# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2015

####################################################################### 
# 
# 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_compound-1a
_database_code_depnum_ccdc_archive 'CCDC 1029797'
_audit_update_record             
;
2015-02-06 deposited with the CCDC.
2015-02-12 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C40 H122 Cl7 Dy6 N8 Na O87'
_chemical_formula_weight         3353.59

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'
Cl Cl 0.1484 0.1585 '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'
Dy Dy -0.1892 4.4098 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      cubic
_space_group_IT_number           213
_space_group_name_H-M_alt        'P 41 3 2'
_space_group_name_Hall           'P 4bd 2ab 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'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'
'z, x, y'
'z+1/2, -x+1/2, -y'
'-z+1/2, -x, y+1/2'
'-z, x+1/2, -y+1/2'
'y, z, x'
'-y, z+1/2, -x+1/2'
'y+1/2, -z+1/2, -x'
'-y+1/2, -z, x+1/2'
'y+3/4, x+1/4, -z+1/4'
'-y+3/4, -x+3/4, -z+3/4'
'y+1/4, -x+1/4, z+3/4'
'-y+1/4, x+3/4, z+1/4'
'x+3/4, z+1/4, -y+1/4'
'-x+1/4, z+3/4, y+1/4'
'-x+3/4, -z+3/4, -y+3/4'
'x+1/4, -z+1/4, y+3/4'
'z+3/4, y+1/4, -x+1/4'
'z+1/4, -y+1/4, x+3/4'
'-z+1/4, y+3/4, x+1/4'
'-z+3/4, -y+3/4, -x+3/4'

_cell_length_a                   35.491(4)
_cell_length_b                   35.491(4)
_cell_length_c                   35.491(4)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     44706(14)
_cell_formula_units_Z            12
_cell_measurement_temperature    123(2)
_cell_measurement_reflns_used    1964
_cell_measurement_theta_min      4.0400
_cell_measurement_theta_max      22.8570

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.495
_exptl_crystal_F_000             19680
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.140
_exptl_crystal_size_mid          0.120
_exptl_crystal_size_min          0.100
_exptl_absorpt_coefficient_mu    3.188
_shelx_estimated_absorpt_T_min   0.664
_shelx_estimated_absorpt_T_max   0.741
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6642
_exptl_absorpt_correction_T_max  0.7414
_exptl_absorpt_process_details   'ABSCOR by T.Higashi 8 March, 1995'

_exptl_special_details           
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
(compiled Dec  3 2012,18:21:49)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;

_diffrn_ambient_temperature      123(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            325513
_diffrn_reflns_av_unetI/netI     0.0203
_diffrn_reflns_av_R_equivalents  0.0663
_diffrn_reflns_limit_h_min       -42
_diffrn_reflns_limit_h_max       41
_diffrn_reflns_limit_k_min       -42
_diffrn_reflns_limit_k_max       42
_diffrn_reflns_limit_l_min       -42
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_theta_min         3.297
_diffrn_reflns_theta_max         24.996
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measured_fraction_theta_full 0.971
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_Laue_measured_fraction_full 0.971
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_point_group_measured_fraction_full 0.971
_reflns_number_total             13128
_reflns_number_gt                11527
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.779
_reflns_Friedel_fraction_max     0.999
_reflns_Friedel_fraction_full    0.972

_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.
According to the charge balance, there are 2 ClO4- counter anions per formula units.
 Based on the EA and TGA analysis, there are 15 guest water molecules per formula units.
 However, they are however severely disordered and were therefore removed by SQUEEZE 
in structural refinement. The SQUEEZE analysis estimate the electron count to be 3396 
within 19941 ?3 void per formula unit for 1a. According to the electron counts and 
the void per formula unit, the number of guest water is 18, which is consistent with
 the number calculated from EA and TGA results.

Non-hydrogen atoms were refined anisotropically, except for 26
disorder atoms were refined isotropically due to disorder. 
Because of disorder, two ClO4- was refined using DIFX command and dy4
and Na1 were refined using part 1,part 2, simu and delu.
The SHELXL restraint command is 
dfix 1.44 0.02 cl2 o19 cl2 o20 cl2 o21 cl2 o22
 dfix 2.35 0.02 o19 o20 o19 o21 o19 o22 o20 o21 o20 o22 o21 o22
 dfix 1.44 0.02 cl1 o15 cl1 o16 cl1 o17 cl1 o18
 dfix 2.35 0.02 o15 o16 o15 o17 o15 o18 o16 o17 o16 o18 o17 o18
 dfix 2.20 0.05 dy4 o11w na1 o14w na1 o15w
isor 0.005 cl1 cl2 o19 o22 o20 o21 o18 o20' o21' o22' o4 o17 c2 c5 dy4
isor 0.001 na1 o9w
isor 0.01 o6w o7w o8w o10w o11w o12w o13w o14w o15w
simu 0.02 dy4 na1
delu 0.02 dy4 na1
Summary of restraints applied refinement
              DFIX   DANG  SAME/SADI CHIV/Z CHIV/NZ FLAT DELU  RIGU   SIMU  ISOR 

       Number 23     0       0       0       0       0       0     0      6    156      

rms sigma     0.0260 0.0000 0.0000 0.0000 0.0000 0.0000 0.0000 0.0000 0.0200 0.0087  

rms deviation 0.0776 0.0000 0.0000 0.0000 0.0000 0.0000 0.0000 0.0000 0.0687 0.0112 


 GooF = S =     1.088;     Restrained GooF =      1.105 for     185 restraints
;

_computing_data_collection       'CrysAlisPro, Agilent Technologies'
_computing_cell_refinement       'CrysAlisPro, Agilent Technologies'
_computing_data_reduction        'CrysAlisPro, Agilent Technologies'
_computing_structure_solution    'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    'Diamond Version 3.2K'
_computing_publication_material  'SHELXL-2013 (Sheldrick, 2013)'

