# Electronic Supplementary Material (ESI) for CrystEngComm.
# This journal is © The Royal Society of Chemistry 2021

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

data_shelx
_database_code_depnum_ccdc_archive 'CCDC 1908246'
loop_
_audit_author_name
_audit_author_address
'Maciej Hodorowicz'
;Faculty of Chemistry Jagiellonian University
Poland
;
_audit_update_record             
;
2019-04-05 deposited with the CCDC.	2021-04-21 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2017/1
_shelx_SHELXL_version_number     2017/1
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C32 H28 N16 Na4 O12 W2'
_chemical_formula_weight         1288.36

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'
W W -0.8490 6.8722 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

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

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   12.1359(3)
_cell_length_b                   13.8894(3)
_cell_length_c                   13.9395(3)
_cell_angle_alpha                92.898(2)
_cell_angle_beta                 97.773(2)
_cell_angle_gamma                100.490(2)
_cell_volume                     2282.32(9)
_cell_formula_units_Z            2
_cell_measurement_temperature    130(2)
_cell_measurement_reflns_used    7071
_cell_measurement_theta_min      2.6958
_cell_measurement_theta_max      28.5294

_exptl_crystal_description       red
_exptl_crystal_colour            plate
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.875
_exptl_crystal_F_000             1240
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.100
_exptl_absorpt_coefficient_mu    5.149
_shelx_estimated_absorpt_T_min   0.307
_shelx_estimated_absorpt_T_max   0.627
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.60573
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET)
(compiled Jul 11 2012,15:38:31)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      129.9(6)
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_wavelength     0.7107
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_source         'SuperNova (Mo) X-ray Source'
_diffrn_radiation_monochromator  mirror
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_detector_area_resol_mean 10.3756
_diffrn_reflns_number            19808
_diffrn_reflns_av_unetI/netI     0.0569
_diffrn_reflns_av_R_equivalents  0.0358
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         2.701
_diffrn_reflns_theta_max         28.591
_diffrn_reflns_theta_full        25.241
_diffrn_measured_fraction_theta_max 0.884
_diffrn_measured_fraction_theta_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.884
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.884
_diffrn_reflns_point_group_measured_fraction_full 0.997
_reflns_number_total             10320
_reflns_number_gt                7659
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET)
(compiled Jul 11 2012,15:38:31)
;
_computing_cell_refinement       
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET)
(compiled Jul 11 2012,15:38:31)
;
_computing_data_reduction        
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET)
(compiled Jul 11 2012,15:38:31)
;
_computing_structure_solution    'SIR-2014 (Burla, 2015)'
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2017)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0179P)²+2.6915P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         10320
_refine_ls_number_parameters     603
_refine_ls_number_restraints     3
_refine_ls_R_factor_all          0.0575
_refine_ls_R_factor_gt           0.0349
_refine_ls_wR_factor_ref         0.0711
_refine_ls_wR_factor_gt          0.0629
_refine_ls_goodness_of_fit_ref   1.070
_refine_ls_restrained_S_all      1.070
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
W1 W 0.56215(2) -0.26449(2) 0.85495(2) 0.01078(6) Uani 1 1 d . . . . .
W2 W 0.94843(2) 0.26852(2) 0.64296(2) 0.01095(6) Uani 1 1 d . . . . .
Na1 Na 0.53646(16) 0.11459(16) 0.79796(14) 0.0183(5) Uani 1 1 d . . . . .
Na3 Na 0.18481(17) 0.07091(17) 0.83191(16) 0.0269(5) Uani 1 1 d . . . . .
