# Electronic Supplementary Material (ESI) for CrystEngComm.
# This journal is © The Royal Society of Chemistry 2020

####################################################################### 
# 
# 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_3er
_database_code_depnum_ccdc_archive 'CCDC 1959264'
loop_
_audit_author_name
_audit_author_address
'Kittipong Chainok'
;Thammasat University
Thailand
;
_audit_update_record             
;
2020-01-07 deposited with the CCDC.	2020-06-23 downloaded from the CCDC.
;
_audit_creation_date             2019-10-14
_audit_creation_method           
;
Olex2 1.3-alpha
(compiled 2019.08.16 svn.r3652 for OlexSys, GUI svn.r5895)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C21 H15 Er8 Na4 O50, 9.6[H2O]'
_chemical_formula_sum            'C21 H15 Er8 Na4 O50'
_chemical_formula_weight         2497.37
_chemical_melting_point          ?
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'
Er Er -0.2586 4.9576 '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'

_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.
;
_space_group_crystal_system      tetragonal
_space_group_IT_number           87
_space_group_name_H-M_alt        'I 4/m'
_space_group_name_Hall           '-I 4'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x, z'
'-x, -y, z'
'y, -x, z'
'x+1/2, y+1/2, z+1/2'
'-y+1/2, x+1/2, z+1/2'
'-x+1/2, -y+1/2, z+1/2'
'y+1/2, -x+1/2, z+1/2'
'-x, -y, -z'
'y, -x, -z'
'x, y, -z'
'-y, x, -z'
'-x+1/2, -y+1/2, -z+1/2'
'y+1/2, -x+1/2, -z+1/2'
'x+1/2, y+1/2, -z+1/2'
'-y+1/2, x+1/2, -z+1/2'

_cell_length_a                   12.4441(2)
_cell_length_b                   12.4441(2)
_cell_length_c                   19.0521(5)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     2950.32(13)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    9954
_cell_measurement_temperature    296.0
_cell_measurement_theta_max      28.29
_cell_measurement_theta_min      3.15
_shelx_estimated_absorpt_T_max   0.299
_shelx_estimated_absorpt_T_min   0.234
_exptl_absorpt_coefficient_mu    11.385
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6162
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0638 before and 0.0410 after correction.
The Ratio of minimum to maximum transmission is 0.8263.
The λ/2 correction factor is Not present.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            pink
_exptl_crystal_colour_primary    pink
_exptl_crystal_density_diffrn    2.811
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             2258
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.14
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0287
_diffrn_reflns_av_unetI/netI     0.0131
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            20538
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.286
_diffrn_reflns_theta_min         3.152
_diffrn_ambient_temperature      296.0
_diffrn_detector                 'Bruker PHOTON 200 area detector'
_diffrn_detector_area_resol_mean 7.39
_diffrn_detector_type            'PHOTON II area detector'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device       'four-circle KAPPA diffractometer'
_diffrn_measurement_device_type  'BRUKER D8 QUEST CMOS PHOTON II'
_diffrn_measurement_method       'ω and φ scans'
_diffrn_radiation_collimation    '0.5 mm'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_xray_symbol    K-L~3~
_diffrn_source                   'sealed x-ray tube'
_diffrn_source_target            Cu
_diffrn_source_type              'Micro focus tube'
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                1706
_reflns_number_total             1891
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT V8.40A (?, 2016)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT V8.40A (?, 2016)'
_computing_molecular_graphics    'Olex2 1.3-alpha (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3-alpha (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL n/a (Sheldrick, 2008)'
_computing_structure_solution    'XT n/a (Sheldrick, 2015)'
_refine_diff_density_max         0.802
_refine_diff_density_min         -1.448
_refine_diff_density_rms         0.129
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.095
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     154
_refine_ls_number_reflns         1891
_refine_ls_number_restraints     22
_refine_ls_R_factor_all          0.0225
_refine_ls_R_factor_gt           0.0199
_refine_ls_restrained_S_all      1.102
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0050P)²+37.7606P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0417
_refine_ls_wR_factor_ref         0.0425
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2. Restrained distances
 O1-H1
 0.85 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
Uanis(O7) \\sim Ueq, Uanis(C4) \\sim Ueq: with sigma of 0.001 and sigma for
terminal atoms of 0.002
4. Rigid body (RIGU) restrains
 Na1, O7, C4
 with sigma for 1-2 distances of 0.0001 and sigma for 1-3 distances of 0.0001
5. Others
 Fixed Sof: O3A(0.5) O3B(0.5) O4A(0.5) O4B(0.5) O5A(0.5) O5B(0.5) O6A(0.5)
 O6B(0.5) O7(0.25) H7(0.125) C3A(0.5) C3B(0.5) C4(0.125) H4C(0.25) H4A(0.25)
 H4B(0.25)
 Fixed X: O7(0.436688) C4(0.5)
 Fixed Y: O7(0.563621) C4(0.5)
 Fixed Z: O7(0.5) C4(0.534289)
6.a Riding coordinates:
 O7(H7), C4(H4C,H4A,H4B)
;
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
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
Er1 Er 0.50001(2) 0.84720(2) 0.68412(2) 0.01562(6) Uani 1 1 d . . . . .
Na1 Na 0.5001(3) 0.7440(3) 0.500000 0.0516(8) Uani 1 2 d S T P A .
O1 O 0.5000(2) 0.8922(2) 0.80289(14) 0.0144(5) Uani 1 1 d D . . . .
H1 H 0.500(4) 0.833(2) 0.824(3) 0.035(15) Uiso 1 1 d D . . . .
O2 O 0.4999(3) 0.9109(2) 0.56959(15) 0.0269(7) Uani 1 1 d . . . . .
O3A O 0.4053(6) 0.7218(6) 0.6087(4) 0.0312(15) Uani 0.5 1 d . . P A -1
O3B O 0.3608(6) 0.7665(6) 0.6171(4) 0.0247(14) Uani 0.5 1 d . . P A -2
O4A O 0.2782(6) 0.5950(6) 0.6086(4) 0.0312(15) Uani 0.5 1 d . . P A -1
O4B O 0.2337(6) 0.6392(6) 0.6170(4) 0.0251(14) Uani 0.5 1 d . . P A -2
O5A O 0.3411(5) 0.7854(5) 0.7351(3) 0.0260(13) Uani 0.5 1 d . . P A -1
O5B O 0.4510(5) 0.6764(4) 0.7299(3) 0.0237(12) Uani 0.5 1 d . . P A -2
O6A O 0.2147(5) 0.6590(5) 0.7353(3) 0.0254(13) Uani 0.5 1 d . . P A -1
O6B O 0.3234(4) 0.5487(5) 0.7299(3) 0.0247(12) Uani 0.5 1 d . . P A -2
O7 O 0.436688 0.563621 0.500000 0.0487(15) Uani 0.25 1 d S U P A -3
H7 H 0.407900 0.530420 0.467860 0.073 Uiso 0.125 1 d R U P A -3
C1 C 0.500000 1.000000 0.5407(3) 0.0138(9) Uani 1 2 d S T P A .
C2 C 0.3220(4) 0.6778(4) 0.6381(2) 0.0289(9) Uani 1 1 d . . . . .
C3A C 0.2924(6) 0.7074(6) 0.7083(4) 0.0208(16) Uani 0.5 1 d . . P A -1
C3B C 0.3673(6) 0.6321(6) 0.7065(4) 0.0162(14) Uani 0.5 1 d . . P A -2
C4 C 0.500000 0.500000 0.534289 0.0468(15) Uani 0.125 1 d S U P A -3
H4C H 0.538570 0.455400 0.500000 0.070 Uiso 0.25 1 d R U P A -3
H4A H 0.550060 0.541770 0.561280 0.070 Uiso 0.25 1 d R U P A -3
H4B H 0.458370 0.455600 0.565310 0.070 Uiso 0.25 1 d R U P A -3


_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
Er1 Er1 3.6788(3) 14_466 ?
Er1 Er1 3.6787(3) 16_656 ?
