# Electronic Supplementary Material (ESI) for New Journal of Chemistry.
# This journal is © The Royal Society of Chemistry and the Centre National de la Recherche Scientifique 2019

####################################################################### 
# 
# 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_t1_sq
_database_code_depnum_ccdc_archive 'CCDC 1921957'
loop_
_audit_author_name
_audit_author_address
'Yuan Huang'
;Soochow university
China
;
_audit_update_record             
;
2019-11-06 deposited with the CCDC.	2019-11-13 downloaded from the CCDC.
;
_audit_creation_date             2019-10-31
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2014/7
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C144 H168 Gd9 N16 O42, H3 O, 4(H2O)'
_chemical_formula_sum            'C144 H179 Gd9 N16 O47'
_chemical_formula_weight         4305.53
_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'
Gd Gd -0.1653 3.9035 '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'

_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           85
_space_group_name_H-M_alt        'P 4/n'
_space_group_name_Hall           '-P 4a'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y+1/2, z'
'-y+1/2, x, z'
'y, -x+1/2, z'
'-x, -y, -z'
'x-1/2, y-1/2, -z'
'y-1/2, -x, -z'
'-y, x-1/2, -z'

_cell_length_a                   21.6307(4)
_cell_length_b                   21.6307(4)
_cell_length_c                   17.8974(7)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     8374.0(5)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    9966
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      2.39
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    3.586
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.4893
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.1410 before and 0.0675 after correction.
The Ratio of minimum to maximum transmission is 0.6562.
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    1.670
_exptl_crystal_density_meas      .
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             4112
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.2
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0716
_diffrn_reflns_av_unetI/netI     0.0716
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            25326
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.672
_diffrn_reflns_theta_min         2.393
_diffrn_ambient_temperature      296.15
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                6036
_reflns_number_total             7925
_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 v8.37A (Bruker, 2015)'
_computing_data_collection       'Bruker SMART APEX II'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_refine_diff_density_max         2.446
_refine_diff_density_min         -1.368
_refine_diff_density_rms         0.251
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.145
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     492
_refine_ls_number_reflns         7925
_refine_ls_number_restraints     9
_refine_ls_R_factor_all          0.1013
_refine_ls_R_factor_gt           0.0758
_refine_ls_restrained_S_all      1.145
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0001P)²+385.1630P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1704
_refine_ls_wR_factor_ref         0.1829
_refine_special_details          
;
The SQUEEZE routine of PLATON was used in the treatment of the crystallographic data. The identities and numbers of the lattice solvents were determined by the TGA and elemental analysis. The calculated mass loss corresponding to the solvent guests from the crystals between 22 and 100?ãC was 2.11%. However, the experimental result 2.34% was nearly consistent with calculated result. This indicates that four mole of water molecule and one hydronium ion might be lost during the test process and elemental analysis results of C 40.21, H 4.19, N 5.21, which are consistent with the experimental data.
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 N4-C35
 1.498 with sigma of 0.02
 O3-H3
 0.8 with sigma of 0.02
3. Rigid bond restraints
 C34, O9
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
4. Uiso/Uaniso restraints and constraints
Uanis(C36) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
5.a Secondary CH2 refined with riding coordinates:
 C10(H10A,H10B), C26(H26A,H26B)
5.b Aromatic/amide H refined with riding coordinates:
 C2(H2A), C5(H5), C6(H6), C7(H7), C11(H11), C12(H12), C13(H13), C14(H14),
 C17(H17), C21(H21), C22(H22), C24(H24), C25(H25), C27(H27), C28(H28), C29(H29),
  C31(H31), C34(H34)
5.c Idealised Me refined as rotating group:
 C19(H19A,H19B,H19C), C30(H30A,H30B,H30C), C32(H32A,H32B,H32C), C33(H33A,H33B,
 H33C), C35(H35A,H35B,H35C), C36(H36A,H36B,H36C)
;
_atom_sites_solution_hydrogens   mixed
_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
Gd1 Gd 0.7500 0.7500 0.71301(7) 0.0159(3) Uani 1 4 d S T P . .
Gd2 Gd 0.63532(3) 0.78351(3) 0.86171(4) 0.01834(17) Uani 1 1 d . . . . .
Gd3 Gd 0.64244(3) 0.69711(3) 0.56476(4) 0.01815(17) Uani 1 1 d . . . . .
O1 O 0.7500 0.7500 0.8695(9) 0.016(4) Uani 1 4 d S T P . .
O2 O 0.6571(4) 0.7807(5) 0.6449(5) 0.018(2) Uani 1 1 d . . . . .
O3 O 0.6640(4) 0.7039(4) 0.7821(5) 0.018(2) Uani 1 1 d D . . . .
O4 O 0.7500 0.7500 0.5549(11) 0.021(4) Uani 1 4 d S T P . .
O5 O 0.6443(4) 0.7841(5) 0.4844(5) 0.023(2) Uani 1 1 d . . . . .
O6 O 0.6525(4) 0.6987(4) 0.9427(5) 0.023(2) Uani 1 1 d . . . . .
O7 O 0.5891(5) 0.6543(5) 0.6600(5) 0.029(2) Uani 1 1 d . . . . .
O8 O 0.5737(5) 0.8184(5) 0.7686(5) 0.029(2) Uani 1 1 d . . . . .
O9 O 0.5658(5) 0.8411(6) 0.9409(7) 0.043(3) Uani 1 1 d . U . . .
O10 O 0.5851(5) 0.6259(6) 0.4892(6) 0.039(3) Uani 1 1 d . . . . .
N1 N 0.5296(5) 0.7360(5) 0.5585(7) 0.022(3) Uani 1 1 d . . . . .
C1 C 0.5425(7) 0.7843(7) 0.4327(8) 0.027(3) Uani 1 1 d . . . . .
O11 O 0.4337(5) 0.9030(6) 0.5997(6) 0.038(3) Uani 1 1 d . . . . .
C2 C 0.5000(7) 0.8603(6) 0.6860(8) 0.026(3) Uani 1 1 d . . . . .
H2A H 0.5299 0.8852 0.6639 0.031 Uiso 1 1 calc R . . . .
C3 C 0.6058(7) 0.7845(7) 0.4247(8) 0.026(3) Uani 1 1 d . . . . .
C4 C 0.5318(7) 0.6395(7) 0.6792(8) 0.024(3) Uani 1 1 d . . . . .
N2 N 0.5541(7) 0.5748(6) 0.3847(7) 0.034(3) Uani 1 1 d . . . . .
C5 C 0.4819(7) 0.7114(6) 0.5928(8) 0.023(3) Uani 1 1 d . . . . .
H5 H 0.4438 0.7283 0.5800 0.028 Uiso 1 1 calc R . . . .
C6 C 0.6308(8) 0.7850(7) 0.3518(8) 0.028(3) Uani 1 1 d . . . . .
H6 H 0.6733 0.7868 0.3446 0.033 Uiso 1 1 calc R . . . .
N3 N 0.5312(6) 0.7230(5) 0.8660(7) 0.026(3) Uani 1 1 d . . . . .
C7 C 0.5256(7) 0.5966(7) 0.7400(8) 0.028(3) Uani 1 1 d . . . . .
H7 H 0.5604 0.5812 0.7642 0.034 Uiso 1 1 calc R . . . .
O12 O 0.4566(6) 0.5373(6) 0.8189(7) 0.045(3) Uani 1 1 d . . . . .
C8 C 0.5176(7) 0.8213(7) 0.7457(8) 0.024(3) Uani 1 1 d . . . . .
C9 C 0.6146(7) 0.6887(6) 1.0014(7) 0.021(3) Uani 1 1 d . . . . .
C10 C 0.5165(7) 0.7906(7) 0.5122(8) 0.027(3) Uani 1 1 d . . . . .
H10A H 0.5343 0.8268 0.5357 0.032 Uiso 1 1 calc R . . . .
H10B H 0.4721 0.7966 0.5094 0.032 Uiso 1 1 calc R . . . .
C11 C 0.6380(8) 0.6893(7) 1.0732(8) 0.030(3) Uani 1 1 d . . . . .
H11 H 0.6800 0.6963 1.0807 0.036 Uiso 1 1 calc R . . . .
C12 C 0.4802(7) 0.7371(7) 0.8303(9) 0.027(3) Uani 1 1 d . . . . .
H12 H 0.4458 0.7135 0.8429 0.033 Uiso 1 1 calc R . . . .
C13 C 0.5991(7) 0.6795(8) 1.1353(10) 0.035(4) Uani 1 1 d . . . . .
H13 H 0.6145 0.6813 1.1837 0.042 Uiso 1 1 calc R . . . .
C14 C 0.5724(7) 0.6229(8) 0.4220(9) 0.030(4) Uani 1 1 d . . . . .
H14 H 0.5763 0.6594 0.3950 0.036 Uiso 1 1 calc R . . . .
C15 C 0.5520(8) 0.6739(7) 0.9867(9) 0.029(3) Uani 1 1 d . . . . .
C16 C 0.4794(7) 0.6642(7) 0.6450(9) 0.031(3) Uani 1 1 d . . . . .
C17 C 0.5038(8) 0.7830(8) 0.3719(10) 0.036(4) Uani 1 1 d . . . . .
H17 H 0.4612 0.7827 0.3786 0.044 Uiso 1 1 calc R . . . .
C18 C 0.4671(8) 0.5785(7) 0.7620(9) 0.031(4) Uani 1 1 d . . . . .
C19 C 0.5525(9) 0.5141(9) 0.4184(10) 0.047(5) Uani 1 1 d . . . . .
H19A H 0.5661 0.5168 0.4694 0.070 Uiso 1 1 calc GR . . . .
H19B H 0.5792 0.4867 0.3913 0.070 Uiso 1 1 calc GR . . . .
H19C H 0.5110 0.4984 0.4170 0.070 Uiso 1 1 calc GR . . . .
C20 C 0.4699(7) 0.7832(7) 0.7752(9) 0.028(3) Uani 1 1 d . . . . .
C21 C 0.5917(9) 0.7827(7) 0.2922(8) 0.037(4) Uani 1 1 d . . . . .
H21 H 0.6080 0.7817 0.2441 0.044 Uiso 1 1 calc R . . . .
C22 C 0.4139(8) 0.6010(8) 0.7260(10) 0.038(4) Uani 1 1 d . . . . .
H22 H 0.3748 0.5873 0.7395 0.046 Uiso 1 1 calc R . . . .
C23 C 0.4412(8) 0.8630(7) 0.6595(9) 0.034(4) Uani 1 1 d . . . . .
C24 C 0.4215(8) 0.6440(8) 0.6703(9) 0.034(4) Uani 1 1 d . . . . .
H24 H 0.3863 0.6606 0.6481 0.041 Uiso 1 1 calc R . . . .
C25 C 0.5152(8) 0.6641(8) 1.0499(9) 0.037(4) Uani 1 1 d . . . . .
H25 H 0.4735 0.6551 1.0432 0.044 Uiso 1 1 calc R . . . .
C26 C 0.5295(8) 0.6656(8) 0.9108(8) 0.033(4) Uani 1 1 d . . . . .
H26A H 0.4873 0.6505 0.9126 0.040 Uiso 1 1 calc R . . . .
H26B H 0.5545 0.6344 0.8862 0.040 Uiso 1 1 calc R . . . .
C27 C 0.5381(9) 0.6674(8) 1.1220(9) 0.040(4) Uani 1 1 d . . . . .
H27 H 0.5115 0.6612 1.1622 0.049 Uiso 1 1 calc R . . . .
C28 C 0.4097(8) 0.7888(9) 0.7474(11) 0.045(5) Uani 1 1 d . . . . .
H28 H 0.3786 0.7648 0.7684 0.054 Uiso 1 1 calc R . . . .
C29 C 0.3948(8) 0.8286(9) 0.6902(11) 0.044(5) Uani 1 1 d . . . . .
H29 H 0.3544 0.8319 0.6729 0.053 Uiso 1 1 calc R . . . .
C30 C 0.5081(9) 0.5071(8) 0.8520(10) 0.045(5) Uani 1 1 d . . . . .
H30A H 0.5329 0.4885 0.8136 0.067 Uiso 1 1 calc GR . . . .
H30B H 0.4938 0.4757 0.8857 0.067 Uiso 1 1 calc GR . . . .
H30C H 0.5325 0.5368 0.8790 0.067 Uiso 1 1 calc GR . . . .
C31 C 0.5283(10) 0.7819(9) 0.3019(10) 0.052(5) Uani 1 1 d . . . . .
H31 H 0.5023 0.7807 0.2605 0.062 Uiso 1 1 calc R . . . .
C32 C 0.3724(9) 0.9072(9) 0.5654(11) 0.052(5) Uani 1 1 d . . . . .
H32A H 0.3764 0.9212 0.5148 0.078 Uiso 1 1 calc GR . . . .
H32B H 0.3475 0.9359 0.5931 0.078 Uiso 1 1 calc GR . . . .
H32C H 0.3531 0.8672 0.5660 0.078 Uiso 1 1 calc GR . . . .
N4 N 0.4886(8) 0.8465(9) 1.0209(10) 0.061(5) Uani 1 1 d D . . . .
C33 C 0.5400(10) 0.5790(10) 0.3053(10) 0.053(5) Uani 1 1 d . . . . .
H33A H 0.4960 0.5787 0.2984 0.079 Uiso 1 1 calc GR . . . .
H33B H 0.5580 0.5445 0.2796 0.079 Uiso 1 1 calc GR . . . .
H33C H 0.5568 0.6168 0.2856 0.079 Uiso 1 1 calc GR . . . .
C34 C 0.5102(10) 0.8479(9) 0.9537(13) 0.055(5) Uani 1 1 d . U . . .
H34 H 0.4832 0.8542 0.9140 0.066 Uiso 1 1 calc R . . . .
C35 C 0.5219(14) 0.8329(14) 1.0896(14) 0.100(10) Uani 1 1 d D . . . .
H35A H 0.5553 0.8049 1.0790 0.150 Uiso 1 1 calc GR . . . .
H35B H 0.4943 0.8142 1.1249 0.150 Uiso 1 1 calc GR . . . .
H35C H 0.5382 0.8705 1.1101 0.150 Uiso 1 1 calc GR . . . .
C36 C 0.4203(15) 0.8478(17) 1.030(2) 0.124(12) Uani 1 1 d . U . . .
H36A H 0.4023 0.8716 0.9901 0.185 Uiso 1 1 calc GR . . . .
H36B H 0.4100 0.8663 1.0770 0.185 Uiso 1 1 calc GR . . . .
H36C H 0.4044 0.8064 1.0282 0.185 Uiso 1 1 calc GR . . . .
H2 H 0.638(6) 0.809(7) 0.664(8) 0.01(4) Uiso 1 1 d . . . . .
H3 H 0.641(7) 0.713(9) 0.749(7) 0.05(6) Uiso 1 1 d D . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Gd1 Gd1 0.000(3) 4_565 ?
Gd1 Gd1 0.000(3) 3_655 ?
Gd1 Gd1 0.000(3) 2_665 ?
Gd1 O1 2.800(16) . ?
Gd1 O2 2.442(9) 2_665 ?
Gd1 O2 2.442(9) . ?
Gd1 O2 2.442(9) 3_655 ?
Gd1 O2 2.442(9) 4_565 ?
Gd1 O3 2.446(9) 3_655 ?
Gd1 O3 2.446(9) 2_665 ?
Gd1 O3 2.446(9) . ?
Gd1 O3 2.446(9) 4_565 ?
Gd2 Gd1 3.7097(11) 4_565 ?
Gd2 Gd1 3.7097(11) 3_655 ?
Gd2 Gd1 3.7097(11) 2_665 ?
Gd2 O1 2.5881(12) . ?
Gd2 O3 2.349(9) 4_565 ?
Gd2 O3 2.319(9) . ?
Gd2 O6 2.428(9) 4_565 ?
Gd2 O6 2.368(9) . ?
Gd2 O8 2.262(10) . ?
Gd2 O9 2.413(11) . ?
Gd2 N3 2.606(12) . ?
Gd3 Gd1 3.7096(11) 3_655 ?
Gd3 Gd1 3.7096(11) 4_565 ?
Gd3 Gd1 3.7096(11) 2_665 ?
Gd3 O2 2.359(9) 3_655 ?
Gd3 O2 2.330(10) . ?
Gd3 O4 2.5986(16) . ?
Gd3 O5 2.369(10) . ?
Gd3 O5 2.428(9) 3_655 ?
Gd3 O7 2.257(10) . ?
Gd3 O10 2.396(11) . ?
Gd3 N1 2.584(11) . ?
O1 Gd1 2.800(16) 2_665 ?
O1 Gd1 2.800(16) 3_655 ?
O1 Gd1 2.800(16) 4_565 ?
O1 Gd2 2.5881(11) 3_655 ?
O1 Gd2 2.5881(11) 2_665 ?
O1 Gd2 2.5881(11) 4_565 ?
O2 Gd1 2.442(9) 3_655 ?
O2 Gd1 2.442(9) 2_665 ?
O2 Gd1 2.442(9) 4_565 ?
O2 Gd3 2.359(9) 4_565 ?
O3 Gd1 2.446(9) 4_565 ?
O3 Gd1 2.446(9) 2_665 ?
O3 Gd1 2.446(9) 3_655 ?
O3 Gd2 2.349(9) 3_655 ?
O4 Gd1 2.83(2) 3_655 ?
O4 Gd1 2.83(2) 2_665 ?
O4 Gd1 2.83(2) 4_565 ?
O4 Gd3 2.5986(15) 2_665 ?
O4 Gd3 2.5986(15) 3_655 ?
O4 Gd3 2.5986(15) 4_565 ?
O5 Gd3 2.428(9) 4_565 ?
O5 C3 1.355(17) . ?
O6 Gd2 2.428(9) 3_655 ?
O6 C9 1.349(16) . ?
O7 C4 1.324(17) . ?
O8 C8 1.283(17) . ?
O9 C34 1.23(2) . ?
O10 C14 1.235(19) . ?
N1 C5 1.313(18) . ?
N1 C10 1.471(18) . ?
C1 C3 1.38(2) . ?
C1 C10 1.54(2) . ?
C1 C17 1.37(2) . ?
O11 C23 1.387(19) . ?
O11 C32 1.463(19) . ?
C2 C8 1.41(2) . ?
C2 C23 1.36(2) . ?
C3 C6 1.41(2) . ?
C4 C7 1.44(2) . ?
C4 C16 1.39(2) . ?
N2 C14 1.30(2) . ?
N2 C19 1.45(2) . ?
N2 C33 1.46(2) . ?
C5 C16 1.38(2) . ?
C6 C21 1.36(2) . ?
N3 C12 1.309(19) . ?
N3 C26 1.479(19) . ?
C7 C18 1.38(2) . ?
O12 C18 1.371(19) . ?
O12 C30 1.42(2) . ?
C8 C20 1.42(2) . ?
C9 C11 1.38(2) . ?
C9 C15 1.42(2) . ?
C11 C13 1.41(2) . ?
C12 C20 1.42(2) . ?
C13 C27 1.37(2) . ?
C15 C25 1.40(2) . ?
C15 C26 1.45(2) . ?
C16 C24 1.40(2) . ?
C17 C31 1.36(3) . ?
C18 C22 1.41(2) . ?
C20 C28 1.40(2) . ?
C21 C31 1.38(3) . ?
C22 C24 1.37(2) . ?
C23 C29 1.36(2) . ?
C25 C27 1.38(2) . ?
C28 C29 1.38(3) . ?
N4 C34 1.29(3) . ?
N4 C35 1.454(17) . ?
N4 C36 1.49(3) . ?

