 2.278(9) . ?
Ni4 O27 2.278(9) 2_655 ?
Ni4 O25 2.293(9) 2_655 ?
Ni4 O25 2.293(9) . ?
Na1 O34A 1.74(4) . ?
Na1 O34 2.21(3) . ?
Na1 O10 2.35(2) . ?
Na1 O35A 2.38(5) . ?
Na1 O35 2.75(3) . ?
Na2 O27 2.278(9) . ?
Na2 O27 2.278(9) 2_655 ?
Na2 O25 2.293(9) 2_655 ?
Na2 O25 2.293(9) . ?
Na2 O29 2.986(9) 2_655 ?
Na2 O29 2.986(9) . ?
Na2 Ni3 3.250(3) 2_655 ?
Na2 W7 3.5136(8) 2_655 ?
Na2 W8 3.5517(8) 2_655 ?
O2 W8 2.000(10) 2_655 ?
O3 W7 1.980(10) 2_655 ?
O6 W9 1.964(11) 2_655 ?
O8 W9 2.310(8) 2_655 ?
O11 W8 2.274(8) 2_655 ?
O11 W7 2.303(8) 2_655 ?
O16 W7 1.944(9) 2_655 ?
O22 Ni2 2.249(9) 2_655 ?
O27 Ni3 1.982(8) 2_655 ?
O33 W6 1.945(9) 2_655 ?
N1 C1 1.305(16) . ?
N1 C3 1.357(16) . ?
N2 C1 1.313(18) . ?
N2 C2 1.35(2) . ?
N3 C4 1.37(2) . ?
N3 C5 1.38(2) . ?
C2 C3 1.36(2) . ?
C4 N3 1.37(2) 2_655 ?
C5 C5 1.31(4) 2_655 ?
N4 C9 1.49(4) . ?
N4 C7 1.55(3) . ?
N4 C6 1.56(3) . ?
N4 C8 1.66(4) . ?
N5 C12 1.49(4) . ?
N5 C14 1.57(4) . ?
N5 C11 1.57(3) . ?
N5 C13 1.62(4) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 W1 O2 99.5(6) . . ?
O1 W1 O3 101.0(6) . . ?
O2 W1 O3 92.0(5) . . ?
O1 W1 O4 100.9(6) . . ?
O2 W1 O4 159.0(4) . . ?
O3 W1 O4 89.1(5) . . ?
O1 W1 O5 99.8(6) . . ?
O2 W1 O5 87.3(5) . . ?
O3 W1 O5 159.0(4) . . ?
O4 W1 O5 84.2(5) . . ?
O1 W1 O11 171.1(5) . . ?
O2 W1 O11 73.5(3) . . ?
O3 W1 O11 74.3(3) . . ?
O4 W1 O11 86.7(3) . . ?
O5 W1 O11 85.5(3) . . ?
O10 W2 O5 101.5(7) . . ?
O10 W2 O9 100.4(6) . . ?
O5 W2 O9 87.5(6) . . ?
O10 W2 O7 97.8(7) . . ?
O5 W2 O7 160.7(4) . . ?
O9 W2 O7 87.3(5) . . ?
O10 W2 O6 98.0(6) . . ?
O5 W2 O6 90.4(5) . . ?
O9 W2 O6 161.5(4) . . ?
O7 W2 O6 88.6(5) . . ?
O10 W2 O8 168.4(7) . . ?
O5 W2 O8 87.6(3) . . ?
O9 W2 O8 87.1(4) . . ?
O7 W2 O8 73.5(4) . . ?
O6 W2 O8 74.5(4) . . ?
O10 W2 Na1 30.2(7) . . ?
O5 W2 Na1 128.0(3) . . ?
O9 W2 Na1 111.9(4) . . ?
O7 W2 Na1 71.0(3) . . ?
O6 W2 Na1 83.7(4) . . ?
O8 W2 Na1 138.5(3) . . ?
O36 W3 O4 101.2(6) . . ?
O36 W3 O14 100.1(6) . . ?
O4 W3 O14 158.3(4) . . ?
O36 W3 O13 101.2(6) . . ?
O4 W3 O13 89.4(5) . . ?
O14 W3 O13 90.6(5) . . ?
O36 W3 O9 99.6(6) . . ?
O4 W3 O9 86.3(6) . . ?
O14 W3 O9 86.0(5) . . ?
O13 W3 O9 159.2(4) . . ?
O36 W3 O12 171.2(5) . . ?
O4 W3 O12 85.9(3) . . ?
O14 W3 O12 73.4(3) . . ?
O13 W3 O12 73.4(3) . . ?
O9 W3 O12 85.9(3) . . ?
O17 W4 O16 101.7(4) . . ?
O17 W4 O24 103.9(4) . . ?
O16 W4 O24 89.9(4) . . ?
O17 W4 O13 98.7(5) . . ?
O16 W4 O13 89.8(4) . . ?
O24 W4 O13 157.0(4) . . ?
O17 W4 O18 98.8(4) . . ?
O16 W4 O18 159.4(4) . . ?
O24 W4 O18 87.3(3) . . ?
O13 W4 O18 85.0(4) . . ?
O17 W4 O12 169.1(4) . . ?
O16 W4 O12 86.2(4) . . ?
O24 W4 O12 83.5(3) . . ?
O13 W4 O12 73.6(4) . . ?
O18 W4 O12 73.3(3) . . ?
O19 W5 O23 103.5(5) . . ?
O19 W5 O20 102.5(4) . . ?
O23 W5 O20 87.8(4) . . ?
O19 W5 O18 98.3(4) . . ?
O23 W5 O18 88.3(4) . . ?
O20 W5 O18 159.1(4) . . ?
O19 W5 O14 97.9(5) . . ?
O23 W5 O14 158.5(4) . . ?
O20 W5 O14 88.3(5) . . ?
O18 W5 O14 87.9(4) . . ?
O19 W5 O12 168.2(4) . . ?
O23 W5 O12 85.1(3) . . ?
O20 W5 O12 85.6(4) . . ?
O18 W5 O12 73.7(3) . . ?
O14 W5 O12 73.5(4) . . ?
O21 W6 O22 104.3(5) . . ?
O21 W6 O20 101.6(5) . . ?
O22 W6 O20 87.8(4) . . ?
O21 W6 O33 99.3(4) . 2_655 ?
O22 W6 O33 88.8(4) . 2_655 ?
O20 W6 O33 159.1(4) . 2_655 ?
O21 W6 O7 98.0(5) . . ?
O22 W6 O7 157.7(4) . . ?
O20 W6 O7 88.3(4) . . ?
O33 W6 O7 86.9(4) 2_655 . ?
O21 W6 O8 169.3(5) . . ?
O22 W6 O8 84.5(3) . . ?
O20 W6 O8 84.7(4) . . ?
O33 W6 O8 74.4(4) 2_655 . ?
O7 W6 O8 73.3(4) . . ?
O28 W7 O27 104.6(5) . . ?
O28 W7 O29 100.0(4) . . ?
O27 W7 O29 92.1(4) . . ?
O28 W7 O16 100.9(4) . 2_655 ?
O27 W7 O16 88.4(4) . 2_655 ?
O29 W7 O16 158.2(4) . 2_655 ?
O28 W7 O3 96.0(5) . 2_655 ?
O27 W7 O3 159.3(4) . 2_655 ?
O29 W7 O3 86.6(4) . 2_655 ?
O16 W7 O3 85.3(4) 2_655 2_655 ?
O28 W7 O11 167.6(4) . 2_655 ?
O27 W7 O11 86.5(3) . 2_655 ?
O29 W7 O11 73.6(3) . 2_655 ?
O16 W7 O11 84.6(3) 2_655 2_655 ?
O3 W7 O11 73.3(4) 2_655 2_655 ?
O28 W7 Na2 100.1(4) . . ?
O27 W7 Na2 35.1(3) . . ?
O29 W7 Na2 58.2(3) . . ?
O16 W7 Na2 123.1(3) 2_655 . ?
O3 W7 Na2 143.2(3) 2_655 . ?
O11 W7 Na2 85.7(2) 2_655 . ?
O30 W8 O25 104.6(5) . . ?
O30 W8 O31 101.1(4) . . ?
O25 W8 O31 89.0(4) . . ?
O30 W8 O29 98.5(4) . . ?
O25 W8 O29 90.6(4) . . ?
O31 W8 O29 159.8(4) . . ?
O30 W8 O2 96.6(5) . 2_655 ?
O25 W8 O2 158.8(4) . 2_655 ?