Er1 Er1 3.8028(3) 3_675 ?
Er1 Na1 3.7356(12) . ?
Er1 O1 2.340(3) 16_656 ?
Er1 O1 2.341(3) 14_466 ?
Er1 O1 2.331(3) . ?
Er1 O2 2.321(3) . ?
Er1 O3A 2.426(7) . ?
Er1 O3B 2.374(6) . ?
Er1 O5A 2.333(6) . ?
Er1 O5B 2.377(5) . ?
Na1 O2 2.464(4) . ?
Na1 O2 2.464(4) 11_556 ?
Na1 O3A 2.399(7) . ?
Na1 O3B 2.840(8) . ?
Na1 O7 2.379(4) . ?
Na1 C4 3.106(3) . ?
O1 H1 0.846(10) . ?
O2 C1 1.238(4) . ?
O3A C2 1.300(8) . ?
O3B C2 1.270(8) . ?
O4A C2 1.295(8) . ?
O4B C2 1.266(8) . ?
O5A C3A 1.253(10) . ?
O5B C3B 1.261(9) . ?
O6A C3A 1.250(10) . ?
O6B C3B 1.255(9) . ?
O7 H7 0.8210 . ?
O7 C4 1.293942(17) . ?
C1 C1 1.552(10) 9_676 ?
C2 C3A 1.434(9) . ?
C2 C3B 1.529(9) . ?
C4 H4C 0.9824 . ?
C4 H4A 0.9606 . ?
C4 H4B 0.9607 . ?

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
Er1 Er1 Er1 62.245(5) 16_656 14_466 ?
Er1 Er1 Er1 58.878(3) 16_656 3_675 ?
Er1 Er1 Er1 58.878(3) 14_466 3_675 ?
Er1 Er1 Na1 144.95(6) 14_466 . ?
Er1 Er1 Na1 144.93(6) 16_656 . ?
Na1 Er1 Er1 110.11(5) . 3_675 ?
O1 Er1 Er1 78.71(6) 14_466 16_656 ?
O1 Er1 Er1 37.96(6) 14_466 14_466 ?
O1 Er1 Er1 37.96(6) 16_656 16_656 ?
O1 Er1 Er1 78.71(6) 16_656 14_466 ?
O1 Er1 Er1 35.66(6) 14_466 3_675 ?
O1 Er1 Er1 38.14(6) . 16_656 ?
O1 Er1 Er1 76.11(6) . 3_675 ?
O1 Er1 Er1 35.67(6) 16_656 3_675 ?
O1 Er1 Er1 38.13(6) . 14_466 ?
O1 Er1 Na1 173.77(8) . . ?
O1 Er1 Na1 112.25(8) 16_656 . ?
O1 Er1 Na1 112.26(8) 14_466 . ?
O1 Er1 O1 72.68(10) . 14_466 ?
O1 Er1 O1 69.97(10) 16_656 14_466 ?
O1 Er1 O1 72.68(10) . 16_656 ?
O1 Er1 O3A 149.71(18) 16_656 . ?
O1 Er1 O3A 107.8(2) 14_466 . ?
O1 Er1 O3A 136.82(18) . . ?
O1 Er1 O3B 89.0(2) 14_466 . ?
O1 Er1 O3B 128.54(19) . . ?
O1 Er1 O3B 144.96(17) 16_656 . ?
O1 Er1 O5A 71.04(16) . . ?
O1 Er1 O5B 146.58(15) 16_656 . ?
O1 Er1 O5B 122.73(17) 14_466 . ?
O1 Er1 O5B 81.86(16) . . ?
O2 Er1 Er1 117.73(8) . 16_656 ?
O2 Er1 Er1 117.71(7) . 14_466 ?
O2 Er1 Er1 70.05(7) . 3_675 ?
O2 Er1 Na1 40.07(8) . . ?
O2 Er1 O1 79.77(10) . 16_656 ?
O2 Er1 O1 79.75(10) . 14_466 ?
O2 Er1 O1 146.16(9) . . ?
O2 Er1 O3A 70.28(19) . . ?
O2 Er1 O3B 68.83(18) . . ?
O2 Er1 O5A 120.22(18) . . ?
O2 Er1 O5B 130.54(16) . . ?
O3A Er1 Er1 119.04(19) . 14_466 ?
O3A Er1 Er1 130.0(2) . 3_675 ?
O3A Er1 Er1 170.93(19) . 16_656 ?
O3A Er1 Na1 39.00(17) . . ?
O3B Er1 Na1 49.5(2) . . ?
O3B Er1 O5B 68.4(2) . . ?
O5A Er1 Er1 56.51(14) . 14_466 ?
O5A Er1 Er1 109.23(15) . 3_675 ?
O5A Er1 Er1 108.93(15) . 16_656 ?
O5A Er1 Na1 106.12(16) . . ?
O5A Er1 O1 74.79(16) . 14_466 ?
O5A Er1 O1 135.20(16) . 16_656 ?
O5A Er1 O3A 67.9(2) . . ?
O5B Er1 Na1 92.13(15) . . ?
Er1 Na1 Er1 139.77(10) 11_556 . ?
O2 Na1 Er1 102.44(11) . 11_556 ?
O2 Na1 Er1 37.33(6) 11_556 11_556 ?
O2 Na1 Er1 102.44(11) 11_556 . ?
O2 Na1 Er1 37.33(6) . . ?
O2 Na1 O2 65.11(15) 11_556 . ?
O2 Na1 O3B 109.8(2) 11_556 . ?
O2 Na1 O3B 59.56(16) . . ?
O2 Na1 C4 135.30(7) . . ?
O2 Na1 C4 159.59(9) 11_556 . ?
O3A Na1 Er1 39.54(17) . . ?
O3A Na1 Er1 148.2(3) . 11_556 ?
O3A Na1 O2 68.4(2) . . ?
O3A Na1 O2 124.1(3) . 11_556 ?
O3B Na1 Er1 134.73(18) . 11_556 ?
O3B Na1 Er1 39.46(13) . . ?
O7 Na1 Er1 108.93(5) . 11_556 ?
O7 Na1 Er1 108.93(5) . . ?
O7 Na1 O2 142.65(12) . . ?
O7 Na1 C4 22.72(3) . . ?
C4 Na1 Er1 97.97(4) . . ?
C4 Na1 Er1 122.26(6) . 11_556 ?
Er1 O1 Er1 108.67(10) 14_466 16_656 ?
Er1 O1 Er1 103.91(10) . 14_466 ?
Er1 O1 Er1 103.90(10) . 16_656 ?
Er1 O1 H1 117(4) 14_466 . ?
Er1 O1 H1 117(4) 16_656 . ?
Er1 O1 H1 105(4) . . ?
Er1 O2 Na1 102.60(11) . . ?
C1 O2 Er1 136.3(3) . . ?
C1 O2 Na1 121.1(3) . . ?
Na1 O3A Er1 101.5(3) . . ?
C2 O3A Er1 113.8(5) . . ?
C2 O3A Na1 144.4(5) . . ?
Er1 O3B Na1 91.1(2) . . ?
C2 O3B Er1 118.4(4) . . ?
C2 O3B Na1 113.2(5) . . ?
C3A O5A Er1 119.7(5) . . ?
C3B O5B Er1 118.3(5) . . ?
Na1 O7 H7 128.3 . . ?
C4 O7 Na1 112.04(8) . . ?
C4 O7 H7 109.5 . . ?
O2 C1 O2 127.3(5) . 3_675 ?
O2 C1 C1 116.4(2) . 9_676 ?
O2 C1 C1 116.4(2) 3_675 9_676 ?
O3A C2 C3A 119.9(6) . . ?
O3B C2 C3B 116.9(5) . . ?
O4A C2 O3A 118.9(6) . . ?
O4A C2 C3A 120.1(6) . . ?
O4B C2 O3B 124.1(6) . . ?
O4B C2 C3B 116.8(5) . . ?
O5A C3A C2 117.0(7) . . ?
O6A C3A O5A 125.4(7) . . ?
