# Electronic Supplementary Material (ESI) for CrystEngComm.
# This journal is © The Royal Society of Chemistry 2018

####################################################################### 
# 
# 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_shelx
_database_code_depnum_ccdc_archive 'CCDC 1860535'
_audit_update_record             
;
2018-08-06 deposited with the CCDC.
2018-10-30 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            'C50 H42 Eu2 N8 O14'
_chemical_formula_weight         1282.83

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'
Eu Eu -0.1578 3.6682 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/c'
_space_group_name_Hall           '-P 2ybc'

_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, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   11.454(2)
_cell_length_b                   16.080(3)
_cell_length_c                   13.689(2)
_cell_angle_alpha                90
_cell_angle_beta                 103.293(3)
_cell_angle_gamma                90
_cell_volume                     2453.7(8)
_cell_formula_units_Z            2
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    2939
_cell_measurement_theta_min      2.22
_cell_measurement_theta_max      22.42

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.736
_exptl_crystal_F_000             1272
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.240
_exptl_crystal_size_mid          0.220
_exptl_crystal_size_min          0.200
_exptl_absorpt_coefficient_mu    2.609
_shelx_estimated_absorpt_T_min   0.573
_shelx_estimated_absorpt_T_max   0.623
_exptl_absorpt_correction_type   none
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'sealed tube'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            12382
_diffrn_reflns_av_unetI/netI     0.0471
_diffrn_reflns_av_R_equivalents  0.0411
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         1.827
_diffrn_reflns_theta_max         25.248
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             4442
_reflns_number_gt                3363
_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 APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_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)+(0.0396P)²+0.0577P] 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         4442
_refine_ls_number_parameters     338
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0514
_refine_ls_R_factor_gt           0.0355
_refine_ls_wR_factor_ref         0.0873
_refine_ls_wR_factor_gt          0.0796
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_restrained_S_all      1.048
_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
Eu1 Eu 0.95258(2) 0.03050(2) 0.12536(2) 0.03873(11) Uani 1 1 d . . . . .
O1 O 0.4188(4) 0.1570(3) 0.5626(3) 0.0752(12) Uani 1 1 d . . . . .
H1H H 0.458469 0.147395 0.521054 0.113 Uiso 1 1 calc R U . . .
O2 O 1.1236(3) 0.0805(2) 0.2678(2) 0.0541(10) Uani 1 1 d . . . . .
O3 O 0.9993(4) 0.1744(2) 0.1884(3) 0.0671(11) Uani 1 1 d . . . . .
O4 O 1.1002(3) 0.0621(2) 0.0357(2) 0.0462(9) Uani 1 1 d . . . . .
O5 O 1.2100(3) 0.0729(2) -0.0750(3) 0.0569(10) Uani 1 1 d . . . . .
O6 O 1.0783(3) -0.0877(2) 0.1474(2) 0.0504(9) Uani 1 1 d . . . . .
O7 O 1.1485(3) -0.1121(2) 0.0111(2) 0.0538(10) Uani 1 1 d . . . . .
