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

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_296
_database_code_depnum_ccdc_archive 'CCDC 2011007'
loop_
_audit_author_name
_audit_author_address
'Berthold Kersting'
;Universitaet Leipzig
Germany
;
_audit_update_record             
;
2020-06-20 deposited with the CCDC.	2020-07-17 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C76 H64 N6 O8 Tb2'
_chemical_formula_weight         1507.17


# start Validation Reply Form
_vrf_RINTA01_296                 
;
PROBLEM: The value of Rint is greater than 0.18
RESPONSE: Crystal quality low due to disordered solvate molecules 
;

_vrf_PLAT020_296                 
;
PROBLEM: 
The Value of Rint is Greater Than 0.12 .........      0.198 Report
RESPONSE: As above
;
_vrf_PLAT601_296                 
;
PROBLEM: Structure Contains Solvent Accessible VOIDS of .        116 Ang**3
RESPONSE: The structure contains two heavily disordered MeCN solvate molecules 
(per dinuclear formula unit) and all attempts to model this disorder failed. The corresponding 
electron density was removed from the structure (and the corresponding F0) 
with the SQUEEZE algorithm implemented in the PLATON program suite. 
The SQUEEZE routine revealed total potential solvent area of 4 x 115 Ang3 per 
unit cell corresponding to approximately two MeCN solvate molecules per formula 
unit. 
;
# end Validation Reply Form


loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Tb Tb -9.1472 9.1891 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           56
_space_group_name_H-M_alt        'P c c n'
_space_group_name_Hall           '-P 2ab 2ac'




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

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

_cell_length_a                   17.0267(5)
_cell_length_b                   16.8322(5)
_cell_length_c                   22.5364(8)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     6458.9(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    180(2)
_cell_measurement_reflns_used    25572
_cell_measurement_theta_min      7.39
_cell_measurement_theta_max      141.73