O6A C3A C2 117.3(7) . . ?
O5B C3B C2 116.3(6) . . ?
O6B C3B O5B 126.6(7) . . ?
O6B C3B C2 116.8(6) . . ?
Na1 C4 H4C 114.3 . . ?
Na1 C4 H4A 65.4 . . ?
Na1 C4 H4B 133.8 . . ?
O7 C4 Na1 45.24(6) . . ?
O7 C4 H4C 107.9 . . ?
O7 C4 H4A 109.5 . . ?
O7 C4 H4B 109.5 . . ?
H4C C4 H4A 110.2 . . ?
H4C C4 H4B 110.3 . . ?
H4A C4 H4B 109.4 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Er1 O2 C1 O2 0.0(2) . . . 3_675 ?
Er1 O2 C1 C1 180.0(2) . . . 9_676 ?
Er1 O3A C2 O4A -166.5(6) . . . . ?
Er1 O3A C2 C3A 1.7(8) . . . . ?
Er1 O3B C2 O4B 163.6(6) . . . . ?
Er1 O3B C2 C3B 1.5(8) . . . . ?
Er1 O5A C3A O6A 170.6(6) . . . . ?
Er1 O5A C3A C2 -15.4(9) . . . . ?
Er1 O5B C3B O6B -171.4(6) . . . . ?
Er1 O5B C3B C2 15.6(8) . . . . ?
Na1 O2 C1 O2 -179.9(3) . . . 3_675 ?
Na1 O2 C1 C1 0.1(3) . . . 9_676 ?
Na1 O3A C2 O4A 22.7(14) . . . . ?
Na1 O3A C2 C3A -169.1(8) . . . . ?
Na1 O3B C2 O4B -91.7(8) . . . . ?
Na1 O3B C2 C3B 106.3(5) . . . . ?
O3A C2 C3A O5A 8.9(10) . . . . ?
O3A C2 C3A O6A -176.7(7) . . . . ?
O3B C2 C3B O5B -11.5(10) . . . . ?
O3B C2 C3B O6B 174.8(7) . . . . ?
O4A C2 C3A O5A 176.9(7) . . . . ?
O4A C2 C3A O6A -8.7(10) . . . . ?
O4B C2 C3B O5B -174.9(7) . . . . ?
O4B C2 C3B O6B 11.4(10) . . . . ?

_smtbx_masks_special_details     ?
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 0.000 0.000 0.500 391.4 100.4 '9.6 water'
2 0.500 0.500 0.000 391.4 100.4 '9.6 water'

_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# 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_1tb
_database_code_depnum_ccdc_archive 'CCDC 1976171'
loop_
_audit_author_name
_audit_author_address
'Kittipong Chainok'
;Thammasat University
Thailand
;
_audit_update_record             
;
2020-01-07 deposited with the CCDC.	2020-06-23 downloaded from the CCDC.
;
_audit_creation_date             2020-01-08
_audit_creation_method           
;
Olex2 1.3
(compiled Nov 21 2019 18:26:39 for OlexSys, GUI svn.r6003)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C10.25 H4 Na2 O25 Tb4, 2.5(O)'
_chemical_formula_sum            'C10.25 H4 Na2 O27.50 Tb4'
_chemical_formula_weight         1248.79
_chemical_melting_point          ?
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'
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'
Tb Tb -0.1723 4.1537 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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.
;
_space_group_crystal_system      tetragonal
_space_group_IT_number           87
_space_group_name_H-M_alt        'I 4/m'
_space_group_name_Hall           '-I 4'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z'
'-y, x, z'
'y, -x, z'
'x+1/2, y+1/2, z+1/2'
'-x+1/2, -y+1/2, z+1/2'
'-y+1/2, x+1/2, z+1/2'
'y+1/2, -x+1/2, z+1/2'
'-x, -y, -z'
'x, y, -z'
'y, -x, -z'
'-y, x, -z'
'-x+1/2, -y+1/2, -z+1/2'
'x+1/2, y+1/2, -z+1/2'
'y+1/2, -x+1/2, -z+1/2'
'-y+1/2, x+1/2, -z+1/2'

_cell_length_a                   12.5792(4)
_cell_length_b                   12.5792(4)
_cell_length_c                   19.2471(8)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     3045.6(2)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    6455
_cell_measurement_temperature    296.0
_cell_measurement_theta_max      25.981
_cell_measurement_theta_min      3.119
_shelx_estimated_absorpt_T_max   0.214
_shelx_estimated_absorpt_T_min   0.180
_exptl_absorpt_coefficient_mu    9.305
_exptl_absorpt_correction_T_max  0.7453
_exptl_absorpt_correction_T_min  0.6129
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.2024 before and 0.0611 after correction.
The Ratio of minimum to maximum transmission is 0.8224.
The λ/2 correction factor is Not present.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.724
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             2270
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.24
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0693
_diffrn_reflns_av_unetI/netI     0.0250
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            20225
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.042
_diffrn_reflns_theta_min         3.239
_diffrn_ambient_temperature      296.0
_diffrn_detector                 'Bruker PHOTON 200 area detector'
_diffrn_detector_area_resol_mean 7.39
_diffrn_detector_type            'PHOTON II area detector'
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device       'four-circle KAPPA diffractometer'
_diffrn_measurement_device_type  'Bruker D8 QUEST CMOS'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_collimation    '0.5 mm'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_xray_symbol    K-L~3~
_diffrn_source                   'sealed x-ray tube'
_diffrn_source_current           30.0
_diffrn_source_power             1.5
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                1355
_reflns_number_total             1553
_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. Completness statistics refer to single and
 composite reflections containing twin component 1 only.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT V8.40A (?, 2016)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT V8.40A (?, 2016)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_refine_diff_density_max         1.845
_refine_diff_density_min         -1.061
_refine_diff_density_rms         0.266
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.255
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     157
_refine_ls_number_reflns         1553
_refine_ls_number_restraints     176
_refine_ls_R_factor_all          0.0524
_refine_ls_R_factor_gt           0.0439
_refine_ls_restrained_S_all      1.257
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0208P)²+184.9491P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1022
_refine_ls_wR_factor_ref         0.1050
_refine_special_details          
;
 Refined as a 2-component twin.
;
_olex2_refinement_description    
;
1. Twinned data refinement
 Scales: 0.499(4)
 0.501(4)
2. Restrained distances
 O1-H1
 0.82 with sigma of 0.001
 Tb1_$2-H1
 2.9 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(O3A) \\sim Ueq, Uanis(O4A) \\sim Ueq, Uanis(O6A) \\sim Ueq, Uanis(C3A)
\\sim Ueq, Uanis(O5A) \\sim Ueq, Uanis(C2) \\sim Ueq: with sigma of 0.001 and
sigma for terminal atoms of 0.002
Uanis(O3B) \\sim Ueq, Uanis(C2) \\sim Ueq, Uanis(O4B) \\sim Ueq, Uanis(C3B)
\\sim Ueq, Uanis(O5B) \\sim Ueq, Uanis(O6B) \\sim Ueq: with sigma of 0.001 and
sigma for terminal atoms of 0.002
Uanis(O3) \\sim Ueq, Uanis(C1) \\sim Ueq: with sigma of 0.001 and sigma for
terminal atoms of 0.002
Uanis(O2) \\sim Ueq, Uanis(C3) \\sim Ueq: with sigma of 0.001 and sigma for
terminal atoms of 0.002
Uanis(Tb1) \\sim Ueq, Uanis(O1) \\sim Ueq: with sigma of 0.001 and sigma for
terminal atoms of 0.002
4. Rigid body (RIGU) restrains
 O3A, O4A, O5A, O6A, C2, C3A
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 O3B, O4B, O5B, O6B, C2, C3B
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 O2, C3
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 O3, C1
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
5. Others
 Fixed Sof: O3(0.25) O3A(0.5) O3B(0.5) O4(0.5) O4A(0.5) O4B(0.5) O5(0.125)
 O5A(0.5) O5B(0.5) O6A(0.5) O6B(0.5) C1(0.0625) C3A(0.5) C3B(0.5)
;
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
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
Tb1 Tb 0.99427(8) 0.65344(4) 0.31578(3) 0.01556(18) Uani 1 1 d . U . . .