Na2 Na 0.36706(17) 0.09370(19) 0.54480(16) 0.0308(6) Uani 1 1 d . . . . .
Na4 Na 0.97270(16) -0.12556(16) 0.71977(14) 0.0176(5) Uani 1 1 d . . . . .
O7 O 0.3584(3) 0.0223(3) 0.8785(3) 0.0306(10) Uani 1 1 d . . . . .
H7A H 0.386160 0.021718 0.945761 0.046 Uiso 1 1 d R U . . .
H7B H 0.352750 -0.045192 0.854601 0.046 Uiso 1 1 d R U . . .
O1 O 0.4557(3) -0.0048(3) 0.6537(3) 0.0245(9) Uani 1 1 d . . . . .
H1A H 0.527511 -0.023445 0.652973 0.037 Uiso 1 1 d R U . . .
H1B H 0.407161 -0.049255 0.668005 0.037 Uiso 1 1 d R U . . .
O2 O 0.4237(3) 0.2135(3) 0.7028(3) 0.0310(10) Uani 1 1 d . . . . .
O3 O 0.1708(3) 0.0494(3) 0.5441(3) 0.0254(9) Uani 1 1 d D . . . .
O4 O 0.3129(3) 0.2538(3) 0.4992(3) 0.0343(11) Uani 1 1 d . . . . .
O5 O 0.3295(3) 0.0300(3) 0.3748(3) 0.0241(9) Uani 1 1 d . . . . .
O6 O 0.5295(3) 0.1917(3) 0.5072(3) 0.0353(11) Uani 1 1 d . . . . .
O8 O 0.1647(3) -0.0560(3) 0.7062(3) 0.0212(8) Uani 1 1 d . . . . .
H8A H 0.217214 -0.098332 0.711737 0.032 Uiso 1 1 d R U . . .
H8B H 0.166982 -0.023292 0.648589 0.032 Uiso 1 1 d R U . . .
O9 O 0.0208(3) -0.0248(3) 0.8743(3) 0.0325(10) Uani 1 1 d . . . . .
O10 O 1.0575(3) -0.2510(3) 0.8008(3) 0.0319(10) Uani 1 1 d . . . . .
H10A H 1.040671 -0.248137 0.865053 0.048 Uiso 1 1 d R U . . .
H10B H 1.134121 -0.220887 0.801243 0.048 Uiso 1 1 d R U . . .
N13 N 0.7823(4) -0.1937(3) 1.0267(3) 0.0193(10) Uani 1 1 d . . . . .
N15 N 0.6122(4) -0.0223(3) 0.8795(3) 0.0201(10) Uani 1 1 d . . . . .
N38 N 0.7279(4) 0.1777(3) 0.7494(3) 0.0211(10) Uani 1 1 d . . . . .
N32 N 0.8493(3) 0.3864(3) 0.6241(3) 0.0148(9) Uani 1 1 d . . . . .
N21 N 1.0675(3) 0.4072(3) 0.6253(3) 0.0126(9) Uani 1 1 d . . . . .
N34 N 1.0594(3) 0.2163(3) 0.4464(3) 0.0190(10) Uani 1 1 d . . . . .
N35 N 1.1925(4) 0.2140(4) 0.7354(3) 0.0214(10) Uani 1 1 d . . . . .
N36 N 0.9360(3) 0.0303(3) 0.6523(3) 0.0216(11) Uani 1 1 d . . . . .
N37 N 0.7442(4) 0.1633(4) 0.4669(3) 0.0250(11) Uani 1 1 d . . . . .
N33 N 0.9958(3) 0.3814(4) 0.8638(3) 0.0207(10) Uani 1 1 d . . . . .
N1 N 0.6468(3) -0.3929(3) 0.8628(3) 0.0123(9) Uani 1 1 d . . . . .
N12 N 0.4320(3) -0.3965(3) 0.8688(3) 0.0134(9) Uani 1 1 d . . . . .
N14 N 0.7747(3) -0.1827(4) 0.7368(3) 0.0222(11) Uani 1 1 d . . . . .
N16 N 0.3308(4) -0.1829(4) 0.7724(3) 0.0231(11) Uani 1 1 d . . . . .
N17 N 0.5017(3) -0.3503(4) 0.6236(3) 0.0213(11) Uani 1 1 d . . . . .
N18 N 0.5383(4) 0.2145(3) 0.9439(3) 0.0209(10) Uani 1 1 d . . . . .
C13 C 0.7042(4) -0.2207(4) 0.9700(4) 0.0151(11) Uani 1 1 d . . . . .
C15 C 0.5942(4) -0.1071(4) 0.8691(4) 0.0133(11) Uani 1 1 d . . . . .
C38 C 0.8070(4) 0.2093(4) 0.7154(4) 0.0179(12) Uani 1 1 d . . . . .
C27 C 0.9067(4) 0.4810(4) 0.6317(3) 0.0144(11) Uani 1 1 d . . . . .
C26 C 1.0273(4) 0.4917(4) 0.6301(3) 0.0150(11) Uani 1 1 d . . . . .
C22 C 1.1785(4) 0.4130(4) 0.6170(3) 0.0143(11) Uani 1 1 d . . . . .
H22 H 1.207231 0.354045 0.612081 0.017 Uiso 1 1 calc R U . . .
C23 C 1.2509(4) 0.5010(4) 0.6154(4) 0.0187(12) Uani 1 1 d . . . . .
H23 H 1.327939 0.502111 0.608464 0.022 Uiso 1 1 calc R U . . .
C24 C 1.2117(4) 0.5881(4) 0.6240(4) 0.0213(12) Uani 1 1 d . . . . .
H24 H 1.261430 0.649630 0.625353 0.026 Uiso 1 1 calc R U . . .
C25 C 1.0991(4) 0.5832(4) 0.6305(4) 0.0182(12) Uani 1 1 d . . . . .
H25 H 1.069614 0.641864 0.635141 0.022 Uiso 1 1 calc R U . . .
C28 C 0.8518(4) 0.5605(4) 0.6369(4) 0.0203(12) Uani 1 1 d . . . . .
H28 H 0.894208 0.625751 0.645520 0.024 Uiso 1 1 calc R U . . .
C29 C 0.7353(5) 0.5437(4) 0.6294(4) 0.0239(13) Uani 1 1 d . . . . .
H29 H 0.696726 0.597116 0.633523 0.029 Uiso 1 1 calc R U . . .
C30 C 0.6757(4) 0.4489(4) 0.6159(4) 0.0213(13) Uani 1 1 d . . . . .
H30 H 0.595248 0.436108 0.607573 0.026 Uiso 1 1 calc R U . . .
C31 C 0.7338(4) 0.3726(4) 0.6146(4) 0.0183(12) Uani 1 1 d . . . . .
H31 H 0.691655 0.307330 0.606747 0.022 Uiso 1 1 calc R U . . .
C34 C 1.0200(4) 0.2362(4) 0.5138(4) 0.0131(10) Uani 1 1 d . . . . .
C35 C 1.1079(4) 0.2352(4) 0.7063(4) 0.0158(11) Uani 1 1 d . . . . .
C36 C 0.9403(4) 0.1142(4) 0.6497(4) 0.0142(11) Uani 1 1 d . . . . .
C37 C 0.8166(4) 0.2030(4) 0.5266(4) 0.0169(11) Uani 1 1 d . . . . .
