# Electronic Supplementary Material (ESI) for Dalton Transactions.
# 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_jtm1136_0m_a_sq
_database_code_depnum_ccdc_archive 'CCDC 2027890'
loop_
_audit_author_name
_audit_author_address
'Joel T. Mague'
;Department of Chemistry, Tulane University
United States of America
;
_audit_update_record             
;
2020-09-05 deposited with the CCDC.	2021-01-13 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C21 H33 N3 Na O67 Si Tb3 W12, 10(H2 O), 2(O)'
_chemical_formula_sum            'C21 H53 N3 Na O79 Si Tb3 W12'
_chemical_formula_weight         4345.70

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'
Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Tb Tb -0.1723 4.1537 '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'
Na Na 0.0362 0.0249 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      trigonal
_space_group_IT_number           146
_space_group_name_H-M_alt        'R 3'
_space_group_name_Hall           'R 3'

_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+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'

_cell_length_a                   18.080(2)
_cell_length_b                   18.080(2)
_cell_length_c                   20.905(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     5918.3(17)
_cell_formula_units_Z            3
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    9877
_cell_measurement_theta_min      2.252
_cell_measurement_theta_max      29.100

_exptl_crystal_description       block
_exptl_crystal_colour            'light yellow'
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    3.658
_exptl_crystal_F_000             5820
_exptl_transmission_factor_min   0.324
_exptl_transmission_factor_max   0.746
_exptl_crystal_size_max          0.220
_exptl_crystal_size_mid          0.210
_exptl_crystal_size_min          0.172
_exptl_absorpt_coefficient_mu    20.212
_shelx_estimated_absorpt_T_min   0.095
_shelx_estimated_absorpt_T_max   0.129
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Krause et al., 2015)'
_exptl_absorpt_correction_T_min  0.10
_exptl_absorpt_correction_T_max  0.13

_exptl_special_details           
;
The diffraction data were obtained from 3 sets of 400 frames,
each of width 0.5° in ω, colllected at φ = 0.00,
90.00 and 180.00° and 2 sets of 800 frames, each of
width 0.45° in φ, collected at ω = --30.00 and 210.00°.
The scan time was 20 sec/frame.
;

_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite

_diffrn_measurement_device_type  'Bruker Smart APEX CCD'
_diffrn_measurement_method       'φ and ω scans'

_diffrn_detector_area_resol_mean 8.3333

_diffrn_reflns_number            38417
_diffrn_reflns_av_unetI/netI     0.0459
_diffrn_reflns_av_R_equivalents  0.0529
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_theta_min         1.625
_diffrn_reflns_theta_max         29.249
_diffrn_reflns_theta_full        29.200
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_point_group_measured_fraction_full 0.992
_reflns_number_total             7090
_reflns_number_gt                6469
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.984
_reflns_Friedel_fraction_max     0.981
_reflns_Friedel_fraction_full    0.986

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

_computing_data_collection       'APEX3 (Bruker, 2016)'
_computing_cell_refinement       'SAINT (Bruker, 2016)'
_computing_data_reduction        'SAINT (Bruker, 2016)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015a)'
_computing_structure_refinement  
'SHELXL-2018/1 (Sheldrick, 2015b)'
_computing_molecular_graphics    'DIAMOND (Brandenburg & Putz, 2012)'
_computing_publication_material  'SHELXTL (Bruker, 2016)'

