# Electronic Supplementary Material (ESI) for Journal of Materials Chemistry C.
# This journal is © The Royal Society of Chemistry 2022

####################################################################### 
# 
# 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_a_a
_database_code_depnum_ccdc_archive 'CCDC 2095653'
loop_
_audit_author_name
_audit_author_address
'Konstantin Lyssenko'
;Chemical Department MSU
Russia
;
_audit_update_record             
;
2021-07-10 deposited with the CCDC.	2022-04-12 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT420_a_a                 
;
PROBLEM: D-H Bond Without Acceptor  O1W      --H1WC     .     Please Check
RESPONSE: wo atoms (O1w and H1wa) of the water molecule occupy the  special position (mirror plane). While H1wc is in the general position  with the occupancy 0.5.   As the consequence of the disorder as well  as disorder of ClO4 anion it was impossible to locate hydrogen atoms which all participate in the formation of H-bonds
;
# Added during the CSD deposition process: Saturday 10 July 2021 05:40 PM
# end Validation Reply Form


_audit_creation_method           SHELXL-2016/6
_shelx_SHELXL_version_number     2016/6
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C39 H41 Er N15, 3(Cl O4), 2(C2 H2 N), H2 O'
_chemical_formula_sum            'C43 H47 Cl3 Er N17 O13'
_chemical_formula_weight         1283.58

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Er Er -0.2586 4.9576 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           64
_space_group_name_H-M_alt        'C m c a'
_space_group_name_Hall           '-C 2bc 2'

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

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

_cell_length_a                   20.9668(4)
_cell_length_b                   21.3554(4)
_cell_length_c                   22.6800(5)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     10155.1(4)
_cell_formula_units_Z            8
_cell_measurement_temperature    120(2)
_cell_measurement_reflns_used    2617
_cell_measurement_theta_min      2.22
_cell_measurement_theta_max      26.22

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.679
_exptl_crystal_F_000             5176
_exptl_transmission_factor_min   0.615
_exptl_transmission_factor_max   0.699
_exptl_crystal_size_max          0.285
_exptl_crystal_size_mid          0.228
_exptl_crystal_size_min          0.204
_exptl_absorpt_coefficient_mu    1.892
_shelx_estimated_absorpt_T_min   0.615
_shelx_estimated_absorpt_T_max   0.699
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   SADABS
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      120(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  "Bruker APEX II CCD area detector'"
_diffrn_measurement_method       'omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            40696
_diffrn_reflns_av_unetI/netI     0.0527
_diffrn_reflns_av_R_equivalents  0.0833
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_theta_min         2.108
_diffrn_reflns_theta_max         28.999
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             6921
_reflns_number_gt                4706
_reflns_threshold_expression     I>2σ(I)
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'Bruker APEX II'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0577P)²+50.0312P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         6921
_refine_ls_number_parameters     381
_refine_ls_number_restraints     36
_refine_ls_R_factor_all          0.0604
_refine_ls_R_factor_gt           0.0402
_refine_ls_wR_factor_ref         0.1164
_refine_ls_wR_factor_gt          0.1058
_refine_ls_goodness_of_fit_ref   0.966
_refine_ls_restrained_S_all      0.988
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000


loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Er1 Er 0.250000 0.32085(2) 0.250000 0.01398(8) Uani 1 2 d S T P . .
N1 N 0.26277(14) 0.26158(15) 0.34894(15) 0.0209(7) Uani 1 1 d . . . . .
N2 N 0.17619(16) 0.23323(15) 0.26690(16) 0.0234(7) Uani 1 1 d . . . . .
N3 N 0.13511(17) 0.15101(16) 0.31249(18) 0.0304(8) Uani 1 1 d . . . . .
N4 N 0.33650(15) 0.35689(15) 0.31416(14) 0.0209(7) Uani 1 1 d . . . . .
N5 N 0.38243(17) 0.37238(18) 0.40067(16) 0.0296(8) Uani 1 1 d . . . . .
N6 N 0.250000 0.4411(2) 0.250000 0.0217(9) Uani 1 2 d S T P . .
N7 N 0.31972(16) 0.36984(15) 0.17716(14) 0.0230(7) Uani 1 1 d . . . . .
N8 N 0.3547(2) 0.4473(2) 0.12088(17) 0.0397(10) Uani 1 1 d . . . . .
C1 C 0.2283(2) 0.20876(19) 0.35987(19) 0.0256(8) Uani 1 1 d . . . . .
C2 C 0.2398(2) 0.1719(2) 0.4097(2) 0.0343(11) Uani 1 1 d . . . . .
H2A H 0.215734 0.134870 0.416489 0.041 Uiso 1 1 calc R U . . .
C3 C 0.2865(3) 0.1902(2) 0.4488(2) 0.0416(12) Uani 1 1 d . . . . .
H3A H 0.295107 0.165490 0.482734 0.050 Uiso 1 1 calc R U . . .
C4 C 0.3210(2) 0.2447(2) 0.4388(2) 0.0350(10) Uani 1 1 d . . . . .
H4A H 0.314670 0.272581 0.473127 0.042 Uiso 1 1 calc R U . . .
H4B H 0.366832 0.233356 0.437865 0.042 Uiso 1 1 calc R U . . .
C5 C 0.30775(19) 0.27904(19) 0.38807(17) 0.0239(8) Uani 1 1 d . . . . .
C6 C 0.18054(19) 0.19713(18) 0.31444(19) 0.0236(8) Uani 1 1 d . . . . .
C7 C 0.12705(19) 0.2099(2) 0.2336(2) 0.0281(9) Uani 1 1 d . . . . .
H7A H 0.113089 0.226317 0.196828 0.034 Uiso 1 1 calc R U . . .
C8 C 0.1015(2) 0.1594(2) 0.2617(2) 0.0342(11) Uani 1 1 d . . . . .
H8A H 0.066729 0.134626 0.248393 0.041 Uiso 1 1 calc R U . . .
C9 C 0.1212(2) 0.1008(2) 0.3548(3) 0.0463(13) Uani 1 1 d . . . . .
H9A H 0.081334 0.079932 0.343751 0.069 Uiso 1 1 calc R U . . .
H9B H 0.116867 0.118671 0.394440 0.069 Uiso 1 1 calc R U . . .
H9C H 0.156110 0.070284 0.354603 0.069 Uiso 1 1 calc R U . . .
C10 C 0.34196(19) 0.33605(19) 0.36932(17) 0.0221(8) Uani 1 1 d . . . . .
C11 C 0.37602(18) 0.40830(19) 0.31049(19) 0.0251(8) Uani 1 1 d . . . . .
H11A H 0.382517 0.433035 0.276193 0.030 Uiso 1 1 calc R U . . .
C12 C 0.4042(2) 0.4180(2) 0.3635(2) 0.0310(10) Uani 1 1 d . . . . .
H12A H 0.433485 0.450422 0.373078 0.037 Uiso 1 1 calc R U . . .
C13 C 0.4034(3) 0.3663(3) 0.4620(2) 0.0562(16) Uani 1 1 d . . . . .
H13A H 0.366297 0.359511 0.487457 0.084 Uiso 1 1 calc R U . . .
H13B H 0.425512 0.404621 0.474110 0.084 Uiso 1 1 calc R U . . .
H13C H 0.432573 0.330567 0.465497 0.084 Uiso 1 1 calc R U . . .
C14 C 0.2821(2) 0.47271(18) 0.20807(19) 0.0272(9) Uani 1 1 d . . . . .
C15 C 0.2823(3) 0.5382(2) 0.2066(2) 0.0409(12) Uani 1 1 d . . . . .
H15A H 0.304236 0.560147 0.176301 0.049 Uiso 1 1 calc R U . . .
C16 C 0.250000 0.5698(3) 0.250000 0.048(2) Uani 1 2 d S T P . .
H16A H 0.249998 0.614263 0.249999 0.058 Uiso 1 2 calc R U P . .
C17 C 0.3175(2) 0.43206(19) 0.16761(18) 0.0271(9) Uani 1 1 d . . . . .
C18 C 0.3597(2) 0.3460(2) 0.13513(19) 0.0310(10) Uani 1 1 d . . . . .
H18A H 0.370247 0.303031 0.130647 0.037 Uiso 1 1 calc R U . . .
C19 C 0.3819(3) 0.3932(3) 0.1008(2) 0.0444(13) Uani 1 1 d . . . . .
H19A H 0.410933 0.389414 0.068848 0.053 Uiso 1 1 calc R U . . .
C20 C 0.3674(4) 0.5093(3) 0.0940(3) 0.0649(19) Uani 1 1 d . . . . .
H20A H 0.327014 0.528104 0.081292 0.097 Uiso 1 1 calc R U . . .
H20B H 0.395525 0.504145 0.059879 0.097 Uiso 1 1 calc R U . . .
H20C H 0.387891 0.536566 0.123103 0.097 Uiso 1 1 calc R U . . .
Cl1 Cl 0.21166(11) 0.000000 0.500000 0.0530(5) Uani 1 2 d S T P . .
Cl2 Cl 0.500000 0.27939(9) 0.57828(7) 0.0378(4) Uani 1 2 d S T P . .
Cl3 Cl 0.500000 -0.01630(7) 0.71873(8) 0.0323(3) Uani 1 2 d S T P . .
O1S O 0.1783(4) 0.0140(4) 0.4515(4) 0.142(3) Uani 1 1 d . U . . .
O2S O 0.2484(3) 0.0539(3) 0.5112(4) 0.110(3) Uani 1 1 d . . . . .
O3S O 0.500000 0.2724(4) 0.6397(3) 0.092(3) Uani 1 2 d S T P . .
O4S O 0.4451(3) 0.2507(2) 0.5530(2) 0.0838(15) Uani 1 1 d . U . . .
O5S O 0.500000 0.3455(2) 0.5634(2) 0.0423(12) Uani 1 2 d S T P . .
O6S O 0.500000 -0.0732(2) 0.6841(3) 0.0635(18) Uani 1 2 d S T P A .
O7S O 0.5686(4) -0.0090(4) 0.7229(5) 0.061(2) Uani 0.5 1 d . . P A 1
O7S' O 0.5321(6) 0.0343(4) 0.6943(5) 0.098(5) Uani 0.5 1 d . . P A 2
O8S O 0.500000 -0.0252(5) 0.7794(5) 0.116(3) Uani 1 2 d S TU P A .
C1S C 0.500000 0.1762(4) 0.7440(3) 0.046(2) Uani 1 2 d S T P . .
H1SB H 0.537320 0.190010 0.723300 0.056 Uiso 0.5 1 d R U P . .
H1SA H 0.500000 0.131580 0.750180 0.056 Uiso 1 2 d R U P . .
N1S N 0.500000 0.2130(3) 0.8527(3) 0.0502(16) Uani 1 2 d S T P . .
C2S C 0.500000 0.1963(3) 0.8054(4) 0.0383(17) Uani 1 2 d S T P . .
O1W O 0.500000 0.4818(3) 0.5571(4) 0.111(3) Uani 1 2 d S T P . .
H1WC H 0.532760 0.496019 0.574516 0.133 Uiso 0.5 1 d R U P . .
H1WA H 0.500000 0.441879 0.558366 0.133 Uiso 1 2 d R U P . .
C3S C 0.500000 0.6148(8) 0.0401(6) 0.090(4) Uani 1 2 d S TU P . .
N3S N 0.500000 0.6608(8) 0.0711(7) 0.183(7) Uani 1 2 d S TU P . .
C4S C 0.500000 0.5699(7) 0.0097(5) 0.088(4) Uani 1 2 d S TU P . .
H4SA H 0.500000 0.579163 -0.031851 0.132 Uiso 1 2 d R U P . .
H4SB H 0.537270 0.546033 0.019409 0.132 Uiso 0.5 1 d R U P . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Er1 N7 2.442(3) . ?
Er1 N7 2.442(3) 7_545 ?
Er1 N4 2.449(3) 7_545 ?
Er1 N4 2.449(3) . ?
Er1 N2 2.458(3) . ?
Er1 N2 2.458(3) 7_545 ?
Er1 N6 2.568(4) . ?
Er1 N1 2.590(3) 7_545 ?
Er1 N1 2.590(3) . ?
N1 C5 1.348(5) . ?
N1 C1 1.362(5) . ?
N2 C6 1.329(5) . ?
N2 C7 1.371(5) . ?
N3 C8 1.362(6) . ?
N3 C6 1.371(5) . ?
N3 C9 1.469(6) . ?
N4 C10 1.333(5) . ?
N4 C11 1.378(5) . ?
N5 C10 1.352(5) . ?
N5 C12 1.367(6) . ?
N5 C13 1.465(6) . ?
N6 C14 1.346(5) . ?
N6 C14 1.346(5) 7_545 ?
N7 C17 1.347(5) . ?
N7 C18 1.367(6) . ?
N8 C19 1.366(7) . ?
N8 C17 1.355(6) . ?
N8 C20 1.481(6) . ?
C1 C2 1.398(6) . ?
C1 C6 1.458(6) . ?
C2 C3 1.379(8) . ?
C2 H2A 0.9500 . ?
C3 C4 1.389(7) . ?
C3 H3A 0.9500 . ?
C4 C5 1.393(6) . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C5 C10 1.476(6) . ?
C7 C8 1.364(6) . ?
C7 H7A 0.9500 . ?
C8 H8A 0.9500 . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C11 C12 1.356(6) . ?
C11 H11A 0.9500 . ?
C12 H12A 0.9500 . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C14 C15 1.398(6) . ?
C14 C17 1.466(7) . ?
C15 C16 1.373(6) . ?
C15 H15A 0.9500 . ?
C16 H16A 0.9500 . ?
C18 C19 1.356(7) . ?
C18 H18A 0.9500 . ?
C19 H19A 0.9500 . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
Cl1 O1S 1.336(8) 4_556 ?
Cl1 O1S 1.336(8) . ?
Cl1 O2S 1.409(6) . ?
Cl1 O2S 1.409(6) 4_556 ?
Cl2 O3S 1.400(6) . ?
Cl2 O4S 1.423(5) . ?
Cl2 O4S 1.423(5) 12_655 ?
Cl2 O5S 1.452(6) . ?
Cl3 O7S' 1.388(8) . ?
Cl3 O7S' 1.388(8) 12_655 ?
Cl3 O8S 1.390(11) . ?
Cl3 O6S 1.447(5) . ?
Cl3 O7S 1.450(7) . ?
Cl3 O7S 1.450(7) 12_655 ?
O7S' O7S' 1.34(3) 12_655 ?
C1S C2S 1.457(11) . ?
C1S H1SB 0.9588 . ?
C1S H1SA 0.9630 . ?
C1S H1SB 0.9589 12_655 ?
N1S C2S 1.132(10) . ?
O1W H1WC 0.8491 . ?
O1W H1WA 0.8528 . ?
O1W H1WC 0.8491 12_655 ?
C3S C4S 1.181(17) . ?
C3S N3S 1.21(2) . ?
C4S H4SA 0.9619 . ?
C4S H4SB 0.9591 . ?
C4S H4SB 0.9591 12_655 ?