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
Gd1 Gd1 Gd1 0(10) 4_565 3_655 ?
Gd1 Gd1 Gd1 0(10) 4_565 2_665 ?
Gd1 Gd1 Gd1 0(10) 3_655 2_665 ?
Gd1 Gd1 O1 0(10) 4_565 . ?
Gd1 Gd1 O1 0(10) 3_655 . ?
Gd1 Gd1 O1 0(10) 2_665 . ?
Gd1 Gd1 O2 0(10) 4_565 2_665 ?
Gd1 Gd1 O2 0(10) 4_565 4_565 ?
Gd1 Gd1 O2 0(10) 3_655 4_565 ?
Gd1 Gd1 O2 0(10) 4_565 3_655 ?
Gd1 Gd1 O2 0(10) 2_665 4_565 ?
Gd1 Gd1 O2 0(10) 2_665 3_655 ?
Gd1 Gd1 O2 0(10) 3_655 2_665 ?
Gd1 Gd1 O2 0(10) 4_565 . ?
Gd1 Gd1 O2 0(10) 3_655 3_655 ?
Gd1 Gd1 O2 0(10) 3_655 . ?
Gd1 Gd1 O2 0(10) 2_665 . ?
Gd1 Gd1 O2 0(10) 2_665 2_665 ?
Gd1 Gd1 O3 0(10) 4_565 4_565 ?
Gd1 Gd1 O3 0(10) 4_565 2_665 ?
Gd1 Gd1 O3 0(10) 3_655 . ?
Gd1 Gd1 O3 0(10) 2_665 4_565 ?
Gd1 Gd1 O3 0(10) 2_665 2_665 ?
Gd1 Gd1 O3 0(10) 4_565 3_655 ?
Gd1 Gd1 O3 0(10) 2_665 . ?
Gd1 Gd1 O3 0(10) 3_655 3_655 ?
Gd1 Gd1 O3 0(10) 3_655 2_665 ?
Gd1 Gd1 O3 0(10) 2_665 3_655 ?
Gd1 Gd1 O3 0(10) 4_565 . ?
Gd1 Gd1 O3 0(10) 3_655 4_565 ?
O2 Gd1 O1 119.9(2) 4_565 . ?
O2 Gd1 O1 119.9(2) . . ?
O2 Gd1 O1 119.9(2) 3_655 . ?
O2 Gd1 O1 119.9(2) 2_665 . ?
O2 Gd1 O2 120.1(5) . 2_665 ?
O2 Gd1 O2 120.1(5) 3_655 4_565 ?
O2 Gd1 O2 75.6(2) 3_655 . ?
O2 Gd1 O2 75.6(2) 3_655 2_665 ?
O2 Gd1 O2 75.6(2) 4_565 2_665 ?
O2 Gd1 O2 75.6(2) . 4_565 ?
O2 Gd1 O3 140.1(3) 4_565 3_655 ?
O2 Gd1 O3 73.2(3) 4_565 2_665 ?
O2 Gd1 O3 74.8(3) 4_565 4_565 ?
O2 Gd1 O3 73.2(3) 2_665 3_655 ?
O2 Gd1 O3 140.1(3) 3_655 4_565 ?
O2 Gd1 O3 142.6(3) 2_665 4_565 ?
O2 Gd1 O3 142.6(3) . 3_655 ?
O2 Gd1 O3 142.6(3) 3_655 2_665 ?
O2 Gd1 O3 74.8(3) 2_665 2_665 ?
O2 Gd1 O3 73.2(3) 3_655 . ?
O2 Gd1 O3 73.2(3) . 4_565 ?
O2 Gd1 O3 74.8(3) . . ?
O2 Gd1 O3 74.8(3) 3_655 3_655 ?
O2 Gd1 O3 142.6(3) 4_565 . ?
O2 Gd1 O3 140.1(3) 2_665 . ?
O2 Gd1 O3 140.1(3) . 2_665 ?
O3 Gd1 O1 59.6(2) 2_665 . ?
O3 Gd1 O1 59.6(2) . . ?
O3 Gd1 O1 59.6(2) 4_565 . ?
O3 Gd1 O1 59.6(2) 3_655 . ?
O3 Gd1 O3 75.18(19) 3_655 . ?
O3 Gd1 O3 75.18(19) 4_565 . ?
O3 Gd1 O3 119.2(4) 2_665 . ?
O3 Gd1 O3 75.18(19) 2_665 3_655 ?
O3 Gd1 O3 119.2(4) 4_565 3_655 ?
O3 Gd1 O3 75.18(19) 2_665 4_565 ?
Gd1 Gd2 Gd1 0.00(3) 3_655 4_565 ?
Gd1 Gd2 Gd1 0.00(3) 2_665 3_655 ?
Gd1 Gd2 Gd1 0.00(3) 2_665 4_565 ?
O1 Gd2 Gd1 48.9(4) . 2_665 ?
O1 Gd2 Gd1 48.9(4) . 4_565 ?
O1 Gd2 Gd1 48.9(4) . 3_655 ?
O1 Gd2 N3 133.3(3) . . ?
O3 Gd2 Gd1 40.1(2) . 3_655 ?
O3 Gd2 Gd1 40.3(2) 4_565 4_565 ?
O3 Gd2 Gd1 40.1(2) . 2_665 ?
O3 Gd2 Gd1 40.1(2) . 4_565 ?
O3 Gd2 Gd1 40.3(2) 4_565 2_665 ?
O3 Gd2 Gd1 40.3(2) 4_565 3_655 ?
O3 Gd2 O1 64.1(3) 4_565 . ?
O3 Gd2 O1 64.4(3) . . ?
O3 Gd2 O3 79.5(4) . 4_565 ?
O3 Gd2 O6 74.3(3) 4_565 4_565 ?
O3 Gd2 O6 76.0(3) . . ?
O3 Gd2 O6 130.3(3) 4_565 . ?
O3 Gd2 O6 129.7(3) . 4_565 ?
O3 Gd2 O9 120.0(4) 4_565 . ?
O3 Gd2 O9 155.6(4) . . ?
O3 Gd2 N3 82.9(4) . . ?
O3 Gd2 N3 143.7(3) 4_565 . ?
O6 Gd2 Gd1 99.3(2) 4_565 2_665 ?
O6 Gd2 Gd1 99.3(2) 4_565 4_565 ?
O6 Gd2 Gd1 100.5(2) . 2_665 ?
O6 Gd2 Gd1 100.5(2) . 3_655 ?
O6 Gd2 Gd1 99.3(2) 4_565 3_655 ?
O6 Gd2 Gd1 100.5(2) . 4_565 ?
O6 Gd2 O1 66.4(3) . . ?
O6 Gd2 O1 65.6(3) 4_565 . ?
O6 Gd2 O6 89.3(4) . 4_565 ?
O6 Gd2 O9 98.0(4) . . ?
O6 Gd2 N3 74.2(4) . . ?
O6 Gd2 N3 139.2(3) 4_565 . ?
O8 Gd2 Gd1 86.0(3) . 3_655 ?
O8 Gd2 Gd1 86.0(3) . 4_565 ?
O8 Gd2 Gd1 86.0(3) . 2_665 ?
O8 Gd2 O1 134.2(4) . . ?
O8 Gd2 O3 76.4(3) . 4_565 ?
O8 Gd2 O3 87.3(4) . . ?
O8 Gd2 O6 125.6(4) . 4_565 ?
O8 Gd2 O6 143.3(4) . . ?
O8 Gd2 O9 83.9(4) . . ?
O8 Gd2 N3 71.3(4) . . ?
O9 Gd2 Gd1 159.9(3) . 2_665 ?
O9 Gd2 Gd1 159.9(3) . 3_655 ?
O9 Gd2 Gd1 159.9(3) . 4_565 ?
O9 Gd2 O1 135.3(4) . . ?
O9 Gd2 O6 72.9(4) . 4_565 ?
O9 Gd2 N3 72.8(4) . . ?
N3 Gd2 Gd1 120.1(3) . 4_565 ?
N3 Gd2 Gd1 120.1(3) . 2_665 ?
N3 Gd2 Gd1 120.1(3) . 3_655 ?
Gd1 Gd3 Gd1 0.00(3) 2_665 3_655 ?
Gd1 Gd3 Gd1 0.00(3) 2_665 4_565 ?
Gd1 Gd3 Gd1 0.00(3) 3_655 4_565 ?
O2 Gd3 Gd1 40.2(2) 3_655 3_655 ?
O2 Gd3 Gd1 40.1(2) . 3_655 ?
O2 Gd3 Gd1 40.2(2) 3_655 2_665 ?
O2 Gd3 Gd1 40.1(2) . 2_665 ?
O2 Gd3 Gd1 40.2(2) 3_655 4_565 ?
O2 Gd3 Gd1 40.1(2) . 4_565 ?
O2 Gd3 O2 79.3(4) . 3_655 ?
O2 Gd3 O4 65.0(4) . . ?
O2 Gd3 O4 64.7(4) 3_655 . ?
O2 Gd3 O5 74.1(3) 3_655 3_655 ?
O2 Gd3 O5 130.4(3) 3_655 . ?
O2 Gd3 O5 129.8(3) . 3_655 ?
O2 Gd3 O5 75.8(3) . . ?
O2 Gd3 O10 156.5(4) . . ?
O2 Gd3 O10 118.2(4) 3_655 . ?
O2 Gd3 N1 144.2(3) 3_655 . ?
O2 Gd3 N1 84.4(4) . . ?
O4 Gd3 Gd1 49.5(4) . 4_565 ?
O4 Gd3 Gd1 49.5(4) . 3_655 ?
O4 Gd3 Gd1 49.5(4) . 2_665 ?
O5 Gd3 Gd1 100.3(2) . 2_665 ?
O5 Gd3 Gd1 100.3(2) . 4_565 ?
O5 Gd3 Gd1 99.1(2) 3_655 3_655 ?
O5 Gd3 Gd1 99.1(2) 3_655 4_565 ?
O5 Gd3 Gd1 100.3(2) . 3_655 ?
O5 Gd3 Gd1 99.1(2) 3_655 2_665 ?
O5 Gd3 O4 66.0(4) . . ?
O5 Gd3 O4 65.3(4) 3_655 . ?
O5 Gd3 O5 90.2(5) . 3_655 ?
O5 Gd3 O10 100.2(4) . . ?
O5 Gd3 N1 74.4(3) . . ?
O5 Gd3 N1 138.2(3) 3_655 . ?
O7 Gd3 Gd1 84.7(2) . 2_665 ?
O7 Gd3 Gd1 84.7(2) . 4_565 ?
O7 Gd3 Gd1 84.7(2) . 3_655 ?
O7 Gd3 O2 75.6(3) . 3_655 ?
O7 Gd3 O2 85.6(4) . . ?
O7 Gd3 O4 133.6(5) . . ?
O7 Gd3 O5 126.1(4) . 3_655 ?
O7 Gd3 O5 142.5(4) . . ?
O7 Gd3 O10 84.1(4) . . ?
O7 Gd3 N1 71.5(4) . . ?
O10 Gd3 Gd1 157.9(3) . 2_665 ?
O10 Gd3 Gd1 157.9(3) . 3_655 ?
O10 Gd3 Gd1 157.9(3) . 4_565 ?
O10 Gd3 O4 135.1(5) . . ?
O10 Gd3 O5 72.7(4) . 3_655 ?
O10 Gd3 N1 72.3(4) . . ?
N1 Gd3 Gd1 121.6(3) . 3_655 ?
N1 Gd3 Gd1 121.6(3) . 2_665 ?
N1 Gd3 Gd1 121.6(3) . 4_565 ?
N1 Gd3 O4 134.4(3) . . ?
Gd1 O1 Gd1 0.0 4_565 2_665 ?
Gd1 O1 Gd1 0.0 4_565 . ?
Gd1 O1 Gd1 0.0 3_655 . ?
Gd1 O1 Gd1 0.0 3_655 4_565 ?
Gd1 O1 Gd1 0.0 3_655 2_665 ?
Gd1 O1 Gd1 0.0 . 2_665 ?
Gd2 O1 Gd1 86.9(4) 2_665 4_565 ?
Gd2 O1 Gd1 86.9(4) 3_655 2_665 ?
Gd2 O1 Gd1 86.9(4) 2_665 2_665 ?
Gd2 O1 Gd1 86.9(4) . 3_655 ?
Gd2 O1 Gd1 86.9(4) . 2_665 ?
Gd2 O1 Gd1 86.9(4) 3_655 . ?
Gd2 O1 Gd1 86.9(4) 3_655 3_655 ?
Gd2 O1 Gd1 86.9(4) 4_565 . ?
Gd2 O1 Gd1 86.9(4) 4_565 2_665 ?
Gd2 O1 Gd1 86.9(4) . . ?
Gd2 O1 Gd1 86.9(4) 4_565 3_655 ?
Gd2 O1 Gd1 86.9(4) 2_665 3_655 ?
Gd2 O1 Gd1 86.9(4) 2_665 . ?
Gd2 O1 Gd1 86.9(4) 4_565 4_565 ?
Gd2 O1 Gd1 86.9(4) . 4_565 ?
Gd2 O1 Gd1 86.9(4) 3_655 4_565 ?
Gd2 O1 Gd2 89.83(4) 4_565 2_665 ?
Gd2 O1 Gd2 89.83(4) 3_655 2_665 ?
Gd2 O1 Gd2 89.83(4) 4_565 . ?
Gd2 O1 Gd2 173.8(7) . 2_665 ?
Gd2 O1 Gd2 173.8(7) 3_655 4_565 ?
Gd2 O1 Gd2 89.83(4) 3_655 . ?
Gd1 O2 Gd1 0.00(5) . 2_665 ?
Gd1 O2 Gd1 0.00(5) 2_665 3_655 ?
Gd1 O2 Gd1 0.00(5) . 3_655 ?
Gd1 O2 Gd1 0.00(5) . 4_565 ?
Gd1 O2 Gd1 0.00(5) 3_655 4_565 ?
Gd1 O2 Gd1 0.00(5) 2_665 4_565 ?
Gd3 O2 Gd1 102.0(4) . 2_665 ?
Gd3 O2 Gd1 101.2(3) 4_565 . ?
Gd3 O2 Gd1 101.2(3) 4_565 4_565 ?
Gd3 O2 Gd1 101.2(3) 4_565 2_665 ?
Gd3 O2 Gd1 102.0(4) . . ?
Gd3 O2 Gd1 102.0(4) . 3_655 ?
Gd3 O2 Gd1 101.2(3) 4_565 3_655 ?
Gd3 O2 Gd1 102.0(4) . 4_565 ?
Gd3 O2 Gd3 102.9(4) . 4_565 ?
Gd1 O3 Gd1 0.00(5) . 2_665 ?
Gd1 O3 Gd1 0.00(5) . 4_565 ?
Gd1 O3 Gd1 0.00(5) 3_655 4_565 ?
Gd1 O3 Gd1 0.00(5) . 3_655 ?
Gd1 O3 Gd1 0.00(5) 2_665 3_655 ?
Gd1 O3 Gd1 0.00(5) 2_665 4_565 ?
Gd2 O3 Gd1 102.2(4) . 3_655 ?
Gd2 O3 Gd1 101.3(3) 3_655 4_565 ?
Gd2 O3 Gd1 101.3(3) 3_655 2_665 ?
Gd2 O3 Gd1 101.3(3) 3_655 3_655 ?
Gd2 O3 Gd1 102.2(4) . 2_665 ?
Gd2 O3 Gd1 102.2(4) . . ?
Gd2 O3 Gd1 102.2(4) . 4_565 ?
Gd2 O3 Gd1 101.3(3) 3_655 . ?
Gd2 O3 Gd2 103.1(3) . 3_655 ?
Gd1 O4 Gd1 0.0 . 3_655 ?
Gd1 O4 Gd1 0.0 . 2_665 ?
Gd1 O4 Gd1 0.0 4_565 2_665 ?
Gd1 O4 Gd1 0.0 4_565 3_655 ?
Gd1 O4 Gd1 0.0 . 4_565 ?
Gd1 O4 Gd1 0.0 2_665 3_655 ?
Gd3 O4 Gd1 86.1(4) 4_565 4_565 ?
Gd3 O4 Gd1 86.1(4) 2_665 3_655 ?
Gd3 O4 Gd1 86.1(4) 2_665 4_565 ?
Gd3 O4 Gd1 86.1(4) 3_655 4_565 ?
Gd3 O4 Gd1 86.1(4) 4_565 3_655 ?
Gd3 O4 Gd1 86.1(4) . . ?
Gd3 O4 Gd1 86.1(4) 3_655 . ?
Gd3 O4 Gd1 86.1(4) 2_665 2_665 ?
Gd3 O4 Gd1 86.1(4) . 3_655 ?
Gd3 O4 Gd1 86.1(4) . 2_665 ?
Gd3 O4 Gd1 86.1(4) 3_655 3_655 ?
Gd3 O4 Gd1 86.1(4) 4_565 2_665 ?
Gd3 O4 Gd1 86.1(4) 2_665 . ?
Gd3 O4 Gd1 86.1(4) 4_565 . ?
Gd3 O4 Gd1 86.1(4) . 4_565 ?
Gd3 O4 Gd1 86.1(4) 3_655 2_665 ?
Gd3 O4 Gd3 89.74(6) 2_665 3_655 ?
Gd3 O4 Gd3 89.74(6) . 4_565 ?
Gd3 O4 Gd3 172.2(9) 2_665 . ?
Gd3 O4 Gd3 89.74(6) . 3_655 ?
Gd3 O4 Gd3 172.2(9) 4_565 3_655 ?
Gd3 O4 Gd3 89.74(6) 2_665 4_565 ?
Gd3 O5 Gd3 99.7(3) . 4_565 ?
C3 O5 Gd3 118.2(8) . . ?
C3 O5 Gd3 138.8(9) . 4_565 ?
Gd2 O6 Gd2 99.3(3) . 3_655 ?
C9 O6 Gd2 136.1(8) . 3_655 ?
C9 O6 Gd2 120.4(8) . . ?
C4 O7 Gd3 140.6(9) . . ?
C8 O8 Gd2 144.0(10) . . ?
C34 O9 Gd2 141.1(13) . . ?
C14 O10 Gd3 134.3(12) . . ?
C5 N1 Gd3 126.2(9) . . ?
C5 N1 C10 115.9(12) . . ?
C10 N1 Gd3 117.9(9) . . ?
C3 C1 C10 117.4(13) . . ?
C17 C1 C3 121.6(15) . . ?
C17 C1 C10 120.8(14) . . ?
C23 O11 C32 117.9(14) . . ?
C23 C2 C8 122.8(15) . . ?
O5 C3 C1 122.0(13) . . ?
O5 C3 C6 119.6(13) . . ?
C1 C3 C6 118.4(14) . . ?
O7 C4 C7 116.2(14) . . ?
O7 C4 C16 123.6(14) . . ?
C16 C4 C7 120.2(14) . . ?
C14 N2 C19 121.4(14) . . ?
C14 N2 C33 121.0(15) . . ?
C19 N2 C33 117.4(14) . . ?
N1 C5 C16 130.1(14) . . ?
C21 C6 C3 119.1(15) . . ?
C12 N3 Gd2 126.6(10) . . ?
C12 N3 C26 116.1(13) . . ?
C26 N3 Gd2 117.3(10) . . ?
C18 C7 C4 119.1(14) . . ?
C18 O12 C30 118.5(14) . . ?
O8 C8 C2 121.8(14) . . ?
O8 C8 C20 122.6(13) . . ?
C2 C8 C20 115.5(13) . . ?
O6 C9 C11 120.0(13) . . ?
O6 C9 C15 118.2(12) . . ?
C11 C9 C15 121.7(13) . . ?
N1 C10 C1 112.4(12) . . ?
C9 C11 C13 120.9(15) . . ?
N3 C12 C20 129.4(14) . . ?
C27 C13 C11 117.9(16) . . ?
O10 C14 N2 127.6(16) . . ?
C9 C15 C26 121.4(14) . . ?
C25 C15 C9 115.4(14) . . ?
C25 C15 C26 123.2(15) . . ?
C4 C16 C24 117.8(15) . . ?
C5 C16 C4 123.2(15) . . ?
C5 C16 C24 118.8(14) . . ?
C31 C17 C1 119.6(16) . . ?
C7 C18 C22 121.3(14) . . ?
O12 C18 C7 123.3(15) . . ?
O12 C18 C22 115.4(14) . . ?
C12 C20 C8 123.4(13) . . ?
C28 C20 C8 119.6(15) . . ?
C28 C20 C12 117.0(15) . . ?
C6 C21 C31 121.2(15) . . ?
C24 C22 C18 118.1(15) . . ?
C2 C23 O11 113.9(15) . . ?
C2 C23 C29 121.7(15) . . ?
C29 C23 O11 124.4(15) . . ?
C22 C24 C16 123.4(16) . . ?
C27 C25 C15 122.8(16) . . ?
C15 C26 N3 113.3(13) . . ?
C13 C27 C25 121.2(16) . . ?
C29 C28 C20 122.5(18) . . ?
C23 C29 C28 117.8(16) . . ?
C17 C31 C21 120.0(16) . . ?
C34 N4 C35 128(2) . . ?
C34 N4 C36 117(2) . . ?
C35 N4 C36 114(2) . . ?
O9 C34 N4 121(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_t_sq_s
_database_code_depnum_ccdc_archive 'CCDC 1922681'
loop_
_audit_author_name
_audit_author_address
'Yuan Huang'
;Soochow university
China
;
_audit_update_record             
;
2019-11-06 deposited with the CCDC.	2019-11-13 downloaded from the CCDC.
;
_audit_creation_date             2019-11-06
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2014/7
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C144 H168 Eu9 N16 O42, H3 O, H2O'
_chemical_formula_sum            'C144 H173 Eu9 N16 O44'
_chemical_formula_weight         4206.47
_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'
Eu Eu -0.1578 3.6682 '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'

_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           85
_space_group_name_H-M_alt        'P 4/n'
_space_group_name_Hall           '-P 4a'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y+1/2, z'
'-y+1/2, x, z'
'y, -x+1/2, z'
'-x, -y, -z'
'x-1/2, y-1/2, -z'
'y-1/2, -x, -z'
'-y, x-1/2, -z'