_refine_special_details          
;
Refinement of F² against ALL reflections.  The weighted R-factor wR and
goodness of fit S are based on F², conventional R-factors R are based
on F, with F set to zero for negative F². The threshold expression of
F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement.  R-factors based
on F² are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger. H-atoms attached to carbon 
were placed in calculated positions (C---H = 0.95 Å) while those 
attached to oxygen were placed in locations which would provide the most 
effective hydrogen bonding interactions with O---H = 0.87 %A. All were 
included as riding contributions with isotropic displacement parameters 
1.2 - 1.5 times those of the attached atoms.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0539P)²+4.6626P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Flack x determined using 2943 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons et al., 2013).
;
_refine_ls_abs_structure_Flack   0.003(7)
_chemical_absolute_configuration ad
_refine_ls_number_reflns         7090
_refine_ls_number_parameters     373
_refine_ls_number_restraints     229
_refine_ls_R_factor_all          0.0394
_refine_ls_R_factor_gt           0.0357
_refine_ls_wR_factor_ref         0.0920
_refine_ls_wR_factor_gt          0.0909
_refine_ls_goodness_of_fit_ref   1.098
_refine_ls_restrained_S_all      1.097
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
W1 W 0.53020(4) 0.25888(4) 0.51846(3) 0.01283(13) Uani 1 1 d . . . . .
Na1 Na 0.666667 0.333333 0.7702(7) 0.049(3) Uani 1 3 d S TU P . .
W2 W 0.48442(4) 0.13127(4) 0.39121(3) 0.01823(14) Uani 1 1 d . . . . .
W3 W 0.61253(5) 0.20977(5) 0.24406(3) 0.02646(17) Uani 1 1 d . . . . .
W4 W 0.69829(4) 0.15398(4) 0.38558(3) 0.01846(15) Uani 1 1 d . . . . .
Tb1 Tb 0.42872(6) 0.17006(5) 0.69923(4) 0.02689(19) Uani 1 1 d . . . . .
Si1 Si 0.666667 0.333333 0.3857(4) 0.014 Uani 1 3 d S T P . .
O1 O 0.4986(9) 0.3188(9) 0.7040(7) 0.035(3) Uani 1 1 d . U . . .
O2 O 0.6372(8) 0.4215(9) 0.7073(6) 0.035(3) Uani 1 1 d . U . . .
O3 O 0.7484(8) 0.6758(8) 0.6238(6) 0.030(3) Uani 1 1 d . U . . .
O4 O 0.6867(8) 0.7200(9) 0.5526(6) 0.036(3) Uani 1 1 d . U . . .
O5 O 0.4038(9) 0.4383(10) 0.5143(7) 0.043(3) Uani 1 1 d . U . . .
H5 H 0.399728 0.480365 0.501989 0.064 Uiso 1 1 calc R U . . .
O6 O 0.2907(9) 0.0733(9) 0.7534(7) 0.037(3) Uani 1 1 d . U . . .
H6A H 0.272469 0.103563 0.773037 0.056 Uiso 1 1 d R U . . .