C33 C 0.9807(4) 0.3406(4) 0.7883(4) 0.0149(11) Uani 1 1 d . . . . .
C6 C 0.5823(4) -0.4836(4) 0.8614(3) 0.0140(11) Uani 1 1 d . . . . .
C7 C 0.4618(4) -0.4859(4) 0.8649(3) 0.0151(11) Uani 1 1 d . . . . .
C11 C 0.3229(4) -0.3934(4) 0.8799(4) 0.0170(11) Uani 1 1 d . . . . .
H11 H 0.300698 -0.331311 0.884009 0.020 Uiso 1 1 calc R U . . .
C10 C 0.2432(4) -0.4771(4) 0.8852(4) 0.0184(12) Uani 1 1 d . . . . .
H10 H 0.167519 -0.472162 0.892052 0.022 Uiso 1 1 calc R U . . .
C9 C 0.2742(4) -0.5685(4) 0.8806(4) 0.0209(13) Uani 1 1 d . . . . .
H9 H 0.220729 -0.626986 0.884052 0.025 Uiso 1 1 calc R U . . .
C8 C 0.3859(4) -0.5716(4) 0.8708(4) 0.0183(12) Uani 1 1 d . . . . .
H8 H 0.410097 -0.632914 0.868098 0.022 Uiso 1 1 calc R U . . .
C5 C 0.6280(4) -0.5687(4) 0.8610(4) 0.0175(11) Uani 1 1 d . . . . .
H5 H 0.579928 -0.631268 0.857453 0.021 Uiso 1 1 calc R U . . .
C4 C 0.7433(4) -0.5613(4) 0.8657(4) 0.0196(12) Uani 1 1 d . . . . .
H4 H 0.775774 -0.618646 0.865798 0.024 Uiso 1 1 calc R U . . .
C3 C 0.8107(4) -0.4698(4) 0.8702(4) 0.0204(12) Uani 1 1 d . . . . .
H3 H 0.890672 -0.462892 0.875350 0.025 Uiso 1 1 calc R U . . .
C2 C 0.7605(4) -0.3876(4) 0.8670(3) 0.0159(11) Uani 1 1 d . . . . .
H2 H 0.807606 -0.324838 0.867873 0.019 Uiso 1 1 calc R U . . .
C14 C 0.7009(4) -0.2103(4) 0.7780(3) 0.0138(11) Uani 1 1 d . . . . .
C16 C 0.4118(4) -0.2112(4) 0.7989(3) 0.0127(10) Uani 1 1 d . . . . .
C17 C 0.5186(4) -0.3227(4) 0.7042(4) 0.0128(11) Uani 1 1 d . . . . .
C18 C 0.5029(4) 0.2329(4) 1.0121(4) 0.0164(11) Uani 1 1 d . . . . .
O12 O 0.9971(3) 0.2442(3) 0.0081(3) 0.0307(10) Uani 1 1 d . . . . .
O11 O 0.1427(3) 0.9359(3) 0.0548(3) 0.0373(11) Uani 1 1 d . . . . .
H11B H 0.128089 0.956030 -0.010876 0.056 Uiso 1 1 d R U . . .
H11A H 0.224248 0.950980 0.063504 0.056 Uiso 1 1 d R U . . .
H3A H 0.147(6) 0.012(4) 0.485(3) 0.08(3) Uiso 1 1 d D . . . .
H3B H 0.136(5) 0.104(3) 0.545(4) 0.05(2) 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 C15 2.143(5) . ?
W1 C16 2.157(5) . ?
W1 C14 2.159(5) . ?
W1 C13 2.164(5) . ?
W1 C18 2.166(5) 2_657 ?
W1 C17 2.172(5) . ?
W1 N1 2.215(4) . ?
W1 N12 2.227(4) . ?
W2 C36 2.135(5) . ?
W2 C37 2.153(6) . ?
W2 C35 2.155(5) . ?
W2 C34 2.163(5) . ?
W2 C38 2.164(5) . ?
W2 C33 2.167(5) . ?
W2 N32 2.208(4) . ?
W2 N21 2.233(4) . ?
Na1 N18 2.398(5) . ?
Na1 O2 2.429(4) . ?
Na1 O1 2.508(4) . ?
Na1 N15 2.515(5) . ?
Na1 N38 2.523(4) . ?
Na1 O7 2.714(4) . ?
Na1 Na2 3.805(3) . ?
Na3 O7 2.347(4) . ?
Na3 O9 2.347(4) . ?
Na3 O8 2.378(4) . ?
Na3 N35 2.451(5) 1_455 ?
Na3 N13 2.481(5) 2_657 ?
Na3 Na4 3.527(3) 1_455 ?
Na2 O6 2.321(4) . ?
Na2 O3 2.347(4) . ?
Na2 O1 2.374(4) . ?
Na2 O5 2.440(4) . ?
Na2 O4 2.519(5) . ?
Na2 O2 2.625(5) . ?
Na4 O8 2.391(4) 1_655 ?
Na4 O10 2.430(5) . ?
Na4 N14 2.437(4) . ?
Na4 O9 2.450(4) 1_655 ?
Na4 N36 2.493(5) . ?
Na4 N34 2.528(5) 2_756 ?
O7 H7A 0.9535 . ?
O7 H7B 0.9667 . ?
O1 H1A 0.9550 . ?
O1 H1B 0.8245 . ?
O3 H3A 0.931(19) . ?
O3 H3B 0.931(19) . ?
O8 H8A 0.9408 . ?
O8 H8B 0.9438 . ?
O10 H10A 0.9459 . ?
O10 H10B 0.9470 . ?
N13 C13 1.141(6) . ?
N15 C15 1.156(7) . ?
N38 C38 1.152(6) . ?
N32 C27 1.363(6) . ?
N32 C31 1.367(6) . ?
N21 C26 1.353(6) . ?
N21 C22 1.356(6) . ?
N34 C34 1.153(6) . ?
N35 C35 1.147(6) . ?
N36 C36 1.159(7) . ?
N37 C37 1.160(7) . ?
N33 C33 1.146(6) . ?
N1 C6 1.355(6) . ?
N1 C2 1.361(6) . ?
N12 C7 1.356(7) . ?
N12 C11 1.362(6) . ?
N14 C14 1.146(6) . ?
N16 C16 1.146(6) . ?
N17 C17 1.148(6) . ?
N18 C18 1.131(6) . ?
C27 C28 1.394(7) . ?
C27 C26 1.447(7) . ?
C26 C25 1.403(7) . ?
C22 C23 1.372(7) . ?
C22 H22 0.9500 . ?
C23 C24 1.384(8) . ?
C23 H23 0.9500 . ?
C24 C25 1.371(7) . ?
C24 H24 0.9500 . ?
C25 H25 0.9500 . ?
C28 C29 1.379(7) . ?
C28 H28 0.9500 . ?
C29 C30 1.372(8) . ?
C29 H29 0.9500 . ?
C30 C31 1.376(7) . ?
C30 H30 0.9500 . ?
C31 H31 0.9500 . ?
C6 C5 1.394(7) . ?
C6 C7 1.464(7) . ?
C7 C8 1.379(7) . ?
C11 C10 1.384(7) . ?
C11 H11 0.9500 . ?
C10 C9 1.389(8) . ?
C10 H10 0.9500 . ?
C9 C8 1.389(7) . ?
C9 H9 0.9500 . ?
C8 H8 0.9500 . ?
C5 C4 1.377(7) . ?
C5 H5 0.9500 . ?
C4 C3 1.374(7) . ?
C4 H4 0.9500 . ?
C3 C2 1.389(7) . ?
C3 H3 0.9500 . ?
C2 H2 0.9500 . ?
O11 H11B 0.9727 . ?
O11 H11A 0.9634 . ?