Na1 Na 1.0050(18) 0.7514(7) 0.500000 0.045(3) Uani 1 2 d S T P . .
O1 O 1.1079(6) 0.4990(11) 0.3033(4) 0.0128(16) Uani 1 1 d D U . . .
H1 H 1.167(3) 0.511(4) 0.319(4) 0.7(8) Uiso 1 1 d D . . . .
O2 O 0.9874(9) 0.5878(7) 0.4311(4) 0.0154(17) Uani 1 1 d . U . . .
O3 O 1.064(6) 0.940(6) 0.500000 0.072(3) Uani 0.5 2 d S TU P A .
O3A O 0.859(2) 0.734(2) 0.3804(13) 0.0165(18) Uani 0.5 1 d . U P A -1
O3B O 0.891(2) 0.766(2) 0.3909(15) 0.0175(19) Uani 0.5 1 d . U P A -2
O4 O 1.282(3) 0.536(3) 0.3965(17) 0.064(10) Uiso 0.5 1 d . . P . .
O4A O 0.748(2) 0.871(2) 0.3907(14) 0.016(2) Uani 0.5 1 d . U P A -1
O4B O 0.774(2) 0.906(2) 0.3904(15) 0.018(2) Uani 0.5 1 d . U P A -2
O5 O 1.000000 1.000000 0.160(8) 0.23(6) Uiso 0.5 4 d S . P . .
O5A O 0.9525(17) 0.8289(18) 0.2787(12) 0.017(2) Uani 0.5 1 d . U P A -1
O5B O 0.8259(16) 0.7093(16) 0.2667(11) 0.016(2) Uani 0.5 1 d . U P A -2
O6A O 0.8232(18) 0.9481(17) 0.2644(12) 0.018(2) Uani 0.5 1 d . U P A -1
O6B O 0.7194(16) 0.8511(17) 0.2578(12) 0.015(2) Uani 0.5 1 d . U P A -2
C1 C 1.000000 1.000000 0.500000 0.0714(18) Uani 0.5 8 d S TU P A .
C2 C 0.8170(14) 0.8246(13) 0.3622(6) 0.0169(13) Uani 1 1 d . U . . .
C3 C 1.000000 0.500000 0.4599(8) 0.014(2) Uani 1 2 d S TU P . .
C3A C 0.865(3) 0.876(3) 0.2948(12) 0.0168(17) Uani 0.5 1 d . U P A -1
C3B C 0.788(3) 0.793(3) 0.2888(12) 0.0165(17) Uani 0.5 1 d . U P A -2


_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
Tb1 O1 2.321(12) 2_765 ?
Tb1 O1 2.364(7) 16_645 ?
Tb1 O1 2.424(13) . ?
Tb1 O2 2.370(8) . ?
Tb1 O3A 2.34(2) . ?
Tb1 O3B 2.40(3) . ?
Tb1 O5A 2.38(2) . ?
Tb1 O5B 2.42(2) . ?
Na1 Na1 0.00000(10) 10_556 ?
Na1 O2 2.458(11) . ?
Na1 O2 2.458(11) 10_556 ?
Na1 O3 2.49(9) . ?
Na1 O3 2.46(9) 11_576 ?
Na1 O3A 2.95(3) . ?
Na1 O3B 2.55(3) . ?
Na1 C1 3.128(10) . ?
O1 H1 0.8200(11) . ?
O2 C3 1.246(11) . ?
O3 O3 1.56(6) 3_755 ?
O3 O3 1.56(6) 11_576 ?
O3 C1 1.10(4) . ?
O3A C2 1.31(3) . ?
O3B C2 1.31(3) . ?
O4A C2 1.18(3) . ?
O4B C2 1.28(3) . ?
O5A C3A 1.28(4) . ?
O5B C3B 1.23(5) . ?
O6A C3A 1.20(4) . ?
O6B C3B 1.28(5) . ?
C2 C3A 1.57(3) . ?
C2 C3B 1.51(3) . ?
C3 C3 1.54(3) 9_766 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Tb1 O1 73.7(4) 2_765 16_645 ?
O1 Tb1 O1 71.9(3) 16_645 . ?
O1 Tb1 O1 69.8(3) 2_765 . ?
O1 Tb1 O2 77.8(3) 2_765 . ?
O1 Tb1 O2 145.6(3) 16_645 . ?
O1 Tb1 O3A 90.6(7) 2_765 . ?
O1 Tb1 O3B 138.2(7) 16_645 . ?
O1 Tb1 O3B 104.4(8) 2_765 . ?
O1 Tb1 O5A 127.8(6) 2_765 . ?
O1 Tb1 O5A 86.7(6) 16_645 . ?
O1 Tb1 O5B 73.4(6) 2_765 . ?
O1 Tb1 O5B 73.9(6) 16_645 . ?
O2 Tb1 O1 80.5(3) . . ?
O2 Tb1 O3B 67.7(7) . . ?
O2 Tb1 O5A 126.6(6) . . ?
O2 Tb1 O5B 115.7(6) . . ?
O3A Tb1 O1 130.3(7) . 16_645 ?
O3A Tb1 O1 146.0(6) . . ?
O3A Tb1 O2 68.0(7) . . ?
O3A Tb1 O5A 66.2(8) . . ?
O3B Tb1 O1 148.1(7) . . ?
O3B Tb1 O5B 65.9(9) . . ?
O5A Tb1 O1 147.6(6) . . ?
O5B Tb1 O1 135.2(5) . . ?
Na1 Na1 Tb1 0(10) 10_556 10_556 ?
Na1 Na1 O2 0(10) 10_556 10_556 ?
Na1 Na1 O2 0(10) 10_556 . ?
Na1 Na1 O3 0(10) 10_556 11_576 ?
Na1 Na1 O3 0(10) 10_556 . ?
Na1 Na1 O3A 0(10) 10_556 . ?
Na1 Na1 O3B 0(10) 10_556 . ?
Na1 Na1 C1 0.0(9) 10_556 . ?
O2 Na1 Tb1 103.4(3) . 10_556 ?
O2 Na1 Tb1 38.09(19) 10_556 10_556 ?
O2 Na1 O2 65.3(4) . 10_556 ?
O2 Na1 O3 139.5(10) 10_556 11_576 ?
O2 Na1 O3 139.5(10) . 11_576 ?
O2 Na1 O3 145.7(5) . . ?
O2 Na1 O3 145.7(5) 10_556 . ?
O2 Na1 O3A 57.4(6) . . ?
O2 Na1 O3A 107.6(7) 10_556 . ?
O2 Na1 O3B 116.9(9) 10_556 . ?
O2 Na1 O3B 64.1(7) . . ?
O2 Na1 C1 146.6(3) 10_556 . ?
O2 Na1 C1 146.6(3) . . ?
O3 Na1 Tb1 107.3(3) 11_576 10_556 ?
O3 Na1 Tb1 108.89(17) . 10_556 ?
O3 Na1 O3 36.7(17) 11_576 . ?
O3 Na1 O3A 104.8(10) . . ?
O3 Na1 O3A 82.2(10) 11_576 . ?
O3 Na1 O3B 75.4(11) 11_576 . ?
O3 Na1 O3B 95.8(11) . . ?
O3 Na1 C1 18.5(13) . . ?
O3 Na1 C1 18.2(13) 11_576 . ?
O3A Na1 Tb1 133.6(8) . 10_556 ?
O3A Na1 C1 93.5(6) . . ?
O3B Na1 Tb1 141.3(10) . 10_556 ?
O3B Na1 C1 85.3(8) . . ?
C1 Na1 Tb1 109.10(15) . 10_556 ?
Tb1 O1 Tb1 109.0(3) 2_765 . ?
Tb1 O1 Tb1 105.3(4) 2_765 15_565 ?