_refine_special_details          
;
 Refined as a 2-component inversion twin.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
;
 w=1/[σ²(Fo²)+(0.1065P)²+153.3978P]
 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_abs_structure_details 
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.030(18)
_chemical_absolute_configuration ad
_refine_ls_number_reflns         13128
_refine_ls_number_parameters     638
_refine_ls_number_restraints     185
_refine_ls_R_factor_all          0.0668
_refine_ls_R_factor_gt           0.0600
_refine_ls_wR_factor_ref         0.1747
_refine_ls_wR_factor_gt          0.1681
_refine_ls_goodness_of_fit_ref   1.088
_refine_ls_restrained_S_all      1.105
_refine_ls_shift/su_max          0.017
_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
Dy1 Dy 0.77410(2) 0.58266(2) 0.01493(2) 0.06593(15) Uani 1 1 d . . . . .
Dy2 Dy 0.72476(2) 0.47812(2) 0.14565(2) 0.05070(11) Uani 1 1 d . . . . .
Dy3 Dy 0.74277(2) 0.3750 0.00723(2) 0.03839(12) Uani 1 2 d S T P . .
Dy4 Dy 0.89017(6) 0.59683(7) -0.12873(7) 0.1381(7) Uani 0.5 1 d D U P A 1
Na1 Na 0.8758(2) 0.6153(2) -0.1345(2) 0.0499(9) Uani 0.5 1 d D U P A 2
N1 N 0.8331(2) 0.5520(3) 0.0462(2) 0.061(2) Uani 1 1 d . . . . .
N2 N 0.8272(4) 0.6330(3) 0.0242(4) 0.096(4) Uani 1 1 d . . . . .
N3 N 0.7073(2) 0.4121(2) 0.1742(2) 0.055(2) Uani 1 1 d . . . . .
N4 N 0.7856(2) 0.4347(2) 0.15358(19) 0.0472(19) Uani 1 1 d . . . . .
O1 O 0.7615(3) 0.6269(2) 0.0600(2) 0.092(3) Uani 1 1 d . . . . .
O2 O 0.7649(6) 0.6860(3) 0.0791(4) 0.154(6) Uani 1 1 d . . . . .
O3 O 0.8169(2) 0.5834(2) -0.0344(2) 0.075(2) Uani 1 1 d . . . . .
O4 O 0.8613(4) 0.6086(4) -0.0714(4) 0.143(4) Uani 1 1 d . U . . .
O5 O 0.7607(2) 0.54877(19) 0.07146(18) 0.0559(18) Uani 1 1 d . . . . .
O6 O 0.77607(19) 0.50887(18) 0.11681(16) 0.0479(16) Uani 1 1 d . . . . .
O7 O 0.7796(2) 0.51779(19) 0.00061(18) 0.0562(18) Uani 1 1 d . . . . .
H7C H 0.7624 0.5072 -0.0169 0.067 Uiso 1 1 calc R U . . .
O8 O 0.76324(18) 0.4889(2) 0.19872(17) 0.0546(17) Uani 1 1 d . . . . .
O9 O 0.81700(18) 0.4897(2) 0.23043(18) 0.0584(18) Uani 1 1 d . . . . .
O10 O 0.73619(18) 0.4349(2) 0.09512(18) 0.0546(17) Uani 1 1 d . . . . .
O11 O 0.77137(17) 0.39685(18) 0.06129(16) 0.0492(16) Uani 1 1 d . . . . .
O12 O 0.6887(2) 0.4819(2) 0.2047(2) 0.0589(19) Uani 1 1 d . . . . .
O13 O 0.6774(2) 0.4565(2) 0.2612(2) 0.067(2) Uani 1 1 d . . . . .
O14 O 0.6598(2) 0.4607(3) 0.1328(2) 0.074(2) Uani 1 1 d . . . . .
H14A H 0.6450 0.4756 0.1162 0.089 Uiso 1 1 calc R U . . .
O15 O 0.8821(4) 0.4266(4) -0.0426(3) 0.172(6) Uani 1 1 d D . . . .
O16 O 0.8813(3) 0.4348(4) -0.1080(2) 0.149(6) Uani 1 1 d D . . . .
O17 O 0.8242(3) 0.4364(5) -0.0727(4) 0.180(6) Uani 1 1 d D U . . .
O18 O 0.8676(6) 0.4845(3) -0.0674(5) 0.248(8) Uani 1 1 d D U . . .
Cl1 Cl 0.86351(10) 0.44347(11) -0.07449(9) 0.0875(10) Uani 1 1 d D U . . .
C1 C 0.8659(3) 0.5791(3) 0.0438(3) 0.071(3) Uani 1 1 d . . . . .
H1A H 0.8854 0.5715 0.0622 0.086 Uiso 1 1 calc R U . . .
H1B H 0.8771 0.5776 0.0183 0.086 Uiso 1 1 calc R U . . .
C2 C 0.8547(4) 0.6186(4) 0.0514(4) 0.090(3) Uani 1 1 d . U . . .
H2A H 0.8438 0.6202 0.0770 0.108 Uiso 1 1 calc R U . . .
H2B H 0.8774 0.6348 0.0508 0.108 Uiso 1 1 calc R U . . .
C3 C 0.8104(5) 0.6675(4) 0.0379(4) 0.101(5) Uani 1 1 d . . . . .
H3A H 0.8029 0.6833 0.0162 0.122 Uiso 1 1 calc R U . . .
H3B H 0.8293 0.6817 0.0527 0.122 Uiso 1 1 calc R U . . .
C4 C 0.7775(5) 0.6604(4) 0.0613(5) 0.102(5) Uani 1 1 d . . . . .
C5 C 0.8467(5) 0.6388(5) -0.0127(4) 0.098(3) Uani 1 1 d . U . . .
H5A H 0.8737 0.6439 -0.0075 0.118 Uiso 1 1 calc R U . . .
H5B H 0.8361 0.6617 -0.0247 0.118 Uiso 1 1 calc R U . . .
C6 C 0.8444(6) 0.6063(5) -0.0411(4) 0.129(6) Uani 1 1 d . . . . .
C7 C 0.8435(3) 0.5161(3) 0.0238(3) 0.060(3) Uani 1 1 d . . . . .
H7A H 0.8549 0.5231 -0.0007 0.072 Uiso 1 1 calc R U . . .
H7B H 0.8621 0.5010 0.0381 0.072 Uiso 1 1 calc R U . . .
C8 C 0.8080(3) 0.4932(3) 0.0173(3) 0.055(3) Uani 1 1 d . . . . .
H8A H 0.8134 0.4719 0.0001 0.066 Uiso 1 1 calc R U . . .
H8B H 0.7987 0.4829 0.0415 0.066 Uiso 1 1 calc R U . . .
C9 C 0.8243(3) 0.5428(3) 0.0844(3) 0.071(3) Uani 1 1 d . . . . .
H9A H 0.8310 0.5647 0.1004 0.085 Uiso 1 1 calc R U . . .
H9B H 0.8405 0.5215 0.0923 0.085 Uiso 1 1 calc R U . . .
C10 C 0.7836(3) 0.5324(3) 0.0919(3) 0.052(2) Uani 1 1 d . . . . .
C11 C 0.7385(3) 0.3846(3) 0.1686(3) 0.057(3) Uani 1 1 d . . . . .
H11A H 0.7386 0.3759 0.1421 0.068 Uiso 1 1 calc R U . . .
H11B H 0.7345 0.3624 0.1850 0.068 Uiso 1 1 calc R U . . .
C12 C 0.7773(3) 0.4028(3) 0.1780(2) 0.057(3) Uani 1 1 d . . . . .
H12A H 0.7772 0.4113 0.2046 0.068 Uiso 1 1 calc R U . . .
H12B H 0.7973 0.3836 0.1752 0.068 Uiso 1 1 calc R U . . .
C13 C 0.8155(3) 0.4560(3) 0.1721(2) 0.047(2) Uani 1 1 d . . . . .
H13A H 0.8288 0.4719 0.1535 0.056 Uiso 1 1 calc R U . . .
H13B H 0.8339 0.4385 0.1836 0.056 Uiso 1 1 calc R U . . .
C14 C 0.7973(3) 0.4808(3) 0.2027(3) 0.050(2) Uani 1 1 d . . . . .
C15 C 0.7987(3) 0.4227(3) 0.1155(3) 0.055(3) Uani 1 1 d . . . . .
H15A H 0.8128 0.3987 0.1176 0.066 Uiso 1 1 calc R U . . .
H15B H 0.8158 0.4420 0.1049 0.066 Uiso 1 1 calc R U . . .
C16 C 0.7643(3) 0.4170(3) 0.0884(3) 0.051(2) Uani 1 1 d . . . . .
C17 C 0.6733(3) 0.3981(4) 0.1508(3) 0.080(4) Uani 1 1 d . . . . .
H17A H 0.6815 0.3926 0.1247 0.096 Uiso 1 1 calc R U . . .
H17B H 0.6631 0.3747 0.1619 0.096 Uiso 1 1 calc R U . . .
C18 C 0.6438(3) 0.4277(4) 0.1503(4) 0.074(3) Uani 1 1 d . . . . .
H18A H 0.6216 0.4189 0.1359 0.089 Uiso 1 1 calc R U . . .
H18B H 0.6357 0.4336 0.1764 0.089 Uiso 1 1 calc R U . . .
C19 C 0.6973(3) 0.4152(3) 0.2133(3) 0.068(3) Uani 1 1 d . . . . .
H19A H 0.7188 0.4059 0.2285 0.082 Uiso 1 1 calc R U . . .
H19B H 0.6758 0.3982 0.2182 0.082 Uiso 1 1 calc R U . . .
C20 C 0.6873(3) 0.4527(3) 0.2270(3) 0.061(3) Uani 1 1 d . . . . .
O5W O 0.80819(18) 0.3883(2) -0.00665(19) 0.0559(18) Uani 1 1 d . . . . .
O4W O 0.7130(2) 0.3404(2) 0.0581(2) 0.072(2) Uani 1 1 d . . . . .
O1W O 0.7541(3) 0.6372(3) -0.0207(3) 0.091(3) Uani 1 1 d . . . . .
O3W O 0.7146(3) 0.5435(2) 0.1604(2) 0.087(3) Uani 1 1 d . . . . .
O2W O 0.6988(2) 0.5095(2) 0.0892(2) 0.070(2) Uani 1 1 d . . . . .
O6W O 0.9073(4) 0.6423(4) -0.1020(4) 0.147(5) Uani 1 1 d . U . . .
O7W O 0.8628(11) 0.5952(11) -0.1961(10) 0.178(8) Uani 0.5 1 d . U P . .
O8W O 0.9427(7) 0.5424(7) -0.1350(8) 0.120(6) Uani 0.5 1 d . U P . .
O9W O 0.8582(4) 0.5386(4) -0.1316(4) 0.1475(10) Uani 1 1 d . U . . .
O10W O 0.8203(10) 0.6135(10) -0.1374(10) 0.163(8) Uani 0.5 1 d . U P . .
O11W O 0.9185(11) 0.6446(10) -0.1680(10) 0.188(8) Uani 0.5 1 d D U P . .
O12W O 0.9330(9) 0.6196(10) -0.0890(9) 0.155(8) Uani 0.5 1 d . U P A .
O13W O 0.8831(8) 0.6709(8) -0.1073(8) 0.132(7) Uani 0.5 1 d . U P A .
O14W O 0.9035(11) 0.5727(10) -0.0958(10) 0.188(8) Uani 0.5 1 d D U P . .
O15W O 0.9273(10) 0.5725(11) -0.1510(11) 0.194(8) Uani 0.5 1 d D U P A .
Cl2 Cl 0.71773(9) 0.27470(10) 0.13879(10) 0.0825(9) Uani 1 1 d D U . . .
O19 O 0.6892(3) 0.2994(3) 0.1495(4) 0.162(5) Uani 1 1 d D U . . .
O20 O 0.7223(4) 0.2733(4) 0.0978(3) 0.087(4) Uani 0.6 1 d D U P B 1
O21 O 0.7528(3) 0.2809(5) 0.1556(5) 0.146(7) Uani 0.6 1 d D U P B 1
O22 O 0.7065(6) 0.2360(3) 0.1499(6) 0.188(8) Uani 0.6 1 d D U P B 1
O20' O 0.7094(10) 0.2491(10) 0.1133(10) 0.130(8) Uani 0.4 1 d . U P B 2
O21' O 0.7423(10) 0.3028(10) 0.1230(9) 0.127(7) Uani 0.4 1 d . U P B 2
O22' O 0.7412(7) 0.2539(7) 0.1669(7) 0.090(6) Uani 0.4 1 d . U P B 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 2.286(8) . ?
Dy1 O3 2.318(8) . ?
Dy1 O7 2.366(7) . ?
Dy1 O5 2.387(7) . ?
Dy1 O1W 2.418(9) . ?
Dy1 O13 2.430(8) 15_564 ?
Dy1 N1 2.609(9) . ?
Dy1 N2 2.618(12) . ?
Dy1 O12 2.717(7) 15_564 ?
Dy1 C20 2.953(11) 15_564 ?
Dy2 O6 2.357(7) . ?
Dy2 O8 2.358(6) . ?
Dy2 O10 2.394(6) . ?
Dy2 O3W 2.406(9) . ?
Dy2 O14 2.429(8) . ?
Dy2 O12 2.459(7) . ?
Dy2 O2W 2.471(7) . ?
Dy2 N3 2.629(8) . ?
Dy2 N4 2.668(8) . ?
Dy3 O9 2.270(6) 8_645 ?
Dy3 O9 2.270(6) 15_564 ?
Dy3 O11 2.305(6) . ?
Dy3 O11 2.305(6) 24 ?
Dy3 O5W 2.420(7) 24 ?
Dy3 O5W 2.420(7) . ?
Dy3 O4W 2.426(7) 24 ?
Dy3 O4W 2.426(7) . ?
Dy4 O14W 1.52(3) . ?
Dy4 O15W 1.76(3) . ?
Dy4 O6W 1.970(15) . ?
Dy4 O12W 2.22(3) . ?
Dy4 O4 2.317(15) . ?
Dy4 O9W 2.359(16) . ?
Dy4 O11W 2.41(3) . ?
Dy4 O10W 2.57(3) . ?
Dy4 O7W 2.58(4) . ?
Dy4 O8W 2.69(3) . ?
Dy4 O13W 2.75(3) . ?
Na1 O6W 1.872(17) . ?
Na1 O10W 1.98(4) . ?
Na1 O11W 2.19(3) . ?
Na1 O13W 2.21(3) . ?
Na1 O14W 2.27(3) . ?
Na1 O4 2.311(17) . ?
Na1 O7W 2.35(4) . ?
Na1 O15W 2.45(3) . ?
Na1 O12W 2.60(3) . ?
Na1 O9W 2.796(17) . ?
N1 C9 1.429(14) . ?
N1 C1 1.512(15) . ?
N1 C7 1.547(15) . ?
N2 C3 1.446(19) . ?
N2 C2 1.465(19) . ?
N2 C5 1.50(2) . ?
N3 C19 1.436(14) . ?
N3 C11 1.491(13) . ?
N3 C17 1.547(13) . ?
N4 C13 1.456(12) . ?
N4 C12 1.458(13) . ?
N4 C15 1.492(12) . ?
O1 C4 1.318(18) . ?
O2 C4 1.19(2) . ?
O3 C6 1.29(2) . ?
O4 C6 1.23(2) . ?
O5 C10 1.234(12) . ?
O6 C10 1.246(12) . ?
O7 C8 1.457(12) . ?
O8 C14 1.249(12) . ?
O9 C14 1.249(11) . ?
O9 Dy3 2.270(6) 11_556 ?
O10 C16 1.208(11) . ?
O11 C16 1.225(11) . ?
O12 C20 1.306(14) . ?
O12 Dy1 2.718(7) 16_645 ?
O13 C20 1.267(12) . ?
O13 Dy1 2.430(8) 16_645 ?
O14 C18 1.444(15) . ?
O15 Cl1 1.441(10) . ?
O16 Cl1 1.382(9) . ?
O17 Cl1 1.419(11) . ?
O18 Cl1 1.485(11) . ?
C1 C2 1.481(19) . ?
C3 C4 1.45(2) . ?
C5 C6 1.54(2) . ?
C7 C8 1.516(14) . ?
C9 C10 1.517(15) . ?
C11 C12 1.555(15) . ?
C13 C14 1.542(13) . ?
C15 C16 1.564(13) . ?
C17 C18 1.481(18) . ?
C19 C20 1.463(17) . ?
C20 Dy1 2.953(11) 16_645 ?
O6W O12W 1.30(3) . ?
O6W O13W 1.34(3) . ?
O8W O15W 1.33(4) . ?
Cl2 O20' 1.32(3) . ?
Cl2 O19 1.394(11) . ?
Cl2 O21 1.398(12) . ?
Cl2 O21' 1.44(3) . ?
Cl2 O20 1.464(10) . ?
Cl2 O22 1.482(12) . ?
Cl2 O22' 1.49(2) . ?