N1 N 0.9214(4) -0.0347(3) 0.2935(3) 0.0428(10) Uani 1 1 d . . . . .
N2 N 0.7702(4) 0.0831(3) 0.1926(3) 0.0455(10) Uani 1 1 d . . . . .
N4 N 0.7220(4) 0.0065(3) 0.5749(3) 0.0471(11) Uani 1 1 d . . . . .
H4 H 0.759280 -0.024498 0.623309 0.056 Uiso 1 1 calc R U . . .
N3 N 0.5902(4) 0.0977(3) 0.4882(3) 0.0505(11) Uani 1 1 d . . . . .
C5 C 0.8401(4) -0.0025(3) 0.3418(4) 0.0397(12) Uani 1 1 d . . . . .
C1 C 0.9913(5) -0.0961(3) 0.3388(4) 0.0513(14) Uani 1 1 d . . . . .
H1 H 1.045388 -0.119923 0.305706 0.062 Uiso 1 1 calc R U . . .
C2 C 0.9874(5) -0.1270(4) 0.4344(4) 0.0569(15) Uani 1 1 d . . . . .
H2 H 1.036811 -0.170561 0.463247 0.068 Uiso 1 1 calc R U . . .
C3 C 0.9093(5) -0.0913(3) 0.4834(4) 0.0507(14) Uani 1 1 d . . . . .
H3 H 0.907144 -0.109107 0.547582 0.061 Uiso 1 1 calc R U . . .
C4 C 0.8327(4) -0.0282(3) 0.4377(4) 0.0425(12) Uani 1 1 d . . . . .
C12 C 0.7459(5) 0.0134(3) 0.4810(4) 0.0467(13) Uani 1 1 d . . . . .
C11 C 0.6654(4) 0.0709(3) 0.4292(4) 0.0474(13) Uani 1 1 d . . . . .
C10 C 0.6667(4) 0.0945(3) 0.3285(4) 0.0431(12) Uani 1 1 d . . . . .
C6 C 0.7576(4) 0.0611(3) 0.2859(4) 0.0418(12) Uani 1 1 d . . . . .
C7 C 0.6913(5) 0.1366(3) 0.1406(4) 0.0533(14) Uani 1 1 d . . . . .
H7 H 0.699550 0.152343 0.077102 0.064 Uiso 1 1 calc R U . . .
C8 C 0.5977(5) 0.1701(3) 0.1760(4) 0.0565(15) Uani 1 1 d . . . . .
H8 H 0.543702 0.206390 0.136193 0.068 Uiso 1 1 calc R U . . .
C9 C 0.5853(5) 0.1495(3) 0.2697(4) 0.0515(14) Uani 1 1 d . . . . .
H9 H 0.523004 0.171949 0.294381 0.062 Uiso 1 1 calc R U . . .
C13 C 0.6277(5) 0.0581(4) 0.5762(4) 0.0510(14) Uani 1 1 d . . . . .
C14 C 0.5728(5) 0.0690(3) 0.6610(4) 0.0496(14) Uani 1 1 d . . . . .
C15 C 0.4691(6) 0.1173(4) 0.6504(5) 0.0620(16) Uani 1 1 d . . . . .
C16 C 0.4142(6) 0.1268(4) 0.7304(6) 0.0739(19) Uani 1 1 d . . . . .
H16 H 0.344781 0.158646 0.722133 0.089 Uiso 1 1 calc R U . . .
C17 C 0.4612(7) 0.0899(5) 0.8214(5) 0.082(2) Uani 1 1 d . . . . .
H17 H 0.423836 0.097346 0.874314 0.098 Uiso 1 1 calc R U . . .
C18 C 0.5642(7) 0.0413(4) 0.8350(5) 0.079(2) Uani 1 1 d . . . . .
H18 H 0.596231 0.016658 0.896760 0.095 Uiso 1 1 calc R U . . .
C19 C 0.6191(6) 0.0301(4) 0.7546(5) 0.0660(17) Uani 1 1 d . . . . .
H19 H 0.686888 -0.003343 0.762730 0.079 Uiso 1 1 calc R U . . .
C20 C 1.0915(5) 0.1553(4) 0.2529(4) 0.0529(14) Uani 1 1 d . . . . .
C21 C 1.1668(6) 0.2235(4) 0.3128(4) 0.083(2) Uani 1 1 d . . . . .
H21A H 1.198335 0.258646 0.268278 0.124 Uiso 1 1 calc R U . . .
H21B H 1.231766 0.199211 0.361309 0.124 Uiso 1 1 calc R U . . .
H21C H 1.117832 0.256026 0.346642 0.124 Uiso 1 1 calc R U . . .
C22 C 1.1856(4) 0.0958(3) 0.0053(4) 0.0423(12) Uani 1 1 d . . . . .
C23 C 1.2533(6) 0.1646(4) 0.0665(4) 0.0732(19) Uani 1 1 d . . . . .
H23A H 1.316480 0.183065 0.036239 0.110 Uiso 1 1 calc R U . . .
H23B H 1.287051 0.144906 0.133201 0.110 Uiso 1 1 calc R U . . .
H23C H 1.199833 0.210051 0.069361 0.110 Uiso 1 1 calc R U . . .
C24 C 1.1354(5) -0.1305(3) 0.0979(4) 0.0481(13) Uani 1 1 d . . . . .
C25 C 1.1955(6) -0.2077(4) 0.1452(4) 0.0747(19) Uani 1 1 d . . . . .
H25A H 1.260255 -0.193040 0.200593 0.112 Uiso 1 1 calc R U . . .
H25B H 1.226447 -0.238378 0.096513 0.112 Uiso 1 1 calc R U . . .
H25C H 1.138515 -0.241336 0.168903 0.112 Uiso 1 1 calc R U . . .


