# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2023

####################################################################### 
# 
# 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_fe3_a_sq
_database_code_depnum_ccdc_archive 'CCDC 2205561'
loop_
_audit_author_name
_audit_author_address
'Natalya Izarova'
;Institute of Inorganic Chemistry, RWTH Aachen University
Germany
;
_audit_update_record             
;
2022-09-06 deposited with the CCDC.	2022-12-12 downloaded from the CCDC.
;

# start Validation Reply Form
_vrf_PLAT201_fe3_a_sq            
;
PROBLEM: Isotropic non-H Atoms in Main Residue(s) .......         28 Report
RESPONSE: Only heavy atoms (W, Fe, P and Na) were refined anisotropically 
which is a common practice in polyoxotungstates crystallography. 
;
_vrf_PLAT973_fe3_a_sq            
;
PROBLEM: Check Calcd Positive Resid. Density on        W5       2.08 eA-3  
RESPONSE: The hole in the electron density can be attributed to inaccuracies 
in absorption correction. Nevertheless, chemical sense does not allow to 
place any other element in this position.
;
_vrf_PLAT342_fe3_a_sq            
;
PROBLEM: Low Bond Precision on  C-C Bonds ...............       0.07 Ang.  
RESPONSE: The issue with the low C-C bond precision most likely arises 
from the rotational disorder of the CH2-OH groups of the 
tris(hydroxymethyl)aminomethane ligands.
;
_vrf_PLAT975_fe3_a_sq            
;
PROBLEM: Check Calcd Resid. Dens.  0.86Ang From O2W     .       1.57 eA-3  
RESPONSE: This alert is due to a heavy disorder of this co-crystallized
solvent water molecule. Modeling of the disorder does not make much sense 
in this case as the refined occupancies of the additional sites will be
very small (less than 10 %). The anaccounted diffuse electron density 
was treated with the SQUEEZE procedure.
;
# end Validation Reply Form

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C36 H130 Cl0.50 Fe3 N9 Na0.50 O88 P2 W15'
_chemical_formula_weight         5113.94

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Na Na 0.0362 0.0249 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 '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      hexagonal
_space_group_IT_number           173
_space_group_name_H-M_alt        'P 63'
_space_group_name_Hall           'P 6c'

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

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

_cell_length_a                   16.376(2)
_cell_length_b                   16.376(2)
_cell_length_c                   25.646(5)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     5956(2)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    6917
_cell_measurement_theta_min      1.45
_cell_measurement_theta_max      24.89

_exptl_crystal_description       octahedron
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    2.851
_exptl_crystal_F_000             4690
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.310
_exptl_crystal_size_mid          0.300
_exptl_crystal_size_min          0.230
_exptl_absorpt_coefficient_mu    14.916
_shelx_estimated_absorpt_T_min   0.091
_shelx_estimated_absorpt_T_max   0.131
_exptl_absorpt_correction_type   integration
_exptl_absorpt_correction_T_min  0.0414
_exptl_absorpt_correction_T_max  0.1126
_exptl_absorpt_process_details   
;
STOE X-Red32, absorption correction by Gaussian integration. 
Afterwards scaling of reflection intensities was performed 
within STOE LANA. 
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'Genix Mo'
_diffrn_measurement_device_type  'STOE STADIVARI'
_diffrn_measurement_method       'rotation method, ω scans'
_diffrn_detector_area_resol_mean 5.81
_diffrn_reflns_number            33235
_diffrn_reflns_av_unetI/netI     0.0769
_diffrn_reflns_av_R_equivalents  0.1158
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_theta_min         2.141
_diffrn_reflns_theta_max         25.027
_diffrn_reflns_theta_full        25.027
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.846
_diffrn_reflns_point_group_measured_fraction_full 0.846
_reflns_number_total             5959
_reflns_number_gt                3856
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.653
_reflns_Friedel_fraction_max     0.685
_reflns_Friedel_fraction_full    0.685

_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. Completness statistics refer to single and
 composite reflections containing twin component 1 only.
;

_computing_data_collection       
;
X-Area Pilatus3_SV 1.31.170.0 (STOE, 2020)
;
_computing_cell_refinement       
;
X-Area Recipe 1.36.0.0 (STOE, 2020)
;
_computing_data_reduction        
;
X-Area Integrate 1.78.3.0 (STOE, 2020)
X-Area LANA 1.83.8.0 (STOE, 2020)
;
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    'Diamond 4'
_computing_publication_material  
;
STOE & Cie GmbH, X-Area, software package for collecting single-crystal or
multi-domain crystal data on STOE area-detector diffractometers, for image 
processing, for the correction and scaling of reflection intensities and 
for outlier rejection, version 1.90, Darmstadt 2020
;
_refine_special_details          
;
 Refined as a 2-component inversion twin.

loop_
  _platon_squeeze_void_nr
  _platon_squeeze_void_average_x
  _platon_squeeze_void_average_y
  _platon_squeeze_void_average_z
  _platon_squeeze_void_volume
  _platon_squeeze_void_count_electrons
  _platon_squeeze_void_content
   1 -0.016 -0.012 -0.053      1545       397 ' '
_platon_squeeze_void_probe_radius                  1.20
_platon_squeeze_details               
The unit cell contains 12 tris(hydroxymethyl)ammonimmethane cations, 
which had to be treated as a diffuse contribution to the overall 
scattering without specific atom positions by SQUEEZE/PLATON.  
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1811P)²] 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_abs_structure_details 
;
 Refined as an inversion twin.
 
;
_refine_ls_abs_structure_Flack   0.33(5)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         5959
_refine_ls_number_parameters     228
_refine_ls_number_restraints     7
_refine_ls_R_factor_all          0.1213
_refine_ls_R_factor_gt           0.0835
_refine_ls_wR_factor_ref         0.2641
_refine_ls_wR_factor_gt          0.2255
_refine_ls_goodness_of_fit_ref   1.012
_refine_ls_restrained_S_all      1.012
_refine_ls_shift/su_max          0.022
_refine_ls_shift/su_mean         0.001