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 O3 130.5(3) . . ?
O1 Dy1 O7 146.6(3) . . ?
O3 Dy1 O7 78.1(3) . . ?
O1 Dy1 O5 73.7(3) . . ?
O3 Dy1 O5 140.5(3) . . ?
O7 Dy1 O5 72.9(2) . . ?
O1 Dy1 O1W 76.0(3) . . ?
O3 Dy1 O1W 77.8(3) . . ?
O7 Dy1 O1W 133.7(3) . . ?
O5 Dy1 O1W 141.6(3) . . ?
O1 Dy1 O13 87.0(3) . 15_564 ?
O3 Dy1 O13 127.4(3) . 15_564 ?
O7 Dy1 O13 85.8(3) . 15_564 ?
O5 Dy1 O13 77.0(2) . 15_564 ?
O1W Dy1 O13 78.5(3) . 15_564 ?
O1 Dy1 N1 98.4(3) . . ?
O3 Dy1 N1 78.4(3) . . ?
O7 Dy1 N1 67.6(3) . . ?
O5 Dy1 N1 66.0(3) . . ?
O1W Dy1 N1 142.3(3) . . ?
O13 Dy1 N1 139.0(3) 15_564 . ?
O1 Dy1 N2 65.4(4) . . ?
O3 Dy1 N2 67.4(4) . . ?
O7 Dy1 N2 129.2(3) . . ?
O5 Dy1 N2 112.5(3) . . ?
O1W Dy1 N2 74.3(4) . . ?
O13 Dy1 N2 144.9(3) 15_564 . ?
N1 Dy1 N2 69.7(3) . . ?
O1 Dy1 O12 129.4(3) . 15_564 ?
O3 Dy1 O12 76.7(3) . 15_564 ?
O7 Dy1 O12 66.7(2) . 15_564 ?
O5 Dy1 O12 114.2(2) . 15_564 ?
O1W Dy1 O12 69.6(3) . 15_564 ?
O13 Dy1 O12 51.1(2) 15_564 15_564 ?
N1 Dy1 O12 131.3(3) . 15_564 ?
N2 Dy1 O12 133.3(3) . 15_564 ?
O1 Dy1 C20 108.4(4) . 15_564 ?
O3 Dy1 C20 102.8(3) . 15_564 ?
O7 Dy1 C20 74.9(3) . 15_564 ?
O5 Dy1 C20 95.2(3) . 15_564 ?
O1W Dy1 C20 72.7(3) . 15_564 ?
O13 Dy1 C20 24.9(3) 15_564 15_564 ?
N1 Dy1 C20 141.5(3) . 15_564 ?
N2 Dy1 C20 146.9(3) . 15_564 ?
O12 Dy1 C20 26.2(3) 15_564 15_564 ?
O6 Dy2 O8 79.9(2) . . ?
O6 Dy2 O10 80.8(2) . . ?
O8 Dy2 O10 127.2(2) . . ?
O6 Dy2 O3W 76.3(3) . . ?
O8 Dy2 O3W 75.9(3) . . ?
O10 Dy2 O3W 143.7(3) . . ?
O6 Dy2 O14 140.3(2) . . ?
O8 Dy2 O14 137.8(2) . . ?
O10 Dy2 O14 81.8(2) . . ?
O3W Dy2 O14 98.3(3) . . ?
O6 Dy2 O12 138.3(2) . . ?
O8 Dy2 O12 67.1(2) . . ?
O10 Dy2 O12 139.6(2) . . ?
O3W Dy2 O12 71.6(3) . . ?
O14 Dy2 O12 71.4(2) . . ?
O6 Dy2 O2W 74.2(2) . . ?
O8 Dy2 O2W 142.3(3) . . ?
O10 Dy2 O2W 75.1(3) . . ?
O3W Dy2 O2W 71.7(3) . . ?
O14 Dy2 O2W 66.9(3) . . ?
O12 Dy2 O2W 118.2(3) . . ?
O6 Dy2 N3 139.7(2) . . ?
O8 Dy2 N3 88.4(2) . . ?
O10 Dy2 N3 76.0(3) . . ?
O3W Dy2 N3 137.8(3) . . ?
O14 Dy2 N3 67.8(3) . . ?
O12 Dy2 N3 66.3(3) . . ?
O2W Dy2 N3 128.8(3) . . ?
O6 Dy2 N4 71.8(2) . . ?
O8 Dy2 N4 62.6(2) . . ?
O10 Dy2 N4 64.7(2) . . ?
O3W Dy2 N4 130.9(3) . . ?
O14 Dy2 N4 129.9(3) . . ?
O12 Dy2 N4 111.3(2) . . ?
O2W Dy2 N4 130.3(2) . . ?
N3 Dy2 N4 68.6(3) . . ?
O9 Dy3 O9 149.5(4) 8_645 15_564 ?
O9 Dy3 O11 94.7(2) 8_645 . ?
O9 Dy3 O11 93.7(2) 15_564 . ?
O9 Dy3 O11 93.7(2) 8_645 24 ?
O9 Dy3 O11 94.7(2) 15_564 24 ?
O11 Dy3 O11 147.8(3) . 24 ?
O9 Dy3 O5W 77.5(3) 8_645 24 ?
O9 Dy3 O5W 77.5(2) 15_564 24 ?
O11 Dy3 O5W 140.8(2) . 24 ?
O11 Dy3 O5W 71.4(2) 24 24 ?
O9 Dy3 O5W 77.5(2) 8_645 . ?
O9 Dy3 O5W 77.5(3) 15_564 . ?
O11 Dy3 O5W 71.4(2) . . ?
O11 Dy3 O5W 140.8(2) 24 . ?
O5W Dy3 O5W 69.3(3) 24 . ?
O9 Dy3 O4W 138.6(3) 8_645 24 ?
O9 Dy3 O4W 71.9(3) 15_564 24 ?
O11 Dy3 O4W 78.2(2) . 24 ?
O11 Dy3 O4W 75.1(2) 24 24 ?
O5W Dy3 O4W 131.9(2) 24 24 ?
O5W Dy3 O4W 134.8(3) . 24 ?
O9 Dy3 O4W 71.9(3) 8_645 . ?
O9 Dy3 O4W 138.6(3) 15_564 . ?
O11 Dy3 O4W 75.1(2) . . ?
O11 Dy3 O4W 78.2(2) 24 . ?
O5W Dy3 O4W 134.8(3) 24 . ?
O5W Dy3 O4W 131.9(2) . . ?
O4W Dy3 O4W 66.8(4) 24 . ?
O14W Dy4 O15W 80.7(19) . . ?
O14W Dy4 O6W 89.6(14) . . ?
O15W Dy4 O6W 112.8(13) . . ?
O14W Dy4 O12W 60.4(16) . . ?
O15W Dy4 O12W 87.3(15) . . ?
O6W Dy4 O12W 35.4(9) . . ?
O14W Dy4 O4 64.2(15) . . ?
O15W Dy4 O4 144.4(14) . . ?
O6W Dy4 O4 64.2(6) . . ?
O12W Dy4 O4 71.3(9) . . ?
O14W Dy4 O9W 72.0(14) . . ?
O15W Dy4 O9W 84.8(13) . . ?
O6W Dy4 O9W 152.6(6) . . ?
O12W Dy4 O9W 132.4(10) . . ?
O4 Dy4 O9W 89.1(5) . . ?
O14W Dy4 O11W 135.1(17) . . ?
O15W Dy4 O11W 77.0(16) . . ?
O6W Dy4 O11W 64.8(10) . . ?
O12W Dy4 O11W 80.0(12) . . ?
O4 Dy4 O11W 124.4(10) . . ?
O9W Dy4 O11W 142.2(10) . . ?
O14W Dy4 O10W 121.4(17) . . ?
O15W Dy4 O10W 141.3(15) . . ?
O6W Dy4 O10W 99.6(9) . . ?
O12W Dy4 O10W 130.6(12) . . ?
O4 Dy4 O10W 68.7(9) . . ?
O9W Dy4 O10W 74.5(9) . . ?
O11W Dy4 O10W 99.8(12) . . ?
O14W Dy4 O7W 144.6(16) . . ?
O15W Dy4 O7W 81.6(15) . . ?
O6W Dy4 O7W 125.5(10) . . ?
O12W Dy4 O7W 148.4(12) . . ?
O4 Dy4 O7W 130.6(9) . . ?
O9W Dy4 O7W 76.1(9) . . ?
O11W Dy4 O7W 68.7(12) . . ?
O10W Dy4 O7W 62.0(11) . . ?
O14W Dy4 O8W 56.4(15) . . ?
O15W Dy4 O8W 25.1(14) . . ?
O6W Dy4 O8W 114.4(7) . . ?
O12W Dy4 O8W 80.8(10) . . ?
O4 Dy4 O8W 120.5(7) . . ?
O9W Dy4 O8W 72.6(7) . . ?
O11W Dy4 O8W 99.7(11) . . ?
O10W Dy4 O8W 145.5(10) . . ?
O7W Dy4 O8W 99.7(10) . . ?
O14W Dy4 O13W 110.7(15) . . ?
O15W Dy4 O13W 131.5(14) . . ?
O6W Dy4 O13W 27.2(7) . . ?
O12W Dy4 O13W 62.6(10) . . ?
O4 Dy4 O13W 62.9(7) . . ?
O9W Dy4 O13W 143.7(7) . . ?
O11W Dy4 O13W 61.7(11) . . ?
O10W Dy4 O13W 74.0(10) . . ?
O7W Dy4 O13W 104.1(10) . . ?
O8W Dy4 O13W 140.6(8) . . ?
O6W Na1 O10W 130.2(12) . . ?
O6W Na1 O11W 71.3(11) . . ?
O10W Na1 O11W 132.7(15) . . ?
O6W Na1 O13W 37.3(8) . . ?
O10W Na1 O13W 99.6(13) . . ?
O11W Na1 O13W 74.5(12) . . ?
O6W Na1 O14W 73.0(10) . . ?
O10W Na1 O14W 116.2(15) . . ?
O11W Na1 O14W 110.3(14) . . ?
O13W Na1 O14W 106.2(12) . . ?
O6W Na1 O4 65.7(6) . . ?
O10W Na1 O4 79.9(11) . . ?
O11W Na1 O4 136.9(11) . . ?
O13W Na1 O4 72.2(8) . . ?
O14W Na1 O4 55.9(10) . . ?
O6W Na1 O7W 148.1(11) . . ?
O10W Na1 O7W 75.2(14) . . ?
O11W Na1 O7W 77.0(14) . . ?
O13W Na1 O7W 134.6(12) . . ?
O14W Na1 O7W 116.6(13) . . ?
O4 Na1 O7W 145.9(10) . . ?
O6W Na1 O15W 91.2(11) . . ?
O10W Na1 O15W 135.4(14) . . ?
O11W Na1 O15W 69.5(14) . . ?
O13W Na1 O15W 124.9(12) . . ?
O14W Na1 O15W 53.7(13) . . ?
O4 Na1 O15W 109.5(10) . . ?
O7W Na1 O15W 74.6(13) . . ?
O6W Na1 O12W 28.3(9) . . ?
O10W Na1 O12W 144.4(13) . . ?
O11W Na1 O12W 76.7(13) . . ?
O13W Na1 O12W 65.5(11) . . ?
O14W Na1 O12W 47.4(12) . . ?
O4 Na1 O12W 65.0(9) . . ?
O7W Na1 O12W 138.7(12) . . ?
O15W Na1 O12W 66.6(12) . . ?
O6W Na1 O9W 127.6(7) . . ?
O10W Na1 O9W 75.4(11) . . ?
O11W Na1 O9W 129.6(11) . . ?
O13W Na1 O9W 151.5(8) . . ?
O14W Na1 O9W 54.9(10) . . ?
O4 Na1 O9W 79.3(5) . . ?
O7W Na1 O9W 72.1(10) . . ?
O15W Na1 O9W 64.5(10) . . ?
O12W Na1 O9W 102.0(9) . . ?
C9 N1 C1 111.5(8) . . ?
C9 N1 C7 110.6(9) . . ?
C1 N1 C7 108.3(8) . . ?
C9 N1 Dy1 108.8(7) . . ?
C1 N1 Dy1 109.1(7) . . ?
C7 N1 Dy1 108.4(6) . . ?
C3 N2 C2 110.4(11) . . ?
C3 N2 C5 111.7(12) . . ?
C2 N2 C5 108.4(13) . . ?
C3 N2 Dy1 108.8(10) . . ?
C2 N2 Dy1 108.9(8) . . ?
C5 N2 Dy1 108.5(9) . . ?
C19 N3 C11 111.4(8) . . ?
C19 N3 C17 110.7(8) . . ?
C11 N3 C17 107.3(8) . . ?
C19 N3 Dy2 111.2(6) . . ?
C11 N3 Dy2 110.9(6) . . ?
C17 N3 Dy2 105.1(7) . . ?
C13 N4 C12 106.4(7) . . ?
C13 N4 C15 109.4(7) . . ?
C12 N4 C15 112.2(8) . . ?
C13 N4 Dy2 109.8(6) . . ?
C12 N4 Dy2 110.3(6) . . ?
C15 N4 Dy2 108.7(5) . . ?
C4 O1 Dy1 124.1(10) . . ?
C6 O3 Dy1 129.9(10) . . ?
C6 O4 Na1 163.6(15) . . ?
C6 O4 Dy4 165.6(14) . . ?
C10 O5 Dy1 126.8(7) . . ?
C10 O6 Dy2 141.6(6) . . ?
C8 O7 Dy1 123.5(5) . . ?
C14 O8 Dy2 127.8(6) . . ?
C14 O9 Dy3 148.3(6) . 11_556 ?
C16 O10 Dy2 128.7(6) . . ?
C16 O11 Dy3 139.5(6) . . ?
C20 O12 Dy2 119.6(6) . . ?
C20 O12 Dy1 87.0(6) . 16_645 ?
Dy2 O12 Dy1 147.8(3) . 16_645 ?
C20 O13 Dy1 101.3(7) . 16_645 ?
C18 O14 Dy2 119.9(6) . . ?
O16 Cl1 O17 116.7(8) . . ?
O16 Cl1 O15 112.1(7) . . ?
O17 Cl1 O15 110.0(8) . . ?
O16 Cl1 O18 108.6(9) . . ?
O17 Cl1 O18 105.2(10) . . ?
O15 Cl1 O18 103.3(9) . . ?
C2 C1 N1 112.7(11) . . ?
N2 C2 C1 112.9(11) . . ?
N2 C3 C4 112.2(12) . . ?
O2 C4 O1 122.8(18) . . ?
O2 C4 C3 118.3(15) . . ?
O1 C4 C3 118.8(14) . . ?
N2 C5 C6 116.5(13) . . ?
O4 C6 O3 124.8(17) . . ?
O4 C6 C5 119.7(16) . . ?
O3 C6 C5 113.1(15) . . ?
C8 C7 N1 108.8(8) . . ?
O7 C8 C7 108.4(8) . . ?
N1 C9 C10 115.5(9) . . ?
O5 C10 O6 126.3(10) . . ?
O5 C10 C9 114.2(9) . . ?
O6 C10 C9 119.5(9) . . ?
N3 C11 C12 110.9(8) . . ?
N4 C12 C11 112.1(8) . . ?
N4 C13 C14 108.0(7) . . ?
O8 C14 O9 125.0(9) . . ?
O8 C14 C13 117.2(8) . . ?
O9 C14 C13 117.7(8) . . ?
N4 C15 C16 110.6(8) . . ?
O10 C16 O11 129.1(9) . . ?
O10 C16 C15 117.1(8) . . ?
O11 C16 C15 113.5(8) . . ?
C18 C17 N3 109.3(10) . . ?
O14 C18 C17 107.6(10) . . ?
N3 C19 C20 116.9(10) . . ?
O13 C20 O12 120.5(10) . . ?
O13 C20 C19 118.7(11) . . ?
O12 C20 C19 120.7(9) . . ?
O13 C20 Dy1 53.8(6) . 16_645 ?
O12 C20 Dy1 66.8(6) . 16_645 ?
C19 C20 Dy1 172.3(8) . 16_645 ?
O12W O6W O13W 165(2) . . ?
O12W O6W Na1 108.6(18) . . ?
O13W O6W Na1 85.2(15) . . ?
O12W O6W Dy4 83.0(17) . . ?
O13W O6W Dy4 110.6(16) . . ?
O15W O8W Dy4 34.3(18) . . ?
O6W O12W Dy4 61.6(15) . . ?
O6W O12W Na1 43.1(13) . . ?
O6W O13W Na1 57.5(12) . . ?
O6W O13W Dy4 42.1(11) . . ?
O8W O15W Dy4 121(3) . . ?
O8W O15W Na1 135(3) . . ?
O20' Cl2 O19 117.4(17) . . ?
O19 Cl2 O21 115.6(9) . . ?
O20' Cl2 O21' 110(2) . . ?
O19 Cl2 O21' 96.3(15) . . ?
O19 Cl2 O20 111.9(8) . . ?
O21 Cl2 O20 109.3(9) . . ?
O19 Cl2 O22 108.4(9) . . ?
O21 Cl2 O22 105.7(10) . . ?
O20 Cl2 O22 105.2(9) . . ?
O20' Cl2 O22' 104.1(18) . . ?
O19 Cl2 O22' 122.2(12) . . ?
O21' Cl2 O22' 105.4(17) . . ?