_exptl_crystal_description       block
_exptl_crystal_colour            gold-yellow
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.550
_exptl_crystal_F_000             3024
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.150
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.100
_exptl_absorpt_coefficient_mu    11.132
_shelx_estimated_absorpt_T_min   0.286
_shelx_estimated_absorpt_T_max   0.402
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_correction_T_min  0.31
_exptl_absorpt_correction_T_max  0.42
_exptl_absorpt_process_details   
;
Busing, W. R. & Levy, H. A. (1957) Acta Cryst. 10, 180-182. 
and Coppens, P., Leiserowitz, L. & Rabinovich, D. (1965) 
Acta Cryst. 1965, 1035-1038.
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      180(2)
_diffrn_radiation_wavelength     1.54186
_diffrn_radiation_type           CuK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Stoe stadivari'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            69266
_diffrn_reflns_av_unetI/netI     0.0815
_diffrn_reflns_av_R_equivalents  0.1975
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         3.693
_diffrn_reflns_theta_max         69.994
_diffrn_reflns_theta_full        67.686
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             6114
_reflns_number_gt                4157
_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       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_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)+(0.1034P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         6114
_refine_ls_number_parameters     416
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1051
_refine_ls_R_factor_gt           0.0719
_refine_ls_wR_factor_ref         0.1835
_refine_ls_wR_factor_gt          0.1647
_refine_ls_goodness_of_fit_ref   1.066
_refine_ls_restrained_S_all      1.066
_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
C1 C 0.5614(6) 0.4198(5) 0.6097(6) 0.087(4) Uani 1 1 d . . . . .
C2 C 0.5519(6) 0.4231(6) 0.5429(5) 0.092(4) Uani 1 1 d . . . . .
H2A H 0.499250 0.444520 0.533339 0.110 Uiso 1 1 calc R U . . .
H2B H 0.591500 0.459894 0.526253 0.110 Uiso 1 1 calc R U . . .
C3 C 0.5611(6) 0.3427(6) 0.5139(5) 0.076(3) Uani 1 1 d . . . . .
C4 C 0.6314(6) 0.3135(7) 0.4879(6) 0.093(4) Uani 1 1 d . . . . .
H4 H 0.676720 0.346377 0.487578 0.111 Uiso 1 1 calc R U . . .
C5 C 0.6356(7) 0.2403(7) 0.4637(5) 0.093(3) Uani 1 1 d . . . . .
H5 H 0.683846 0.221342 0.447979 0.111 Uiso 1 1 calc R U . . .
C6 C 0.5698(5) 0.1934(7) 0.4619(4) 0.075(3) Uani 1 1 d . . . . .
H6 H 0.572250 0.143099 0.442883 0.090 Uiso 1 1 calc R U . . .
C7 C 0.4997(5) 0.2178(5) 0.4873(3) 0.056(2) Uani 1 1 d . . . . .
C8 C 0.4290(5) 0.1648(5) 0.4896(3) 0.060(2) Uani 1 1 d . . . . .
H8A H 0.432591 0.124405 0.457809 0.072 Uiso 1 1 calc R U . . .
H8B H 0.381051 0.196780 0.482651 0.072 Uiso 1 1 calc R U . . .
C9 C 0.4230(4) 0.1240(4) 0.5489(3) 0.0469(17) Uani 1 1 d . . . . .
C10 C 0.4774(5) 0.0653(4) 0.5607(4) 0.0554(19) Uani 1 1 d . . . . .
H10 H 0.513883 0.050929 0.530654 0.066 Uiso 1 1 calc R U . . .
C11 C 0.4807(5) 0.0268(4) 0.6145(4) 0.058(2) Uani 1 1 d . . . . .
H11 H 0.516376 -0.015824 0.620594 0.069 Uiso 1 1 calc R U . . .
C12 C 0.4312(5) 0.0513(4) 0.6598(4) 0.0544(19) Uani 1 1 d . . . . .
H12 H 0.436397 0.028117 0.697992 0.065 Uiso 1 1 calc R U . . .
C13 C 0.3740(4) 0.1091(4) 0.6505(3) 0.0411(15) Uani 1 1 d . . . . .
C14 C 0.3254(4) 0.1341(4) 0.7033(3) 0.0421(15) Uani 1 1 d . . . . .
H14A H 0.277981 0.162448 0.689157 0.051 Uiso 1 1 calc R U . . .
H14B H 0.307900 0.086194 0.725072 0.051 Uiso 1 1 calc R U . . .
C15 C 0.3702(5) 0.1871(4) 0.7448(3) 0.0470(17) Uani 1 1 d . . . . .
C16 C 0.4014(5) 0.1576(5) 0.7986(3) 0.060(2) Uani 1 1 d . . . . .
H16 H 0.393936 0.103239 0.808464 0.072 Uiso 1 1 calc R U . . .
C17 C 0.4424(6) 0.2057(6) 0.8370(4) 0.071(3) Uani 1 1 d . . . . .
H17 H 0.462765 0.184533 0.872888 0.085 Uiso 1 1 calc R U . . .
C18 C 0.4541(6) 0.2858(6) 0.8230(4) 0.076(3) Uani 1 1 d . . . . .
H18 H 0.481966 0.319064 0.849813 0.091 Uiso 1 1 calc R U . . .
C19 C 0.4254(5) 0.3171(5) 0.7707(4) 0.060(2) Uani 1 1 d . . . . .
C20 C 0.4388(6) 0.4039(5) 0.7528(4) 0.075(3) Uani 1 1 d . . . . .
H20A H 0.391228 0.424907 0.733097 0.090 Uiso 1 1 calc R U . . .
H20B H 0.448889 0.436232 0.788704 0.090 Uiso 1 1 calc R U . . .
C21 C 0.5079(5) 0.4099(4) 0.7113(5) 0.065(2) Uani 1 1 d . . . . .
C22 C 0.5851(7) 0.3957(5) 0.7330(6) 0.087(3) Uani 1 1 d . . . . .