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 0.43589(13) 0.63813(12) 0.73277(10) 0.0586(5) Uani 1 1 d . . . . .
W2 W 0.57745(14) 0.75027(15) 0.61404(6) 0.0616(7) Uani 1 1 d . . . . .
W3 W 0.50465(14) 0.90824(13) 0.61408(6) 0.0601(6) Uani 1 1 d . . . . .
W4 W 0.57709(14) 0.74864(15) 0.46632(7) 0.0617(7) Uani 1 1 d . . . . .
W5 W 0.50184(14) 0.90682(13) 0.46622(7) 0.0592(6) Uani 1 1 d . . . . .
P1 P 0.333333 0.666667 0.6186(8) 0.049(5) Uani 1 3 d S T P . .
P2 P 0.333333 0.666667 0.4594(8) 0.054(6) Uani 1 3 d S T P . .
Fe1 Fe 0.3567(5) 0.7927(4) 0.3521(3) 0.0574(17) Uani 1 1 d . . . . .
O1T O 0.494(2) 0.6126(18) 0.7789(11) 0.050(7) Uiso 1 1 d . . . . .
O2T O 0.689(2) 0.766(2) 0.6263(12) 0.064(9) Uiso 1 1 d . . . . .
O3T O 0.5747(19) 1.0286(19) 0.6280(10) 0.052(7) Uiso 1 1 d . . . . .
O4T O 0.684(2) 0.7662(19) 0.4598(11) 0.054(7) Uiso 1 1 d . . . . .
O5T O 0.554(3) 1.021(3) 0.4612(15) 0.101(13) Uiso 1 1 d . . . . .
O1P1 O 0.333333 0.666667 0.6837(16) 0.033(11) Uiso 1 3 d S . P . .
O2P1 O 0.428(2) 0.740(2) 0.5998(12) 0.065(9) Uiso 1 1 d . . . . .
O1P2 O 0.255(2) 0.6895(18) 0.4783(12) 0.053(8) Uiso 1 1 d . . . . .
O2P2 O 0.333333 0.666667 0.399(3) 0.10(3) Uiso 1 3 d S . P . .
O11 O 0.438(2) 0.747(2) 0.7603(14) 0.070(9) Uiso 1 1 d . . . . .
O12 O 0.532(3) 0.722(2) 0.6859(13) 0.072(9) Uiso 1 1 d . . . . .
O13 O 0.467(2) 0.871(2) 0.6833(12) 0.067(9) Uiso 1 1 d . . . . .
O23 O 0.5112(19) 0.6188(18) 0.6031(10) 0.049(7) Uiso 1 1 d . . . . .
O24 O 0.5860(19) 0.7696(18) 0.5397(16) 0.074(8) Uiso 1 1 d . . . . .
O32 O 0.5985(19) 0.8764(19) 0.6280(11) 0.058(8) Uiso 1 1 d . . . . .
O35 O 0.5253(18) 0.9064(17) 0.5442(16) 0.063(7) Uiso 1 1 d . . . . .
O45 O 0.384(2) 0.890(2) 0.4847(12) 0.068(9) Uiso 1 1 d . . . . .
O54 O 0.596(2) 0.868(2) 0.4621(14) 0.074(9) Uiso 1 1 d . . . . .
O4F1 O 0.534(2) 0.715(2) 0.3990(11) 0.058(8) Uiso 1 1 d . . . . .
O5F1 O 0.460(2) 0.870(2) 0.3989(12) 0.062(8) Uiso 1 1 d . . . . .
O11L O 0.243(2) 0.679(2) 0.3170(14) 0.074(10) Uiso 1 1 d . . . . .
O12L O 0.378(2) 0.888(2) 0.3024(12) 0.063(9) Uiso 1 1 d . . . . .
C1 C 0.512(3) 0.886(3) 0.2572(18) 0.059(11) Uiso 1 1 d . . . . .
C11 C 0.216(3) 0.693(3) 0.2665(19) 0.062(12) Uiso 1 1 d . . . . .
C12 C 0.436(3) 0.908(3) 0.2582(16) 0.062(11) Uiso 1 1 d . . . . .
O13L O 0.655(3) 0.915(3) 0.2078(17) 0.048(14) Uiso 0.56(5) 1 d . . P A 1
C13 C 0.567(3) 0.920(3) 0.2054(17) 0.066(11) Uiso 0.56(5) 1 d . . P A 1
N1A N 0.584(2) 0.941(3) 0.3031(13) 0.049(9) Uiso 0.56(5) 1 d . . P A 1
C14 C 0.584(2) 0.941(3) 0.3031(13) 0.049(9) Uiso 0.44(5) 1 d . . P A 2
O14L O 0.695(3) 0.862(3) 0.3322(18) 0.031(15) Uiso 0.44(5) 1 d . . P A 2
N1B N 0.567(3) 0.920(3) 0.2054(17) 0.066(11) Uiso 0.44(5) 1 d . . P A 2
Na1 Na 0.642(7) 0.574(7) 0.543(6) 0.07(2) Uani 0.1667 1 d . U P . .
O1W O 0.354(4) 1.087(4) 0.244(2) 0.080(15) Uiso 0.6 1 d . . P . .
O2W O 0.595(12) 0.440(13) 0.558(7) 0.09(5) Uiso 0.2 1 d . . P . .
O3W O 0.826(7) 0.775(7) 0.540(7) 0.06(2) Uiso 0.25 1 d . . P . .
O4W O 0.993(7) 0.756(7) 0.538(5) 0.06(3) Uiso 0.25 1 d . . P . .
O5W O 0.821(6) 1.060(6) 0.240(4) 0.04(2) Uiso 0.25 1 d . . P . .
O22L O 0.353(5) 1.028(5) 0.340(2) 0.045(16) Uiso 0.4 1 d . . P . .
O21L O 0.385(4) 1.283(4) 0.382(2) 0.048(15) Uiso 0.4 1 d . . P . .
N2 N 0.334(5) 1.121(5) 0.427(3) 0.037(16) Uiso 0.4 1 d . . P . .
C2 C 0.420(6) 1.154(7) 0.400(4) 0.04(2) Uiso 0.4 1 d . . P . .
C21 C 0.424(6) 1.227(6) 0.362(3) 0.03(2) Uiso 0.4 1 d . . P . .
C22 C 0.401(7) 1.064(7) 0.337(4) 0.04(2) Uiso 0.4 1 d . . P . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
W1 O1T 1.70(3) . ?
W1 O11 1.90(3) . ?
W1 O12 1.91(4) . ?
W1 O11 1.95(3) 3_565 ?
W1 O13 1.99(3) 3_565 ?
W1 O1P1 2.33(2) . ?
W2 O2T 1.74(3) . ?
W2 O23 1.89(3) . ?
W2 O24 1.93(4) . ?
W2 O32 1.95(3) . ?
W2 O12 1.95(3) . ?
W2 O2P1 2.40(3) . ?
W3 O3T 1.75(3) . ?
W3 O35 1.83(4) . ?
W3 O13 1.88(3) . ?
W3 O32 1.89(3) . ?
W3 O23 1.93(3) 2_665 ?
W3 O2P1 2.42(3) . ?
W4 O4T 1.64(3) . ?
W4 O54 1.81(3) . ?
W4 O4F1 1.84(3) . ?
W4 O24 1.91(4) . ?
W4 O45 1.94(3) 3_565 ?
W4 O1P2 2.32(3) 3_565 ?
W5 O5T 1.62(4) . ?
W5 O5F1 1.84(3) . ?
W5 O45 1.87(3) . ?
W5 O54 1.95(3) . ?
W5 O35 2.04(4) . ?
W5 O1P2 2.32(3) 3_565 ?
P1 O2P1 1.48(3) 2_665 ?
P1 O2P1 1.48(3) . ?
P1 O2P1 1.48(3) 3_565 ?
P1 O1P1 1.67(4) . ?
P2 O2P2 1.55(8) . ?
P2 O1P2 1.58(3) . ?
P2 O1P2 1.58(3) 3_565 ?
P2 O1P2 1.58(3) 2_665 ?
Fe1 O4F1 1.87(3) 2_665 ?
Fe1 O11L 1.89(3) 3_565 ?
Fe1 O12L 1.91(3) . ?
Fe1 O5F1 1.94(3) . ?
Fe1 O11L 2.07(3) . ?
Fe1 O2P2 2.25(4) . ?
O23 Na1 3.01(11) . ?
O11L C11 1.42(6) . ?
O12L C12 1.41(5) . ?
C1 C12 1.46(6) . ?
C1 C11 1.50(6) 3_565 ?
C1 C13 1.54(6) . ?
C1 N1B 1.54(6) . ?
C1 N1A 1.58(5) . ?
C1 C14 1.58(5) . ?
O13L C13 1.48(6) . ?
Na1 O2W 2.0(2) . ?
O22L C22 0.71(9) . ?
O21L C21 1.45(10) . ?
N2 C2 1.41(11) . ?
C2 C21 1.51(12) . ?
C2 C22 2.11(13) . ?