Tb1 O1 Tb1 102.1(4) 15_565 . ?
Tb1 O1 H1 111(4) . . ?
Tb1 O1 H1 128(3) 2_765 . ?
Tb1 O1 H1 98(5) 15_565 . ?
Tb1 O2 Na1 102.1(3) . . ?
Tb1 O2 Na1 102.1(3) . 10_556 ?
Na1 O2 Na1 0.000(2) 10_556 . ?
C3 O2 Tb1 136.1(8) . . ?
C3 O2 Na1 119.4(8) . . ?
C3 O2 Na1 119.4(8) . 10_556 ?
Na1 O3 Na1 126.7(17) 3_755 10_556 ?
Na1 O3 Na1 126.7(17) 3_755 . ?
Na1 O3 Na1 0.0(10) . 10_556 ?
O3 O3 Na1 161(6) 3_755 10_556 ?
O3 O3 Na1 71(6) 11_576 10_556 ?
O3 O3 Na1 71(6) 11_576 . ?
O3 O3 Na1 163(6) 11_576 3_755 ?
O3 O3 Na1 161(6) 3_755 . ?
O3 O3 Na1 73(6) 3_755 3_755 ?
O3 O3 O3 89.999(17) 11_576 3_755 ?
C1 O3 Na1 116(6) . 10_556 ?
C1 O3 Na1 116(6) . . ?
C1 O3 Na1 118(6) . 3_755 ?
C1 O3 O3 45.001(19) . 11_576 ?
C1 O3 O3 44.998(3) . 3_755 ?
Tb1 O3A Na1 89.8(9) . . ?
C2 O3A Tb1 122.2(16) . . ?
C2 O3A Na1 113.4(15) . . ?
Tb1 O3B Na1 98.7(10) . . ?
C2 O3B Tb1 117.5(18) . . ?
C2 O3B Na1 142(2) . . ?
C3A O5A Tb1 123.0(18) . . ?
C3B O5B Tb1 116.8(19) . . ?
Na1 C1 Na1 89.999(2) 11_576 . ?
Na1 C1 Na1 90.000(1) 9_776 11_576 ?
Na1 C1 Na1 180.0(8) 9_776 . ?
Na1 C1 Na1 90.001(1) 3_755 10_556 ?
Na1 C1 Na1 180.0 3_755 11_576 ?
Na1 C1 Na1 89.999(2) 11_576 10_556 ?
Na1 C1 Na1 90.001(1) 3_755 . ?
Na1 C1 Na1 0.000(7) . 10_556 ?
Na1 C1 Na1 180.0(8) 9_776 10_556 ?
Na1 C1 Na1 90.000(1) 9_776 3_755 ?
O3 C1 Na1 134(5) . 9_776 ?
O3 C1 Na1 136(5) 9_776 3_755 ?
O3 C1 Na1 136(5) 3_755 10_556 ?
O3 C1 Na1 44(5) 9_776 11_576 ?
O3 C1 Na1 46(5) . 10_556 ?
O3 C1 Na1 136(5) . 11_576 ?
O3 C1 Na1 46(5) 9_776 9_776 ?
O3 C1 Na1 134(5) 11_576 3_755 ?
O3 C1 Na1 44(5) . 3_755 ?
O3 C1 Na1 46(5) 3_755 3_755 ?
O3 C1 Na1 44(5) 11_576 10_556 ?
O3 C1 Na1 136(5) 3_755 . ?
O3 C1 Na1 134(5) 9_776 10_556 ?
O3 C1 Na1 134(5) 9_776 . ?
O3 C1 Na1 46(5) . . ?
O3 C1 Na1 136(5) 11_576 9_776 ?
O3 C1 Na1 44(5) 3_755 9_776 ?
O3 C1 Na1 46(5) 11_576 11_576 ?
O3 C1 Na1 134(5) 3_755 11_576 ?
O3 C1 Na1 44(5) 11_576 . ?
O3 C1 O3 90.00(4) 3_755 . ?
O3 C1 O3 89.998(3) 11_576 . ?
O3 C1 O3 90.00(5) 11_576 9_776 ?
O3 C1 O3 180(6) 9_776 . ?
O3 C1 O3 180.00(2) 11_576 3_755 ?
O3 C1 O3 90.000(1) 3_755 9_776 ?
O3A C2 C3A 115(2) . . ?
O3B C2 C3B 115(3) . . ?
O4A C2 O3A 127.2(16) . . ?
O4A C2 C3A 118(2) . . ?
O4B C2 O3B 125.2(16) . . ?
O4B C2 C3B 120(3) . . ?
O2 C3 O2 127.2(15) . 2_765 ?
O2 C3 C3 116.4(7) . 9_766 ?
O2 C3 C3 116.4(7) 2_765 9_766 ?
O5A C3A C2 110(2) . . ?
O6A C3A O5A 127(2) . . ?
O6A C3A C2 123(3) . . ?
O5B C3B O6B 126(2) . . ?
O5B C3B C2 117(3) . . ?
O6B C3B C2 117(3) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Tb1 O2 C3 O2 -7.1(7) . . . 2_765 ?
Tb1 O2 C3 C3 172.9(7) . . . 9_766 ?
Tb1 O3A C2 O4A 179(2) . . . . ?
Tb1 O3A C2 C3A -1(3) . . . . ?
Tb1 O3B C2 O4B -162(2) . . . . ?
Tb1 O3B C2 C3B 15(3) . . . . ?
Tb1 O5A C3A O6A -157(2) . . . . ?
Tb1 O5A C3A C2 22(3) . . . . ?
Tb1 O5B C3B O6B 159(2) . . . . ?
Tb1 O5B C3B C2 -28(3) . . . . ?
Na1 O2 C3 O2 -166.2(10) . . . 2_765 ?
Na1 O2 C3 O2 -166.2(10) 10_556 . . 2_765 ?
Na1 O2 C3 C3 13.8(10) 10_556 . . 9_766 ?
Na1 O2 C3 C3 13.8(10) . . . 9_766 ?
Na1 O3 C1 Na1 180.0 10_556 . . 3_755 ?
Na1 O3 C1 Na1 0.0 . . . 11_576 ?
Na1 O3 C1 Na1 0.0 10_556 . . 11_576 ?
Na1 O3 C1 Na1 180.0 3_755 . . 11_576 ?
Na1 O3 C1 Na1 180.0 . . . 9_776 ?
Na1 O3 C1 Na1 180.0 3_755 . . 10_556 ?
Na1 O3 C1 Na1 0.0 . . . 10_556 ?
Na1 O3 C1 Na1 0.0 3_755 . . 9_776 ?
Na1 O3 C1 Na1 180.0 . . . 3_755 ?
Na1 O3 C1 Na1 180.0 10_556 . . 9_776 ?
Na1 O3 C1 Na1 0.0 10_556 . . . ?
Na1 O3 C1 Na1 180.0 3_755 . . . ?
Na1 O3 C1 O3 0.0 3_755 . . 3_755 ?
Na1 O3 C1 O3 180.0 10_556 . . 3_755 ?
Na1 O3 C1 O3 0.0 10_556 . . 11_576 ?
Na1 O3 C1 O3 180.0 3_755 . . 11_576 ?
Na1 O3 C1 O3 0.0 . . . 11_576 ?
Na1 O3 C1 O3 180.0 . . . 3_755 ?
Na1 O3A C2 O4A -76(2) . . . . ?
Na1 O3A C2 C3A 104.3(16) . . . . ?
Na1 O3B C2 O4B -3(4) . . . . ?
Na1 O3B C2 C3B 174(2) . . . . ?
O3 O3 C1 Na1 180.0 11_576 . . 3_755 ?
O3 O3 C1 Na1 180.0 3_755 . . . ?
O3 O3 C1 Na1 0.0 11_576 . . 10_556 ?
O3 O3 C1 Na1 180.0 11_576 . . 9_776 ?
O3 O3 C1 Na1 0.0 11_576 . . 11_576 ?
O3 O3 C1 Na1 0.0 3_755 . . 9_776 ?