H22 H 0.593361 0.384463 0.773820 0.104 Uiso 1 1 calc R U . . .
C23 C 0.6482(7) 0.3985(6) 0.6940(7) 0.095(4) Uani 1 1 d . . . . .
H23 H 0.700037 0.393016 0.708990 0.114 Uiso 1 1 calc R U . . .
C24 C 0.6370(7) 0.4089(6) 0.6346(7) 0.095(4) Uani 1 1 d . . . . .
H24 H 0.681369 0.408751 0.609125 0.114 Uiso 1 1 calc R U . . .
C25 C 0.4986(6) 0.4230(4) 0.6506(5) 0.076(3) Uani 1 1 d . . . . .
C26 C 0.3829(4) 0.2682(4) 0.7307(3) 0.0424(15) Uani 1 1 d . . . . .
C27 C 0.3674(4) 0.1443(3) 0.5933(3) 0.0386(14) Uani 1 1 d . . . . .
C28 C 0.4952(5) 0.2922(6) 0.5132(4) 0.065(2) Uani 1 1 d . . . . .
C29 C 0.3992(6) 0.5226(5) 0.6381(5) 0.081(3) Uani 1 1 d . . . . .
H29A H 0.419334 0.556532 0.605582 0.097 Uiso 1 1 calc R U . . .
H29B H 0.419662 0.542983 0.676261 0.097 Uiso 1 1 calc R U . . .
C30 C 0.3105(6) 0.5221(5) 0.6383(6) 0.081(3) Uani 1 1 d . . . . .
H30A H 0.290819 0.499434 0.675958 0.097 Uiso 1 1 calc R U . . .
H30B H 0.290269 0.577027 0.634497 0.097 Uiso 1 1 calc R U . . .
C31 C 0.2473(5) 0.5042(5) 0.5463(5) 0.071(3) Uani 1 1 d . . . . .
H31 H 0.224680 0.555524 0.550124 0.085 Uiso 1 1 calc R U . . .
C32 C 0.2380(5) 0.4607(5) 0.4901(5) 0.070(3) Uani 1 1 d . . . . .
C33 C 0.1986(6) 0.4932(8) 0.4425(6) 0.093(4) Uani 1 1 d . . . . .
H33 H 0.172096 0.542583 0.446294 0.111 Uiso 1 1 calc R U . . .
C34 C 0.1983(6) 0.4531(10) 0.3900(6) 0.114(6) Uani 1 1 d . . . . .
H34 H 0.171132 0.473857 0.356609 0.136 Uiso 1 1 calc R U . . .
C35 C 0.2382(6) 0.3819(8) 0.3861(5) 0.087(3) Uani 1 1 d . . . . .
H35 H 0.238684 0.352103 0.350322 0.105 Uiso 1 1 calc R U . . .
C36 C 0.2774(5) 0.3554(7) 0.4360(5) 0.076(3) Uani 1 1 d . . . . .
H36 H 0.306678 0.307493 0.432703 0.091 Uiso 1 1 calc R U . . .
C37 C 0.5648(6) 0.2078(6) 0.6561(5) 0.084(3) Uani 1 1 d . . . . .
H37A H 0.564804 0.191333 0.614370 0.125 Uiso 1 1 calc R U . . .
H37B H 0.589339 0.260251 0.659639 0.125 Uiso 1 1 calc R U . . .
H37C H 0.510617 0.210428 0.670612 0.125 Uiso 1 1 calc R U . . .
C38 C 0.6091(6) 0.1502(6) 0.6913(5) 0.080(3) Uani 1 1 d . . . . .
N1 N 0.2844(4) 0.4752(4) 0.5894(4) 0.0645(19) Uani 1 1 d . . . . .
N2 N 0.2773(4) 0.3910(4) 0.4872(3) 0.0644(19) Uani 1 1 d . . . . .
N017 N 0.6449(7) 0.1050(7) 0.7170(5) 0.117(4) Uani 1 1 d . . . . .
O1 O 0.4226(4) 0.4416(3) 0.6293(3) 0.0691(17) Uani 1 1 d . . . . .
O2 O 0.4283(3) 0.3178(4) 0.5372(3) 0.0646(15) Uani 1 1 d . . . . .
O3 O 0.3071(3) 0.1954(3) 0.5819(2) 0.0392(10) Uani 1 1 d . . . . .
O4 O 0.3574(3) 0.2973(3) 0.6797(2) 0.0462(11) Uani 1 1 d . . . . .
Tb01 Tb 0.32764(3) 0.33112(2) 0.59112(2) 0.04521(17) Uani 1 1 d . . . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 C25 1.413(14) . ?
C1 C24 1.416(15) . ?
C1 C2 1.515(15) . ?
C2 C3 1.510(15) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C3 C28 1.407(13) . ?
C3 C4 1.421(14) . ?
C4 C5 1.349(16) . ?
C4 H4 0.9500 . ?
C5 C6 1.371(15) . ?
C5 H5 0.9500 . ?
C6 C7 1.385(12) . ?
C6 H6 0.9500 . ?
C7 C28 1.383(13) . ?
C7 C8 1.500(12) . ?
C8 C9 1.506(10) . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C9 C10 1.381(10) . ?
C9 C27 1.419(10) . ?
C10 C11 1.376(11) . ?
C10 H10 0.9500 . ?
C11 C12 1.386(11) . ?
C11 H11 0.9500 . ?
C12 C13 1.392(10) . ?
C12 H12 0.9500 . ?
C13 C27 1.425(9) . ?
C13 C14 1.509(9) . ?
C14 C15 1.500(10) . ?
C14 H14A 0.9900 . ?
C14 H14B 0.9900 . ?
C15 C16 1.415(10) . ?
C15 C26 1.418(10) . ?
C16 C17 1.374(12) . ?
C16 H16 0.9500 . ?
C17 C18 1.400(15) . ?
C17 H17 0.9500 . ?
C18 C19 1.381(12) . ?
C18 H18 0.9500 . ?
C19 C26 1.418(10) . ?
C19 C20 1.533(12) . ?
C20 C21 1.506(13) . ?
C20 H20A 0.9900 . ?
C20 H20B 0.9900 . ?
C21 C25 1.393(13) . ?
C21 C22 1.423(13) . ?
C22 C23 1.389(15) . ?
C22 H22 0.9500 . ?
C23 C24 1.363(16) . ?
C23 H23 0.9500 . ?
C24 H24 0.9500 . ?
C25 O1 1.416(11) . ?
C26 O4 1.323(8) . ?
C27 O3 1.364(8) . ?
C28 O2 1.333(10) . ?
C29 O1 1.434(9) . ?
C29 C30 1.510(13) . ?
C29 H29A 0.9900 . ?
C29 H29B 0.9900 . ?
C30 N1 1.426(13) . ?
C30 H30A 0.9900 . ?
C30 H30B 0.9900 . ?
C31 N1 1.258(11) . ?
C31 C32 1.472(14) . ?
C31 H31 0.9500 . ?
C32 N2 1.352(11) . ?
C32 C33 1.378(13) . ?
C33 C34 1.362(19) . ?
C33 H33 0.9500 . ?
C34 C35 1.381(18) . ?
C34 H34 0.9500 . ?
C35 C36 1.382(13) . ?
C35 H35 0.9500 . ?
C36 N2 1.299(12) . ?
C36 H36 0.9500 . ?
C37 C38 1.463(14) . ?
C37 H37A 0.9800 . ?
C37 H37B 0.9800 . ?
C37 H37C 0.9800 . ?
C38 N017 1.132(13) . ?
N1 Tb01 2.534(7) . ?
N2 Tb01 2.691(7) . ?
O1 Tb01 2.610(5) . ?
O2 Tb01 2.114(5) . ?
O3 Tb01 2.321(5) . ?
O3 Tb01 2.346(5) 2 ?
O4 Tb01 2.136(5) . ?
Tb01 Tb01 3.8012(8) 2 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C25 C1 C24 115.6(12) . . ?