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
N7 Er1 N7 129.26(16) . 7_545 ?
N7 Er1 N4 84.65(12) . 7_545 ?
N7 Er1 N4 79.86(11) 7_545 7_545 ?
N7 Er1 N4 79.86(11) . . ?
N7 Er1 N4 84.65(12) 7_545 . ?
N4 Er1 N4 143.37(15) 7_545 . ?
N7 Er1 N2 143.96(11) . . ?
N7 Er1 N2 81.01(11) 7_545 . ?
N4 Er1 N2 82.28(11) 7_545 . ?
N4 Er1 N2 127.78(11) . . ?
N7 Er1 N2 81.01(11) . 7_545 ?
N7 Er1 N2 143.96(11) 7_545 7_545 ?
N4 Er1 N2 127.79(11) 7_545 7_545 ?
N4 Er1 N2 82.28(11) . 7_545 ?
N2 Er1 N2 80.86(16) . 7_545 ?
N7 Er1 N6 64.63(8) . . ?
N7 Er1 N6 64.63(8) 7_545 . ?
N4 Er1 N6 71.68(7) 7_545 . ?
N4 Er1 N6 71.68(7) . . ?
N2 Er1 N6 139.57(8) . . ?
N2 Er1 N6 139.57(8) 7_545 . ?
N7 Er1 N1 71.64(10) . 7_545 ?
N7 Er1 N1 137.20(10) 7_545 7_545 ?
N4 Er1 N1 64.04(10) 7_545 7_545 ?
N4 Er1 N1 138.14(10) . 7_545 ?
N2 Er1 N1 72.43(11) . 7_545 ?
N2 Er1 N1 63.77(11) 7_545 7_545 ?
N6 Er1 N1 119.25(8) . 7_545 ?
N7 Er1 N1 137.20(10) . . ?
N7 Er1 N1 71.64(10) 7_545 . ?
N4 Er1 N1 138.14(10) 7_545 . ?
N4 Er1 N1 64.04(10) . . ?
N2 Er1 N1 63.77(11) . . ?
N2 Er1 N1 72.42(11) 7_545 . ?
N6 Er1 N1 119.25(8) . . ?
N1 Er1 N1 121.49(15) 7_545 . ?
C5 N1 C1 118.7(3) . . ?
C5 N1 Er1 120.5(2) . . ?
C1 N1 Er1 120.5(3) . . ?
C6 N2 C7 106.8(3) . . ?
C6 N2 Er1 121.7(3) . . ?
C7 N2 Er1 131.5(3) . . ?
C8 N3 C6 107.0(3) . . ?
C8 N3 C9 123.1(4) . . ?
C6 N3 C9 129.9(4) . . ?
C10 N4 C11 105.7(3) . . ?
C10 N4 Er1 121.1(3) . . ?
C11 N4 Er1 131.3(3) . . ?
C10 N5 C12 107.1(3) . . ?
C10 N5 C13 129.6(4) . . ?
C12 N5 C13 123.3(4) . . ?
C14 N6 C14 119.8(5) . 7_545 ?
C14 N6 Er1 120.1(2) . . ?
C14 N6 Er1 120.1(2) 7_545 . ?
C17 N7 C18 106.0(4) . . ?
C17 N7 Er1 120.7(3) . . ?
C18 N7 Er1 132.8(3) . . ?
C19 N8 C17 107.3(4) . . ?
C19 N8 C20 122.9(5) . . ?
C17 N8 C20 129.8(5) . . ?
N1 C1 C2 121.5(4) . . ?
N1 C1 C6 112.1(3) . . ?
C2 C1 C6 126.4(4) . . ?
C3 C2 C1 118.9(4) . . ?
C3 C2 H2A 120.6 . . ?
C1 C2 H2A 120.6 . . ?
C2 C3 C4 120.2(4) . . ?
C2 C3 H3A 119.9 . . ?
C4 C3 H3A 119.9 . . ?
C5 C4 C3 118.2(4) . . ?
C5 C4 H4A 107.8 . . ?
C3 C4 H4A 107.8 . . ?
C5 C4 H4B 107.8 . . ?
C3 C4 H4B 107.8 . . ?
H4A C4 H4B 107.1 . . ?
N1 C5 C4 122.6(4) . . ?
N1 C5 C10 112.2(3) . . ?
C4 C5 C10 125.1(4) . . ?
N2 C6 N3 110.1(4) . . ?
N2 C6 C1 121.5(3) . . ?
N3 C6 C1 128.5(4) . . ?
C8 C7 N2 108.9(4) . . ?
C8 C7 H7A 125.5 . . ?
N2 C7 H7A 125.5 . . ?
N3 C8 C7 107.3(4) . . ?
N3 C8 H8A 126.4 . . ?
C7 C8 H8A 126.4 . . ?
N3 C9 H9A 109.5 . . ?
N3 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
N3 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
N4 C10 N5 110.9(4) . . ?
N4 C10 C5 120.3(4) . . ?
N5 C10 C5 128.8(4) . . ?
C12 C11 N4 109.3(4) . . ?
C12 C11 H11A 125.4 . . ?
N4 C11 H11A 125.4 . . ?
C11 C12 N5 107.0(4) . . ?
C11 C12 H12A 126.5 . . ?
N5 C12 H12A 126.5 . . ?
N5 C13 H13A 109.5 . . ?
N5 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
N5 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
N6 C14 C15 121.4(5) . . ?
N6 C14 C17 113.5(3) . . ?
C15 C14 C17 125.1(4) . . ?
C16 C15 C14 118.2(5) . . ?
C16 C15 H15A 120.9 . . ?
C14 C15 H15A 120.9 . . ?
C15 C16 C15 121.1(6) 7_545 . ?
C15 C16 H16A 119.5 7_545 . ?
C15 C16 H16A 119.5 . . ?
N7 C17 N8 110.1(4) . . ?
N7 C17 C14 120.1(4) . . ?
N8 C17 C14 129.7(4) . . ?
C19 C18 N7 109.5(4) . . ?
C19 C18 H18A 125.2 . . ?
N7 C18 H18A 125.2 . . ?
C18 C19 N8 107.1(4) . . ?
C18 C19 H19A 126.5 . . ?
N8 C19 H19A 126.5 . . ?
N8 C20 H20A 109.5 . . ?
N8 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
N8 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
O1S Cl1 O1S 116.9(8) 4_556 . ?
O1S Cl1 O2S 108.7(5) 4_556 . ?
O1S Cl1 O2S 104.6(5) . . ?
O1S Cl1 O2S 104.6(5) 4_556 4_556 ?
O1S Cl1 O2S 108.7(5) . 4_556 ?
O2S Cl1 O2S 113.7(5) . 4_556 ?
O3S Cl2 O4S 110.7(3) . . ?
O3S Cl2 O4S 110.7(3) . 12_655 ?
O4S Cl2 O4S 107.8(5) . 12_655 ?
O3S Cl2 O5S 109.6(4) . . ?
O4S Cl2 O5S 109.0(2) . . ?
O4S Cl2 O5S 109.0(2) 12_655 . ?
O7S' Cl3 O8S 120.1(6) . . ?
O7S' Cl3 O8S 120.1(6) 12_655 . ?
O7S' Cl3 O6S 115.9(4) . . ?
O7S' Cl3 O6S 115.9(4) 12_655 . ?
O8S Cl3 O6S 115.1(5) . . ?
O8S Cl3 O7S 87.2(4) . . ?
O6S Cl3 O7S 97.2(3) . . ?
O8S Cl3 O7S 87.2(4) . 12_655 ?
O6S Cl3 O7S 97.2(3) . 12_655 ?
O7S Cl3 O7S 165.6(7) . 12_655 ?
O7S' O7S' Cl3 61.0(6) 12_655 . ?
C2S C1S H1SB 112.1 . . ?
C2S C1S H1SA 98.7 . . ?
H1SB C1S H1SA 112.1 . . ?
C2S C1S H1SB 112.1(2) . 12_655 ?
H1SB C1S H1SB 109.4 . 12_655 ?
H1SA C1S H1SB 112.1 . 12_655 ?
N1S C2S C1S 178.7(8) . . ?
H1WC O1W H1WA 110.0 . . ?
H1WC O1W H1WC 108.0 . 12_655 ?
H1WA O1W H1WC 110.0 . 12_655 ?
C4S C3S N3S 179.8(15) . . ?
C3S C4S H4SA 114.0 . . ?
C3S C4S H4SB 107.2 . . ?
H4SA C4S H4SB 109.6 . . ?
C3S C4S H4SB 107.2(4) . 12_655 ?
H4SA C4S H4SB 109.6 . 12_655 ?
H4SB C4S H4SB 109.1 . 12_655 ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O1W H1WA O5S 0.85 2.06 2.914(9) 178.8 .

_refine_diff_density_max         1.763
_refine_diff_density_min         -1.115
_refine_diff_density_rms         0.144



_exptl_crystal_preparation       'Magnetic properties,Luminescent'
####################################################################### 
# 
# 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_a
_database_code_depnum_ccdc_archive 'CCDC 2095656'
loop_
_audit_author_name
_audit_author_address
'Konstantin Lyssenko'
;Chemical Department MSU
Russia
;
_audit_update_record             
;
2021-07-10 deposited with the CCDC.	2022-04-12 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2016/6
_shelx_SHELXL_version_number     2016/6
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C39 H41 Eu N15, 3(Cl O4), 2(C2 H2 N), H2 O'
_chemical_formula_sum            'C43 H47 Cl3 Eu N17 O13'
_chemical_formula_weight         1268.28

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Eu Eu -0.1578 3.6682 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           64
_space_group_name_H-M_alt        'C m c a'
_space_group_name_Hall           '-C 2bc 2'

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

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

_cell_length_a                   20.9145(14)
_cell_length_b                   21.4762(11)
_cell_length_c                   22.7944(12)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     10238.4(10)
_cell_formula_units_Z            8
_cell_measurement_temperature    120(2)
_cell_measurement_reflns_used    9967
_cell_measurement_theta_min      2.22
_cell_measurement_theta_max      31.22

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.646
_exptl_crystal_F_000             5136
_exptl_transmission_factor_min   0.753
_exptl_transmission_factor_max   0.832
_exptl_crystal_size_max          0.390
_exptl_crystal_size_mid          0.210
_exptl_crystal_size_min          0.210
_exptl_absorpt_coefficient_mu    1.462
_shelx_estimated_absorpt_T_min   0.599
_shelx_estimated_absorpt_T_max   0.749
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6689
_exptl_absorpt_correction_T_max  0.7468
_exptl_absorpt_process_details   
;
 SADABS 2016/2: Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D.,
 J. Appl. Cryst. 48 (2015) 3-10
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      120(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_measurement_device_type  "Bruker APEX II CCD area detector'"
_diffrn_measurement_method       'omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            53374
_diffrn_reflns_av_unetI/netI     0.0273
_diffrn_reflns_av_R_equivalents  0.0444
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_theta_min         1.896
_diffrn_reflns_theta_max         28.994
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 0.997
_reflns_number_total             6987
_reflns_number_gt                5158
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'Bruker APEX II'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0525P)²+71.7218P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         6987
_refine_ls_number_parameters     381
_refine_ls_number_restraints     48
_refine_ls_R_factor_all          0.0592
_refine_ls_R_factor_gt           0.0409
_refine_ls_wR_factor_ref         0.1205
_refine_ls_wR_factor_gt          0.1100
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_restrained_S_all      1.074
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

_vrf_PLAT420_a                   
;
PROBLEM: D-H Without Acceptor       O1W      --H1WC     .     Please Check 
RESPONSE: Two atoms (O1w and H1wa) of the water molecule occupy the 
special position (mirror plane). While H1wc is in the general position 
with the occupancy 0.5.   As the consequence of the disorder as well 
as disorder of ClO4 anion it was impossible to locate hydrogen atoms which
all participate in the formation of H-bonds