O3 O3 C1 Na1 0.0 3_755 . . 3_755 ?
O3 O3 C1 Na1 0.0 11_576 . . . ?
O3 O3 C1 Na1 180.0 3_755 . . 11_576 ?
O3 O3 C1 Na1 180.0 3_755 . . 10_556 ?
O3 O3 C1 O3 180.0 11_576 . . 3_755 ?
O3 O3 C1 O3 180.0 3_755 . . 11_576 ?
O3A C2 C3A O5A -13(3) . . . . ?
O3A C2 C3A O6A 166(2) . . . . ?
O3B C2 C3B O5B 9(3) . . . . ?
O3B C2 C3B O6B -177(2) . . . . ?
O4A C2 C3A O5A 167(2) . . . . ?
O4A C2 C3A O6A -14(3) . . . . ?
O4B C2 C3B O5B -174(2) . . . . ?
O4B C2 C3B O6B 0(3) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.499(4)
2 0.501(4)

####################################################################### 
# 
# 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_2dy
_database_code_depnum_ccdc_archive 'CCDC 1976172'
loop_
_audit_author_name
_audit_author_address
'Kittipong Chainok'
;Thammasat University
Thailand
;
_audit_update_record             
;
2020-01-07 deposited with the CCDC.	2020-06-23 downloaded from the CCDC.
;
_audit_creation_date             2020-01-08
_audit_creation_method           
;
Olex2 1.3
(compiled Nov 21 2019 18:26:39 for OlexSys, GUI svn.r6003)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C10.25 H4 Dy4 Na2 O25, 2.5(O)'
_chemical_formula_sum            'C10.25 H4 Dy4 Na2 O27.50'
_chemical_formula_weight         1263.11
_chemical_melting_point          ?
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'
Dy Dy -0.1892 4.4098 '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'

_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.
;
_space_group_crystal_system      tetragonal
_space_group_IT_number           87
_space_group_name_H-M_alt        'I 4/m'
_space_group_name_Hall           '-I 4'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z'
'-y, x, z'
'y, -x, z'
'x+1/2, y+1/2, z+1/2'
'-x+1/2, -y+1/2, z+1/2'
'-y+1/2, x+1/2, z+1/2'
'y+1/2, -x+1/2, z+1/2'
'-x, -y, -z'
'x, y, -z'
'y, -x, -z'
'-y, x, -z'
'-x+1/2, -y+1/2, -z+1/2'
'x+1/2, y+1/2, -z+1/2'
'y+1/2, -x+1/2, -z+1/2'
'-y+1/2, x+1/2, -z+1/2'

_cell_length_a                   12.5277(3)
_cell_length_b                   12.5277(3)
_cell_length_c                   19.1754(8)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     3009.45(19)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    5000
_cell_measurement_temperature    296.0
_cell_measurement_theta_max      26.38
_cell_measurement_theta_min      3.13
_shelx_estimated_absorpt_T_max   0.199
_shelx_estimated_absorpt_T_min   0.167
_exptl_absorpt_coefficient_mu    9.948
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.5446
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0997 before and 0.0541 after correction.
The Ratio of minimum to maximum transmission is 0.7306.
The λ/2 correction factor is Not present.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.788
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             2286
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.24
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0479
_diffrn_reflns_av_unetI/netI     0.0257
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            13464
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.378
_diffrn_reflns_theta_min         3.131
_diffrn_ambient_temperature      296.0
_diffrn_detector                 'Bruker PHOTON 200 area detector'
_diffrn_detector_area_resol_mean 7.39
_diffrn_detector_type            'PHOTON II area detector'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device       'four-circle KAPPA diffractometer'
_diffrn_measurement_device_type  'BRUKER D8 QUEST CMOS PHOTON II'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_collimation    '0.5 mm'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_xray_symbol    K-L~3~
_diffrn_source                   'sealed x-ray tube'
_diffrn_source_current           30.0
_diffrn_source_power             1.5
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                1377
_reflns_number_total             1602
_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. Completness statistics refer to single and
 composite reflections containing twin component 1 only.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       ?
_computing_data_collection       ?
_computing_data_reduction        ?
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_refine_diff_density_max         1.663
_refine_diff_density_min         -0.795
_refine_diff_density_rms         0.222
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.104
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     157
_refine_ls_number_reflns         1602
_refine_ls_number_restraints     176
_refine_ls_R_factor_all          0.0390
_refine_ls_R_factor_gt           0.0309
_refine_ls_restrained_S_all      1.100
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0387P)²+56.7143P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0789
_refine_ls_wR_factor_ref         0.0824
_refine_special_details          
;
 Refined as a 2-component twin.
;
_olex2_refinement_description    
;
1. Twinned data refinement
 Scales: 0.478(2)
 0.522(2)
2. Restrained distances
 O1-H1
 0.82 with sigma of 0.001
 Dy1_$2-H1
 2.9 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(O3A) \\sim Ueq, Uanis(O4A) \\sim Ueq, Uanis(O6A) \\sim Ueq, Uanis(C3A)
\\sim Ueq, Uanis(O5A) \\sim Ueq, Uanis(C2) \\sim Ueq: with sigma of 0.001 and
sigma for terminal atoms of 0.002
Uanis(O3B) \\sim Ueq, Uanis(C2) \\sim Ueq, Uanis(O4B) \\sim Ueq, Uanis(C3B)
\\sim Ueq, Uanis(O5B) \\sim Ueq, Uanis(O6B) \\sim Ueq: with sigma of 0.001 and
sigma for terminal atoms of 0.002
Uanis(O3) \\sim Ueq, Uanis(C1) \\sim Ueq: with sigma of 0.001 and sigma for
terminal atoms of 0.002
Uanis(O2) \\sim Ueq, Uanis(C3) \\sim Ueq: with sigma of 0.001 and sigma for
terminal atoms of 0.002
Uanis(Dy1) \\sim Ueq, Uanis(O1) \\sim Ueq: with sigma of 0.001 and sigma for
terminal atoms of 0.002
4. Rigid body (RIGU) restrains
 O3A, O4A, O5A, O6A, C2, C3A
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 O3B, O4B, O5B, O6B, C2, C3B
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 O2, C3
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 O3, C1
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
5. Others
 Fixed Sof: O3(0.25) O3A(0.5) O3B(0.5) O4(0.5) O4A(0.5) O4B(0.5) O5(0.125)
 O5A(0.5) O5B(0.5) O6A(0.5) O6B(0.5) C1(0.0625) C3A(0.5) C3B(0.5)
;
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
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
Dy1 Dy 0.99128(4) 0.65302(3) 0.31579(2) 0.01495(14) Uani 1 1 d . U . . .
Na1 Na 1.0001(12) 0.7553(5) 0.500000 0.0517(18) Uani 1 2 d S T P . .
O1 O 1.1076(4) 0.5044(6) 0.3027(3) 0.0136(11) Uani 1 1 d D U . . .
H1 H 1.151(3) 0.528(3) 0.3306(16) 0.04(3) Uiso 1 1 d D . . . .
O2 O 0.9887(6) 0.5879(5) 0.4312(3) 0.0206(12) Uani 1 1 d . U . . .
O3 O 1.067(3) 0.932(3) 0.500000 0.075(3) Uani 0.5 2 d S TU P A .
O3A O 0.8559(13) 0.7378(13) 0.3830(9) 0.0197(16) Uani 0.5 1 d . U P A -1
O3B O 0.8893(14) 0.7720(14) 0.3895(10) 0.0206(16) Uani 0.5 1 d . U P A -2
O4 O 1.285(2) 0.526(2) 0.3945(12) 0.084(8) Uiso 0.5 1 d . . P . .
O4A O 0.7378(13) 0.8727(14) 0.3884(9) 0.0210(19) Uani 0.5 1 d . U P A -1
O4B O 0.7737(15) 0.9095(14) 0.3926(10) 0.023(2) Uani 0.5 1 d . U P A -2
O5 O 1.000000 1.000000 0.162(5) 0.23(4) Uiso 0.5 4 d S . P . .