_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 O7 2.357(3) 3_755 ?
Eu1 O6 2.361(3) . ?
Eu1 O4 2.362(3) . ?
Eu1 O5 2.474(4) 3_755 ?
Eu1 O3 2.484(4) . ?
Eu1 O2 2.556(3) . ?
Eu1 N2 2.610(4) . ?
Eu1 O4 2.614(3) 3_755 ?
Eu1 N1 2.627(4) . ?
Eu1 C20 2.886(6) . ?
Eu1 C22 2.920(5) 3_755 ?
Eu1 Eu1 3.9542(7) 3_755 ?
O1 C15 1.365(7) . ?
O1 H1H 0.8200 . ?
O2 C20 1.260(7) . ?
O3 C20 1.249(7) . ?
O4 C22 1.269(6) . ?
O5 C22 1.250(6) . ?
O6 C24 1.251(6) . ?
O7 C24 1.267(5) . ?
N1 C1 1.332(6) . ?
N1 C5 1.362(6) . ?
N2 C7 1.329(6) . ?
N2 C6 1.365(6) . ?
N4 C13 1.367(7) . ?
N4 C12 1.378(6) . ?
N4 H4 0.8600 . ?
N3 C13 1.342(7) . ?
N3 C11 1.378(6) . ?
C5 C4 1.398(7) . ?
C5 C6 1.479(7) . ?
C1 C2 1.410(7) . ?
C1 H1 0.9300 . ?
C2 C3 1.362(7) . ?
C2 H2 0.9300 . ?
C3 C4 1.392(7) . ?
C3 H3 0.9300 . ?
C4 C12 1.434(7) . ?
C12 C11 1.381(7) . ?
C11 C10 1.434(7) . ?
C10 C9 1.399(7) . ?
C10 C6 1.411(6) . ?
C7 C8 1.383(7) . ?
C7 H7 0.9300 . ?
C8 C9 1.364(7) . ?
C8 H8 0.9300 . ?
C9 H9 0.9300 . ?
C13 C14 1.453(7) . ?
C14 C15 1.398(8) . ?
C14 C19 1.414(8) . ?
C15 C16 1.391(8) . ?
C16 C17 1.374(9) . ?
C16 H16 0.9300 . ?
C17 C18 1.391(9) . ?
C17 H17 0.9300 . ?
C18 C19 1.399(8) . ?
C18 H18 0.9300 . ?
C19 H19 0.9300 . ?
C20 C21 1.515(7) . ?
C21 H21A 0.9600 . ?
C21 H21B 0.9600 . ?
C21 H21C 0.9600 . ?
C22 C23 1.493(7) . ?
C23 H23A 0.9600 . ?
C23 H23B 0.9600 . ?
C23 H23C 0.9600 . ?
C24 C25 1.494(7) . ?
C25 H25A 0.9600 . ?
C25 H25B 0.9600 . ?
C25 H25C 0.9600 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O7 Eu1 O6 136.35(11) 3_755 . ?
O7 Eu1 O4 75.42(12) 3_755 . ?
O6 Eu1 O4 75.61(12) . . ?
O7 Eu1 O5 87.28(13) 3_755 3_755 ?
O6 Eu1 O5 83.82(13) . 3_755 ?
O4 Eu1 O5 125.65(12) . 3_755 ?
O7 Eu1 O3 77.53(13) 3_755 . ?
O6 Eu1 O3 128.94(13) . . ?
O4 Eu1 O3 81.79(12) . . ?
O5 Eu1 O3 144.23(13) 3_755 . ?
O7 Eu1 O2 125.47(13) 3_755 . ?
O6 Eu1 O2 79.47(12) . . ?
O4 Eu1 O2 79.28(11) . . ?
O5 Eu1 O2 145.09(12) 3_755 . ?
O3 Eu1 O2 51.38(13) . . ?
O7 Eu1 N2 79.15(12) 3_755 . ?
O6 Eu1 N2 136.87(12) . . ?
O4 Eu1 N2 147.16(13) . . ?
O5 Eu1 N2 72.78(12) 3_755 . ?
O3 Eu1 N2 72.64(13) . . ?
O2 Eu1 N2 99.46(12) . . ?
O7 Eu1 O4 70.91(12) 3_755 3_755 ?
O6 Eu1 O4 70.45(11) . 3_755 ?
O4 Eu1 O4 74.85(13) . 3_755 ?
O5 Eu1 O4 50.83(11) 3_755 3_755 ?
O3 Eu1 O4 144.43(12) . 3_755 ?
O2 Eu1 O4 144.19(11) . 3_755 ?
N2 Eu1 O4 115.70(12) . 3_755 ?
O7 Eu1 N1 140.84(13) 3_755 . ?
O6 Eu1 N1 76.61(12) . . ?
O4 Eu1 N1 143.03(12) . . ?
O5 Eu1 N1 74.37(12) 3_755 . ?
O3 Eu1 N1 97.42(13) . . ?
O2 Eu1 N1 72.04(12) . . ?
N2 Eu1 N1 62.57(13) . . ?
O4 Eu1 N1 117.38(12) 3_755 . ?
O7 Eu1 C20 101.20(16) 3_755 . ?
O6 Eu1 C20 104.28(16) . . ?
O4 Eu1 C20 78.66(13) . . ?
O5 Eu1 C20 155.68(13) 3_755 . ?
O3 Eu1 C20 25.52(14) . . ?
O2 Eu1 C20 25.89(14) . . ?
N2 Eu1 C20 86.34(15) . . ?
O4 Eu1 C20 153.48(12) 3_755 . ?
N1 Eu1 C20 85.11(14) . . ?
O7 Eu1 C22 78.70(13) 3_755 3_755 ?
O6 Eu1 C22 75.36(13) . 3_755 ?
O4 Eu1 C22 100.57(13) . 3_755 ?
O5 Eu1 C22 25.09(11) 3_755 3_755 ?
O3 Eu1 C22 154.66(14) . 3_755 ?
O2 Eu1 C22 153.96(13) . 3_755 ?
N2 Eu1 C22 94.39(14) . 3_755 ?
O4 Eu1 C22 25.76(11) 3_755 3_755 ?
N1 Eu1 C22 95.46(13) . 3_755 ?