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
C15 W1 C16 69.77(18) . . ?
C15 W1 C14 71.23(18) . . ?
C16 W1 C14 111.02(18) . . ?
C15 W1 C13 74.06(19) . . ?
C16 W1 C13 137.37(19) . . ?
C14 W1 C13 76.71(18) . . ?
C15 W1 C18 77.38(18) . 2_657 ?
C16 W1 C18 78.99(18) . 2_657 ?
C14 W1 C18 140.28(19) . 2_657 ?
C13 W1 C18 71.66(18) . 2_657 ?
C15 W1 C17 112.13(19) . . ?
C16 W1 C17 74.13(18) . . ?
C14 W1 C17 71.18(17) . . ?
C13 W1 C17 142.40(17) . . ?
C18 W1 C17 145.45(18) 2_657 . ?
C15 W1 N1 142.92(16) . . ?
C16 W1 N1 145.81(17) . . ?
C14 W1 N1 81.59(16) . . ?
C13 W1 N1 75.51(17) . . ?
C18 W1 N1 112.18(17) 2_657 . ?
C17 W1 N1 80.87(17) . . ?
C15 W1 N12 142.71(16) . . ?
C16 W1 N12 80.68(16) . . ?
C14 W1 N12 143.19(17) . . ?
C13 W1 N12 119.02(17) . . ?
C18 W1 N12 75.01(17) 2_657 . ?
C17 W1 N12 79.52(16) . . ?
N1 W1 N12 72.02(14) . . ?
C36 W2 C37 75.6(2) . . ?
C36 W2 C35 68.12(19) . . ?
C37 W2 C35 135.4(2) . . ?
C36 W2 C34 79.90(18) . . ?
C37 W2 C34 69.49(17) . . ?
C35 W2 C34 79.17(18) . . ?
C36 W2 C38 71.17(18) . . ?
C37 W2 C38 75.65(19) . . ?
C35 W2 C38 114.10(19) . . ?
C34 W2 C38 139.1(2) . . ?
C36 W2 C33 110.05(19) . . ?
C37 W2 C33 143.83(17) . . ?
C35 W2 C33 75.23(18) . . ?
C34 W2 C33 146.01(17) . . ?
C38 W2 C33 73.00(19) . . ?
C36 W2 N32 145.42(16) . . ?
C37 W2 N32 78.60(18) . . ?
C35 W2 N32 144.28(18) . . ?
C34 W2 N32 111.93(16) . . ?
C38 W2 N32 80.44(17) . . ?
C33 W2 N32 78.83(17) . . ?
C36 W2 N21 141.89(16) . . ?
C37 W2 N21 120.68(17) . . ?
C35 W2 N21 78.84(17) . . ?
C34 W2 N21 75.63(16) . . ?
C38 W2 N21 142.98(18) . . ?
C33 W2 N21 77.77(16) . . ?
N32 W2 N21 71.94(15) . . ?
N18 Na1 O2 91.50(16) . . ?
N18 Na1 O1 157.81(15) . . ?
O2 Na1 O1 80.12(15) . . ?
N18 Na1 N15 96.36(16) . . ?
O2 Na1 N15 165.48(18) . . ?
O1 Na1 N15 88.13(15) . . ?
N18 Na1 N38 103.17(16) . . ?
O2 Na1 N38 99.81(15) . . ?
O1 Na1 N38 98.52(14) . . ?
N15 Na1 N38 90.29(15) . . ?
N18 Na1 O7 75.30(14) . . ?
O2 Na1 O7 93.60(14) . . ?
O1 Na1 O7 84.70(13) . . ?
N15 Na1 O7 76.72(13) . . ?
N38 Na1 O7 166.55(16) . . ?
N18 Na1 Na2 133.25(14) . . ?
O2 Na1 Na2 43.14(11) . . ?
O1 Na1 Na2 37.54(10) . . ?
N15 Na1 Na2 125.67(13) . . ?
N38 Na1 Na2 96.72(12) . . ?
O7 Na1 Na2 93.74(10) . . ?
O7 Na3 O9 117.89(18) . . ?
O7 Na3 O8 82.77(15) . . ?
O9 Na3 O8 84.06(14) . . ?
O7 Na3 N35 115.80(16) . 1_455 ?
O9 Na3 N35 126.23(17) . 1_455 ?
O8 Na3 N35 100.04(16) . 1_455 ?
O7 Na3 N13 92.17(16) . 2_657 ?
O9 Na3 N13 95.91(15) . 2_657 ?
O8 Na3 N13 174.22(17) . 2_657 ?
N35 Na3 N13 84.66(16) 1_455 2_657 ?
O7 Na3 Na4 112.44(13) . 1_455 ?
O9 Na3 Na4 43.81(10) . 1_455 ?
O8 Na3 Na4 42.44(9) . 1_455 ?
N35 Na3 Na4 110.73(13) 1_455 1_455 ?
N13 Na3 Na4 138.85(12) 2_657 1_455 ?
O6 Na2 O3 154.00(18) . . ?
O6 Na2 O1 98.17(15) . . ?
O3 Na2 O1 107.45(15) . . ?
O6 Na2 O5 86.87(15) . . ?
O3 Na2 O5 86.19(15) . . ?
O1 Na2 O5 115.30(17) . . ?
O6 Na2 O4 73.55(15) . . ?
O3 Na2 O4 81.53(15) . . ?
O1 Na2 O4 152.41(18) . . ?
O5 Na2 O4 90.90(15) . . ?
O6 Na2 O2 80.08(15) . . ?
O3 Na2 O2 100.30(15) . . ?
O1 Na2 O2 78.76(14) . . ?
O5 Na2 O2 162.23(16) . . ?
O4 Na2 O2 73.93(15) . . ?
O6 Na2 Na1 83.81(12) . . ?
O3 Na2 Na1 113.09(12) . . ?
O1 Na2 Na1 40.07(11) . . ?
O5 Na2 Na1 151.13(12) . . ?
O4 Na2 Na1 112.34(13) . . ?
O2 Na2 Na1 39.24(10) . . ?
O8 Na4 O10 83.50(14) 1_655 . ?
O8 Na4 N14 175.27(18) 1_655 . ?
O10 Na4 N14 100.05(16) . . ?
O8 Na4 O9 81.62(14) 1_655 1_655 ?
O10 Na4 O9 87.70(16) . 1_655 ?
N14 Na4 O9 95.33(15) . 1_655 ?
O8 Na4 N36 82.85(14) 1_655 . ?
O10 Na4 N36 164.82(17) . . ?
N14 Na4 N36 93.24(16) . . ?
O9 Na4 N36 83.76(16) 1_655 . ?
O8 Na4 N34 92.49(14) 1_655 2_756 ?
O10 Na4 N34 94.27(16) . 2_756 ?
N14 Na4 N34 90.37(16) . 2_756 ?
O9 Na4 N34 173.55(15) 1_655 2_756 ?
N36 Na4 N34 92.94(16) . 2_756 ?
O8 Na4 Na3 42.16(10) 1_655 1_655 ?
O10 Na4 Na3 94.45(12) . 1_655 ?
N14 Na4 Na3 133.89(14) . 1_655 ?
O9 Na4 Na3 41.56(10) 1_655 1_655 ?
N36 Na4 Na3 70.89(12) . 1_655 ?
N34 Na4 Na3 132.06(11) 2_756 1_655 ?
Na3 O7 Na1 115.91(17) . . ?
Na3 O7 H7A 119.6 . . ?
Na1 O7 H7A 105.6 . . ?
Na3 O7 H7B 109.1 . . ?
Na1 O7 H7B 101.8 . . ?
H7A O7 H7B 102.6 . . ?
Na2 O1 Na1 102.39(16) . . ?
Na2 O1 H1A 127.7 . . ?
Na1 O1 H1A 90.5 . . ?
Na2 O1 H1B 109.1 . . ?
Na1 O1 H1B 110.8 . . ?
H1A O1 H1B 112.9 . . ?
Na1 O2 Na2 97.61(16) . . ?
Na2 O3 H3A 102(4) . . ?
Na2 O3 H3B 113(4) . . ?
H3A O3 H3B 110(4) . . ?
Na3 O8 Na4 95.39(13) . 1_455 ?
Na3 O8 H8A 117.5 . . ?
Na4 O8 H8A 117.1 1_455 . ?
Na3 O8 H8B 104.9 . . ?
Na4 O8 H8B 109.6 1_455 . ?
H8A O8 H8B 111.0 . . ?
Na3 O9 Na4 94.63(14) . 1_455 ?
Na4 O10 H10A 106.3 . . ?
Na4 O10 H10B 97.1 . . ?
H10A O10 H10B 108.9 . . ?
C13 N13 Na3 130.9(4) . 2_657 ?
C15 N15 Na1 136.3(4) . . ?
C38 N38 Na1 170.5(4) . . ?
C27 N32 C31 116.8(5) . . ?
C27 N32 W2 118.1(3) . . ?
C31 N32 W2 124.8(4) . . ?
C26 N21 C22 118.0(4) . . ?
C26 N21 W2 117.2(3) . . ?
C22 N21 W2 124.6(4) . . ?
C34 N34 Na4 146.7(4) . 2_756 ?