_cell_length_a                   21.6995(3)
_cell_length_b                   21.6995(3)
_cell_length_c                   17.9503(7)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     8452.2(4)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    9833
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      27.47
_cell_measurement_theta_min      2.46
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    3.361
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.2669
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.2085 before and 0.0688 after correction.
The Ratio of minimum to maximum transmission is 0.3580.
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    1.636
_exptl_crystal_density_meas      .
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             4094
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0740
_diffrn_reflns_av_unetI/netI     0.0699
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            24961
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.679
_diffrn_reflns_theta_min         2.629
_diffrn_ambient_temperature      296.15
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                5844
_reflns_number_total             8031
_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 v8.37A (Bruker, 2015)'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_refine_diff_density_max         2.189
_refine_diff_density_min         -1.776
_refine_diff_density_rms         0.233
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.085
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     484
_refine_ls_number_reflns         8031
_refine_ls_number_restraints     7
_refine_ls_R_factor_all          0.1087
_refine_ls_R_factor_gt           0.0758
_refine_ls_restrained_S_all      1.085
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+308.0675P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1560
_refine_ls_wR_factor_ref         0.1755
_refine_special_details          
;
The SQUEEZE routine of PLATON was used in the treatment of the crystallographic data. The identities and numbers of the lattice solvents were determined by the TGA and elemental analysis. The calculated mass loss corresponding to the solvent guests from the crystals between 24 and 100?ãC was 0.87%. However, the experimental result 0.71% was nearly consistent with calculated result. This indicates that one mole of water molecule and one hydronium ion might be lost during the test process and elemental analysis results of C 41.18, H 4.15, N 5.34, which are consistent with the experimental data.
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All O(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Rigid bond restraints
 O3, C24
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C6) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
4.a Riding coordinates:
 O8(H8), O10(H10)
4.b Secondary CH2 refined with riding coordinates:
 C12(H12A,H12B), C32(H32A,H32B)
4.c Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C8(H8A), C10(H10A), C13(H13), C14(H14), C16(H16),
 C17(H17), C18(H18), C19(H19), C20(H20), C24(H24), C30(H30), C31(H31), C34(H34),
  C35(H35), C36(H36)
4.d Idealised Me refined as rotating group:
 C21(H21A,H21B,H21C), C22(H22A,H22B,H22C), C23(H23A,H23B,H23C), C25(H25A,H25B,
 H25C), C26(H26A,H26B,H26C), C33(H33A,H33B,H33C)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_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
Eu1 Eu 0.7500 0.7500 0.71259(7) 0.0242(3) Uani 1 4 d S T P . .
Eu2 Eu 0.63511(3) 0.71616(3) 0.86129(3) 0.02564(17) Uani 1 1 d . . . . .
Eu3 Eu 0.69681(3) 0.64224(3) 0.56415(3) 0.02603(17) Uani 1 1 d . . . . .
O1 O 0.6553(5) 0.5889(4) 0.6600(5) 0.035(2) Uani 1 1 d . . . . .
O2 O 0.5743(4) 0.6815(5) 0.7685(5) 0.036(2) Uani 1 1 d . . . . .
O3 O 0.5660(5) 0.6581(5) 0.9403(6) 0.051(3) Uani 1 1 d . U . . .
O4 O 0.6244(5) 0.5860(5) 0.4886(6) 0.046(3) Uani 1 1 d . . . . .
O5 O 0.4329(5) 0.5974(5) 0.6002(6) 0.047(3) Uani 1 1 d . . . . .
O6 O 0.5372(5) 0.4577(5) 0.8188(6) 0.053(3) Uani 1 1 d . . . . .
O7 O 0.7500 0.7500 0.8705(9) 0.024(4) Uani 1 4 d S T P . .
O8 O 0.6573(4) 0.7194(4) 0.6442(4) 0.0240(18) Uani 1 1 d . . . . .
H8 H 0.6448 0.6846 0.6596 0.029 Uiso 1 1 d R . . . .
O9 O 0.7500 0.7500 0.5541(9) 0.022(3) Uani 1 4 d S T P . .
O10 O 0.7041(4) 0.6638(4) 0.7813(4) 0.0280(19) Uani 1 1 d . . . . .
H10 H 0.6827 0.6380 0.7566 0.034 Uiso 1 1 d R . . . .
O11 O 0.6446(4) 0.7164(4) 0.4837(4) 0.031(2) Uani 1 1 d . . . . .
O12 O 0.6521(4) 0.8012(4) 0.9422(4) 0.031(2) Uani 1 1 d . . . . .
N1 N 0.7351(5) 0.5299(5) 0.5589(6) 0.030(2) Uani 1 1 d . . . . .
N2 N 0.5748(6) 0.5541(6) 0.3846(6) 0.041(3) Uani 1 1 d . . . . .
N3 N 0.5321(6) 0.7760(6) 0.8655(6) 0.038(3) Uani 1 1 d . . . . .
N4 N 0.4893(8) 0.6512(9) 1.0230(9) 0.079(5) Uani 1 1 d . . . . .
C1 C 0.4999(6) 0.6406(6) 0.6848(7) 0.029(3) Uani 1 1 d . . . . .
H1 H 0.5298 0.6166 0.6614 0.035 Uiso 1 1 calc R . . . .
C2 C 0.7102(6) 0.4820(6) 0.5912(7) 0.032(3) Uani 1 1 d . . . . .
H2 H 0.7258 0.4440 0.5762 0.038 Uiso 1 1 calc R . . . .
C3 C 0.5967(6) 0.5261(7) 0.7386(7) 0.035(3) Uani 1 1 d . . . . .
H3 H 0.5808 0.5610 0.7618 0.042 Uiso 1 1 calc R . . . .
C4 C 0.6143(6) 0.8116(6) 0.9998(6) 0.031(3) Uani 1 1 d . . . . .
C5 C 0.5426(6) 0.7156(6) 0.4336(7) 0.033(3) Uani 1 1 d . . . . .
C6 C 0.6054(6) 0.7152(6) 0.4238(8) 0.033(3) Uani 1 1 d . U . . .
C7 C 0.6395(6) 0.5319(6) 0.6794(8) 0.032(3) Uani 1 1 d . . . . .
C8 C 0.6313(7) 0.7150(6) 0.3519(7) 0.036(3) Uani 1 1 d . . . . .
H8A H 0.6737 0.7129 0.3449 0.043 Uiso 1 1 calc R . . . .
C9 C 0.6634(7) 0.4794(6) 0.6454(8) 0.035(3) Uani 1 1 d . . . . .
C10 C 0.6376(7) 0.8107(6) 1.0730(7) 0.036(3) Uani 1 1 d . . . . .
H10A H 0.6792 0.8031 1.0810 0.043 Uiso 1 1 calc R . . . .
C11 C 0.5788(6) 0.4677(7) 0.7613(8) 0.038(3) Uani 1 1 d . . . . .
C12 C 0.7897(7) 0.5170(7) 0.5115(7) 0.037(3) Uani 1 1 d . . . . .
H12A H 0.7955 0.4728 0.5085 0.045 Uiso 1 1 calc R . . . .
H12B H 0.8259 0.5344 0.5351 0.045 Uiso 1 1 calc R . . . .
C13 C 0.5987(7) 0.8213(7) 1.1339(7) 0.039(3) Uani 1 1 d . . . . .
H13 H 0.6139 0.8203 1.1823 0.047 Uiso 1 1 calc R . . . .
C14 C 0.4808(6) 0.7634(6) 0.8295(8) 0.034(3) Uani 1 1 d . . . . .
H14 H 0.4470 0.7881 0.8411 0.041 Uiso 1 1 calc R . . . .
C15 C 0.5176(6) 0.6786(6) 0.7447(7) 0.033(3) Uani 1 1 d . . . . .
C16 C 0.6231(7) 0.5711(6) 0.4222(8) 0.039(3) Uani 1 1 d . . . . .
H16 H 0.6603 0.5721 0.3966 0.047 Uiso 1 1 calc R . . . .
C17 C 0.5040(7) 0.7171(7) 0.3728(8) 0.042(4) Uani 1 1 d . . . . .
H17 H 0.4615 0.7176 0.3800 0.051 Uiso 1 1 calc R . . . .
C18 C 0.5380(8) 0.8331(7) 1.1206(8) 0.047(4) Uani 1 1 d . . . . .
H18 H 0.5115 0.8387 1.1607 0.056 Uiso 1 1 calc R . . . .
C19 C 0.4103(7) 0.7095(8) 0.7473(10) 0.052(4) Uani 1 1 d . . . . .
H19 H 0.3792 0.7324 0.7697 0.062 Uiso 1 1 calc R . . . .
C20 C 0.5277(9) 0.7180(8) 0.3004(9) 0.058(5) Uani 1 1 d . . . . .
H20 H 0.5016 0.7185 0.2593 0.070 Uiso 1 1 calc R . . . .
C21 C 0.5789(10) 0.5393(10) 0.3058(9) 0.071(6) Uani 1 1 d . . . . .
H21A H 0.6206 0.5448 0.2892 0.106 Uiso 1 1 calc GR . . . .
H21B H 0.5522 0.5661 0.2781 0.106 Uiso 1 1 calc GR . . . .
H21C H 0.5667 0.4973 0.2980 0.106 Uiso 1 1 calc GR . . . .
C22 C 0.5088(8) 0.5087(8) 0.8511(9) 0.056(5) Uani 1 1 d . . . . .
H22A H 0.4905 0.5337 0.8129 0.084 Uiso 1 1 calc GR . . . .
H22B H 0.5389 0.5325 0.8777 0.084 Uiso 1 1 calc GR . . . .
H22C H 0.4775 0.4950 0.8850 0.084 Uiso 1 1 calc GR . . . .
C23 C 0.3736(8) 0.5935(9) 0.5660(11) 0.064(5) Uani 1 1 d . . . . .
H23A H 0.3734 0.5605 0.5304 0.096 Uiso 1 1 calc GR . . . .
H23B H 0.3645 0.6317 0.5412 0.096 Uiso 1 1 calc GR . . . .
H23C H 0.3429 0.5858 0.6035 0.096 Uiso 1 1 calc GR . . . .
C24 C 0.5126(10) 0.6518(9) 0.9553(13) 0.076(6) Uani 1 1 d . U . . .
H24 H 0.4852 0.6470 0.9158 0.091 Uiso 1 1 calc R . . . .
C25 C 0.5218(11) 0.6640(12) 1.0858(15) 0.099(8) Uani 1 1 d . . . . .
H25A H 0.5615 0.6447 1.0830 0.149 Uiso 1 1 calc GR . . . .
H25B H 0.4999 0.6487 1.1284 0.149 Uiso 1 1 calc GR . . . .
H25C H 0.5270 0.7078 1.0903 0.149 Uiso 1 1 calc GR . . . .
C26 C 0.4210(13) 0.6484(14) 1.0276(18) 0.127(11) Uani 1 1 d . . . . .
H26A H 0.4045 0.6894 1.0296 0.190 Uiso 1 1 calc GR . . . .
H26B H 0.4091 0.6263 1.0717 0.190 Uiso 1 1 calc GR . . . .
H26C H 0.4051 0.6276 0.9845 0.190 Uiso 1 1 calc GR . . . .
C27 C 0.4403(7) 0.6374(7) 0.6596(8) 0.041(4) Uani 1 1 d . . . . .
C28 C 0.5519(6) 0.8265(7) 0.9882(7) 0.035(3) Uani 1 1 d . . . . .
C29 C 0.4703(6) 0.7166(7) 0.7748(8) 0.036(3) Uani 1 1 d . . . . .
C30 C 0.6025(7) 0.4147(7) 0.7264(8) 0.043(4) Uani 1 1 d . . . . .
H30 H 0.5902 0.3756 0.7417 0.052 Uiso 1 1 calc R . . . .
C31 C 0.5151(7) 0.8369(7) 1.0495(8) 0.039(3) Uani 1 1 d . . . . .
H31 H 0.4738 0.8468 1.0426 0.047 Uiso 1 1 calc R . . . .
C32 C 0.5279(7) 0.8333(6) 0.9098(7) 0.038(3) Uani 1 1 d . . . . .
H32A H 0.4852 0.8463 0.9118 0.046 Uiso 1 1 calc R . . . .
H32B H 0.5511 0.8654 0.8847 0.046 Uiso 1 1 calc R . . . .
C33 C 0.5130(7) 0.5529(8) 0.4183(9) 0.049(4) Uani 1 1 d . . . . .
H33A H 0.4977 0.5114 0.4188 0.073 Uiso 1 1 calc GR . . . .
H33B H 0.4856 0.5784 0.3897 0.073 Uiso 1 1 calc GR . . . .
H33C H 0.5152 0.5682 0.4684 0.073 Uiso 1 1 calc GR . . . .
C34 C 0.5907(8) 0.7180(7) 0.2916(8) 0.048(4) Uani 1 1 d . . . . .
H34 H 0.6069 0.7202 0.2437 0.058 Uiso 1 1 calc R . . . .
C35 C 0.3943(7) 0.6717(8) 0.6905(9) 0.050(4) Uani 1 1 d . . . . .
H35 H 0.3539 0.6693 0.6734 0.059 Uiso 1 1 calc R . . . .
C36 C 0.6432(8) 0.4215(7) 0.6706(9) 0.048(4) Uani 1 1 d . . . . .
H36 H 0.6588 0.3864 0.6477 0.057 Uiso 1 1 calc R . . . .


_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
Eu1 Eu2 3.7255(10) . ?
Eu1 Eu2 3.7255(10) 2_665 ?
Eu1 O7 2.834(16) . ?
Eu1 O8 2.448(8) 4_565 ?
Eu1 O8 2.448(8) 3_655 ?
Eu1 O8 2.448(8) 2_665 ?
Eu1 O8 2.448(8) . ?
Eu1 O9 2.844(17) . ?
Eu1 O10 2.452(8) 3_655 ?
Eu1 O10 2.452(8) 4_565 ?
Eu1 O10 2.452(8) 2_665 ?
Eu1 O10 2.452(8) . ?
Eu2 Eu2 3.6754(9) 4_565 ?
Eu2 Eu2 3.6755(9) 3_655 ?
Eu2 O2 2.255(9) . ?
Eu2 O3 2.418(10) . ?
Eu2 O7 2.6041(13) . ?
Eu2 O10 2.365(8) . ?
Eu2 O10 2.333(8) 4_565 ?
Eu2 O12 2.378(8) . ?
Eu2 O12 2.439(8) 3_655 ?
Eu2 N3 2.586(12) . ?
Eu3 Eu3 3.6879(9) 4_565 ?
Eu3 Eu3 3.6878(9) 3_655 ?
Eu3 O1 2.261(9) . ?
Eu3 O4 2.408(10) . ?
Eu3 O8 2.367(8) . ?
Eu3 O8 2.339(8) 3_655 ?
Eu3 O9 2.6139(14) . ?
Eu3 O11 2.374(9) 3_655 ?
Eu3 O11 2.440(8) . ?
Eu3 N1 2.576(11) . ?
Eu3 C6 3.261(14) 3_655 ?
O1 C7 1.330(16) . ?
O2 C15 1.302(15) . ?
O3 C24 1.20(2) . ?
O4 C16 1.236(17) . ?
O5 C23 1.430(17) . ?
O5 C27 1.385(17) . ?
O6 C11 1.387(17) . ?
O6 C22 1.39(2) . ?
O7 Eu2 2.6042(12) 2_665 ?
O7 Eu2 2.6042(12) 4_565 ?
O7 Eu2 2.6042(12) 3_655 ?
O8 Eu3 2.339(8) 4_565 ?
O9 Eu3 2.6139(13) 4_565 ?
O9 Eu3 2.6139(13) 2_665 ?
O9 Eu3 2.6139(13) 3_655 ?
O10 Eu2 2.333(8) 3_655 ?
O11 Eu3 2.374(8) 4_565 ?
O11 C6 1.372(15) . ?
O12 Eu2 2.439(8) 4_565 ?
O12 C4 1.338(15) . ?
N1 C2 1.307(17) . ?
N1 C12 1.487(17) . ?
N2 C16 1.300(19) . ?
N2 C21 1.453(19) . ?
N2 C33 1.472(19) . ?
N3 C14 1.316(18) . ?
N3 C32 1.478(17) . ?
N4 C24 1.32(2) . ?
N4 C25 1.36(3) . ?
N4 C26 1.49(3) . ?
C1 C15 1.410(17) . ?
C1 C27 1.372(19) . ?
C2 C9 1.408(19) . ?
C3 C7 1.417(19) . ?
C3 C11 1.39(2) . ?
C4 C10 1.408(18) . ?
C4 C28 1.409(19) . ?
C5 C6 1.375(19) . ?
C5 C12 1.508(18) 4_565 ?
C5 C17 1.377(18) . ?
C6 Eu3 3.261(14) 4_565 ?
C6 C8 1.407(19) . ?
C7 C9 1.393(19) . ?
C8 C34 1.40(2) . ?
C9 C36 1.40(2) . ?
C10 C13 1.399(19) . ?
C11 C30 1.41(2) . ?
C12 C5 1.508(18) 3_655 ?
C13 C18 1.36(2) . ?
C14 C29 1.431(19) . ?
C15 C29 1.424(19) . ?
C17 C20 1.40(2) . ?
C18 C31 1.37(2) . ?
C19 C29 1.40(2) . ?
C19 C35 1.35(2) . ?
C20 C34 1.38(2) . ?
C27 C35 1.36(2) . ?
C28 C31 1.379(19) . ?
C28 C32 1.508(19) . ?
C30 C36 1.34(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
Eu2 Eu1 Eu2 88.47(3) . 2_665 ?
O7 Eu1 Eu2 44.235(16) . . ?
O7 Eu1 Eu2 44.235(16) . 2_665 ?
O7 Eu1 O9 180.0 . . ?
O8 Eu1 Eu2 112.26(19) 4_565 2_665 ?
O8 Eu1 Eu2 164.28(19) 2_665 . ?
O8 Eu1 Eu2 164.28(18) . 2_665 ?
O8 Eu1 Eu2 75.90(18) 2_665 2_665 ?
O8 Eu1 Eu2 109.89(19) 4_565 . ?
O8 Eu1 Eu2 75.90(18) . . ?
O8 Eu1 Eu2 112.26(19) 3_655 . ?
O8 Eu1 Eu2 109.89(19) 3_655 2_665 ?
O8 Eu1 O7 120.11(18) . . ?
O8 Eu1 O7 120.11(18) 4_565 . ?
O8 Eu1 O7 120.11(18) 3_655 . ?
O8 Eu1 O7 120.11(18) 2_665 . ?
O8 Eu1 O8 75.42(16) 3_655 2_665 ?
O8 Eu1 O8 75.42(16) 2_665 4_565 ?
O8 Eu1 O8 75.42(16) . 3_655 ?
O8 Eu1 O8 75.42(16) . 4_565 ?
O8 Eu1 O8 119.8(4) 3_655 4_565 ?
O8 Eu1 O8 119.8(4) . 2_665 ?
O8 Eu1 O9 59.89(18) 3_655 . ?
O8 Eu1 O9 59.89(18) 4_565 . ?
O8 Eu1 O9 59.89(18) 2_665 . ?
O8 Eu1 O9 59.89(18) . . ?
O8 Eu1 O10 142.4(3) 4_565 3_655 ?
O8 Eu1 O10 140.3(3) . 3_655 ?
O8 Eu1 O10 142.4(3) 2_665 . ?
O8 Eu1 O10 74.7(3) 2_665 3_655 ?
O8 Eu1 O10 74.7(3) 3_655 . ?
O8 Eu1 O10 73.3(3) 2_665 2_665 ?
O8 Eu1 O10 140.3(3) 3_655 2_665 ?
O8 Eu1 O10 74.7(3) 4_565 2_665 ?
O8 Eu1 O10 73.3(3) 3_655 3_655 ?
O8 Eu1 O10 73.3(3) . . ?
O8 Eu1 O10 140.3(3) 4_565 . ?
O8 Eu1 O10 142.4(3) 3_655 4_565 ?
O8 Eu1 O10 142.4(3) . 2_665 ?
O8 Eu1 O10 140.3(3) 2_665 4_565 ?
O8 Eu1 O10 73.3(3) 4_565 4_565 ?
O8 Eu1 O10 74.7(3) . 4_565 ?
O9 Eu1 Eu2 135.765(16) . 2_665 ?
O9 Eu1 Eu2 135.765(16) . . ?
O10 Eu1 Eu2 94.02(19) 3_655 . ?
O10 Eu1 Eu2 38.5(2) 2_665 2_665 ?
O10 Eu1 Eu2 93.55(19) 2_665 . ?
O10 Eu1 Eu2 37.7(2) 4_565 . ?
O10 Eu1 Eu2 37.7(2) 3_655 2_665 ?
O10 Eu1 Eu2 38.5(2) . . ?
O10 Eu1 Eu2 93.55(19) . 2_665 ?
O10 Eu1 Eu2 94.02(19) 4_565 2_665 ?
O10 Eu1 O7 59.80(19) 3_655 . ?
O10 Eu1 O7 59.80(19) 2_665 . ?
O10 Eu1 O7 59.80(19) 4_565 . ?
O10 Eu1 O7 59.80(19) . . ?
O10 Eu1 O9 120.20(19) 2_665 . ?
O10 Eu1 O9 120.20(19) . . ?
O10 Eu1 O9 120.20(19) 4_565 . ?
O10 Eu1 O9 120.20(19) 3_655 . ?
O10 Eu1 O10 75.35(17) 2_665 3_655 ?
O10 Eu1 O10 119.6(4) . 2_665 ?
O10 Eu1 O10 119.6(4) 3_655 4_565 ?
O10 Eu1 O10 75.35(17) . 3_655 ?
O10 Eu1 O10 75.35(17) . 4_565 ?
O10 Eu1 O10 75.35(17) 2_665 4_565 ?
Eu2 Eu2 Eu1 60.444(9) 3_655 . ?
Eu2 Eu2 Eu1 60.445(9) 4_565 . ?
Eu2 Eu2 Eu2 90.001(1) 4_565 3_655 ?
O2 Eu2 Eu1 85.9(2) . . ?
O2 Eu2 Eu2 110.8(2) . 3_655 ?
O2 Eu2 Eu2 125.0(3) . 4_565 ?
O2 Eu2 O3 84.0(4) . . ?
O2 Eu2 O7 134.6(4) . . ?
O2 Eu2 O10 87.1(3) . 4_565 ?
O2 Eu2 O10 76.2(3) . . ?
O2 Eu2 O12 125.5(3) . 3_655 ?
O2 Eu2 O12 143.2(3) . . ?
O2 Eu2 N3 71.5(4) . . ?
O3 Eu2 Eu1 159.7(3) . . ?
O3 Eu2 Eu2 139.0(3) . 4_565 ?
O3 Eu2 Eu2 107.2(3) . 3_655 ?
O3 Eu2 O7 134.7(4) . . ?
O3 Eu2 O12 72.8(3) . 3_655 ?
O3 Eu2 N3 73.1(4) . . ?
O7 Eu2 Eu1 49.4(4) . . ?
O7 Eu2 Eu2 45.12(2) . 4_565 ?
O7 Eu2 Eu2 45.11(2) . 3_655 ?
O10 Eu2 Eu1 40.0(2) 4_565 . ?
O10 Eu2 Eu1 40.2(2) . . ?
O10 Eu2 Eu2 38.8(2) 4_565 4_565 ?
O10 Eu2 Eu2 96.8(2) . 4_565 ?
O10 Eu2 Eu2 96.9(2) 4_565 3_655 ?
O10 Eu2 Eu2 38.2(2) . 3_655 ?
O10 Eu2 O3 119.9(4) . . ?
O10 Eu2 O3 155.9(3) 4_565 . ?
O10 Eu2 O7 64.4(3) . . ?
O10 Eu2 O7 64.8(3) 4_565 . ?
O10 Eu2 O10 79.3(4) 4_565 . ?
O10 Eu2 O12 130.2(3) . . ?
O10 Eu2 O12 129.7(3) 4_565 3_655 ?
O10 Eu2 O12 74.3(3) . 3_655 ?
O10 Eu2 O12 76.0(3) 4_565 . ?
O10 Eu2 N3 143.7(3) . . ?
O10 Eu2 N3 82.9(3) 4_565 . ?
O12 Eu2 Eu1 100.4(2) . . ?
O12 Eu2 Eu1 99.2(2) 3_655 . ?
O12 Eu2 Eu2 103.3(2) 3_655 4_565 ?
O12 Eu2 Eu2 39.7(2) 3_655 3_655 ?
O12 Eu2 Eu2 40.9(2) . 4_565 ?
O12 Eu2 Eu2 103.6(2) . 3_655 ?
O12 Eu2 O3 98.2(4) . . ?
O12 Eu2 O7 66.0(3) . . ?
O12 Eu2 O7 65.2(3) 3_655 . ?
O12 Eu2 O12 89.5(4) . 3_655 ?
O12 Eu2 N3 74.1(3) . . ?
O12 Eu2 N3 139.3(3) 3_655 . ?
N3 Eu2 Eu1 120.0(3) . . ?
N3 Eu2 Eu2 88.4(3) . 4_565 ?
N3 Eu2 Eu2 177.7(3) . 3_655 ?
N3 Eu2 O7 133.2(3) . . ?
Eu3 Eu3 Eu1 60.357(9) 4_565 . ?
Eu3 Eu3 Eu1 60.358(9) 3_655 . ?
Eu3 Eu3 Eu3 90.0 3_655 4_565 ?
O1 Eu3 Eu1 84.3(2) . . ?
O1 Eu3 Eu3 110.9(2) . 4_565 ?
O1 Eu3 Eu3 122.8(2) . 3_655 ?
O1 Eu3 O4 84.7(3) . . ?
O1 Eu3 O8 75.9(3) . . ?
O1 Eu3 O8 85.1(3) . 3_655 ?
O1 Eu3 O9 133.3(4) . . ?
O1 Eu3 O11 142.2(3) . 3_655 ?
O1 Eu3 O11 127.0(3) . . ?
O1 Eu3 N1 70.9(3) . . ?
O1 Eu3 C6 134.1(3) . 3_655 ?
O4 Eu3 Eu1 157.3(3) . . ?
O4 Eu3 Eu3 141.3(3) . 3_655 ?
O4 Eu3 Eu3 105.7(3) . 4_565 ?
O4 Eu3 O9 134.7(4) . . ?
O4 Eu3 O11 72.4(3) . . ?
O4 Eu3 N1 73.1(3) . . ?
O4 Eu3 C6 79.8(4) . 3_655 ?
O8 Eu3 Eu1 40.06(19) . . ?
O8 Eu3 Eu1 39.9(2) 3_655 . ?
O8 Eu3 Eu3 96.6(2) . 3_655 ?
O8 Eu3 Eu3 38.68(19) 3_655 3_655 ?
O8 Eu3 Eu3 38.14(19) . 4_565 ?
O8 Eu3 Eu3 96.7(2) 3_655 4_565 ?
O8 Eu3 O4 117.6(3) . . ?
O8 Eu3 O4 157.5(3) 3_655 . ?
O8 Eu3 O8 79.0(4) 3_655 . ?
O8 Eu3 O9 64.8(3) 3_655 . ?
O8 Eu3 O9 64.4(3) . . ?
O8 Eu3 O11 129.9(3) . 3_655 ?
O8 Eu3 O11 75.7(3) 3_655 3_655 ?
O8 Eu3 O11 74.0(3) . . ?
O8 Eu3 O11 129.2(3) 3_655 . ?
O8 Eu3 N1 143.9(3) . . ?
O8 Eu3 N1 84.5(3) 3_655 . ?
O8 Eu3 C6 93.1(3) 3_655 3_655 ?
O8 Eu3 C6 148.7(3) . 3_655 ?
O9 Eu3 Eu1 49.6(4) . . ?
O9 Eu3 Eu3 45.14(3) . 3_655 ?
O9 Eu3 Eu3 45.13(3) . 4_565 ?
O9 Eu3 C6 84.7(4) . 3_655 ?
O11 Eu3 Eu1 98.8(2) . . ?
O11 Eu3 Eu1 100.1(2) 3_655 . ?
O11 Eu3 Eu3 39.34(19) . 4_565 ?
O11 Eu3 Eu3 103.5(2) 3_655 4_565 ?
O11 Eu3 Eu3 40.7(2) 3_655 3_655 ?
O11 Eu3 Eu3 103.2(2) . 3_655 ?
O11 Eu3 O4 100.8(3) 3_655 . ?
O11 Eu3 O9 64.8(3) . . ?
O11 Eu3 O9 65.7(3) 3_655 . ?
O11 Eu3 O11 89.7(4) 3_655 . ?
O11 Eu3 N1 138.7(3) . . ?
O11 Eu3 N1 75.1(3) 3_655 . ?
O11 Eu3 C6 21.7(3) 3_655 3_655 ?
O11 Eu3 C6 88.6(3) . 3_655 ?
N1 Eu3 Eu1 121.3(2) . . ?
N1 Eu3 Eu3 177.9(2) . 4_565 ?
N1 Eu3 Eu3 89.9(2) . 3_655 ?
N1 Eu3 O9 134.6(2) . . ?
N1 Eu3 C6 63.3(3) . 3_655 ?
C6 Eu3 Eu1 121.6(2) 3_655 . ?
C6 Eu3 Eu3 61.6(2) 3_655 3_655 ?
C6 Eu3 Eu3 114.8(2) 3_655 4_565 ?
C7 O1 Eu3 141.1(8) . . ?
C15 O2 Eu2 144.2(9) . . ?
C24 O3 Eu2 142.2(12) . . ?
C16 O4 Eu3 133.7(11) . . ?
C27 O5 C23 118.1(13) . . ?
C11 O6 C22 118.3(12) . . ?
Eu2 O7 Eu1 86.4(4) . . ?
Eu2 O7 Eu1 86.4(4) 2_665 . ?
Eu2 O7 Eu1 86.4(4) 4_565 . ?
Eu2 O7 Eu1 86.4(4) 3_655 . ?
Eu2 O7 Eu2 89.77(4) 2_665 3_655 ?
Eu2 O7 Eu2 89.77(5) . 3_655 ?
Eu2 O7 Eu2 172.7(7) . 2_665 ?
Eu2 O7 Eu2 89.77(5) . 4_565 ?
Eu2 O7 Eu2 89.77(5) 2_665 4_565 ?
Eu2 O7 Eu2 172.7(7) 3_655 4_565 ?
Eu3 O8 Eu1 102.3(3) 4_565 . ?
Eu3 O8 Eu1 101.5(3) . . ?
Eu3 O8 Eu3 103.2(3) 4_565 . ?
Eu3 O9 Eu1 86.1(4) 4_565 . ?
Eu3 O9 Eu1 86.1(4) . . ?
Eu3 O9 Eu1 86.1(4) 3_655 . ?
Eu3 O9 Eu1 86.1(4) 2_665 . ?
Eu3 O9 Eu3 89.73(5) 4_565 . ?
Eu3 O9 Eu3 89.73(5) 3_655 . ?
Eu3 O9 Eu3 172.1(7) 3_655 4_565 ?
Eu3 O9 Eu3 89.73(5) 2_665 3_655 ?
Eu3 O9 Eu3 89.73(5) 2_665 4_565 ?
Eu3 O9 Eu3 172.1(7) 2_665 . ?
Eu2 O10 Eu1 102.2(3) 3_655 . ?
Eu2 O10 Eu1 101.3(3) . . ?
Eu2 O10 Eu2 102.9(3) 3_655 . ?
Eu3 O11 Eu3 100.0(3) 4_565 . ?
C6 O11 Eu3 137.7(8) . . ?
C6 O11 Eu3 118.6(8) . 4_565 ?
Eu2 O12 Eu2 99.4(3) . 4_565 ?
C4 O12 Eu2 120.5(8) . . ?
C4 O12 Eu2 135.6(8) . 4_565 ?
C2 N1 Eu3 127.2(9) . . ?
C2 N1 C12 115.6(11) . . ?
C12 N1 Eu3 117.1(8) . . ?
C16 N2 C21 121.2(15) . . ?
C16 N2 C33 121.8(13) . . ?
C21 N2 C33 116.9(14) . . ?
C14 N3 Eu2 127.8(9) . . ?
C14 N3 C32 112.7(12) . . ?
C32 N3 Eu2 119.4(9) . . ?
C24 N4 C25 124(2) . . ?
C24 N4 C26 116(2) . . ?
C25 N4 C26 119(2) . . ?
C27 C1 C15 122.5(13) . . ?
N1 C2 C9 129.5(13) . . ?
C11 C3 C7 119.0(14) . . ?
O12 C4 C10 120.0(13) . . ?
O12 C4 C28 120.9(11) . . ?
C10 C4 C28 119.1(12) . . ?
C6 C5 C12 118.9(12) . 4_565 ?
C6 C5 C17 120.1(13) . . ?
C17 C5 C12 120.8(13) . 4_565 ?
O11 C6 Eu3 39.7(6) . 4_565 ?
O11 C6 C5 120.9(12) . . ?
O11 C6 C8 118.2(12) . . ?
C5 C6 Eu3 98.0(9) . 4_565 ?
C5 C6 C8 120.9(13) . . ?
C8 C6 Eu3 127.8(9) . 4_565 ?
O1 C7 C3 116.6(12) . . ?
O1 C7 C9 123.5(12) . . ?
C9 C7 C3 120.0(13) . . ?
C34 C8 C6 117.4(14) . . ?
C7 C9 C2 122.5(13) . . ?
C7 C9 C36 118.3(13) . . ?
C36 C9 C2 119.0(13) . . ?
C13 C10 C4 120.7(13) . . ?
O6 C11 C3 122.9(14) . . ?
O6 C11 C30 116.2(13) . . ?
C3 C11 C30 120.9(13) . . ?
N1 C12 C5 113.6(11) . 3_655 ?
C18 C13 C10 118.5(13) . . ?
N3 C14 C29 128.2(13) . . ?
O2 C15 C1 122.4(13) . . ?
O2 C15 C29 121.9(12) . . ?
C1 C15 C29 115.6(12) . . ?
O4 C16 N2 126.4(15) . . ?
C5 C17 C20 120.9(14) . . ?
C13 C18 C31 121.7(14) . . ?
C35 C19 C29 124.8(16) . . ?
C34 C20 C17 118.2(14) . . ?
O3 C24 N4 125(2) . . ?
C1 C27 O5 113.2(13) . . ?
C35 C27 O5 124.8(13) . . ?
C35 C27 C1 122.0(14) . . ?
C4 C28 C32 119.5(12) . . ?
C31 C28 C4 118.5(12) . . ?
C31 C28 C32 122.0(13) . . ?
C15 C29 C14 123.8(12) . . ?
C19 C29 C14 117.9(14) . . ?
C19 C29 C15 118.2(14) . . ?
C36 C30 C11 118.8(14) . . ?
C18 C31 C28 121.5(14) . . ?
N3 C32 C28 113.4(11) . . ?
C20 C34 C8 122.5(15) . . ?
C19 C35 C27 116.6(14) . . ?
C30 C36 C9 123.0(15) . . ?