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
O1T W1 O11 102.9(14) . . ?
O1T W1 O12 104.5(15) . . ?
O11 W1 O12 86.4(15) . . ?
O1T W1 O11 98.3(14) . 3_565 ?
O11 W1 O11 89(2) . 3_565 ?
O12 W1 O11 157.2(15) . 3_565 ?
O1T W1 O13 99.6(13) . 3_565 ?
O11 W1 O13 157.4(14) . 3_565 ?
O12 W1 O13 89.2(14) . 3_565 ?
O11 W1 O13 86.8(14) 3_565 3_565 ?
O1T W1 O1P1 168.0(13) . . ?
O11 W1 O1P1 71.9(11) . . ?
O12 W1 O1P1 86.2(12) . . ?
O11 W1 O1P1 71.1(12) 3_565 . ?
O13 W1 O1P1 85.7(12) 3_565 . ?
O2T W2 O23 99.1(13) . . ?
O2T W2 O24 99.8(13) . . ?
O23 W2 O24 89.6(11) . . ?
O2T W2 O32 101.1(14) . . ?
O23 W2 O32 158.9(12) . . ?
O24 W2 O32 92.8(12) . . ?
O2T W2 O12 96.3(15) . . ?
O23 W2 O12 86.4(13) . . ?
O24 W2 O12 163.8(13) . . ?
O32 W2 O12 85.5(13) . . ?
O2T W2 O2P1 175.7(13) . . ?
O23 W2 O2P1 85.0(12) . . ?
O24 W2 O2P1 81.3(11) . . ?
O32 W2 O2P1 74.7(11) . . ?
O12 W2 O2P1 82.7(13) . . ?
O3T W3 O35 101.3(12) . . ?
O3T W3 O13 95.6(14) . . ?
O35 W3 O13 162.8(13) . . ?
O3T W3 O32 96.1(12) . . ?
O35 W3 O32 89.9(12) . . ?
O13 W3 O32 85.0(14) . . ?
O3T W3 O23 103.5(12) . 2_665 ?
O35 W3 O23 92.6(12) . 2_665 ?
O13 W3 O23 86.6(13) . 2_665 ?
O32 W3 O23 159.3(12) . 2_665 ?
O3T W3 O2P1 171.4(12) . . ?
O35 W3 O2P1 80.1(11) . . ?
O13 W3 O2P1 82.8(13) . . ?
O32 W3 O2P1 75.3(11) . . ?
O23 W3 O2P1 84.8(11) 2_665 . ?
O4T W4 O54 102.0(15) . . ?
O4T W4 O4F1 100.2(14) . . ?
O54 W4 O4F1 95.6(14) . . ?
O4T W4 O24 95.2(13) . . ?
O54 W4 O24 84.8(14) . . ?
O4F1 W4 O24 164.2(12) . . ?
O4T W4 O45 102.1(14) . 3_565 ?
O54 W4 O45 154.4(15) . 3_565 ?
O4F1 W4 O45 88.2(13) . 3_565 ?
O24 W4 O45 84.9(13) . 3_565 ?
O4T W4 O1P2 172.3(12) . 3_565 ?
O54 W4 O1P2 70.6(13) . 3_565 ?
O4F1 W4 O1P2 83.3(12) . 3_565 ?
O24 W4 O1P2 81.9(11) . 3_565 ?
O45 W4 O1P2 84.8(13) 3_565 3_565 ?
O5T W5 O5F1 101.2(18) . . ?
O5T W5 O45 95.8(17) . . ?
O5F1 W5 O45 89.8(15) . . ?
O5T W5 O54 108.8(17) . . ?
O5F1 W5 O54 94.3(15) . . ?
O45 W5 O54 153.7(15) . . ?
O5T W5 O35 95.1(16) . . ?
O5F1 W5 O35 163.5(12) . . ?
O45 W5 O35 86.2(12) . . ?
O54 W5 O35 82.6(13) . . ?
O5T W5 O1P2 175.7(16) . 3_565 ?
O5F1 W5 O1P2 82.5(12) . 3_565 ?
O45 W5 O1P2 86.3(13) . 3_565 ?
O54 W5 O1P2 68.6(12) . 3_565 ?
O35 W5 O1P2 81.3(10) . 3_565 ?
O2P1 P1 O2P1 110.0(14) 2_665 . ?
O2P1 P1 O2P1 110.0(14) 2_665 3_565 ?
O2P1 P1 O2P1 110.0(14) . 3_565 ?
O2P1 P1 O1P1 109.0(14) 2_665 . ?
O2P1 P1 O1P1 109.0(14) . . ?
O2P1 P1 O1P1 109.0(14) 3_565 . ?
O2P2 P2 O1P2 107.8(13) . . ?
O2P2 P2 O1P2 107.8(13) . 3_565 ?
O1P2 P2 O1P2 111.0(12) . 3_565 ?
O2P2 P2 O1P2 107.8(13) . 2_665 ?
O1P2 P2 O1P2 111.0(12) . 2_665 ?
O1P2 P2 O1P2 111.0(12) 3_565 2_665 ?
O4F1 Fe1 O11L 168.3(15) 2_665 3_565 ?
O4F1 Fe1 O12L 96.8(13) 2_665 . ?
O11L Fe1 O12L 93.8(15) 3_565 . ?
O4F1 Fe1 O5F1 83.8(14) 2_665 . ?
O11L Fe1 O5F1 89.7(15) 3_565 . ?
O12L Fe1 O5F1 97.7(14) . . ?
O4F1 Fe1 O11L 95.8(14) 2_665 . ?
O11L Fe1 O11L 88(2) 3_565 . ?
O12L Fe1 O11L 99.3(14) . . ?
O5F1 Fe1 O11L 162.9(14) . . ?
O4F1 Fe1 O2P2 91.5(16) 2_665 . ?
O11L Fe1 O2P2 78.4(16) 3_565 . ?
O12L Fe1 O2P2 170(2) . . ?
O5F1 Fe1 O2P2 88.0(16) . . ?
O11L Fe1 O2P2 74.9(15) . . ?
P1 O1P1 W1 122.8(9) . 2_665 ?
P1 O1P1 W1 122.8(9) . 3_565 ?
W1 O1P1 W1 93.5(12) 2_665 3_565 ?
P1 O1P1 W1 122.8(9) . . ?
W1 O1P1 W1 93.5(12) 2_665 . ?
W1 O1P1 W1 93.5(12) 3_565 . ?
P1 O2P1 W2 128.3(17) . . ?
P1 O2P1 W3 127.7(17) . . ?
W2 O2P1 W3 88.0(11) . . ?
P2 O1P2 W4 127.6(16) . 2_665 ?
P2 O1P2 W5 126.2(15) . 2_665 ?
W4 O1P2 W5 93.3(11) 2_665 2_665 ?
P2 O2P2 Fe1 122.3(17) . . ?
P2 O2P2 Fe1 122.3(17) . 2_665 ?
Fe1 O2P2 Fe1 94(2) . 2_665 ?
P2 O2P2 Fe1 122.3(17) . 3_565 ?
Fe1 O2P2 Fe1 94(2) . 3_565 ?
Fe1 O2P2 Fe1 94(2) 2_665 3_565 ?
W1 O11 W1 123.5(18) . 2_665 ?
W1 O12 W2 147(2) . . ?
W3 O13 W1 147.7(19) . 2_665 ?
W2 O23 W3 151.5(15) . 3_565 ?
W2 O23 Na1 106(2) . . ?
W3 O23 Na1 102(2) 3_565 . ?
W4 O24 W2 162.8(15) . . ?
W3 O32 W2 121.4(14) . . ?
W3 O35 W5 157.8(15) . . ?
W5 O45 W4 145.0(19) . 2_665 ?
W4 O54 W5 127.5(18) . . ?
W4 O4F1 Fe1 150.4(18) . 3_565 ?
W5 O5F1 Fe1 149(2) . . ?
C11 O11L Fe1 129(3) . 2_665 ?
C11 O11L Fe1 117(3) . . ?
Fe1 O11L Fe1 112.4(18) 2_665 . ?
C12 O12L Fe1 123(3) . . ?
C12 C1 C11 112(4) . 3_565 ?
C12 C1 C13 110(4) . . ?
C11 C1 C13 112(4) 3_565 . ?
C12 C1 N1B 110(4) . . ?
C11 C1 N1B 112(4) 3_565 . ?
C12 C1 N1A 109(3) . . ?
C11 C1 N1A 106(3) 3_565 . ?
C13 C1 N1A 107(3) . . ?
C12 C1 C14 109(3) . . ?
C11 C1 C14 106(3) 3_565 . ?
N1B C1 C14 107(3) . . ?
O11L C11 C1 110(4) . 2_665 ?
O12L C12 C1 121(4) . . ?
O13L C13 C1 111(4) . . ?
O2W Na1 O23 104(7) . . ?
N2 C2 C21 106(7) . . ?
N2 C2 C22 110(7) . . ?
C21 C2 C22 89(6) . . ?
O21L C21 C2 114(7) . . ?
O22L C22 C2 103(10) . . ?

_refine_diff_density_max         2.540
_refine_diff_density_min         -3.109
_refine_diff_density_rms         0.340




####################################################################### 
# 
# 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_fe6_a_sq
_database_code_depnum_ccdc_archive 'CCDC 2205567'
loop_
_audit_author_name
_audit_author_address
'Natalya Izarova'
;Institute of Inorganic Chemistry, RWTH Aachen University
Germany
;
_audit_update_record             
;
2022-09-06 deposited with the CCDC.	2022-12-12 downloaded from the CCDC.
;

# start Validation Reply Form
_vrf_PLAT201_fe6_a_sq            
;
PROBLEM: Isotropic non-H Atoms in Main Residue(s) .......         11 Report
RESPONSE: Only heavy atoms (W, Fe, P, Na) as well as O atoms of the polyoxotungstate
skeleton were refined anisotropically which is the common practice in 
polyoxotungstates crystallography. 
;
_vrf_PLAT430_fe6_a_sq            
;
PROBLEM: Short Inter D...A Contact  O12L     ..O8W      .       2.77 Ang.  
RESPONSE: The relatively short O...O contacts arise due to hydrogen 
bonding.
;
_vrf_PLAT910_fe6_a_sq            
;
PROBLEM: Missing # of FCF Reflection(s) Below Theta(Min).         42 Note  
RESPONSE: Missing reflections are in diffractometer restricted areas
like beamstop. Nevertheless, the total amount of collected reflections 
well exceeds that required for statistically relevant refinement to assure 
true results.
;
# end Validation Reply Form

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C72 H248 Cl Fe6 N18 Na O188 P4 W30'
_chemical_formula_weight         10407.79

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Na Na 0.0362 0.0249 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
W W -0.8490 6.8722 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/c'
_space_group_name_Hall           '-P 2ybc'

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

_cell_length_a                   15.158(3)
_cell_length_b                   23.486(5)
_cell_length_c                   30.191(6)
_cell_angle_alpha                90
_cell_angle_beta                 94.36(3)
_cell_angle_gamma                90
_cell_volume                     10717(4)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    20544
_cell_measurement_theta_min      1.62
_cell_measurement_theta_max      24.95


_exptl_crystal_description       rod
_exptl_crystal_colour            orange
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    3.225
_exptl_crystal_F_000             9548
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.330
_exptl_crystal_size_mid          0.105
_exptl_crystal_size_min          0.090
_exptl_absorpt_coefficient_mu    16.586
_shelx_estimated_absorpt_T_min   0.073
_shelx_estimated_absorpt_T_max   0.317
_exptl_absorpt_correction_type   integration
_exptl_absorpt_correction_T_min  0.0242
_exptl_absorpt_correction_T_max  0.2476
_exptl_absorpt_process_details   
;
STOE X-Red32, absorption correction by Gaussian integration. 
Afterwards scaling of reflection intensities was performed 
within STOE LANA.
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'Genix Mo'
_diffrn_measurement_device_type  'STOE STADIVARI'
_diffrn_measurement_method       'rotation method, ω scans'
_diffrn_detector_area_resol_mean 5.81
_diffrn_reflns_number            99339
_diffrn_reflns_av_unetI/netI     0.0770
_diffrn_reflns_av_R_equivalents  0.0990
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_theta_min         3.185
_diffrn_reflns_theta_max         25.027
_diffrn_reflns_theta_full        25.028
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measured_fraction_theta_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_point_group_measured_fraction_full 0.995
_reflns_number_total             18824
_reflns_number_gt                13031
_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.
 
loop_
  _platon_squeeze_void_nr
  _platon_squeeze_void_average_x
  _platon_squeeze_void_average_y
  _platon_squeeze_void_average_z
  _platon_squeeze_void_volume
  _platon_squeeze_void_count_electrons
  _platon_squeeze_void_content
   1 -0.001  0.497  0.006      4475      1718 ' '
_platon_squeeze_void_probe_radius                  1.20
_platon_squeeze_details                           
The unit cell contains 28 tris(hydroxymethyl)ammonimmethane cations, 
26.5 of which had to be treated as a diffuse contribution to the overall 
scattering without specific atom positions by SQUEEZE/PLATON.  
;