C25 C1 C2 124.5(9) . . ?
C24 C1 C2 119.8(11) . . ?
C3 C2 C1 112.8(8) . . ?
C3 C2 H2A 109.0 . . ?
C1 C2 H2A 109.0 . . ?
C3 C2 H2B 109.0 . . ?
C1 C2 H2B 109.0 . . ?
H2A C2 H2B 107.8 . . ?
C28 C3 C4 117.2(10) . . ?
C28 C3 C2 117.6(9) . . ?
C4 C3 C2 125.2(10) . . ?
C5 C4 C3 121.8(11) . . ?
C5 C4 H4 119.1 . . ?
C3 C4 H4 119.1 . . ?
C4 C5 C6 119.6(10) . . ?
C4 C5 H5 120.2 . . ?
C6 C5 H5 120.2 . . ?
C5 C6 C7 121.4(11) . . ?
C5 C6 H6 119.3 . . ?
C7 C6 H6 119.3 . . ?
C28 C7 C6 119.3(9) . . ?
C28 C7 C8 118.6(7) . . ?
C6 C7 C8 122.0(9) . . ?
C7 C8 C9 110.9(6) . . ?
C7 C8 H8A 109.5 . . ?
C9 C8 H8A 109.5 . . ?
C7 C8 H8B 109.5 . . ?
C9 C8 H8B 109.5 . . ?
H8A C8 H8B 108.1 . . ?
C10 C9 C27 119.0(7) . . ?
C10 C9 C8 116.9(7) . . ?
C27 C9 C8 124.1(7) . . ?
C11 C10 C9 122.3(7) . . ?
C11 C10 H10 118.9 . . ?
C9 C10 H10 118.9 . . ?
C10 C11 C12 118.9(7) . . ?
C10 C11 H11 120.5 . . ?
C12 C11 H11 120.5 . . ?
C11 C12 C13 121.6(7) . . ?
C11 C12 H12 119.2 . . ?
C13 C12 H12 119.2 . . ?
C12 C13 C27 118.8(7) . . ?
C12 C13 C14 117.5(6) . . ?
C27 C13 C14 123.6(6) . . ?
C15 C14 C13 112.2(6) . . ?
C15 C14 H14A 109.2 . . ?
C13 C14 H14A 109.2 . . ?
C15 C14 H14B 109.2 . . ?
C13 C14 H14B 109.2 . . ?
H14A C14 H14B 107.9 . . ?
C16 C15 C26 118.2(7) . . ?
C16 C15 C14 121.1(7) . . ?
C26 C15 C14 120.7(6) . . ?
C17 C16 C15 121.6(8) . . ?
C17 C16 H16 119.2 . . ?
C15 C16 H16 119.2 . . ?
C16 C17 C18 119.9(8) . . ?
C16 C17 H17 120.0 . . ?
C18 C17 H17 120.0 . . ?
C19 C18 C17 120.5(8) . . ?
C19 C18 H18 119.7 . . ?
C17 C18 H18 119.7 . . ?
C18 C19 C26 120.2(8) . . ?
C18 C19 C20 122.3(8) . . ?
C26 C19 C20 117.5(7) . . ?
C21 C20 C19 110.2(7) . . ?
C21 C20 H20A 109.6 . . ?
C19 C20 H20A 109.6 . . ?
C21 C20 H20B 109.6 . . ?
C19 C20 H20B 109.6 . . ?
H20A C20 H20B 108.1 . . ?
C25 C21 C22 117.9(10) . . ?
C25 C21 C20 122.2(8) . . ?
C22 C21 C20 119.7(10) . . ?
C23 C22 C21 119.4(12) . . ?
C23 C22 H22 120.3 . . ?
C21 C22 H22 120.3 . . ?
C24 C23 C22 121.1(12) . . ?
C24 C23 H23 119.4 . . ?
C22 C23 H23 119.4 . . ?
C23 C24 C1 122.3(13) . . ?
C23 C24 H24 118.9 . . ?
C1 C24 H24 118.9 . . ?
C21 C25 C1 123.3(10) . . ?
C21 C25 O1 118.0(10) . . ?
C1 C25 O1 118.6(10) . . ?
O4 C26 C19 120.3(7) . . ?
O4 C26 C15 120.0(6) . . ?
C19 C26 C15 119.6(7) . . ?
O3 C27 C9 121.4(6) . . ?
O3 C27 C13 119.5(6) . . ?
C9 C27 C13 119.0(6) . . ?
O2 C28 C7 120.7(8) . . ?
O2 C28 C3 118.7(10) . . ?
C7 C28 C3 120.5(8) . . ?
O1 C29 C30 105.8(7) . . ?
O1 C29 H29A 110.6 . . ?
C30 C29 H29A 110.6 . . ?
O1 C29 H29B 110.6 . . ?
C30 C29 H29B 110.6 . . ?
H29A C29 H29B 108.7 . . ?
N1 C30 C29 108.2(9) . . ?
N1 C30 H30A 110.1 . . ?
C29 C30 H30A 110.1 . . ?
N1 C30 H30B 110.1 . . ?
C29 C30 H30B 110.1 . . ?
H30A C30 H30B 108.4 . . ?
N1 C31 C32 121.7(8) . . ?
N1 C31 H31 119.1 . . ?
C32 C31 H31 119.1 . . ?
N2 C32 C33 123.2(11) . . ?
N2 C32 C31 114.9(8) . . ?
C33 C32 C31 121.6(10) . . ?
C34 C33 C32 118.8(11) . . ?
C34 C33 H33 120.6 . . ?
C32 C33 H33 120.6 . . ?
C33 C34 C35 118.9(10) . . ?
C33 C34 H34 120.6 . . ?
C35 C34 H34 120.6 . . ?
C34 C35 C36 117.8(12) . . ?
C34 C35 H35 121.1 . . ?
C36 C35 H35 121.1 . . ?
N2 C36 C35 124.8(11) . . ?
N2 C36 H36 117.6 . . ?
C35 C36 H36 117.6 . . ?
C38 C37 H37A 109.5 . . ?
C38 C37 H37B 109.5 . . ?
H37A C37 H37B 109.5 . . ?
C38 C37 H37C 109.5 . . ?
H37A C37 H37C 109.5 . . ?
H37B C37 H37C 109.5 . . ?
N017 C38 C37 177.6(13) . . ?
C31 N1 C30 122.5(8) . . ?
C31 N1 Tb01 122.0(6) . . ?
C30 N1 Tb01 115.3(6) . . ?
C36 N2 C32 116.4(8) . . ?
C36 N2 Tb01 126.8(6) . . ?
C32 N2 Tb01 116.1(6) . . ?
C25 O1 C29 114.7(7) . . ?
C25 O1 Tb01 121.4(4) . . ?
C29 O1 Tb01 123.4(5) . . ?
C28 O2 Tb01 164.0(5) . . ?
C27 O3 Tb01 119.3(4) . . ?
C27 O3 Tb01 126.9(4) . 2 ?
Tb01 O3 Tb01 109.07(18) . 2 ?
C26 O4 Tb01 171.3(5) . . ?
O2 Tb01 O4 108.5(2) . . ?
O2 Tb01 O3 88.1(2) . . ?
O4 Tb01 O3 81.81(17) . . ?
O2 Tb01 O3 136.2(2) . 2 ?
O4 Tb01 O3 105.33(18) . 2 ?
O3 Tb01 O3 69.96(18) . 2 ?
O2 Tb01 N1 109.2(2) . . ?
O4 Tb01 N1 109.7(2) . . ?
O3 Tb01 N1 153.7(2) . . ?
O3 Tb01 N1 84.0(2) 2 . ?
O2 Tb01 O1 76.3(2) . . ?
O4 Tb01 O1 74.60(19) . . ?
O3 Tb01 O1 145.53(16) . . ?
O3 Tb01 O1 140.39(17) 2 . ?
N1 Tb01 O1 60.2(2) . . ?
O2 Tb01 N2 78.3(2) . . ?
O4 Tb01 N2 171.4(2) . . ?
O3 Tb01 N2 104.0(2) . . ?
O3 Tb01 N2 71.48(19) 2 . ?
N1 Tb01 N2 62.3(3) . . ?
O1 Tb01 N2 102.6(2) . . ?
O2 Tb01 Tb01 119.19(16) . 2 ?
O4 Tb01 Tb01 88.49(13) . 2 ?
O3 Tb01 Tb01 35.68(11) . 2 ?
O3 Tb01 Tb01 35.25(11) 2 2 ?
N1 Tb01 Tb01 119.02(16) . 2 ?
O1 Tb01 Tb01 160.49(15) . 2 ?
N2 Tb01 Tb01 92.73(16) . 2 ?