_refine_diff_density_max         2.279
_refine_diff_density_min         -0.736
_refine_diff_density_rms         0.145


# SQUEEZE RESULTS (APPEND TO CIF)
# Note: Data are Listed for all Voids in the P1 Unit Cell
# i.e. Centre of Gravity, Solvent Accessible Volume,
# Recovered number of Electrons in the Void and
# Details about the Squeezed Material
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 -0.051 -0.063 -0.053 19941 3396 ' '
_platon_squeeze_details          
;
;

# compound-1a RESULTS (APPEND TO CIF)
_platon_compound-1a_details      
;
According to the charge balance, there are 2 ClO4- counter anions per formula units.
 Based on the EA and TGA analysis, there are 15 guest water molecules per formula units.
 However, they are however severely disordered and were therefore removed by SQUEEZE 
in structural refinement. The SQUEEZE analysis estimate the electron count to be 3396 
within 19941 ?3 void per formula unit for 1a. According to the electron counts and 
the void per formula unit, the number of guest water is 18, which is consistent with
 the number calculated from EA and TGA results.
;

_vrf_CHEMW03_compound-1a         
;
PROBLEM: ALERT: The ratio of given/expected molecular weight as
RESPONSE: This is caused by the given molecular weight being increased 
from the atom count to account fortwo ClO4- and 15 water molecules
per formula unit. This valueis calculated based upon elemental analysis data
 and TGA data.
;


_vrf_PLAT043_compound-1a         
;
PROBLEM: Check Reported Molecular Weight ................   
RESPONSE: This is caused by the given molecular weight being increased 
from the atom count to account for two ClO4- and 15 water molecules
per formula unit. This valueis calculated based upon elemental analysis data
 and TGA data.
;

_vrf_PLAT602_compound-1a         
;
PROBLEM: very large solvent Accessible VOIDS in structure        
RESPONSE: This is caused by two ClO4- and 15 water molecules
per formula unit was omitted in refinement. 
;


# end Validation Reply Form

_shelxl_version_number           2013-2

####################################################################### 
# 
# 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_compound-1b
_database_code_depnum_ccdc_archive 'CCDC 1029798'
_audit_update_record             
;
2015-02-06 deposited with the CCDC.
2015-02-12 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C40 H122 Cl7 Dy6 N8 Na O87'
_chemical_formula_weight         3353.59