O5A O 0.9448(11) 0.8281(12) 0.2704(9) 0.0205(17) Uani 0.5 1 d . U P A -1
O5B O 0.8324(12) 0.7142(11) 0.2632(9) 0.0208(17) Uani 0.5 1 d . U P A -2
O6A O 0.8238(12) 0.9576(11) 0.2722(9) 0.0209(19) Uani 0.5 1 d . U P A -1
O6B O 0.7152(11) 0.8477(12) 0.2612(9) 0.0218(19) Uani 0.5 1 d . U P A -2
C1 C 1.000000 1.000000 0.500000 0.0749(18) Uani 0.5 8 d S TU P A .
C2 C 0.8171(8) 0.8288(8) 0.3622(4) 0.0197(9) Uani 1 1 d . U . . .
C3 C 1.000000 0.500000 0.4598(6) 0.0161(16) Uani 1 2 d S TU P . .
C3A C 0.8649(16) 0.8749(16) 0.2939(9) 0.0192(14) Uani 0.5 1 d . U P A -1
C3B C 0.7885(18) 0.7936(17) 0.2880(8) 0.0198(14) Uani 0.5 1 d . U P A -2


_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
Dy1 O1 2.343(5) 16_645 ?
Dy1 O1 2.343(7) 2_765 ?
Dy1 O1 2.378(7) . ?
Dy1 H1 2.56(5) . ?
Dy1 O2 2.358(6) . ?
Dy1 O3A 2.380(16) . ?
Dy1 O3B 2.419(16) . ?
Dy1 O5A 2.430(15) . ?
Dy1 O5B 2.360(15) . ?
Na1 Na1 0.000(13) 10_556 ?
Na1 O2 2.482(8) . ?
Na1 O2 2.482(8) 10_556 ?
Na1 O3 2.37(5) . ?
Na1 O3 2.38(5) 11_576 ?
Na1 O3A 2.89(2) . ?
Na1 O3B 2.54(2) . ?
Na1 C1 3.065(6) . ?
O1 H1 0.8200(11) . ?
O2 C3 1.239(7) . ?
O3 O3 1.69(4) 3_755 ?
O3 O3 1.69(4) 11_576 ?
O3 C1 1.20(3) . ?
O3A C2 1.302(19) . ?
O3B C2 1.265(19) . ?
O4A C2 1.242(19) . ?
O4B C2 1.29(2) . ?
O5A C3A 1.25(3) . ?
O5B C3B 1.23(3) . ?
O6A C3A 1.23(3) . ?
O6B C3B 1.25(3) . ?
C2 C3A 1.551(18) . ?
C2 C3B 1.532(18) . ?
C3 C3 1.54(2) 9_766 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Dy1 O1 72.8(2) 16_645 2_765 ?
O1 Dy1 O1 72.1(2) 16_645 . ?
O1 Dy1 O1 69.7(2) 2_765 . ?
O1 Dy1 H1 86.6(8) 16_645 . ?
O1 Dy1 H1 84.8(5) 2_765 . ?
O1 Dy1 H1 18.6(5) . . ?
O1 Dy1 O2 78.6(2) 2_765 . ?
O1 Dy1 O2 145.7(2) 16_645 . ?
O1 Dy1 O3A 130.5(4) 16_645 . ?
O1 Dy1 O3A 147.5(4) . . ?
O1 Dy1 O3A 93.3(5) 2_765 . ?
O1 Dy1 O3B 150.2(4) . . ?
O1 Dy1 O3B 136.7(5) 16_645 . ?
O1 Dy1 O3B 107.6(5) 2_765 . ?
O1 Dy1 O5A 126.5(4) 2_765 . ?
O1 Dy1 O5A 144.6(4) . . ?
O1 Dy1 O5A 82.9(4) 16_645 . ?
O1 Dy1 O5B 77.4(4) 2_765 . ?
O1 Dy1 O5B 71.5(4) 16_645 . ?
O2 Dy1 O1 80.6(2) . . ?
O2 Dy1 H1 72.2(8) . . ?
O2 Dy1 O3A 68.7(4) . . ?
O2 Dy1 O3B 70.0(4) . . ?
O2 Dy1 O5A 130.2(4) . . ?
O2 Dy1 O5B 120.1(4) . . ?
O3A Dy1 H1 140.4(9) . . ?
O3A Dy1 O5A 67.7(6) . . ?
O3B Dy1 H1 136.5(8) . . ?
O5A Dy1 H1 141.3(7) . . ?
O5B Dy1 O1 136.6(4) . . ?
O5B Dy1 H1 155.0(6) . . ?
O5B Dy1 O3B 66.7(6) . . ?
Na1 Na1 Dy1 0(10) 10_556 10_556 ?
Na1 Na1 O2 0(10) 10_556 10_556 ?
Na1 Na1 O2 0(10) 10_556 . ?
Na1 Na1 O3 0(10) 10_556 . ?
Na1 Na1 O3 0(10) 10_556 11_576 ?
Na1 Na1 O3A 0(10) 10_556 . ?
Na1 Na1 O3B 0(10) 10_556 . ?
Na1 Na1 C1 0.0(7) 10_556 . ?
O2 Na1 Dy1 37.87(13) 10_556 10_556 ?
O2 Na1 Dy1 102.1(2) . 10_556 ?
O2 Na1 O2 64.3(3) 10_556 . ?
O2 Na1 O3A 59.1(4) . . ?
O2 Na1 O3A 108.2(5) 10_556 . ?
O2 Na1 O3B 118.8(6) 10_556 . ?
O2 Na1 O3B 66.1(4) . . ?
O2 Na1 C1 147.66(16) 10_556 . ?
O2 Na1 C1 147.66(16) . . ?
O3 Na1 Dy1 107.9(2) 11_576 10_556 ?
O3 Na1 Dy1 109.21(16) . 10_556 ?
O3 Na1 O2 144.1(5) . . ?
O3 Na1 O2 140.2(6) 11_576 10_556 ?
O3 Na1 O2 144.1(5) . 10_556 ?
O3 Na1 O2 140.2(6) 11_576 . ?
O3 Na1 O3 41.7(13) . 11_576 ?
O3 Na1 O3A 107.0(6) . . ?
O3 Na1 O3A 81.2(6) 11_576 . ?
O3 Na1 O3B 74.2(6) 11_576 . ?
O3 Na1 O3B 96.7(6) . . ?
O3 Na1 C1 20.9(8) 11_576 . ?
O3 Na1 C1 20.8(8) . . ?
O3A Na1 Dy1 133.3(5) . 10_556 ?
O3A Na1 C1 94.3(4) . . ?
O3B Na1 Dy1 142.7(7) . 10_556 ?
O3B Na1 C1 85.3(4) . . ?
C1 Na1 Dy1 109.93(9) . 10_556 ?
Dy1 O1 Dy1 104.6(3) 15_565 2_765 ?
Dy1 O1 Dy1 103.5(2) 15_565 . ?
Dy1 O1 Dy1 108.9(2) 2_765 . ?
Dy1 O1 H1 118(3) 15_565 . ?
Dy1 O1 H1 126(2) 2_765 . ?
Dy1 O1 H1 94(4) . . ?
Dy1 O2 Na1 101.9(2) . . ?
Dy1 O2 Na1 101.9(2) . 10_556 ?
Na1 O2 Na1 0.0(7) 10_556 . ?
C3 O2 Dy1 136.2(6) . . ?
C3 O2 Na1 120.6(6) . 10_556 ?
C3 O2 Na1 120.6(6) . . ?
Na1 O3 Na1 131.7(13) 10_556 3_755 ?
Na1 O3 Na1 131.7(13) . 3_755 ?
Na1 O3 Na1 0.0(7) . 10_556 ?
O3 O3 Na1 70(3) 11_576 . ?
O3 O3 Na1 159(3) 11_576 3_755 ?
O3 O3 Na1 70(3) 11_576 10_556 ?
O3 O3 Na1 69(3) 3_755 3_755 ?
O3 O3 Na1 160(3) 3_755 . ?