_refine_diff_density_max         2.154
_refine_diff_density_min         -0.987
_refine_diff_density_rms         0.147

####################################################################### 
# 
# 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_292
_database_code_depnum_ccdc_archive 'CCDC 2011008'
loop_
_audit_author_name
_audit_author_address
'Berthold Kersting'
;University of Leipzig
Germany
;
_audit_update_record             
;
2020-06-20 deposited with the CCDC.	2020-07-17 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C76 H64 Dy2 N6 O8'
_chemical_formula_weight         1514.33



# start Validation Reply Form


_vrf_RINTA01_292                 
;
PROBLEM: The value of Rint is greater than 0.18
RESPONSE: Crystal quality low due to disordered solvate molecules 
;

_vrf_PLAT020_292                 
;
PROBLEM: The Value of Rint is Greater Than 0.12  .........      0.236 Report
RESPONSE: As above

;
_vrf_PLAT601_292                 
;
PROBLEM: Structure Contains Solvent Accessible VOIDS of .        112 Ang**3
RESPONSE: 

The two MeCN solvate molecules in this structures were found to be heavily 
disordered and all attempts to model this disorder failed. The corresponding 
electron density was removed from the structure (and the corresponding F0) 
with the SQUEEZE algorithm implemented in the PLATON program suite. 
The SQUEEZE routine revealed total potential solvent area of 112 A3 per unit 
corresponding to approximately two MeCN solvate molecules per formula unit. 
;



# end Validation Reply Form


loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Dy Dy -9.8046 9.8477 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 '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'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           56
_space_group_name_H-M_alt        'P c c n'
_space_group_name_Hall           '-P 2ab 2ac'

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

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

_cell_length_a                   16.8208(5)
_cell_length_b                   16.9909(4)
_cell_length_c                   22.5406(7)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     6442.1(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    180(2)
_cell_measurement_reflns_used    25716
_cell_measurement_theta_min      7.4
_cell_measurement_theta_max      141.81