;
# end Validation Reply Form


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 0.250000 0.32117(2) 0.250000 0.01702(8) Uani 1 2 d S T P . .
N1 N 0.26396(14) 0.26081(14) 0.35029(14) 0.0236(6) Uani 1 1 d . . . . .
N2 N 0.17545(16) 0.23187(14) 0.26916(15) 0.0263(6) Uani 1 1 d . . . . .
N3 N 0.13605(17) 0.14990(15) 0.31535(18) 0.0350(8) Uani 1 1 d . . . . .
N4 N 0.33846(15) 0.35660(14) 0.31600(14) 0.0249(6) Uani 1 1 d . . . . .
N5 N 0.38320(18) 0.37142(17) 0.40246(16) 0.0358(8) Uani 1 1 d . . . . .
N6 N 0.250000 0.4429(2) 0.250000 0.0253(9) Uani 1 2 d S T P . .
N7 N 0.32070(16) 0.37266(15) 0.17651(14) 0.0280(7) Uani 1 1 d . . . . .
N8 N 0.3548(2) 0.4503(2) 0.12128(17) 0.0447(10) Uani 1 1 d . . . . .
C1 C 0.2292(2) 0.20863(18) 0.36141(18) 0.0292(8) Uani 1 1 d . . . . .
C2 C 0.2410(2) 0.1717(2) 0.4108(2) 0.0402(11) Uani 1 1 d . . . . .
H2A H 0.216567 0.135179 0.418069 0.048 Uiso 1 1 calc R U . . .
C3 C 0.2891(3) 0.1898(3) 0.4487(2) 0.0509(13) Uani 1 1 d . . . . .
H3A H 0.298771 0.164809 0.481955 0.061 Uiso 1 1 calc R U . . .
C4 C 0.3235(2) 0.2440(2) 0.4389(2) 0.0422(11) Uani 1 1 d . . . . .
H4A H 0.369430 0.232975 0.437556 0.051 Uiso 1 1 calc R U . . .
H4B H 0.317297 0.271616 0.473239 0.051 Uiso 1 1 calc R U . . .
C5 C 0.30938(19) 0.27823(18) 0.38866(16) 0.0278(8) Uani 1 1 d . . . . .
C6 C 0.18066(19) 0.19636(17) 0.31689(18) 0.0275(8) Uani 1 1 d . . . . .
C7 C 0.12646(19) 0.20767(19) 0.2364(2) 0.0326(9) Uani 1 1 d . . . . .
H7A H 0.112135 0.223420 0.199784 0.039 Uiso 1 1 calc R U . . .
C8 C 0.1015(2) 0.1573(2) 0.2649(2) 0.0391(10) Uani 1 1 d . . . . .
H8A H 0.066774 0.132151 0.252183 0.047 Uiso 1 1 calc R U . . .
C9 C 0.1233(3) 0.1000(2) 0.3577(3) 0.0516(14) Uani 1 1 d . . . . .
H9A H 0.083848 0.078274 0.346764 0.077 Uiso 1 1 calc R U . . .
H9B H 0.118397 0.117977 0.397013 0.077 Uiso 1 1 calc R U . . .
H9C H 0.159002 0.070517 0.357751 0.077 Uiso 1 1 calc R U . . .
C10 C 0.34339(18) 0.33496(18) 0.37068(17) 0.0261(8) Uani 1 1 d . . . . .
C11 C 0.37696(19) 0.40809(18) 0.31345(19) 0.0292(8) Uani 1 1 d . . . . .
H11A H 0.383237 0.433250 0.279658 0.035 Uiso 1 1 calc R U . . .
C12 C 0.4048(2) 0.4178(2) 0.3664(2) 0.0361(9) Uani 1 1 d . . . . .
H12A H 0.433545 0.450289 0.376479 0.043 Uiso 1 1 calc R U . . .
C13 C 0.4040(4) 0.3649(3) 0.4636(2) 0.070(2) Uani 1 1 d . . . . .
H13A H 0.366955 0.355617 0.488423 0.105 Uiso 1 1 calc R U . . .
H13B H 0.423843 0.403867 0.476675 0.105 Uiso 1 1 calc R U . . .
H13C H 0.435117 0.330948 0.466570 0.105 Uiso 1 1 calc R U . . .
C14 C 0.2825(2) 0.47458(17) 0.20838(18) 0.0295(8) Uani 1 1 d . . . . .
C15 C 0.2830(3) 0.5394(2) 0.2076(2) 0.0450(12) Uani 1 1 d . . . . .
H15A H 0.305825 0.561383 0.178104 0.054 Uiso 1 1 calc R U . . .
C16 C 0.250000 0.5708(3) 0.250000 0.053(2) Uani 1 2 d S T P . .
H16A H 0.249997 0.615031 0.249999 0.064 Uiso 1 2 calc R U P . .
C17 C 0.3182(2) 0.43435(18) 0.16795(18) 0.0310(9) Uani 1 1 d . . . . .
C18 C 0.3604(2) 0.3495(2) 0.13410(19) 0.0380(10) Uani 1 1 d . . . . .
H18A H 0.371474 0.306958 0.129257 0.046 Uiso 1 1 calc R U . . .
C19 C 0.3813(3) 0.3972(3) 0.1000(2) 0.0506(13) Uani 1 1 d . . . . .
H19A H 0.409377 0.394011 0.067363 0.061 Uiso 1 1 calc R U . . .
C20 C 0.3674(3) 0.5113(3) 0.0952(3) 0.0678(19) Uani 1 1 d . . . . .
H20A H 0.326904 0.530478 0.083266 0.102 Uiso 1 1 calc R U . . .
H20B H 0.395055 0.506367 0.060839 0.102 Uiso 1 1 calc R U . . .
H20C H 0.388653 0.538054 0.124110 0.102 Uiso 1 1 calc R U . . .
Cl1 Cl 0.21151(12) 0.000000 0.500000 0.0640(6) Uani 1 2 d S T P . .
Cl2 Cl 0.500000 0.27844(8) 0.57848(7) 0.0441(4) Uani 1 2 d S T P . .
Cl3 Cl 0.500000 -0.01610(6) 0.72036(8) 0.0364(3) Uani 1 2 d S T P . .
O1S O 0.1868(5) 0.0130(5) 0.4501(5) 0.187(4) Uani 1 1 d . U . . .
O2S O 0.2477(3) 0.0539(3) 0.5091(5) 0.135(3) Uani 1 1 d . . . . .
O3S O 0.500000 0.2677(4) 0.6385(3) 0.122(3) Uani 1 2 d S T P . .
O4S O 0.4454(3) 0.2501(3) 0.5524(3) 0.1051(18) Uani 1 1 d . U . . .
O5S O 0.500000 0.3443(2) 0.5655(2) 0.0519(13) Uani 1 2 d S T P . .
O6S O 0.500000 -0.0727(2) 0.6866(3) 0.0677(18) Uani 1 2 d S T P A .
O7S O 0.5684(4) -0.0067(4) 0.7238(4) 0.059(2) Uani 0.5 1 d . U P A 1
O7S' O 0.5318(5) 0.0345(5) 0.6961(4) 0.082(3) Uani 0.5 1 d . U P A 2
O8S O 0.500000 -0.0253(4) 0.7820(4) 0.116(3) Uani 1 2 d S TU P A .
C1S C 0.500000 0.1756(4) 0.7438(3) 0.055(2) Uani 1 2 d S T P . .
H1SB H 0.537320 0.189424 0.723097 0.066 Uiso 0.5 1 d R U P . .
H1SA H 0.500000 0.130994 0.749977 0.066 Uiso 1 2 d R U P . .
N1S N 0.500000 0.2146(3) 0.8510(3) 0.0574(17) Uani 1 2 d S T P . .
C2S C 0.500000 0.1973(4) 0.8044(4) 0.0461(17) Uani 1 2 d S T P . .
O1W O 0.500000 0.4809(3) 0.5564(4) 0.107(3) Uani 1 2 d S T P . .
H1WC H 0.532760 0.495108 0.573871 0.128 Uiso 0.5 1 d R U P . .
H1WA H 0.500000 0.440968 0.557721 0.128 Uiso 1 2 d R U P . .
C3S C 0.500000 0.6164(6) 0.0406(5) 0.083(3) Uani 1 2 d S TU P . .
N3S N 0.500000 0.6629(8) 0.0769(8) 0.194(7) Uani 1 2 d S TU P . .
C4S C 0.500000 0.5724(6) 0.0091(5) 0.088(3) Uani 1 2 d S TU P . .
H4SA H 0.500000 0.581597 -0.032413 0.132 Uiso 1 2 d R U P . .
H4SB H 0.537270 0.548467 0.018847 0.132 Uiso 0.5 1 d R U P . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Eu1 N7 2.493(3) . ?
Eu1 N7 2.493(3) 7_545 ?
Eu1 N2 2.510(3) 7_545 ?
Eu1 N2 2.510(3) . ?
Eu1 N4 2.503(3) . ?
Eu1 N4 2.503(3) 7_545 ?
Eu1 N6 2.615(4) . ?
Eu1 N1 2.644(3) 7_545 ?
Eu1 N1 2.644(3) . ?
N1 C5 1.344(5) . ?
N1 C1 1.360(5) . ?
N2 C6 1.333(5) . ?
N2 C7 1.370(5) . ?
N3 C6 1.367(5) . ?
N3 C8 1.367(6) . ?
N3 C9 1.467(5) . ?
N4 C10 1.334(5) . ?
N4 C11 1.369(5) . ?
N5 C10 1.353(5) . ?
N5 C12 1.367(6) . ?
N5 C13 1.467(6) . ?
N6 C14 1.351(5) . ?
N6 C14 1.351(5) 7_545 ?
N7 C17 1.340(5) . ?
N7 C18 1.367(5) . ?
N8 C19 1.358(7) . ?
N8 C17 1.355(6) . ?
N8 C20 1.462(6) . ?
C1 C2 1.399(6) . ?
C1 C6 1.459(6) . ?
C2 C3 1.384(7) . ?
C2 H2A 0.9500 . ?
C3 C4 1.386(7) . ?
C3 H3A 0.9500 . ?
C4 C5 1.392(5) . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C5 C10 1.469(6) . ?
C7 C8 1.366(6) . ?
C7 H7A 0.9500 . ?
C8 H8A 0.9500 . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C11 C12 1.356(6) . ?
C11 H11A 0.9500 . ?
C12 H12A 0.9500 . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C14 C15 1.392(5) . ?
C14 C17 1.466(6) . ?
C15 C16 1.366(6) . ?
C15 H15A 0.9500 . ?
C16 H16A 0.9500 . ?
C18 C19 1.358(7) . ?
C18 H18A 0.9500 . ?
C19 H19A 0.9500 . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
Cl1 O1S 1.281(10) 4_556 ?
Cl1 O1S 1.281(10) . ?
Cl1 O2S 1.399(6) 4_556 ?
Cl1 O2S 1.399(6) . ?
Cl2 O3S 1.387(6) . ?
Cl2 O4S 1.423(6) 12_655 ?
Cl2 O4S 1.423(6) . ?
Cl2 O5S 1.446(5) . ?
Cl3 O7S' 1.389(10) . ?
Cl3 O7S' 1.389(10) 12_655 ?
Cl3 O8S 1.419(10) . ?
Cl3 O6S 1.439(5) . ?
Cl3 O7S 1.446(8) . ?
Cl3 O7S 1.446(8) 12_655 ?
O7S' O7S' 1.329(19) 12_655 ?
C1S C2S 1.457(11) . ?
C1S H1SB 0.9589 . ?
C1S H1SA 0.9684 . ?
C1S H1SB 0.9589 12_655 ?
N1S C2S 1.127(10) . ?
O1W H1WC 0.8493 . ?
O1W H1WA 0.8576 . ?
O1W H1WC 0.8493 12_655 ?
C3S C4S 1.187(15) . ?
C3S N3S 1.298(19) . ?
C4S H4SA 0.9668 . ?
C4S H4SB 0.9593 . ?
C4S H4SB 0.9592 12_655 ?

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
N7 Eu1 N7 127.33(15) . 7_545 ?
N7 Eu1 N2 81.58(11) . 7_545 ?
N7 Eu1 N2 145.52(11) 7_545 7_545 ?
N7 Eu1 N2 145.52(11) . . ?
N7 Eu1 N2 81.58(11) 7_545 . ?
N2 Eu1 N2 80.35(15) 7_545 . ?
N7 Eu1 N4 80.25(11) . . ?
N7 Eu1 N4 84.24(11) 7_545 . ?
N2 Eu1 N4 82.98(10) 7_545 . ?
N2 Eu1 N4 125.93(10) . . ?
N7 Eu1 N4 84.24(11) . 7_545 ?
N7 Eu1 N4 80.24(11) 7_545 7_545 ?
N2 Eu1 N4 125.94(10) 7_545 7_545 ?
N2 Eu1 N4 82.98(10) . 7_545 ?
N4 Eu1 N4 144.60(14) . 7_545 ?
N7 Eu1 N6 63.67(8) . . ?
N7 Eu1 N6 63.67(8) 7_545 . ?
N2 Eu1 N6 139.83(7) 7_545 . ?
N2 Eu1 N6 139.82(7) . . ?
N4 Eu1 N6 72.30(7) . . ?
N4 Eu1 N6 72.30(7) 7_545 . ?
N7 Eu1 N1 72.67(10) . 7_545 ?
N7 Eu1 N1 137.13(10) 7_545 7_545 ?
N2 Eu1 N1 62.84(10) 7_545 7_545 ?
N2 Eu1 N1 72.98(10) . 7_545 ?
N4 Eu1 N1 138.62(10) . 7_545 ?
N4 Eu1 N1 63.12(10) 7_545 7_545 ?
N6 Eu1 N1 119.36(7) . 7_545 ?
N7 Eu1 N1 137.13(10) . . ?
N7 Eu1 N1 72.67(10) 7_545 . ?
N2 Eu1 N1 72.98(10) 7_545 . ?
N2 Eu1 N1 62.84(10) . . ?
N4 Eu1 N1 63.11(10) . . ?
N4 Eu1 N1 138.62(10) 7_545 . ?
N6 Eu1 N1 119.36(7) . . ?
N1 Eu1 N1 121.29(14) 7_545 . ?
C5 N1 C1 119.1(3) . . ?
C5 N1 Eu1 120.3(2) . . ?
C1 N1 Eu1 120.4(3) . . ?
C6 N2 C7 106.8(3) . . ?
C6 N2 Eu1 121.9(3) . . ?
C7 N2 Eu1 131.3(3) . . ?
C6 N3 C8 107.4(3) . . ?
C6 N3 C9 129.8(4) . . ?
C8 N3 C9 122.8(4) . . ?
C10 N4 C11 106.0(3) . . ?
C10 N4 Eu1 120.8(2) . . ?
C11 N4 Eu1 130.9(2) . . ?
C10 N5 C12 107.6(3) . . ?
C10 N5 C13 129.5(4) . . ?
C12 N5 C13 122.8(4) . . ?
C14 N6 C14 119.6(5) . 7_545 ?
C14 N6 Eu1 120.2(2) . . ?
C14 N6 Eu1 120.2(2) 7_545 . ?
C17 N7 C18 106.3(4) . . ?
C17 N7 Eu1 120.8(3) . . ?
C18 N7 Eu1 132.4(3) . . ?
C19 N8 C17 107.4(4) . . ?
C19 N8 C20 122.3(5) . . ?
C17 N8 C20 130.3(5) . . ?
N1 C1 C2 121.5(4) . . ?
N1 C1 C6 113.0(3) . . ?
C2 C1 C6 125.4(4) . . ?
C3 C2 C1 118.1(4) . . ?
C3 C2 H2A 120.9 . . ?
C1 C2 H2A 120.9 . . ?
C4 C3 C2 120.8(4) . . ?
C4 C3 H3A 119.6 . . ?
C2 C3 H3A 119.6 . . ?
C3 C4 C5 117.8(4) . . ?
C3 C4 H4A 107.9 . . ?
C5 C4 H4A 107.9 . . ?
C3 C4 H4B 107.9 . . ?
C5 C4 H4B 107.9 . . ?
H4A C4 H4B 107.2 . . ?
N1 C5 C4 122.6(4) . . ?
N1 C5 C10 113.0(3) . . ?
C4 C5 C10 124.3(4) . . ?
N2 C6 N3 109.9(4) . . ?
N2 C6 C1 121.4(3) . . ?
N3 C6 C1 128.6(4) . . ?
C8 C7 N2 109.1(4) . . ?
C8 C7 H7A 125.4 . . ?
N2 C7 H7A 125.4 . . ?
C7 C8 N3 106.8(4) . . ?
C7 C8 H8A 126.6 . . ?
N3 C8 H8A 126.6 . . ?
N3 C9 H9A 109.5 . . ?
N3 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
N3 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
N4 C10 N5 110.2(4) . . ?
N4 C10 C5 120.8(3) . . ?
N5 C10 C5 128.9(4) . . ?
C12 C11 N4 109.8(4) . . ?
C12 C11 H11A 125.1 . . ?
N4 C11 H11A 125.1 . . ?
C11 C12 N5 106.4(4) . . ?
C11 C12 H12A 126.8 . . ?
N5 C12 H12A 126.8 . . ?
N5 C13 H13A 109.5 . . ?
N5 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
N5 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
N6 C14 C15 121.0(4) . . ?
N6 C14 C17 113.6(3) . . ?
C15 C14 C17 125.3(4) . . ?
C16 C15 C14 118.8(5) . . ?
C16 C15 H15A 120.6 . . ?
C14 C15 H15A 120.6 . . ?
C15 C16 C15 120.8(6) . 7_545 ?
C15 C16 H16A 119.6 . . ?
C15 C16 H16A 119.6 7_545 . ?
N7 C17 N8 110.0(4) . . ?
N7 C17 C14 120.7(4) . . ?
N8 C17 C14 129.2(4) . . ?
C19 C18 N7 109.1(5) . . ?
C19 C18 H18A 125.5 . . ?
N7 C18 H18A 125.5 . . ?
C18 C19 N8 107.3(4) . . ?
C18 C19 H19A 126.4 . . ?
N8 C19 H19A 126.4 . . ?
N8 C20 H20A 109.5 . . ?
N8 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
N8 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
O1S Cl1 O1S 132.3(10) 4_556 . ?
O1S Cl1 O2S 99.8(6) 4_556 4_556 ?
O1S Cl1 O2S 105.5(6) . 4_556 ?
O1S Cl1 O2S 105.5(6) 4_556 . ?
O1S Cl1 O2S 99.8(6) . . ?
O2S Cl1 O2S 114.5(6) 4_556 . ?
O3S Cl2 O4S 109.9(3) . 12_655 ?
O3S Cl2 O4S 109.9(3) . . ?
O4S Cl2 O4S 106.7(5) 12_655 . ?
O3S Cl2 O5S 111.4(5) . . ?
O4S Cl2 O5S 109.4(3) 12_655 . ?
O4S Cl2 O5S 109.4(3) . . ?
O7S' Cl3 O8S 120.3(5) . . ?
O7S' Cl3 O8S 120.3(5) 12_655 . ?
O7S' Cl3 O6S 116.6(5) . . ?
O7S' Cl3 O6S 116.6(5) 12_655 . ?
O8S Cl3 O6S 114.3(5) . . ?
O8S Cl3 O7S 88.1(4) . . ?
O6S Cl3 O7S 98.4(3) . . ?
O8S Cl3 O7S 88.1(4) . 12_655 ?
O6S Cl3 O7S 98.4(3) . 12_655 ?
O7S Cl3 O7S 162.8(7) . 12_655 ?
O7S' O7S' Cl3 61.4(4) 12_655 . ?
C2S C1S H1SB 111.5 . . ?
C2S C1S H1SA 100.3 . . ?
H1SB C1S H1SA 112.2 . . ?
C2S C1S H1SB 111.5(2) . 12_655 ?
H1SB C1S H1SB 109.0 . 12_655 ?
H1SA C1S H1SB 112.2 . 12_655 ?
N1S C2S C1S 179.4(8) . . ?
H1WC O1W H1WA 110.1 . . ?
H1WC O1W H1WC 107.6 . 12_655 ?
H1WA O1W H1WC 110.1 . 12_655 ?
C4S C3S N3S 177.5(13) . . ?
C3S C4S H4SA 115.4 . . ?
C3S C4S H4SB 106.6 . . ?
H4SA C4S H4SB 109.7 . . ?
C3S C4S H4SB 106.6(4) . 12_655 ?
H4SA C4S H4SB 109.7 . 12_655 ?
H4SB C4S H4SB 108.7 . 12_655 ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O1W H1WA O5S 0.86 2.08 2.940(8) 177.1 .