H6B H 0.298280 0.041694 0.780987 0.056 Uiso 1 1 d R U . . .
O7 O 0.4493(9) 0.0688(9) 0.7713(7) 0.037(3) Uani 1 1 d . U . . .
H7A H 0.481342 0.052578 0.751791 0.055 Uiso 1 1 d R U . . .
H7B H 0.399853 0.024398 0.779631 0.055 Uiso 1 1 d R U . . .
O8 O 0.4425(9) 0.2119(10) 0.8106(7) 0.042(3) Uani 1 1 d . U . . .
H8A H 0.472045 0.267327 0.813154 0.063 Uiso 1 1 d R U . . .
H8B H 0.468793 0.190038 0.831314 0.063 Uiso 1 1 d R U . . .
O9 O 0.3291(8) 0.2225(8) 0.6837(6) 0.030(3) Uani 1 1 d . U . . .
H9A H 0.281512 0.181911 0.667892 0.044 Uiso 1 1 d R U . . .
H9B H 0.351373 0.265502 0.657422 0.044 Uiso 1 1 d R U . . .
O10 O 0.4844(7) 0.2330(7) 0.5937(5) 0.018(2) Uani 1 1 d . U . . .
O11 O 0.6259(6) 0.2381(6) 0.5277(5) 0.0119(18) Uani 1 1 d . U . . .
O12 O 0.6737(8) 0.1775(8) 0.3035(6) 0.025(2) Uani 1 1 d . U . . .
O13 O 0.6899(8) 0.0559(7) 0.3772(6) 0.026(2) Uani 1 1 d . U . . .
O14 O 0.5696(8) 0.2780(8) 0.2081(6) 0.030(3) Uani 1 1 d . U . . .
O15 O 0.4516(6) 0.2856(6) 0.4770(5) 0.0147(19) Uani 1 1 d . U . . .
O16 O 0.4713(6) 0.1469(7) 0.4796(5) 0.019(2) Uani 1 1 d . U . . .
O17 O 0.4088(7) 0.0261(7) 0.3810(6) 0.026(3) Uani 1 1 d . U . . .
O18 O 0.4121(7) 0.1832(7) 0.3755(5) 0.021(2) Uani 1 1 d . U . . .
O19 O 0.5807(7) 0.1234(6) 0.4057(5) 0.019(2) Uani 1 1 d . U . . .
O20 O 0.5766(9) 0.1307(9) 0.1889(7) 0.038(3) Uani 1 1 d . U . . .
O21 O 0.5243(8) 0.1627(8) 0.3059(6) 0.027(3) Uani 1 1 d . U . . .
O22 O 0.666667 0.333333 0.3068(9) 0.020(3) Uani 1 3 d S TU P . .
O23 O 0.5692(6) 0.2770(6) 0.4121(5) 0.0133(19) Uani 1 1 d . U . . .
N1 N 0.6112(9) 0.5258(9) 0.6335(7) 0.026(3) Uani 1 1 d . U . . .
C1 C 0.5595(11) 0.3904(11) 0.6849(9) 0.028(4) Uani 1 1 d . U . . .
C2 C 0.5478(11) 0.4441(11) 0.6387(9) 0.027(4) Uani 1 1 d . U . . .
C3 C 0.4739(10) 0.4111(11) 0.5994(8) 0.024(3) Uani 1 1 d . U . . .
H3 H 0.429205 0.353474 0.603296 0.029 Uiso 1 1 calc R U . . .
C4 C 0.4691(11) 0.4649(12) 0.5559(9) 0.029(4) Uani 1 1 d . U . . .
C5 C 0.5359(12) 0.5509(12) 0.5526(9) 0.029(4) Uani 1 1 d . U . . .
H5A H 0.532855 0.589672 0.523499 0.035 Uiso 1 1 calc R U . . .
C6 C 0.6050(11) 0.5772(11) 0.5920(8) 0.024(3) Uani 1 1 d . U . . .
C7 C 0.6861(11) 0.6659(11) 0.5891(8) 0.025(3) Uani 1 1 d . U . . .
O24 O 0.1636(17) 0.1901(18) 0.7317(14) 0.068(7) Uani 0.71(3) 1 d . U P A 1
H24A H 0.161874 0.203499 0.771389 0.103 Uiso 0.71(3) 1 d R U P A 1
H24B H 0.169345 0.145139 0.730122 0.103 Uiso 0.71(3) 1 d R U P A 1
O24A O 0.155(4) 0.100(4) 0.718(3) 0.068(7) Uani 0.29(3) 1 d . U P A 2