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'
Cl Cl 0.1484 0.1585 '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'
Dy Dy -0.1892 4.4098 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      cubic
_space_group_IT_number           212
_space_group_name_H-M_alt        'P 43 3 2'
_space_group_name_Hall           'P 4acd 2ab 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'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'
'z, x, y'
'z+1/2, -x+1/2, -y'
'-z+1/2, -x, y+1/2'
'-z, x+1/2, -y+1/2'
'y, z, x'
'-y, z+1/2, -x+1/2'
'y+1/2, -z+1/2, -x'
'-y+1/2, -z, x+1/2'
'y+1/4, x+3/4, -z+3/4'
'-y+1/4, -x+1/4, -z+1/4'
'y+3/4, -x+3/4, z+1/4'
'-y+3/4, x+1/4, z+3/4'
'x+1/4, z+3/4, -y+3/4'
'-x+3/4, z+1/4, y+3/4'
'-x+1/4, -z+1/4, -y+1/4'
'x+3/4, -z+3/4, y+1/4'
'z+1/4, y+3/4, -x+3/4'
'z+3/4, -y+3/4, x+1/4'
'-z+3/4, y+1/4, x+3/4'
'-z+1/4, -y+1/4, -x+1/4'

_cell_length_a                   35.3561(3)
_cell_length_b                   35.3561(3)
_cell_length_c                   35.3561(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     44197.0(11)
_cell_formula_units_Z            12
_cell_measurement_temperature    123(2)
_cell_measurement_reflns_used    8995
_cell_measurement_theta_min      3.3034
_cell_measurement_theta_max      29.1968

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.512
_exptl_crystal_F_000             19680
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.080
_exptl_crystal_size_min          0.080
_exptl_absorpt_coefficient_mu    3.225
_shelx_estimated_absorpt_T_min   0.739
_shelx_estimated_absorpt_T_max   0.782
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.7390
_exptl_absorpt_correction_T_max  0.7828
_exptl_absorpt_process_details   'ABSCOR by T.Higashi 8 March, 1995'

_exptl_special_details           
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET)
(compiled Jul 11 2012,15:38:31)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;

_diffrn_ambient_temperature      123(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            43803
_diffrn_reflns_av_unetI/netI     0.0928
_diffrn_reflns_av_R_equivalents  0.0736
_diffrn_reflns_limit_h_min       -42
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_k_min       -36
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_theta_min         3.310
_diffrn_reflns_theta_max         24.985
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measured_fraction_theta_full 0.969
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_Laue_measured_fraction_full 0.969
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_point_group_measured_fraction_full 0.970
_reflns_number_total             12949
_reflns_number_gt                7991
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.778
_reflns_Friedel_fraction_max     1.000
_reflns_Friedel_fraction_full    0.970

_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.
According to the charge balance, there are 2 ClO4- counter anions per formula units.
 Based on the EA and TGA analysis, there are 15 guest water molecules per formula units.
 However, they are however severely disordered and were therefore removed by SQUEEZE 
in structural refinement. The SQUEEZE analysis estimate the electron count to be 3396 
within 19941 ?3 void per formula unit for 1b. According to the electron counts and 
the void per formula unit, the number of guest water is 18, which is consistent with
 the number calculated from EA and TGA results.

Non-hydrogen atoms were refined anisotropically, except for 27
 disorder atoms were refined isotropically due to disorder. 
Because of disorder, nine bonds was refined using DIFX command and dy4
and Na1 were refined using simu and delu.Because of disorder, two ClO4-
 and 15 water molecules were omited per formula unit. This valueis calculated based upon elemental analysis data and TGA data.
The SHELXL restraint command is
isor 0.01 o1w o6w o7w o8w o9w o10w o11w o12w o13w o14w
isor 0.005 o2 c19 o4 c3 c4 c1 o15 o16 c10
isor 0.005 o20 o21 o22 o20' o21' o22' o19
isor 0.002 dy4 na1
dfix 2.35 0.05 o19 o22' o22' o21' o22' o20' dy4 o11w
dfix 2.10 0.05 na1 o14w
dfix 1.50 0.02 c3 n1 n1 c1
dfix 1.50 0.02 c1 c2 c3 c4
dfix 2.10 0.05 h3a h1a h3b h5a
delu 0.01 c1 c2 n1 c5 o7w o12w
simu 0.01 o7w o12w
delu 0.007 dy4 na1
simu 0.007 dy4 na1

Summary of restraints applied refinement
          DFIX   DANG SAME/SADI CHIV/Z CHIV/NZ  FLAT   DELU   RIGU   SIMU    ISOR    

    Number   11      0      0       0       0       0       5       0      12     168  

 rms sigma    0.0417 0.0000 0.0000  0.0000 0.0000 0.0000 0.0100 0.0000 0.0150 0.0114

 rms deviation 0.0899 0.0000 0.0000 0.0000 0.0000 0.0000 0.0161 0.0000 0.0317 0.0156


 GooF = S =     1.039;     Restrained GooF =      1.069 for     196 restraints
;

_computing_data_collection       'CrysAlisPro, Agilent Technologies'
_computing_cell_refinement       'CrysAlisPro, Agilent Technologies'
_computing_data_reduction        'CrysAlisPro, Agilent Technologies'
_computing_structure_solution    'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    'Diamond Version 3.2K'
_computing_publication_material  'SHELXL-2013 (Sheldrick, 2013)'