O31 W8 O2 87.9(4) . 2_655 ?
O29 W8 O2 85.3(4) . 2_655 ?
O30 W8 O11 167.4(4) . 2_655 ?
O25 W8 O11 86.0(3) . 2_655 ?
O31 W8 O11 85.7(3) . 2_655 ?
O29 W8 O11 74.2(3) . 2_655 ?
O2 W8 O11 72.8(4) 2_655 2_655 ?
O30 W8 Na2 99.6(4) . . ?
O25 W8 Na2 34.4(3) . . ?
O31 W8 Na2 123.0(3) . . ?
O29 W8 Na2 57.2(3) . . ?
O2 W8 Na2 140.8(3) 2_655 . ?
O11 W8 Na2 85.2(2) 2_655 . ?
O32 W9 O26 103.9(5) . . ?
O32 W9 O31 102.2(5) . . ?
O26 W9 O31 89.2(4) . . ?
O32 W9 O33 98.1(5) . . ?
O26 W9 O33 88.8(4) . . ?
O31 W9 O33 159.5(4) . . ?
O32 W9 O6 97.7(5) . 2_655 ?
O26 W9 O6 158.3(4) . 2_655 ?
O31 W9 O6 88.9(5) . 2_655 ?
O33 W9 O6 85.5(5) . 2_655 ?
O32 W9 O8 168.4(4) . 2_655 ?
O26 W9 O8 84.7(3) . 2_655 ?
O31 W9 O8 85.6(3) . 2_655 ?
O33 W9 O8 73.9(3) . 2_655 ?
O6 W9 O8 73.6(4) 2_655 2_655 ?
O8 Sb1 O12 88.8(3) . . ?
O8 Sb1 O11 89.1(3) . . ?
O12 Sb1 O11 89.5(3) . . ?
O11 Sb2 O12 100.1(5) . . ?
O11 Sb2 O8 99.4(5) . . ?
O12 Sb2 O8 97.9(5) . . ?
C4 Ni1 O23 102.0(3) . . ?
C4 Ni1 O23 102.0(3) . 2_655 ?
O23 Ni1 O23 156.1(5) . 2_655 ?
C4 Ni1 O22 102.4(3) . 2_655 ?
O23 Ni1 O22 83.6(4) . 2_655 ?
O23 Ni1 O22 91.3(4) 2_655 2_655 ?
C4 Ni1 O22 102.4(3) . . ?
O23 Ni1 O22 91.3(4) . . ?
O23 Ni1 O22 83.6(4) 2_655 . ?
O22 Ni1 O22 155.2(5) 2_655 . ?
O24 Ni2 O23 84.2(3) . . ?
O24 Ni2 O26 74.4(3) . . ?
O23 Ni2 O26 128.0(3) . . ?
O24 Ni2 O22 126.6(3) . 2_655 ?
O23 Ni2 O22 73.6(3) . 2_655 ?
O26 Ni2 O22 82.3(3) . 2_655 ?
O24 Ni2 O37 116.6(7) . . ?
O23 Ni2 O37 121.1(8) . . ?
O26 Ni2 O37 110.8(8) . . ?
O22 Ni2 O37 116.5(7) 2_655 . ?
O27 Ni3 O25 87.2(3) 2_655 . ?
O27 Ni3 N1 101.7(4) 2_655 . ?
O25 Ni3 N1 103.3(4) . . ?
O27 Ni3 O24 90.2(3) 2_655 . ?
O25 Ni3 O24 156.6(3) . . ?
N1 Ni3 O24 100.0(4) . . ?
O27 Ni3 O26 158.0(4) 2_655 . ?
O25 Ni3 O26 90.5(4) . . ?
N1 Ni3 O26 100.2(4) . . ?
O24 Ni3 O26 83.4(4) . . ?
O27 Ni3 Na2 43.8(2) 2_655 . ?
O25 Ni3 Na2 44.2(2) . . ?
N1 Ni3 Na2 114.2(3) . . ?
O24 Ni3 Na2 125.5(3) . . ?
O26 Ni3 Na2 126.8(3) . . ?
O27 Ni4 O27 127.6(5) . 2_655 ?
O27 Ni4 O25 73.6(3) . 2_655 ?
O27 Ni4 O25 83.8(3) 2_655 2_655 ?
O27 Ni4 O25 83.8(3) . . ?
O27 Ni4 O25 73.6(3) 2_655 . ?
O25 Ni4 O25 127.7(5) 2_655 . ?
O34A Na1 O10 98.4(15) . . ?
O34 Na1 O10 87.7(10) . . ?
O34A Na1 O35A 95.3(19) . . ?
O10 Na1 O35A 83.5(13) . . ?
O34 Na1 O35 118.2(12) . . ?
O10 Na1 O35 51.6(7) . . ?
O34A Na1 W2 79.8(14) . . ?
O34 Na1 W2 75.9(8) . . ?
O10 Na1 W2 21.5(4) . . ?
O35A Na1 W2 74.7(12) . . ?
O35 Na1 W2 73.1(6) . . ?
O27 Na2 O27 127.6(5) . 2_655 ?
O27 Na2 O25 73.6(3) . 2_655 ?
O27 Na2 O25 83.8(3) 2_655 2_655 ?
O27 Na2 O25 83.8(3) . . ?
O27 Na2 O25 73.6(3) 2_655 . ?
O25 Na2 O25 127.7(5) 2_655 . ?
O27 Na2 O29 131.7(3) . 2_655 ?
O27 Na2 O29 60.2(3) 2_655 2_655 ?
O25 Na2 O29 59.2(3) 2_655 2_655 ?
O25 Na2 O29 132.8(3) . 2_655 ?
O27 Na2 O29 60.2(3) . . ?
O27 Na2 O29 131.7(3) 2_655 . ?
O25 Na2 O29 132.8(3) 2_655 . ?
O25 Na2 O29 59.2(3) . . ?
O29 Na2 O29 158.2(4) 2_655 . ?
O27 Na2 Ni3 37.0(2) . 2_655 ?
O27 Na2 Ni3 104.1(3) 2_655 2_655 ?
O25 Na2 Ni3 37.3(2) 2_655 2_655 ?
O25 Na2 Ni3 104.0(2) . 2_655 ?
O29 Na2 Ni3 96.48(18) 2_655 2_655 ?
O29 Na2 Ni3 97.18(17) . 2_655 ?
O27 Na2 Ni3 104.1(3) . . ?
O27 Na2 Ni3 37.0(2) 2_655 . ?
O25 Na2 Ni3 104.0(2) 2_655 . ?
O25 Na2 Ni3 37.3(2) . . ?
O29 Na2 Ni3 97.18(17) 2_655 . ?
O29 Na2 Ni3 96.48(18) . . ?
Ni3 Na2 Ni3 102.30(14) 2_655 . ?
O27 Na2 W7 141.8(3) . 2_655 ?
O27 Na2 W7 27.4(2) 2_655 2_655 ?
O25 Na2 W7 74.6(2) 2_655 2_655 ?
O25 Na2 W7 99.4(2) . 2_655 ?
O29 Na2 W7 33.44(16) 2_655 2_655 ?
O29 Na2 W7 151.40(17) . 2_655 ?
Ni3 Na2 W7 107.05(8) 2_655 2_655 ?
Ni3 Na2 W7 64.08(4) . 2_655 ?
O27 Na2 W7 27.4(2) . . ?
O27 Na2 W7 141.8(3) 2_655 . ?
O25 Na2 W7 99.4(2) 2_655 . ?
O25 Na2 W7 74.6(2) . . ?
O29 Na2 W7 151.40(17) 2_655 . ?
O29 Na2 W7 33.44(16) . . ?
Ni3 Na2 W7 64.08(4) 2_655 . ?
Ni3 Na2 W7 107.05(8) . . ?
W7 Na2 W7 166.82(15) 2_655 . ?
O27 Na2 W8 98.6(2) . 2_655 ?
O27 Na2 W8 75.1(2) 2_655 2_655 ?
O25 Na2 W8 26.6(2) 2_655 2_655 ?
O25 Na2 W8 141.8(3) . 2_655 ?
O29 Na2 W8 33.21(17) 2_655 2_655 ?
O29 Na2 W8 152.00(17) . 2_655 ?
Ni3 Na2 W8 63.52(4) 2_655 2_655 ?
Ni3 Na2 W8 107.01(8) . 2_655 ?
W7 Na2 W8 56.269(16) 2_655 2_655 ?
W7 Na2 W8 121.82(4) . 2_655 ?