H24C H 0.160072 0.084199 0.756787 0.103 Uiso 0.29(3) 1 d R U P A 2
H24D H 0.143652 0.141309 0.721056 0.103 Uiso 0.29(3) 1 d R U P A 2
O25 O 0.7275(13) 0.8795(12) 0.6313(10) 0.065(5) Uani 1 1 d . U . . .
H25A H 0.754780 0.910346 0.664411 0.098 Uiso 1 1 d R U . . .
H25B H 0.723810 0.911985 0.602278 0.098 Uiso 1 1 d R U . . .
O26 O 0.8890(14) 0.7724(14) 0.5468(12) 0.047(6) Uani 0.6667 1 d . U P . .
H26A H 0.903129 0.733003 0.548488 0.071 Uiso 0.6667 1 d R U P . .
H26B H 0.884848 0.784079 0.507029 0.071 Uiso 0.6667 1 d R U P . .
O27 O 0.3812(16) 0.3143(16) 0.8716(12) 0.053(6) Uani 0.6667 1 d . U P . .
O28 O 0.869(3) 0.828(3) 0.625(2) 0.122(15) Uani 0.6667 1 d . U P . .
H28A H 0.873613 0.816072 0.664724 0.184 Uiso 0.6667 1 d R U P . .
H28B H 0.855333 0.867155 0.623264 0.184 Uiso 0.6667 1 d 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 O10 1.729(11) . ?
W1 O11 1.867(9) 3_665 ?
W1 O15 1.922(10) . ?
W1 O16 1.934(10) . ?
W1 O11 1.955(9) . ?
W1 O23 2.307(10) . ?
Na1 O2 2.324(17) 3_665 ?
Na1 O2 2.324(17) 2_655 ?
Na1 O2 2.324(17) . ?
Na1 Tb1 4.090(6) . ?
Na1 Tb1 4.090(6) 2_655 ?
Na1 Tb1 4.090(6) 3_665 ?
W2 O17 1.711(12) . ?
W2 O19 1.841(11) . ?
W2 O16 1.901(11) . ?
W2 O21 1.902(12) . ?
W2 O18 1.982(11) . ?
W2 O23 2.332(10) . ?
W3 O20 1.693(14) . ?
W3 O21 1.892(12) . ?
W3 O14 1.910(13) . ?
W3 O14 1.934(12) 2_655 ?
W3 O12 1.937(12) . ?
W3 O22 2.342(11) . ?
W4 O13 1.711(11) . ?
W4 O12 1.874(12) . ?
W4 O18 1.889(11) 2_655 ?
W4 O15 1.928(11) 2_655 ?
W4 O19 1.957(10) . ?
W4 O23 2.374(10) 2_655 ?
Tb1 O1 2.333(14) . ?
Tb1 O2 2.410(14) 2_655 ?
Tb1 O3 2.415(13) 2_655 ?
Tb1 O8 2.423(15) . ?
Tb1 O9 2.440(12) . ?
Tb1 O10 2.456(11) . ?
Tb1 N1 2.482(14) 2_655 ?
Tb1 O6 2.491(13) . ?
Tb1 O7 2.538(13) . ?
Si1 O23 1.629(10) 2_655 ?
Si1 O23 1.629(10) 3_665 ?
Si1 O23 1.629(10) . ?
Si1 O22 1.65(2) . ?
O1 C1 1.27(2) . ?
O2 C1 1.31(2) . ?
O3 C7 1.27(2) . ?
O4 C7 1.24(2) . ?
O5 C4 1.35(2) . ?
O5 H5 0.8400 . ?
O6 H6A 0.8702 . ?
O6 H6B 0.8699 . ?
O7 H7A 0.8699 . ?
O7 H7B 0.8700 . ?
O8 H8A 0.8700 . ?
O8 H8B 0.8700 . ?
O9 H9A 0.8701 . ?
O9 H9B 0.8701 . ?
N1 C6 1.32(2) . ?
N1 C2 1.35(2) . ?
C1 C2 1.46(2) . ?
C2 C3 1.42(2) . ?
C3 C4 1.37(3) . ?
C3 H3 0.9500 . ?
C4 C5 1.42(2) . ?
C5 C6 1.37(2) . ?
C5 H5A 0.9500 . ?
C6 C7 1.54(2) . ?
O24 H24A 0.8699 . ?
O24 H24B 0.8700 . ?
O24A H24C 0.8700 . ?
O24A H24D 0.8699 . ?
O25 H25A 0.8701 . ?
O25 H25B 0.8700 . ?
O26 H26A 0.8699 . ?
O26 H26B 0.8701 . ?
O28 H28A 0.8701 . ?
O28 H28B 0.8699 . ?