C35 N35 Na3 117.1(4) . 1_655 ?
C36 N36 Na4 157.6(4) . . ?
C6 N1 C2 116.9(5) . . ?
C6 N1 W1 118.7(3) . . ?
C2 N1 W1 124.4(3) . . ?
C7 N12 C11 117.4(4) . . ?
C7 N12 W1 118.6(3) . . ?
C11 N12 W1 123.9(4) . . ?
C14 N14 Na4 155.3(4) . . ?
C18 N18 Na1 152.6(4) . . ?
N13 C13 W1 175.6(4) . . ?
N15 C15 W1 178.0(5) . . ?
N38 C38 W2 176.3(5) . . ?
N32 C27 C28 122.0(4) . . ?
N32 C27 C26 114.8(5) . . ?
C28 C27 C26 123.2(5) . . ?
N21 C26 C25 121.2(4) . . ?
N21 C26 C27 115.9(5) . . ?
C25 C26 C27 122.9(5) . . ?
N21 C22 C23 122.5(5) . . ?
N21 C22 H22 118.8 . . ?
C23 C22 H22 118.8 . . ?
C22 C23 C24 119.9(5) . . ?
C22 C23 H23 120.0 . . ?
C24 C23 H23 120.0 . . ?
C25 C24 C23 118.2(5) . . ?
C25 C24 H24 120.9 . . ?
C23 C24 H24 120.9 . . ?
C24 C25 C26 120.1(5) . . ?
C24 C25 H25 120.0 . . ?
C26 C25 H25 120.0 . . ?
C29 C28 C27 119.4(5) . . ?
C29 C28 H28 120.3 . . ?
C27 C28 H28 120.3 . . ?
C30 C29 C28 119.3(5) . . ?
C30 C29 H29 120.4 . . ?
C28 C29 H29 120.4 . . ?
C29 C30 C31 119.2(5) . . ?
C29 C30 H30 120.4 . . ?
C31 C30 H30 120.4 . . ?
N32 C31 C30 123.1(5) . . ?
N32 C31 H31 118.5 . . ?
C30 C31 H31 118.5 . . ?
N34 C34 W2 177.7(4) . . ?
N35 C35 W2 176.1(5) . . ?
N36 C36 W2 179.3(4) . . ?
N37 C37 W2 176.3(5) . . ?
N33 C33 W2 177.4(5) . . ?
N1 C6 C5 122.4(4) . . ?
N1 C6 C7 115.4(5) . . ?
C5 C6 C7 122.2(5) . . ?
N12 C7 C8 122.4(5) . . ?
N12 C7 C6 114.7(4) . . ?
C8 C7 C6 122.7(5) . . ?
N12 C11 C10 122.5(5) . . ?
N12 C11 H11 118.8 . . ?
C10 C11 H11 118.8 . . ?
C11 C10 C9 119.7(5) . . ?
C11 C10 H10 120.1 . . ?
C9 C10 H10 120.1 . . ?
C10 C9 C8 117.8(5) . . ?
C10 C9 H9 121.1 . . ?
C8 C9 H9 121.1 . . ?
C7 C8 C9 120.1(5) . . ?
C7 C8 H8 119.9 . . ?
C9 C8 H8 119.9 . . ?
C4 C5 C6 119.6(5) . . ?
C4 C5 H5 120.2 . . ?
C6 C5 H5 120.2 . . ?
C3 C4 C5 118.9(5) . . ?
C3 C4 H4 120.5 . . ?
C5 C4 H4 120.5 . . ?
C4 C3 C2 119.2(5) . . ?
C4 C3 H3 120.4 . . ?
C2 C3 H3 120.4 . . ?
N1 C2 C3 123.0(5) . . ?
N1 C2 H2 118.5 . . ?
C3 C2 H2 118.5 . . ?
N14 C14 W1 179.1(5) . . ?
N16 C16 W1 177.6(4) . . ?
N17 C17 W1 175.9(4) . . ?
N18 C18 W1 178.0(5) . 2_657 ?
H11B O11 H11A 98.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C31 N32 C27 C28 4.6(7) . . . . ?
W2 N32 C27 C28 -169.2(4) . . . . ?
C31 N32 C27 C26 -173.1(4) . . . . ?
W2 N32 C27 C26 13.1(5) . . . . ?
C22 N21 C26 C25 -2.4(7) . . . . ?
W2 N21 C26 C25 173.0(4) . . . . ?
C22 N21 C26 C27 175.6(4) . . . . ?
W2 N21 C26 C27 -8.9(5) . . . . ?
N32 C27 C26 N21 -2.5(6) . . . . ?
C28 C27 C26 N21 179.8(4) . . . . ?
N32 C27 C26 C25 175.5(4) . . . . ?
C28 C27 C26 C25 -2.2(8) . . . . ?
C26 N21 C22 C23 1.3(7) . . . . ?
W2 N21 C22 C23 -173.7(4) . . . . ?
N21 C22 C23 C24 1.0(8) . . . . ?
C22 C23 C24 C25 -2.3(7) . . . . ?
C23 C24 C25 C26 1.2(7) . . . . ?
N21 C26 C25 C24 1.2(7) . . . . ?
C27 C26 C25 C24 -176.7(5) . . . . ?
N32 C27 C28 C29 -3.2(7) . . . . ?
C26 C27 C28 C29 174.3(5) . . . . ?
C27 C28 C29 C30 -0.7(8) . . . . ?
C28 C29 C30 C31 2.9(8) . . . . ?
C27 N32 C31 C30 -2.3(7) . . . . ?
W2 N32 C31 C30 171.1(4) . . . . ?
C29 C30 C31 N32 -1.4(8) . . . . ?
C2 N1 C6 C5 -2.1(7) . . . . ?
W1 N1 C6 C5 176.6(4) . . . . ?
C2 N1 C6 C7 175.2(4) . . . . ?
W1 N1 C6 C7 -6.1(5) . . . . ?
C11 N12 C7 C8 0.6(7) . . . . ?
W1 N12 C7 C8 -178.6(4) . . . . ?
C11 N12 C7 C6 -175.0(4) . . . . ?
W1 N12 C7 C6 5.8(6) . . . . ?
N1 C6 C7 N12 0.1(6) . . . . ?
C5 C6 C7 N12 177.5(4) . . . . ?
N1 C6 C7 C8 -175.4(4) . . . . ?
C5 C6 C7 C8 1.9(8) . . . . ?
C7 N12 C11 C10 -1.2(7) . . . . ?
W1 N12 C11 C10 177.9(4) . . . . ?
N12 C11 C10 C9 0.9(8) . . . . ?
C11 C10 C9 C8 0.1(7) . . . . ?
N12 C7 C8 C9 0.3(8) . . . . ?
C6 C7 C8 C9 175.6(5) . . . . ?
C10 C9 C8 C7 -0.7(8) . . . . ?
N1 C6 C5 C4 2.4(8) . . . . ?
C7 C6 C5 C4 -174.7(5) . . . . ?
C6 C5 C4 C3 -0.3(8) . . . . ?
C5 C4 C3 C2 -1.8(8) . . . . ?
C6 N1 C2 C3 -0.2(7) . . . . ?
W1 N1 C2 C3 -178.8(4) . . . . ?
C4 C3 C2 N1 2.2(8) . . . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
O7 H7A N15 0.95 2.43 3.344(6) 159.8 2_657 yes
O7 H7B N16 0.97 2.13 3.086(6) 167.8 . yes
O1 H1A O5 0.96 1.85 2.771(5) 162.4 2_656 yes
O1 H1B N37 0.82 2.67 3.185(6) 122.0 2_656 yes
O1 H1B N16 0.82 2.54 3.298(6) 154.3 . yes
O8 H8A N16 0.94 2.09 2.996(6) 161.1 . yes
O8 H8B O3 0.94 1.81 2.756(5) 175.0 . yes
O10 H10A O12 0.95 1.89 2.832(5) 178.4 2_756 yes
O10 H10B N16 0.95 2.44 3.363(6) 164.2 1_655 yes
C22 H22 O4 0.95 2.65 3.452(6) 142.2 1_655 yes
C22 H22 N35 0.95 2.66 3.310(7) 126.3 . yes
C23 H23 N17 0.95 2.64 3.337(6) 130.8 1_665 yes
C28 H28 N34 0.95 2.61 3.406(7) 141.9 2_766 yes
C31 H31 O6 0.95 2.50 3.325(7) 144.8 . yes
C11 H11 N16 0.95 2.65 3.343(7) 130.5 . yes
C10 H10 N33 0.95 2.61 3.243(7) 124.7 1_445 yes
C5 H5 N18 0.95 2.52 3.331(7) 143.9 1_545 yes
O11 H11B O9 0.97 1.98 2.870(6) 150.5 1_564 yes
O11 H11A N15 0.96 2.08 2.997(6) 158.2 2_666 yes
O3 H3A N36 0.931(19) 2.05(3) 2.935(6) 159(6) 2_656 yes
O3 H3B N34 0.931(19) 2.37(4) 3.165(6) 144(5) 1_455 yes