O27 Na2 W8 75.1(2) . . ?
O27 Na2 W8 98.6(2) 2_655 . ?
O25 Na2 W8 141.8(3) 2_655 . ?
O25 Na2 W8 26.6(2) . . ?
O29 Na2 W8 152.00(17) 2_655 . ?
O29 Na2 W8 33.21(17) . . ?
Ni3 Na2 W8 107.01(8) 2_655 . ?
Ni3 Na2 W8 63.52(4) . . ?
W7 Na2 W8 121.82(4) 2_655 . ?
W7 Na2 W8 56.269(16) . . ?
W8 Na2 W8 165.96(15) 2_655 . ?
W1 O2 W8 119.3(5) . 2_655 ?
W1 O3 W7 119.3(5) . 2_655 ?
W3 O4 W1 153.4(7) . . ?
W2 O5 W1 151.0(6) . . ?
W2 O6 W9 118.3(5) . 2_655 ?
W2 O7 W6 119.0(5) . . ?
Sb2 O8 W6 119.3(5) . . ?
Sb1 O8 W6 114.1(4) . . ?
Sb2 O8 W2 131.0(5) . . ?
Sb1 O8 W2 138.7(4) . . ?
W6 O8 W2 94.1(3) . . ?
Sb2 O8 W9 117.1(4) . 2_655 ?
Sb1 O8 W9 113.2(4) . 2_655 ?
W6 O8 W9 93.1(3) . 2_655 ?
W2 O8 W9 93.6(3) . 2_655 ?
W2 O9 W3 148.4(7) . . ?
W2 O10 Na1 128.3(10) . . ?
Sb2 O11 W8 118.3(5) . 2_655 ?
Sb1 O11 W8 114.1(4) . 2_655 ?
Sb2 O11 W7 117.4(4) . 2_655 ?
Sb1 O11 W7 113.4(3) . 2_655 ?
W8 O11 W7 93.4(3) 2_655 2_655 ?
Sb2 O11 W1 131.6(5) . . ?
Sb1 O11 W1 138.6(4) . . ?
W8 O11 W1 94.4(3) 2_655 . ?
W7 O11 W1 93.0(3) 2_655 . ?
Sb2 O12 W5 119.1(5) . . ?
Sb1 O12 W5 114.0(4) . . ?
Sb2 O12 W4 117.0(5) . . ?
Sb1 O12 W4 113.4(4) . . ?
W5 O12 W4 94.7(3) . . ?
Sb2 O12 W3 131.6(5) . . ?
Sb1 O12 W3 139.1(4) . . ?
W5 O12 W3 93.0(3) . . ?
W4 O12 W3 93.1(3) . . ?
W3 O13 W4 119.9(5) . . ?
W3 O14 W5 120.0(5) . . ?
W4 O16 W7 151.8(5) . 2_655 ?
W5 O18 W4 118.2(4) . . ?
W5 O20 W6 153.8(5) . . ?
W6 O22 Ni1 137.8(5) . . ?
W6 O22 Ni2 119.8(4) . 2_655 ?
Ni1 O22 Ni2 99.6(4) . 2_655 ?
W5 O23 Ni1 137.9(5) . . ?
W5 O23 Ni2 118.2(4) . . ?
Ni1 O23 Ni2 102.0(4) . . ?
W4 O24 Ni3 136.1(4) . . ?
W4 O24 Ni2 118.8(4) . . ?
Ni3 O24 Ni2 101.6(4) . . ?
W8 O25 Ni3 140.8(5) . . ?
W8 O25 Na2 119.0(4) . . ?
Ni3 O25 Na2 98.4(3) . . ?
W8 O25 Ni4 119.0(4) . . ?
Ni3 O25 Ni4 98.4(3) . . ?
W9 O26 Ni3 138.0(5) . . ?
W9 O26 Ni2 119.8(4) . . ?
Ni3 O26 Ni2 99.8(4) . . ?
W7 O27 Ni3 141.6(5) . 2_655 ?
W7 O27 Ni4 117.5(4) . . ?
Ni3 O27 Ni4 99.2(4) 2_655 . ?
W7 O27 Na2 117.5(4) . . ?
Ni3 O27 Na2 99.2(4) 2_655 . ?
W7 O29 W8 118.2(4) . . ?
W7 O29 Na2 88.4(3) . . ?
W8 O29 Na2 89.6(3) . . ?
W9 O31 W8 151.7(5) . . ?
W9 O33 W6 118.3(5) . 2_655 ?
C1 N1 C3 108.0(11) . . ?
C1 N1 Ni3 123.6(9) . . ?
C3 N1 Ni3 128.2(9) . . ?
C1 N2 C2 107.4(12) . . ?
C4 N3 C5 105.7(18) . . ?
N1 C1 N2 110.5(13) . . ?
N2 C2 C3 107.6(15) . . ?
N1 C3 C2 106.4(14) . . ?
N3 C4 N3 109(2) . 2_655 ?
N3 C4 Ni1 125.3(10) . . ?
N3 C4 Ni1 125.3(10) 2_655 . ?
C5 C5 N3 109.6(12) 2_655 . ?
C9 N4 C7 118(3) . . ?
C9 N4 C6 116(3) . . ?
C7 N4 C6 107(3) . . ?
C9 N4 C8 107(3) . . ?
C7 N4 C8 106(3) . . ?
C6 N4 C8 102(3) . . ?
C12 N5 C14 117(3) . . ?
C12 N5 C11 111(3) . . ?
C14 N5 C11 107(2) . . ?
C12 N5 C13 111(3) . . ?
C14 N5 C13 100(3) . . ?
C11 N5 C13 109(3) . . ?

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
O36 W3 O4 W1 128.9(13) . . . . ?
O14 W3 O4 W1 -40(2) . . . . ?
O13 W3 O4 W1 -129.8(13) . . . . ?
O9 W3 O4 W1 29.8(13) . . . . ?
O12 W3 O4 W1 -56.4(13) . . . . ?
O10 W2 O5 W1 -130.7(13) . . . . ?
O9 W2 O5 W1 -30.6(12) . . . . ?
O7 W2 O5 W1 44(2) . . . . ?
O6 W2 O5 W1 131.0(12) . . . . ?
O8 W2 O5 W1 56.6(12) . . . . ?
Na1 W2 O5 W1 -146.7(10) . . . . ?
O11 Sb2 O8 W6 175.7(4) . . . . ?
O12 Sb2 O8 W6 74.1(6) . . . . ?
O11 Sb2 O8 W2 49.1(7) . . . . ?
O12 Sb2 O8 W2 -52.5(7) . . . . ?
O11 Sb2 O8 W9 -73.4(6) . . . 2_655 ?
O12 Sb2 O8 W9 -175.0(4) . . . 2_655 ?
O5 W2 O10 Na1 -154.4(10) . . . . ?
O9 W2 O10 Na1 116.0(11) . . . . ?
O7 W2 O10 Na1 27.4(11) . . . . ?
O6 W2 O10 Na1 -62.3(11) . . . . ?
O8 W2 O10 Na1 -13(4) . . . . ?
O12 Sb2 O11 W8 174.4(4) . . . 2_655 ?
O8 Sb2 O11 W8 74.6(6) . . . 2_655 ?
O12 Sb2 O11 W7 -74.7(6) . . . 2_655 ?
O8 Sb2 O11 W7 -174.6(4) . . . 2_655 ?
O12 Sb2 O11 W1 48.0(7) . . . . ?
O8 Sb2 O11 W1 -51.9(7) . . . . ?
O11 Sb2 O12 W5 -174.1(4) . . . . ?
O8 Sb2 O12 W5 -73.0(6) . . . . ?
O11 Sb2 O12 W4 73.1(6) . . . . ?
O8 Sb2 O12 W4 174.2(4) . . . . ?
O11 Sb2 O12 W3 -49.1(8) . . . . ?
O8 Sb2 O12 W3 52.0(7) . . . . ?
O17 W4 O16 W7 -125.8(12) . . . 2_655 ?
O24 W4 O16 W7 -21.7(12) . . . 2_655 ?
O13 W4 O16 W7 135.3(12) . . . 2_655 ?
O18 W4 O16 W7 60.1(19) . . . 2_655 ?
O12 W4 O16 W7 61.8(12) . . . 2_655 ?
O21 W6 O22 Ni1 72.1(8) . . . . ?
O20 W6 O22 Ni1 -29.3(7) . . . . ?
O33 W6 O22 Ni1 171.4(7) 2_655 . . . ?