_refine_diff_density_max         2.367
_refine_diff_density_min         -1.333
_refine_diff_density_rms         0.125



####################################################################### 
# 
# 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_a_a_CCDC1
_database_code_depnum_ccdc_archive 'CCDC 2095657'
loop_
_audit_author_name
_audit_author_address
'Konstantin Lyssenko'
;Chemical Department MSU
Russia
;
_audit_update_record             
;
2021-07-10 deposited with the CCDC.	2022-04-12 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2016/6
_shelx_SHELXL_version_number     2016/6
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C39 H41 Tb N15, 3(Cl O4), 2(C2 H2 N), H2 O'
_chemical_formula_sum            'C43 H47 Cl3 N17 O13 Tb'
_chemical_formula_weight         1275.24

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Tb Tb -0.1723 4.1537 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           64
_space_group_name_H-M_alt        'C m c a'
_space_group_name_Hall           '-C 2bc 2'

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

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

_cell_length_a                   20.8878(4)
_cell_length_b                   21.4260(4)
_cell_length_c                   22.7165(5)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     10166.6(4)
_cell_formula_units_Z            8
_cell_measurement_temperature    120(2)
_cell_measurement_reflns_used    1730
_cell_measurement_theta_min      2.222
_cell_measurement_theta_max      27.32

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.666
_exptl_crystal_F_000             5152
_exptl_transmission_factor_min   0.753
_exptl_transmission_factor_max   0.832
_exptl_crystal_size_max          0.455
_exptl_crystal_size_mid          0.421
_exptl_crystal_size_min          0.335
_exptl_absorpt_coefficient_mu    1.630
_shelx_estimated_absorpt_T_min   0.524
_shelx_estimated_absorpt_T_max   0.611
_exptl_absorpt_correction_type   ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      120(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  "Bruker APEX II CCD area detector'"
_diffrn_measurement_method       'omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            78532
_diffrn_reflns_av_unetI/netI     0.0265
_diffrn_reflns_av_R_equivalents  0.0520
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_theta_min         1.901
_diffrn_reflns_theta_max         28.997
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             6931
_reflns_number_gt                4988
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'Bruker APEX II'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0525P)²+71.7218P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         6931
_refine_ls_number_parameters     381
_refine_ls_number_restraints     48
_refine_ls_R_factor_all          0.0611
_refine_ls_R_factor_gt           0.0406
_refine_ls_wR_factor_ref         0.1210
_refine_ls_wR_factor_gt          0.1101
_refine_ls_goodness_of_fit_ref   1.068
_refine_ls_restrained_S_all      1.085
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Tb1 Tb 0.250000 0.32161(2) 0.250000 0.01805(8) Uani 1 2 d S T P . .
N1 N 0.26355(15) 0.26162(15) 0.35013(15) 0.0247(7) Uani 1 1 d . . . . .
N2 N 0.17606(17) 0.23343(15) 0.26830(16) 0.0270(7) Uani 1 1 d . . . . .
N3 N 0.13604(18) 0.15147(16) 0.31467(18) 0.0355(9) Uani 1 1 d . . . . .
N4 N 0.33755(16) 0.35734(15) 0.31574(14) 0.0253(7) Uani 1 1 d . . . . .
N5 N 0.38253(19) 0.37215(18) 0.40270(17) 0.0363(9) Uani 1 1 d . . . . .
N6 N 0.250000 0.4423(2) 0.250000 0.0253(9) Uani 1 2 d S T P . .
N7 N 0.32006(17) 0.37207(16) 0.17656(15) 0.0287(7) Uani 1 1 d . . . . .
N8 N 0.3553(2) 0.4489(2) 0.12118(18) 0.0453(11) Uani 1 1 d . . . . .
C1 C 0.2294(2) 0.20950(19) 0.36101(19) 0.0287(8) Uani 1 1 d . . . . .
C2 C 0.2409(2) 0.1720(2) 0.4102(2) 0.0413(12) Uani 1 1 d . . . . .
H2A H 0.216809 0.135049 0.416881 0.050 Uiso 1 1 calc R U . . .
C3 C 0.2889(3) 0.1903(3) 0.4491(2) 0.0496(13) Uani 1 1 d . . . . .
H3A H 0.298288 0.165342 0.482655 0.059 Uiso 1 1 calc R U . . .
C4 C 0.3230(2) 0.2446(2) 0.4392(2) 0.0421(11) Uani 1 1 d . . . . .
H4A H 0.369064 0.233641 0.437817 0.051 Uiso 1 1 calc R U . . .
H4B H 0.316794 0.272202 0.473652 0.051 Uiso 1 1 calc R U . . .
C5 C 0.3090(2) 0.2791(2) 0.38885(17) 0.0291(8) Uani 1 1 d . . . . .
C6 C 0.1811(2) 0.19750(18) 0.31599(19) 0.0288(8) Uani 1 1 d . . . . .
C7 C 0.1268(2) 0.2095(2) 0.2352(2) 0.0328(9) Uani 1 1 d . . . . .
H7A H 0.112749 0.225110 0.198326 0.039 Uiso 1 1 calc R U . . .
C8 C 0.1015(2) 0.1595(2) 0.2641(2) 0.0397(11) Uani 1 1 d . . . . .
H8A H 0.066337 0.134773 0.251488 0.048 Uiso 1 1 calc R U . . .
C9 C 0.1226(3) 0.1020(2) 0.3575(3) 0.0528(14) Uani 1 1 d . . . . .
H9A H 0.083649 0.079646 0.345817 0.079 Uiso 1 1 calc R U . . .
H9B H 0.116479 0.120441 0.396523 0.079 Uiso 1 1 calc R U . . .
H9C H 0.158650 0.072740 0.358641 0.079 Uiso 1 1 calc R U . . .
C10 C 0.34274(19) 0.33573(19) 0.37063(18) 0.0268(8) Uani 1 1 d . . . . .
C11 C 0.37610(19) 0.4087(2) 0.3127(2) 0.0309(9) Uani 1 1 d . . . . .
H11A H 0.382538 0.433722 0.278648 0.037 Uiso 1 1 calc R U . . .
C12 C 0.4039(2) 0.4184(2) 0.3662(2) 0.0374(10) Uani 1 1 d . . . . .
H12A H 0.432632 0.451049 0.376193 0.045 Uiso 1 1 calc R U . . .
C13 C 0.4039(4) 0.3655(3) 0.4639(2) 0.0663(18) Uani 1 1 d . . . . .
H13A H 0.367210 0.354826 0.488816 0.099 Uiso 1 1 calc R U . . .
H13B H 0.422602 0.404963 0.477303 0.099 Uiso 1 1 calc R U . . .
H13C H 0.436067 0.332359 0.466338 0.099 Uiso 1 1 calc R U . . .
C14 C 0.2822(2) 0.47366(18) 0.20807(19) 0.0310(9) Uani 1 1 d . . . . .
C15 C 0.2826(3) 0.5387(2) 0.2072(3) 0.0470(13) Uani 1 1 d . . . . .
H15A H 0.304950 0.560895 0.177382 0.056 Uiso 1 1 calc R U . . .
C16 C 0.250000 0.5695(3) 0.250000 0.054(2) Uani 1 2 d S T P . .
H16A H 0.249999 0.613805 0.250001 0.064 Uiso 1 2 calc R U P . .
C17 C 0.3180(2) 0.43345(19) 0.16785(18) 0.0314(9) Uani 1 1 d . . . . .
C18 C 0.3602(2) 0.3486(2) 0.1344(2) 0.0387(11) Uani 1 1 d . . . . .
H18A H 0.371066 0.305835 0.129927 0.046 Uiso 1 1 calc R U . . .
C19 C 0.3819(3) 0.3956(3) 0.1001(2) 0.0498(14) Uani 1 1 d . . . . .
H19A H 0.410351 0.392090 0.067634 0.060 Uiso 1 1 calc R U . . .
C20 C 0.3686(3) 0.5098(3) 0.0949(3) 0.0680(19) Uani 1 1 d . . . . .
H20A H 0.328437 0.528713 0.081506 0.102 Uiso 1 1 calc R U . . .
H20B H 0.397562 0.504606 0.061355 0.102 Uiso 1 1 calc R U . . .
H20C H 0.388683 0.536944 0.124331 0.102 Uiso 1 1 calc R U . . .
Cl1 Cl 0.21115(12) 0.000000 0.500000 0.0619(6) Uani 1 2 d S T P . .
Cl2 Cl 0.500000 0.27649(10) 0.57807(8) 0.0497(4) Uani 1 2 d S T P . .
Cl3 Cl 0.500000 -0.01676(7) 0.72076(8) 0.0371(3) Uani 1 2 d S T P . .
O1S O 0.1904(6) 0.0133(5) 0.4485(5) 0.196(4) Uani 1 1 d . U . . .
O2S O 0.2468(3) 0.0542(3) 0.5097(5) 0.141(3) Uani 1 1 d . . . . .
O3S O 0.500000 0.2664(5) 0.6385(3) 0.122(4) Uani 1 2 d S T P . .
O4S O 0.4452(3) 0.2492(3) 0.5517(3) 0.1051(18) Uani 1 1 d . U . . .
O5S O 0.500000 0.3427(3) 0.5655(3) 0.0578(14) Uani 1 2 d S T P . .
O6S O 0.500000 -0.0733(2) 0.6871(3) 0.0684(19) Uani 1 2 d S T P A .
O7S O 0.5684(4) -0.0077(4) 0.7243(4) 0.064(2) Uani 0.5 1 d . U P A 1
O7S' O 0.5306(5) 0.0341(5) 0.6957(4) 0.082(3) Uani 0.5 1 d . U P A 2
O8S O 0.500000 -0.0250(5) 0.7827(5) 0.121(3) Uani 1 2 d S TU P A .
C1S C 0.500000 0.1749(4) 0.7445(3) 0.055(2) Uani 1 2 d S T P . .
H1SB H 0.537320 0.188753 0.723800 0.066 Uiso 0.5 1 d R U P . .
H1SA H 0.500000 0.130323 0.750680 0.066 Uiso 1 2 d R U P . .
N1S N 0.500000 0.2125(4) 0.8524(3) 0.0589(18) Uani 1 2 d S T P . .
C2S C 0.500000 0.1956(4) 0.8052(4) 0.0453(17) Uani 1 2 d S T P . .
O1W O 0.500000 0.4819(6) 0.5511(7) 0.197(6) Uani 1 2 d S T P . .
H1WC H 0.532760 0.496104 0.568564 0.236 Uiso 0.5 1 d R U P . .
H1WA H 0.500000 0.441964 0.552414 0.236 Uiso 1 2 d R U P . .
C3S C 0.500000 0.6162(7) 0.0411(5) 0.081(3) Uani 1 2 d S TU P . .
N3S N 0.500000 0.6617(7) 0.0755(7) 0.187(7) Uani 1 2 d S TU P . .
C4S C 0.500000 0.5734(7) 0.0112(5) 0.093(4) Uani 1 2 d S TU P . .
H4SA H 0.500000 0.582650 -0.030307 0.140 Uiso 1 2 d R U P . .
H4SB H 0.537270 0.549520 0.020953 0.140 Uiso 0.5 1 d R U P . .