_refine_special_details          
;
 Refined as a 2-component inversion twin.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
;
 w=1/[σ²(Fo²)+(0.1199P)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_abs_structure_details 
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.02(2)
_chemical_absolute_configuration ad
_refine_ls_number_reflns         12949
_refine_ls_number_parameters     628
_refine_ls_number_restraints     196
_refine_ls_R_factor_all          0.1197
_refine_ls_R_factor_gt           0.0754
_refine_ls_wR_factor_ref         0.2119
_refine_ls_wR_factor_gt          0.1890
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_restrained_S_all      1.069
_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
Dy1 Dy 0.48232(2) 0.72667(3) -0.08335(2) 0.0717(2) Uani 1 1 d . . . . .
Dy2 Dy 0.35224(2) 0.77632(2) 0.02250(2) 0.05460(18) Uani 1 1 d . . . . .
Dy3 Dy 0.49153(2) 0.75847(2) 0.1250 0.03965(19) Uani 1 2 d S T P . .
Dy4 Dy 0.62576(8) 0.60998(8) -0.09898(8) 0.1349(9) Uani 0.5 1 d D U P A 1
Na1 Na 0.6334(4) 0.6251(4) -0.1198(4) 0.0800(16) Uani 0.5 1 d D U P A 2
Cl1 Cl 0.57194(12) 0.63633(13) 0.05629(15) 0.0900(15) Uani 1 1 d . . . . .
Cl2 Cl 0.46526(12) 0.89018(13) 0.02459(14) 0.0841(14) Uani 1 1 d . . . . .
O1 O 0.4361(3) 0.7381(5) -0.1271(3) 0.104(5) Uani 1 1 d . . . . .
O2 O 0.4214(5) 0.7366(5) -0.1869(4) 0.128(5) Uani 1 1 d . U . . .
O3 O 0.5329(3) 0.6840(3) -0.0838(3) 0.084(4) Uani 1 1 d . . . . .
O4 O 0.5712(5) 0.6413(5) -0.1087(5) 0.139(4) Uani 1 1 d . U . . .
O6 O 0.3812(2) 0.7244(2) -0.0077(2) 0.042(2) Uani 1 1 d . . . . .
O5 O 0.4261(3) 0.7402(2) -0.0482(2) 0.060(3) Uani 1 1 d . . . . .
O7 O 0.4982(3) 0.7202(3) -0.0189(2) 0.057(3) Uani 1 1 d . . . . .
H7C H 0.5167 0.7367 -0.0085 0.069 Uiso 1 1 calc R U . . .
O9 O 0.4372(2) 0.7302(2) 0.1035(2) 0.044(2) Uani 1 1 d . . . . .
O8 O 0.4035(2) 0.7649(2) 0.0652(3) 0.065(3) Uani 1 1 d . . . . .
O10 O 0.3000(2) 0.7378(2) 0.0118(3) 0.054(2) Uani 1 1 d . . . . .
O11 O 0.2682(2) 0.6835(2) 0.0110(3) 0.068(3) Uani 1 1 d . . . . .
O12 O 0.2932(3) 0.8126(3) 0.0188(3) 0.066(3) Uani 1 1 d . . . . .
O13 O 0.2373(3) 0.8258(3) 0.0446(3) 0.068(3) Uani 1 1 d . . . . .
O14 O 0.3648(3) 0.8418(3) 0.0401(3) 0.075(3) Uani 1 1 d . . . . .
H14A H 0.3820 0.8565 0.0256 0.090 Uiso 1 1 calc R U . . .
O15 O 0.5639(7) 0.6373(8) 0.0155(7) 0.225(8) Uani 1 1 d . U . . .
O16 O 0.5663(6) 0.6733(6) 0.0621(6) 0.173(6) Uani 1 1 d . U . . .
O17 O 0.5396(4) 0.6173(5) 0.0695(5) 0.143(6) Uani 1 1 d . . . . .
O18 O 0.6047(3) 0.6167(4) 0.0648(5) 0.141(6) Uani 1 1 d . . . . .
O19 O 0.4384(4) 0.9039(4) 0.0463(4) 0.121(5) Uani 1 1 d D U . . .
O20 O 0.4716(6) 0.8490(6) 0.0220(7) 0.108(6) Uani 0.6 1 d . U P B 1
O22 O 0.4566(10) 0.9019(10) -0.0127(10) 0.178(8) Uani 0.6 1 d . U P B 1
O21 O 0.4999(6) 0.9065(6) 0.0266(6) 0.100(6) Uani 0.6 1 d . U P B 1
O20' O 0.4916(8) 0.8774(9) 0.0482(8) 0.092(7) Uani 0.4 1 d D U P B 2
O21' O 0.4898(7) 0.9201(6) 0.0011(7) 0.066(6) Uani 0.4 1 d D U P B 2
O22' O 0.4552(12) 0.8682(11) -0.0069(10) 0.188(9) Uani 0.4 1 d D U P B 2
N1 N 0.4736(4) 0.6732(4) -0.1341(4) 0.091(4) Uani 1 1 d D U . . .
N4 N 0.3439(3) 0.7155(3) 0.0669(3) 0.043(3) Uani 1 1 d . . . . .
N3 N 0.3224(3) 0.7949(3) 0.0890(3) 0.056(3) Uani 1 1 d . . . . .
N2 N 0.4525(3) 0.6664(3) -0.0508(3) 0.058(3) Uani 1 1 d . . . . .
C3 C 0.5099(4) 0.6539(6) -0.1406(5) 0.107(4) Uani 1 1 d D U . . .
H3A H 0.5205 0.6643 -0.1643 0.128 Uiso 1 1 calc DR U . . .
H3B H 0.5040 0.6269 -0.1455 0.128 Uiso 1 1 calc DR U . . .
C4 C 0.5409(5) 0.6548(7) -0.1117(5) 0.112(4) Uani 1 1 d D U . . .
C1 C 0.4616(5) 0.6900(4) -0.1709(4) 0.094(3) Uani 1 1 d D U . . .
H1A H 0.4840 0.6988 -0.1853 0.113 Uiso 1 1 calc DR U . . .
H1B H 0.4480 0.6710 -0.1863 0.113 Uiso 1 1 calc R U . . .
C2 C 0.4367(5) 0.7220(5) -0.1622(6) 0.099(5) Uani 1 1 d D U . . .
C5 C 0.4468(6) 0.6455(5) -0.1196(6) 0.125(6) Uani 1 1 d . U . . .
H5A H 0.4487 0.6221 -0.1348 0.150 Uiso 1 1 calc DR U . . .
H5B H 0.4208 0.6555 -0.1224 0.150 Uiso 1 1 calc R U . . .
C6 C 0.4536(5) 0.6363(6) -0.0793(5) 0.091(6) Uani 1 1 d . . . . .
H6A H 0.4347 0.6170 -0.0718 0.109 Uiso 1 1 calc R U . . .
H6B H 0.4788 0.6241 -0.0776 0.109 Uiso 1 1 calc R U . . .
C7 C 0.4124(4) 0.6761(4) -0.0426(4) 0.068(4) Uani 1 1 d . . . . .
H7A H 0.4034 0.6597 -0.0217 0.081 Uiso 1 1 calc R U . . .
H7B H 0.3971 0.6701 -0.0652 0.081 Uiso 1 1 calc R U . . .
C8 C 0.4049(4) 0.7168(3) -0.0317(3) 0.047(3) Uani 1 1 d . . . . .
C9 C 0.4737(4) 0.6561(4) -0.0179(4) 0.062(4) Uani 1 1 d . . . . .
H9A H 0.4981 0.6447 -0.0254 0.074 Uiso 1 1 calc R U . . .
H9B H 0.4594 0.6373 -0.0028 0.074 Uiso 1 1 calc R U . . .
C10 C 0.4808(4) 0.6918(4) 0.0059(4) 0.051(3) Uani 1 1 d . U . . .
H10A H 0.4566 0.7015 0.0162 0.061 Uiso 1 1 calc R U . . .
H10B H 0.4978 0.6859 0.0273 0.061 Uiso 1 1 calc R U . . .
C11 C 0.3813(4) 0.7034(3) 0.0793(4) 0.053(4) Uani 1 1 d . . . . .
H11A H 0.3911 0.6844 0.0611 0.063 Uiso 1 1 calc R U . . .
H11B H 0.3789 0.6908 0.1041 0.063 Uiso 1 1 calc R U . . .
C12 C 0.4109(4) 0.7364(3) 0.0828(4) 0.049(4) Uani 1 1 d . . . . .
C13 C 0.3246(3) 0.6854(3) 0.0452(4) 0.044(3) Uani 1 1 d . . . . .
H13A H 0.3127 0.6671 0.0627 0.053 Uiso 1 1 calc R U . . .
H13B H 0.3431 0.6716 0.0294 0.053 Uiso 1 1 calc R U . . .
C14 C 0.2948(3) 0.7034(3) 0.0204(3) 0.038(3) Uani 1 1 d . . . . .
C15 C 0.3206(4) 0.7231(4) 0.0995(4) 0.057(4) Uani 1 1 d . . . . .
H15A H 0.3247 0.7033 0.1188 0.068 Uiso 1 1 calc R U . . .
H15B H 0.2936 0.7224 0.0920 0.068 Uiso 1 1 calc R U . . .
C16 C 0.3300(3) 0.7621(4) 0.1163(3) 0.053(4) Uani 1 1 d . . . . .
H16A H 0.3148 0.7659 0.1395 0.064 Uiso 1 1 calc R U . . .
H16B H 0.3570 0.7625 0.1236 0.064 Uiso 1 1 calc R U . . .
C17 C 0.2839(4) 0.8053(4) 0.0851(4) 0.063(4) Uani 1 1 d . . . . .
H17A H 0.2790 0.8276 0.1012 0.076 Uiso 1 1 calc R U . . .
H17B H 0.2680 0.7843 0.0944 0.076 Uiso 1 1 calc R U . . .
C18 C 0.2729(4) 0.8140(4) 0.0473(4) 0.053(4) Uani 1 1 d . . . . .
C19 C 0.3463(5) 0.8282(5) 0.1033(5) 0.076(4) Uani 1 1 d . U . . .
H19A H 0.3724 0.8197 0.1089 0.091 Uiso 1 1 calc R U . . .
H19B H 0.3351 0.8388 0.1267 0.091 Uiso 1 1 calc R U . . .
C20 C 0.3464(5) 0.8580(5) 0.0717(5) 0.098(6) Uani 1 1 d . . . . .
H20A H 0.3202 0.8652 0.0651 0.118 Uiso 1 1 calc R U . . .
H20B H 0.3601 0.8810 0.0801 0.118 Uiso 1 1 calc R U . . .
O2W O 0.3381(3) 0.7865(3) -0.0437(3) 0.079(3) Uani 1 1 d . . . . .
O1W O 0.5172(3) 0.7467(4) -0.1393(3) 0.092(4) Uani 1 1 d . U . . .
O3W O 0.4097(3) 0.8012(3) -0.0094(3) 0.070(3) Uani 1 1 d . . . . .
O4W O 0.4404(3) 0.7911(3) 0.1590(3) 0.080(3) Uani 1 1 d . . . . .
O5W O 0.5567(3) 0.7443(3) 0.1388(3) 0.063(3) Uani 1 1 d . . . . .
O6W O 0.6312(5) 0.6392(5) -0.0383(5) 0.149(6) Uani 1 1 d . U . . .
O8W O 0.6690(18) 0.5706(18) -0.1482(18) 0.272(9) Uani 0.5 1 d . U P . .
O9W O 0.6384(10) 0.6808(9) -0.1119(10) 0.138(8) Uani 0.5 1 d . U P . .
O10W O 0.6892(9) 0.6268(10) -0.0921(9) 0.137(8) Uani 0.5 1 d . U P . .
O11W O 0.5766(9) 0.5967(10) -0.0583(9) 0.148(11) Uani 0.5 1 d D U P A 1
O7W O 0.5922(6) 0.5873(5) -0.1398(6) 0.182(6) Uani 1 1 d . U . A 1
O12W O 0.6140(12) 0.6174(11) -0.1693(11) 0.179(9) Uani 0.5 1 d . U P A 2
O14W O 0.6046(7) 0.5939(7) -0.0853(8) 0.114(8) Uani 0.5 1 d D U P A 2
O13W O 0.6514(11) 0.5699(11) -0.0596(11) 0.164(8) Uani 0.5 1 d . 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
Dy1 O1 2.284(10) . ?
Dy1 O3 2.338(11) . ?
Dy1 O7 2.359(8) . ?
Dy1 O5 2.394(10) . ?
Dy1 O13 2.423(10) 17 ?
Dy1 O1W 2.435(11) . ?
Dy1 N1 2.625(14) . ?
Dy1 N2 2.643(11) . ?
Dy1 O12 2.716(10) 17 ?
Dy1 C18 2.961(13) 17 ?
Dy2 O10 2.327(9) . ?
Dy2 O6 2.357(8) . ?
Dy2 O8 2.394(9) . ?
Dy2 O2W 2.418(10) . ?
Dy2 O14 2.439(10) . ?
Dy2 O12 2.456(10) . ?
Dy2 O3W 2.485(9) . ?
Dy2 N3 2.659(11) . ?
Dy2 N4 2.680(10) . ?
Dy3 O11 2.274(9) 17 ?
Dy3 O11 2.274(9) 7_564 ?
Dy3 O9 2.294(8) . ?
Dy3 O9 2.294(8) 14_665 ?
Dy3 O5W 2.409(9) . ?
Dy3 O5W 2.409(9) 14_665 ?
Dy3 O4W 2.460(10) 14_665 ?
Dy3 O4W 2.460(10) . ?
Dy4 O7W 2.03(2) . ?
Dy4 O13W 2.18(4) . ?
Dy4 O4 2.250(18) . ?
Dy4 O11W 2.30(3) . ?
Dy4 O10W 2.33(3) . ?
Dy4 O6W 2.388(17) . ?
Dy4 O9W 2.58(3) . ?
Dy4 O8W 2.70(6) . ?
Na1 O12W 1.90(4) . ?
Na1 O14W 1.93(3) . ?
Na1 O9W 2.00(4) . ?
Na1 O10W 2.20(3) . ?
Na1 O4 2.31(2) . ?
Na1 O8W 2.51(7) . ?
Na1 O6W 2.92(2) . ?
Na1 O13W 2.96(4) . ?
Cl1 O16 1.34(2) . ?
Cl1 O18 1.383(13) . ?
Cl1 O17 1.406(15) . ?
Cl1 O15 1.47(3) . ?
Cl2 O19 1.315(15) . ?
Cl2 O20' 1.33(3) . ?
Cl2 O21 1.35(2) . ?
Cl2 O22' 1.40(3) . ?
Cl2 O22 1.41(4) . ?
Cl2 O20 1.48(2) . ?
Cl2 O21' 1.60(2) . ?
O1 C2 1.37(2) . ?
O2 C2 1.15(2) . ?
O3 C4 1.46(2) . ?
O4 C4 1.18(2) . ?
O6 C8 1.225(15) . ?
O5 C8 1.259(15) . ?
O7 C10 1.469(15) . ?
O7 H7C 0.9500 . ?
O9 C12 1.203(15) . ?
O8 C12 1.213(15) . ?
O10 C14 1.265(14) . ?
O11 C14 1.220(14) . ?
O11 Dy3 2.274(9) 10_655 ?
O12 C18 1.240(17) . ?
O12 Dy1 2.716(10) 20_454 ?
O13 C18 1.331(15) . ?
O13 Dy1 2.423(10) 20_454 ?
O14 C20 1.42(2) . ?
O14 H14A 0.9500 . ?
N1 C5 1.46(2) . ?
N1 C3 1.471(17) . ?
N1 C1 1.492(16) . ?
N4 C15 1.441(17) . ?
N4 C11 1.455(16) . ?
N4 C13 1.479(15) . ?
N3 C17 1.415(17) . ?
N3 C16 1.532(17) . ?
N3 C19 1.533(19) . ?
N2 C9 1.429(18) . ?
N2 C6 1.47(2) . ?
N2 C7 1.487(18) . ?
C3 C4 1.498(19) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C1 C2 1.467(18) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C5 C6 1.48(3) . ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
C6 H6A 0.9900 . ?
C6 H6B 0.9900 . ?
C7 C8 1.509(19) . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C9 C10 1.535(18) . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C11 C12 1.573(18) . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C13 C14 1.513(16) . ?
C13 H13A 0.9900 . ?
C13 H13B 0.9900 . ?
C15 C16 1.541(19) . ?
C15 H15A 0.9900 . ?
C15 H15B 0.9900 . ?
C16 H16A 0.9900 . ?
C16 H16B 0.9900 . ?
C17 C18 1.42(2) . ?
C17 H17A 0.9900 . ?
C17 H17B 0.9900 . ?
C18 Dy1 2.961(13) 20_454 ?
C19 C20 1.54(2) . ?
C19 H19A 0.9900 . ?
C19 H19B 0.9900 . ?
C20 H20A 0.9900 . ?
C20 H20B 0.9900 . ?