O7 W6 O22 Ni1 -109.5(11) . . . . ?
O8 W6 O22 Ni1 -114.1(7) . . . . ?
O21 W6 O22 Ni2 -84.3(6) . . . 2_655 ?
O20 W6 O22 Ni2 174.3(5) . . . 2_655 ?
O33 W6 O22 Ni2 15.0(5) 2_655 . . 2_655 ?
O7 W6 O22 Ni2 94.1(11) . . . 2_655 ?
O8 W6 O22 Ni2 89.5(5) . . . 2_655 ?
O19 W5 O23 Ni1 -75.6(8) . . . . ?
O20 W5 O23 Ni1 26.7(7) . . . . ?
O18 W5 O23 Ni1 -173.8(7) . . . . ?
O14 W5 O23 Ni1 106.3(12) . . . . ?
O12 W5 O23 Ni1 112.5(7) . . . . ?
O19 W5 O23 Ni2 85.0(5) . . . . ?
O20 W5 O23 Ni2 -172.6(5) . . . . ?
O18 W5 O23 Ni2 -13.1(5) . . . . ?
O14 W5 O23 Ni2 -93.1(12) . . . . ?
O12 W5 O23 Ni2 -86.9(5) . . . . ?
O17 W4 O24 Ni3 71.7(7) . . . . ?
O16 W4 O24 Ni3 -30.3(7) . . . . ?
O13 W4 O24 Ni3 -119.6(10) . . . . ?
O18 W4 O24 Ni3 170.0(7) . . . . ?
O12 W4 O24 Ni3 -116.5(7) . . . . ?
O17 W4 O24 Ni2 -83.0(5) . . . . ?
O16 W4 O24 Ni2 175.0(5) . . . . ?
O13 W4 O24 Ni2 85.8(11) . . . . ?
O18 W4 O24 Ni2 15.4(5) . . . . ?
O12 W4 O24 Ni2 88.9(5) . . . . ?
O30 W8 O25 Ni3 75.2(8) . . . . ?
O31 W8 O25 Ni3 -26.0(7) . . . . ?
O29 W8 O25 Ni3 174.2(7) . . . . ?
O2 W8 O25 Ni3 -107.5(12) 2_655 . . . ?
O11 W8 O25 Ni3 -111.7(7) 2_655 . . . ?
Na2 W8 O25 Ni3 160.9(11) . . . . ?
O30 W8 O25 Na2 -85.7(5) . . . . ?
O31 W8 O25 Na2 173.1(5) . . . . ?
O29 W8 O25 Na2 13.2(5) . . . . ?
O2 W8 O25 Na2 91.5(12) 2_655 . . . ?
O11 W8 O25 Na2 87.4(4) 2_655 . . . ?
O30 W8 O25 Ni4 -85.7(5) . . . . ?
O31 W8 O25 Ni4 173.1(5) . . . . ?
O29 W8 O25 Ni4 13.2(5) . . . . ?
O2 W8 O25 Ni4 91.5(12) 2_655 . . . ?
O11 W8 O25 Ni4 87.4(4) 2_655 . . . ?
O32 W9 O26 Ni3 -74.8(8) . . . . ?
O31 W9 O26 Ni3 27.6(7) . . . . ?
O33 W9 O26 Ni3 -172.8(7) . . . . ?
O6 W9 O26 Ni3 112.4(12) 2_655 . . . ?
O8 W9 O26 Ni3 113.2(7) 2_655 . . . ?
O32 W9 O26 Ni2 83.3(6) . . . . ?
O31 W9 O26 Ni2 -174.3(5) . . . . ?
O33 W9 O26 Ni2 -14.7(5) . . . . ?
O6 W9 O26 Ni2 -89.5(12) 2_655 . . . ?
O8 W9 O26 Ni2 -88.7(5) 2_655 . . . ?
O28 W7 O27 Ni3 -74.4(8) . . . 2_655 ?
O29 W7 O27 Ni3 -175.3(8) . . . 2_655 ?
O16 W7 O27 Ni3 26.5(8) 2_655 . . 2_655 ?
O3 W7 O27 Ni3 98.7(13) 2_655 . . 2_655 ?
O11 W7 O27 Ni3 111.2(8) 2_655 . . 2_655 ?
Na2 W7 O27 Ni3 -161.3(11) . . . 2_655 ?
O28 W7 O27 Ni4 86.9(5) . . . . ?
O29 W7 O27 Ni4 -14.0(5) . . . . ?
O16 W7 O27 Ni4 -172.2(5) 2_655 . . . ?
O3 W7 O27 Ni4 -100.0(11) 2_655 . . . ?
O11 W7 O27 Ni4 -87.5(4) 2_655 . . . ?
O28 W7 O27 Na2 86.9(5) . . . . ?
O29 W7 O27 Na2 -14.0(5) . . . . ?
O16 W7 O27 Na2 -172.2(5) 2_655 . . . ?
O3 W7 O27 Na2 -100.0(11) 2_655 . . . ?
O11 W7 O27 Na2 -87.5(4) 2_655 . . . ?
C3 N1 C1 N2 -0.6(19) . . . . ?
Ni3 N1 C1 N2 175.5(11) . . . . ?
C2 N2 C1 N1 -1(2) . . . . ?
C1 N2 C2 C3 3(3) . . . . ?
C1 N1 C3 C2 2(2) . . . . ?
Ni3 N1 C3 C2 -173.7(14) . . . . ?
N2 C2 C3 N1 -3(3) . . . . ?
C5 N3 C4 N3 -0.6(13) . . . 2_655 ?
C5 N3 C4 Ni1 179.4(13) . . . . ?
C4 N3 C5 C5 2(4) . . . 2_655 ?

_refine_diff_density_max         2.496
_refine_diff_density_min         -2.436
_refine_diff_density_rms         0.285



####################################################################### 
# 
# 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_NaCo5_2
_audit_block_doi                 10.5517/ccdc.csd.cc20sd4c
_database_code_depnum_ccdc_archive 'CCDC 1870482'
loop_
_citation_id
_citation_doi
_citation_year
1 10.1039/C8CC07884J 2019
loop_
_audit_author_name
_audit_author_address
'Lubin Ni'
;School of Chemistry and Chemical Engineering, Yangzhou University
China
;
_audit_update_record             
;
2018-10-02 deposited with the CCDC.	2020-02-05 downloaded from the CCDC.
;

_publ_intended_journal           Chem.Commun

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C25 Co5.30 N10 Na0.70 O76 Sb2 W18'
_chemical_formula_weight         5537.57

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'
Co Co 0.3494 0.9721 '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'

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

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

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

_cell_length_a                   22.354(4)
_cell_length_b                   22.392(5)
_cell_length_c                   25.922(5)
_cell_angle_alpha                90
_cell_angle_beta                 114.195(5)
_cell_angle_gamma                90
_cell_volume                     11836(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    9899
_cell_measurement_theta_min      2.2709
_cell_measurement_theta_max      27.5398

_exptl_crystal_description       bluk
_exptl_crystal_colour            blue
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    3.108
_exptl_crystal_F_000             9651
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.06
_exptl_absorpt_coefficient_mu    18.667
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.729
_exptl_absorpt_correction_T_max  0.788
_exptl_absorpt_process_details   
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET)
(compiled Nov  6 2009,16:24:50)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   
;
 ?
;
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  graphite
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            53613
_diffrn_reflns_av_unetI/netI     0.0972
_diffrn_reflns_av_R_equivalents  0.0930
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_theta_min         1.809
_diffrn_reflns_theta_max         27.101
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measured_fraction_theta_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_point_group_measured_fraction_full 0.992
_reflns_number_total             12999
_reflns_number_gt                8151
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 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.
;

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and
 goodness of fit S are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The threshold expression of
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
 not relevant to the choice of reflections for refinement.  R-factors based
 on F² are statistically about twice as large as those based on F, and R-
 factors based on ALL data will be even larger.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0562P)²+2123.7388P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   .
_refine_ls_hydrogen_treatment    undef
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         12999
_refine_ls_number_parameters     403
_refine_ls_number_restraints     31
_refine_ls_R_factor_all          0.1377
_refine_ls_R_factor_gt           0.0833
_refine_ls_wR_factor_ref         0.2144
_refine_ls_wR_factor_gt          0.1886
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_restrained_S_all      1.027
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
W1 W 0.24239(6) 0.53508(6) 0.53681(5) 0.0532(3) Uani 1 1 d . . . . .