_refine_diff_density_max         1.228
_refine_diff_density_min         -1.019
_refine_diff_density_rms         0.159



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

data_shelx_CCDC1
_database_code_depnum_ccdc_archive 'CCDC 1969728'
loop_
_audit_author_name
_audit_author_address
'Maciej Hodorowicz'
;Faculty of Chemistry, Jagiellonian University
Poland
;
_audit_update_record             
;
2019-12-03 deposited with the CCDC.	2021-04-21 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2016/6
_shelx_SHELXL_version_number     2016/6
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C18 H11 N9 Na2 O4.90 W'
_chemical_formula_weight         661.57

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'
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'
W W -0.8490 6.8722 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

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

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   8.5595(2)
_cell_length_b                   9.86220(10)
_cell_length_c                   13.8861(3)
_cell_angle_alpha                94.3490(10)
_cell_angle_beta                 99.660(2)
_cell_angle_gamma                98.2060(10)
_cell_volume                     1137.75(4)
_cell_formula_units_Z            2
_cell_measurement_temperature    130(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       ?
_exptl_crystal_colour            ?
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.931
_exptl_crystal_F_000             634
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.050
_exptl_absorpt_coefficient_mu    5.165
_shelx_estimated_absorpt_T_min   0.425
_shelx_estimated_absorpt_T_max   0.782
_exptl_absorpt_correction_type   ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      130(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  ?
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            39905
_diffrn_reflns_av_unetI/netI     0.0579
_diffrn_reflns_av_R_equivalents  0.0992
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         2.097
_diffrn_reflns_theta_max         32.170
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.877
_diffrn_measured_fraction_theta_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.877
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.877
_diffrn_reflns_point_group_measured_fraction_full 0.995
_reflns_number_total             7030
_reflns_number_gt                6231
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXT 2014/4 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0819P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         7030
_refine_ls_number_parameters     358
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0542
_refine_ls_R_factor_gt           0.0469
_refine_ls_wR_factor_ref         0.1232
_refine_ls_wR_factor_gt          0.1191
_refine_ls_goodness_of_fit_ref   1.076
_refine_ls_restrained_S_all      1.076
_refine_ls_shift/su_max          0.031
_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 0.91490(2) 0.70253(2) 0.23319(2) 0.01411(8) Uani 1 1 d . . . . .
Na1 Na 0.4849(5) 0.6452(5) 0.4271(3) 0.0775(11) Uani 1 1 d . . . . .
Na2 Na 0.8202(3) 0.7417(2) 0.61957(17) 0.0310(5) Uani 1 1 d . . . . .
O3 O 0.6323(7) 0.7310(6) 0.7313(6) 0.0656(19) Uani 1 1 d . . . . .
O1A O 0.3706(9) 0.4628(7) 0.4461(6) 0.022(2) Uani 0.474(13) 1 d . . P A 1
O1B O 0.2642(10) 0.5221(9) 0.4796(7) 0.036(2) Uani 0.526(13) 1 d . . P A 2
O2 O 0.6070(6) 0.8268(8) 0.5100(5) 0.073(2) Uani 1 1 d . . . . .
N1 N 1.0213(5) 0.7820(4) 0.1096(3) 0.0178(8) Uani 1 1 d . . . . .
N2 N 0.8062(5) 0.5609(4) 0.0979(3) 0.0187(8) Uani 1 1 d . . . . .
N6 N 1.0171(6) 1.0314(5) 0.3190(3) 0.0253(9) Uani 1 1 d . . . . .
N8 N 0.6334(6) 0.8714(5) 0.1306(5) 0.0434(15) Uani 1 1 d . . . . .
N7 N 0.5876(8) 0.5493(6) 0.2998(6) 0.054(2) Uani 1 1 d . . . . .
N3 N 1.3043(7) 0.7470(7) 0.3218(6) 0.063(2) Uani 1 1 d . . . . .
N4 N 1.0117(6) 0.4002(5) 0.2854(3) 0.0256(9) Uani 1 1 d . . . . .
C1 C 0.9553(6) 0.7236(5) 0.0173(4) 0.0186(9) Uani 1 1 d . . . . .
C7 C 1.0024(7) 0.7772(6) -0.0658(4) 0.0271(11) Uani 1 1 d . . . . .
H7 H 0.950816 0.737361 -0.129663 0.033 Uiso 1 1 calc R U . . .
C8 C 1.1232(8) 0.8872(6) -0.0544(5) 0.0312(13) Uani 1 1 d . . . . .
H8 H 1.156350 0.924792 -0.110095 0.037 Uiso 1 1 calc R U . . .
C9 C 1.1953(8) 0.9423(6) 0.0385(5) 0.0332(14) Uani 1 1 d . . . . .
H9 H 1.282253 1.016445 0.047857 0.040 Uiso 1 1 calc R U . . .
C10 C 1.1410(7) 0.8893(6) 0.1193(4) 0.0268(11) Uani 1 1 d . . . . .
H10 H 1.190106 0.930381 0.183340 0.032 Uiso 1 1 calc R U . . .
C2 C 0.8355(6) 0.6008(5) 0.0112(4) 0.0187(9) Uani 1 1 d . . . . .
C6 C 0.7654(7) 0.5239(6) -0.0782(4) 0.0281(12) Uani 1 1 d . . . . .
H6 H 0.789349 0.553607 -0.138382 0.034 Uiso 1 1 calc R U . . .
C5 C 0.6606(7) 0.4038(6) -0.0773(5) 0.0320(14) Uani 1 1 d . . . . .
H5 H 0.608390 0.351032 -0.137062 0.038 Uiso 1 1 calc R U . . .
C4 C 0.6332(6) 0.3617(5) 0.0114(5) 0.0312(13) Uani 1 1 d . . . . .
H4 H 0.563861 0.278019 0.013341 0.037 Uiso 1 1 calc R U . . .
C3 C 0.7061(6) 0.4408(5) 0.0974(4) 0.0244(10) Uani 1 1 d . . . . .
H3 H 0.685828 0.410493 0.158148 0.029 Uiso 1 1 calc R U . . .
C12 C 0.9797(6) 0.5053(5) 0.2660(4) 0.0201(9) Uani 1 1 d . . . . .
C14 C 0.9778(6) 0.9158(5) 0.2885(3) 0.0174(8) Uani 1 1 d . . . . .
C16 C 0.7275(6) 0.8089(5) 0.1671(4) 0.0237(10) Uani 1 1 d . . . . .
C15 C 0.6993(7) 0.6053(6) 0.2763(6) 0.0315(14) Uani 1 1 d . . . . .
C11 C 1.1698(7) 0.7271(6) 0.2886(5) 0.0313(13) Uani 1 1 d . . . . .
C13 C 0.9388(11) 0.7198(6) 0.3900(5) 0.0416(17) Uani 1 1 d . . . . .
O4A O 1.4731(17) 0.9895(16) 0.3038(17) 0.050(6) Uani 0.51(4) 1 d . . P B 3
O4B O 1.4956(12) 1.0138(10) 0.2526(13) 0.029(4) Uani 0.49(4) 1 d . . P B 4
O5 O 0.2105(10) 0.6291(8) 0.5522(6) 0.039(3) Uani 0.582(19) 1 d . . . . .
O6 O 0.6954(17) 0.1864(13) 0.2471(11) 0.027(5) Uani 0.290(18) 1 d . . . . .
C17 C 0.4082(6) 0.8211(5) 0.5876(6) 0.0394(17) Uani 1 1 d . . . . .
H17A H 0.379281 0.740103 0.538943 0.059 Uiso 1 1 calc R U . . .
H17B H 0.400727 0.792687 0.652984 0.059 Uiso 1 1 calc R U . . .
H17C H 0.518224 0.864693 0.586946 0.059 Uiso 1 1 calc R U . . .
N9 N 0.2021(10) 0.9550(9) 0.5300(7) 0.066(2) Uani 1 1 d . . . . .
C18 C 0.3039(10) 0.9139(9) 0.5647(7) 0.0524(19) Uani 1 1 d . . . . .
N5A N 0.997(3) 0.7315(12) 0.4771(8) 0.017(4) Uani 0.42(5) 1 d . . P C 5
N5B N 0.913(4) 0.7214(11) 0.4702(7) 0.028(5) Uani 0.58(5) 1 d . . P C 6