_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_t9_sq
_database_code_depnum_ccdc_archive 'CCDC 1924487'
loop_
_audit_author_name
_audit_author_address
'Yuan Huang'
;Soochow university
China
;
_audit_update_record             
;
2019-11-06 deposited with the CCDC.	2019-11-13 downloaded from the CCDC.
;
_audit_creation_date             2019-10-31
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2014/7
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C144 H168 N16 O42 Tb9, H3 O, 3(H2O)'
_chemical_formula_sum            'C144 H177 N16 O46 Tb9'
_chemical_formula_weight         4296.52
_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'
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'
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           85
_space_group_name_H-M_alt        'P 4/n'
_space_group_name_Hall           '-P 4a'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y+1/2, z'
'-y+1/2, x, z'
'y, -x+1/2, z'
'-x, -y, -z'
'x-1/2, y-1/2, -z'
'y-1/2, -x, -z'
'-y, x-1/2, -z'

_cell_length_a                   21.5916(3)
_cell_length_b                   21.5916(3)
_cell_length_c                   17.8737(4)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     8332.7(3)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    12737
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      29.6590
_cell_measurement_theta_min      3.1210
_shelx_estimated_absorpt_T_max   0.802
_shelx_estimated_absorpt_T_min   0.514
_exptl_absorpt_coefficient_mu    3.841
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.77832
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.684
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             4130
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.06
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0481
_diffrn_reflns_av_unetI/netI     0.0443
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            32014
_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         25.678
_diffrn_reflns_theta_min         3.106
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'multiwire proportional'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                6183
_reflns_number_total             7897
_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       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_refine_diff_density_max         2.043
_refine_diff_density_min         -1.399
_refine_diff_density_rms         0.151
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     492
_refine_ls_number_reflns         7897
_refine_ls_number_restraints     86
_refine_ls_R_factor_all          0.0592
_refine_ls_R_factor_gt           0.0403
_refine_ls_restrained_S_all      1.073
_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)+(0.0268P)²+66.3568P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0862
_refine_ls_wR_factor_ref         0.0982
_refine_special_details          
;
The SQUEEZE routine of PLATON was used in the treatment of the crystallographic data. The identities and numbers of the lattice solvents were determined by the TGA and elemental analysis. The calculated mass loss corresponding to the solvent guests from the crystals between 30 and 100?ãC was 1.70%. However, the experimental result 1.79% was nearly consistent with calculated result. This indicates that three water molecules and one hydronium ion might be lost during the test process and elemental analysis results of C 40.24, H 4.15, N 5.21, which are consistent with the experimental data.
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Rigid bond restraints
 C34, N4, O10, C35, C36
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.001
3. Uiso/Uaniso restraints and constraints
C34 \\sim N4 \\sim O10 \\sim C35 \\sim C36: within 2A with sigma of 0.005 and
sigma for terminal atoms of 0.001
Uanis(C34) \\sim Ueq, Uanis(N4) \\sim Ueq, Uanis(O10) \\sim Ueq, Uanis(C35)
\\sim Ueq, Uanis(C36) \\sim Ueq: with sigma of 0.01 and sigma for terminal
atoms of 0.02
4. Rigid body (RIGU) restrains
 C34, N4, O10, C35, C36
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
5.a Secondary CH2 refined with riding coordinates:
 C23(H23A,H23B), C24(H24A,H24B)
5.b Aromatic/amide H refined with riding coordinates:
 C3(H3A), C5(H5), C8(H8), C9(H9), C10(H10), C13(H13), C15(H15), C16(H16),
 C18(H18), C19(H19), C20(H20), C22(H22), C25(H25), C26(H26), C29(H29), C30(H30),
  C31(H31), C34(H34)
5.c Idealised Me refined as rotating group:
 C27(H27A,H27B,H27C), C28(H28A,H28B,H28C), C32(H32A,H32B,H32C), C33(H33A,H33B,
 H33C), C35(H35A,H35B,H35C), C36(H36A,H36B,H36C)
;
_atom_sites_solution_hydrogens   mixed
_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 0.7500 0.7500 0.71167(3) 0.01908(14) Uani 1 4 d S T P . .
Tb2 Tb 0.64442(2) 0.69840(2) 0.56513(2) 0.02130(9) Uani 1 1 d . . . . .
Tb3 Tb 0.63672(2) 0.77995(2) 0.85885(2) 0.02232(9) Uani 1 1 d . . . . .
O1 O 0.7500 0.7500 0.5559(5) 0.024(2) Uani 1 4 d S T P . .
O2 O 0.6588(2) 0.7796(2) 0.6431(3) 0.0271(11) Uani 1 1 d . . . . .
O3 O 0.7032(2) 0.8334(2) 0.7809(3) 0.0274(11) Uani 1 1 d . . . . .
O4 O 0.7500 0.7500 0.8698(5) 0.030(2) Uani 1 4 d S T P . .
O5 O 0.6467(2) 0.7822(2) 0.4846(2) 0.0311(11) Uani 1 1 d . . . . .
O6 O 0.6555(2) 0.6980(2) 0.9387(3) 0.0330(12) Uani 1 1 d . . . . .
O7 O 0.5922(2) 0.6537(2) 0.6575(3) 0.0344(12) Uani 1 1 d . . . . .
O8 O 0.5759(2) 0.8158(2) 0.7681(3) 0.0366(12) Uani 1 1 d . . . . .
O9 O 0.5885(2) 0.6288(3) 0.4897(3) 0.0448(14) Uani 1 1 d . . . . .
O10 O 0.5684(3) 0.8324(3) 0.9391(4) 0.0676(16) Uani 1 1 d . U . . .
O11 O 0.4594(3) 0.5350(3) 0.8162(3) 0.0529(16) Uani 1 1 d . . . . .
N1 N 0.5330(3) 0.7373(3) 0.5594(3) 0.0346(14) Uani 1 1 d . . . . .
N2 N 0.5355(3) 0.7194(3) 0.8632(3) 0.0374(15) Uani 1 1 d . . . . .
O12 O 0.4315(3) 0.9020(3) 0.6027(4) 0.0583(17) Uani 1 1 d . . . . .
N3 N 0.5547(3) 0.5788(3) 0.3857(4) 0.0428(17) Uani 1 1 d . . . . .
C1 C 0.6090(4) 0.7843(3) 0.4249(4) 0.0327(17) Uani 1 1 d . . . . .
C2 C 0.6190(4) 0.6860(3) 0.9980(4) 0.0320(17) Uani 1 1 d . . . . .
C3 C 0.4853(4) 0.7115(4) 0.5901(4) 0.0354(17) Uani 1 1 d . . . . .
H3A H 0.4472 0.7274 0.5754 0.042 Uiso 1 1 calc R . . . .
C4 C 0.5363(3) 0.6375(3) 0.6777(4) 0.0325(17) Uani 1 1 d . . . . .
C5 C 0.5286(4) 0.5948(3) 0.7370(4) 0.0336(17) Uani 1 1 d . . . . .
H5 H 0.5632 0.5789 0.7614 0.040 Uiso 1 1 calc R . . . .
C6 C 0.5445(3) 0.7866(3) 0.4345(4) 0.0339(17) Uani 1 1 d . . . . .
C7 C 0.4826(3) 0.6623(4) 0.6433(4) 0.0335(17) Uani 1 1 d . . . . .
C8 C 0.6419(4) 0.6893(4) 1.0710(4) 0.0384(18) Uani 1 1 d . . . . .
H8 H 0.6835 0.6986 1.0791 0.046 Uiso 1 1 calc R . . . .
C9 C 0.5006(4) 0.8577(4) 0.6864(4) 0.0397(19) Uani 1 1 d . . . . .
H9 H 0.5308 0.8817 0.6631 0.048 Uiso 1 1 calc R . . . .
C10 C 0.6326(4) 0.7846(3) 0.3520(4) 0.0373(18) Uani 1 1 d . . . . .
H10 H 0.6752 0.7849 0.3443 0.045 Uiso 1 1 calc R . . . .
C11 C 0.5182(3) 0.8185(4) 0.7452(4) 0.0348(17) Uani 1 1 d . . . . .
C12 C 0.4704(4) 0.5766(4) 0.7589(4) 0.0379(18) Uani 1 1 d . . . . .
C13 C 0.4842(4) 0.7325(4) 0.8304(4) 0.0389(18) Uani 1 1 d . . . . .
H13 H 0.4509 0.7070 0.8423 0.047 Uiso 1 1 calc R . . . .
C14 C 0.4406(4) 0.8621(4) 0.6620(4) 0.0412(19) Uani 1 1 d . . . . .
C15 C 0.4170(4) 0.6001(4) 0.7247(5) 0.047(2) Uani 1 1 d . . . . .
H15 H 0.3777 0.5872 0.7394 0.057 Uiso 1 1 calc R . . . .
C16 C 0.6037(5) 0.6790(4) 1.1308(4) 0.049(2) Uani 1 1 d . . . . .
H16 H 0.6196 0.6813 1.1791 0.059 Uiso 1 1 calc R . . . .
N4 N 0.4883(5) 0.8433(5) 1.0181(7) 0.1027(19) Uani 1 1 d . U . . .
C17 C 0.4711(4) 0.7814(4) 0.7777(4) 0.0400(19) Uani 1 1 d . . . . .
C18 C 0.5060(4) 0.7851(4) 0.3732(5) 0.049(2) Uani 1 1 d . . . . .
H18 H 0.4634 0.7848 0.3805 0.059 Uiso 1 1 calc R . . . .
C19 C 0.5737(4) 0.6285(4) 0.4223(5) 0.047(2) Uani 1 1 d . . . . .
H19 H 0.5762 0.6656 0.3961 0.056 Uiso 1 1 calc R . . . .
C20 C 0.5926(5) 0.7845(4) 0.2910(4) 0.048(2) Uani 1 1 d . . . . .
H20 H 0.6087 0.7848 0.2427 0.058 Uiso 1 1 calc R . . . .
C21 C 0.5563(4) 0.6712(4) 0.9877(4) 0.0373(18) Uani 1 1 d . . . . .
C22 C 0.4247(4) 0.6429(4) 0.6685(5) 0.046(2) Uani 1 1 d . . . . .
H22 H 0.3896 0.6598 0.6462 0.055 Uiso 1 1 calc R . . . .
C23 C 0.5349(4) 0.6621(4) 0.9080(4) 0.0398(19) Uani 1 1 d . . . . .
H23A H 0.5615 0.6318 0.8841 0.048 Uiso 1 1 calc R . . . .
H23B H 0.4932 0.6455 0.9085 0.048 Uiso 1 1 calc R . . . .
C24 C 0.5202(4) 0.7921(4) 0.5131(4) 0.0389(18) Uani 1 1 d . . . . .
H24A H 0.5387 0.8281 0.5366 0.047 Uiso 1 1 calc R . . . .
H24B H 0.4758 0.7987 0.5112 0.047 Uiso 1 1 calc R . . . .
C25 C 0.5185(4) 0.6617(4) 1.0481(5) 0.049(2) Uani 1 1 d . . . . .
H25 H 0.4768 0.6528 1.0405 0.058 Uiso 1 1 calc R . . . .
C26 C 0.5289(5) 0.7838(4) 0.3013(4) 0.050(2) Uani 1 1 d . . . . .
H26 H 0.5022 0.7826 0.2605 0.060 Uiso 1 1 calc R . . . .
C27 C 0.5501(5) 0.5182(4) 0.4207(5) 0.058(3) Uani 1 1 d . . . . .
H27A H 0.5786 0.4903 0.3971 0.088 Uiso 1 1 calc GR . . . .
H27B H 0.5086 0.5028 0.4151 0.088 Uiso 1 1 calc GR . . . .
H27C H 0.5599 0.5216 0.4729 0.088 Uiso 1 1 calc GR . . . .
C28 C 0.5401(5) 0.5831(5) 0.3062(5) 0.066(3) Uani 1 1 d . . . . .
H28A H 0.5391 0.6259 0.2915 0.099 Uiso 1 1 calc GR . . . .
H28B H 0.5004 0.5647 0.2971 0.099 Uiso 1 1 calc GR . . . .
H28C H 0.5711 0.5617 0.2778 0.099 Uiso 1 1 calc GR . . . .
C29 C 0.4105(4) 0.7863(4) 0.7503(5) 0.055(2) Uani 1 1 d . . . . .
H29 H 0.3800 0.7610 0.7706 0.066 Uiso 1 1 calc R . . . .
C30 C 0.3944(4) 0.8272(5) 0.6948(6) 0.059(3) Uani 1 1 d . . . . .
H30 H 0.3534 0.8312 0.6796 0.071 Uiso 1 1 calc R . . . .
C31 C 0.5417(5) 0.6652(4) 1.1207(5) 0.053(2) Uani 1 1 d . . . . .
H31 H 0.5160 0.6583 1.1617 0.063 Uiso 1 1 calc R . . . .
C32 C 0.5112(5) 0.5041(4) 0.8492(5) 0.058(3) Uani 1 1 d . . . . .
H32A H 0.5371 0.4875 0.8104 0.087 Uiso 1 1 calc GR . . . .
H32B H 0.4967 0.4710 0.8805 0.087 Uiso 1 1 calc GR . . . .
H32C H 0.5345 0.5329 0.8787 0.087 Uiso 1 1 calc GR . . . .
C33 C 0.3709(5) 0.9053(5) 0.5711(7) 0.082(4) Uani 1 1 d . . . . .
H33A H 0.3706 0.9351 0.5313 0.123 Uiso 1 1 calc GR . . . .
H33B H 0.3419 0.9175 0.6090 0.123 Uiso 1 1 calc GR . . . .
H33C H 0.3595 0.8654 0.5518 0.123 Uiso 1 1 calc GR . . . .
C34 C 0.5191(6) 0.8397(6) 0.9594(8) 0.0940(19) Uani 1 1 d . U . . .
H34 H 0.4930 0.8447 0.9185 0.113 Uiso 1 1 calc R . . . .
C35 C 0.5184(6) 0.8341(7) 1.0886(8) 0.1037(19) Uani 1 1 d . U . . .
H35A H 0.5541 0.8083 1.0817 0.155 Uiso 1 1 calc GR . . . .
H35B H 0.4902 0.8145 1.1227 0.155 Uiso 1 1 calc GR . . . .
H35C H 0.5309 0.8735 1.1085 0.155 Uiso 1 1 calc GR . . . .
C36 C 0.4240(6) 0.8556(7) 1.0231(8) 0.1039(19) Uani 1 1 d . U . . .
H36A H 0.4178 0.8960 1.0443 0.156 Uiso 1 1 calc GR . . . .
H36B H 0.4047 0.8251 1.0544 0.156 Uiso 1 1 calc GR . . . .
H36C H 0.4060 0.8542 0.9740 0.156 Uiso 1 1 calc GR . . . .
H2 H 0.638(3) 0.793(3) 0.677(4) 0.03(2) Uiso 1 1 d . . . . .
H3 H 0.687(3) 0.853(3) 0.751(4) 0.03(2) Uiso 1 1 d . . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Tb1 Tb2 3.6467(5) 3_655 ?
Tb1 Tb2 3.6466(5) . ?
Tb1 O1 2.784(8) . ?
Tb1 O2 2.405(5) 4_565 ?
Tb1 O2 2.405(5) 3_655 ?
Tb1 O2 2.405(5) 2_665 ?
Tb1 O2 2.406(5) . ?
Tb1 O3 2.408(5) 2_665 ?
Tb1 O3 2.408(5) 3_655 ?
Tb1 O3 2.408(5) . ?
Tb1 O3 2.408(5) 4_565 ?
Tb1 O4 2.826(9) . ?
Tb2 Tb2 3.5883(4) 4_565 ?
Tb2 Tb2 3.5884(4) 3_655 ?
Tb2 O1 2.5427(7) . ?
Tb2 O2 2.262(5) . ?
Tb2 O2 2.315(5) 3_655 ?
Tb2 O5 2.313(5) . ?
Tb2 O5 2.413(5) 3_655 ?
Tb2 O7 2.220(5) . ?
Tb2 O9 2.353(5) . ?
Tb2 N1 2.551(6) . ?
Tb3 Tb3 3.5779(5) 4_565 ?
Tb3 Tb3 3.5779(4) 3_655 ?
Tb3 O3 2.259(5) 3_655 ?
Tb3 O3 2.310(5) . ?
Tb3 O4 2.5374(8) . ?
Tb3 O6 2.309(5) . ?
Tb3 O6 2.394(5) 4_565 ?
Tb3 O8 2.226(5) . ?
Tb3 O10 2.348(7) . ?
Tb3 N2 2.548(6) . ?
O1 Tb2 2.5427(6) 4_565 ?
O1 Tb2 2.5427(6) 3_655 ?
O1 Tb2 2.5427(6) 2_665 ?
O2 Tb2 2.315(5) 4_565 ?
O2 H2 0.81(8) . ?
O3 Tb3 2.259(5) 4_565 ?
O3 H3 0.77(7) . ?
O4 Tb3 2.5375(8) 3_655 ?
O4 Tb3 2.5375(8) 2_665 ?
O4 Tb3 2.5375(8) 4_565 ?
O5 Tb2 2.413(5) 4_565 ?
O5 C1 1.342(8) . ?
O6 Tb3 2.394(5) 3_655 ?
O6 C2 1.345(8) . ?
O7 C4 1.307(8) . ?
O8 C11 1.313(9) . ?
O9 C19 1.246(9) . ?
O10 C34 1.136(13) . ?
O11 C12 1.382(9) . ?
O11 C32 1.430(11) . ?
N1 C3 1.292(9) . ?
N1 C24 1.470(9) . ?
N2 C13 1.285(10) . ?
N2 C23 1.473(9) . ?
O12 C14 1.380(10) . ?
O12 C33 1.427(11) . ?
N3 C19 1.322(10) . ?
N3 C27 1.454(11) . ?
N3 C28 1.458(10) . ?
C1 C6 1.404(11) . ?
C1 C10 1.400(10) . ?
C2 C8 1.399(10) . ?
C2 C21 1.403(11) . ?
C3 H3A 0.9300 . ?
C3 C7 1.426(10) . ?
C4 C5 1.416(10) . ?
C4 C7 1.418(10) . ?
C5 H5 0.9300 . ?
C5 C12 1.373(10) . ?
C6 C18 1.376(10) . ?
C6 C24 1.504(10) . ?
C7 C22 1.392(11) . ?
C8 H8 0.9300 . ?
C8 C16 1.369(11) . ?
C9 H9 0.9300 . ?
C9 C11 1.402(11) . ?
C9 C14 1.372(11) . ?
C10 H10 0.9300 . ?
C10 C20 1.391(11) . ?
C11 C17 1.420(11) . ?
C12 C15 1.401(12) . ?
C13 H13 0.9300 . ?
C13 C17 1.442(11) . ?
C14 C30 1.381(12) . ?
C15 H15 0.9300 . ?
C15 C22 1.376(12) . ?
C16 H16 0.9300 . ?
C16 C31 1.382(13) . ?
N4 C34 1.244(14) . ?
N4 C35 1.431(17) . ?
N4 C36 1.416(15) . ?
C17 C29 1.402(11) . ?
C18 H18 0.9300 . ?
C18 C26 1.377(12) . ?
C19 H19 0.9300 . ?
C20 H20 0.9300 . ?
C20 C26 1.387(13) . ?
C21 C23 1.509(10) . ?
C21 C25 1.369(11) . ?
C22 H22 0.9300 . ?
C23 H23A 0.9700 . ?
C23 H23B 0.9700 . ?
C24 H24A 0.9700 . ?
C24 H24B 0.9700 . ?
C25 H25 0.9300 . ?
C25 C31 1.395(12) . ?
C26 H26 0.9300 . ?
C27 H27A 0.9600 . ?
C27 H27B 0.9600 . ?
C27 H27C 0.9600 . ?
C28 H28A 0.9600 . ?
C28 H28B 0.9600 . ?
C28 H28C 0.9600 . ?
C29 H29 0.9300 . ?
C29 C30 1.372(12) . ?
C30 H30 0.9300 . ?
C31 H31 0.9300 . ?
C32 H32A 0.9600 . ?
C32 H32B 0.9600 . ?
C32 H32C 0.9600 . ?
C33 H33A 0.9600 . ?
C33 H33B 0.9600 . ?
C33 H33C 0.9600 . ?
C34 H34 0.9300 . ?
C35 H35A 0.9600 . ?
C35 H35B 0.9600 . ?
C35 H35C 0.9600 . ?
C36 H36A 0.9600 . ?
C36 H36B 0.9600 . ?
C36 H36C 0.9600 . ?