W2 W 0.20124(5) 0.53423(6) 0.66173(6) 0.0531(3) Uani 1 1 d . . . . .
W3 W 0.22137(6) 0.39079(6) 0.59850(5) 0.0539(3) Uani 1 1 d . . . . .
W4 W 0.33132(5) 0.62087(4) 0.73360(5) 0.0386(3) Uani 1 1 d . . . . .
W5 W 0.31191(5) 0.49169(5) 0.78925(5) 0.0407(3) Uani 1 1 d . . . . .
W6 W 0.33276(5) 0.34760(5) 0.72653(5) 0.0413(3) Uani 1 1 d . . . . .
W7 W 0.37149(6) 0.34643(5) 0.61487(4) 0.0422(3) Uani 1 1 d . . . . .
W8 W 0.39150(5) 0.49005(5) 0.55164(4) 0.0392(3) Uani 1 1 d . . . . .
W9 W 0.37330(5) 0.62065(4) 0.60752(4) 0.0385(3) Uani 1 1 d . . . . .
Sb1 Sb 0.38735(16) 0.48628(15) 0.68952(15) 0.0240(8) Uani 0.7 1 d . . P A 1
Sb1A Sb 0.3712(4) 0.4866(4) 0.6803(3) 0.0126(18) Uiso 0.3 1 d . . P A 2
Co1 Co 0.5000 0.3284(4) 0.7500 0.041(2) Uani 0.3 2 d S T P B 1
Co2 Co 0.5000 0.62167(19) 0.7500 0.0332(10) Uani 1 2 d S T P . .
Co3 Co 0.53254(15) 0.56366(13) 0.64810(13) 0.0315(7) Uani 1 1 d . . . . .
Co4 Co 0.47012(16) 0.41773(14) 0.83706(13) 0.0344(7) Uani 1 1 d . . . . .
Na1 Na 0.5000 0.3284(4) 0.7500 0.041(2) Uani 0.7 2 d S T P B 2
O1 O 0.1452(12) 0.3627(11) 0.5590(11) 0.083(7) Uiso 1 1 d . . . . .
O2 O 0.1160(11) 0.5512(10) 0.6389(10) 0.076(6) Uiso 1 1 d . . . . .
O3 O 0.1738(12) 0.5521(11) 0.4773(10) 0.079(7) Uiso 1 1 d . . . . .
O4 O 0.2286(9) 0.4553(8) 0.5535(8) 0.051(5) Uiso 1 1 d . . . . .
O5 O 0.1990(9) 0.4534(8) 0.6370(8) 0.054(5) Uiso 1 1 d . . . . .
O6 O 0.208(3) 0.550(2) 0.589(2) 0.046(15) Uiso 0.5 1 d . . P C 2
O6A O 0.216(3) 0.563(3) 0.597(2) 0.058(18) Uiso 0.5 1 d . . P C 1
O7 O 0.2186(10) 0.5079(9) 0.7361(8) 0.057(5) Uiso 1 1 d . . . . .
O8 O 0.2372(9) 0.6121(8) 0.6917(8) 0.054(5) Uiso 1 1 d . . . . .
O9 O 0.2834(9) 0.6106(8) 0.5494(8) 0.054(5) Uiso 1 1 d . . . . .
O10 O 0.2981(9) 0.5066(8) 0.5032(8) 0.054(5) Uiso 1 1 d . . . . .
O11 O 0.2752(9) 0.3444(9) 0.5737(8) 0.056(5) Uiso 1 1 d . . . . .
O12 O 0.2422(10) 0.3439(9) 0.6624(9) 0.060(5) Uiso 1 1 d . . . . .
O13 O 0.3446(7) 0.5219(7) 0.6099(6) 0.033(3) Uiso 1 1 d . . . . .
O14 O 0.3136(7) 0.5224(6) 0.7056(6) 0.029(3) Uiso 1 1 d . . . . .
O15 O 0.3299(8) 0.4149(7) 0.6588(7) 0.039(4) Uiso 1 1 d . . . . .
O16 O 0.3381(9) 0.6351(8) 0.6627(7) 0.047(4) Uiso 1 1 d . . . . .
O17 O 0.4014(8) 0.5766(7) 0.5560(7) 0.037(4) Uiso 1 1 d . . . . .
O18 O 0.3669(9) 0.4125(8) 0.5646(8) 0.051(5) Uiso 1 1 d . . . . .
O19 O 0.3600(8) 0.3032(7) 0.6745(7) 0.042(4) Uiso 1 1 d . . . . .
O20 O 0.3259(10) 0.2900(9) 0.7662(9) 0.065(6) Uiso 1 1 d . . . . .
O21 O 0.3226(8) 0.5777(8) 0.7951(7) 0.046(4) Uiso 1 1 d . . . . .
O22 O 0.3312(10) 0.6918(9) 0.7577(8) 0.061(5) Uiso 1 1 d . . . . .
O23 O 0.3911(9) 0.6909(8) 0.5914(8) 0.051(5) Uiso 1 1 d . . . . .
O24 O 0.4190(9) 0.4784(8) 0.5006(8) 0.054(5) Uiso 1 1 d . . . . .
O25 O 0.3892(10) 0.2896(9) 0.5798(8) 0.059(5) Uiso 1 1 d . . . . .
O26 O 0.3001(10) 0.4785(9) 0.8512(9) 0.062(5) Uiso 1 1 d . . . . .
O27 O 0.4518(9) 0.6005(8) 0.6673(8) 0.051(5) Uiso 1 1 d . . . . .
O28 O 0.4668(8) 0.4846(7) 0.6180(7) 0.040(4) Uiso 1 1 d . . . . .
O29 O 0.4506(8) 0.3730(7) 0.6633(7) 0.042(4) Uiso 1 1 d . . . . .
O30 O 0.4183(8) 0.3741(7) 0.7676(7) 0.043(4) Uiso 1 1 d . . . . .
O31 O 0.4017(8) 0.4843(8) 0.8129(7) 0.043(4) Uiso 1 1 d . . . . .
O32 O 0.4194(9) 0.5995(8) 0.7640(7) 0.048(4) Uiso 1 1 d . . . . .
O33 O 0.562(2) 0.6047(18) 0.5771(17) 0.155(14) Uiso 1 1 d . . . . .
O34 O 0.3029(9) 0.4111(9) 0.7569(8) 0.055(5) Uiso 1 1 d . . . . .
N1 N 0.4515(12) 0.3766(9) 0.8984(9) 0.049(6) Uani 1 1 d . . . . .
N2 N 0.4330(15) 0.3699(15) 0.9753(10) 0.072(8) Uani 1 1 d . . . . .
N3 N 0.511(2) 0.7482(13) 0.712(2) 0.16(2) Uani 1 1 d . . . . .
C1 C 0.4389(14) 0.4065(13) 0.9390(12) 0.054(7) Uani 1 1 d . . . . .
C2 C 0.447(2) 0.3157(19) 0.9649(17) 0.094(13) Uani 1 1 d . . . . .
C3 C 0.4576(18) 0.3166(12) 0.9107(14) 0.065(9) Uani 1 1 d . . . . .
C4 C 0.5000 0.7128(13) 0.7500 0.034(7) Uani 1 2 d S T P . .
O39A O 0.448(7) 0.798(6) 0.570(6) 0.11(5) Uiso 0.25 1 d . . P D 1
O39 O 0.421(4) 0.800(3) 0.553(3) 0.033(16) Uiso 0.25 1 d . . P E 2
O35 O 0.371(3) 0.906(3) 0.775(2) 0.101(17) Uiso 0.5 1 d . . P F 2
O36 O 0.363(2) 0.190(2) 0.836(2) 0.079(14) Uiso 0.5 1 d . . P G 2
O36A O 0.372(3) 0.178(3) 0.804(3) 0.13(2) Uiso 0.5 1 d . . P H 1
O37 O 0.454(5) 0.746(5) 0.926(5) 0.22(4) Uiso 0.5 1 d . . P . .
O38 O 0.3615(17) 0.7939(16) 0.8227(15) 0.134(12) Uiso 1 1 d . . . . .
O40 O -0.067(2) 0.691(2) 0.543(2) 0.083(14) Uiso 0.5 1 d . . P . .
N4 N 0.274(3) 0.345(3) 0.405(3) 0.31(4) Uiso 1 1 d D . . . .
C6 C 0.349(3) 0.338(4) 0.418(4) 0.61(15) Uiso 1 1 d D . . . .
C7 C 0.255(3) 0.305(2) 0.443(2) 0.17(2) Uiso 1 1 d D . . . .