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
O10 W1 O11 102.3(5) . 3_665 ?
O10 W1 O15 99.4(5) . . ?
O11 W1 O15 92.3(4) 3_665 . ?
O10 W1 O16 99.2(5) . . ?
O11 W1 O16 157.8(4) 3_665 . ?
O15 W1 O16 89.1(4) . . ?
O10 W1 O11 102.1(5) . . ?
O11 W1 O11 85.3(5) 3_665 . ?
O15 W1 O11 158.4(4) . . ?
O16 W1 O11 85.2(4) . . ?
O10 W1 O23 170.5(4) . . ?
O11 W1 O23 85.8(4) 3_665 . ?
O15 W1 O23 75.0(4) . . ?
O16 W1 O23 73.3(4) . . ?
O11 W1 O23 83.4(4) . . ?
O2 Na1 O2 91.1(6) 3_665 2_655 ?
O2 Na1 O2 91.1(6) 3_665 . ?
O2 Na1 O2 91.1(6) 2_655 . ?
O2 Na1 Tb1 118.1(5) 3_665 . ?
O2 Na1 Tb1 30.9(3) 2_655 . ?
O2 Na1 Tb1 76.7(4) . . ?
O2 Na1 Tb1 30.9(3) 3_665 2_655 ?
O2 Na1 Tb1 76.7(4) 2_655 2_655 ?
O2 Na1 Tb1 118.1(5) . 2_655 ?
Tb1 Na1 Tb1 107.6(2) . 2_655 ?
O2 Na1 Tb1 76.7(4) 3_665 3_665 ?
O2 Na1 Tb1 118.1(5) 2_655 3_665 ?
O2 Na1 Tb1 30.9(3) . 3_665 ?
Tb1 Na1 Tb1 107.6(2) . 3_665 ?
Tb1 Na1 Tb1 107.6(2) 2_655 3_665 ?
O17 W2 O19 101.3(5) . . ?
O17 W2 O16 101.3(5) . . ?
O19 W2 O16 92.5(5) . . ?
O17 W2 O21 100.8(5) . . ?
O19 W2 O21 86.9(5) . . ?
O16 W2 O21 157.5(5) . . ?
O17 W2 O18 99.0(5) . . ?
O19 W2 O18 159.6(5) . . ?
O16 W2 O18 86.0(5) . . ?
O21 W2 O18 86.9(5) . . ?
O17 W2 O23 170.6(4) . . ?
O19 W2 O23 86.8(4) . . ?
O16 W2 O23 73.2(4) . . ?
O21 W2 O23 84.3(4) . . ?
O18 W2 O23 73.3(4) . . ?
O20 W3 O21 101.7(6) . . ?
O20 W3 O14 99.8(6) . . ?
O21 W3 O14 92.1(5) . . ?
O20 W3 O14 101.3(6) . 2_655 ?
O21 W3 O14 156.8(5) . 2_655 ?
O14 W3 O14 86.8(7) . 2_655 ?
O20 W3 O12 102.6(6) . . ?
O21 W3 O12 84.6(5) . . ?
O14 W3 O12 157.6(5) . . ?
O14 W3 O12 87.7(5) 2_655 . ?
O20 W3 O22 171.1(6) . . ?
O21 W3 O22 84.4(5) . . ?
O14 W3 O22 73.4(5) . . ?
O14 W3 O22 73.0(5) 2_655 . ?
O12 W3 O22 84.2(5) . . ?
O13 W4 O12 103.4(6) . . ?
O13 W4 O18 102.3(5) . 2_655 ?