_computing_data_collection       
;
X-Area Pilatus3_SV 1.31.170.0 (STOE, 2020)
;
_computing_cell_refinement       
;
X-Area Recipe 1.36.0.0 (STOE, 2020)
;
_computing_data_reduction        
;
X-Area Integrate 1.78.3.0 (STOE, 2020)
X-Area X-Red 1.65.2.0 (STOE, 2020) 
;
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    'Diamond 4'
_computing_publication_material  
;
STOE & Cie GmbH, X-Area, software package for collecting single-crystal or
multi-domain crystal data on STOE area-detector diffractometers, for image 
processing, for the correction and scaling of reflection intensities and 
for outlier rejection, version 1.90, Darmstadt 2020
;
_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)+(0.0850P)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         18824
_refine_ls_number_parameters     862
_refine_ls_number_restraints     22
_refine_ls_R_factor_all          0.0797
_refine_ls_R_factor_gt           0.0539
_refine_ls_wR_factor_ref         0.1447
_refine_ls_wR_factor_gt          0.1353
_refine_ls_goodness_of_fit_ref   1.007
_refine_ls_restrained_S_all      1.007
_refine_ls_shift/su_max          0.003
_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 1.02116(4) 0.66191(3) 1.07009(2) 0.02998(17) Uani 1 1 d . . . . .
W2 W 1.11789(4) 0.64036(3) 1.17437(2) 0.03244(18) Uani 1 1 d . . . . .
W3 W 1.19708(5) 0.57164(3) 1.08666(2) 0.03583(19) Uani 1 1 d . . . . .
W4 W 1.06037(4) 0.81784(3) 1.08354(2) 0.02257(15) Uani 1 1 d . . . . .
W5 W 1.15328(4) 0.79661(3) 1.18601(2) 0.02551(16) Uani 1 1 d . . . . .
W6 W 1.34363(4) 0.69919(3) 1.20382(2) 0.02982(17) Uani 1 1 d . . . . .
W7 W 1.42123(4) 0.63160(3) 1.11743(2) 0.03288(18) Uani 1 1 d . . . . .
W8 W 1.31563(4) 0.65282(3) 1.00417(2) 0.02960(17) Uani 1 1 d . . . . .
W9 W 1.14363(4) 0.74165(3) 0.98792(2) 0.02459(16) Uani 1 1 d . . . . .
W10 W 1.21927(4) 0.94009(3) 1.06467(2) 0.01989(15) Uani 1 1 d . . . . .
W11 W 1.68759(4) 1.08273(3) 0.83171(2) 0.02202(15) Uani 1 1 d . . . . .
W12 W 1.49940(4) 0.82225(3) 1.18642(2) 0.02539(16) Uani 1 1 d . . . . .
W13 W 1.57721(4) 0.75565(3) 1.09850(2) 0.02729(17) Uani 1 1 d . . . . .
W14 W 1.47410(4) 0.77519(3) 0.98778(2) 0.02507(16) Uani 1 1 d . . . . .
W15 W 1.30254(4) 0.86536(3) 0.97247(2) 0.02041(15) Uani 1 1 d . . . . .
P1 P 1.2318(3) 0.71807(18) 1.09801(12) 0.0233(9) Uani 1 1 d . . . . .
P2 P 1.5959(2) 1.14902(16) 0.92079(12) 0.0176(8) Uani 1 1 d . . . . .
Fe1 Fe 1.43537(12) 0.97847(9) 1.02777(6) 0.0200(5) Uani 1 1 d . . . . .
Fe2 Fe 1.47247(13) 1.04629(10) 0.87296(7) 0.0229(5) Uani 1 1 d . . . . .
Fe3 Fe 1.40174(13) 1.10757(10) 0.96046(7) 0.0240(5) Uani 1 1 d . . . . .
O0F1 O 1.3153(6) 0.9777(4) 1.0522(3) 0.020(2) Uani 1 1 d . . . . .
O1F O 1.4438(6) 1.0419(4) 0.9907(3) 0.020(2) Uani 1 1 d . U . . .
O1T O 0.9127(7) 0.6447(5) 1.0502(4) 0.049(3) Uani 1 1 d . . . . .
O2T O 1.0711(7) 0.6112(5) 1.2195(4) 0.044(3) Uani 1 1 d . U . . .
O3T O 1.1998(8) 0.4990(5) 1.0781(4) 0.050(3) Uani 1 1 d . . . . .
O4T O 0.9578(6) 0.8478(4) 1.0687(3) 0.030(3) Uani 1 1 d . U . . .
O5T O 1.1140(7) 0.8147(5) 1.2353(3) 0.034(3) Uani 1 1 d . . . . .
O6T O 1.3656(6) 0.6856(5) 1.2594(3) 0.035(3) Uani 1 1 d . . . . .
O7T O 1.4925(8) 0.5745(5) 1.1192(4) 0.053(3) Uani 1 1 d . . . . .
O8T O 1.3502(7) 0.6017(5) 0.9687(4) 0.037(3) Uani 1 1 d . . . . .
O9T O 1.0703(7) 0.7467(5) 0.9421(3) 0.031(3) Uani 1 1 d . . . . .
O10T O 1.1382(6) 0.9870(4) 1.0468(3) 0.026(2) Uani 1 1 d . . . . .
O11T O 1.7075(7) 1.0461(5) 0.7842(3) 0.035(3) Uani 1 1 d . . . . .
O12T O 1.5427(7) 0.8250(5) 1.2408(3) 0.033(3) Uani 1 1 d . . . . .
O13T O 1.6705(7) 0.7120(5) 1.0986(4) 0.044(3) Uani 1 1 d . . . . .
O14T O 1.5313(7) 0.7396(5) 0.9486(4) 0.039(3) Uani 1 1 d . . . . .
O15T O 1.2508(6) 0.8878(4) 0.9232(3) 0.026(2) Uani 1 1 d . . . . .
O1P1 O 1.1671(6) 0.6675(4) 1.1051(3) 0.027(2) Uani 1 1 d . . . . .
O2P1 O 1.1882(6) 0.7718(4) 1.1137(3) 0.018(2) Uani 1 1 d . . . . .
O3P1 O 1.3200(6) 0.7061(4) 1.1258(3) 0.025(2) Uani 1 1 d . . . . .
O4P1 O 1.2458(6) 0.7197(4) 1.0482(3) 0.028(3) Uani 1 1 d . . . . .
O1P2 O 1.6795(5) 1.1254(4) 0.9021(3) 0.017(2) Uani 1 1 d . . . . .
O2P2 O 1.4514(6) 0.8073(4) 1.1111(3) 0.023(2) Uani 1 1 d . . . . .
O3P2 O 1.3789(6) 0.8225(4) 1.0336(3) 0.024(2) Uani 1 1 d . . . . .
O4P2 O 1.5308(6) 1.0988(4) 0.9283(3) 0.021(2) Uani 1 1 d . . . . .
O1F2 O 1.5932(6) 1.0443(4) 0.8476(3) 0.027(2) Uani 1 1 d . . . . .
O2F2 O 1.5435(6) 0.8866(5) 1.1658(3) 0.029(3) Uani 1 1 d . . . . .