_exptl_crystal_description       block
_exptl_crystal_colour            gold-yellow
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.561
_exptl_crystal_F_000             3032
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.124
_exptl_crystal_size_mid          0.085
_exptl_crystal_size_min          0.053
_exptl_absorpt_coefficient_mu    12.775
_shelx_estimated_absorpt_T_min   0.300
_shelx_estimated_absorpt_T_max   0.551
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_correction_T_min  0.32
_exptl_absorpt_correction_T_max  0.56
_exptl_absorpt_process_details   
;
Busing, W. R. & Levy, H. A. (1957) Acta Cryst. 10, 180-182. 
and Coppens, P., Leiserowitz, L. & Rabinovich, D. (1965) 
Acta Cryst. 1965, 1035-1038.
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      180(2)
_diffrn_radiation_wavelength     1.54186
_diffrn_radiation_type           CuK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Stoe stadivari'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            69509
_diffrn_reflns_av_unetI/netI     0.0901
_diffrn_reflns_av_R_equivalents  0.2359
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         3.698
_diffrn_reflns_theta_max         69.990
_diffrn_reflns_theta_full        67.686
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measured_fraction_theta_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_point_group_measured_fraction_full 0.996
_reflns_number_total             6070
_reflns_number_gt                4153
_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       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_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)+(0.1415P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         6070
_refine_ls_number_parameters     415
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1034
_refine_ls_R_factor_gt           0.0713
_refine_ls_wR_factor_ref         0.2067
_refine_ls_wR_factor_gt          0.1817
_refine_ls_goodness_of_fit_ref   0.946
_refine_ls_restrained_S_all      0.946
_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
C1 C 0.4209(6) 0.4378(7) 0.1096(6) 0.077(3) Uani 1 1 d . . . . .
C2 C 0.4219(7) 0.4481(6) 0.0409(6) 0.086(4) Uani 1 1 d . . . . .
H2A H 0.443032 0.500948 0.031185 0.104 Uiso 1 1 calc R U . . .
H2B H 0.458187 0.408565 0.023447 0.104 Uiso 1 1 calc R U . . .
C3 C 0.3417(6) 0.4393(6) 0.0137(5) 0.068(3) Uani 1 1 d . . . . .
C4 C 0.3134(8) 0.3698(6) -0.0128(6) 0.087(4) Uani 1 1 d . . . . .
H4 H 0.346603 0.324619 -0.013041 0.104 Uiso 1 1 calc R U . . .
C5 C 0.2403(8) 0.3649(7) -0.0382(6) 0.092(4) Uani 1 1 d . . . . .
H5 H 0.222760 0.316949 -0.055418 0.111 Uiso 1 1 calc R U . . .
C6 C 0.1928(8) 0.4293(6) -0.0385(4) 0.071(3) Uani 1 1 d . . . . .
H6 H 0.141803 0.425938 -0.056369 0.085 Uiso 1 1 calc R U . . .
C7 C 0.2170(6) 0.5012(5) -0.0131(3) 0.052(2) Uani 1 1 d . . . . .
C8 C 0.1655(5) 0.5725(5) -0.0096(3) 0.048(2) Uani 1 1 d . . . . .
H8A H 0.125768 0.570843 -0.042010 0.057 Uiso 1 1 calc R U . . .
H8B H 0.198593 0.620100 -0.015274 0.057 Uiso 1 1 calc R U . . .
C9 C 0.1233(4) 0.5777(4) 0.0489(3) 0.0372(16) Uani 1 1 d . . . . .
C10 C 0.0652(5) 0.5221(5) 0.0607(4) 0.047(2) Uani 1 1 d . . . . .
H10 H 0.051617 0.485371 0.030559 0.057 Uiso 1 1 calc R U . . .
C11 C 0.0264(5) 0.5180(5) 0.1144(4) 0.052(2) Uani 1 1 d . . . . .
H11 H -0.015843 0.481818 0.120365 0.062 Uiso 1 1 calc R U . . .
C12 C 0.0508(4) 0.5685(5) 0.1599(4) 0.047(2) Uani 1 1 d . . . . .
H12 H 0.027095 0.564229 0.197988 0.056 Uiso 1 1 calc R U . . .
C13 C 0.1097(4) 0.6253(4) 0.1499(3) 0.0322(15) Uani 1 1 d . . . . .
C14 C 0.1360(4) 0.6746(5) 0.2031(3) 0.0388(16) Uani 1 1 d . . . . .
H14A H 0.165430 0.721338 0.188763 0.047 Uiso 1 1 calc R U . . .
H14B H 0.088391 0.693401 0.224695 0.047 Uiso 1 1 calc R U . . .
C15 C 0.1875(4) 0.6297(4) 0.2448(3) 0.0355(16) Uani 1 1 d . . . . .
C16 C 0.1577(5) 0.5982(5) 0.2977(3) 0.050(2) Uani 1 1 d . . . . .
H16 H 0.103156 0.605182 0.307381 0.061 Uiso 1 1 calc R U . . .
C17 C 0.2072(7) 0.5564(6) 0.3366(4) 0.065(3) Uani 1 1 d . . . . .
H17 H 0.186014 0.534461 0.372007 0.078 Uiso 1 1 calc R U . . .
C18 C 0.2847(7) 0.5474(6) 0.3238(4) 0.069(3) Uani 1 1 d . . . . .
H18 H 0.318055 0.521531 0.351692 0.082 Uiso 1 1 calc R U . . .
C19 C 0.3180(5) 0.5749(6) 0.2705(4) 0.054(2) Uani 1 1 d . . . . .
C20 C 0.4038(5) 0.5598(6) 0.2520(4) 0.065(3) Uani 1 1 d . . . . .
H20A H 0.425322 0.607626 0.232698 0.077 Uiso 1 1 calc R U . . .
H20B H 0.436136 0.549136 0.287790 0.077 Uiso 1 1 calc R U . . .
C21 C 0.4106(5) 0.4918(6) 0.2102(5) 0.061(3) Uani 1 1 d . . . . .