O12 W4 O18 92.8(5) . 2_655 ?
O13 W4 O15 98.5(5) . 2_655 ?
O12 W4 O15 157.1(5) . 2_655 ?
O18 W4 O15 88.6(5) 2_655 2_655 ?
O13 W4 O19 102.0(5) . . ?
O12 W4 O19 85.1(5) . . ?
O18 W4 O19 155.4(5) 2_655 . ?
O15 W4 O19 84.3(4) 2_655 . ?
O13 W4 O23 170.8(5) . 2_655 ?
O12 W4 O23 85.2(4) . 2_655 ?
O18 W4 O23 73.9(4) 2_655 2_655 ?
O15 W4 O23 73.3(4) 2_655 2_655 ?
O19 W4 O23 81.6(4) . 2_655 ?
O1 Tb1 O2 74.6(5) . 2_655 ?
O1 Tb1 O3 130.1(5) . 2_655 ?
O2 Tb1 O3 129.1(4) 2_655 2_655 ?
O1 Tb1 O8 71.8(5) . . ?
O2 Tb1 O8 84.4(5) 2_655 . ?
O3 Tb1 O8 140.9(5) 2_655 . ?
O1 Tb1 O9 68.7(4) . . ?
O2 Tb1 O9 142.9(4) 2_655 . ?
O3 Tb1 O9 74.7(4) 2_655 . ?
O8 Tb1 O9 89.3(5) . . ?
O1 Tb1 O10 69.1(4) . . ?
O2 Tb1 O10 77.0(4) 2_655 . ?
O3 Tb1 O10 75.0(4) 2_655 . ?
O8 Tb1 O10 139.9(4) . . ?
O9 Tb1 O10 84.9(4) . . ?
O1 Tb1 N1 125.4(5) . 2_655 ?
O2 Tb1 N1 65.7(5) 2_655 2_655 ?
O3 Tb1 N1 64.4(5) 2_655 2_655 ?
O8 Tb1 N1 135.3(5) . 2_655 ?
O9 Tb1 N1 134.6(4) . 2_655 ?
O10 Tb1 N1 66.6(4) . 2_655 ?
O1 Tb1 O6 124.4(5) . . ?
O2 Tb1 O6 140.2(5) 2_655 . ?
O3 Tb1 O6 68.9(4) 2_655 . ?
O8 Tb1 O6 72.1(5) . . ?
O9 Tb1 O6 70.0(4) . . ?
O10 Tb1 O6 140.2(4) . . ?
N1 Tb1 O6 110.1(5) 2_655 . ?
O1 Tb1 O7 128.1(5) . . ?
O2 Tb1 O7 70.2(5) 2_655 . ?
O3 Tb1 O7 101.8(4) 2_655 . ?
O8 Tb1 O7 68.0(5) . . ?
O9 Tb1 O7 139.6(4) . . ?
O10 Tb1 O7 133.9(4) . . ?
N1 Tb1 O7 70.8(5) 2_655 . ?
O6 Tb1 O7 71.4(5) . . ?
O1 Tb1 Na1 52.0(3) . . ?
O2 Tb1 Na1 29.6(3) 2_655 . ?
O3 Tb1 Na1 157.0(3) 2_655 . ?
O8 Tb1 Na1 61.2(4) . . ?
O9 Tb1 Na1 118.8(3) . . ?
O10 Tb1 Na1 87.3(3) . . ?
N1 Tb1 Na1 95.3(4) 2_655 . ?
O6 Tb1 Na1 131.7(4) . . ?
O7 Tb1 Na1 79.9(3) . . ?
O23 Si1 O23 109.1(5) 2_655 3_665 ?
O23 Si1 O23 109.1(5) 2_655 . ?
O23 Si1 O23 109.1(5) 3_665 . ?
O23 Si1 O22 109.8(5) 2_655 . ?
O23 Si1 O22 109.8(5) 3_665 . ?