O3F3 O 1.6180(6) 0.8225(4) 1.0801(3) 0.028(3) Uani 1 1 d . . . . .
O4F3 O 1.5462(6) 0.8352(5) 0.9976(3) 0.030(3) Uani 1 1 d . . . . .
O5F1 O 1.3778(6) 0.9228(4) 0.9846(3) 0.021(2) Uani 1 1 d . . . . .
O12 O 1.0141(7) 0.6433(5) 1.1332(3) 0.037(3) Uani 1 1 d . . . . .
O13 O 1.0758(7) 0.5865(5) 1.0648(3) 0.037(3) Uani 1 1 d . . . . .
O14 O 1.0125(6) 0.7380(4) 1.0862(3) 0.025(2) Uani 1 1 d . . . . .
O19 O 1.0759(6) 0.6839(4) 1.0190(3) 0.029(3) Uani 1 1 d . . . . .
O23 O 1.1499(7) 0.5717(5) 1.1460(4) 0.043(3) Uani 1 1 d . . . . .
O25 O 1.1046(6) 0.7184(5) 1.1832(3) 0.031(3) Uani 1 1 d . . . . .
O26 O 1.2361(7) 0.6502(5) 1.1944(4) 0.041(3) Uani 1 1 d . . . . .
O37 O 1.3088(7) 0.5878(5) 1.1140(4) 0.040(3) Uani 1 1 d . . . . .
O38 O 1.2342(7) 0.6011(5) 1.0342(3) 0.033(3) Uani 1 1 d . . . . .
O45 O 1.0535(6) 0.8176(4) 1.1469(3) 0.022(2) Uani 1 1 d . . . . .
O49 O 1.0960(6) 0.7943(4) 1.0277(3) 0.022(2) Uani 1 1 d . . . . .
O56 O 1.2594(6) 0.7575(4) 1.2052(3) 0.028(3) Uani 1 1 d . . . . .
O67 O 1.4071(7) 0.6378(5) 1.1804(3) 0.037(3) Uani 1 1 d . . . . .
O78 O 1.3922(6) 0.6390(5) 1.0564(3) 0.033(3) Uani 1 1 d . . . . .
O89 O 1.2104(6) 0.6777(4) 0.9686(3) 0.027(3) Uani 1 1 d . . . . .
O101 O 1.2282(6) 0.9567(4) 1.1270(3) 0.017(2) Uani 1 1 d . . . . .
O105 O 1.2229(5) 0.8920(4) 1.0146(3) 0.019(2) Uani 1 1 d . . . . .
O112 O 1.3871(6) 0.8558(4) 1.1893(3) 0.023(2) Uani 1 1 d . . . . .
O123 O 1.5863(6) 0.7734(5) 1.1611(3) 0.029(3) Uani 1 1 d . . . . .
O134 O 1.5175(6) 0.7400(4) 1.0421(3) 0.026(2) Uani 1 1 d . . . . .
O145 O 1.3885(7) 0.8143(5) 0.9496(3) 0.029(3) Uani 1 1 d . . . . .
O410 O 1.1319(6) 0.8796(4) 1.0828(3) 0.026(2) Uani 1 1 d . . . . .
O511 O 1.2141(6) 0.8616(5) 1.1736(3) 0.027(3) Uani 1 1 d . . . . .
O612 O 1.4332(6) 0.7500(5) 1.1947(3) 0.032(3) Uani 1 1 d . . . . .
O713 O 1.4993(7) 0.6884(5) 1.1185(3) 0.031(3) Uani 1 1 d . . . . .
O814 O 1.3789(6) 0.7145(5) 0.9889(3) 0.031(3) Uani 1 1 d . . . . .
O915 O 1.2265(6) 0.7934(4) 0.9735(3) 0.027(3) Uani 1 1 d . . . . .
O11L O 1.5124(6) 0.9855(4) 0.9157(3) 0.021(2) Uani 1 1 d . . . . .
O12L O 1.4221(6) 0.9915(4) 0.8317(3) 0.025(2) Uani 1 1 d . . . . .
O13L O 1.5114(12) 0.8225(8) 0.8144(6) 0.044(5) Uani 0.604(15) 1 d . . P A 1
O14L O 1.5929(19) 0.8190(12) 0.8709(9) 0.044(5) Uani 0.396(15) 1 d . . P A 2
O21L O 1.3644(6) 1.0638(4) 0.9040(3) 0.025(2) Uani 1 1 d . . . . .
O22L O 1.2843(6) 1.1136(5) 0.9792(3) 0.030(3) Uani 1 1 d . . . . .
O23L O 1.0559(7) 1.0271(5) 0.9312(4) 0.045(3) Uani 1 1 d . . . . .
N1 N 1.5774(8) 0.9298(6) 0.8310(4) 0.038(3) Uiso 1 1 d . . . . .
H1A H 1.623672 0.948890 0.842414 0.045 Uiso 1 1 calc R U . . .
H1B H 1.572124 0.922006 0.802428 0.045 Uiso 1 1 calc R U . . .
N2 N 1.1914(8) 1.1041(6) 0.8974(4) 0.034(3) Uiso 1 1 d . . . . .
H2A H 1.189376 1.136757 0.911550 0.041 Uiso 1 1 calc R U . . .
H2B H 1.181683 1.103053 0.868286 0.041 Uiso 1 1 calc R U . . .
C1 C 1.5056(10) 0.9103(7) 0.8610(5) 0.031(4) Uiso 1 1 d . . . . .
C2 C 1.2112(8) 1.0511(6) 0.9224(4) 0.016(3) Uiso 1 1 d . . . . .
C11 C 1.5306(10) 0.9288(7) 0.9069(5) 0.030(4) Uiso 1 1 d . . . . .
H11A H 1.499091 0.904617 0.927446 0.036 Uiso 1 1 calc R U . . .
H11B H 1.594777 0.922264 0.913359 0.036 Uiso 1 1 calc R U . . .
C12 C 1.4178(12) 0.9348(8) 0.8391(6) 0.050(5) Uiso 1 1 d . . . . .
H12A H 1.403173 0.915022 0.810546 0.060 Uiso 1 1 calc R U . . .
H12B H 1.369604 0.927021 0.858652 0.060 Uiso 1 1 calc R U . . .
C13 C 1.5073(11) 0.8417(8) 0.8607(5) 0.039(4) Uiso 1 1 d . . . . .
C21 C 1.2940(9) 1.0224(7) 0.9058(5) 0.025(4) Uiso 1 1 d . . . . .
H21A H 1.313616 0.990994 0.926164 0.030 Uiso 1 1 calc R U . . .
H21B H 1.279688 1.006068 0.875921 0.030 Uiso 1 1 calc R U . . .
C22 C 1.2239(10) 1.0695(7) 0.9711(5) 0.035(4) Uiso 1 1 d . . . . .
H22A H 1.166003 1.081625 0.981004 0.042 Uiso 1 1 calc R U . . .
H22B H 1.244041 1.036246 0.989320 0.042 Uiso 1 1 calc R U . . .
C23 C 1.1375(11) 1.0074(8) 0.9145(6) 0.042(4) Uiso 1 1 d . . . . .
H23A H 1.127633 0.999841 0.882223 0.050 Uiso 1 1 calc R U . . .
H23B H 1.155648 0.971284 0.929374 0.050 Uiso 1 1 calc R U . . .
Na1 Na 1.000000 1.000000 1.000000 0.055(3) Uani 1 2 d S . P . .
O1W O 0.9704(9) 1.0959(7) 1.0247(5) 0.039(4) Uiso 0.75 1 d . . P . .
O2W O 1.8409(14) 0.7363(10) 0.6196(7) 0.038(6) Uiso 0.5 1 d . . P . .
O3W O 1.5286(18) 0.5786(13) 0.2372(9) 0.038(8) Uiso 0.375 1 d . . P . .
O4W O 1.2583(16) 0.3539(12) 0.3101(8) 0.056(7) Uiso 0.5 1 d . . P . .
O5W O 0.9489(15) 0.4790(11) 0.3489(7) 0.048(6) Uiso 0.5 1 d . . P . .