_vrf_PLAT420_a                   
;
PROBLEM: D-H Without Acceptor       O1W      --H1WC     .     Please Check 
RESPONSE: Two atoms (O1w and H1wa) of the water molecule occupy the 
special position (mirror plane). While H1wc is in the general position 
with the occupancy 0.5.   As the consequence of the disorder as well 
as disorder of ClO4 anion it was impossible to locate hydrogen atoms which
all participate in the formation of H-bonds

;
# end Validation Reply Form



_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 N7 2.469(3) . ?
Tb1 N7 2.469(3) 7_545 ?
Tb1 N2 2.475(3) 7_545 ?
Tb1 N2 2.475(3) . ?
Tb1 N4 2.482(3) . ?
Tb1 N4 2.482(3) 7_545 ?
Tb1 N6 2.586(4) . ?
Tb1 N1 2.628(3) 7_545 ?
Tb1 N1 2.628(3) . ?
N1 C5 1.347(5) . ?
N1 C1 1.348(5) . ?
N2 C6 1.333(5) . ?
N2 C7 1.373(5) . ?
N3 C6 1.363(5) . ?
N3 C8 1.366(6) . ?
N3 C9 1.466(6) . ?
N4 C10 1.335(5) . ?
N4 C11 1.366(5) . ?
N5 C10 1.353(5) . ?
N5 C12 1.367(6) . ?
N5 C13 1.466(6) . ?
N6 C14 1.345(5) 7_545 ?
N6 C14 1.346(5) . ?
N7 C17 1.331(5) . ?
N7 C18 1.368(6) . ?
N8 C19 1.356(8) . ?
N8 C17 1.356(6) . ?
N8 C20 1.462(6) . ?
C1 C2 1.398(6) . ?
C1 C6 1.459(6) . ?
C2 C3 1.393(8) . ?
C2 H2A 0.9500 . ?
C3 C4 1.384(7) . ?
C3 H3A 0.9500 . ?
C4 C5 1.392(6) . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C5 C10 1.463(6) . ?
C7 C8 1.363(6) . ?
C7 H7A 0.9500 . ?
C8 H8A 0.9500 . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C11 C12 1.363(6) . ?
C11 H11A 0.9500 . ?
C12 H12A 0.9500 . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C14 C15 1.394(6) . ?
C14 C17 1.462(7) . ?
C15 C16 1.358(7) . ?
C15 H15A 0.9500 . ?
C16 H16A 0.9500 . ?
C18 C19 1.352(7) . ?
C18 H18A 0.9500 . ?
C19 H19A 0.9500 . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
Cl1 O1S 1.280(11) . ?
Cl1 O1S 1.280(11) 4_556 ?
Cl1 O2S 1.397(7) 4_556 ?
Cl1 O2S 1.397(7) . ?
Cl2 O3S 1.389(7) . ?
Cl2 O4S 1.418(6) . ?
Cl2 O4S 1.418(6) 12_655 ?
Cl2 O5S 1.448(6) . ?
Cl3 O7S' 1.386(10) 12_655 ?
Cl3 O7S' 1.386(10) . ?
Cl3 O8S 1.418(11) . ?
Cl3 O6S 1.432(5) . ?
Cl3 O7S 1.444(9) 12_655 ?
Cl3 O7S 1.444(9) . ?
O7S' O7S' 1.278(19) 12_655 ?
C1S C2S 1.448(12) . ?
C1S H1SB 0.9571 . ?
C1S H1SA 0.9661 . ?
C1S H1SB 0.9572 12_655 ?
N1S C2S 1.133(11) . ?
O1W H1WC 0.8477 . ?
O1W H1WA 0.8556 . ?
O1W H1WC 0.8477 12_655 ?
C3S C4S 1.142(16) . ?
C3S N3S 1.248(19) . ?
C4S H4SA 0.9635 . ?
C4S H4SB 0.9577 . ?
C4S H4SB 0.9576 12_655 ?

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
N7 Tb1 N7 128.05(16) . 7_545 ?
N7 Tb1 N2 81.43(12) . 7_545 ?
N7 Tb1 N2 144.85(11) 7_545 7_545 ?
N7 Tb1 N2 144.85(11) . . ?
N7 Tb1 N2 81.43(12) 7_545 . ?
N2 Tb1 N2 80.50(16) 7_545 . ?
N7 Tb1 N4 80.49(11) . . ?
N7 Tb1 N4 83.98(12) 7_545 . ?
N2 Tb1 N4 82.92(11) 7_545 . ?
N2 Tb1 N4 126.45(11) . . ?
N7 Tb1 N4 83.98(12) . 7_545 ?
N7 Tb1 N4 80.49(11) 7_545 7_545 ?
N2 Tb1 N4 126.45(11) 7_545 7_545 ?
N2 Tb1 N4 82.92(11) . 7_545 ?
N4 Tb1 N4 144.07(15) . 7_545 ?
N7 Tb1 N6 64.03(8) . . ?
N7 Tb1 N6 64.03(8) 7_545 . ?
N2 Tb1 N6 139.75(8) 7_545 . ?
N2 Tb1 N6 139.75(8) . . ?
N4 Tb1 N6 72.03(7) . . ?
N4 Tb1 N6 72.03(8) 7_545 . ?
N7 Tb1 N1 72.13(11) . 7_545 ?
N7 Tb1 N1 137.34(11) 7_545 7_545 ?
N2 Tb1 N1 63.16(11) 7_545 7_545 ?
N2 Tb1 N1 72.83(11) . 7_545 ?
N4 Tb1 N1 138.68(10) . 7_545 ?
N4 Tb1 N1 63.31(10) 7_545 7_545 ?
N6 Tb1 N1 119.28(7) . 7_545 ?
N7 Tb1 N1 137.34(11) . . ?
N7 Tb1 N1 72.13(11) 7_545 . ?
N2 Tb1 N1 72.83(11) 7_545 . ?
N2 Tb1 N1 63.16(11) . . ?
N4 Tb1 N1 63.31(10) . . ?
N4 Tb1 N1 138.68(10) 7_545 . ?
N6 Tb1 N1 119.28(7) . . ?
N1 Tb1 N1 121.43(15) 7_545 . ?
C5 N1 C1 118.9(4) . . ?
C5 N1 Tb1 120.3(3) . . ?
C1 N1 Tb1 120.4(3) . . ?
C6 N2 C7 106.7(3) . . ?
C6 N2 Tb1 121.9(3) . . ?
C7 N2 Tb1 131.4(3) . . ?
C6 N3 C8 107.0(4) . . ?
C6 N3 C9 129.9(4) . . ?
C8 N3 C9 123.1(4) . . ?
C10 N4 C11 106.2(3) . . ?
C10 N4 Tb1 121.0(3) . . ?
C11 N4 Tb1 130.7(3) . . ?
C10 N5 C12 107.0(4) . . ?
C10 N5 C13 129.9(4) . . ?
C12 N5 C13 123.1(4) . . ?
C14 N6 C14 120.1(5) 7_545 . ?
C14 N6 Tb1 119.9(2) 7_545 . ?
C14 N6 Tb1 119.9(2) . . ?
C17 N7 C18 106.2(4) . . ?
C17 N7 Tb1 120.9(3) . . ?
C18 N7 Tb1 132.5(3) . . ?
C19 N8 C17 107.9(4) . . ?
C19 N8 C20 121.9(5) . . ?
C17 N8 C20 130.2(5) . . ?
N1 C1 C2 122.1(4) . . ?
N1 C1 C6 112.6(3) . . ?
C2 C1 C6 125.3(4) . . ?
C3 C2 C1 118.0(4) . . ?
C3 C2 H2A 121.0 . . ?
C1 C2 H2A 121.0 . . ?
C4 C3 C2 120.2(4) . . ?
C4 C3 H3A 119.9 . . ?
C2 C3 H3A 119.9 . . ?
C3 C4 C5 118.2(5) . . ?
C3 C4 H4A 107.8 . . ?
C5 C4 H4A 107.8 . . ?
C3 C4 H4B 107.8 . . ?
C5 C4 H4B 107.8 . . ?
H4A C4 H4B 107.1 . . ?
N1 C5 C4 122.5(4) . . ?
N1 C5 C10 112.7(3) . . ?
C4 C5 C10 124.8(4) . . ?
N2 C6 N3 110.2(4) . . ?
N2 C6 C1 121.5(4) . . ?
N3 C6 C1 128.3(4) . . ?
C8 C7 N2 108.7(4) . . ?
C8 C7 H7A 125.6 . . ?
N2 C7 H7A 125.6 . . ?
C7 C8 N3 107.4(4) . . ?
C7 C8 H8A 126.3 . . ?
N3 C8 H8A 126.3 . . ?
N3 C9 H9A 109.5 . . ?
N3 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
N3 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
N4 C10 N5 110.7(4) . . ?
N4 C10 C5 120.9(4) . . ?
N5 C10 C5 128.5(4) . . ?
C12 C11 N4 109.1(4) . . ?
C12 C11 H11A 125.4 . . ?
N4 C11 H11A 125.4 . . ?
C11 C12 N5 107.0(4) . . ?
C11 C12 H12A 126.5 . . ?
N5 C12 H12A 126.5 . . ?
N5 C13 H13A 109.5 . . ?
N5 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
N5 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
N6 C14 C15 120.8(5) . . ?
N6 C14 C17 113.8(3) . . ?
C15 C14 C17 125.3(4) . . ?
C16 C15 C14 118.2(5) . . ?
C16 C15 H15A 120.9 . . ?
C14 C15 H15A 120.9 . . ?
C15 C16 C15 121.9(6) 7_545 . ?
C15 C16 H16A 119.0 7_545 . ?
C15 C16 H16A 119.0 . . ?
N7 C17 N8 109.8(4) . . ?
N7 C17 C14 120.4(4) . . ?
N8 C17 C14 129.7(4) . . ?
C19 C18 N7 109.6(5) . . ?
C19 C18 H18A 125.2 . . ?
N7 C18 H18A 125.2 . . ?
C18 C19 N8 106.6(4) . . ?
C18 C19 H19A 126.7 . . ?
N8 C19 H19A 126.7 . . ?
N8 C20 H20A 109.5 . . ?
N8 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
N8 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
O1S Cl1 O1S 140.4(11) . 4_556 ?
O1S Cl1 O2S 102.8(7) . 4_556 ?
O1S Cl1 O2S 98.0(6) 4_556 4_556 ?
O1S Cl1 O2S 98.0(6) . . ?
O1S Cl1 O2S 102.8(7) 4_556 . ?
O2S Cl1 O2S 115.5(7) 4_556 . ?
O3S Cl2 O4S 110.7(3) . . ?
O3S Cl2 O4S 110.7(3) . 12_655 ?
O4S Cl2 O4S 107.7(6) . 12_655 ?
O3S Cl2 O5S 110.3(5) . . ?
O4S Cl2 O5S 108.7(3) . . ?
O4S Cl2 O5S 108.7(3) 12_655 . ?
O7S' Cl3 O7S' 54.9(8) 12_655 . ?
O7S' Cl3 O8S 120.4(6) 12_655 . ?
O7S' Cl3 O8S 120.4(6) . . ?
O7S' Cl3 O6S 116.4(5) 12_655 . ?
O7S' Cl3 O6S 116.4(5) . . ?
O8S Cl3 O6S 115.1(5) . . ?
O8S Cl3 O7S 87.8(4) . 12_655 ?
O6S Cl3 O7S 98.2(4) . 12_655 ?
O8S Cl3 O7S 87.8(4) . . ?
O6S Cl3 O7S 98.2(4) . . ?
O7S Cl3 O7S 163.4(7) 12_655 . ?
O7S' O7S' Cl3 62.5(4) 12_655 . ?
C2S C1S H1SB 111.9 . . ?
C2S C1S H1SA 99.4 . . ?
H1SB C1S H1SA 112.2 . . ?
C2S C1S H1SB 111.9(2) . 12_655 ?
H1SB C1S H1SB 109.1 . 12_655 ?
H1SA C1S H1SB 112.2 . 12_655 ?
N1S C2S C1S 179.1(9) . . ?
H1WC O1W H1WA 110.1 . . ?
H1WC O1W H1WC 107.7 . 12_655 ?
H1WA O1W H1WC 110.1 . 12_655 ?
C4S C3S N3S 177.8(14) . . ?
C3S C4S H4SA 114.7 . . ?
C3S C4S H4SB 107.0 . . ?
H4SA C4S H4SB 109.6 . . ?
C3S C4S H4SB 107.0(4) . 12_655 ?
H4SA C4S H4SB 109.6 . 12_655 ?
H4SB C4S H4SB 108.8 . 12_655 ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O1W H1WA O5S 0.86 2.15 2.999(13) 174.0 .

_refine_diff_density_max         2.457
_refine_diff_density_min         -1.112
_refine_diff_density_rms         0.127



####################################################################### 
# 
# 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_a_CCDC1
_database_code_depnum_ccdc_archive 'CCDC 2095654'
loop_
_audit_author_name
_audit_author_address
'Konstantin Lyssenko'
;Chemical Department MSU
Russia
;
_audit_update_record             
;
2021-07-10 deposited with the CCDC.	2022-04-12 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2016/6
_shelx_SHELXL_version_number     2016/6
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C39 H41 N15 Yb, 3(Cl O4), 2(C2 H2 N), H2 O'
_chemical_formula_sum            'C43 H47 Cl3 N17 O13 Yb'
_chemical_formula_weight         1289.36

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Yb Yb -0.3850 5.5486 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           64
_space_group_name_H-M_alt        'C m c a'
_space_group_name_Hall           '-C 2bc 2'

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

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

_cell_length_a                   21.0313(12)
_cell_length_b                   21.2857(12)
_cell_length_c                   22.6301(12)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     10130.7(10)
_cell_formula_units_Z            8
_cell_measurement_temperature    120(2)
_cell_measurement_reflns_used    2281
_cell_measurement_theta_min      3
_cell_measurement_theta_max      25

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.691
_exptl_crystal_F_000             5192
_exptl_transmission_factor_min   0.526
_exptl_transmission_factor_max   0.629
_exptl_crystal_size_max          0.353
_exptl_crystal_size_mid          0.272
_exptl_crystal_size_min          0.245
_exptl_absorpt_coefficient_mu    2.086
_shelx_estimated_absorpt_T_min   0.526
_shelx_estimated_absorpt_T_max   0.629
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   SADABS
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      120(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  "Bruker APEX II CCD area detector'"
_diffrn_measurement_method       'omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            33773
_diffrn_reflns_av_unetI/netI     0.1121
_diffrn_reflns_av_R_equivalents  0.1678
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_theta_min         1.937
_diffrn_reflns_theta_max         27.498
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             5984
_reflns_number_gt                3241
_reflns_threshold_expression     I>2σ(I)
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

# start Validation Reply Form
_vrf_PLAT420_a                   
;
PROBLEM: D-H Without Acceptor       O1W      --H1WC     .     Please Check 
RESPONSE: Two atoms (O1w and H1wa) of the water molecule occupy the 
special position (mirror plane). While H1wc is in the general position 
with the occupancy 0.5.   As the consequence of the disorder as well 
as disorder of ClO4 anion it was impossible to locate hydrogen atoms which
all participate in the formation of H-bonds