C20 Eu1 C22 179.22(14) . 3_755 ?
O7 Eu1 Eu1 68.50(8) 3_755 3_755 ?
O6 Eu1 Eu1 68.31(8) . 3_755 ?
O4 Eu1 Eu1 39.65(8) . 3_755 ?
O5 Eu1 Eu1 86.02(8) 3_755 3_755 ?
O3 Eu1 Eu1 116.89(9) . 3_755 ?
O2 Eu1 Eu1 115.15(8) . 3_755 ?
N2 Eu1 Eu1 142.04(9) . 3_755 ?
O4 Eu1 Eu1 35.20(7) 3_755 3_755 ?
N1 Eu1 Eu1 141.37(9) . 3_755 ?
C20 Eu1 Eu1 118.30(10) . 3_755 ?
C22 Eu1 Eu1 60.93(10) 3_755 3_755 ?
C15 O1 H1H 109.5 . . ?
C20 O2 Eu1 91.8(3) . . ?
C20 O3 Eu1 95.5(4) . . ?
C22 O4 Eu1 163.8(3) . . ?
C22 O4 Eu1 90.7(3) . 3_755 ?
Eu1 O4 Eu1 105.15(13) . 3_755 ?
C22 O5 Eu1 97.8(3) . 3_755 ?
C24 O6 Eu1 138.8(3) . . ?
C24 O7 Eu1 136.9(3) . 3_755 ?
C1 N1 C5 117.5(4) . . ?
C1 N1 Eu1 121.1(3) . . ?
C5 N1 Eu1 121.3(3) . . ?
C7 N2 C6 117.7(4) . . ?
C7 N2 Eu1 121.4(3) . . ?
C6 N2 Eu1 120.7(3) . . ?
C13 N4 C12 106.8(4) . . ?
C13 N4 H4 126.6 . . ?
C12 N4 H4 126.6 . . ?
C13 N3 C11 105.3(4) . . ?
N1 C5 C4 122.6(5) . . ?
N1 C5 C6 116.0(4) . . ?
C4 C5 C6 121.3(4) . . ?
N1 C1 C2 123.3(5) . . ?
N1 C1 H1 118.3 . . ?
C2 C1 H1 118.3 . . ?
C3 C2 C1 118.3(5) . . ?
C3 C2 H2 120.9 . . ?
C1 C2 H2 120.9 . . ?
C2 C3 C4 120.2(5) . . ?
C2 C3 H3 119.9 . . ?
C4 C3 H3 119.9 . . ?
C3 C4 C5 118.0(5) . . ?
C3 C4 C12 125.4(5) . . ?
C5 C4 C12 116.6(5) . . ?
N4 C12 C11 106.3(4) . . ?
N4 C12 C4 130.7(5) . . ?
C11 C12 C4 123.0(5) . . ?
N3 C11 C12 110.0(4) . . ?
N3 C11 C10 128.9(5) . . ?
C12 C11 C10 121.1(5) . . ?
C9 C10 C6 117.5(5) . . ?
C9 C10 C11 124.6(5) . . ?
C6 C10 C11 118.0(5) . . ?
N2 C6 C10 122.3(5) . . ?
N2 C6 C5 118.1(4) . . ?
C10 C6 C5 119.6(4) . . ?
N2 C7 C8 123.4(5) . . ?
N2 C7 H7 118.3 . . ?
C8 C7 H7 118.3 . . ?
C9 C8 C7 119.5(5) . . ?
C9 C8 H8 120.3 . . ?
C7 C8 H8 120.3 . . ?
C8 C9 C10 119.7(5) . . ?
C8 C9 H9 120.2 . . ?
C10 C9 H9 120.2 . . ?
N3 C13 N4 111.5(5) . . ?
N3 C13 C14 123.6(5) . . ?
N4 C13 C14 124.9(5) . . ?
C15 C14 C19 118.2(5) . . ?
C15 C14 C13 119.8(5) . . ?
C19 C14 C13 122.0(5) . . ?
O1 C15 C16 117.7(6) . . ?
O1 C15 C14 121.8(5) . . ?
C16 C15 C14 120.4(6) . . ?
C17 C16 C15 120.8(6) . . ?
C17 C16 H16 119.6 . . ?
C15 C16 H16 119.6 . . ?
C16 C17 C18 120.5(6) . . ?
C16 C17 H17 119.8 . . ?
C18 C17 H17 119.8 . . ?
C17 C18 C19 119.2(7) . . ?
C17 C18 H18 120.4 . . ?
C19 C18 H18 120.4 . . ?
C18 C19 C14 120.8(6) . . ?
C18 C19 H19 119.6 . . ?
C14 C19 H19 119.6 . . ?
O3 C20 O2 121.1(5) . . ?
O3 C20 C21 119.2(6) . . ?
O2 C20 C21 119.7(6) . . ?
O3 C20 Eu1 59.0(3) . . ?
O2 C20 Eu1 62.3(3) . . ?
C21 C20 Eu1 175.7(4) . . ?
C20 C21 H21A 109.5 . . ?
C20 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
C20 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
O5 C22 O4 120.5(5) . . ?
O5 C22 C23 121.3(5) . . ?
O4 C22 C23 118.2(5) . . ?
O5 C22 Eu1 57.1(3) . 3_755 ?
O4 C22 Eu1 63.5(3) . 3_755 ?
C23 C22 Eu1 176.1(4) . 3_755 ?
C22 C23 H23A 109.5 . . ?
C22 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
C22 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
O6 C24 O7 124.7(5) . . ?
O6 C24 C25 118.0(5) . . ?
O7 C24 C25 117.3(5) . . ?
C24 C25 H25A 109.5 . . ?
C24 C25 H25B 109.5 . . ?
H25A C25 H25B 109.5 . . ?
C24 C25 H25C 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?