C8 C 0.258(3) 0.4130(19) 0.406(2) 0.134(19) Uiso 1 1 d D . . . .
C9 C 0.233(3) 0.327(3) 0.338(2) 0.19(3) Uiso 1 1 d D . . . .
N5 N 0.228(3) 0.323(3) 0.878(3) 0.29(2) Uiso 1 1 d D U . . .
C10 C 0.285(4) 0.315(4) 0.858(4) 0.29(2) Uiso 1 1 d D U . . .
C11 C 0.169(3) 0.284(4) 0.844(3) 0.29(2) Uiso 1 1 d D U . . .
C12 C 0.211(4) 0.390(3) 0.877(4) 0.29(2) Uiso 1 1 d D U . . .
C13 C 0.258(4) 0.301(4) 0.944(3) 0.29(2) Uiso 1 1 d D U . . .
C5 C 0.492(2) 0.8056(15) 0.7715(19) 0.101(17) Uani 1 1 d . . . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
W1 O3 1.71(2) . ?
W1 O6 1.84(5) . ?
W1 O9 1.887(19) . ?
W1 O4 1.892(18) . ?
W1 O10 1.899(19) . ?
W1 O6A 1.99(6) . ?
W1 O13 2.312(15) . ?
W2 O2 1.79(2) . ?
W2 O7 1.90(2) . ?
W2 O5 1.913(19) . ?
W2 O8 1.944(19) . ?
W2 O6A 1.95(6) . ?
W2 O6 1.98(5) . ?
W2 O14 2.309(14) . ?
W3 O1 1.71(3) . ?
W3 O12 1.85(2) . ?
W3 O11 1.890(19) . ?
W3 O5 1.904(19) . ?
W3 O4 1.905(18) . ?
W3 O15 2.347(16) . ?
W4 O22 1.71(2) . ?
W4 O32 1.859(18) . ?
W4 O16 1.932(18) . ?
W4 O21 1.942(17) . ?
W4 O8 1.943(19) . ?
W4 O14 2.304(14) . ?
W5 O26 1.75(2) . ?
W5 O31 1.850(17) . ?
W5 O21 1.939(18) . ?
W5 O34 1.964(19) . ?
W5 O7 2.01(2) . ?
W5 O14 2.289(14) . ?
W6 O20 1.70(2) . ?
W6 O30 1.863(17) . ?
W6 O34 1.876(19) . ?
W6 O19 1.964(17) . ?
W6 O12 2.03(2) . ?
W6 O15 2.295(16) . ?
W6 Na1 3.5592(17) . ?
W7 O25 1.70(2) . ?
W7 O29 1.800(17) . ?
W7 O19 1.927(17) . ?
W7 O18 1.946(18) . ?
W7 O11 1.973(19) . ?
W7 O15 2.319(16) . ?
W7 Na1 3.5268(17) . ?
W8 O24 1.692(19) . ?
W8 O28 1.853(16) . ?
W8 O18 1.892(19) . ?
W8 O17 1.949(16) . ?
W8 O10 1.981(19) . ?
W8 O13 2.278(15) . ?
W9 O23 1.715(18) . ?
W9 O27 1.860(18) . ?
W9 O16 1.921(18) . ?
W9 O17 1.960(15) . ?
W9 O9 1.970(19) . ?
W9 O13 2.309(15) . ?
Sb1 O15 2.000(17) . ?
Sb1 O14 2.028(14) . ?
Sb1 O13 2.048(15) . ?
Sb1A O15 1.823(18) . ?
Sb1A O13 1.850(17) . ?
Sb1A O14 1.850(16) . ?
Co1 O29 2.289(17) 2_656 ?
Co1 O29 2.289(17) . ?
Co1 O30 2.297(17) 2_656 ?
Co1 O30 2.297(17) . ?
Co2 O27 2.021(18) . ?
Co2 O27 2.021(18) 2_656 ?
Co2 O32 2.039(18) 2_656 ?
Co2 O32 2.039(18) . ?
Co2 C4 2.04(3) . ?
Co3 O27 2.218(18) . ?
Co3 O28 2.228(17) . ?
Co3 O32 2.232(18) 2_656 ?
Co3 O31 2.263(17) 2_656 ?
Co3 O33 2.38(4) . ?
Co4 O30 1.957(17) . ?
Co4 N1 2.02(2) . ?
Co4 O29 2.037(17) 2_656 ?
Co4 O31 2.042(17) . ?
Co4 O28 2.059(17) 2_656 ?
Co4 Na1 3.283(6) . ?
Na1 O29 2.289(17) 2_656 ?
Na1 O29 2.289(17) . ?
Na1 O30 2.297(17) 2_656 ?
Na1 O30 2.297(17) . ?
Na1 O19 2.987(17) . ?
Na1 O19 2.987(17) 2_656 ?
Na1 Co4 3.283(6) 2_656 ?
Na1 W7 3.5268(16) 2_656 ?
Na1 W6 3.5591(17) 2_656 ?
O28 Co4 2.059(17) 2_656 ?
O29 Co4 2.037(17) 2_656 ?
O31 Co3 2.263(17) 2_656 ?
O32 Co3 2.232(18) 2_656 ?
N1 C1 1.37(3) . ?
N1 C3 1.37(3) . ?
N2 C1 1.30(4) . ?
N2 C2 1.31(5) . ?
N3 C5 1.37(5) 2_656 ?
N3 C4 1.38(5) . ?
C2 C3 1.52(5) . ?
C4 N3 1.37(5) 2_656 ?
N4 C7 1.52(4) . ?
N4 C8 1.56(4) . ?
N4 C6 1.58(4) . ?
N4 C9 1.66(6) . ?
N5 C11 1.53(4) . ?
N5 C10 1.55(4) . ?
N5 C12 1.56(4) . ?
N5 C13 1.65(6) . ?
C5 C5 1.31(9) 2_656 ?
C5 N3 1.37(5) 2_656 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O3 W1 O6 97.9(18) . . ?
O3 W1 O9 98.5(10) . . ?
O6 W1 O9 92.0(17) . . ?
O3 W1 O4 104.2(10) . . ?
O6 W1 O4 80.9(17) . . ?
O9 W1 O4 156.9(8) . . ?
O3 W1 O10 100.0(10) . . ?
O6 W1 O10 161.2(17) . . ?
O9 W1 O10 91.0(8) . . ?
O4 W1 O10 89.2(8) . . ?
O3 W1 O6A 101.3(19) . . ?
O9 W1 O6A 81.8(17) . . ?
O4 W1 O6A 89.6(18) . . ?
O10 W1 O6A 158.2(18) . . ?
O3 W1 O13 170.0(9) . . ?
O6 W1 O13 89.2(17) . . ?
O9 W1 O13 74.1(7) . . ?
O4 W1 O13 83.8(7) . . ?
O10 W1 O13 73.7(7) . . ?
O6A W1 O13 84.5(17) . . ?
O2 W2 O7 98.6(10) . . ?
O2 W2 O5 102.2(9) . . ?
O7 W2 O5 90.7(8) . . ?
O2 W2 O8 98.7(9) . . ?
O7 W2 O8 89.6(8) . . ?
O5 W2 O8 158.8(8) . . ?
O2 W2 O6A 100.4(19) . . ?
O7 W2 O6A 160.1(18) . . ?
O5 W2 O6A 91.1(18) . . ?
O8 W2 O6A 81.6(18) . . ?
O2 W2 O6 97.8(17) . . ?
O7 W2 O6 162.9(16) . . ?
O5 W2 O6 81.2(16) . . ?
O8 W2 O6 92.5(16) . . ?
O2 W2 O14 169.5(8) . . ?
O7 W2 O14 74.6(7) . . ?
O5 W2 O14 86.0(7) . . ?
O8 W2 O14 73.6(7) . . ?
O6A W2 O14 85.7(18) . . ?
O6 W2 O14 89.7(16) . . ?
O1 W3 O12 98.7(11) . . ?
O1 W3 O11 102.2(10) . . ?
O12 W3 O11 91.8(9) . . ?
O1 W3 O5 100.0(10) . . ?
O12 W3 O5 88.4(8) . . ?
O11 W3 O5 157.5(8) . . ?
O1 W3 O4 103.1(10) . . ?
O12 W3 O4 157.6(8) . . ?
O11 W3 O4 89.0(8) . . ?
O5 W3 O4 82.5(8) . . ?
O1 W3 O15 171.3(9) . . ?
O12 W3 O15 73.9(7) . . ?