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 O3 131.0(4) . . ?
O1 Dy1 O7 147.3(4) . . ?
O3 Dy1 O7 76.2(4) . . ?
O1 Dy1 O5 73.8(4) . . ?
O3 Dy1 O5 140.1(4) . . ?
O7 Dy1 O5 73.5(3) . . ?
O1 Dy1 O13 87.2(5) . 17 ?
O3 Dy1 O13 125.8(3) . 17 ?
O7 Dy1 O13 88.4(3) . 17 ?
O5 Dy1 O13 78.7(3) . 17 ?
O1 Dy1 O1W 76.2(4) . . ?
O3 Dy1 O1W 78.2(4) . . ?
O7 Dy1 O1W 133.8(3) . . ?
O5 Dy1 O1W 141.6(4) . . ?
O13 Dy1 O1W 76.4(4) 17 . ?
O1 Dy1 N1 65.2(5) . . ?
O3 Dy1 N1 67.7(4) . . ?
O7 Dy1 N1 128.2(4) . . ?
O5 Dy1 N1 113.7(3) . . ?
O13 Dy1 N1 142.9(4) 17 . ?
O1W Dy1 N1 73.4(4) . . ?
O1 Dy1 N2 98.8(5) . . ?
O3 Dy1 N2 77.7(4) . . ?
O7 Dy1 N2 66.1(3) . . ?
O5 Dy1 N2 66.6(3) . . ?
O13 Dy1 N2 141.3(3) 17 . ?
O1W Dy1 N2 142.3(4) . . ?
N1 Dy1 N2 70.7(4) . . ?
O1 Dy1 O12 130.6(4) . 17 ?
O3 Dy1 O12 75.5(3) . 17 ?
O7 Dy1 O12 66.7(3) . 17 ?
O5 Dy1 O12 114.1(3) . 17 ?
O13 Dy1 O12 51.0(3) 17 17 ?
O1W Dy1 O12 70.1(3) . 17 ?
N1 Dy1 O12 132.2(4) . 17 ?
N2 Dy1 O12 129.8(3) . 17 ?
O1 Dy1 C18 110.7(5) . 17 ?
O3 Dy1 C18 100.1(4) . 17 ?
O7 Dy1 C18 75.1(3) . 17 ?
O5 Dy1 C18 96.5(3) . 17 ?
O13 Dy1 C18 26.3(3) 17 17 ?
O1W Dy1 C18 72.4(4) . 17 ?
N1 Dy1 C18 145.4(4) . 17 ?
N2 Dy1 C18 140.6(4) . 17 ?
O12 Dy1 C18 24.7(3) 17 17 ?
O10 Dy2 O6 79.3(3) . . ?
O10 Dy2 O8 127.2(3) . . ?
O6 Dy2 O8 79.9(3) . . ?
O10 Dy2 O2W 76.4(3) . . ?
O6 Dy2 O2W 76.6(3) . . ?
O8 Dy2 O2W 142.3(3) . . ?
O10 Dy2 O14 137.9(3) . . ?
O6 Dy2 O14 140.9(3) . . ?
O8 Dy2 O14 82.1(3) . . ?
O2W Dy2 O14 98.2(4) . . ?
O10 Dy2 O12 67.8(3) . . ?
O6 Dy2 O12 138.8(3) . . ?
O8 Dy2 O12 140.0(3) . . ?
O2W Dy2 O12 72.2(3) . . ?
O14 Dy2 O12 70.8(3) . . ?
O10 Dy2 O3W 141.5(3) . . ?
O6 Dy2 O3W 73.5(3) . . ?
O8 Dy2 O3W 74.2(3) . . ?
O2W Dy2 O3W 71.2(3) . . ?
O14 Dy2 O3W 68.3(3) . . ?
O12 Dy2 O3W 119.1(3) . . ?
O10 Dy2 N3 88.5(3) . . ?
O6 Dy2 N3 139.9(3) . . ?
O8 Dy2 N3 77.6(3) . . ?
O2W Dy2 N3 137.4(3) . . ?
O14 Dy2 N3 67.2(4) . . ?
O12 Dy2 N3 65.2(3) . . ?
O3W Dy2 N3 129.6(3) . . ?
O10 Dy2 N4 62.5(3) . . ?
O6 Dy2 N4 71.8(3) . . ?
O8 Dy2 N4 65.0(3) . . ?
O2W Dy2 N4 131.6(3) . . ?
O14 Dy2 N4 129.3(4) . . ?
O12 Dy2 N4 111.0(3) . . ?
O3W Dy2 N4 129.8(3) . . ?
N3 Dy2 N4 68.7(3) . . ?
O11 Dy3 O11 149.1(5) 17 7_564 ?
O11 Dy3 O9 93.6(3) 17 . ?
O11 Dy3 O9 95.0(3) 7_564 . ?
O11 Dy3 O9 95.0(3) 17 14_665 ?
O11 Dy3 O9 93.6(3) 7_564 14_665 ?
O9 Dy3 O9 147.0(4) . 14_665 ?
O11 Dy3 O5W 78.2(3) 17 . ?
O11 Dy3 O5W 76.5(4) 7_564 . ?
O9 Dy3 O5W 141.1(3) . . ?
O9 Dy3 O5W 71.9(3) 14_665 . ?
O11 Dy3 O5W 76.5(4) 17 14_665 ?
O11 Dy3 O5W 78.2(3) 7_564 14_665 ?
O9 Dy3 O5W 71.9(3) . 14_665 ?
O9 Dy3 O5W 141.1(3) 14_665 14_665 ?
O5W Dy3 O5W 69.1(5) . 14_665 ?
O11 Dy3 O4W 73.9(4) 17 14_665 ?
O11 Dy3 O4W 137.0(4) 7_564 14_665 ?
O9 Dy3 O4W 76.4(3) . 14_665 ?
O9 Dy3 O4W 75.6(3) 14_665 14_665 ?
O5W Dy3 O4W 134.5(3) . 14_665 ?
O5W Dy3 O4W 134.6(3) 14_665 14_665 ?
O11 Dy3 O4W 137.0(4) 17 . ?
O11 Dy3 O4W 73.9(4) 7_564 . ?
O9 Dy3 O4W 75.6(3) . . ?
O9 Dy3 O4W 76.4(3) 14_665 . ?
O5W Dy3 O4W 134.6(3) . . ?
O5W Dy3 O4W 134.5(3) 14_665 . ?
O4W Dy3 O4W 63.1(5) 14_665 . ?
O7W Dy4 O13W 116.0(12) . . ?
O7W Dy4 O4 65.5(6) . . ?
O13W Dy4 O4 140.6(11) . . ?
O7W Dy4 O11W 85.5(10) . . ?
O13W Dy4 O11W 77.5(13) . . ?
O4 Dy4 O11W 63.1(10) . . ?
O7W Dy4 O10W 137.4(10) . . ?
O13W Dy4 O10W 72.5(13) . . ?
O4 Dy4 O10W 135.6(10) . . ?
O11W Dy4 O10W 135.4(12) . . ?
O7W Dy4 O6W 148.7(7) . . ?
O13W Dy4 O6W 71.0(11) . . ?
O4 Dy4 O6W 89.6(6) . . ?
O11W Dy4 O6W 65.7(9) . . ?
O10W Dy4 O6W 73.6(9) . . ?
O7W Dy4 O9W 111.0(9) . . ?
O13W Dy4 O9W 132.0(13) . . ?
O4 Dy4 O9W 69.2(9) . . ?
O11W Dy4 O9W 115.9(12) . . ?
O10W Dy4 O9W 66.8(11) . . ?
O6W Dy4 O9W 74.1(9) . . ?
O7W Dy4 O8W 70.7(15) . . ?
O13W Dy4 O8W 80.9(18) . . ?
O4 Dy4 O8W 129.8(15) . . ?
O11W Dy4 O8W 136.4(16) . . ?
O10W Dy4 O8W 69.8(16) . . ?
O6W Dy4 O8W 139.1(15) . . ?
O9W Dy4 O8W 106.7(16) . . ?
O12W Na1 O14W 108.1(17) . . ?
O12W Na1 O9W 107.6(17) . . ?
O14W Na1 O9W 121.3(14) . . ?
O12W Na1 O10W 137.3(16) . . ?
O14W Na1 O10W 102.0(13) . . ?
O9W Na1 O10W 80.3(14) . . ?
O12W Na1 O4 81.3(14) . . ?
O14W Na1 O4 62.1(9) . . ?
O9W Na1 O4 79.4(12) . . ?
O10W Na1 O4 140.5(11) . . ?
O12W Na1 O8W 72.6(19) . . ?
O14W Na1 O8W 94.6(17) . . ?
O9W Na1 O8W 140.2(19) . . ?
O10W Na1 O8W 75.6(18) . . ?
O4 Na1 O8W 137.4(16) . . ?
O12W Na1 O6W 157.4(14) . . ?
O14W Na1 O6W 57.5(10) . . ?
O9W Na1 O6W 72.3(11) . . ?
O10W Na1 O6W 65.3(10) . . ?
O4 Na1 O6W 76.4(7) . . ?
O8W Na1 O6W 122.6(16) . . ?
O12W Na1 O13W 130.3(16) . . ?
O14W Na1 O13W 44.2(11) . . ?
O9W Na1 O13W 122.1(14) . . ?
O10W Na1 O13W 60.4(12) . . ?
O4 Na1 O13W 104.3(10) . . ?
O8W Na1 O13W 71.0(17) . . ?
O6W Na1 O13W 53.8(9) . . ?
O16 Cl1 O18 125.6(12) . . ?
O16 Cl1 O17 107.3(12) . . ?
O18 Cl1 O17 111.5(9) . . ?
O16 Cl1 O15 95.6(14) . . ?
O18 Cl1 O15 112.8(13) . . ?
O17 Cl1 O15 100.3(13) . . ?
O19 Cl2 O20' 105.3(15) . . ?
O19 Cl2 O21 117.7(12) . . ?
O19 Cl2 O22' 119.0(19) . . ?
O20' Cl2 O22' 119(2) . . ?
O19 Cl2 O22 106.2(17) . . ?
O21 Cl2 O22 96.9(17) . . ?
O19 Cl2 O20 120.6(11) . . ?
O21 Cl2 O20 106.6(13) . . ?
O22 Cl2 O20 105.3(18) . . ?
O19 Cl2 O21' 117.0(11) . . ?
O20' Cl2 O21' 99.8(16) . . ?
O22' Cl2 O21' 95.3(18) . . ?
C2 O1 Dy1 122.1(10) . . ?
C4 O3 Dy1 127.6(10) . . ?
C4 O4 Dy4 173.3(18) . . ?
C4 O4 Na1 162.2(17) . . ?
C8 O6 Dy2 141.6(8) . . ?
C8 O5 Dy1 126.9(8) . . ?
C10 O7 Dy1 122.8(7) . . ?
C10 O7 H7C 118.6 . . ?
Dy1 O7 H7C 118.6 . . ?
C12 O9 Dy3 140.3(8) . . ?
C12 O8 Dy2 128.8(8) . . ?
C14 O10 Dy2 129.7(7) . . ?
C14 O11 Dy3 148.8(8) . 10_655 ?
C18 O12 Dy2 117.9(9) . . ?
C18 O12 Dy1 88.8(8) . 20_454 ?
Dy2 O12 Dy1 147.6(4) . 20_454 ?
C18 O13 Dy1 100.1(8) . 20_454 ?
C20 O14 Dy2 120.1(9) . . ?
C20 O14 H14A 119.9 . . ?
Dy2 O14 H14A 119.9 . . ?
C5 N1 C3 108.1(14) . . ?
C5 N1 C1 113.0(13) . . ?
C3 N1 C1 107.2(12) . . ?
C5 N1 Dy1 108.6(10) . . ?
C3 N1 Dy1 109.8(10) . . ?
C1 N1 Dy1 110.0(9) . . ?
C15 N4 C11 109.7(10) . . ?
C15 N4 C13 106.4(9) . . ?
C11 N4 C13 111.4(9) . . ?
C15 N4 Dy2 112.4(8) . . ?
C11 N4 Dy2 108.2(7) . . ?
C13 N4 Dy2 108.8(7) . . ?
C17 N3 C16 115.3(11) . . ?
C17 N3 C19 111.3(11) . . ?
C16 N3 C19 106.0(10) . . ?
C17 N3 Dy2 111.0(8) . . ?
C16 N3 Dy2 107.4(7) . . ?
C19 N3 Dy2 105.3(8) . . ?
C9 N2 C6 111.1(11) . . ?
C9 N2 C7 113.5(11) . . ?
C6 N2 C7 109.1(11) . . ?
C9 N2 Dy1 110.5(8) . . ?
C6 N2 Dy1 106.0(9) . . ?
C7 N2 Dy1 106.2(8) . . ?
N1 C3 C4 121.4(15) . . ?
N1 C3 H3A 107.0 . . ?
C4 C3 H3A 107.0 . . ?
N1 C3 H3B 107.0 . . ?
C4 C3 H3B 107.0 . . ?
H3A C3 H3B 106.7 . . ?
O4 C4 O3 113.7(16) . . ?
O4 C4 C3 136(2) . . ?
O3 C4 C3 109.6(16) . . ?
C2 C1 N1 107.2(13) . . ?
C2 C1 H1A 110.3 . . ?
N1 C1 H1A 110.3 . . ?
C2 C1 H1B 110.3 . . ?
N1 C1 H1B 110.3 . . ?
H1A C1 H1B 108.5 . . ?
O2 C2 O1 119.8(17) . . ?
O2 C2 C1 118.1(18) . . ?
O1 C2 C1 121.3(15) . . ?
N1 C5 C6 112.5(14) . . ?
N1 C5 H5A 109.1 . . ?
C6 C5 H5A 109.1 . . ?
N1 C5 H5B 109.1 . . ?
C6 C5 H5B 109.1 . . ?
H5A C5 H5B 107.8 . . ?
N2 C6 C5 119.8(16) . . ?
N2 C6 H6A 107.4 . . ?
C5 C6 H6A 107.4 . . ?
N2 C6 H6B 107.4 . . ?
C5 C6 H6B 107.4 . . ?
H6A C6 H6B 106.9 . . ?
N2 C7 C8 115.9(11) . . ?
N2 C7 H7A 108.3 . . ?
C8 C7 H7A 108.3 . . ?
N2 C7 H7B 108.3 . . ?
C8 C7 H7B 108.3 . . ?
H7A C7 H7B 107.4 . . ?
O6 C8 O5 125.6(12) . . ?
O6 C8 C7 120.3(11) . . ?
O5 C8 C7 114.0(12) . . ?
N2 C9 C10 108.8(11) . . ?
N2 C9 H9A 109.9 . . ?
C10 C9 H9A 109.9 . . ?
N2 C9 H9B 109.9 . . ?
C10 C9 H9B 109.9 . . ?
H9A C9 H9B 108.3 . . ?
O7 C10 C9 107.8(10) . . ?
O7 C10 H10A 110.2 . . ?
C9 C10 H10A 110.2 . . ?
O7 C10 H10B 110.2 . . ?
C9 C10 H10B 110.2 . . ?
H10A C10 H10B 108.5 . . ?
N4 C11 C12 114.2(10) . . ?
N4 C11 H11A 108.7 . . ?
C12 C11 H11A 108.7 . . ?
N4 C11 H11B 108.7 . . ?
C12 C11 H11B 108.7 . . ?
H11A C11 H11B 107.6 . . ?
O9 C12 O8 128.9(12) . . ?
O9 C12 C11 115.4(11) . . ?
O8 C12 C11 115.6(12) . . ?
N4 C13 C14 108.7(9) . . ?
N4 C13 H13A 109.9 . . ?
C14 C13 H13A 109.9 . . ?
N4 C13 H13B 109.9 . . ?
C14 C13 H13B 109.9 . . ?
H13A C13 H13B 108.3 . . ?
O11 C14 O10 127.0(11) . . ?
O11 C14 C13 116.8(10) . . ?
O10 C14 C13 116.2(10) . . ?
N4 C15 C16 110.5(10) . . ?
N4 C15 H15A 109.5 . . ?
C16 C15 H15A 109.5 . . ?
N4 C15 H15B 109.5 . . ?
C16 C15 H15B 109.5 . . ?
H15A C15 H15B 108.1 . . ?
N3 C16 C15 113.4(10) . . ?
N3 C16 H16A 108.9 . . ?
C15 C16 H16A 108.9 . . ?
N3 C16 H16B 108.9 . . ?
C15 C16 H16B 108.9 . . ?
H16A C16 H16B 107.7 . . ?
N3 C17 C18 114.4(12) . . ?
N3 C17 H17A 108.7 . . ?
C18 C17 H17A 108.7 . . ?
N3 C17 H17B 108.7 . . ?
C18 C17 H17B 108.7 . . ?
H17A C17 H17B 107.6 . . ?
O12 C18 O13 120.0(13) . . ?
O12 C18 C17 126.6(12) . . ?
O13 C18 C17 113.3(12) . . ?
O12 C18 Dy1 66.5(7) . 20_454 ?
O13 C18 Dy1 53.7(7) . 20_454 ?
C17 C18 Dy1 166.8(10) . 20_454 ?
N3 C19 C20 106.7(13) . . ?
N3 C19 H19A 110.4 . . ?
C20 C19 H19A 110.4 . . ?
N3 C19 H19B 110.4 . . ?
C20 C19 H19B 110.4 . . ?
H19A C19 H19B 108.6 . . ?
O14 C20 C19 107.4(14) . . ?
O14 C20 H20A 110.2 . . ?
C19 C20 H20A 110.2 . . ?
O14 C20 H20B 110.2 . . ?
C19 C20 H20B 110.2 . . ?
H20A C20 H20B 108.5 . . ?

