#------------------------------------------------------------------------------
#$Date: 2023-11-30 18:32:54 +0200 (Thu, 30 Nov 2023) $
#$Revision: 287896 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/12/27/7122761.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7122761
loop_
_publ_author_name
'Zhao, Hongxia'
'Tao, Li'
'Zhang, Fengmin'
'Zhang, Ying'
'Liu, Yanqing'
'Xu, Hongjie'
'Diao, Guowang'
'Ni, Lubin'
_publ_section_title
;
 Transition Metal Substituted Sandwich-Type Polyoxometalates with Strong
 Metal--C (imidazole) Bond as Anticancer Agents
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/C8CC07884J
_journal_year                    2018
_chemical_formula_sum            'C25 N10 Na1.7 Ni5.3 O82 Sb2 W18'
_chemical_formula_weight         5655.40
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2018-10-02 deposited with the CCDC.
2018-12-20 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 114.014(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   22.4271(14)
_cell_length_b                   22.3391(14)
_cell_length_c                   25.7151(15)
_cell_measurement_reflns_used    9899
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.5398
_cell_measurement_theta_min      2.2709
_cell_volume                     11768.2(13)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0380
_diffrn_reflns_av_unetI/netI     0.0365
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            55150
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.103
_diffrn_reflns_theta_min         1.809
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    18.885
_exptl_absorpt_correction_T_max  0.788
_exptl_absorpt_correction_T_min  0.729
_exptl_absorpt_correction_type   multi-scan
_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_crystal_colour            orange
_exptl_crystal_density_diffrn    3.192
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       bluk
_exptl_crystal_F_000             9908
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.09
_refine_diff_density_max         2.496
_refine_diff_density_min         -2.436
_refine_diff_density_rms         0.285
_refine_ls_extinction_coef       0.000107(7)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     589
_refine_ls_number_reflns         12881
_refine_ls_number_restraints     20
_refine_ls_restrained_S_all      1.066
_refine_ls_R_factor_all          0.0705
_refine_ls_R_factor_gt           0.0517
_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)+(0.0327P)²+636.8115P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1123
_refine_ls_wR_factor_ref         0.1241
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10150
_reflns_number_total             12881
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c8cc07884j2.cif
_cod_data_source_block           Na1Ni5_1
_cod_original_formula_sum        'C25 N10 Na1.70 Ni5.30 O82 Sb2 W18'
_cod_database_code               7122761
_shelx_shelxl_version_number     2014/7
_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.
;
_exptl_absorpt_special_details
;
 ?
;
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'
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 . . . .
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'
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
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_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
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_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_4
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