O11 W3 O15 74.0(7) . . ?
O5 W3 O15 84.5(7) . . ?
O4 W3 O15 84.8(7) . . ?
O22 W4 O32 104.2(9) . . ?
O22 W4 O16 102.0(9) . . ?
O32 W4 O16 87.9(8) . . ?
O22 W4 O21 98.5(9) . . ?
O32 W4 O21 88.2(7) . . ?
O16 W4 O21 159.5(7) . . ?
O22 W4 O8 97.7(9) . . ?
O32 W4 O8 158.1(8) . . ?
O16 W4 O8 88.5(8) . . ?
O21 W4 O8 87.6(8) . . ?
O22 W4 O14 168.4(8) . . ?
O32 W4 O14 84.4(7) . . ?
O16 W4 O14 85.9(6) . . ?
O21 W4 O14 73.7(6) . . ?
O8 W4 O14 73.8(7) . . ?
O26 W5 O31 103.4(9) . . ?
O26 W5 O21 98.9(9) . . ?
O31 W5 O21 88.9(7) . . ?
O26 W5 O34 102.0(9) . . ?
O31 W5 O34 88.1(8) . . ?
O21 W5 O34 158.9(8) . . ?
O26 W5 O7 99.0(9) . . ?
O31 W5 O7 157.6(8) . . ?
O21 W5 O7 86.3(8) . . ?
O34 W5 O7 88.7(8) . . ?
O26 W5 O14 169.6(8) . . ?
O31 W5 O14 84.4(6) . . ?
O21 W5 O14 74.1(6) . . ?
O34 W5 O14 84.8(7) . . ?
O7 W5 O14 73.2(7) . . ?
O20 W6 O30 102.9(9) . . ?
O20 W6 O34 100.8(9) . . ?
O30 W6 O34 88.7(8) . . ?
O20 W6 O19 99.3(9) . . ?
O30 W6 O19 91.1(7) . . ?
O34 W6 O19 159.4(8) . . ?
O20 W6 O12 99.0(9) . . ?
O30 W6 O12 158.1(8) . . ?
O34 W6 O12 88.2(8) . . ?
O19 W6 O12 84.4(7) . . ?
O20 W6 O15 169.3(8) . . ?
O30 W6 O15 85.9(7) . . ?
O34 W6 O15 85.4(7) . . ?
O19 W6 O15 74.1(6) . . ?
O12 W6 O15 72.2(7) . . ?
O20 W6 Na1 98.9(7) . . ?
O30 W6 Na1 35.0(5) . . ?
O34 W6 Na1 123.3(6) . . ?
O19 W6 Na1 57.0(5) . . ?
O12 W6 Na1 139.6(6) . . ?
O15 W6 Na1 84.7(4) . . ?
O25 W7 O29 104.0(8) . . ?
O25 W7 O19 100.9(8) . . ?
O29 W7 O19 91.3(7) . . ?
O25 W7 O18 99.9(9) . . ?
O29 W7 O18 89.0(8) . . ?
O19 W7 O18 158.5(7) . . ?
O25 W7 O11 97.8(9) . . ?
O29 W7 O11 158.1(8) . . ?
O19 W7 O11 87.0(7) . . ?
O18 W7 O11 84.7(8) . . ?
O25 W7 O15 169.8(8) . . ?
O29 W7 O15 85.2(7) . . ?
O19 W7 O15 74.1(6) . . ?
O18 W7 O15 84.5(7) . . ?
O11 W7 O15 73.3(7) . . ?
O25 W7 Na1 99.9(7) . . ?
O29 W7 Na1 34.7(5) . . ?
O19 W7 Na1 57.9(5) . . ?
O18 W7 Na1 123.4(6) . . ?
O11 W7 Na1 143.0(6) . . ?
O15 W7 Na1 85.2(4) . . ?
O24 W8 O28 103.4(8) . . ?
O24 W8 O18 102.9(8) . . ?
O28 W8 O18 89.7(7) . . ?
O24 W8 O17 97.5(8) . . ?
O28 W8 O17 88.5(7) . . ?
O18 W8 O17 159.5(7) . . ?
O24 W8 O10 99.2(8) . . ?
O28 W8 O10 157.1(7) . . ?
O18 W8 O10 88.6(8) . . ?
O17 W8 O10 85.2(7) . . ?
O24 W8 O13 168.6(7) . . ?
O28 W8 O13 84.0(6) . . ?
O18 W8 O13 85.6(7) . . ?
O17 W8 O13 73.9(6) . . ?
O10 W8 O13 73.1(7) . . ?
O23 W9 O27 101.0(8) . . ?
O23 W9 O16 103.5(8) . . ?
O27 W9 O16 87.4(8) . . ?
O23 W9 O17 97.1(8) . . ?
O27 W9 O17 89.4(7) . . ?
O16 W9 O17 159.3(7) . . ?
O23 W9 O9 100.6(8) . . ?
O27 W9 O9 158.3(8) . . ?
O16 W9 O9 89.3(8) . . ?
O17 W9 O9 86.1(7) . . ?
O23 W9 O13 168.1(7) . . ?
O27 W9 O13 85.6(7) . . ?
O16 W9 O13 86.4(7) . . ?
O17 W9 O13 73.0(6) . . ?
O9 W9 O13 72.8(7) . . ?
O15 Sb1 O14 87.6(6) . . ?
O15 Sb1 O13 87.2(6) . . ?
O14 Sb1 O13 88.2(6) . . ?
O15 Sb1A O13 99.0(8) . . ?
O15 Sb1A O14 98.7(8) . . ?
O13 Sb1A O14 100.1(8) . . ?
O29 Co1 O29 128.2(9) 2_656 . ?
O29 Co1 O30 84.1(6) 2_656 2_656 ?
O29 Co1 O30 73.3(6) . 2_656 ?
O29 Co1 O30 73.3(6) 2_656 . ?
O29 Co1 O30 84.1(6) . . ?
O30 Co1 O30 127.1(9) 2_656 . ?
O27 Co2 O27 152.8(11) . 2_656 ?
O27 Co2 O32 83.1(7) . 2_656 ?
O27 Co2 O32 90.3(7) 2_656 2_656 ?
O27 Co2 O32 90.3(7) . . ?
O27 Co2 O32 83.1(7) 2_656 . ?
O32 Co2 O32 151.8(10) 2_656 . ?
O27 Co2 C4 103.6(5) . . ?
O27 Co2 C4 103.6(5) 2_656 . ?
O32 Co2 C4 104.1(5) 2_656 . ?
O32 Co2 C4 104.1(5) . . ?
O27 Co3 O28 83.9(6) . . ?
O27 Co3 O32 74.5(7) . 2_656 ?
O28 Co3 O32 128.0(6) . 2_656 ?
O27 Co3 O31 129.1(7) . 2_656 ?
O28 Co3 O31 75.4(6) . 2_656 ?
O32 Co3 O31 82.7(6) 2_656 2_656 ?
O27 Co3 O33 122.8(11) . . ?
O28 Co3 O33 112.9(11) . . ?
O32 Co3 O33 118.7(11) 2_656 . ?
O31 Co3 O33 108.2(11) 2_656 . ?
O30 Co4 N1 105.1(9) . . ?
O30 Co4 O29 86.5(7) . 2_656 ?
N1 Co4 O29 103.8(7) . 2_656 ?
O30 Co4 O31 89.8(7) . . ?
N1 Co4 O31 101.8(7) . . ?
O29 Co4 O31 154.2(7) 2_656 . ?
O30 Co4 O28 153.3(7) . 2_656 ?
N1 Co4 O28 101.5(8) . 2_656 ?
O29 Co4 O28 88.0(7) 2_656 2_656 ?
O31 Co4 O28 84.0(7) . 2_656 ?
O30 Co4 Na1 43.4(5) . . ?
N1 Co4 Na1 115.4(6) . . ?
O29 Co4 Na1 43.6(5) 2_656 . ?
O31 Co4 Na1 124.9(5) . . ?
O28 Co4 Na1 123.2(5) 2_656 . ?
O29 Na1 O29 128.2(9) 2_656 . ?
O29 Na1 O30 84.1(6) 2_656 2_656 ?
O29 Na1 O30 73.3(6) . 2_656 ?
O29 Na1 O30 73.3(6) 2_656 . ?
O29 Na1 O30 84.1(6) . . ?
O30 Na1 O30 127.1(9) 2_656 . ?
O29 Na1 O19 132.9(5) 2_656 . ?