_refine_diff_density_max         3.263
_refine_diff_density_min         -0.707
_refine_diff_density_rms         0.156


# SQUEEZE RESULTS (APPEND TO CIF)
# Note: Data are Listed for all Voids in the P1 Unit Cell
# i.e. Centre of Gravity, Solvent Accessible Volume,
# Recovered number of Electrons in the Void and
# Details about the Squeezed Material
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 0.081 0.073 0.080 19345 3375 ' '
2 0.936 0.064 0.564 10 2 ' '
3 0.686 0.186 0.314 10 2 ' '
4 0.186 0.314 0.686 10 2 ' '
5 0.436 0.436 0.436 10 2 ' '
6 0.064 0.564 0.936 10 2 ' '
7 0.314 0.686 0.186 10 2 ' '
8 0.814 0.814 0.814 10 2 ' '
9 0.564 0.936 0.064 10 2 ' '
_platon_squeeze_details          
;
;

# compound-1b RESULTS (APPEND TO CIF)

_platon_compound-1b_details      
;
According to the charge balance, there are 2 ClO4- counter anions per formula units.
 Based on the EA and TGA analysis, there are 15 guest water molecules per formula units.
 However, they are however severely disordered and were therefore removed by SQUEEZE 
in structural refinement. The SQUEEZE analysis estimate the electron count to be 3396 
within 19941 A3 void per formula unit for 1b. According to the electron counts and 
the void per formula unit, the number of guest water is 18, which is consistent with
 the number calculated from EA and TGA results.
;

_vrf_CHEMW03_compound-1b         
;
PROBLEM: ALERT The ratio of given/expected molecular weight as
RESPONSE: This is caused by the given molecular weight being increased 
from the atom count to account for two ClO4- and 15 water molecules per formula unit.
This value is calculated based upon elemental analysis data and TGA data.
;

_vrf_PLAT043_compound-1b         
;
PROBLEM: Check Reported Molecular Weight ................   
RESPONSE: This is caused by the given molecular weight being increased 
from the atom count to account for two ClO4- and 15 water molecules per formula unit. 
This valueis calculated based upon elemental analysis data and TGA data.
;

_vrf_PLAT602_compound-1b         
;
PROBLEM: very large Solvent Accessible VOIDS in structure.       
RESPONSE: This is caused by two ClO4- and 15 water molecules per formula unit was omitted in refinement. 
;

_vrf_PLAT420_compound-1b         
;
PROBLEM: D-H Without Acceptor   O14    -   H14A 
RESPONSE: This is caused by the water molecules were removed in refinement. 
;

# end Validation Reply Form


_shelxl_version_number           2013-2