_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 C14 2.144(5) . ?
W1 C13 2.144(6) . ?
W1 C15 2.153(6) . ?
W1 C16 2.156(5) . ?
W1 C12 2.158(5) . ?
W1 C11 2.161(6) . ?
W1 N1 2.216(4) . ?
W1 N2 2.234(4) . ?
Na1 O1A 1.980(9) . ?
Na1 O2 2.091(9) . ?
Na1 N7 2.302(9) . ?
Na1 N3 2.333(8) 1_455 ?
Na1 O1B 2.348(10) . ?
Na1 O1A 2.386(9) 2_666 ?
Na1 C15 3.047(8) . ?
Na1 Na2 3.542(5) . ?
Na1 Na1 3.644(9) 2_666 ?
Na2 N5B 2.349(14) . ?
Na2 O3 2.413(7) . ?
Na2 O1A 2.418(7) 2_666 ?
Na2 N4 2.447(5) 2_766 ?
Na2 O2 2.460(6) . ?
Na2 N6 2.469(5) 2_776 ?
Na2 N5A 2.69(2) . ?
Na2 O1B 2.787(10) 2_666 ?
O1B O5 1.572(13) . ?
N1 C10 1.346(6) . ?
N1 C1 1.359(6) . ?
N2 C2 1.347(7) . ?
N2 C3 1.358(6) . ?
N6 C14 1.167(6) . ?
N8 C16 1.157(7) . ?
N7 C15 1.143(8) . ?
N3 C11 1.149(8) . ?
N4 C12 1.149(7) . ?
C1 C7 1.401(7) . ?
C1 C2 1.458(7) . ?
C7 C8 1.367(9) . ?
C7 H7 0.9500 . ?
C8 C9 1.368(10) . ?
C8 H8 0.9500 . ?
C9 C10 1.395(8) . ?
C9 H9 0.9500 . ?
C10 H10 0.9500 . ?
C2 C6 1.398(7) . ?
C6 C5 1.383(9) . ?
C6 H6 0.9500 . ?
C5 C4 1.376(10) . ?
C5 H5 0.9500 . ?
C4 C3 1.376(8) . ?
C4 H4 0.9500 . ?
C3 H3 0.9500 . ?
C13 N5B 1.169(12) . ?
C13 N5A 1.218(16) . ?
C17 C18 1.385(10) . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
N9 C18 1.070(11) . ?