O6W O 1.7547(15) 0.5841(11) 0.3675(8) 0.050(7) Uiso 0.5 1 d . . P . .
O7W O 1.650(2) 0.7478(14) 0.3002(10) 0.050(9) Uiso 0.375 1 d . . P . .
O8W O 1.347(2) 0.4428(14) 0.2626(10) 0.008(7) Uiso 0.25 1 d . . P . .
O31 O 1.321(2) 0.7345(15) 0.8804(11) 0.053(9) Uiso 0.375 1 d . . P . .
O32 O 1.542(2) 0.6573(14) 0.8842(10) 0.045(8) Uiso 0.375 1 d . . P . .
O33 O 1.262(3) 0.6409(18) 0.8012(12) 0.073(11) Uiso 0.375 1 d . . P . .
N3 N 1.393(2) 0.5982(15) 0.8523(11) 0.040(9) Uiso 0.375 1 d D . P . .
C3 C 1.3894(18) 0.6563(15) 0.8449(9) 0.024(9) Uiso 0.375 1 d D . P . .
C31 C 1.344(3) 0.6789(18) 0.8807(11) 0.032(10) Uiso 0.375 1 d D . P . .
H31A H 1.288685 0.656442 0.882455 0.039 Uiso 0.375 1 calc R U P . .
H31B H 1.380821 0.671718 0.908544 0.039 Uiso 0.375 1 calc R U P . .
C32 C 1.486(2) 0.6742(19) 0.8481(13) 0.033(11) Uiso 0.375 1 d D . P . .
H32A H 1.511603 0.660402 0.820980 0.040 Uiso 0.375 1 calc R U P . .
H32B H 1.486987 0.716307 0.847088 0.040 Uiso 0.375 1 calc R U P . .
C33 C 1.339(2) 0.6628(18) 0.7990(10) 0.026(9) Uiso 0.375 1 d D . P . .
H33A H 1.333276 0.703595 0.790873 0.031 Uiso 0.375 1 calc R U P . .
H33B H 1.370675 0.643078 0.776051 0.031 Uiso 0.375 1 calc R U P . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
W1 O1T 1.754(11) . ?
W1 O14 1.859(10) . ?
W1 O19 1.878(10) . ?
W1 O12 1.966(9) . ?
W1 O13 1.966(11) . ?
W1 O1P1 2.382(9) . ?
W2 O2T 1.724(11) . ?
W2 O26 1.862(10) . ?
W2 O25 1.865(11) . ?
W2 O23 1.906(12) . ?
W2 O12 1.931(10) . ?
W2 O1P1 2.360(10) . ?
W3 O3T 1.727(13) . ?
W3 O38 1.854(10) . ?
W3 O37 1.866(10) . ?
W3 O13 1.937(11) . ?
W3 O23 1.977(12) . ?
W3 O1P1 2.371(10) . ?
W4 O4T 1.735(10) . ?
W4 O410 1.812(10) . ?
W4 O49 1.893(9) . ?
W4 O45 1.924(8) . ?
W4 O14 2.015(10) . ?
W4 O2P1 2.342(8) . ?
W5 O5T 1.700(10) . ?
W5 O511 1.835(11) . ?
W5 O56 1.903(9) . ?
W5 O45 1.912(9) . ?
W5 O25 1.979(11) . ?
W5 O2P1 2.359(9) . ?
W6 O6T 1.715(10) . ?
W6 O612 1.844(10) . ?
W6 O56 1.876(10) . ?
W6 O67 1.899(12) . ?
W6 O26 1.998(10) . ?
W6 O3P1 2.361(9) . ?
W7 O7T 1.720(12) . ?
W7 O713 1.782(11) . ?
W7 O78 1.871(10) . ?
W7 O67 1.933(10) . ?
W7 O37 1.986(11) . ?
W7 O3P1 2.355(10) . ?
W8 O8T 1.718(11) . ?
W8 O814 1.817(11) . ?
W8 O78 1.913(10) . ?
W8 O89 1.944(9) . ?
W8 O38 1.998(11) . ?
W8 O4P1 2.359(10) . ?
W9 O9T 1.711(9) . ?
W9 O915 1.824(10) . ?
W9 O49 1.903(9) . ?
W9 O89 1.925(10) . ?
W9 O19 1.980(10) . ?
W9 O4P1 2.354(10) . ?
W10 O10T 1.707(10) . ?
W10 O0F1 1.769(9) . ?
W10 O105 1.892(9) . ?
W10 O101 1.916(9) . ?
W10 O410 2.045(10) . ?
W10 O1P2 2.343(9) 3_877 ?
W11 O11T 1.719(10) . ?
W11 O1F2 1.788(9) . ?
W11 O112 1.913(9) 3_877 ?
W11 O101 1.950(8) 3_877 ?
W11 O511 1.999(10) 3_877 ?
W11 O1P2 2.362(9) . ?
W12 O12T 1.723(9) . ?
W12 O2F2 1.784(11) . ?
W12 O112 1.885(9) . ?
W12 O123 1.946(10) . ?
W12 O612 1.997(11) . ?
W12 O2P2 2.362(9) . ?
W13 O13T 1.746(11) . ?
W13 O3F3 1.792(11) . ?
W13 O134 1.902(9) . ?
W13 O123 1.930(9) . ?
W13 O713 2.088(11) . ?
W13 O2P2 2.316(9) . ?
W14 O14T 1.733(10) . ?
W14 O4F3 1.794(10) . ?
W14 O134 1.908(9) . ?
W14 O145 1.905(10) . ?
W14 O814 2.030(10) . ?
W14 O3P2 2.352(9) . ?
W15 O15T 1.711(9) . ?
W15 O5F1 1.787(9) . ?
W15 O105 1.923(9) . ?
W15 O145 1.936(10) . ?
W15 O915 2.048(10) . ?
W15 O3P2 2.331(10) . ?
P1 O2P1 1.517(10) . ?
P1 O4P1 1.536(10) . ?
P1 O3P1 1.548(10) . ?
P1 O1P1 1.566(10) . ?
P2 O1P2 1.529(9) . ?
P2 O2P2 1.544(10) 3_877 ?
P2 O3P2 1.552(10) 3_877 ?
P2 O4P2 1.566(10) . ?
Fe1 O1F 1.875(9) . ?
Fe1 O11L 2.012(9) 3_877 ?
Fe1 O5F1 1.999(10) . ?
Fe1 O0F1 2.014(9) . ?
Fe1 O1F 2.012(9) 3_877 ?
Fe1 O4P2 2.283(10) 3_877 ?
Fe1 Fe1 2.859(4) 3_877 ?
Fe2 O12L 1.909(9) . ?
Fe2 O2F2 1.967(10) 3_877 ?
Fe2 O11L 1.989(9) . ?
Fe2 O21L 1.992(10) . ?
Fe2 O1F2 2.037(10) . ?
Fe2 O4P2 2.207(9) . ?
Fe3 O1F 1.878(9) . ?
Fe3 O22L 1.914(10) . ?
Fe3 O4F3 1.971(10) 3_877 ?
Fe3 O21L 2.032(9) . ?
Fe3 O3F3 2.055(10) 3_877 ?
Fe3 O4P2 2.257(9) . ?
O10T Na1 2.455(9) . ?
O11L C11 1.389(17) . ?
O12L C12 1.35(2) . ?
O13L C13 1.47(2) . ?
O14L C13 1.42(3) . ?
O21L C21 1.448(17) . ?
O22L C22 1.392(18) . ?
O23L C23 1.446(19) . ?
O23L Na1 2.390(11) . ?
N1 C1 1.54(2) . ?
N2 C2 1.476(18) . ?
C1 C11 1.47(2) . ?
C1 C12 1.55(2) . ?
C1 C13 1.61(2) . ?
C2 C22 1.531(19) . ?
C2 C23 1.52(2) . ?
C2 C21 1.542(19) . ?
Na1 O1W 2.426(15) 3_777 ?
Na1 O1W 2.426(15) . ?
O31 C31 1.35(5) . ?
O32 C32 1.39(4) . ?
O33 C33 1.28(5) . ?
N3 C3 1.38(4) . ?
C3 C31 1.432(19) . ?
C3 C32 1.514(19) . ?
C3 C33 1.541(19) . ?