O23 Si1 O22 109.8(5) . . ?
C1 O1 Tb1 148.5(12) . . ?
C1 O2 Na1 118.2(11) . . ?
C1 O2 Tb1 121.6(11) . 3_665 ?
Na1 O2 Tb1 119.5(6) . 3_665 ?
C7 O3 Tb1 124.4(11) . 3_665 ?
C4 O5 H5 109.5 . . ?
Tb1 O6 H6A 109.5 . . ?
Tb1 O6 H6B 109.3 . . ?
H6A O6 H6B 109.5 . . ?
Tb1 O7 H7A 109.1 . . ?
Tb1 O7 H7B 109.3 . . ?
H7A O7 H7B 109.5 . . ?
Tb1 O8 H8A 109.0 . . ?
Tb1 O8 H8B 109.3 . . ?
H8A O8 H8B 109.5 . . ?
Tb1 O9 H9A 109.5 . . ?
Tb1 O9 H9B 109.3 . . ?
H9A O9 H9B 109.5 . . ?
W1 O10 Tb1 166.4(6) . . ?
W1 O11 W1 151.7(5) 2_655 . ?
W4 O12 W3 153.0(7) . . ?
W3 O14 W3 121.8(7) . 3_665 ?
W1 O15 W4 120.5(5) . 3_665 ?
W2 O16 W1 121.3(6) . . ?
W4 O18 W2 121.3(5) 3_665 . ?
W2 O19 W4 151.5(6) . . ?
W3 O21 W2 152.1(7) . . ?
Si1 O22 W3 124.1(4) . 2_655 ?
Si1 O22 W3 124.1(4) . . ?
W3 O22 W3 91.7(6) 2_655 . ?
Si1 O22 W3 124.1(4) . 3_665 ?
W3 O22 W3 91.7(6) 2_655 3_665 ?
W3 O22 W3 91.7(6) . 3_665 ?
Si1 O23 W1 125.0(6) . . ?
Si1 O23 W2 122.5(5) . . ?
W1 O23 W2 92.2(4) . . ?
Si1 O23 W4 124.7(5) . 3_665 ?
W1 O23 W4 91.1(3) . 3_665 ?
W2 O23 W4 91.6(3) . 3_665 ?
C6 N1 C2 120.0(15) . . ?
C6 N1 Tb1 122.2(11) . 3_665 ?
C2 N1 Tb1 117.7(11) . 3_665 ?
O1 C1 O2 121.4(16) . . ?
O1 C1 C2 123.0(16) . . ?
O2 C1 C2 115.6(16) . . ?
N1 C2 C3 121.4(16) . . ?
N1 C2 C1 117.1(16) . . ?
C3 C2 C1 121.5(16) . . ?
C4 C3 C2 117.8(16) . . ?
C4 C3 H3 121.1 . . ?
C2 C3 H3 121.1 . . ?
O5 C4 C3 122.1(17) . . ?
O5 C4 C5 118.3(17) . . ?
C3 C4 C5 119.5(16) . . ?
C6 C5 C4 118.8(16) . . ?
C6 C5 H5A 120.6 . . ?
C4 C5 H5A 120.6 . . ?
N1 C6 C5 122.5(16) . . ?
N1 C6 C7 112.8(15) . . ?
C5 C6 C7 124.5(16) . . ?
O4 C7 O3 125.7(16) . . ?
O4 C7 C6 118.2(15) . . ?
O3 C7 C6 116.0(15) . . ?
H24A O24 H24B 109.5 . . ?
H24C O24A H24D 109.5 . . ?
H25A O25 H25B 109.5 . . ?
H26A O26 H26B 109.5 . . ?
H28A O28 H28B 109.5 . . ?