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
C14 W1 C13 71.2(2) . . ?
C14 W1 C15 112.7(2) . . ?
C13 W1 C15 69.2(3) . . ?
C14 W1 C16 72.16(18) . . ?
C13 W1 C16 111.4(3) . . ?
C15 W1 C16 74.7(2) . . ?
C14 W1 C12 139.78(18) . . ?
C13 W1 C12 78.6(2) . . ?
C15 W1 C12 79.02(19) . . ?
C16 W1 C12 145.64(18) . . ?
C14 W1 C11 76.10(19) . . ?
C13 W1 C11 74.6(3) . . ?
C15 W1 C11 136.5(3) . . ?
C16 W1 C11 143.1(2) . . ?
C12 W1 C11 70.7(2) . . ?
C14 W1 N1 80.87(16) . . ?
C13 W1 N1 144.0(2) . . ?
C15 W1 N1 145.0(2) . . ?
C16 W1 N1 79.76(18) . . ?
C12 W1 N1 112.14(16) . . ?
C11 W1 N1 77.0(2) . . ?
C14 W1 N2 142.98(17) . . ?
C13 W1 N2 142.4(2) . . ?
C15 W1 N2 79.5(2) . . ?
C16 W1 N2 78.33(18) . . ?
C12 W1 N2 75.41(17) . . ?
C11 W1 N2 120.14(19) . . ?
N1 W1 N2 72.19(15) . . ?
O1A Na1 O2 139.7(4) . . ?
O1A Na1 N7 91.0(3) . . ?
O2 Na1 N7 120.3(3) . . ?
O1A Na1 N3 106.7(3) . 1_455 ?
O2 Na1 N3 96.9(3) . 1_455 ?
N7 Na1 N3 92.9(3) . 1_455 ?
O2 Na1 O1B 119.3(4) . . ?
N7 Na1 O1B 119.7(3) . . ?
N3 Na1 O1B 88.2(3) 1_455 . ?
O1A Na1 O1A 67.2(3) . 2_666 ?
O2 Na1 O1A 83.6(3) . 2_666 ?
N7 Na1 O1A 96.5(3) . 2_666 ?
N3 Na1 O1A 168.8(4) 1_455 2_666 ?
O1A Na1 C15 108.6(3) . . ?
O2 Na1 C15 101.5(3) . . ?
N7 Na1 C15 18.9(2) . . ?
N3 Na1 C15 94.0(3) 1_455 . ?
O1B Na1 C15 138.6(3) . . ?
O1A Na1 C15 96.9(3) 2_666 . ?
O1A Na1 Na2 109.0(3) . . ?
O2 Na1 Na2 42.82(17) . . ?
N7 Na1 Na2 104.6(2) . . ?
N3 Na1 Na2 139.6(2) 1_455 . ?
O1B Na1 Na2 112.5(3) . . ?
O1A Na1 Na2 42.84(19) 2_666 . ?
C15 Na1 Na2 92.00(18) . . ?
O1A Na1 Na1 37.1(2) . 2_666 ?
O2 Na1 Na1 110.0(3) . 2_666 ?
N7 Na1 Na1 94.9(2) . 2_666 ?
N3 Na1 Na1 143.0(3) 1_455 2_666 ?
O1A Na1 Na1 30.05(19) 2_666 2_666 ?
C15 Na1 Na1 104.6(2) . 2_666 ?
Na2 Na1 Na1 72.38(13) . 2_666 ?
N5B Na2 O3 158.6(8) . . ?
O3 Na2 O1A 76.7(3) . 2_666 ?
N5B Na2 N4 99.9(5) . 2_766 ?
O3 Na2 N4 92.54(19) . 2_766 ?
O1A Na2 N4 89.6(2) 2_666 2_766 ?
N5B Na2 O2 79.4(7) . . ?
O3 Na2 O2 84.2(2) . . ?
O1A Na2 O2 75.6(2) 2_666 . ?
N4 Na2 O2 165.2(2) 2_766 . ?
O3 Na2 N6 99.7(2) . 2_776 ?
O1A Na2 N6 171.9(2) 2_666 2_776 ?
N4 Na2 N6 97.91(18) 2_766 2_776 ?
O2 Na2 N6 96.8(2) . 2_776 ?
O3 Na2 N5A 172.1(5) . . ?
N4 Na2 N5A 90.2(4) 2_766 . ?
O2 Na2 N5A 91.3(5) . . ?
N6 Na2 N5A 87.3(4) 2_776 . ?
O3 Na2 O1B 100.2(2) . 2_666 ?
O1A Na2 O1B 27.3(3) 2_666 2_666 ?
N4 Na2 O1B 74.9(2) 2_766 2_666 ?
O2 Na2 O1B 91.5(3) . 2_666 ?
N6 Na2 O1B 159.0(2) 2_776 2_666 ?
N5B Na2 Na1 71.5(7) . . ?
O3 Na2 Na1 87.2(2) . . ?
O1A Na2 Na1 42.15(19) 2_666 . ?
N4 Na2 Na1 130.34(15) 2_766 . ?
O2 Na2 Na1 35.3(2) . . ?
N6 Na2 Na1 131.10(15) 2_776 . ?
N5A Na2 Na1 85.4(5) . . ?
O1B Na2 Na1 56.5(2) 2_666 . ?
Na1 O1A Na1 112.8(3) . 2_666 ?
Na1 O1A Na2 149.5(4) . 2_666 ?
Na1 O1A Na2 95.0(3) 2_666 2_666 ?
O5 O1B Na1 104.7(5) . . ?
O5 O1B Na2 143.8(5) . 2_666 ?
Na1 O1B Na2 111.2(4) . 2_666 ?
Na1 O2 Na2 101.9(3) . . ?
C10 N1 C1 117.7(4) . . ?
C10 N1 W1 124.4(4) . . ?
C1 N1 W1 117.8(3) . . ?
C2 N2 C3 118.2(4) . . ?
C2 N2 W1 117.7(3) . . ?
C3 N2 W1 124.0(4) . . ?
C14 N6 Na2 162.9(4) . 2_776 ?
C15 N7 Na1 120.5(6) . . ?
C11 N3 Na1 137.9(7) . 1_655 ?
C12 N4 Na2 151.6(4) . 2_766 ?
N1 C1 C7 121.7(5) . . ?
N1 C1 C2 115.5(4) . . ?
C7 C1 C2 122.7(5) . . ?
C8 C7 C1 119.6(5) . . ?
C8 C7 H7 120.2 . . ?
C1 C7 H7 120.2 . . ?
C7 C8 C9 118.9(5) . . ?
C7 C8 H8 120.6 . . ?
C9 C8 H8 120.6 . . ?
C8 C9 C10 119.8(5) . . ?
C8 C9 H9 120.1 . . ?
C10 C9 H9 120.1 . . ?
N1 C10 C9 122.2(5) . . ?
N1 C10 H10 118.9 . . ?
C9 C10 H10 118.9 . . ?
N2 C2 C6 122.3(5) . . ?
N2 C2 C1 115.4(4) . . ?
C6 C2 C1 122.1(5) . . ?
C5 C6 C2 118.6(6) . . ?
C5 C6 H6 120.7 . . ?
C2 C6 H6 120.7 . . ?
C4 C5 C6 119.0(5) . . ?
C4 C5 H5 120.5 . . ?
C6 C5 H5 120.5 . . ?
C5 C4 C3 120.0(5) . . ?
C5 C4 H4 120.0 . . ?
C3 C4 H4 120.0 . . ?
N2 C3 C4 121.8(6) . . ?
N2 C3 H3 119.1 . . ?
C4 C3 H3 119.1 . . ?
N4 C12 W1 178.2(5) . . ?
N6 C14 W1 177.8(4) . . ?
N8 C16 W1 176.3(5) . . ?
N7 C15 W1 177.3(5) . . ?
N7 C15 Na1 40.6(5) . . ?
W1 C15 Na1 140.8(3) . . ?
N3 C11 W1 175.8(6) . . ?
N5B C13 W1 164.2(17) . . ?
N5A C13 W1 161.8(14) . . ?
C18 C17 H17A 109.5 . . ?
C18 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
C18 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
N9 C18 C17 159.9(10) . . ?
C13 N5A Na2 123.0(18) . . ?
C13 N5B Na2 169(2) . . ?

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
C10 N1 C1 C7 -3.8(7) . . . . ?
W1 N1 C1 C7 172.6(4) . . . . ?
C10 N1 C1 C2 175.1(5) . . . . ?
W1 N1 C1 C2 -8.5(6) . . . . ?
N1 C1 C7 C8 3.2(8) . . . . ?
C2 C1 C7 C8 -175.6(5) . . . . ?
C1 C7 C8 C9 0.1(8) . . . . ?
C7 C8 C9 C10 -2.5(9) . . . . ?
C1 N1 C10 C9 1.3(8) . . . . ?
W1 N1 C10 C9 -174.9(4) . . . . ?
C8 C9 C10 N1 1.9(9) . . . . ?
C3 N2 C2 C6 0.7(7) . . . . ?
W1 N2 C2 C6 -176.0(4) . . . . ?
C3 N2 C2 C1 -174.4(4) . . . . ?
W1 N2 C2 C1 8.8(5) . . . . ?
N1 C1 C2 N2 -0.3(7) . . . . ?
C7 C1 C2 N2 178.6(5) . . . . ?
N1 C1 C2 C6 -175.4(5) . . . . ?
C7 C1 C2 C6 3.5(8) . . . . ?
N2 C2 C6 C5 1.0(8) . . . . ?
C1 C2 C6 C5 175.8(5) . . . . ?
C2 C6 C5 C4 -2.2(8) . . . . ?
C6 C5 C4 C3 1.8(8) . . . . ?
C2 N2 C3 C4 -1.1(7) . . . . ?
W1 N2 C3 C4 175.4(4) . . . . ?
C5 C4 C3 N2 -0.1(8) . . . . ?
W1 C13 N5A Na2 179.0(16) . . . . ?
W1 C13 N5B Na2 -37(8) . . . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
C7 H7 N4 0.95 2.56 3.374(7) 144.4 2_765
C10 H10 O4B 0.95 2.62 3.294(13) 128.3 .
C4 H4 N8 0.95 2.59 3.269(7) 128.3 2_665
C3 H3 N7 0.95 2.63 3.298(9) 127.6 .
C3 H3 O6 0.95 2.62 3.378(14) 137.4 .
C17 H17A O1B 0.98 2.26 3.183(11) 155.7 .
C17 H17A O5 0.98 1.73 2.314(9) 114.5 .
C17 H17B O3 0.98 2.28 2.816(10) 113.2 .
C17 H17B O6 0.98 1.74 2.598(15) 143.9 2_666
C17 H17C O2 0.98 1.47 2.158(9) 122.5 .

_refine_diff_density_max         2.204
_refine_diff_density_min         -3.048
_refine_diff_density_rms         0.271