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
Tb2 Tb1 Tb2 58.946(9) . 3_655 ?
O1 Tb1 Tb2 44.091(8) . . ?
O1 Tb1 Tb2 44.092(8) . 3_655 ?
O1 Tb1 O4 180.0 . . ?
O2 Tb1 Tb2 38.52(11) 2_665 3_655 ?
O2 Tb1 Tb2 93.68(12) 4_565 3_655 ?
O2 Tb1 Tb2 37.23(11) 3_655 3_655 ?
O2 Tb1 Tb2 92.88(12) . 3_655 ?
O2 Tb1 Tb2 92.88(12) 4_565 . ?
O2 Tb1 Tb2 38.53(11) 3_655 . ?
O2 Tb1 Tb2 37.22(11) . . ?
O2 Tb1 Tb2 93.68(12) 2_665 . ?
O2 Tb1 O1 59.36(12) . . ?
O2 Tb1 O1 59.36(12) 3_655 . ?
O2 Tb1 O1 59.36(12) 4_565 . ?
O2 Tb1 O1 59.36(12) 2_665 . ?
O2 Tb1 O2 118.7(2) 3_655 4_565 ?
O2 Tb1 O2 118.7(2) 2_665 . ?
O2 Tb1 O2 74.94(11) 3_655 . ?
O2 Tb1 O2 74.95(11) 3_655 2_665 ?
O2 Tb1 O2 74.95(11) 4_565 2_665 ?
O2 Tb1 O2 74.95(11) 4_565 . ?
O2 Tb1 O3 139.67(16) 2_665 3_655 ?
O2 Tb1 O3 143.55(16) 2_665 . ?
O2 Tb1 O3 76.20(16) 2_665 4_565 ?
O2 Tb1 O3 76.20(16) . 3_655 ?
O2 Tb1 O3 143.55(16) 3_655 4_565 ?
O2 Tb1 O3 76.20(16) 3_655 2_665 ?
O2 Tb1 O3 143.55(16) . 2_665 ?
O2 Tb1 O3 139.67(16) 4_565 2_665 ?
O2 Tb1 O3 73.71(17) . . ?
O2 Tb1 O3 73.70(17) 3_655 3_655 ?
O2 Tb1 O3 73.70(17) 4_565 4_565 ?
O2 Tb1 O3 73.70(17) 2_665 2_665 ?
O2 Tb1 O3 139.67(16) . 4_565 ?
O2 Tb1 O3 143.55(16) 4_565 3_655 ?
O2 Tb1 O3 76.20(16) 4_565 . ?
O2 Tb1 O3 139.67(16) 3_655 . ?
O2 Tb1 O4 120.64(12) 4_565 . ?
O2 Tb1 O4 120.64(12) . . ?
O2 Tb1 O4 120.64(12) 2_665 . ?
O2 Tb1 O4 120.64(12) 3_655 . ?
O3 Tb1 Tb2 76.89(12) 2_665 3_655 ?
O3 Tb1 Tb2 113.76(11) 4_565 3_655 ?
O3 Tb1 Tb2 109.59(12) 3_655 3_655 ?
O3 Tb1 Tb2 113.77(12) 2_665 . ?
O3 Tb1 Tb2 76.89(12) 3_655 . ?
O3 Tb1 Tb2 109.59(12) . . ?
O3 Tb1 Tb2 164.81(12) . 3_655 ?
O3 Tb1 Tb2 164.80(12) 4_565 . ?
O3 Tb1 O1 120.93(12) 3_655 . ?
O3 Tb1 O1 120.93(12) 4_565 . ?
O3 Tb1 O1 120.93(12) . . ?
O3 Tb1 O1 120.93(12) 2_665 . ?
O3 Tb1 O3 74.69(11) 4_565 2_665 ?
O3 Tb1 O3 74.69(11) . 3_655 ?
O3 Tb1 O3 74.69(11) 3_655 2_665 ?
O3 Tb1 O3 118.1(2) 4_565 3_655 ?
O3 Tb1 O3 118.1(2) . 2_665 ?
O3 Tb1 O3 74.68(11) . 4_565 ?
O3 Tb1 O4 59.07(12) 2_665 . ?
O3 Tb1 O4 59.07(12) . . ?
O3 Tb1 O4 59.07(12) 4_565 . ?
O3 Tb1 O4 59.07(12) 3_655 . ?
O4 Tb1 Tb2 135.909(8) . . ?
O4 Tb1 Tb2 135.908(8) . 3_655 ?
Tb2 Tb2 Tb1 60.528(5) 4_565 . ?
Tb2 Tb2 Tb1 60.528(5) 3_655 . ?
Tb2 Tb2 Tb2 90.0 4_565 3_655 ?
O1 Tb2 Tb1 49.63(19) . . ?
O1 Tb2 Tb2 45.122(13) . 4_565 ?
O1 Tb2 Tb2 45.121(12) . 3_655 ?
O1 Tb2 N1 134.34(15) . . ?
O2 Tb2 Tb1 40.05(12) . . ?
O2 Tb2 Tb1 40.33(12) 3_655 . ?
O2 Tb2 Tb2 38.90(12) . 4_565 ?
O2 Tb2 Tb2 96.83(12) 3_655 4_565 ?
O2 Tb2 Tb2 37.84(12) 3_655 3_655 ?
O2 Tb2 Tb2 96.99(13) . 3_655 ?
O2 Tb2 O1 64.26(18) 3_655 . ?
O2 Tb2 O1 64.96(19) . . ?
O2 Tb2 O2 79.5(2) . 3_655 ?
O2 Tb2 O5 76.89(16) . . ?
O2 Tb2 O5 73.95(16) 3_655 3_655 ?
O2 Tb2 O5 129.48(17) . 3_655 ?
O2 Tb2 O9 118.22(19) 3_655 . ?
O2 Tb2 O9 156.78(18) . . ?
O2 Tb2 N1 144.47(18) 3_655 . ?
O2 Tb2 N1 84.21(19) . . ?
O5 Tb2 Tb1 99.18(11) 3_655 . ?
O5 Tb2 Tb1 101.21(11) . . ?
O5 Tb2 Tb2 41.66(11) . 4_565 ?
O5 Tb2 Tb2 102.98(12) 3_655 4_565 ?
O5 Tb2 Tb2 103.55(12) . 3_655 ?
O5 Tb2 Tb2 39.58(11) 3_655 3_655 ?
O5 Tb2 O1 66.28(17) . . ?
O5 Tb2 O1 64.91(16) 3_655 . ?
O5 Tb2 O2 130.40(17) . 3_655 ?
O5 Tb2 O5 88.7(2) . 3_655 ?
O5 Tb2 O9 98.89(19) . . ?
O5 Tb2 N1 74.77(18) . . ?
O5 Tb2 N1 138.36(17) 3_655 . ?
O7 Tb2 Tb1 85.19(12) . . ?
O7 Tb2 Tb2 125.16(13) . 4_565 ?
O7 Tb2 Tb2 109.84(13) . 3_655 ?
O7 Tb2 O1 134.0(2) . . ?
O7 Tb2 O2 87.06(18) . . ?
O7 Tb2 O2 75.64(17) . 3_655 ?
O7 Tb2 O5 144.43(18) . . ?
O7 Tb2 O5 125.15(18) . 3_655 ?
O7 Tb2 O9 83.54(19) . . ?
O7 Tb2 N1 72.15(19) . . ?
O9 Tb2 Tb1 158.08(15) . . ?
O9 Tb2 Tb2 106.16(13) . 3_655 ?
O9 Tb2 Tb2 140.44(15) . 4_565 ?
O9 Tb2 O1 134.7(2) . . ?
O9 Tb2 O5 72.54(17) . 3_655 ?
O9 Tb2 N1 72.71(19) . . ?
N1 Tb2 Tb1 121.19(13) . . ?
N1 Tb2 Tb2 89.71(14) . 4_565 ?
N1 Tb2 Tb2 177.69(13) . 3_655 ?
Tb3 Tb3 Tb1 60.650(5) 4_565 . ?
Tb3 Tb3 Tb1 60.651(5) 3_655 . ?
Tb3 Tb3 Tb3 90.001(1) 3_655 4_565 ?
O3 Tb3 Tb1 40.29(12) . . ?
O3 Tb3 Tb1 40.02(13) 3_655 . ?
O3 Tb3 Tb3 96.87(13) . 3_655 ?
O3 Tb3 Tb3 38.96(12) 3_655 3_655 ?
O3 Tb3 Tb3 97.02(13) 3_655 4_565 ?
O3 Tb3 Tb3 37.96(12) . 4_565 ?
O3 Tb3 O3 79.5(2) 3_655 . ?
O3 Tb3 O4 64.8(2) . . ?
O3 Tb3 O4 65.5(2) 3_655 . ?
O3 Tb3 O6 74.04(16) . 4_565 ?
O3 Tb3 O6 129.59(18) 3_655 4_565 ?
O3 Tb3 O6 76.64(17) 3_655 . ?
O3 Tb3 O10 121.2(2) . . ?
O3 Tb3 O10 155.5(2) 3_655 . ?
O3 Tb3 N2 143.89(19) . . ?
O3 Tb3 N2 83.5(2) 3_655 . ?
O4 Tb3 Tb1 50.5(2) . . ?
O4 Tb3 Tb3 45.169(16) . 4_565 ?
O4 Tb3 Tb3 45.171(17) . 3_655 ?
O4 Tb3 N2 133.94(15) . . ?
O6 Tb3 Tb1 101.09(12) . . ?
O6 Tb3 Tb1 99.35(11) 4_565 . ?
O6 Tb3 Tb3 103.04(12) 4_565 3_655 ?
O6 Tb3 Tb3 41.36(12) . 3_655 ?
O6 Tb3 Tb3 103.53(13) . 4_565 ?
O6 Tb3 Tb3 39.59(11) 4_565 4_565 ?
O6 Tb3 O3 130.32(18) . . ?
O6 Tb3 O4 64.53(17) 4_565 . ?
O6 Tb3 O4 65.69(18) . . ?
O6 Tb3 O6 88.9(2) . 4_565 ?
O6 Tb3 O10 95.8(2) . . ?
O6 Tb3 N2 139.00(18) 4_565 . ?
O6 Tb3 N2 74.84(19) . . ?
O8 Tb3 Tb1 86.05(13) . . ?
O8 Tb3 Tb3 109.55(13) . 4_565 ?
O8 Tb3 Tb3 126.66(14) . 3_655 ?
O8 Tb3 O3 75.68(18) . . ?
O8 Tb3 O3 88.49(18) . 3_655 ?
O8 Tb3 O4 135.5(2) . . ?
O8 Tb3 O6 145.12(18) . . ?
O8 Tb3 O6 123.90(18) . 4_565 ?
O8 Tb3 O10 84.7(2) . . ?
O8 Tb3 N2 72.23(19) . . ?
O10 Tb3 Tb1 161.19(18) . . ?
O10 Tb3 Tb3 137.09(19) . 3_655 ?
O10 Tb3 Tb3 107.48(16) . 4_565 ?
O10 Tb3 O4 132.9(3) . . ?
O10 Tb3 O6 72.7(2) . 4_565 ?
O10 Tb3 N2 71.9(2) . . ?
N2 Tb3 Tb1 120.39(14) . . ?
N2 Tb3 Tb3 178.13(14) . 4_565 ?
N2 Tb3 Tb3 89.31(15) . 3_655 ?
Tb2 O1 Tb1 86.28(19) 4_565 . ?
Tb2 O1 Tb1 86.28(19) 3_655 . ?
Tb2 O1 Tb1 86.28(19) . . ?
Tb2 O1 Tb1 86.28(19) 2_665 . ?
Tb2 O1 Tb2 89.76(2) 2_665 3_655 ?
Tb2 O1 Tb2 89.76(2) . 3_655 ?
Tb2 O1 Tb2 89.76(2) . 4_565 ?
Tb2 O1 Tb2 172.6(4) . 2_665 ?
Tb2 O1 Tb2 89.76(2) 2_665 4_565 ?
Tb2 O1 Tb2 172.6(4) 4_565 3_655 ?
Tb1 O2 H2 100(5) . . ?
Tb2 O2 Tb1 102.72(19) . . ?
Tb2 O2 Tb1 101.14(18) 4_565 . ?
Tb2 O2 Tb2 103.26(18) . 4_565 ?
Tb2 O2 H2 114(5) 4_565 . ?
Tb2 O2 H2 131(5) . . ?
Tb1 O3 H3 105(6) . . ?
Tb3 O3 Tb1 101.36(19) . . ?
Tb3 O3 Tb1 102.9(2) 4_565 . ?
Tb3 O3 Tb3 103.09(19) 4_565 . ?
Tb3 O3 H3 127(6) 4_565 . ?
Tb3 O3 H3 114(6) . . ?
Tb3 O4 Tb1 85.6(2) 3_655 . ?
Tb3 O4 Tb1 85.6(2) . . ?
Tb3 O4 Tb1 85.6(2) 4_565 . ?
Tb3 O4 Tb1 85.6(2) 2_665 . ?
Tb3 O4 Tb3 89.66(3) 3_655 2_665 ?
Tb3 O4 Tb3 171.2(4) . 2_665 ?
Tb3 O4 Tb3 171.2(4) 3_655 4_565 ?
Tb3 O4 Tb3 89.66(3) 4_565 2_665 ?
Tb3 O4 Tb3 89.66(3) . 3_655 ?
Tb3 O4 Tb3 89.66(3) . 4_565 ?
Tb2 O5 Tb2 98.77(16) . 4_565 ?
C1 O5 Tb2 120.5(4) . . ?
C1 O5 Tb2 137.1(4) . 4_565 ?
Tb3 O6 Tb3 99.04(17) . 3_655 ?
C2 O6 Tb3 122.1(4) . . ?
C2 O6 Tb3 134.7(4) . 3_655 ?
C4 O7 Tb2 142.2(5) . . ?
C11 O8 Tb3 143.3(5) . . ?
C19 O9 Tb2 133.5(6) . . ?
C34 O10 Tb3 148.3(8) . . ?
C12 O11 C32 118.3(7) . . ?
C3 N1 Tb2 126.3(5) . . ?
C3 N1 C24 115.9(6) . . ?
C24 N1 Tb2 117.7(5) . . ?
C13 N2 Tb3 127.8(5) . . ?
C13 N2 C23 115.2(6) . . ?
C23 N2 Tb3 117.0(5) . . ?
C14 O12 C33 117.7(7) . . ?
C19 N3 C27 122.6(7) . . ?
C19 N3 C28 119.9(8) . . ?
C27 N3 C28 117.4(7) . . ?
O5 C1 C6 120.4(6) . . ?
O5 C1 C10 121.4(7) . . ?
C10 C1 C6 118.3(7) . . ?
O6 C2 C8 121.2(7) . . ?
O6 C2 C21 120.3(7) . . ?
C8 C2 C21 118.4(7) . . ?
N1 C3 H3A 115.2 . . ?
N1 C3 C7 129.6(7) . . ?
C7 C3 H3A 115.2 . . ?
O7 C4 C5 119.3(7) . . ?
O7 C4 C7 122.3(7) . . ?
C5 C4 C7 118.4(7) . . ?
C4 C5 H5 119.8 . . ?
C12 C5 C4 120.4(7) . . ?
C12 C5 H5 119.8 . . ?
C1 C6 C24 117.5(7) . . ?
C18 C6 C1 120.1(7) . . ?
C18 C6 C24 122.4(7) . . ?
C4 C7 C3 122.4(7) . . ?
C22 C7 C3 118.5(7) . . ?
C22 C7 C4 118.7(7) . . ?
C2 C8 H8 119.8 . . ?
C16 C8 C2 120.4(8) . . ?
C16 C8 H8 119.8 . . ?
C11 C9 H9 118.8 . . ?
C14 C9 H9 118.8 . . ?
C14 C9 C11 122.4(8) . . ?
C1 C10 H10 119.8 . . ?
C20 C10 C1 120.3(8) . . ?
C20 C10 H10 119.8 . . ?
O8 C11 C9 121.2(7) . . ?
O8 C11 C17 121.8(7) . . ?
C9 C11 C17 117.0(7) . . ?
O11 C12 C15 114.6(7) . . ?
C5 C12 O11 123.6(7) . . ?
C5 C12 C15 121.8(7) . . ?
N2 C13 H13 115.6 . . ?
N2 C13 C17 128.9(7) . . ?
C17 C13 H13 115.6 . . ?
O12 C14 C30 124.4(7) . . ?
C9 C14 O12 114.9(7) . . ?
C9 C14 C30 120.7(8) . . ?
C12 C15 H15 121.2 . . ?
C22 C15 C12 117.5(8) . . ?
C22 C15 H15 121.2 . . ?
C8 C16 H16 119.4 . . ?
C8 C16 C31 121.2(8) . . ?
C31 C16 H16 119.4 . . ?
C34 N4 C35 119.4(13) . . ?
C34 N4 C36 126.1(14) . . ?
C36 N4 C35 114.5(11) . . ?
C11 C17 C13 122.7(7) . . ?
C29 C17 C11 118.9(8) . . ?
C29 C17 C13 117.8(7) . . ?
C6 C18 H18 119.1 . . ?
C6 C18 C26 121.8(8) . . ?
C26 C18 H18 119.1 . . ?
O9 C19 N3 124.2(9) . . ?
O9 C19 H19 117.9 . . ?
N3 C19 H19 117.9 . . ?
C10 C20 H20 119.6 . . ?
C26 C20 C10 120.7(8) . . ?
C26 C20 H20 119.6 . . ?
C2 C21 C23 116.6(7) . . ?
C25 C21 C2 120.4(7) . . ?
C25 C21 C23 122.8(7) . . ?
C7 C22 H22 118.4 . . ?
C15 C22 C7 123.2(8) . . ?
C15 C22 H22 118.4 . . ?
N2 C23 C21 113.7(6) . . ?
N2 C23 H23A 108.8 . . ?
N2 C23 H23B 108.8 . . ?
C21 C23 H23A 108.8 . . ?
C21 C23 H23B 108.8 . . ?
H23A C23 H23B 107.7 . . ?
N1 C24 C6 113.4(6) . . ?
N1 C24 H24A 108.9 . . ?
N1 C24 H24B 108.9 . . ?
C6 C24 H24A 108.9 . . ?
C6 C24 H24B 108.9 . . ?
H24A C24 H24B 107.7 . . ?
C21 C25 H25 119.6 . . ?
C21 C25 C31 120.8(8) . . ?
C31 C25 H25 119.6 . . ?
C18 C26 C20 118.7(7) . . ?
C18 C26 H26 120.7 . . ?
C20 C26 H26 120.7 . . ?
N3 C27 H27A 109.5 . . ?
N3 C27 H27B 109.5 . . ?
N3 C27 H27C 109.5 . . ?
H27A C27 H27B 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
N3 C28 H28A 109.5 . . ?
N3 C28 H28B 109.5 . . ?
N3 C28 H28C 109.5 . . ?
H28A C28 H28B 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
C17 C29 H29 118.7 . . ?
C30 C29 C17 122.6(8) . . ?
C30 C29 H29 118.7 . . ?
C14 C30 H30 120.8 . . ?
C29 C30 C14 118.3(8) . . ?
C29 C30 H30 120.8 . . ?
C16 C31 C25 118.8(8) . . ?
C16 C31 H31 120.6 . . ?
C25 C31 H31 120.6 . . ?
O11 C32 H32A 109.5 . . ?
O11 C32 H32B 109.5 . . ?
O11 C32 H32C 109.5 . . ?
H32A C32 H32B 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
O12 C33 H33A 109.5 . . ?
O12 C33 H33B 109.5 . . ?
O12 C33 H33C 109.5 . . ?
H33A C33 H33B 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
O10 C34 N4 141.2(16) . . ?
O10 C34 H34 109.4 . . ?
N4 C34 H34 109.4 . . ?
N4 C35 H35A 109.5 . . ?
N4 C35 H35B 109.5 . . ?
N4 C35 H35C 109.5 . . ?
H35A C35 H35B 109.5 . . ?
H35A C35 H35C 109.5 . . ?
H35B C35 H35C 109.5 . . ?
N4 C36 H36A 109.5 . . ?
N4 C36 H36B 109.5 . . ?
N4 C36 H36C 109.5 . . ?
H36A C36 H36B 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?