C22 C 0.3982(6) 0.4134(7) 0.2326(6) 0.076(3) Uani 1 1 d . . . . .
H22 H 0.389965 0.405483 0.273847 0.092 Uiso 1 1 calc R U . . .
C23 C 0.3981(7) 0.3501(8) 0.1949(7) 0.088(4) Uani 1 1 d . . . . .
H23 H 0.391143 0.298386 0.209988 0.105 Uiso 1 1 calc R U . . .
C24 C 0.4082(7) 0.3620(8) 0.1353(8) 0.094(4) Uani 1 1 d . . . . .
H24 H 0.406624 0.317600 0.109711 0.113 Uiso 1 1 calc R U . . .
C25 C 0.4244(5) 0.5002(6) 0.1507(5) 0.063(3) Uani 1 1 d . . . . .
C26 C 0.2686(4) 0.6169(4) 0.2302(3) 0.0325(15) Uani 1 1 d . . . . .
C27 C 0.1446(4) 0.6335(4) 0.0930(3) 0.0308(14) Uani 1 1 d . . . . .
C28 C 0.2927(6) 0.5049(5) 0.0139(4) 0.057(3) Uani 1 1 d . . . . .
C29 C 0.5231(5) 0.6012(6) 0.1382(5) 0.064(3) Uani 1 1 d . . . . .
H29A H 0.557443 0.581682 0.105690 0.077 Uiso 1 1 calc R U . . .
H29B H 0.543385 0.580171 0.176260 0.077 Uiso 1 1 calc R U . . .
C30 C 0.5228(5) 0.6914(6) 0.1393(6) 0.076(3) Uani 1 1 d . . . . .
H30A H 0.500548 0.710952 0.177174 0.091 Uiso 1 1 calc R U . . .
H30B H 0.577456 0.712142 0.134779 0.091 Uiso 1 1 calc R U . . .
C31 C 0.5050(5) 0.7531(5) 0.0448(5) 0.060(3) Uani 1 1 d . . . . .
H31 H 0.557274 0.773892 0.047609 0.072 Uiso 1 1 calc R U . . .
C32 C 0.4594(6) 0.7621(5) -0.0097(5) 0.064(3) Uani 1 1 d . . . . .
C33 C 0.4930(8) 0.8018(6) -0.0583(6) 0.083(4) Uani 1 1 d . . . . .
H33 H 0.542574 0.828372 -0.055475 0.100 Uiso 1 1 calc R U . . .
C34 C 0.4502(11) 0.8001(7) -0.1103(6) 0.113(6) Uani 1 1 d . . . . .
H34 H 0.470123 0.826885 -0.144223 0.136 Uiso 1 1 calc R U . . .
C35 C 0.3804(9) 0.7612(6) -0.1141(5) 0.086(4) Uani 1 1 d . . . . .
H35 H 0.351120 0.760675 -0.150115 0.103 Uiso 1 1 calc R U . . .
C36 C 0.3517(7) 0.7209(6) -0.0632(5) 0.073(3) Uani 1 1 d . . . . .
H36 H 0.303469 0.691963 -0.065932 0.088 Uiso 1 1 calc R U . . .
C37 C 0.2080(6) 0.4336(6) 0.1555(6) 0.076(3) Uani 1 1 d . . . . .
H37A H 0.241803 0.396569 0.133669 0.114 Uiso 1 1 calc R U . . .
H37B H 0.240960 0.465643 0.181932 0.114 Uiso 1 1 calc R U . . .
H37C H 0.180236 0.467877 0.127302 0.114 Uiso 1 1 calc R U . . .
C38 C 0.1492(7) 0.3894(7) 0.1908(5) 0.070(3) Uani 1 1 d . . . . .
Dy1 Dy 0.33057(2) 0.67241(3) 0.09114(2) 0.03769(19) Uani 1 1 d . . . . .
N1 N 0.4735(4) 0.7163(4) 0.0899(4) 0.0545(19) Uani 1 1 d . . . . .
N2 N 0.3901(5) 0.7225(4) -0.0121(4) 0.059(2) Uani 1 1 d . . . . .
N3 N 0.1044(7) 0.3548(8) 0.2156(6) 0.111(4) Uani 1 1 d . . . . .
O1 O 0.4407(3) 0.5768(4) 0.1288(3) 0.0592(17) Uani 1 1 d . . . . .
O2 O 0.3167(4) 0.5708(4) 0.0383(3) 0.0591(17) Uani 1 1 d . . . . .
O3 O 0.1955(3) 0.6925(3) 0.0822(2) 0.0295(10) Uani 1 1 d . . . . .
O4 O 0.2981(3) 0.6429(3) 0.1799(2) 0.0382(11) Uani 1 1 d . . . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 C25 1.410(15) . ?
C1 C24 1.428(17) . ?
C1 C2 1.559(17) . ?
C2 C3 1.489(16) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C3 C28 1.387(13) . ?
C3 C4 1.406(15) . ?
C4 C5 1.357(18) . ?
C4 H4 0.9500 . ?
C5 C6 1.356(16) . ?
C5 H5 0.9500 . ?
C6 C7 1.408(12) . ?
C6 H6 0.9500 . ?
C7 C28 1.412(14) . ?
C7 C8 1.491(12) . ?
C8 C9 1.501(11) . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C9 C10 1.385(11) . ?
C9 C27 1.419(10) . ?
C10 C11 1.377(12) . ?
C10 H10 0.9500 . ?
C11 C12 1.398(11) . ?
C11 H11 0.9500 . ?
C12 C13 1.401(10) . ?
C12 H12 0.9500 . ?
C13 C27 1.417(9) . ?
C13 C14 1.529(10) . ?
C14 C15 1.488(10) . ?
C14 H14A 0.9900 . ?
C14 H14B 0.9900 . ?
C15 C16 1.401(10) . ?
C15 C26 1.420(10) . ?
C16 C17 1.403(13) . ?
C16 H16 0.9500 . ?
C17 C18 1.343(16) . ?
C17 H17 0.9500 . ?
C18 C19 1.407(13) . ?
C18 H18 0.9500 . ?
C19 C26 1.422(10) . ?
C19 C20 1.523(13) . ?
C20 C21 1.496(14) . ?
C20 H20A 0.9900 . ?
C20 H20B 0.9900 . ?
C21 C25 1.368(14) . ?
C21 C22 1.439(14) . ?
C22 C23 1.371(17) . ?
C22 H22 0.9500 . ?
C23 C24 1.369(18) . ?
C23 H23 0.9500 . ?
C24 H24 0.9500 . ?
C25 O1 1.419(11) . ?
C26 O4 1.315(8) . ?
C27 O3 1.341(9) . ?
C28 O2 1.312(10) . ?
C29 O1 1.462(10) . ?
C29 C30 1.533(14) . ?
C29 H29A 0.9900 . ?
C29 H29B 0.9900 . ?
C30 N1 1.451(14) . ?
C30 H30A 0.9900 . ?
C30 H30B 0.9900 . ?
C31 N1 1.305(12) . ?
C31 C32 1.456(15) . ?
C31 H31 0.9500 . ?
C32 N2 1.348(12) . ?
C32 C33 1.407(14) . ?
C33 C34 1.38(2) . ?
C33 H33 0.9500 . ?
C34 C35 1.35(2) . ?
C34 H34 0.9500 . ?
C35 C36 1.422(13) . ?
C35 H35 0.9500 . ?
C36 N2 1.319(14) . ?
C36 H36 0.9500 . ?
C37 C38 1.474(15) . ?
C37 H37A 0.9800 . ?
C37 H37B 0.9800 . ?
C37 H37C 0.9800 . ?
C38 N3 1.108(14) . ?
Dy1 O2 2.110(6) . ?
Dy1 O4 2.133(5) . ?
Dy1 O3 2.306(5) . ?
Dy1 O3 2.346(5) 2_565 ?
Dy1 N1 2.517(7) . ?
Dy1 O1 2.606(6) . ?
Dy1 N2 2.673(7) . ?
Dy1 Dy1 3.7814(8) 2_565 ?