;
# end Validation Reply Form

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

_computing_data_collection       'Bruker APEX II'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0809P)²+20.4297P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         5984
_refine_ls_number_parameters     381
_refine_ls_number_restraints     36
_refine_ls_R_factor_all          0.1286
_refine_ls_R_factor_gt           0.0598
_refine_ls_wR_factor_ref         0.1780
_refine_ls_wR_factor_gt          0.1407
_refine_ls_goodness_of_fit_ref   1.007
_refine_ls_restrained_S_all      1.010
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Yb1 Yb 0.250000 0.32090(2) 0.250000 0.02204(15) Uani 1 2 d S T P . .
N1 N 0.2627(3) 0.2619(3) 0.3486(3) 0.0272(17) Uani 1 1 d . . . . .
N2 N 0.1773(3) 0.2344(3) 0.2661(3) 0.0275(16) Uani 1 1 d . . . . .
N3 N 0.1348(3) 0.1510(3) 0.3119(3) 0.0344(17) Uani 1 1 d . . . . .
N4 N 0.3356(4) 0.3577(3) 0.3139(3) 0.0285(16) Uani 1 1 d . . . . .
N5 N 0.3823(4) 0.3722(3) 0.3997(3) 0.0361(18) Uani 1 1 d . . . . .
N6 N 0.250000 0.4403(4) 0.250000 0.030(2) Uani 1 2 d S T P . .
N7 N 0.3188(4) 0.3699(3) 0.1772(3) 0.0313(17) Uani 1 1 d . . . . .
N8 N 0.3545(4) 0.4466(4) 0.1206(4) 0.047(2) Uani 1 1 d . . . . .
C1 C 0.2283(4) 0.2088(4) 0.3598(4) 0.032(2) Uani 1 1 d . . . . .
C2 C 0.2388(4) 0.1719(4) 0.4090(4) 0.038(2) Uani 1 1 d . . . . .
H2A H 0.214362 0.135053 0.415550 0.046 Uiso 1 1 calc R U . . .
C3 C 0.2854(5) 0.1896(5) 0.4486(4) 0.047(3) Uani 1 1 d . . . . .
H3A H 0.293886 0.164170 0.482218 0.056 Uiso 1 1 calc R U . . .
C4 C 0.3206(5) 0.2453(4) 0.4393(4) 0.041(2) Uani 1 1 d . . . . .
H4A H 0.313487 0.273475 0.473500 0.049 Uiso 1 1 calc R U . . .
H4B H 0.366331 0.234379 0.438771 0.049 Uiso 1 1 calc R U . . .
C5 C 0.3066(4) 0.2789(4) 0.3874(3) 0.0296(19) Uani 1 1 d . . . . .
C6 C 0.1809(4) 0.1973(4) 0.3136(4) 0.034(2) Uani 1 1 d . . . . .
C7 C 0.1275(4) 0.2109(4) 0.2337(4) 0.036(2) Uani 1 1 d . . . . .
H7A H 0.112995 0.227691 0.197160 0.043 Uiso 1 1 calc R U . . .
C8 C 0.1018(4) 0.1599(4) 0.2614(4) 0.040(2) Uani 1 1 d . . . . .
H8A H 0.067203 0.135242 0.247703 0.049 Uiso 1 1 calc R U . . .
C9 C 0.1213(5) 0.1013(5) 0.3535(5) 0.055(3) Uani 1 1 d . . . . .
H9A H 0.083486 0.078139 0.340614 0.083 Uiso 1 1 calc R U . . .
H9B H 0.113514 0.119489 0.392666 0.083 Uiso 1 1 calc R U . . .
H9C H 0.157645 0.072620 0.355581 0.083 Uiso 1 1 calc R U . . .
C10 C 0.3409(4) 0.3354(4) 0.3693(4) 0.0286(19) Uani 1 1 d . . . . .
C11 C 0.3756(4) 0.4086(4) 0.3096(4) 0.033(2) Uani 1 1 d . . . . .
H11A H 0.382370 0.433238 0.275168 0.040 Uiso 1 1 calc R U . . .
C12 C 0.4036(4) 0.4179(4) 0.3628(4) 0.035(2) Uani 1 1 d . . . . .
H12A H 0.432835 0.450291 0.372511 0.042 Uiso 1 1 calc R U . . .
C13 C 0.4046(6) 0.3667(5) 0.4619(4) 0.059(3) Uani 1 1 d . . . . .
H13A H 0.368051 0.359441 0.487881 0.088 Uiso 1 1 calc R U . . .
H13B H 0.426160 0.405532 0.473562 0.088 Uiso 1 1 calc R U . . .
H13C H 0.434246 0.331309 0.465161 0.088 Uiso 1 1 calc R U . . .
C14 C 0.2821(5) 0.4728(4) 0.2073(4) 0.033(2) Uani 1 1 d . . . . .
C15 C 0.2813(6) 0.5382(5) 0.2074(5) 0.051(3) Uani 1 1 d . . . . .
H15A H 0.303033 0.560629 0.177237 0.061 Uiso 1 1 calc R U . . .
C16 C 0.250000 0.5699(5) 0.250000 0.057(4) Uani 1 2 d S T P . .
H16A H 0.249998 0.614495 0.249999 0.069 Uiso 1 2 calc R U P . .
C17 C 0.3170(5) 0.4310(4) 0.1676(4) 0.036(2) Uani 1 1 d . . . . .
C18 C 0.3592(5) 0.3445(5) 0.1355(4) 0.040(2) Uani 1 1 d . . . . .
H18A H 0.369704 0.301350 0.131417 0.048 Uiso 1 1 calc R U . . .
C19 C 0.3816(5) 0.3928(5) 0.1010(5) 0.054(3) Uani 1 1 d . . . . .
H19A H 0.410738 0.389080 0.069101 0.064 Uiso 1 1 calc R U . . .
C20 C 0.3678(7) 0.5085(5) 0.0944(5) 0.073(4) Uani 1 1 d . . . . .
H20A H 0.327800 0.528211 0.082184 0.110 Uiso 1 1 calc R U . . .
H20B H 0.395436 0.503274 0.059829 0.110 Uiso 1 1 calc R U . . .
H20C H 0.389082 0.535183 0.123589 0.110 Uiso 1 1 calc R U . . .
Cl1 Cl 0.2115(2) 0.000000 0.500000 0.0593(11) Uani 1 2 d S T P . .
Cl2 Cl 0.500000 0.27970(17) 0.57858(15) 0.0461(8) Uani 1 2 d S T P . .
Cl3 Cl 0.500000 -0.01685(13) 0.71721(17) 0.0425(8) Uani 1 2 d S T P . .
O1S O 0.1782(7) 0.0140(6) 0.4517(6) 0.143(5) Uani 1 1 d . U . . .
O2S O 0.2479(6) 0.0539(4) 0.5120(7) 0.123(5) Uani 1 1 d . . . . .
O3S O 0.500000 0.2743(6) 0.6406(5) 0.092(5) Uani 1 2 d S T P . .
O4S O 0.4454(5) 0.2508(5) 0.5544(4) 0.093(3) Uani 1 1 d . U . . .
O5S O 0.500000 0.3464(4) 0.5624(4) 0.054(3) Uani 1 2 d S T P . .
O6S O 0.500000 -0.0738(4) 0.6843(5) 0.065(3) Uani 1 2 d S T P A .
O7S O 0.5678(7) -0.0082(8) 0.7237(9) 0.074(5) Uani 0.5 1 d . . P A 1
O7S' O 0.5286(11) 0.0348(7) 0.6924(9) 0.114(11) Uani 0.5 1 d . . P A 2
O8S O 0.500000 -0.0244(8) 0.7796(9) 0.130(6) Uani 1 2 d S TU P A .
C1S C 0.500000 0.1764(7) 0.7437(7) 0.054(4) Uani 1 2 d S T P . .
H1SB H 0.537320 0.190215 0.723044 0.064 Uiso 0.5 1 d R U P . .
H1SA H 0.500000 0.131785 0.749924 0.064 Uiso 1 2 d R U P . .
N1S N 0.500000 0.2137(6) 0.8526(6) 0.052(3) Uani 1 2 d S T P . .
C2S C 0.500000 0.1966(7) 0.8056(8) 0.045(4) Uani 1 2 d S T P . .
O1W O 0.500000 0.4819(6) 0.5565(7) 0.134(7) Uani 1 2 d S T P . .
H1WC H 0.532760 0.496111 0.573971 0.161 Uiso 0.5 1 d R U P . .
H1WA H 0.500000 0.441971 0.557821 0.161 Uiso 1 2 d R U P . .
C3S C 0.500000 0.6199(16) 0.0408(13) 0.124(9) Uani 1 2 d S TU P . .
N3S N 0.500000 0.6618(13) 0.0710(13) 0.178(11) Uani 1 2 d S TU P . .
C4S C 0.500000 0.5687(12) 0.0120(11) 0.107(8) Uani 1 2 d S TU P . .
H4SA H 0.500000 0.577911 -0.029531 0.161 Uiso 1 2 d R U P . .
H4SB H 0.537270 0.544781 0.021729 0.161 Uiso 0.5 1 d R U P . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Yb1 N7 2.428(7) . ?
Yb1 N7 2.428(7) 7_545 ?
Yb1 N2 2.420(6) . ?
Yb1 N2 2.420(6) 7_545 ?
Yb1 N4 2.439(7) 7_545 ?
Yb1 N4 2.439(7) . ?
Yb1 N6 2.541(8) . ?
Yb1 N1 2.574(7) 7_545 ?
Yb1 N1 2.574(7) . ?
N1 C1 1.366(11) . ?
N1 C5 1.325(10) . ?
N2 C6 1.336(10) . ?
N2 C7 1.375(11) . ?
N3 C8 1.349(11) . ?
N3 C6 1.383(11) . ?
N3 C9 1.445(11) . ?
N4 C10 1.345(10) . ?
N4 C11 1.376(11) . ?
N5 C10 1.358(11) . ?
N5 C12 1.356(11) . ?
N5 C13 1.488(11) . ?
N6 C14 1.366(10) . ?
N6 C14 1.366(10) 7_545 ?
N7 C17 1.320(10) . ?
N7 C18 1.380(12) . ?
N8 C19 1.354(14) . ?
N8 C17 1.364(12) . ?
N8 C20 1.472(12) . ?
C1 C2 1.380(13) . ?
C1 C6 1.465(13) . ?
C2 C3 1.380(14) . ?
C2 H2A 0.9500 . ?
C3 C4 1.414(13) . ?
C3 H3A 0.9500 . ?
C4 C5 1.406(12) . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C5 C10 1.462(12) . ?
C7 C8 1.365(13) . ?
C7 H7A 0.9500 . ?
C8 H8A 0.9500 . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C11 C12 1.355(12) . ?
C11 H11A 0.9500 . ?
C12 H12A 0.9500 . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C14 C15 1.393(12) . ?
C14 C17 1.462(13) . ?
C15 C16 1.349(13) . ?
C15 H15A 0.9500 . ?
C16 H16A 0.9500 . ?
C18 C19 1.374(13) . ?
C18 H18A 0.9500 . ?
C19 H19A 0.9500 . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
Cl1 O1S 1.331(14) 4_556 ?
Cl1 O1S 1.331(14) . ?
Cl1 O2S 1.406(10) . ?
Cl1 O2S 1.406(10) 4_556 ?
Cl2 O3S 1.408(11) . ?
Cl2 O4S 1.413(10) . ?
Cl2 O4S 1.413(10) 12_655 ?
Cl2 O5S 1.466(10) . ?
Cl3 O7S' 1.373(16) . ?
Cl3 O7S' 1.373(16) 12_655 ?
Cl3 O8S 1.421(19) . ?
Cl3 O6S 1.423(10) . ?
Cl3 O7S 1.446(14) . ?
Cl3 O7S 1.446(14) 12_655 ?
O7S' O7S' 1.20(5) 12_655 ?
C1S C2S 1.47(2) . ?
C1S H1SB 0.9600 . ?
C1S H1SA 0.9599 . ?
C1S H1SB 0.9601 12_655 ?
N1S C2S 1.123(18) . ?
O1W H1WC 0.8500 . ?
O1W H1WA 0.8500 . ?
O1W H1WC 0.8501 12_655 ?
C3S C4S 1.27(3) . ?
C3S N3S 1.12(3) . ?
C4S H4SA 0.9597 . ?
C4S H4SB 0.9600 . ?
C4S H4SB 0.9600 12_655 ?