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
O1T W1 O14 103.1(5) . . ?
O1T W1 O19 104.1(5) . . ?
O14 W1 O19 89.7(4) . . ?
O1T W1 O12 99.3(5) . . ?
O14 W1 O12 87.1(4) . . ?
O19 W1 O12 156.5(4) . . ?
O1T W1 O13 98.9(5) . . ?
O14 W1 O13 157.7(4) . . ?
O19 W1 O13 88.1(5) . . ?
O12 W1 O13 86.1(5) . . ?
O1T W1 O1P1 168.4(5) . . ?
O14 W1 O1P1 85.0(4) . . ?
O19 W1 O1P1 84.0(4) . . ?
O12 W1 O1P1 72.5(4) . . ?
O13 W1 O1P1 72.7(4) . . ?
O2T W2 O26 103.6(5) . . ?
O2T W2 O25 102.8(5) . . ?
O26 W2 O25 86.8(5) . . ?
O2T W2 O23 98.9(5) . . ?
O26 W2 O23 88.8(5) . . ?
O25 W2 O23 158.3(5) . . ?
O2T W2 O12 99.1(5) . . ?
O26 W2 O12 157.3(5) . . ?
O25 W2 O12 88.0(5) . . ?
O23 W2 O12 87.9(5) . . ?
O2T W2 O1P1 169.6(4) . . ?
O26 W2 O1P1 83.9(4) . . ?
O25 W2 O1P1 84.6(4) . . ?
O23 W2 O1P1 73.8(4) . . ?
O12 W2 O1P1 73.6(4) . . ?
O3T W3 O38 103.2(5) . . ?
O3T W3 O37 103.7(5) . . ?
O38 W3 O37 88.7(5) . . ?
O3T W3 O13 99.2(5) . . ?
O38 W3 O13 89.1(5) . . ?
O37 W3 O13 156.9(5) . . ?
O3T W3 O23 98.7(5) . . ?
O38 W3 O23 158.0(5) . . ?
O37 W3 O23 88.7(5) . . ?
O13 W3 O23 84.8(5) . . ?
O3T W3 O1P1 168.7(5) . . ?
O38 W3 O1P1 85.6(4) . . ?
O37 W3 O1P1 83.5(4) . . ?
O13 W3 O1P1 73.4(4) . . ?
O23 W3 O1P1 72.4(4) . . ?
O4T W4 O410 101.3(5) . . ?
O4T W4 O49 101.5(4) . . ?
O410 W4 O49 90.7(4) . . ?
O4T W4 O45 98.2(4) . . ?
O410 W4 O45 95.3(4) . . ?
O49 W4 O45 157.9(4) . . ?
O4T W4 O14 94.0(4) . . ?
O410 W4 O14 164.4(4) . . ?
O49 W4 O14 83.8(4) . . ?
O45 W4 O14 84.9(4) . . ?
O4T W4 O2P1 170.8(4) . . ?
O410 W4 O2P1 84.0(4) . . ?
O49 W4 O2P1 85.9(4) . . ?
O45 W4 O2P1 73.6(4) . . ?
O14 W4 O2P1 81.1(3) . . ?
O5T W5 O511 100.7(5) . . ?
O5T W5 O56 101.4(5) . . ?
O511 W5 O56 92.1(4) . . ?
O5T W5 O45 99.4(4) . . ?
O511 W5 O45 92.6(4) . . ?
O56 W5 O45 157.4(4) . . ?
O5T W5 O25 96.6(5) . . ?
O511 W5 O25 162.6(4) . . ?
O56 W5 O25 82.5(4) . . ?
O45 W5 O25 86.5(4) . . ?
O5T W5 O2P1 172.4(4) . . ?
O511 W5 O2P1 82.2(4) . . ?
O56 W5 O2P1 85.3(4) . . ?
O45 W5 O2P1 73.4(3) . . ?
O25 W5 O2P1 80.8(4) . . ?
O6T W6 O612 100.2(5) . . ?
O6T W6 O56 101.3(5) . . ?
O612 W6 O56 92.3(5) . . ?
O6T W6 O67 99.1(5) . . ?
O612 W6 O67 92.0(5) . . ?
O56 W6 O67 158.1(4) . . ?
O6T W6 O26 97.3(5) . . ?
O612 W6 O26 162.5(4) . . ?
O56 W6 O26 82.8(5) . . ?
O67 W6 O26 86.6(5) . . ?
O6T W6 O3P1 172.8(5) . . ?
O612 W6 O3P1 82.1(4) . . ?
O56 W6 O3P1 85.4(4) . . ?
O67 W6 O3P1 73.9(4) . . ?
O26 W6 O3P1 80.7(4) . . ?
O7T W7 O713 99.7(5) . . ?
O7T W7 O78 101.7(5) . . ?
O713 W7 O78 93.1(4) . . ?
O7T W7 O67 98.3(5) . . ?
O713 W7 O67 92.8(5) . . ?
O78 W7 O67 157.8(4) . . ?
O7T W7 O37 97.6(5) . . ?
O713 W7 O37 162.7(5) . . ?
O78 W7 O37 82.0(4) . . ?
O67 W7 O37 86.1(5) . . ?
O7T W7 O3P1 171.5(5) . . ?
O713 W7 O3P1 83.1(4) . . ?
O78 W7 O3P1 86.0(4) . . ?
O67 W7 O3P1 73.5(4) . . ?
O37 W7 O3P1 80.0(4) . . ?
O8T W8 O814 101.9(5) . . ?
O8T W8 O78 101.5(5) . . ?
O814 W8 O78 92.6(5) . . ?
O8T W8 O89 98.2(5) . . ?
O814 W8 O89 92.7(4) . . ?
O78 W8 O89 158.0(4) . . ?
O8T W8 O38 94.9(5) . . ?
O814 W8 O38 163.1(4) . . ?
O78 W8 O38 83.1(4) . . ?
O89 W8 O38 85.7(4) . . ?
O8T W8 O4P1 171.1(4) . . ?
O814 W8 O4P1 83.1(4) . . ?
O78 W8 O4P1 85.4(4) . . ?
O89 W8 O4P1 74.1(4) . . ?
O38 W8 O4P1 80.2(4) . . ?
O9T W9 O915 100.2(4) . . ?
O9T W9 O49 102.1(5) . . ?
O915 W9 O49 91.1(4) . . ?
O9T W9 O89 97.7(5) . . ?
O915 W9 O89 93.5(4) . . ?
O49 W9 O89 158.5(4) . . ?
O9T W9 O19 95.9(4) . . ?
O915 W9 O19 163.9(4) . . ?
O49 W9 O19 84.9(4) . . ?
O89 W9 O19 85.0(4) . . ?
O9T W9 O4P1 171.2(4) . . ?
O915 W9 O4P1 84.6(4) . . ?
O49 W9 O4P1 85.1(4) . . ?
O89 W9 O4P1 74.5(4) . . ?
O19 W9 O4P1 79.5(4) . . ?
O10T W10 O0F1 101.2(4) . . ?
O10T W10 O105 101.3(4) . . ?
O0F1 W10 O105 93.0(4) . . ?
O10T W10 O101 100.1(4) . . ?
O0F1 W10 O101 96.3(4) . . ?
O105 W10 O101 154.5(4) . . ?
O10T W10 O410 93.9(4) . . ?
O0F1 W10 O410 164.8(4) . . ?
O105 W10 O410 81.9(4) . . ?
O101 W10 O410 83.0(4) . . ?
O10T W10 O1P2 172.4(4) . 3_877 ?
O0F1 W10 O1P2 84.1(4) . 3_877 ?
O105 W10 O1P2 83.8(3) . 3_877 ?
O101 W10 O1P2 73.7(3) . 3_877 ?
O410 W10 O1P2 81.2(4) . 3_877 ?
O11T W11 O1F2 99.6(5) . . ?
O11T W11 O112 103.7(5) . 3_877 ?
O1F2 W11 O112 90.3(4) . 3_877 ?
O11T W11 O101 98.5(5) . 3_877 ?
O1F2 W11 O101 95.0(4) . 3_877 ?
O112 W11 O101 155.9(4) 3_877 3_877 ?
O11T W11 O511 94.6(4) . 3_877 ?
O1F2 W11 O511 165.7(4) . 3_877 ?
O112 W11 O511 84.6(4) 3_877 3_877 ?
O101 W11 O511 84.7(4) 3_877 3_877 ?
O11T W11 O1P2 171.1(4) . . ?
O1F2 W11 O1P2 82.9(4) . . ?
O112 W11 O1P2 84.8(3) 3_877 . ?
O101 W11 O1P2 72.7(3) 3_877 . ?
O511 W11 O1P2 83.4(3) 3_877 . ?
O12T W12 O2F2 100.1(5) . . ?
O12T W12 O112 102.7(4) . . ?
O2F2 W12 O112 91.5(4) . . ?
O12T W12 O123 100.2(4) . . ?
O2F2 W12 O123 94.5(5) . . ?
O112 W12 O123 154.9(4) . . ?
O12T W12 O612 94.1(5) . . ?
O2F2 W12 O612 165.6(4) . . ?
O112 W12 O612 83.4(4) . . ?
O123 W12 O612 84.8(4) . . ?
O12T W12 O2P2 172.4(4) . . ?
O2F2 W12 O2P2 83.4(4) . . ?
O112 W12 O2P2 83.9(4) . . ?
O123 W12 O2P2 72.7(3) . . ?
O612 W12 O2P2 82.7(4) . . ?
O13T W13 O3F3 102.5(5) . . ?
O13T W13 O134 102.6(5) . . ?
O3F3 W13 O134 92.4(4) . . ?
O13T W13 O123 97.4(5) . . ?
O3F3 W13 O123 96.5(5) . . ?
O134 W13 O123 155.7(4) . . ?
O13T W13 O713 91.8(5) . . ?
O3F3 W13 O713 165.6(4) . . ?
O134 W13 O713 82.6(4) . . ?
O123 W13 O713 83.2(4) . . ?
O13T W13 O2P2 169.8(4) . . ?
O3F3 W13 O2P2 84.2(4) . . ?
O134 W13 O2P2 84.6(4) . . ?
O123 W13 O2P2 74.0(4) . . ?
O713 W13 O2P2 81.9(4) . . ?
O14T W14 O4F3 99.3(5) . . ?
O14T W14 O134 102.7(5) . . ?
O4F3 W14 O134 91.9(5) . . ?
O14T W14 O145 100.0(5) . . ?
O4F3 W14 O145 95.7(5) . . ?
O134 W14 O145 154.5(4) . . ?
O14T W14 O814 93.8(5) . . ?
O4F3 W14 O814 166.8(4) . . ?
O134 W14 O814 83.2(4) . . ?
O145 W14 O814 84.0(4) . . ?
O14T W14 O3P2 171.9(4) . . ?
O4F3 W14 O3P2 85.7(4) . . ?
O134 W14 O3P2 83.4(4) . . ?
O145 W14 O3P2 73.0(4) . . ?
O814 W14 O3P2 81.6(4) . . ?