O3 O3 Na1 160(3) 3_755 10_556 ?
O3 O3 O3 90.000(9) 11_576 3_755 ?
C1 O3 Na1 114(3) . 3_755 ?
C1 O3 Na1 115(3) . 10_556 ?
C1 O3 Na1 115(3) . . ?
C1 O3 O3 45.001(5) . 11_576 ?
C1 O3 O3 44.999(2) . 3_755 ?
Dy1 O3A Na1 90.5(5) . . ?
C2 O3A Dy1 119.4(10) . . ?
C2 O3A Na1 113.9(11) . . ?
Dy1 O3B Na1 98.5(6) . . ?
C2 O3B Dy1 118.9(12) . . ?
C2 O3B Na1 141.4(12) . . ?
C3A O5A Dy1 119.2(13) . . ?
C3B O5B Dy1 118.3(13) . . ?
Na1 C1 Na1 90.000(2) 3_755 9_776 ?
Na1 C1 Na1 90.000(2) 11_576 10_556 ?
Na1 C1 Na1 90.000(1) . 3_755 ?
Na1 C1 Na1 0.0(6) . 10_556 ?
Na1 C1 Na1 180.0 9_776 10_556 ?
Na1 C1 Na1 90.000(2) . 11_576 ?
Na1 C1 Na1 180.0 . 9_776 ?
Na1 C1 Na1 90.000(1) 3_755 10_556 ?
Na1 C1 Na1 90.000(1) 11_576 9_776 ?
Na1 C1 Na1 180.0 3_755 11_576 ?
O3 C1 Na1 135(3) 3_755 11_576 ?
O3 C1 Na1 45(3) 9_776 11_576 ?
O3 C1 Na1 135(3) 11_576 9_776 ?
O3 C1 Na1 45(3) . . ?
O3 C1 Na1 135(3) 11_576 3_755 ?
O3 C1 Na1 135(3) . 9_776 ?
O3 C1 Na1 45(3) 11_576 10_556 ?
O3 C1 Na1 45(3) 9_776 9_776 ?
O3 C1 Na1 135(3) 9_776 . ?
O3 C1 Na1 45(3) . 3_755 ?
O3 C1 Na1 135(3) 3_755 . ?
O3 C1 Na1 135(3) 9_776 3_755 ?
O3 C1 Na1 45(3) . 10_556 ?
O3 C1 Na1 135(3) 9_776 10_556 ?
O3 C1 Na1 135(3) 3_755 10_556 ?
O3 C1 Na1 45(3) 3_755 9_776 ?
O3 C1 Na1 45(3) 11_576 . ?
O3 C1 Na1 135(3) . 11_576 ?
O3 C1 Na1 45(3) 11_576 11_576 ?
O3 C1 Na1 45(3) 3_755 3_755 ?
O3 C1 O3 180.00(2) . 9_776 ?
O3 C1 O3 90.00(2) 11_576 9_776 ?
O3 C1 O3 90.000(3) 3_755 9_776 ?
O3 C1 O3 89.998(9) . 11_576 ?
O3 C1 O3 90.002(10) . 3_755 ?
O3 C1 O3 180.000(11) 11_576 3_755 ?
O3A C2 C3A 116.1(13) . . ?
O3B C2 O4B 123.9(10) . . ?
O3B C2 C3B 112.9(15) . . ?
O4A C2 O3A 124.3(11) . . ?
O4A C2 C3A 119.1(13) . . ?
O4B C2 C3B 123.2(15) . . ?
O2 C3 O2 127.3(10) 2_765 . ?
O2 C3 C3 116.3(5) . 9_766 ?
O2 C3 C3 116.3(5) 2_765 9_766 ?
O5A C3A C2 116.2(16) . . ?
O6A C3A O5A 127.6(16) . . ?
O6A C3A C2 115.9(17) . . ?
O5B C3B O6B 127.3(16) . . ?
O5B C3B C2 119.1(18) . . ?
O6B C3B C2 113.3(18) . . ?

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
Dy1 O2 C3 O2 -4.8(4) . . . 2_765 ?
Dy1 O2 C3 C3 175.2(4) . . . 9_766 ?
Dy1 O3A C2 O4A 170.6(14) . . . . ?
Dy1 O3A C2 C3A -0.5(17) . . . . ?
Dy1 O3B C2 O4B -165.0(14) . . . . ?
Dy1 O3B C2 C3B 13.3(17) . . . . ?
Dy1 O5A C3A O6A -171.7(16) . . . . ?
Dy1 O5A C3A C2 14(2) . . . . ?
Dy1 O5B C3B O6B 167.3(16) . . . . ?
Dy1 O5B C3B C2 -18(2) . . . . ?
Na1 O2 C3 O2 -169.0(7) 10_556 . . 2_765 ?
Na1 O2 C3 O2 -169.0(7) . . . 2_765 ?
Na1 O2 C3 C3 11.0(7) 10_556 . . 9_766 ?
Na1 O2 C3 C3 11.0(7) . . . 9_766 ?
Na1 O3 C1 Na1 180.0 . . . 3_755 ?
Na1 O3 C1 Na1 180.0 10_556 . . 9_776 ?
Na1 O3 C1 Na1 0.0 10_556 . . . ?
Na1 O3 C1 Na1 0.0 . . . 10_556 ?
Na1 O3 C1 Na1 0.0 . . . 11_576 ?
Na1 O3 C1 Na1 180.0 3_755 . . . ?
Na1 O3 C1 Na1 180.0 3_755 . . 10_556 ?
Na1 O3 C1 Na1 180.0 3_755 . . 11_576 ?
Na1 O3 C1 Na1 180.0 . . . 9_776 ?
Na1 O3 C1 Na1 0.0 10_556 . . 11_576 ?
Na1 O3 C1 Na1 0.0 3_755 . . 9_776 ?
Na1 O3 C1 Na1 180.0 10_556 . . 3_755 ?
Na1 O3 C1 O3 180.0 . . . 3_755 ?
Na1 O3 C1 O3 180.0 3_755 . . 11_576 ?
Na1 O3 C1 O3 0.0 . . . 11_576 ?
Na1 O3 C1 O3 0.0 3_755 . . 3_755 ?
Na1 O3 C1 O3 180.0 10_556 . . 3_755 ?
Na1 O3 C1 O3 0.0 10_556 . . 11_576 ?
Na1 O3A C2 O4A -84.2(15) . . . . ?
Na1 O3A C2 C3A 104.7(11) . . . . ?
Na1 O3B C2 O4B -1(3) . . . . ?
Na1 O3B C2 C3B 177.8(17) . . . . ?
O3 O3 C1 Na1 180.0 3_755 . . 11_576 ?
O3 O3 C1 Na1 0.0 3_755 . . 9_776 ?
O3 O3 C1 Na1 180.0 3_755 . . 10_556 ?
O3 O3 C1 Na1 180.0 11_576 . . 3_755 ?
O3 O3 C1 Na1 0.0 11_576 . . . ?
O3 O3 C1 Na1 0.0 3_755 . . 3_755 ?
O3 O3 C1 Na1 180.0 11_576 . . 9_776 ?
O3 O3 C1 Na1 0.0 11_576 . . 11_576 ?
O3 O3 C1 Na1 0.0 11_576 . . 10_556 ?
O3 O3 C1 Na1 180.0 3_755 . . . ?
O3 O3 C1 O3 180.0 11_576 . . 3_755 ?
O3 O3 C1 O3 180.0 3_755 . . 11_576 ?
O3A C2 C3A O5A -9(2) . . . . ?
O3A C2 C3A O6A 175.9(16) . . . . ?
O3B C2 C3B O5B 3(2) . . . . ?
O3B C2 C3B O6B 178.3(16) . . . . ?
O4A C2 C3A O5A 179.4(16) . . . . ?
O4A C2 C3A O6A 4(2) . . . . ?
O4B C2 C3B O5B -178.6(17) . . . . ?
O4B C2 C3B O6B -3(2) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.478(2)
2 0.522(2)