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
N7 Yb1 N7 129.1(3) . 7_545 ?
N7 Yb1 N2 143.7(2) . . ?
N7 Yb1 N2 81.2(2) 7_545 . ?
N7 Yb1 N2 81.2(2) . 7_545 ?
N7 Yb1 N2 143.7(2) 7_545 7_545 ?
N2 Yb1 N2 81.0(3) . 7_545 ?
N7 Yb1 N4 84.3(3) . 7_545 ?
N7 Yb1 N4 79.9(2) 7_545 7_545 ?
N2 Yb1 N4 82.4(2) . 7_545 ?
N2 Yb1 N4 128.4(2) 7_545 7_545 ?
N7 Yb1 N4 79.9(2) . . ?
N7 Yb1 N4 84.3(3) 7_545 . ?
N2 Yb1 N4 128.4(2) . . ?
N2 Yb1 N4 82.4(2) 7_545 . ?
N4 Yb1 N4 142.6(3) 7_545 . ?
N7 Yb1 N6 64.55(16) . . ?
N7 Yb1 N6 64.56(16) 7_545 . ?
N2 Yb1 N6 139.49(15) . . ?
N2 Yb1 N6 139.49(15) 7_545 . ?
N4 Yb1 N6 71.28(15) 7_545 . ?
N4 Yb1 N6 71.28(15) . . ?
N7 Yb1 N1 71.6(2) . 7_545 ?
N7 Yb1 N1 137.4(2) 7_545 7_545 ?
N2 Yb1 N1 72.2(2) . 7_545 ?
N2 Yb1 N1 64.1(2) 7_545 7_545 ?
N4 Yb1 N1 64.3(2) 7_545 7_545 ?
N4 Yb1 N1 138.4(2) . 7_545 ?
N6 Yb1 N1 119.22(15) . 7_545 ?
N7 Yb1 N1 137.4(2) . . ?
N7 Yb1 N1 71.6(2) 7_545 . ?
N2 Yb1 N1 64.1(2) . . ?
N2 Yb1 N1 72.2(2) 7_545 . ?
N4 Yb1 N1 138.4(2) 7_545 . ?
N4 Yb1 N1 64.3(2) . . ?
N6 Yb1 N1 119.22(15) . . ?
N1 Yb1 N1 121.6(3) 7_545 . ?
C1 N1 C5 118.2(7) . . ?
C1 N1 Yb1 120.6(6) . . ?
C5 N1 Yb1 120.9(5) . . ?
C6 N2 C7 104.9(7) . . ?
C6 N2 Yb1 122.4(5) . . ?
C7 N2 Yb1 132.7(5) . . ?
C8 N3 C6 106.5(7) . . ?
C8 N3 C9 123.6(8) . . ?
C6 N3 C9 129.9(8) . . ?
C10 N4 C11 107.0(7) . . ?
C10 N4 Yb1 120.0(6) . . ?
C11 N4 Yb1 131.5(6) . . ?
C10 N5 C12 108.3(7) . . ?
C10 N5 C13 129.4(8) . . ?
C12 N5 C13 122.3(8) . . ?
C14 N6 C14 119.2(9) . 7_545 ?
C14 N6 Yb1 120.4(5) . . ?
C14 N6 Yb1 120.4(5) 7_545 . ?
C17 N7 C18 106.9(8) . . ?
C17 N7 Yb1 121.2(6) . . ?
C18 N7 Yb1 131.5(6) . . ?
C19 N8 C17 107.1(8) . . ?
C19 N8 C20 123.0(9) . . ?
C17 N8 C20 129.9(10) . . ?
N1 C1 C2 122.4(8) . . ?
N1 C1 C6 111.5(8) . . ?
C2 C1 C6 126.2(8) . . ?
C3 C2 C1 118.9(8) . . ?
C3 C2 H2A 120.6 . . ?
C1 C2 H2A 120.6 . . ?
C2 C3 C4 120.2(9) . . ?
C2 C3 H3A 119.9 . . ?
C4 C3 H3A 119.9 . . ?
C5 C4 C3 116.2(9) . . ?
C5 C4 H4A 108.2 . . ?
C3 C4 H4A 108.2 . . ?
C5 C4 H4B 108.2 . . ?
C3 C4 H4B 108.2 . . ?
H4A C4 H4B 107.4 . . ?
N1 C5 C4 124.1(8) . . ?
N1 C5 C10 112.5(7) . . ?
C4 C5 C10 123.4(8) . . ?
N2 C6 N3 111.0(8) . . ?
N2 C6 C1 120.9(7) . . ?
N3 C6 C1 128.0(8) . . ?
C8 C7 N2 110.2(8) . . ?
C8 C7 H7A 124.9 . . ?
N2 C7 H7A 124.9 . . ?
N3 C8 C7 107.3(8) . . ?
N3 C8 H8A 126.3 . . ?
C7 C8 H8A 126.3 . . ?
N3 C9 H9A 109.5 . . ?
N3 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
N3 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
N4 C10 N5 108.8(7) . . ?
N4 C10 C5 120.7(8) . . ?
N5 C10 C5 130.5(8) . . ?
C12 C11 N4 108.5(8) . . ?
C12 C11 H11A 125.7 . . ?
N4 C11 H11A 125.7 . . ?
C11 C12 N5 107.4(8) . . ?
C11 C12 H12A 126.3 . . ?
N5 C12 H12A 126.3 . . ?
N5 C13 H13A 109.5 . . ?
N5 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
N5 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
N6 C14 C15 120.0(9) . . ?
N6 C14 C17 112.0(7) . . ?
C15 C14 C17 127.9(9) . . ?
C16 C15 C14 120.4(10) . . ?
C16 C15 H15A 119.8 . . ?
C14 C15 H15A 119.8 . . ?
C15 C16 C15 120.0(12) 7_545 . ?
C15 C16 H16A 120.0 7_545 . ?
C15 C16 H16A 120.0 . . ?
N7 C17 N8 110.6(8) . . ?
N7 C17 C14 120.8(8) . . ?
N8 C17 C14 128.4(8) . . ?
C19 C18 N7 107.9(9) . . ?
C19 C18 H18A 126.0 . . ?
N7 C18 H18A 126.0 . . ?
C18 C19 N8 107.5(9) . . ?
C18 C19 H19A 126.2 . . ?
N8 C19 H19A 126.2 . . ?
N8 C20 H20A 109.5 . . ?
N8 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
N8 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
O1S Cl1 O1S 116.6(13) 4_556 . ?
O1S Cl1 O2S 108.1(9) 4_556 . ?
O1S Cl1 O2S 105.2(8) . . ?
O1S Cl1 O2S 105.2(8) 4_556 4_556 ?
O1S Cl1 O2S 108.1(9) . 4_556 ?
O2S Cl1 O2S 114.0(10) . 4_556 ?
O3S Cl2 O4S 110.5(5) . . ?
O3S Cl2 O4S 110.5(5) . 12_655 ?
O4S Cl2 O4S 108.7(9) . 12_655 ?
O3S Cl2 O5S 109.1(7) . . ?
O4S Cl2 O5S 109.0(5) . . ?
O4S Cl2 O5S 109.0(5) 12_655 . ?
O7S' Cl3 O8S 119.8(11) . . ?
O7S' Cl3 O8S 119.8(11) 12_655 . ?
O7S' Cl3 O6S 117.9(9) . . ?
O7S' Cl3 O6S 117.9(9) 12_655 . ?
O8S Cl3 O6S 115.1(9) . . ?
O8S Cl3 O7S 85.0(8) . . ?
O6S Cl3 O7S 99.3(6) . . ?
O8S Cl3 O7S 85.0(8) . 12_655 ?
O6S Cl3 O7S 99.3(6) . 12_655 ?
O7S Cl3 O7S 161.3(12) . 12_655 ?
O7S' O7S' Cl3 64.0(10) 12_655 . ?
C2S C1S H1SB 112.1 . . ?
C2S C1S H1SA 98.6 . . ?
H1SB C1S H1SA 112.0 . . ?
C2S C1S H1SB 112.1(4) . 12_655 ?
H1SB C1S H1SB 109.7 . 12_655 ?
H1SA C1S H1SB 112.0 . 12_655 ?
N1S C2S C1S 178.1(15) . . ?
H1WC O1W H1WA 109.9 . . ?
H1WC O1W H1WC 108.3 . 12_655 ?
H1WA O1W H1WC 109.9 . 12_655 ?
C4S C3S N3S 173(3) . . ?
C3S C4S H4SA 109.1 . . ?
C3S C4S H4SB 109.7 . . ?
H4SA C4S H4SB 109.5 . . ?
C3S C4S H4SB 109.7(9) . 12_655 ?
H4SA C4S H4SB 109.5 . 12_655 ?
H4SB C4S H4SB 109.5 . 12_655 ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O1W H1WA O5S 0.85 2.04 2.887(16) 179.1 .

_refine_diff_density_max         1.534
_refine_diff_density_min         -1.435



####################################################################### 
# 
# 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_dy
_database_code_depnum_ccdc_archive 'CCDC 2095655'
loop_
_audit_author_name
_audit_author_address
'Konstantin Lyssenko'
;Chemical Department MSU
Russia
;
_audit_update_record             
;
2021-07-10 deposited with the CCDC.	2022-04-12 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2016/6
_shelx_SHELXL_version_number     2016/6
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C39 H41 Dy N15, 3(Cl O4), 2(C2 H2 N), H2 O'
_chemical_formula_sum            'C43 H47 Cl3 Dy N17 O13'
_chemical_formula_weight         1278.82

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Dy Dy -0.1892 4.4098 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           64
_space_group_name_H-M_alt        'C m c a'
_space_group_name_Hall           '-C 2bc 2'

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

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

_cell_length_a                   20.8878(4)
_cell_length_b                   21.4260(4)
_cell_length_c                   22.7165(5)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     10166.6(4)
_cell_formula_units_Z            8
_cell_measurement_temperature    120(2)
_cell_measurement_reflns_used    1594
_cell_measurement_theta_min      3
_cell_measurement_theta_max      25

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.671
_exptl_crystal_F_000             5160
_exptl_transmission_factor_min   0.431
_exptl_transmission_factor_max   0.594
_exptl_crystal_size_max          0.485
_exptl_crystal_size_mid          0.401
_exptl_crystal_size_min          0.345
_exptl_absorpt_coefficient_mu    1.709
_shelx_estimated_absorpt_T_min   0.491
_shelx_estimated_absorpt_T_max   0.590
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   SADABS
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      120(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  "Bruker APEX II CCD area detector'"
_diffrn_measurement_method       'omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            67068
_diffrn_reflns_av_unetI/netI     0.0484
_diffrn_reflns_av_R_equivalents  0.1208
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_theta_min         1.630
_diffrn_reflns_theta_max         28.997
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             6939
_reflns_number_gt                5308
_reflns_threshold_expression     I>2σ(I)
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'Bruker APEX II'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0577P)²+50.0312P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         6939
_refine_ls_number_parameters     381
_refine_ls_number_restraints     36
_refine_ls_R_factor_all          0.0561
_refine_ls_R_factor_gt           0.0435
_refine_ls_wR_factor_ref         0.1260
_refine_ls_wR_factor_gt          0.1180
_refine_ls_goodness_of_fit_ref   1.067
_refine_ls_restrained_S_all      1.091
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

# start Validation Reply Form
_vrf_PLAT420_a                   
;
PROBLEM: D-H Without Acceptor       O1W      --H1WC     .     Please Check 
RESPONSE: Two atoms (O1w and H1wa) of the water molecule occupy the 
special position (mirror plane). While H1wc is in the general position 
with the occupancy 0.5.   As the consequence of the disorder as well 
as disorder of ClO4 anion it was impossible to locate hydrogen atoms which
all participate in the formation of H-bonds