_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_t2_sq
_database_code_depnum_ccdc_archive 'CCDC 1922397'
loop_
_audit_author_name
_audit_author_address
'Yuan Huang'
;Soochow university
China
;
_audit_update_record             
;
2019-11-06 deposited with the CCDC.	2019-11-13 downloaded from the CCDC.
;
_audit_creation_date             2019-11-06
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2014/7
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C144 H168 Ho9 N16 O42, H3 O, 2(H2O)'
_chemical_formula_sum            'C144 H175 Ho9 N16 O45'
_chemical_formula_weight         4332.56
_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'
Ho Ho -0.2175 4.6783 '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'

_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           85
_space_group_name_H-M_alt        'P 4/n'
_space_group_name_Hall           '-P 4a'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y+1/2, z'
'-y+1/2, x, z'
'y, -x+1/2, z'
'-x, -y, -z'
'x-1/2, y-1/2, -z'
'y-1/2, -x, -z'
'-y, x-1/2, -z'

_cell_length_a                   21.6913(4)
_cell_length_b                   21.6913(4)
_cell_length_c                   17.8971(7)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     8420.8(5)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    8558
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.9450
_cell_measurement_theta_min      3.1760
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    4.250
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.54908
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.688
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             4166
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.08
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.1107
_diffrn_reflns_av_unetI/netI     0.1493
_diffrn_reflns_Laue_measured_fraction_full 0.986
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            37511
_diffrn_reflns_point_group_measured_fraction_full 0.986
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.499
_diffrn_reflns_theta_min         3.039
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device_type  'multiwire proportional'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4686
_reflns_number_total             7747
_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       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_refine_diff_density_max         2.564
_refine_diff_density_min         -1.057
_refine_diff_density_rms         0.177
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.827
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     492
_refine_ls_number_reflns         7747
_refine_ls_number_restraints     86
_refine_ls_R_factor_all          0.0877
_refine_ls_R_factor_gt           0.0548
_refine_ls_restrained_S_all      0.834
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     'w=1/[σ²(Fo²)] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0985
_refine_ls_wR_factor_ref         0.1131
_refine_special_details          
;
The SQUEEZE routine of PLATON was used in the treatment of the crystallographic data. The identities and numbers of the lattice solvents were determined by the TGA and elemental analysis. The calculated mass loss corresponding to the solvent guests from the crystals between 28 and 65?ãC was 1.27%. However, the experimental result 1.28% was consistent with calculated result. This indicates that two water molecules and one hydronium ion might be lost during the test process and elemental analysis results of C 39.90, H 4.07, N 5.17, which are consistent with the experimental data.
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Rigid bond restraints
 C35, N1
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
 O8, C36, N1
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
 O8, C36, C35, N1, C34
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
3. Uiso/Uaniso restraints and constraints
C35 \\sim C36 \\sim C34: within 2A with sigma of 0.01 and sigma for terminal
atoms of 0.02
O8 \\sim C36 \\sim N1: within 2A with sigma of 0.01 and sigma for terminal
atoms of 0.02
O8 \\sim C36 \\sim N1 \\sim C35 \\sim C34: within 2A with sigma of 0.01 and
sigma for terminal atoms of 0.02
Uanis(C34) \\sim Ueq, Uanis(C36) \\sim Ueq, Uanis(C35) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
Uanis(C36) \\sim Ueq, Uanis(O8) \\sim Ueq, Uanis(N1) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
Uanis(O8) \\sim Ueq, Uanis(C36) \\sim Ueq, Uanis(C35) \\sim Ueq, Uanis(N1)
\\sim Ueq, Uanis(C34) \\sim Ueq: with sigma of 0.01 and sigma for terminal
atoms of 0.02
4. Rigid body (RIGU) restrains
 C36, C34, C35
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
 O8, C36, C35, N1, C34
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
5.a Secondary CH2 refined with riding coordinates:
 C7(H7A,H7B), C24(H24A,H24B)
5.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C8(H8), C10(H10), C11(H11A), C13(H13),
 C18(H18), C19(H19), C22(H22), C23(H23), C26(H26), C27(H27), C28(H28), C29(H29),
  C33(H33), C36(H36)
5.c Idealised Me refined as rotating group:
 C15(H15A,H15B,H15C), C16(H16A,H16B,H16C), C31(H31A,H31B,H31C), C32(H32A,H32B,
 H32C), C34(H34A,H34B,H34C), C35(H35A,H35B,H35C)
;
_atom_sites_solution_hydrogens   mixed
_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
Ho1 Ho 0.30163(2) 0.14431(2) 0.43554(2) 0.02754(14) Uani 1 1 d . . . . .
Ho2 Ho 0.2500 0.2500 0.28858(4) 0.0252(2) Uani 1 4 d S T P . .
Ho3 Ho 0.36330(2) 0.21967(2) 0.14137(2) 0.02758(14) Uani 1 1 d . . . . .
O1 O 0.5679(4) 0.0992(3) 0.3975(4) 0.060(2) Uani 1 1 d . . . . .
O2 O 0.4242(3) 0.1841(3) 0.2322(3) 0.0339(15) Uani 1 1 d . . . . .
O3 O 0.3447(3) 0.3015(3) 0.0622(3) 0.0357(16) Uani 1 1 d . . . . .
O4 O 0.5408(4) 0.4650(3) 0.1859(4) 0.057(2) Uani 1 1 d . . . . .
O5 O 0.4080(3) 0.3457(3) 0.3415(3) 0.0383(16) Uani 1 1 d . . . . .
O6 O 0.3527(3) 0.2174(3) 0.5163(3) 0.0335(16) Uani 1 1 d . . . . .
O7 O 0.3713(3) 0.0886(3) 0.5108(4) 0.0478(18) Uani 1 1 d . . . . .
O8 O 0.4312(4) 0.1674(4) 0.0600(4) 0.064(2) Uani 1 1 d . U . . .
O9 O 0.3342(3) 0.2974(3) 0.2203(3) 0.0310(15) Uani 1 1 d . . . . .
O10 O 0.2500 0.2500 0.1309(6) 0.031(3) Uani 1 4 d S T P . .
O11 O 0.3410(3) 0.2204(3) 0.3566(3) 0.0284(15) Uani 1 1 d . . . . .
O12 O 0.2500 0.2500 0.4437(6) 0.026(3) Uani 1 4 d S T P . .
N1 N 0.5093(5) 0.1551(5) -0.0195(7) 0.085(3) Uani 1 1 d . U . . .
N2 N 0.4646(4) 0.2797(4) 0.1372(4) 0.037(2) Uani 1 1 d . . . . .
N3 N 0.4662(4) 0.2626(4) 0.4407(4) 0.035(2) Uani 1 1 d . . . . .
N4 N 0.4213(4) 0.0544(4) 0.6144(4) 0.045(2) Uani 1 1 d . . . . .
C1 C 0.3819(5) 0.3131(4) 0.0025(5) 0.036(2) Uani 1 1 d . . . . .
C2 C 0.3585(5) 0.3099(4) -0.0708(5) 0.042(3) Uani 1 1 d . . . . .
H2 H 0.3171 0.3006 -0.0784 0.051 Uiso 1 1 calc R . . . .
C3 C 0.3957(6) 0.3203(5) -0.1303(5) 0.046(3) Uani 1 1 d . . . . .
H3 H 0.3798 0.3180 -0.1784 0.056 Uiso 1 1 calc R . . . .
C4 C 0.4593(5) 0.3349(5) -0.1194(6) 0.052(3) Uani 1 1 d . . . . .
H4 H 0.4852 0.3422 -0.1598 0.063 Uiso 1 1 calc R . . . .
C5 C 0.4808(5) 0.3377(5) -0.0480(6) 0.053(3) Uani 1 1 d . . . . .
H5 H 0.5224 0.3460 -0.0400 0.063 Uiso 1 1 calc R . . . .
C6 C 0.4441(5) 0.3288(4) 0.0110(5) 0.037(2) Uani 1 1 d . . . . .
C7 C 0.4657(5) 0.3378(4) 0.0925(5) 0.040(3) Uani 1 1 d . . . . .
H7A H 0.5073 0.3540 0.0923 0.048 Uiso 1 1 calc R . . . .
H7B H 0.4393 0.3680 0.1165 0.048 Uiso 1 1 calc R . . . .
C8 C 0.5157(5) 0.2670(5) 0.1705(5) 0.043(3) Uani 1 1 d . . . . .
H8 H 0.5487 0.2928 0.1593 0.052 Uiso 1 1 calc R . . . .
C9 C 0.5283(5) 0.2187(5) 0.2222(5) 0.045(3) Uani 1 1 d . . . . .
C10 C 0.5892(5) 0.2137(5) 0.2502(6) 0.052(3) Uani 1 1 d . . . . .
H10 H 0.6199 0.2389 0.2306 0.062 Uiso 1 1 calc R . . . .
C11 C 0.6038(5) 0.1731(6) 0.3049(7) 0.062(3) Uani 1 1 d . . . . .
H11A H 0.6447 0.1686 0.3194 0.075 Uiso 1 1 calc R . . . .
C12 C 0.5596(5) 0.1390(5) 0.3386(6) 0.045(3) Uani 1 1 d . . . . .
C13 C 0.4989(5) 0.1418(5) 0.3141(5) 0.045(3) Uani 1 1 d . . . . .
H13 H 0.4693 0.1173 0.3369 0.054 Uiso 1 1 calc R . . . .
C14 C 0.4816(5) 0.1810(5) 0.2554(5) 0.038(2) Uani 1 1 d . . . . .
C15 C 0.6275(5) 0.0961(6) 0.4310(7) 0.073(4) Uani 1 1 d . . . . .
H15A H 0.6580 0.0893 0.3931 0.109 Uiso 1 1 calc GR . . . .
H15B H 0.6285 0.0628 0.4663 0.109 Uiso 1 1 calc GR . . . .
H15C H 0.6361 0.1342 0.4563 0.109 Uiso 1 1 calc GR . . . .
C16 C 0.4886(6) 0.4946(5) 0.1524(6) 0.065(4) Uani 1 1 d . . . . .
H16A H 0.5025 0.5237 0.1157 0.098 Uiso 1 1 calc GR . . . .
H16B H 0.4654 0.5157 0.1902 0.098 Uiso 1 1 calc GR . . . .
H16C H 0.4630 0.4642 0.1289 0.098 Uiso 1 1 calc GR . . . .
C17 C 0.5286(5) 0.4210(5) 0.2420(5) 0.044(3) Uani 1 1 d . . . . .
C18 C 0.5821(5) 0.3998(5) 0.2766(6) 0.052(3) Uani 1 1 d . . . . .
H18 H 0.6208 0.4139 0.2624 0.063 Uiso 1 1 calc R . . . .
C19 C 0.5750(5) 0.3578(5) 0.3321(6) 0.048(3) Uani 1 1 d . . . . .
H19 H 0.6103 0.3415 0.3541 0.058 Uiso 1 1 calc R . . . .
C20 C 0.5171(4) 0.3376(4) 0.3582(5) 0.035(2) Uani 1 1 d . . . . .
C21 C 0.4644(4) 0.3615(4) 0.3231(5) 0.033(2) Uani 1 1 d . . . . .
C22 C 0.4708(4) 0.4050(5) 0.2630(5) 0.038(2) Uani 1 1 d . . . . .
H22 H 0.4364 0.4216 0.2393 0.046 Uiso 1 1 calc R . . . .
C23 C 0.5144(4) 0.2881(4) 0.4101(5) 0.033(2) Uani 1 1 d . . . . .
H23 H 0.5522 0.2716 0.4242 0.039 Uiso 1 1 calc R . . . .
C24 C 0.4798(4) 0.2085(4) 0.4871(5) 0.042(3) Uani 1 1 d . . . . .
H24A H 0.5241 0.2027 0.4893 0.050 Uiso 1 1 calc R . . . .
H24B H 0.4621 0.1723 0.4638 0.050 Uiso 1 1 calc R . . . .
C25 C 0.4549(5) 0.2141(4) 0.5663(5) 0.038(2) Uani 1 1 d . . . . .
C26 C 0.4932(5) 0.2147(5) 0.6274(6) 0.047(3) Uani 1 1 d . . . . .
H26 H 0.5356 0.2147 0.6201 0.057 Uiso 1 1 calc R . . . .
C27 C 0.4704(5) 0.2155(5) 0.6996(5) 0.054(3) Uani 1 1 d . . . . .
H27 H 0.4969 0.2168 0.7404 0.065 Uiso 1 1 calc R . . . .
C28 C 0.4064(6) 0.2141(5) 0.7097(6) 0.050(3) Uani 1 1 d . . . . .
H28 H 0.3900 0.2129 0.7576 0.060 Uiso 1 1 calc R . . . .
C29 C 0.3679(5) 0.2145(4) 0.6487(5) 0.038(3) Uani 1 1 d . . . . .
H29 H 0.3255 0.2145 0.6562 0.046 Uiso 1 1 calc R . . . .
C30 C 0.3904(5) 0.2151(4) 0.5766(5) 0.035(2) Uani 1 1 d . . . . .
C31 C 0.4811(5) 0.0486(6) 0.5782(6) 0.067(4) Uani 1 1 d . . . . .
H31A H 0.4969 0.0077 0.5858 0.100 Uiso 1 1 calc GR . . . .
H31B H 0.5092 0.0780 0.5992 0.100 Uiso 1 1 calc GR . . . .
H31C H 0.4767 0.0562 0.5256 0.100 Uiso 1 1 calc GR . . . .
C32 C 0.4175(6) 0.0389(6) 0.6950(6) 0.066(4) Uani 1 1 d . . . . .
H32A H 0.4419 0.0676 0.7232 0.099 Uiso 1 1 calc GR . . . .
H32B H 0.4329 -0.0022 0.7028 0.099 Uiso 1 1 calc GR . . . .
H32C H 0.3754 0.0411 0.7111 0.099 Uiso 1 1 calc GR . . . .
C33 C 0.3724(5) 0.0726(5) 0.5782(6) 0.050(3) Uani 1 1 d . . . . .
H33 H 0.3354 0.0739 0.6044 0.059 Uiso 1 1 calc R . . . .
C34 C 0.4834(9) 0.1640(8) -0.0908(10) 0.137(6) Uani 1 1 d . U . . .
H34A H 0.4585 0.1291 -0.1037 0.206 Uiso 1 1 calc GR . . . .
H34B H 0.5158 0.1686 -0.1269 0.206 Uiso 1 1 calc GR . . . .
H34C H 0.4584 0.2005 -0.0905 0.206 Uiso 1 1 calc GR . . . .
C35 C 0.5755(8) 0.1401(10) -0.0232(11) 0.151(6) Uani 1 1 d . U . . .
H35A H 0.5964 0.1705 -0.0528 0.227 Uiso 1 1 calc GR . . . .
H35B H 0.5807 0.1002 -0.0457 0.227 Uiso 1 1 calc GR . . . .
H35C H 0.5924 0.1397 0.0263 0.227 Uiso 1 1 calc GR . . . .
C36 C 0.4767(7) 0.1598(7) 0.0399(9) 0.093(3) Uani 1 1 d . U . . .
H36 H 0.5025 0.1545 0.0809 0.112 Uiso 1 1 calc R . . . .
H9 H 0.361(5) 0.301(5) 0.267(6) 0.07(4) Uiso 1 1 d . . . . .
H11 H 0.356(8) 0.201(8) 0.327(9) 0.16(8) Uiso 1 1 d . . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ho1 Ho1 3.6083(6) 3 ?
Ho1 Ho1 3.6083(6) 4 ?
Ho1 O5 2.244(6) 4 ?
Ho1 O6 2.331(6) 4 ?
Ho1 O6 2.415(6) . ?
Ho1 O7 2.357(7) . ?
Ho1 O11 2.333(6) . ?
Ho1 O11 2.281(6) 4 ?
Ho1 O12 2.5556(8) . ?
Ho1 N3 2.545(8) 4 ?
Ho2 O9 2.426(6) 2 ?
Ho2 O9 2.426(6) . ?
Ho2 O9 2.426(6) 4 ?
Ho2 O9 2.426(6) 3 ?
Ho2 O10 2.822(10) . ?
Ho2 O11 2.406(6) . ?
Ho2 O11 2.406(6) 2 ?
Ho2 O11 2.406(6) 3 ?
Ho2 O11 2.406(6) 4 ?
Ho2 O12 2.776(11) . ?
Ho3 Ho3 3.5980(6) 4 ?
Ho3 O2 2.233(6) . ?
Ho3 O3 2.308(6) . ?
Ho3 O3 2.399(6) 4 ?
Ho3 O8 2.361(7) . ?
Ho3 O9 2.289(6) . ?
Ho3 O9 2.324(6) 4 ?
Ho3 O10 2.5510(9) . ?
Ho3 N2 2.555(8) . ?
O1 C12 1.373(11) . ?
O1 C15 1.426(12) . ?
O2 C14 1.312(11) . ?
O3 Ho3 2.399(6) 3 ?
O3 C1 1.362(10) . ?
O4 C16 1.432(13) . ?
O4 C17 1.410(12) . ?
O5 Ho1 2.244(6) 3 ?
O5 C21 1.312(10) . ?
O6 Ho1 2.331(6) 3 ?
O6 C30 1.355(10) . ?
O7 C33 1.256(11) . ?
O8 C36 1.063(14) . ?
O9 Ho3 2.324(6) 3 ?
O9 H9 1.01(11) . ?
O10 Ho3 2.5510(9) 4 ?
O10 Ho3 2.5511(9) 3 ?
O10 Ho3 2.5510(9) 2 ?
O11 Ho1 2.281(6) 3 ?
O11 H11 0.76(16) . ?
O12 Ho1 2.5556(8) 3 ?
O12 Ho1 2.5556(8) 2 ?
O12 Ho1 2.5556(8) 4 ?
N1 C34 1.408(18) . ?
N1 C35 1.474(18) . ?
N1 C36 1.280(16) . ?
N2 C7 1.492(11) . ?
N2 C8 1.288(12) . ?
N3 Ho1 2.545(8) 3 ?
N3 C23 1.302(11) . ?
N3 C24 1.467(11) . ?
N4 C31 1.457(13) . ?
N4 C32 1.482(12) . ?
N4 C33 1.304(12) . ?
C1 C2 1.408(13) . ?
C1 C6 1.399(14) . ?
C2 H2 0.9300 . ?
C2 C3 1.355(13) . ?
C3 H3 0.9300 . ?
C3 C4 1.428(15) . ?
C4 H4 0.9300 . ?
C4 C5 1.362(14) . ?
C5 H5 0.9300 . ?
C5 C6 1.336(13) . ?
C6 C7 1.544(12) . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C8 H8 0.9300 . ?
C8 C9 1.425(14) . ?
C9 C10 1.416(14) . ?
C9 C14 1.432(14) . ?
C10 H10 0.9300 . ?
C10 C11 1.353(14) . ?
C11 H11A 0.9300 . ?
C11 C12 1.353(15) . ?
C12 C13 1.390(14) . ?
C13 H13 0.9300 . ?
C13 C14 1.403(13) . ?
C15 H15A 0.9600 . ?
C15 H15B 0.9600 . ?
C15 H15C 0.9600 . ?
C16 H16A 0.9600 . ?
C16 H16B 0.9600 . ?
C16 H16C 0.9600 . ?
C17 C18 1.393(14) . ?
C17 C22 1.355(13) . ?
C18 H18 0.9300 . ?
C18 C19 1.356(14) . ?
C19 H19 0.9300 . ?
C19 C20 1.411(13) . ?
C20 C21 1.402(13) . ?
C20 C23 1.422(13) . ?
C21 C22 1.439(13) . ?
C22 H22 0.9300 . ?
C23 H23 0.9300 . ?
C24 H24A 0.9700 . ?
C24 H24B 0.9700 . ?
C24 C25 1.521(13) . ?
C25 C26 1.374(13) . ?
C25 C30 1.411(14) . ?
C26 H26 0.9300 . ?
C26 C27 1.383(13) . ?
C27 H27 0.9300 . ?
C27 C28 1.399(15) . ?
C28 H28 0.9300 . ?
C28 C29 1.375(13) . ?
C29 H29 0.9300 . ?
C29 C30 1.379(12) . ?
C31 H31A 0.9600 . ?
C31 H31B 0.9600 . ?
C31 H31C 0.9600 . ?
C32 H32A 0.9600 . ?
C32 H32B 0.9600 . ?
C32 H32C 0.9600 . ?
C33 H33 0.9300 . ?
C34 H34A 0.9600 . ?
C34 H34B 0.9600 . ?
C34 H34C 0.9600 . ?
C35 H35A 0.9600 . ?
C35 H35B 0.9600 . ?
C35 H35C 0.9600 . ?
C36 H36 0.9300 . ?