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
O11 W1 O10 Tb1 -124(3) 3_665 . . . ?
O15 W1 O10 Tb1 141(3) . . . . ?
O16 W1 O10 Tb1 50(3) . . . . ?
O11 W1 O10 Tb1 -37(3) . . . . ?
O13 W4 O12 W3 128.0(15) . . . . ?
O18 W4 O12 W3 -128.7(15) 2_655 . . . ?
O15 W4 O12 W3 -36(2) 2_655 . . . ?
O19 W4 O12 W3 26.7(15) . . . . ?
O23 W4 O12 W3 -55.2(15) 2_655 . . . ?
O17 W2 O19 W4 124.8(13) . . . . ?
O16 W2 O19 W4 -133.2(13) . . . . ?
O21 W2 O19 W4 24.3(13) . . . . ?
O18 W2 O19 W4 -48(2) . . . . ?
O23 W2 O19 W4 -60.2(13) . . . . ?
O20 W3 O21 W2 127.5(15) . . . . ?
O14 W3 O21 W2 -132.1(15) . . . . ?
O14 W3 O21 W2 -45(2) 2_655 . . . ?
O12 W3 O21 W2 25.7(15) . . . . ?
O22 W3 O21 W2 -59.0(15) . . . . ?
O23 Si1 O22 W3 -58.9(4) 2_655 . . 2_655 ?
O23 Si1 O22 W3 61.1(4) 3_665 . . 2_655 ?
O23 Si1 O22 W3 -178.9(4) . . . 2_655 ?
O23 Si1 O22 W3 61.1(4) 2_655 . . . ?
O23 Si1 O22 W3 -178.9(4) 3_665 . . . ?
O23 Si1 O22 W3 -58.9(4) . . . . ?
O23 Si1 O22 W3 -178.9(4) 2_655 . . 3_665 ?
O23 Si1 O22 W3 -58.9(4) 3_665 . . 3_665 ?
O23 Si1 O22 W3 61.1(4) . . . 3_665 ?
O23 Si1 O23 W1 62.0(6) 2_655 . . . ?
O23 Si1 O23 W1 -57.1(7) 3_665 . . . ?
O22 Si1 O23 W1 -177.6(4) . . . . ?
O23 Si1 O23 W2 -58.1(11) 2_655 . . . ?
O23 Si1 O23 W2 -177.3(4) 3_665 . . . ?
O22 Si1 O23 W2 62.3(6) . . . . ?
O23 Si1 O23 W4 -176.9(4) 2_655 . . 3_665 ?
O23 Si1 O23 W4 63.9(11) 3_665 . . 3_665 ?
O22 Si1 O23 W4 -56.5(6) . . . 3_665 ?
Tb1 O1 C1 O2 -78(3) . . . . ?
Tb1 O1 C1 C2 103(2) . . . . ?
Na1 O2 C1 O1 10(2) . . . . ?
Tb1 O2 C1 O1 -160.1(13) 3_665 . . . ?
Na1 O2 C1 C2 -171.8(12) . . . . ?
Tb1 O2 C1 C2 18(2) 3_665 . . . ?
C6 N1 C2 C3 1(2) . . . . ?
Tb1 N1 C2 C3 -175.3(12) 3_665 . . . ?
C6 N1 C2 C1 179.0(15) . . . . ?
Tb1 N1 C2 C1 3(2) 3_665 . . . ?
O1 C1 C2 N1 164.9(17) . . . . ?
O2 C1 C2 N1 -13(2) . . . . ?
O1 C1 C2 C3 -17(3) . . . . ?
O2 C1 C2 C3 164.7(16) . . . . ?
N1 C2 C3 C4 0(2) . . . . ?
C1 C2 C3 C4 -177.9(16) . . . . ?
C2 C3 C4 O5 176.5(16) . . . . ?
C2 C3 C4 C5 -2(2) . . . . ?
O5 C4 C5 C6 -176.2(18) . . . . ?
C3 C4 C5 C6 2(2) . . . . ?
C2 N1 C6 C5 0(3) . . . . ?
Tb1 N1 C6 C5 175.5(13) 3_665 . . . ?
C2 N1 C6 C7 -175.7(14) . . . . ?
Tb1 N1 C6 C7 0.3(19) 3_665 . . . ?
C4 C5 C6 N1 -1(3) . . . . ?
C4 C5 C6 C7 173.7(15) . . . . ?
Tb1 O3 C7 O4 176.1(13) 3_665 . . . ?
Tb1 O3 C7 C6 -6(2) 3_665 . . . ?
N1 C6 C7 O4 -178.6(16) . . . . ?
C5 C6 C7 O4 6(3) . . . . ?
N1 C6 C7 O3 4(2) . . . . ?
C5 C6 C7 O3 -171.4(16) . . . . ?

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
O5 H5 O24 0.84 2.38 2.97(3) 127 9_554 yes
O6 H6A O20 0.87 2.19 2.96(2) 146 8_545 yes
O6 H6B O4 0.87 2.37 3.08(2) 130 4_445 yes
O7 H7A O18 0.87 2.28 2.882(18) 126 6 yes
O7 H7B O17 0.87 2.39 3.059(18) 134 6 yes
O9 H9A O24A 0.87 2.26 2.89(6) 128 . yes
O24 H24A O5 0.87 2.21 2.97(3) 146 5 yes
O24A H24C O20 0.87 2.17 2.97(7) 151 8_545 yes
O25 H25A O24 0.87 1.77 2.64(3) 180 2_665 yes
O25 H25B O27 0.87 1.89 2.76(3) 179 7_554 yes
O26 H26A O27 0.87 2.10 2.78(3) 134 8_654 yes
O26 H26B O7 0.87 2.16 2.83(3) 135 7_554 yes
O28 H28A O24A 0.87 1.59 2.31(8) 139 3_665 yes
O28 H28B O25 0.87 2.44 3.14(5) 139 . yes

_refine_diff_density_max         3.940
_refine_diff_density_min         -2.669
_refine_diff_density_rms         0.309