O29 Na1 O19 59.0(5) . . ?
O30 Na1 O19 131.2(5) 2_656 . ?
O30 Na1 O19 60.6(5) . . ?
O29 Na1 O19 59.0(5) 2_656 2_656 ?
O29 Na1 O19 132.9(5) . 2_656 ?
O30 Na1 O19 60.6(5) 2_656 2_656 ?
O30 Na1 O19 131.2(5) . 2_656 ?
O19 Na1 O19 158.3(7) . 2_656 ?
O29 Na1 Co4 37.9(4) 2_656 . ?
O29 Na1 Co4 104.9(5) . . ?
O30 Na1 Co4 105.5(5) 2_656 . ?
O30 Na1 Co4 35.9(4) . . ?
O19 Na1 Co4 96.4(3) . . ?
O19 Na1 Co4 96.8(3) 2_656 . ?
O29 Na1 Co4 104.9(5) 2_656 2_656 ?
O29 Na1 Co4 37.9(4) . 2_656 ?
O30 Na1 Co4 35.9(4) 2_656 2_656 ?
O30 Na1 Co4 105.5(5) . 2_656 ?
O19 Na1 Co4 96.8(3) . 2_656 ?
O19 Na1 Co4 96.4(3) 2_656 2_656 ?
Co4 Na1 Co4 104.9(3) . 2_656 ?
O29 Na1 W7 142.6(5) 2_656 . ?
O29 Na1 W7 26.6(4) . . ?
O30 Na1 W7 98.2(4) 2_656 . ?
O30 Na1 W7 75.9(4) . . ?
O19 Na1 W7 33.1(3) . . ?
O19 Na1 W7 151.7(3) 2_656 . ?
Co4 Na1 W7 107.48(16) . . ?
Co4 Na1 W7 63.88(9) 2_656 . ?
O29 Na1 W7 26.6(4) 2_656 2_656 ?
O29 Na1 W7 142.6(5) . 2_656 ?
O30 Na1 W7 75.9(4) 2_656 2_656 ?
O30 Na1 W7 98.2(4) . 2_656 ?
O19 Na1 W7 151.7(3) . 2_656 ?
O19 Na1 W7 33.1(3) 2_656 2_656 ?
Co4 Na1 W7 63.88(9) . 2_656 ?
Co4 Na1 W7 107.48(16) 2_656 2_656 ?
W7 Na1 W7 166.8(3) . 2_656 ?
O29 Na1 W6 74.3(4) 2_656 2_656 ?
O29 Na1 W6 99.5(4) . 2_656 ?
O30 Na1 W6 27.7(4) 2_656 2_656 ?
O30 Na1 W6 141.0(5) . 2_656 ?
O19 Na1 W6 151.6(3) . 2_656 ?
O19 Na1 W6 33.5(3) 2_656 2_656 ?
Co4 Na1 W6 107.70(16) . 2_656 ?
Co4 Na1 W6 63.15(9) 2_656 2_656 ?
W7 Na1 W6 121.79(7) . 2_656 ?
W7 Na1 W6 56.31(3) 2_656 2_656 ?
O29 Na1 W6 99.5(4) 2_656 . ?
O29 Na1 W6 74.3(4) . . ?
O30 Na1 W6 141.0(5) 2_656 . ?
O30 Na1 W6 27.7(4) . . ?
O19 Na1 W6 33.5(3) . . ?
O19 Na1 W6 151.6(3) 2_656 . ?
Co4 Na1 W6 63.15(9) . . ?
Co4 Na1 W6 107.70(16) 2_656 . ?
W7 Na1 W6 56.32(3) . . ?
W7 Na1 W6 121.79(7) 2_656 . ?
W6 Na1 W6 166.1(3) 2_656 . ?
W1 O4 W3 156.6(11) . . ?
W3 O5 W2 153.6(11) . . ?
W1 O6 W2 153(3) . . ?
W2 O6A W1 141(3) . . ?
W2 O7 W5 118.5(10) . . ?
W4 O8 W2 119.3(10) . . ?
W1 O9 W9 120.4(10) . . ?
W1 O10 W8 119.4(10) . . ?
W3 O11 W7 120.6(10) . . ?
W3 O12 W6 120.7(10) . . ?
Sb1A O13 W8 118.1(8) . . ?
Sb1 O13 W8 113.2(7) . . ?
Sb1A O13 W9 117.1(8) . . ?
Sb1 O13 W9 112.3(7) . . ?
W8 O13 W9 94.2(5) . . ?
Sb1A O13 W1 132.3(8) . . ?
Sb1 O13 W1 140.5(7) . . ?
W8 O13 W1 93.7(5) . . ?
W9 O13 W1 92.8(5) . . ?
Sb1A O14 W5 119.3(7) . . ?
Sb1 O14 W5 113.9(6) . . ?
Sb1A O14 W4 118.1(7) . . ?
Sb1 O14 W4 113.4(6) . . ?
W5 O14 W4 93.3(5) . . ?
Sb1A O14 W2 130.5(8) . . ?
Sb1 O14 W2 139.1(7) . . ?
W5 O14 W2 93.7(5) . . ?
W4 O14 W2 93.3(5) . . ?
Sb1A O15 W6 119.5(8) . . ?
Sb1 O15 W6 114.1(7) . . ?
Sb1A O15 W7 118.6(8) . . ?
Sb1 O15 W7 113.7(7) . . ?
W6 O15 W7 92.9(6) . . ?
Sb1A O15 W3 131.5(9) . . ?
Sb1 O15 W3 140.2(8) . . ?
W6 O15 W3 93.2(6) . . ?
W7 O15 W3 92.0(6) . . ?
W9 O16 W4 153.7(10) . . ?
W8 O17 W9 118.6(8) . . ?
W8 O18 W7 151.3(11) . . ?
W7 O19 W6 118.5(8) . . ?
W7 O19 Na1 89.0(6) . . ?
W6 O19 Na1 89.5(6) . . ?
W5 O21 W4 118.7(9) . . ?
W9 O27 Co2 137.5(10) . . ?
W9 O27 Co3 118.7(9) . . ?
Co2 O27 Co3 101.3(8) . . ?
W8 O28 Co4 136.4(9) . 2_656 ?
W8 O28 Co3 119.4(8) . . ?
Co4 O28 Co3 100.3(7) 2_656 . ?
W7 O29 Co4 140.2(9) . 2_656 ?
W7 O29 Co1 118.7(8) . . ?
Co4 O29 Co1 98.5(7) 2_656 . ?
W7 O29 Na1 118.7(8) . . ?
Co4 O29 Na1 98.5(7) 2_656 . ?
W6 O30 Co4 140.0(9) . . ?
W6 O30 Na1 117.3(8) . . ?
Co4 O30 Na1 100.7(7) . . ?
W6 O30 Co1 117.3(8) . . ?
Co4 O30 Co1 100.7(7) . . ?
W5 O31 Co4 137.8(9) . . ?
W5 O31 Co3 119.7(8) . 2_656 ?
Co4 O31 Co3 99.7(7) . 2_656 ?
W4 O32 Co2 136.2(10) . . ?
W4 O32 Co3 120.5(9) . 2_656 ?
Co2 O32 Co3 100.3(7) . 2_656 ?
W6 O34 W5 152.1(11) . . ?
C1 N1 C3 109(2) . . ?
C1 N1 Co4 123.7(17) . . ?
C3 N1 Co4 126.4(17) . . ?
C1 N2 C2 109(3) . . ?
C5 N3 C4 105(4) 2_656 . ?
N2 C1 N1 111(3) . . ?
N2 C2 C3 109(3) . . ?
N1 C3 C2 101(3) . . ?
N3 C4 N3 110(4) 2_656 . ?
N3 C4 Co2 125(2) 2_656 . ?
N3 C4 Co2 125(2) . . ?
C7 N4 C8 116(4) . . ?
C7 N4 C6 111(4) . . ?
C8 N4 C6 110(4) . . ?
C7 N4 C9 110(4) . . ?
C8 N4 C9 104(4) . . ?
C6 N4 C9 106(4) . . ?
C11 N5 C10 113(4) . . ?
C11 N5 C12 113(4) . . ?
C10 N5 C12 110(4) . . ?
C11 N5 C13 108(4) . . ?
C10 N5 C13 106(4) . . ?
C12 N5 C13 107(4) . . ?
C5 C5 N3 110(3) 2_656 2_656 ?

_refine_diff_density_max         3.336
_refine_diff_density_min         -2.805
_refine_diff_density_rms         0.437