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
Ho1 Ho1 Ho1 90.0 3 4 ?
O5 Ho1 Ho1 124.59(17) 4 4 ?
O5 Ho1 Ho1 109.88(16) 4 3 ?
O5 Ho1 O6 144.4(2) 4 4 ?
O5 Ho1 O6 125.8(2) 4 . ?
O5 Ho1 O7 84.0(2) 4 . ?
O5 Ho1 O11 86.3(2) 4 4 ?
O5 Ho1 O11 75.4(2) 4 . ?
O5 Ho1 O12 133.1(3) 4 . ?
O5 Ho1 N3 72.1(2) 4 4 ?
O6 Ho1 Ho1 39.65(13) . 3 ?
O6 Ho1 Ho1 41.38(14) 4 4 ?
O6 Ho1 Ho1 102.75(15) . 4 ?
O6 Ho1 Ho1 103.22(15) 4 3 ?
O6 Ho1 O6 88.3(3) 4 . ?
O6 Ho1 O7 99.3(2) 4 . ?
O6 Ho1 O11 130.0(2) 4 . ?
O6 Ho1 O12 65.1(2) . . ?
O6 Ho1 O12 66.2(2) 4 . ?
O6 Ho1 N3 75.1(2) 4 4 ?
O6 Ho1 N3 138.5(2) . 4 ?
O7 Ho1 Ho1 140.61(18) . 4 ?
O7 Ho1 Ho1 106.06(16) . 3 ?
O7 Ho1 O6 72.6(2) . . ?
O7 Ho1 O12 135.1(3) . . ?
O7 Ho1 N3 73.1(2) . 4 ?
O11 Ho1 Ho1 39.08(16) 4 4 ?
O11 Ho1 Ho1 96.67(17) . 4 ?
O11 Ho1 Ho1 96.82(17) 4 3 ?
O11 Ho1 Ho1 38.04(16) . 3 ?
O11 Ho1 O6 74.3(2) . . ?
O11 Ho1 O6 129.3(2) 4 . ?
O11 Ho1 O6 77.0(2) 4 4 ?
O11 Ho1 O7 118.3(2) . . ?
O11 Ho1 O7 157.0(2) 4 . ?
O11 Ho1 O11 79.0(3) 4 . ?
O11 Ho1 O12 64.6(2) 4 . ?
O11 Ho1 O12 63.9(2) . . ?
O11 Ho1 N3 84.1(2) 4 4 ?
O11 Ho1 N3 144.1(2) . 4 ?
O12 Ho1 Ho1 45.093(14) . 3 ?
O12 Ho1 Ho1 45.093(15) . 4 ?
N3 Ho1 Ho1 89.52(18) 4 4 ?
N3 Ho1 Ho1 177.86(16) 4 3 ?
N3 Ho1 O12 134.23(18) 4 . ?
O9 Ho2 O9 75.30(14) 2 3 ?
O9 Ho2 O9 119.5(3) 4 3 ?
O9 Ho2 O9 119.5(3) 2 . ?
O9 Ho2 O9 75.30(14) 3 . ?
O9 Ho2 O9 75.30(14) 2 4 ?
O9 Ho2 O9 75.30(14) 4 . ?
O9 Ho2 O10 59.75(15) . . ?
O9 Ho2 O10 59.75(15) 3 . ?
O9 Ho2 O10 59.75(15) 4 . ?
O9 Ho2 O10 59.75(15) 2 . ?
O9 Ho2 O12 120.25(15) 3 . ?
O9 Ho2 O12 120.25(15) 4 . ?
O9 Ho2 O12 120.25(15) . . ?
O9 Ho2 O12 120.25(15) 2 . ?
O11 Ho2 O9 143.5(2) . 3 ?
O11 Ho2 O9 139.4(2) . 2 ?
O11 Ho2 O9 72.9(2) . 4 ?
O11 Ho2 O9 75.6(2) 3 3 ?
O11 Ho2 O9 72.9(2) 4 2 ?
O11 Ho2 O9 139.4(2) 4 3 ?
O11 Ho2 O9 75.6(2) 4 4 ?
O11 Ho2 O9 72.9(2) 2 3 ?
O11 Ho2 O9 143.5(2) 2 4 ?
O11 Ho2 O9 75.6(2) . . ?
O11 Ho2 O9 75.6(2) 2 2 ?
O11 Ho2 O9 72.9(2) 3 . ?
O11 Ho2 O9 139.4(2) 3 4 ?
O11 Ho2 O9 143.5(2) 4 . ?
O11 Ho2 O9 139.4(2) 2 . ?
O11 Ho2 O9 143.5(2) 3 2 ?
O11 Ho2 O10 120.41(16) 2 . ?
O11 Ho2 O10 120.41(16) 4 . ?
O11 Ho2 O10 120.41(16) . . ?
O11 Ho2 O10 120.41(16) 3 . ?
O11 Ho2 O11 75.15(15) . 3 ?
O11 Ho2 O11 75.15(15) . 4 ?
O11 Ho2 O11 119.2(3) 3 4 ?
O11 Ho2 O11 119.2(3) . 2 ?
O11 Ho2 O11 75.15(15) 3 2 ?
O11 Ho2 O11 75.15(15) 4 2 ?
O11 Ho2 O12 59.59(16) 4 . ?
O11 Ho2 O12 59.59(16) 3 . ?
O11 Ho2 O12 59.59(16) . . ?
O11 Ho2 O12 59.59(16) 2 . ?
O12 Ho2 O10 180.0 . . ?
O2 Ho3 Ho3 109.85(16) . 4 ?
O2 Ho3 O3 124.0(2) . 4 ?
O2 Ho3 O3 144.8(2) . . ?
O2 Ho3 O8 85.1(3) . . ?
O2 Ho3 O9 88.2(2) . . ?
O2 Ho3 O9 75.4(2) . 4 ?
O2 Ho3 O10 135.4(3) . . ?
O2 Ho3 N2 71.9(2) . . ?
O3 Ho3 Ho3 39.22(14) 4 4 ?
O3 Ho3 Ho3 103.50(16) . 4 ?
O3 Ho3 O3 89.3(3) . 4 ?
O3 Ho3 O8 95.7(3) . . ?
O3 Ho3 O9 130.7(2) . 4 ?
O3 Ho3 O10 64.5(2) 4 . ?
O3 Ho3 O10 65.7(2) . . ?
O3 Ho3 N2 74.9(2) . . ?
O3 Ho3 N2 139.4(2) 4 . ?
O8 Ho3 Ho3 107.45(19) . 4 ?
O8 Ho3 O3 72.8(2) . 4 ?
O8 Ho3 O10 132.8(3) . . ?
O8 Ho3 N2 72.0(3) . . ?
O9 Ho3 Ho3 97.45(15) . 4 ?
O9 Ho3 Ho3 38.39(15) 4 4 ?
O9 Ho3 O3 76.3(2) . . ?
O9 Ho3 O3 73.9(2) 4 4 ?
O9 Ho3 O3 129.8(2) . 4 ?
O9 Ho3 O8 155.0(2) . . ?
O9 Ho3 O8 121.1(2) 4 . ?
O9 Ho3 O9 80.0(3) . 4 ?
O9 Ho3 O10 65.3(2) 4 . ?
O9 Ho3 O10 65.8(2) . . ?
O9 Ho3 N2 143.4(2) 4 . ?
O9 Ho3 N2 83.1(2) . . ?
O10 Ho3 Ho3 45.154(17) . 4 ?
O10 Ho3 N2 134.00(19) . . ?
N2 Ho3 Ho3 178.20(16) . 4 ?
C12 O1 C15 118.1(9) . . ?
C14 O2 Ho3 143.9(6) . . ?
Ho3 O3 Ho3 99.7(2) . 3 ?
C1 O3 Ho3 134.9(5) . 3 ?
C1 O3 Ho3 121.3(5) . . ?
C17 O4 C16 116.9(8) . . ?
C21 O5 Ho1 140.4(6) . 3 ?
Ho1 O6 Ho1 99.0(2) 3 . ?
C30 O6 Ho1 136.8(5) . . ?
C30 O6 Ho1 120.4(5) . 3 ?
C33 O7 Ho1 134.7(7) . . ?
C36 O8 Ho3 149.5(11) . . ?
Ho2 O9 H9 93(6) . . ?
Ho3 O9 Ho2 101.9(2) . . ?
Ho3 O9 Ho2 100.9(2) 3 . ?
Ho3 O9 Ho3 102.5(2) . 3 ?
Ho3 O9 H9 114(6) . . ?
Ho3 O9 H9 137(6) 3 . ?
Ho3 O10 Ho2 85.8(2) 4 . ?
Ho3 O10 Ho2 85.8(2) 3 . ?
Ho3 O10 Ho2 85.8(2) 2 . ?
Ho3 O10 Ho2 85.8(2) . . ?
Ho3 O10 Ho3 89.69(3) 3 . ?
Ho3 O10 Ho3 171.6(5) 3 4 ?
Ho3 O10 Ho3 89.69(3) 4 . ?
Ho3 O10 Ho3 89.69(3) 3 2 ?
Ho3 O10 Ho3 89.69(3) 4 2 ?
Ho3 O10 Ho3 171.6(5) . 2 ?
Ho1 O11 Ho1 102.9(2) 3 . ?
Ho1 O11 Ho2 102.8(3) 3 . ?
Ho1 O11 Ho2 101.3(2) . . ?
Ho1 O11 H11 144(10) 3 . ?
Ho1 O11 H11 101(10) . . ?
Ho2 O11 H11 99(10) . . ?
Ho1 O12 Ho1 89.81(3) 4 2 ?
Ho1 O12 Ho1 89.81(3) 3 . ?
Ho1 O12 Ho1 89.81(3) 4 . ?
Ho1 O12 Ho1 173.5(5) . 2 ?
Ho1 O12 Ho1 173.5(5) 4 3 ?
Ho1 O12 Ho1 89.81(3) 3 2 ?
Ho1 O12 Ho2 86.7(2) 4 . ?
Ho1 O12 Ho2 86.7(2) . . ?
Ho1 O12 Ho2 86.7(2) 3 . ?
Ho1 O12 Ho2 86.7(2) 2 . ?
C34 N1 C35 112.1(13) . . ?
C36 N1 C34 121.4(15) . . ?
C36 N1 C35 126.4(16) . . ?
C7 N2 Ho3 117.4(6) . . ?
C8 N2 Ho3 128.1(7) . . ?
C8 N2 C7 114.5(8) . . ?
C23 N3 Ho1 126.8(6) . 3 ?
C23 N3 C24 114.6(8) . . ?
C24 N3 Ho1 118.4(6) . 3 ?
C31 N4 C32 117.6(8) . . ?
C33 N4 C31 121.9(9) . . ?
C33 N4 C32 120.6(9) . . ?
O3 C1 C2 120.5(9) . . ?
O3 C1 C6 122.1(9) . . ?
C6 C1 C2 117.5(8) . . ?
C1 C2 H2 119.7 . . ?
C3 C2 C1 120.6(10) . . ?
C3 C2 H2 119.7 . . ?
C2 C3 H3 119.8 . . ?
C2 C3 C4 120.3(9) . . ?
C4 C3 H3 119.8 . . ?
C3 C4 H4 121.0 . . ?
C5 C4 C3 118.0(9) . . ?
C5 C4 H4 121.0 . . ?
C4 C5 H5 119.0 . . ?
C6 C5 C4 122.0(11) . . ?
C6 C5 H5 119.0 . . ?
C1 C6 C7 115.2(8) . . ?
C5 C6 C1 121.6(9) . . ?
C5 C6 C7 123.1(10) . . ?
N2 C7 C6 113.3(7) . . ?
N2 C7 H7A 108.9 . . ?
N2 C7 H7B 108.9 . . ?
C6 C7 H7A 108.9 . . ?
C6 C7 H7B 108.9 . . ?
H7A C7 H7B 107.7 . . ?
N2 C8 H8 115.7 . . ?
N2 C8 C9 128.6(10) . . ?
C9 C8 H8 115.7 . . ?
C8 C9 C14 123.5(10) . . ?
C10 C9 C8 117.8(10) . . ?
C10 C9 C14 118.0(9) . . ?
C9 C10 H10 119.2 . . ?
C11 C10 C9 121.6(10) . . ?
C11 C10 H10 119.2 . . ?
C10 C11 H11A 119.6 . . ?
C12 C11 C10 120.9(11) . . ?
C12 C11 H11A 119.6 . . ?
O1 C12 C13 113.3(10) . . ?
C11 C12 O1 126.4(10) . . ?
C11 C12 C13 120.3(10) . . ?
C12 C13 H13 119.4 . . ?
C12 C13 C14 121.2(10) . . ?
C14 C13 H13 119.4 . . ?
O2 C14 C9 120.8(9) . . ?
O2 C14 C13 121.4(9) . . ?
C13 C14 C9 117.8(9) . . ?
O1 C15 H15A 109.5 . . ?
O1 C15 H15B 109.5 . . ?
O1 C15 H15C 109.5 . . ?
H15A C15 H15B 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
O4 C16 H16A 109.5 . . ?
O4 C16 H16B 109.5 . . ?
O4 C16 H16C 109.5 . . ?
H16A C16 H16B 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C18 C17 O4 112.6(9) . . ?
C22 C17 O4 123.0(10) . . ?
C22 C17 C18 124.2(10) . . ?
C17 C18 H18 121.5 . . ?
C19 C18 C17 117.0(10) . . ?
C19 C18 H18 121.5 . . ?
C18 C19 H19 118.3 . . ?
C18 C19 C20 123.4(10) . . ?
C20 C19 H19 118.3 . . ?
C19 C20 C23 119.2(9) . . ?
C21 C20 C19 117.6(9) . . ?
C21 C20 C23 122.5(9) . . ?
O5 C21 C20 123.5(8) . . ?
O5 C21 C22 116.6(8) . . ?
C20 C21 C22 119.9(8) . . ?
C17 C22 C21 117.7(9) . . ?
C17 C22 H22 121.2 . . ?
C21 C22 H22 121.2 . . ?
N3 C23 C20 128.9(9) . . ?
N3 C23 H23 115.5 . . ?
C20 C23 H23 115.5 . . ?
N3 C24 H24A 109.0 . . ?
N3 C24 H24B 109.0 . . ?
N3 C24 C25 113.1(8) . . ?
H24A C24 H24B 107.8 . . ?
C25 C24 H24A 109.0 . . ?
C25 C24 H24B 109.0 . . ?
C26 C25 C24 121.9(10) . . ?
C26 C25 C30 119.7(9) . . ?
C30 C25 C24 118.4(9) . . ?
C25 C26 H26 119.1 . . ?
C25 C26 C27 121.8(11) . . ?
C27 C26 H26 119.1 . . ?
C26 C27 H27 120.8 . . ?
C26 C27 C28 118.3(9) . . ?
C28 C27 H27 120.8 . . ?
C27 C28 H28 120.0 . . ?
C29 C28 C27 120.0(10) . . ?
C29 C28 H28 120.0 . . ?
C28 C29 H29 119.1 . . ?
C28 C29 C30 121.8(10) . . ?
C30 C29 H29 119.1 . . ?
O6 C30 C25 119.6(8) . . ?
O6 C30 C29 122.0(10) . . ?
C29 C30 C25 118.3(9) . . ?
N4 C31 H31A 109.5 . . ?
N4 C31 H31B 109.5 . . ?
N4 C31 H31C 109.5 . . ?
H31A C31 H31B 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
N4 C32 H32A 109.5 . . ?
N4 C32 H32B 109.5 . . ?
N4 C32 H32C 109.5 . . ?
H32A C32 H32B 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
O7 C33 N4 125.3(11) . . ?
O7 C33 H33 117.3 . . ?
N4 C33 H33 117.3 . . ?
N1 C34 H34A 109.5 . . ?
N1 C34 H34B 109.5 . . ?
N1 C34 H34C 109.5 . . ?
H34A C34 H34B 109.5 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 109.5 . . ?
N1 C35 H35A 109.5 . . ?
N1 C35 H35B 109.5 . . ?
N1 C35 H35C 109.5 . . ?
H35A C35 H35B 109.5 . . ?
H35A C35 H35C 109.5 . . ?
H35B C35 H35C 109.5 . . ?
O8 C36 N1 143.7(19) . . ?
O8 C36 H36 108.2 . . ?
N1 C36 H36 108.2 . . ?

_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_t2_sq_s
_database_code_depnum_ccdc_archive 'CCDC 1923033'
loop_
_audit_author_name
_audit_author_address
'Yuan Huang'
;Soochow university
China
;
_audit_update_record             
;
2019-11-06 deposited with the CCDC.	2019-11-13 downloaded from the CCDC.
;
_audit_creation_date             2019-11-06
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2014/7
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C144 H168 Dy9 N16 O42, H3 O, 6(H2O)'
_chemical_formula_sum            'C144 H183 Dy9 N16 O49'
_chemical_formula_weight         4395.59
_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'
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'

_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           85
_space_group_name_H-M_alt        'P 4/n'
_space_group_name_Hall           '-P 4a'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y+1/2, z'
'-y+1/2, x, z'
'y, -x+1/2, z'
'-x, -y, -z'
'x-1/2, y-1/2, -z'
'y-1/2, -x, -z'
'-y, x-1/2, -z'

_cell_length_a                   21.5445(3)
_cell_length_b                   21.5445(3)
_cell_length_c                   17.8651(6)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     8292.4(4)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    9755
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      27.49
_cell_measurement_theta_min      2.28
_shelx_estimated_absorpt_T_max   0.496
_shelx_estimated_absorpt_T_min   0.496
_exptl_absorpt_coefficient_mu    4.077
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.3445
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.2349 before and 0.0621 after correction.
The Ratio of minimum to maximum transmission is 0.4620.
The λ/2 correction factor is Not present.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_lustre     ?
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.705
_exptl_crystal_density_meas      .
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             4148
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0541
_diffrn_reflns_av_unetI/netI     0.0514
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            25516
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.677
_diffrn_reflns_theta_min         2.402
_diffrn_ambient_temperature      296.15
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_diffrn_special_details          ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                6416
_reflns_number_total             7851
_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 v8.37A (Bruker, 2015)'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_refine_diff_density_max         2.453
_refine_diff_density_min         -1.559
_refine_diff_density_rms         0.187
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.096
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     492
_refine_ls_number_reflns         7851
_refine_ls_number_restraints     26
_refine_ls_R_factor_all          0.0614
_refine_ls_R_factor_gt           0.0471
_refine_ls_restrained_S_all      1.097
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0001P)²+131.9418P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1056
_refine_ls_wR_factor_ref         0.1133
_refine_special_details          
;
The SQUEEZE routine of PLATON was used in the treatment of the crystallographic data. The identities and numbers of the lattice solvents were determined by the TGA and elemental analysis. The calculated mass loss corresponding to the solvent guests from the crystals between 29 and 90?ãC was 2.89%. However, the experimental result 2.88% was consistent with calculated result. This indicates that six water molecules and one hydronium ion might be lost during the test process and elemental analysis results of C 39.45, H 4.21, N 5.11, which are consistent with the experimental data.
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 O3-H3
 0.86 with sigma of 0.005
 O1-H1
 0.86 with sigma of 0.005
3. Rigid bond restraints
 C36, N4, C35, C34
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
4. Uiso/Uaniso restraints and constraints
Uanis(C34) \\sim Ueq, Uanis(C36) \\sim Ueq, Uanis(C35) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
5.a Secondary CH2 refined with riding coordinates:
 C17(H17A,H17B), C21(H21A,H21B)
5.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3A), C8(H8), C10(H10), C11(H11), C13(H13), C18(H18), C19(H19),
 C20(H20), C22(H22), C23(H23), C24(H24), C25(H25), C26(H26), C27(H27), C30(H30),
  C32(H32), C34(H34)
5.c Idealised Me refined as rotating group:
 C28(H28A,H28B,H28C), C29(H29A,H29B,H29C), C31(H31A,H31B,H31C), C33(H33A,H33B,
 H33C), C35(H35A,H35B,H35C), C36(H36A,H36B,H36C)
;
_atom_sites_solution_hydrogens   mixed
_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
Dy1 Dy 0.7500 0.7500 0.71335(4) 0.01623(16) Uani 1 4 d S T P . .
Dy2 Dy 0.85686(2) 0.69769(2) 0.56586(2) 0.01823(10) Uani 1 1 d . . . . .
Dy3 Dy 0.78222(2) 0.63586(2) 0.86134(2) 0.01837(10) Uani 1 1 d . . . . .
O1 O 0.8422(2) 0.7805(2) 0.6451(3) 0.0176(11) Uani 1 1 d D . . . .
H3 H 0.854(3) 0.677(3) 0.754(4) 0.02(2) Uiso 1 1 d D . . . .
O2 O 0.7500 0.7500 0.5563(6) 0.019(2) Uani 1 4 d S T P . .
O3 O 0.8352(2) 0.7037(2) 0.7818(3) 0.0180(11) Uani 1 1 d D . . . .
H1 H 0.866(3) 0.803(3) 0.672(4) 0.01(2) Uiso 1 1 d D . . . .
O4 O 0.7500 0.7500 0.8711(6) 0.021(2) Uani 1 4 d S T P . .
O5 O 0.8543(3) 0.7832(3) 0.4849(3) 0.0221(12) Uani 1 1 d . . . . .
O6 O 0.9101(3) 0.6539(3) 0.6599(3) 0.0250(13) Uani 1 1 d . . . . .
O7 O 0.6984(3) 0.6538(3) 0.9421(3) 0.0231(12) Uani 1 1 d . . . . .
O8 O 0.8178(3) 0.5750(3) 0.7687(3) 0.0272(13) Uani 1 1 d . . . . .
O9 O 0.8378(3) 0.5675(3) 0.9417(4) 0.0415(17) Uani 1 1 d . . . . .
O10 O 0.9135(3) 0.6265(3) 0.4905(4) 0.0367(16) Uani 1 1 d . . . . .
O11 O 1.0431(3) 0.5356(3) 0.8187(4) 0.0414(17) Uani 1 1 d . . . . .
O12 O 0.9033(3) 0.4327(3) 0.6011(4) 0.0408(17) Uani 1 1 d . . . . .
N1 N 0.9694(3) 0.7366(3) 0.5599(4) 0.0229(15) Uani 1 1 d . . . . .
N2 N 0.7225(3) 0.5327(3) 0.8653(4) 0.0240(15) Uani 1 1 d . . . . .
N3 N 0.9450(4) 0.5762(4) 0.3860(4) 0.0323(17) Uani 1 1 d . . . . .
N4 N 0.8432(5) 0.4873(5) 1.0211(6) 0.054(2) Uani 1 1 d . U . . .
C1 C 0.8925(4) 0.7842(4) 0.4249(4) 0.0238(18) Uani 1 1 d . . . . .
C2 C 0.8597(4) 0.5015(4) 0.6863(5) 0.0267(19) Uani 1 1 d . . . . .
H2 H 0.8836 0.5323 0.6639 0.032 Uiso 1 1 calc R . . . .
C3 C 1.0180(4) 0.7113(4) 0.5913(5) 0.0247(18) Uani 1 1 d . . . . .
H3A H 1.0562 0.7270 0.5764 0.030 Uiso 1 1 calc R . . . .
C4 C 0.9561(4) 0.7855(4) 0.4341(5) 0.0245(18) Uani 1 1 d . . . . .
C5 C 0.6877(4) 0.6166(4) 1.0008(4) 0.0243(18) Uani 1 1 d . . . . .
C6 C 0.9660(4) 0.6383(4) 0.6796(5) 0.0254(18) Uani 1 1 d . . . . .
C7 C 1.0199(4) 0.6634(4) 0.6448(5) 0.0258(18) Uani 1 1 d . . . . .
C8 C 0.9740(4) 0.5956(4) 0.7389(5) 0.0274(19) Uani 1 1 d . . . . .
H8 H 0.9393 0.5794 0.7630 0.033 Uiso 1 1 calc R . . . .
C9 C 0.8202(4) 0.5173(4) 0.7459(5) 0.0248(18) Uani 1 1 d . . . . .
C10 C 0.6896(4) 0.6393(4) 1.0742(5) 0.0289(19) Uani 1 1 d . . . . .
H10 H 0.6980 0.6811 1.0827 0.035 Uiso 1 1 calc R . . . .
C11 C 0.8682(5) 0.7851(4) 0.3523(5) 0.031(2) Uani 1 1 d . . . . .
H11 H 0.8255 0.7864 0.3451 0.037 Uiso 1 1 calc R . . . .
C12 C 0.7831(4) 0.4702(4) 0.7773(5) 0.0279(19) Uani 1 1 d . . . . .
C13 C 0.7352(4) 0.4808(4) 0.8314(5) 0.0280(19) Uani 1 1 d . . . . .
H13 H 0.7105 0.4469 0.8435 0.034 Uiso 1 1 calc R . . . .
C14 C 1.0323(4) 0.5775(4) 0.7615(5) 0.030(2) Uani 1 1 d . . . . .
C15 C 0.8640(4) 0.4406(4) 0.6598(5) 0.029(2) Uani 1 1 d . . . . .
C16 C 0.6727(4) 0.5538(4) 0.9893(5) 0.0270(19) Uani 1 1 d . . . . .
C17 C 0.9822(4) 0.7915(4) 0.5129(5) 0.0286(19) Uani 1 1 d . . . . .
H17A H 1.0268 0.7976 0.5099 0.034 Uiso 1 1 calc R . . . .
H17B H 0.9645 0.8279 0.5366 0.034 Uiso 1 1 calc R . . . .
C18 C 0.9269(4) 0.6253(4) 0.4232(5) 0.031(2) Uani 1 1 d . . . . .
H18 H 0.9237 0.6624 0.3969 0.037 Uiso 1 1 calc R . . . .
C19 C 0.9075(6) 0.7841(4) 0.2910(5) 0.040(3) Uani 1 1 d . . . . .
H19 H 0.8911 0.7837 0.2429 0.048 Uiso 1 1 calc R . . . .
C20 C 0.6792(5) 0.6000(5) 1.1339(5) 0.037(2) Uani 1 1 d . . . . .
H20 H 0.6810 0.6154 1.1825 0.045 Uiso 1 1 calc R . . . .
C21 C 0.6644(4) 0.5316(4) 0.9102(5) 0.029(2) Uani 1 1 d . . . . .
H21A H 0.6485 0.4895 0.9113 0.035 Uiso 1 1 calc R . . . .
H21B H 0.6337 0.5574 0.8857 0.035 Uiso 1 1 calc R . . . .
C22 C 0.9951(5) 0.7842(5) 0.3727(5) 0.036(2) Uani 1 1 d . . . . .
H22 H 1.0379 0.7836 0.3798 0.043 Uiso 1 1 calc R . . . .
C23 C 1.0848(4) 0.6005(5) 0.7267(6) 0.037(2) Uani 1 1 d . . . . .
H23 H 1.1240 0.5872 0.7411 0.044 Uiso 1 1 calc R . . . .
C24 C 0.7890(5) 0.4097(5) 0.7482(7) 0.046(3) Uani 1 1 d . . . . .
H24 H 0.7640 0.3787 0.7683 0.055 Uiso 1 1 calc R . . . .
C25 C 1.0778(5) 0.6436(4) 0.6703(6) 0.035(2) Uani 1 1 d . . . . .
H25 H 1.1133 0.6602 0.6483 0.042 Uiso 1 1 calc R . . . .
C26 C 0.6632(4) 0.5159(5) 1.0503(5) 0.037(2) Uani 1 1 d . . . . .
H26 H 0.6545 0.4741 1.0426 0.045 Uiso 1 1 calc R . . . .
C27 C 0.8293(5) 0.3938(5) 0.6924(7) 0.047(3) Uani 1 1 d . . . . .
H27 H 0.8333 0.3528 0.6768 0.057 Uiso 1 1 calc R . . . .
C28 C 0.9483(5) 0.5155(5) 0.4203(6) 0.039(2) Uani 1 1 d . . . . .
H28A H 0.9904 0.5010 0.4194 0.059 Uiso 1 1 calc GR . . . .
H28B H 0.9224 0.4871 0.3931 0.059 Uiso 1 1 calc GR . . . .
H28C H 0.9342 0.5181 0.4712 0.059 Uiso 1 1 calc GR . . . .
C29 C 0.9602(6) 0.5809(6) 0.3064(6) 0.050(3) Uani 1 1 d . . . . .
H29A H 0.9299 0.5586 0.2776 0.075 Uiso 1 1 calc GR . . . .
H29B H 1.0006 0.5634 0.2977 0.075 Uiso 1 1 calc GR . . . .
H29C H 0.9602 0.6237 0.2916 0.075 Uiso 1 1 calc GR . . . .
C30 C 0.9714(5) 0.7836(5) 0.3012(6) 0.043(3) Uani 1 1 d . . . . .
H30 H 0.9979 0.7830 0.2601 0.052 Uiso 1 1 calc R . . . .
C31 C 0.9921(5) 0.5054(5) 0.8518(6) 0.044(3) Uani 1 1 d . . . . .
H31A H 0.9659 0.4885 0.8134 0.067 Uiso 1 1 calc GR . . . .
H31B H 0.9689 0.5345 0.8812 0.067 Uiso 1 1 calc GR . . . .
H31C H 1.0067 0.4724 0.8834 0.067 Uiso 1 1 calc GR . . . .
C32 C 0.6661(5) 0.5383(5) 1.1220(5) 0.041(2) Uani 1 1 d . . . . .
H32 H 0.6593 0.5119 1.1624 0.049 Uiso 1 1 calc R . . . .
C33 C 0.9080(6) 0.3719(6) 0.5676(7) 0.057(3) Uani 1 1 d . . . . .
H33A H 0.9369 0.3732 0.5268 0.085 Uiso 1 1 calc GR . . . .
H33B H 0.8680 0.3594 0.5493 0.085 Uiso 1 1 calc GR . . . .
H33C H 0.9221 0.3427 0.6044 0.085 Uiso 1 1 calc GR . . . .
C34 C 0.8441(7) 0.5145(7) 0.9571(9) 0.074(4) Uani 1 1 d . U . . .
H34 H 0.8508 0.4883 0.9165 0.088 Uiso 1 1 calc R . . . .
C35 C 0.8333(9) 0.5226(9) 1.0873(10) 0.099(5) Uani 1 1 d . U . . .
H35A H 0.8714 0.5255 1.1149 0.148 Uiso 1 1 calc GR . . . .
H35B H 0.8023 0.5028 1.1175 0.148 Uiso 1 1 calc GR . . . .
H35C H 0.8195 0.5636 1.0740 0.148 Uiso 1 1 calc GR . . . .
C36 C 0.8514(11) 0.4218(8) 1.0279(14) 0.130(7) Uani 1 1 d . U . . .
H36A H 0.8135 0.4033 1.0454 0.196 Uiso 1 1 calc GR . . . .
H36B H 0.8841 0.4133 1.0629 0.196 Uiso 1 1 calc GR . . . .
H36C H 0.8620 0.4047 0.9800 0.196 Uiso 1 1 calc GR . . . .