O15T W15 O5F1 100.9(4) . . ?
O15T W15 O105 101.8(4) . . ?
O5F1 W15 O105 92.4(4) . . ?
O15T W15 O145 99.1(4) . . ?
O5F1 W15 O145 96.0(4) . . ?
O105 W15 O145 155.6(4) . . ?
O15T W15 O915 92.6(4) . . ?
O5F1 W15 O915 166.4(4) . . ?
O105 W15 O915 82.9(4) . . ?
O145 W15 O915 83.6(4) . . ?
O15T W15 O3P2 171.3(4) . . ?
O5F1 W15 O3P2 83.9(4) . . ?
O105 W15 O3P2 85.2(3) . . ?
O145 W15 O3P2 73.0(3) . . ?
O915 W15 O3P2 83.0(4) . . ?
O2P1 P1 O4P1 112.3(6) . . ?
O2P1 P1 O3P1 111.1(6) . . ?
O4P1 P1 O3P1 111.0(6) . . ?
O2P1 P1 O1P1 107.2(6) . . ?
O4P1 P1 O1P1 106.8(6) . . ?
O3P1 P1 O1P1 108.2(6) . . ?
O1P2 P2 O2P2 111.7(5) . 3_877 ?
O1P2 P2 O3P2 109.2(5) . 3_877 ?
O2P2 P2 O3P2 109.7(6) 3_877 3_877 ?
O1P2 P2 O4P2 109.3(5) . . ?
O2P2 P2 O4P2 108.8(5) 3_877 . ?
O3P2 P2 O4P2 108.1(5) 3_877 . ?
O1F Fe1 O11L 97.6(4) . 3_877 ?
O1F Fe1 O5F1 100.2(4) . . ?
O11L Fe1 O5F1 162.2(4) 3_877 . ?
O1F Fe1 O0F1 109.3(4) . . ?
O11L Fe1 O0F1 90.1(4) 3_877 . ?
O5F1 Fe1 O0F1 82.6(4) . . ?
O1F Fe1 O1F 85.4(4) . 3_877 ?
O11L Fe1 O1F 91.5(4) 3_877 3_877 ?
O5F1 Fe1 O1F 91.5(4) . 3_877 ?
O0F1 Fe1 O1F 164.9(4) . 3_877 ?
O1F Fe1 O4P2 163.1(4) . 3_877 ?
O11L Fe1 O4P2 77.6(4) 3_877 3_877 ?
O5F1 Fe1 O4P2 85.8(4) . 3_877 ?
O0F1 Fe1 O4P2 87.2(4) . 3_877 ?
O1F Fe1 O4P2 78.6(3) 3_877 3_877 ?
O1F Fe1 Fe1 44.6(3) . 3_877 ?
O11L Fe1 Fe1 96.0(3) 3_877 3_877 ?
O5F1 Fe1 Fe1 97.7(3) . 3_877 ?
O0F1 Fe1 Fe1 153.6(3) . 3_877 ?
O1F Fe1 Fe1 40.8(3) 3_877 3_877 ?
O4P2 Fe1 Fe1 119.2(2) 3_877 3_877 ?
O12L Fe2 O2F2 97.3(4) . 3_877 ?
O12L Fe2 O11L 91.5(4) . . ?
O2F2 Fe2 O11L 168.3(4) 3_877 . ?
O12L Fe2 O21L 98.3(4) . . ?
O2F2 Fe2 O21L 92.6(4) 3_877 . ?
O11L Fe2 O21L 93.6(4) . . ?
O12L Fe2 O1F2 93.7(4) . . ?
O2F2 Fe2 O1F2 82.4(4) 3_877 . ?
O11L Fe2 O1F2 89.4(4) . . ?
O21L Fe2 O1F2 167.5(4) . . ?
O12L Fe2 O4P2 171.1(4) . . ?
O2F2 Fe2 O4P2 91.5(4) 3_877 . ?
O11L Fe2 O4P2 79.9(4) . . ?
O21L Fe2 O4P2 79.9(4) . . ?
O1F2 Fe2 O4P2 88.8(4) . . ?
O1F Fe3 O22L 101.9(4) . . ?
O1F Fe3 O4F3 98.2(4) . 3_877 ?
O22L Fe3 O4F3 95.5(4) . 3_877 ?
O1F Fe3 O21L 93.1(4) . . ?
O22L Fe3 O21L 94.5(4) . . ?
O4F3 Fe3 O21L 163.0(4) 3_877 . ?
O1F Fe3 O3F3 166.7(4) . 3_877 ?
O22L Fe3 O3F3 91.1(4) . 3_877 ?
O4F3 Fe3 O3F3 82.6(4) 3_877 3_877 ?
O21L Fe3 O3F3 83.5(4) . 3_877 ?
O1F Fe3 O4P2 82.0(4) . . ?
O22L Fe3 O4P2 171.7(4) . . ?
O4F3 Fe3 O4P2 91.2(4) 3_877 . ?
O21L Fe3 O4P2 77.8(4) . . ?
O3F3 Fe3 O4P2 84.7(4) 3_877 . ?
W10 O0F1 Fe1 149.7(5) . . ?
Fe1 O1F Fe3 155.1(5) . . ?
Fe1 O1F Fe1 94.6(4) . 3_877 ?
Fe3 O1F Fe1 110.1(4) . 3_877 ?
W10 O10T Na1 145.6(5) . . ?
P1 O1P1 W3 123.7(6) . . ?
P1 O1P1 W2 124.8(5) . . ?
W3 O1P1 W2 91.8(3) . . ?
P1 O1P1 W1 123.4(5) . . ?
W3 O1P1 W1 91.8(3) . . ?
W2 O1P1 W1 91.9(3) . . ?
P1 O2P1 W4 129.1(5) . . ?
P1 O2P1 W5 128.9(5) . . ?
W4 O2P1 W5 90.5(3) . . ?
P1 O3P1 W7 128.2(6) . . ?
P1 O3P1 W6 127.8(6) . . ?
W7 O3P1 W6 90.3(3) . . ?
P1 O4P1 W8 129.5(6) . . ?
P1 O4P1 W9 129.1(6) . . ?
W8 O4P1 W9 90.4(3) . . ?
P2 O1P2 W10 127.9(5) . 3_877 ?
P2 O1P2 W11 125.9(5) . . ?
W10 O1P2 W11 91.7(3) 3_877 . ?
P2 O2P2 W13 126.5(5) 3_877 . ?
P2 O2P2 W12 126.6(6) 3_877 . ?
W13 O2P2 W12 92.2(3) . . ?
P2 O3P2 W15 126.2(5) 3_877 . ?
P2 O3P2 W14 127.2(5) 3_877 . ?
W15 O3P2 W14 91.6(3) . . ?
P2 O4P2 Fe2 122.1(5) . . ?
P2 O4P2 Fe3 124.8(5) . . ?
Fe2 O4P2 Fe3 93.8(3) . . ?
P2 O4P2 Fe1 124.5(5) . 3_877 ?
Fe2 O4P2 Fe1 93.1(4) . 3_877 ?
Fe3 O4P2 Fe1 89.2(3) . 3_877 ?
W11 O1F2 Fe2 148.1(6) . . ?
W12 O2F2 Fe2 148.7(5) . 3_877 ?
W13 O3F3 Fe3 147.9(5) . 3_877 ?
W14 O4F3 Fe3 148.3(6) . 3_877 ?
W15 O5F1 Fe1 150.2(5) . . ?
W2 O12 W1 122.0(5) . . ?
W3 O13 W1 122.0(5) . . ?
W1 O14 W4 148.3(6) . . ?
W1 O19 W9 148.8(6) . . ?
W2 O23 W3 122.0(6) . . ?
W2 O25 W5 151.0(6) . . ?
W2 O26 W6 150.7(6) . . ?
W3 O37 W7 151.0(6) . . ?
W3 O38 W8 148.5(6) . . ?
W5 O45 W4 121.0(5) . . ?
W4 O49 W9 154.1(5) . . ?
W6 O56 W5 155.0(6) . . ?
W6 O67 W7 121.4(5) . . ?
W7 O78 W8 155.5(6) . . ?
W9 O89 W8 119.7(5) . . ?
W10 O101 W11 121.7(5) . 3_877 ?
W10 O105 W15 141.3(5) . . ?
W12 O112 W11 144.5(5) . 3_877 ?
W13 O123 W12 120.8(4) . . ?
W14 O134 W13 142.7(6) . . ?
W14 O145 W15 122.0(5) . . ?
W4 O410 W10 163.6(5) . . ?
W5 O511 W11 161.7(6) . 3_877 ?
W6 O612 W12 162.1(6) . . ?
W7 O713 W13 161.9(5) . . ?
W8 O814 W14 162.5(6) . . ?
W9 O915 W15 162.2(6) . . ?
C11 O11L Fe2 128.2(8) . . ?
C11 O11L Fe1 119.7(8) . 3_877 ?
Fe2 O11L Fe1 109.2(4) . 3_877 ?
C12 O12L Fe2 125.2(10) . . ?
C21 O21L Fe2 120.9(8) . . ?
C21 O21L Fe3 117.9(8) . . ?
Fe2 O21L Fe3 108.2(4) . . ?
C22 O22L Fe3 120.5(10) . . ?
C23 O23L Na1 126.0(10) . . ?
C11 C1 N1 108.8(13) . . ?
C11 C1 C12 116.2(14) . . ?
N1 C1 C12 105.1(13) . . ?
C11 C1 C13 107.3(13) . . ?
N1 C1 C13 106.5(12) . . ?
C12 C1 C13 112.4(13) . . ?
N2 C2 C22 105.0(12) . . ?
N2 C2 C23 111.7(11) . . ?
C22 C2 C23 112.3(12) . . ?
N2 C2 C21 109.9(11) . . ?
C22 C2 C21 112.9(11) . . ?
C23 C2 C21 105.1(12) . . ?
O11L C11 C1 115.0(13) . . ?
O12L C12 C1 112.7(14) . . ?
O14L C13 C1 113.0(17) . . ?
O13L C13 C1 108.3(14) . . ?
O21L C21 C2 109.8(12) . . ?
O22L C22 C2 114.3(13) . . ?
O23L C23 C2 111.6(14) . . ?
O23L Na1 O23L 180.0 . 3_777 ?
O23L Na1 O1W 83.9(4) . 3_777 ?
O23L Na1 O1W 96.1(5) 3_777 3_777 ?
O23L Na1 O1W 96.1(5) . . ?
O23L Na1 O1W 83.9(5) 3_777 . ?
O1W Na1 O1W 180.0 3_777 . ?
O23L Na1 O10T 100.9(3) . . ?
O23L Na1 O10T 79.1(3) 3_777 . ?
O1W Na1 O10T 83.8(4) 3_777 . ?
O1W Na1 O10T 96.2(4) . . ?
O23L Na1 O10T 79.1(3) . 3_777 ?
O23L Na1 O10T 100.9(3) 3_777 3_777 ?
O1W Na1 O10T 96.2(4) 3_777 3_777 ?
O1W Na1 O10T 83.8(4) . 3_777 ?
O10T Na1 O10T 180.0 . 3_777 ?
N3 C3 C31 105(3) . . ?
N3 C3 C32 104(3) . . ?
C31 C3 C32 112(3) . . ?
N3 C3 C33 105(3) . . ?
C31 C3 C33 114(3) . . ?
C32 C3 C33 116(3) . . ?
O31 C31 C3 119(4) . . ?
O32 C32 C3 120(3) . . ?
O33 C33 C3 108(3) . . ?

_refine_diff_density_max         3.162
_refine_diff_density_min         -2.256
_refine_diff_density_rms         0.374