;
# end Validation Reply Form


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 0.250000 0.32082(2) 0.250000 0.01431(8) Uani 1 2 d S T P . .
N1 N 0.26302(14) 0.26102(14) 0.34958(14) 0.0210(6) Uani 1 1 d . . . . .
N2 N 0.17588(15) 0.23271(14) 0.26771(15) 0.0227(6) Uani 1 1 d . . . . .
N3 N 0.13524(16) 0.15063(15) 0.31363(17) 0.0315(8) Uani 1 1 d . . . . .
N4 N 0.33739(14) 0.35673(14) 0.31488(13) 0.0210(6) Uani 1 1 d . . . . .
N5 N 0.38248(17) 0.37206(17) 0.40189(15) 0.0322(8) Uani 1 1 d . . . . .
N6 N 0.250000 0.4415(2) 0.250000 0.0228(9) Uani 1 2 d S T P . .
N7 N 0.32019(15) 0.37080(14) 0.17681(13) 0.0244(6) Uani 1 1 d . . . . .
N8 N 0.3549(2) 0.44804(19) 0.12086(16) 0.0412(10) Uani 1 1 d . . . . .
C1 C 0.22876(19) 0.20877(18) 0.36051(17) 0.0259(8) Uani 1 1 d . . . . .
C2 C 0.2403(2) 0.1715(2) 0.4099(2) 0.0361(10) Uani 1 1 d . . . . .
H2A H 0.216477 0.134392 0.416506 0.043 Uiso 1 1 calc R U . . .
C3 C 0.2874(3) 0.1902(2) 0.4490(2) 0.0442(12) Uani 1 1 d . . . . .
H3A H 0.296167 0.165753 0.482907 0.053 Uiso 1 1 calc R U . . .
C4 C 0.3220(2) 0.2446(2) 0.43887(18) 0.0364(10) Uani 1 1 d . . . . .
H4A H 0.315771 0.272444 0.473205 0.044 Uiso 1 1 calc R U . . .
H4B H 0.367995 0.233461 0.437702 0.044 Uiso 1 1 calc R U . . .
C5 C 0.30827(17) 0.27879(17) 0.38841(16) 0.0243(7) Uani 1 1 d . . . . .
C6 C 0.18045(17) 0.19666(16) 0.31527(18) 0.0244(7) Uani 1 1 d . . . . .
C7 C 0.12652(19) 0.20912(19) 0.2345(2) 0.0291(8) Uani 1 1 d . . . . .
H7A H 0.112244 0.225252 0.197848 0.035 Uiso 1 1 calc R U . . .
C8 C 0.1013(2) 0.1584(2) 0.2632(2) 0.0361(10) Uani 1 1 d . . . . .
H8A H 0.066505 0.133321 0.250136 0.043 Uiso 1 1 calc R U . . .
C9 C 0.1220(2) 0.1006(2) 0.3563(3) 0.0486(13) Uani 1 1 d . . . . .
H9A H 0.082460 0.079031 0.345296 0.073 Uiso 1 1 calc R U . . .
H9B H 0.117194 0.118722 0.395709 0.073 Uiso 1 1 calc R U . . .
H9C H 0.157645 0.070862 0.356444 0.073 Uiso 1 1 calc R U . . .
C10 C 0.34225(17) 0.33555(18) 0.36980(16) 0.0236(7) Uani 1 1 d . . . . .
C11 C 0.37650(17) 0.40813(18) 0.31151(18) 0.0259(8) Uani 1 1 d . . . . .
H11A H 0.383098 0.432851 0.277323 0.031 Uiso 1 1 calc R U . . .
C12 C 0.4043(2) 0.4180(2) 0.36480(19) 0.0321(9) Uani 1 1 d . . . . .
H12A H 0.433239 0.450611 0.374564 0.039 Uiso 1 1 calc R U . . .
C13 C 0.4033(3) 0.3661(3) 0.4629(2) 0.0604(16) Uani 1 1 d . . . . .
H13A H 0.365926 0.359380 0.488247 0.091 Uiso 1 1 calc R U . . .
H13B H 0.425433 0.404287 0.475020 0.091 Uiso 1 1 calc R U . . .
H13C H 0.432498 0.330461 0.466524 0.091 Uiso 1 1 calc R U . . .
C14 C 0.2822(2) 0.47300(17) 0.20828(18) 0.0287(8) Uani 1 1 d . . . . .
C15 C 0.2827(2) 0.53848(19) 0.2069(2) 0.0423(12) Uani 1 1 d . . . . .
H15A H 0.305069 0.560369 0.176950 0.051 Uiso 1 1 calc R U . . .
C16 C 0.250000 0.5701(3) 0.250000 0.047(2) Uani 1 2 d S T P . .
H16A H 0.249998 0.614425 0.249999 0.057 Uiso 1 2 calc R U P . .
C17 C 0.3179(2) 0.43248(18) 0.16794(17) 0.0283(9) Uani 1 1 d . . . . .
C18 C 0.3600(2) 0.3470(2) 0.13476(17) 0.0324(9) Uani 1 1 d . . . . .
H18A H 0.370785 0.304140 0.130324 0.039 Uiso 1 1 calc R U . . .
C19 C 0.3818(3) 0.3943(3) 0.1002(2) 0.0468(13) Uani 1 1 d . . . . .
H19A H 0.410288 0.390691 0.067810 0.056 Uiso 1 1 calc R U . . .
C20 C 0.3681(3) 0.5093(3) 0.0941(2) 0.0662(19) Uani 1 1 d . . . . .
H20A H 0.327661 0.528737 0.081999 0.099 Uiso 1 1 calc R U . . .
H20B H 0.395697 0.503884 0.059645 0.099 Uiso 1 1 calc R U . . .
H20C H 0.389557 0.536164 0.122922 0.099 Uiso 1 1 calc R U . . .
Cl1 Cl 0.21171(11) 0.000000 0.500000 0.0558(5) Uani 1 2 d S T P . .
Cl2 Cl 0.500000 0.27845(8) 0.57800(7) 0.0394(3) Uani 1 2 d S T P . .
Cl3 Cl 0.500000 -0.01604(6) 0.71956(7) 0.0319(3) Uani 1 2 d S T P . .
O1S O 0.1822(4) 0.0140(4) 0.4509(4) 0.151(3) Uani 1 1 d . U . . .
O2S O 0.2479(3) 0.0540(3) 0.5104(5) 0.123(3) Uani 1 1 d . . . . .
O3S O 0.500000 0.2695(4) 0.6389(2) 0.102(3) Uani 1 2 d S T P . .
O4S O 0.4452(3) 0.2499(2) 0.5522(2) 0.0884(15) Uani 1 1 d . U . . .
O5S O 0.500000 0.3446(2) 0.5641(2) 0.0441(11) Uani 1 2 d S T P . .
O6S O 0.500000 -0.0727(2) 0.6852(3) 0.0649(18) Uani 1 2 d S T P A .
O7S O 0.5691(3) -0.0082(4) 0.7233(4) 0.059(2) Uani 0.5 1 d . . P A 1
O7S' O 0.5315(5) 0.0348(4) 0.6946(4) 0.084(3) Uani 0.5 1 d . . P A 2
O8S O 0.500000 -0.0249(4) 0.7805(4) 0.110(3) Uani 1 2 d S TU P A .
C1S C 0.500000 0.1759(4) 0.7446(3) 0.047(2) Uani 1 2 d S T P . .
H1SB H 0.537320 0.189753 0.723925 0.057 Uiso 0.5 1 d R U P . .
H1SA H 0.500000 0.131323 0.750805 0.057 Uiso 1 2 d R U P . .
N1S N 0.500000 0.2132(3) 0.8525(3) 0.0506(15) Uani 1 2 d S T P . .
C2S C 0.500000 0.1963(3) 0.8055(3) 0.0384(15) Uani 1 2 d S T P . .
O1W O 0.500000 0.4817(3) 0.5560(4) 0.111(3) Uani 1 2 d S T P . .
H1WC H 0.532760 0.495920 0.573422 0.134 Uiso 0.5 1 d R U P . .
H1WA H 0.500000 0.441780 0.557272 0.134 Uiso 1 2 d R U P . .
C3S C 0.500000 0.6167(7) 0.0412(5) 0.079(3) Uani 1 2 d S TU P . .
N3S N 0.500000 0.6618(7) 0.0729(7) 0.177(7) Uani 1 2 d S TU P . .
C4S C 0.500000 0.5728(6) 0.0102(5) 0.084(3) Uani 1 2 d S TU P . .
H4SA H 0.500000 0.582041 -0.031348 0.126 Uiso 1 2 d R U P . .
H4SB H 0.537270 0.548911 0.019912 0.126 Uiso 0.5 1 d R U P . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Dy1 N7 2.462(3) . ?
Dy1 N7 2.462(3) 7_545 ?
Dy1 N4 2.469(3) 7_545 ?
Dy1 N4 2.469(3) . ?
Dy1 N2 2.474(3) . ?
Dy1 N2 2.474(3) 7_545 ?
Dy1 N6 2.586(5) . ?
Dy1 N1 2.614(3) 7_545 ?
Dy1 N1 2.614(3) . ?
N1 C5 1.348(5) . ?
N1 C1 1.352(5) . ?
N2 C6 1.332(5) . ?
N2 C7 1.374(5) . ?
N3 C8 1.358(6) . ?
N3 C6 1.366(5) . ?
N3 C9 1.471(5) . ?
N4 C10 1.331(5) . ?
N4 C11 1.373(5) . ?
N5 C10 1.360(5) . ?
N5 C12 1.374(6) . ?
N5 C13 1.459(5) . ?
N6 C14 1.343(5) . ?
N6 C14 1.344(5) 7_545 ?
N7 C17 1.338(5) . ?
N7 C18 1.366(5) . ?
N8 C17 1.361(5) . ?
N8 C19 1.363(7) . ?
N8 C20 1.473(6) . ?
C1 C2 1.398(6) . ?
C1 C6 1.463(6) . ?
C2 C3 1.384(7) . ?
C2 H2A 0.9500 . ?
C3 C4 1.391(7) . ?
C3 H3A 0.9500 . ?
C4 C5 1.390(5) . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C5 C10 1.470(5) . ?
C7 C8 1.373(6) . ?
C7 H7A 0.9500 . ?
C8 H8A 0.9500 . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C11 C12 1.359(6) . ?
C11 H11A 0.9500 . ?
C12 H12A 0.9500 . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C14 C15 1.403(5) . ?
C14 C17 1.466(6) . ?
C15 C16 1.372(6) . ?
C15 H15A 0.9500 . ?
C16 H16A 0.9500 . ?
C18 C19 1.362(6) . ?
C18 H18A 0.9500 . ?
C19 H19A 0.9500 . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
Cl1 O1S 1.310(9) 4_556 ?
Cl1 O1S 1.310(9) . ?
Cl1 O2S 1.403(6) . ?
Cl1 O2S 1.403(6) 4_556 ?
Cl2 O3S 1.396(6) . ?
Cl2 O4S 1.424(5) . ?
Cl2 O4S 1.424(5) 12_655 ?
Cl2 O5S 1.453(5) . ?
Cl3 O7S' 1.392(7) . ?
Cl3 O7S' 1.392(7) 12_655 ?
Cl3 O8S 1.398(10) . ?
Cl3 O6S 1.444(5) . ?
Cl3 O7S 1.457(6) . ?
Cl3 O7S 1.457(6) 12_655 ?
O7S' O7S' 1.31(2) 12_655 ?
C1S C2S 1.450(10) . ?
C1S H1SB 0.9571 . ?
C1S H1SA 0.9661 . ?
C1S H1SB 0.9572 12_655 ?
N1S C2S 1.128(9) . ?
O1W H1WC 0.8477 . ?
O1W H1WA 0.8556 . ?
O1W H1WC 0.8477 12_655 ?
C3S C4S 1.176(16) . ?
C3S N3S 1.203(18) . ?
C4S H4SA 0.9635 . ?
C4S H4SB 0.9577 . ?
C4S H4SB 0.9576 12_655 ?

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
N7 Dy1 N7 128.44(15) . 7_545 ?
N7 Dy1 N4 84.36(11) . 7_545 ?
N7 Dy1 N4 80.05(10) 7_545 7_545 ?
N7 Dy1 N4 80.05(10) . . ?
N7 Dy1 N4 84.36(11) 7_545 . ?
N4 Dy1 N4 143.69(14) 7_545 . ?
N7 Dy1 N2 144.52(10) . . ?
N7 Dy1 N2 81.34(11) 7_545 . ?
N4 Dy1 N2 82.66(10) 7_545 . ?
N4 Dy1 N2 127.10(10) . . ?
N7 Dy1 N2 81.34(11) . 7_545 ?
N7 Dy1 N2 144.52(10) 7_545 7_545 ?
N4 Dy1 N2 127.10(10) 7_545 7_545 ?
N4 Dy1 N2 82.66(10) . 7_545 ?
N2 Dy1 N2 80.55(14) . 7_545 ?
N7 Dy1 N6 64.22(7) . . ?
N7 Dy1 N6 64.22(7) 7_545 . ?
N4 Dy1 N6 71.84(7) 7_545 . ?
N4 Dy1 N6 71.84(7) . . ?
N2 Dy1 N6 139.72(7) . . ?
N2 Dy1 N6 139.72(7) 7_545 . ?
N7 Dy1 N1 71.99(10) . 7_545 ?
N7 Dy1 N1 137.36(10) 7_545 7_545 ?
N4 Dy1 N1 63.85(10) 7_545 7_545 ?
N4 Dy1 N1 138.27(9) . 7_545 ?
N2 Dy1 N1 72.64(10) . 7_545 ?
N2 Dy1 N1 63.28(10) 7_545 7_545 ?
N6 Dy1 N1 119.35(7) . 7_545 ?
N7 Dy1 N1 137.37(10) . . ?
N7 Dy1 N1 71.98(10) 7_545 . ?
N4 Dy1 N1 138.26(9) 7_545 . ?
N4 Dy1 N1 63.85(10) . . ?
N2 Dy1 N1 63.28(10) . . ?
N2 Dy1 N1 72.64(10) 7_545 . ?
N6 Dy1 N1 119.35(7) . . ?
N1 Dy1 N1 121.30(14) 7_545 . ?
C5 N1 C1 119.0(3) . . ?
C5 N1 Dy1 120.1(2) . . ?
C1 N1 Dy1 120.7(3) . . ?
C6 N2 C7 106.6(3) . . ?
C6 N2 Dy1 122.0(2) . . ?
C7 N2 Dy1 131.4(3) . . ?
C8 N3 C6 107.2(3) . . ?
C8 N3 C9 123.2(4) . . ?
C6 N3 C9 129.6(4) . . ?
C10 N4 C11 106.3(3) . . ?
C10 N4 Dy1 120.6(2) . . ?
C11 N4 Dy1 131.0(2) . . ?
C10 N5 C12 106.8(3) . . ?
C10 N5 C13 130.0(4) . . ?
C12 N5 C13 123.2(4) . . ?
C14 N6 C14 119.8(5) . 7_545 ?
C14 N6 Dy1 120.1(2) . . ?
C14 N6 Dy1 120.1(2) 7_545 . ?
C17 N7 C18 106.6(3) . . ?
C17 N7 Dy1 120.7(3) . . ?
C18 N7 Dy1 132.2(3) . . ?
C17 N8 C19 107.3(4) . . ?
C17 N8 C20 130.4(5) . . ?
C19 N8 C20 122.2(4) . . ?
N1 C1 C2 121.9(4) . . ?
N1 C1 C6 112.5(3) . . ?
C2 C1 C6 125.5(4) . . ?
C3 C2 C1 118.1(4) . . ?
C3 C2 H2A 120.9 . . ?
C1 C2 H2A 120.9 . . ?
C2 C3 C4 120.4(4) . . ?
C2 C3 H3A 119.8 . . ?
C4 C3 H3A 119.8 . . ?
C5 C4 C3 118.0(4) . . ?
C5 C4 H4A 107.8 . . ?
C3 C4 H4A 107.8 . . ?
C5 C4 H4B 107.8 . . ?
C3 C4 H4B 107.8 . . ?
H4A C4 H4B 107.1 . . ?
N1 C5 C4 122.4(4) . . ?
N1 C5 C10 112.6(3) . . ?
C4 C5 C10 124.9(4) . . ?
N2 C6 N3 110.3(4) . . ?
N2 C6 C1 121.1(3) . . ?
N3 C6 C1 128.6(3) . . ?
C8 C7 N2 108.7(4) . . ?
C8 C7 H7A 125.7 . . ?
N2 C7 H7A 125.7 . . ?
N3 C8 C7 107.2(4) . . ?
N3 C8 H8A 126.4 . . ?
C7 C8 H8A 126.4 . . ?
N3 C9 H9A 109.5 . . ?
N3 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
N3 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
N4 C10 N5 110.7(3) . . ?
N4 C10 C5 121.0(3) . . ?
N5 C10 C5 128.3(3) . . ?
C12 C11 N4 109.2(4) . . ?
C12 C11 H11A 125.4 . . ?
N4 C11 H11A 125.4 . . ?
C11 C12 N5 107.0(4) . . ?
C11 C12 H12A 126.5 . . ?
N5 C12 H12A 126.5 . . ?
N5 C13 H13A 109.5 . . ?
N5 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
N5 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
N6 C14 C15 121.4(4) . . ?
N6 C14 C17 113.5(3) . . ?
C15 C14 C17 125.1(4) . . ?
C16 C15 C14 118.3(5) . . ?
C16 C15 H15A 120.8 . . ?
C14 C15 H15A 120.8 . . ?
C15 C16 C15 120.8(5) 7_545 . ?
C15 C16 H16A 119.6 7_545 . ?
C15 C16 H16A 119.6 . . ?
N7 C17 N8 109.9(4) . . ?
N7 C17 C14 120.6(3) . . ?
N8 C17 C14 129.4(4) . . ?
C19 C18 N7 109.1(4) . . ?
C19 C18 H18A 125.4 . . ?
N7 C18 H18A 125.4 . . ?
C18 C19 N8 107.1(4) . . ?
C18 C19 H19A 126.5 . . ?
N8 C19 H19A 126.5 . . ?
N8 C20 H20A 109.5 . . ?
N8 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
N8 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
O1S Cl1 O1S 123.8(8) 4_556 . ?
O1S Cl1 O2S 107.4(6) 4_556 . ?
O1S Cl1 O2S 102.0(5) . . ?
O1S Cl1 O2S 102.0(5) 4_556 4_556 ?
O1S Cl1 O2S 107.4(6) . 4_556 ?
O2S Cl1 O2S 114.8(6) . 4_556 ?
O3S Cl2 O4S 110.4(3) . . ?
O3S Cl2 O4S 110.4(3) . 12_655 ?
O4S Cl2 O4S 107.1(5) . 12_655 ?
O3S Cl2 O5S 110.4(4) . . ?
O4S Cl2 O5S 109.2(2) . . ?
O4S Cl2 O5S 109.2(2) 12_655 . ?
O7S' Cl3 O8S 120.6(5) . . ?
O7S' Cl3 O8S 120.6(5) 12_655 . ?
O7S' Cl3 O6S 116.0(4) . . ?
O7S' Cl3 O6S 116.0(4) 12_655 . ?
O8S Cl3 O6S 114.9(4) . . ?
O8S Cl3 O7S 87.6(4) . . ?
O6S Cl3 O7S 97.4(3) . . ?
O8S Cl3 O7S 87.6(4) . 12_655 ?
O6S Cl3 O7S 97.4(3) . 12_655 ?
O7S Cl3 O7S 165.1(6) . 12_655 ?
O7S' O7S' Cl3 61.8(5) 12_655 . ?
C2S C1S H1SB 112.0 . . ?
C2S C1S H1SA 99.1 . . ?
H1SB C1S H1SA 112.2 . . ?
C2S C1S H1SB 112.02(19) . 12_655 ?
H1SB C1S H1SB 109.1 . 12_655 ?
H1SA C1S H1SB 112.2 . 12_655 ?
N1S C2S C1S 178.8(7) . . ?
H1WC O1W H1WA 110.1 . . ?
H1WC O1W H1WC 107.7 . 12_655 ?
H1WA O1W H1WC 110.1 . 12_655 ?
C4S C3S N3S 179.8(13) . . ?
C3S C4S H4SA 115.0 . . ?
C3S C4S H4SB 106.8 . . ?
H4SA C4S H4SB 109.6 . . ?
C3S C4S H4SB 106.8(4) . 12_655 ?
H4SA C4S H4SB 109.6 . 12_655 ?
H4SB C4S H4SB 108.8 . 12_655 ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O1W H1WA O5S 0.86 2.09 2.942(9) 177.7 .

_refine_diff_density_max         1.973
_refine_diff_density_min         -1.922
_refine_diff_density_rms         0.148