_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 Dy2 3.6759(6) 4_565 ?
Dy1 Dy2 3.6759(6) 2_665 ?
Dy1 O1 2.421(5) . ?
Dy1 O1 2.421(5) 2_665 ?
Dy1 O1 2.421(5) 4_565 ?
Dy1 O1 2.421(5) 3_655 ?
Dy1 O2 2.806(11) . ?
Dy1 O3 2.421(5) 3_655 ?
Dy1 O3 2.421(5) 2_665 ?
Dy1 O3 2.421(5) . ?
Dy1 O3 2.421(5) 4_565 ?
Dy1 O4 2.818(11) . ?
Dy2 Dy2 3.6250(5) 4_565 ?
Dy2 Dy2 3.6250(5) 3_655 ?
Dy2 O1 2.335(5) 4_565 ?
Dy2 O1 2.300(5) . ?
Dy2 O2 2.5690(8) . ?
Dy2 O5 2.423(5) 4_565 ?
Dy2 O5 2.343(5) . ?
Dy2 O6 2.243(6) . ?
Dy2 O10 2.379(6) . ?
Dy2 N1 2.567(7) . ?
Dy3 Dy3 3.6135(5) 3_655 ?
Dy3 Dy3 3.6136(5) 4_565 ?
Dy3 O3 2.336(5) . ?
Dy3 O3 2.296(5) 4_565 ?
Dy3 O4 2.5611(8) . ?
Dy3 O7 2.408(6) 3_655 ?
Dy3 O7 2.343(5) . ?
Dy3 O8 2.246(6) . ?
Dy3 O9 2.380(6) . ?
Dy3 N2 2.570(7) . ?
O1 Dy2 2.335(5) 3_655 ?
O2 Dy2 2.5690(8) 2_665 ?
O2 Dy2 2.5690(8) 3_655 ?
O2 Dy2 2.5690(8) 4_565 ?
O3 Dy3 2.296(5) 3_655 ?
O4 Dy3 2.5611(8) 3_655 ?
O4 Dy3 2.5611(8) 4_565 ?
O4 Dy3 2.5611(8) 2_665 ?
O5 Dy2 2.423(5) 3_655 ?
O5 C1 1.350(10) . ?
O6 C6 1.297(10) . ?
O7 Dy3 2.408(5) 4_565 ?
O7 C5 1.341(10) . ?
O8 C9 1.308(10) . ?
O9 C34 1.184(16) . ?
O10 C18 1.235(11) . ?
O11 C14 1.385(11) . ?
O11 C31 1.408(13) . ?
O12 C15 1.359(11) . ?
O12 C33 1.443(12) . ?
N1 C3 1.306(11) . ?
N1 C17 1.477(10) . ?
N2 C13 1.300(11) . ?
N2 C21 1.487(11) . ?
N3 C18 1.310(11) . ?
N3 C28 1.446(12) . ?
N3 C29 1.464(12) . ?
N4 C34 1.285(16) . ?
N4 C35 1.422(18) . ?
N4 C36 1.427(18) . ?
C1 C4 1.381(12) . ?
C1 C11 1.399(12) . ?
C2 C9 1.405(12) . ?
C2 C15 1.400(12) . ?
C3 C7 1.407(12) . ?
C4 C17 1.521(12) . ?
C4 C22 1.383(12) . ?
C5 C10 1.399(12) . ?
C5 C16 1.405(12) . ?
C6 C7 1.423(12) . ?
C6 C8 1.415(12) . ?
C7 C25 1.397(13) . ?
C8 C14 1.374(12) . ?
C9 C12 1.409(12) . ?
C10 C20 1.380(13) . ?
C11 C19 1.383(13) . ?
C12 C13 1.432(12) . ?
C12 C24 1.408(13) . ?
C14 C23 1.382(14) . ?
C15 C27 1.383(14) . ?
C16 C21 1.502(12) . ?
C16 C26 1.377(13) . ?
C19 C30 1.389(16) . ?
C20 C32 1.376(15) . ?
C22 C30 1.376(14) . ?
C23 C25 1.378(14) . ?
C24 C27 1.367(16) . ?
C26 C32 1.371(14) . ?

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
Dy2 Dy1 Dy2 59.084(11) 4_565 2_665 ?
O1 Dy1 Dy2 94.01(13) . 2_665 ?
O1 Dy1 Dy2 38.54(13) 3_655 2_665 ?
O1 Dy1 Dy2 38.54(12) 2_665 4_565 ?
O1 Dy1 Dy2 93.48(12) 4_565 2_665 ?
O1 Dy1 Dy2 93.48(12) . 4_565 ?
O1 Dy1 Dy2 37.69(12) 4_565 4_565 ?
O1 Dy1 Dy2 37.69(12) 2_665 2_665 ?
O1 Dy1 Dy2 94.01(13) 3_655 4_565 ?
O1 Dy1 O1 75.33(11) 2_665 4_565 ?
O1 Dy1 O1 75.33(11) . 4_565 ?
O1 Dy1 O1 119.6(2) . 2_665 ?
O1 Dy1 O1 75.33(11) . 3_655 ?
O1 Dy1 O1 119.6(2) 4_565 3_655 ?
O1 Dy1 O1 75.33(11) 2_665 3_655 ?
O1 Dy1 O2 59.78(12) 2_665 . ?
O1 Dy1 O2 59.78(12) . . ?
O1 Dy1 O2 59.78(12) 4_565 . ?
O1 Dy1 O2 59.78(12) 3_655 . ?
O1 Dy1 O3 142.95(18) 2_665 3_655 ?
O1 Dy1 O3 139.86(17) 4_565 3_655 ?
O1 Dy1 O3 73.17(17) . 3_655 ?
O1 Dy1 O3 73.16(17) 3_655 2_665 ?
O1 Dy1 O3 142.95(18) 4_565 2_665 ?
O1 Dy1 O3 75.17(18) . . ?
O1 Dy1 O3 139.86(17) 2_665 . ?
O1 Dy1 O3 75.17(18) 3_655 3_655 ?
O1 Dy1 O3 139.86(17) . 2_665 ?
O1 Dy1 O3 142.95(18) . 4_565 ?
O1 Dy1 O3 73.16(17) 4_565 . ?
O1 Dy1 O3 73.16(17) 2_665 4_565 ?
O1 Dy1 O3 142.95(18) 3_655 . ?
O1 Dy1 O3 75.17(18) 4_565 4_565 ?
O1 Dy1 O3 139.86(18) 3_655 4_565 ?
O1 Dy1 O3 75.17(18) 2_665 2_665 ?
O1 Dy1 O4 120.22(12) . . ?
O1 Dy1 O4 120.22(12) 3_655 . ?
O1 Dy1 O4 120.22(12) 2_665 . ?
O1 Dy1 O4 120.22(12) 4_565 . ?
O2 Dy1 Dy2 44.211(10) . 4_565 ?
O2 Dy1 Dy2 44.211(9) . 2_665 ?
O2 Dy1 O4 180.0 . . ?
O3 Dy1 Dy2 76.17(12) 4_565 4_565 ?
O3 Dy1 Dy2 109.66(12) 4_565 2_665 ?
O3 Dy1 Dy2 112.82(12) 3_655 2_665 ?
O3 Dy1 Dy2 112.82(12) 2_665 4_565 ?
O3 Dy1 Dy2 76.17(12) 2_665 2_665 ?
O3 Dy1 Dy2 109.66(12) . 4_565 ?
O3 Dy1 Dy2 164.44(12) 3_655 4_565 ?
O3 Dy1 Dy2 164.44(12) . 2_665 ?
O3 Dy1 O2 120.34(12) 2_665 . ?
O3 Dy1 O2 120.34(12) 3_655 . ?
O3 Dy1 O2 120.34(12) . . ?
O3 Dy1 O2 120.34(12) 4_565 . ?
O3 Dy1 O3 75.21(11) . 4_565 ?
O3 Dy1 O3 75.21(11) . 3_655 ?
O3 Dy1 O3 75.21(11) 4_565 2_665 ?
O3 Dy1 O3 119.3(2) 3_655 4_565 ?
O3 Dy1 O3 75.21(11) 3_655 2_665 ?
O3 Dy1 O3 119.3(2) . 2_665 ?
O3 Dy1 O4 59.66(12) 4_565 . ?
O3 Dy1 O4 59.66(12) . . ?
O3 Dy1 O4 59.66(12) 2_665 . ?
O3 Dy1 O4 59.66(12) 3_655 . ?
O4 Dy1 Dy2 135.789(9) . 2_665 ?
O4 Dy1 Dy2 135.789(10) . 4_565 ?
Dy2 Dy2 Dy1 60.457(6) 4_565 . ?
Dy2 Dy2 Dy1 60.457(6) 3_655 . ?
Dy2 Dy2 Dy2 89.998(1) 4_565 3_655 ?
O1 Dy2 Dy1 40.07(13) . . ?
O1 Dy2 Dy1 40.25(13) 4_565 . ?
O1 Dy2 Dy2 38.19(12) 4_565 4_565 ?
O1 Dy2 Dy2 96.99(13) . 4_565 ?
O1 Dy2 Dy2 38.89(13) . 3_655 ?
O1 Dy2 Dy2 96.88(13) 4_565 3_655 ?
O1 Dy2 O1 79.4(2) . 4_565 ?
O1 Dy2 O2 65.0(2) . . ?
O1 Dy2 O2 64.6(2) 4_565 . ?
O1 Dy2 O5 129.54(19) . 4_565 ?
O1 Dy2 O5 74.35(18) 4_565 4_565 ?
O1 Dy2 O5 76.55(19) . . ?
O1 Dy2 O5 130.37(19) 4_565 . ?
O1 Dy2 O10 117.9(2) 4_565 . ?
O1 Dy2 O10 156.9(2) . . ?
O1 Dy2 N1 84.4(2) . . ?
O1 Dy2 N1 144.2(2) 4_565 . ?
O2 Dy2 Dy1 49.6(2) . . ?
O2 Dy2 Dy2 45.127(17) . 4_565 ?
O2 Dy2 Dy2 45.126(17) . 3_655 ?
O5 Dy2 Dy1 99.17(13) 4_565 . ?
O5 Dy2 Dy1 100.79(13) . . ?
O5 Dy2 Dy2 103.46(14) . 4_565 ?
O5 Dy2 Dy2 103.01(13) 4_565 3_655 ?
O5 Dy2 Dy2 41.31(13) . 3_655 ?
O5 Dy2 Dy2 39.66(13) 4_565 4_565 ?
O5 Dy2 O2 66.0(2) . . ?
O5 Dy2 O2 64.9(2) 4_565 . ?
O5 Dy2 O5 88.8(3) . 4_565 ?
O5 Dy2 O10 99.7(2) . . ?
O5 Dy2 N1 74.9(2) . . ?
O5 Dy2 N1 138.2(2) 4_565 . ?
O6 Dy2 Dy1 85.00(14) . . ?
O6 Dy2 Dy2 110.35(15) . 4_565 ?
O6 Dy2 Dy2 124.35(15) . 3_655 ?
O6 Dy2 O1 75.61(19) . 4_565 ?
O6 Dy2 O1 86.3(2) . . ?
O6 Dy2 O2 133.9(3) . . ?
O6 Dy2 O5 143.7(2) . . ?
O6 Dy2 O5 126.0(2) . 4_565 ?
O6 Dy2 O10 83.7(2) . . ?
O6 Dy2 N1 71.6(2) . . ?
O10 Dy2 Dy1 157.67(17) . . ?
O10 Dy2 Dy2 106.05(16) . 4_565 ?
O10 Dy2 Dy2 140.95(17) . 3_655 ?
O10 Dy2 O2 134.8(3) . . ?
O10 Dy2 O5 72.5(2) . 4_565 ?
O10 Dy2 N1 72.7(2) . . ?
N1 Dy2 Dy1 121.41(15) . . ?
N1 Dy2 Dy2 177.62(15) . 4_565 ?
N1 Dy2 Dy2 89.86(15) . 3_655 ?
N1 Dy2 O2 134.46(15) . . ?
Dy3 Dy3 Dy1 60.569(6) 3_655 . ?
Dy3 Dy3 Dy1 60.569(6) 4_565 . ?
Dy3 Dy3 Dy3 90.0 3_655 4_565 ?
O3 Dy3 Dy1 40.24(13) . . ?
O3 Dy3 Dy1 40.03(14) 4_565 . ?
O3 Dy3 Dy3 96.95(13) . 4_565 ?
O3 Dy3 Dy3 38.32(12) . 3_655 ?
O3 Dy3 Dy3 39.12(13) 4_565 4_565 ?
O3 Dy3 Dy3 97.08(13) 4_565 3_655 ?
O3 Dy3 O3 79.3(3) 4_565 . ?
O3 Dy3 O4 64.7(2) . . ?
O3 Dy3 O4 65.3(2) 4_565 . ?
O3 Dy3 O7 74.61(18) . 3_655 ?
O3 Dy3 O7 129.86(19) 4_565 3_655 ?
O3 Dy3 O7 76.60(19) 4_565 . ?
O3 Dy3 O7 130.38(19) . . ?
O3 Dy3 O9 155.8(2) 4_565 . ?
O3 Dy3 O9 120.5(2) . . ?
O3 Dy3 N2 83.3(2) 4_565 . ?
O3 Dy3 N2 143.4(2) . . ?
O4 Dy3 Dy1 49.9(2) . . ?
O4 Dy3 Dy3 45.133(18) . 4_565 ?
O4 Dy3 Dy3 45.134(18) . 3_655 ?
O4 Dy3 N2 133.89(16) . . ?
O7 Dy3 Dy1 100.77(13) . . ?
O7 Dy3 Dy1 99.48(13) 3_655 . ?
O7 Dy3 Dy3 103.44(14) . 3_655 ?
O7 Dy3 Dy3 41.15(13) . 4_565 ?
O7 Dy3 Dy3 39.83(13) 3_655 3_655 ?
O7 Dy3 Dy3 103.07(14) 3_655 4_565 ?
O7 Dy3 O4 65.8(2) . . ?
O7 Dy3 O4 65.0(2) 3_655 . ?
O7 Dy3 O7 88.8(3) . 3_655 ?
O7 Dy3 O9 96.8(2) . . ?
O7 Dy3 N2 74.9(2) . . ?
O7 Dy3 N2 139.0(2) 3_655 . ?
O8 Dy3 Dy1 85.73(15) . . ?
O8 Dy3 Dy3 125.68(16) . 4_565 ?
O8 Dy3 Dy3 110.04(15) . 3_655 ?
O8 Dy3 O3 87.4(2) . 4_565 ?
O8 Dy3 O3 75.55(19) . . ?
O8 Dy3 O4 134.7(3) . . ?
O8 Dy3 O7 144.4(2) . . ?
O8 Dy3 O7 124.9(2) . 3_655 ?
O8 Dy3 O9 84.9(2) . . ?
O8 Dy3 N2 71.7(2) . . ?
O9 Dy3 Dy1 160.49(18) . . ?
O9 Dy3 Dy3 137.84(19) . 4_565 ?
O9 Dy3 Dy3 107.10(17) . 3_655 ?
O9 Dy3 O4 133.6(3) . . ?
O9 Dy3 O7 72.3(2) . 3_655 ?
O9 Dy3 N2 72.5(2) . . ?
N2 Dy3 Dy1 120.27(15) . . ?
N2 Dy3 Dy3 178.22(15) . 3_655 ?
N2 Dy3 Dy3 89.19(16) . 4_565 ?
Dy2 O1 Dy1 101.2(2) 3_655 . ?
Dy2 O1 Dy1 102.2(2) . . ?
Dy2 O1 Dy2 102.9(2) . 3_655 ?
Dy2 O2 Dy1 86.2(2) . . ?
Dy2 O2 Dy1 86.2(2) 3_655 . ?
Dy2 O2 Dy1 86.2(2) 2_665 . ?
Dy2 O2 Dy1 86.2(2) 4_565 . ?
Dy2 O2 Dy2 172.3(5) 2_665 . ?
Dy2 O2 Dy2 89.75(3) 3_655 . ?
Dy2 O2 Dy2 89.74(3) 4_565 . ?
Dy2 O2 Dy2 172.3(5) 3_655 4_565 ?
Dy2 O2 Dy2 89.74(3) 3_655 2_665 ?
Dy2 O2 Dy2 89.74(3) 4_565 2_665 ?
Dy3 O3 Dy1 101.2(2) . . ?
Dy3 O3 Dy1 102.4(2) 3_655 . ?
Dy3 O3 Dy3 102.6(2) 3_655 . ?
Dy3 O4 Dy1 86.1(2) 4_565 . ?
Dy3 O4 Dy1 86.1(2) 3_655 . ?
Dy3 O4 Dy1 86.1(2) . . ?
Dy3 O4 Dy1 86.1(2) 2_665 . ?
Dy3 O4 Dy3 89.73(3) 3_655 2_665 ?
Dy3 O4 Dy3 172.2(5) . 2_665 ?
Dy3 O4 Dy3 89.73(3) 4_565 2_665 ?
Dy3 O4 Dy3 172.2(5) 4_565 3_655 ?
Dy3 O4 Dy3 89.74(3) . 4_565 ?
Dy3 O4 Dy3 89.73(3) . 3_655 ?
Dy2 O5 Dy2 99.03(19) . 3_655 ?
C1 O5 Dy2 138.1(5) . 3_655 ?
C1 O5 Dy2 119.2(5) . . ?
C6 O6 Dy2 141.8(5) . . ?
Dy3 O7 Dy3 99.02(19) . 4_565 ?
C5 O7 Dy3 121.0(5) . . ?
C5 O7 Dy3 135.7(5) . 4_565 ?
C9 O8 Dy3 142.9(6) . . ?
C34 O9 Dy3 142.7(9) . . ?
C18 O10 Dy2 133.0(6) . . ?
C14 O11 C31 118.7(8) . . ?
C15 O12 C33 118.4(8) . . ?
C3 N1 Dy2 127.1(6) . . ?
C3 N1 C17 115.3(7) . . ?
C17 N1 Dy2 117.5(5) . . ?
C13 N2 Dy3 128.7(6) . . ?
C13 N2 C21 114.5(7) . . ?
C21 N2 Dy3 116.7(5) . . ?
C18 N3 C28 122.0(8) . . ?
C18 N3 C29 120.3(9) . . ?
C28 N3 C29 117.6(8) . . ?
C34 N4 C35 119.8(13) . . ?
C34 N4 C36 121.6(15) . . ?
C35 N4 C36 118.5(15) . . ?
O5 C1 C4 120.7(7) . . ?
O5 C1 C11 120.6(8) . . ?
C4 C1 C11 118.7(8) . . ?
C15 C2 C9 121.6(9) . . ?
N1 C3 C7 128.3(8) . . ?
C1 C4 C17 118.6(7) . . ?
C1 C4 C22 120.6(8) . . ?
C22 C4 C17 120.7(8) . . ?
O7 C5 C10 121.2(8) . . ?
O7 C5 C16 120.0(7) . . ?
C10 C5 C16 118.7(8) . . ?
O6 C6 C7 122.7(8) . . ?
O6 C6 C8 119.0(8) . . ?
C8 C6 C7 118.3(8) . . ?
C3 C7 C6 123.5(8) . . ?
C25 C7 C3 118.1(8) . . ?
C25 C7 C6 118.1(8) . . ?
C14 C8 C6 121.0(8) . . ?
O8 C9 C2 119.3(8) . . ?
O8 C9 C12 122.6(8) . . ?
C2 C9 C12 118.1(8) . . ?
C20 C10 C5 120.3(9) . . ?
C19 C11 C1 120.4(9) . . ?
C9 C12 C13 124.2(8) . . ?
C24 C12 C9 118.0(9) . . ?
C24 C12 C13 117.5(9) . . ?
N2 C13 C12 127.1(8) . . ?
C8 C14 O11 123.7(9) . . ?
C8 C14 C23 120.9(8) . . ?
C23 C14 O11 115.4(8) . . ?
O12 C15 C2 114.8(8) . . ?
O12 C15 C27 124.8(8) . . ?
C27 C15 C2 120.4(9) . . ?
C5 C16 C21 118.2(8) . . ?
C26 C16 C5 119.3(8) . . ?
C26 C16 C21 122.5(8) . . ?
N1 C17 C4 112.9(7) . . ?
O10 C18 N3 125.4(9) . . ?
C11 C19 C30 120.2(9) . . ?
C32 C20 C10 120.4(9) . . ?
N2 C21 C16 113.7(7) . . ?
C30 C22 C4 120.8(10) . . ?
C25 C23 C14 118.8(9) . . ?
C27 C24 C12 124.0(10) . . ?
C23 C25 C7 122.8(9) . . ?
C32 C26 C16 121.6(10) . . ?
C24 C27 C15 117.9(9) . . ?
C22 C30 C19 119.3(9) . . ?
C26 C32 C20 119.6(9) . . ?
O9 C34 N4 130.2(16) . . ?

_olex2_submission_special_instructions 'No special instructions were received'