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
C25 C1 C24 114.7(13) . . ?
C25 C1 C2 124.6(10) . . ?
C24 C1 C2 120.4(12) . . ?
C3 C2 C1 112.9(9) . . ?
C3 C2 H2A 109.0 . . ?
C1 C2 H2A 109.0 . . ?
C3 C2 H2B 109.0 . . ?
C1 C2 H2B 109.0 . . ?
H2A C2 H2B 107.8 . . ?
C28 C3 C4 118.3(11) . . ?
C28 C3 C2 117.1(10) . . ?
C4 C3 C2 124.6(11) . . ?
C5 C4 C3 122.5(11) . . ?
C5 C4 H4 118.7 . . ?
C3 C4 H4 118.7 . . ?
C6 C5 C4 119.1(11) . . ?
C6 C5 H5 120.5 . . ?
C4 C5 H5 120.5 . . ?
C5 C6 C7 121.9(12) . . ?
C5 C6 H6 119.1 . . ?
C7 C6 H6 119.1 . . ?
C28 C7 C6 118.3(9) . . ?
C28 C7 C8 117.7(7) . . ?
C6 C7 C8 123.9(10) . . ?
C7 C8 C9 111.7(6) . . ?
C7 C8 H8A 109.3 . . ?
C9 C8 H8A 109.3 . . ?
C7 C8 H8B 109.3 . . ?
C9 C8 H8B 109.3 . . ?
H8A C8 H8B 107.9 . . ?
C10 C9 C27 120.0(7) . . ?
C10 C9 C8 117.5(7) . . ?
C27 C9 C8 122.4(7) . . ?
C11 C10 C9 122.5(7) . . ?
C11 C10 H10 118.8 . . ?
C9 C10 H10 118.8 . . ?
C10 C11 C12 118.4(7) . . ?
C10 C11 H11 120.8 . . ?
C12 C11 H11 120.8 . . ?
C11 C12 C13 120.8(8) . . ?
C11 C12 H12 119.6 . . ?
C13 C12 H12 119.6 . . ?
C12 C13 C27 120.4(7) . . ?
C12 C13 C14 117.2(7) . . ?
C27 C13 C14 122.4(6) . . ?
C15 C14 C13 112.6(6) . . ?
C15 C14 H14A 109.1 . . ?
C13 C14 H14A 109.1 . . ?
C15 C14 H14B 109.1 . . ?
C13 C14 H14B 109.1 . . ?
H14A C14 H14B 107.8 . . ?
C16 C15 C26 118.9(7) . . ?
C16 C15 C14 121.7(7) . . ?
C26 C15 C14 119.5(6) . . ?
C15 C16 C17 120.9(8) . . ?
C15 C16 H16 119.6 . . ?
C17 C16 H16 119.6 . . ?
C18 C17 C16 120.0(9) . . ?
C18 C17 H17 120.0 . . ?
C16 C17 H17 120.0 . . ?
C17 C18 C19 122.1(9) . . ?
C17 C18 H18 118.9 . . ?
C19 C18 H18 118.9 . . ?
C18 C19 C26 118.7(9) . . ?
C18 C19 C20 123.7(9) . . ?
C26 C19 C20 117.6(8) . . ?
C21 C20 C19 112.0(8) . . ?
C21 C20 H20A 109.2 . . ?
C19 C20 H20A 109.2 . . ?
C21 C20 H20B 109.2 . . ?
C19 C20 H20B 109.2 . . ?
H20A C20 H20B 107.9 . . ?
C25 C21 C22 117.7(11) . . ?
C25 C21 C20 123.3(9) . . ?
C22 C21 C20 118.9(11) . . ?
C23 C22 C21 120.6(12) . . ?
C23 C22 H22 119.7 . . ?
C21 C22 H22 119.7 . . ?
C22 C23 C24 119.5(13) . . ?
C22 C23 H23 120.2 . . ?
C24 C23 H23 120.2 . . ?
C23 C24 C1 123.3(14) . . ?
C23 C24 H24 118.3 . . ?
C1 C24 H24 118.3 . . ?
C21 C25 C1 123.9(10) . . ?
C21 C25 O1 118.1(10) . . ?
C1 C25 O1 117.9(10) . . ?
O4 C26 C19 120.0(7) . . ?
O4 C26 C15 120.6(6) . . ?
C19 C26 C15 119.4(7) . . ?
O3 C27 C13 120.2(6) . . ?
O3 C27 C9 122.2(6) . . ?
C13 C27 C9 117.6(7) . . ?
O2 C28 C3 120.3(11) . . ?
O2 C28 C7 119.8(8) . . ?
C3 C28 C7 119.9(9) . . ?
O1 C29 C30 106.4(7) . . ?
O1 C29 H29A 110.5 . . ?
C30 C29 H29A 110.5 . . ?
O1 C29 H29B 110.5 . . ?
C30 C29 H29B 110.5 . . ?
H29A C29 H29B 108.6 . . ?
N1 C30 C29 106.3(9) . . ?
N1 C30 H30A 110.5 . . ?
C29 C30 H30A 110.5 . . ?
N1 C30 H30B 110.5 . . ?
C29 C30 H30B 110.5 . . ?
H30A C30 H30B 108.7 . . ?
N1 C31 C32 119.5(8) . . ?
N1 C31 H31 120.2 . . ?
C32 C31 H31 120.2 . . ?
N2 C32 C33 123.7(12) . . ?
N2 C32 C31 116.0(9) . . ?
C33 C32 C31 119.8(10) . . ?
C34 C33 C32 116.4(12) . . ?
C34 C33 H33 121.8 . . ?
C32 C33 H33 121.8 . . ?
C35 C34 C33 121.3(11) . . ?
C35 C34 H34 119.4 . . ?
C33 C34 H34 119.4 . . ?
C34 C35 C36 118.8(13) . . ?
C34 C35 H35 120.6 . . ?
C36 C35 H35 120.6 . . ?
N2 C36 C35 121.8(11) . . ?
N2 C36 H36 119.1 . . ?
C35 C36 H36 119.1 . . ?
C38 C37 H37A 109.5 . . ?
C38 C37 H37B 109.5 . . ?
H37A C37 H37B 109.5 . . ?
C38 C37 H37C 109.5 . . ?
H37A C37 H37C 109.5 . . ?
H37B C37 H37C 109.5 . . ?
N3 C38 C37 177.5(14) . . ?
O2 Dy1 O4 108.0(2) . . ?
O2 Dy1 O3 87.9(2) . . ?
O4 Dy1 O3 82.21(18) . . ?
O2 Dy1 O3 137.0(2) . 2_565 ?
O4 Dy1 O3 105.23(19) . 2_565 ?
O3 Dy1 O3 70.34(19) . 2_565 ?
O2 Dy1 N1 109.9(2) . . ?
O4 Dy1 N1 109.0(2) . . ?
O3 Dy1 N1 153.7(2) . . ?
O3 Dy1 N1 83.6(2) 2_565 . ?
O2 Dy1 O1 75.7(2) . . ?
O4 Dy1 O1 74.4(2) . . ?
O3 Dy1 O1 145.20(17) . . ?
O3 Dy1 O1 140.44(18) 2_565 . ?
N1 Dy1 O1 60.6(2) . . ?
O2 Dy1 N2 79.1(2) . . ?
O4 Dy1 N2 170.9(2) . . ?
O3 Dy1 N2 104.2(2) . . ?
O3 Dy1 N2 71.52(19) 2_565 . ?
N1 Dy1 N2 62.5(3) . . ?
O1 Dy1 N2 102.5(2) . . ?
O2 Dy1 Dy1 119.43(18) . 2_565 ?
O4 Dy1 Dy1 88.86(14) . 2_565 ?
O3 Dy1 Dy1 35.99(11) . 2_565 ?
O3 Dy1 Dy1 35.27(12) 2_565 2_565 ?
N1 Dy1 Dy1 118.57(17) . 2_565 ?
O1 Dy1 Dy1 160.79(16) . 2_565 ?
N2 Dy1 Dy1 92.64(18) . 2_565 ?
C31 N1 C30 120.3(8) . . ?
C31 N1 Dy1 122.6(7) . . ?
C30 N1 Dy1 116.8(6) . . ?
C36 N2 C32 118.1(9) . . ?
C36 N2 Dy1 124.7(6) . . ?
C32 N2 Dy1 116.5(7) . . ?
C25 O1 C29 113.1(7) . . ?
C25 O1 Dy1 123.2(4) . . ?
C29 O1 Dy1 123.0(5) . . ?
C28 O2 Dy1 165.8(6) . . ?
C27 O3 Dy1 120.2(4) . . ?
C27 O3 Dy1 126.6(4) . 2_565 ?
Dy1 O3 Dy1 108.74(19) . 2_565 ?
C26 O4 Dy1 170.0(5) . . ?

_refine_diff_density_max         1.410
_refine_diff_density_min         -1.344
_refine_diff_density_rms         0.141