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
_geom_hbond_publ_flag
O1 H1H N3 0.82 1.85 2.593(6) 149.5 . yes
N4 H4 O2 0.86 1.98 2.822(6) 167.2 3_756 yes

_refine_diff_density_max         0.892
_refine_diff_density_min         -0.518
_refine_diff_density_rms         0.098



####################################################################### 
# 
# 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_shelx_CCDC1
_database_code_depnum_ccdc_archive 'CCDC 1860538'
_audit_update_record             
;
2018-08-06 deposited with the CCDC.
2018-10-30 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            'C23 H16 N5 O7 Tb'
_chemical_formula_weight         633.33

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

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/n'
_space_group_name_Hall           '-P 2yn'

_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+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   15.764(8)
_cell_length_b                   7.932(4)
_cell_length_c                   18.869(9)
_cell_angle_alpha                90
_cell_angle_beta                 91.802(8)
_cell_angle_gamma                90
_cell_volume                     2358(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    2492
_cell_measurement_theta_min      2.51
_cell_measurement_theta_max      25.40

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.784
_exptl_crystal_F_000             1240
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.120
_exptl_absorpt_coefficient_mu    3.053
_shelx_estimated_absorpt_T_min   0.580
_shelx_estimated_absorpt_T_max   0.711
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.5834
_exptl_absorpt_correction_T_max  0.6928
_exptl_absorpt_process_details   'SADABS (Bruker, 2002)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            11615
_diffrn_reflns_av_unetI/netI     0.0818
_diffrn_reflns_av_R_equivalents  0.0617
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         1.658
_diffrn_reflns_theta_max         25.243
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             4277
_reflns_number_gt                2830
_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 APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    'Bruker APEX2'
_computing_publication_material  'Bruker APEX2'
_refine_special_details          
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0831P)²+3.1147P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         4277
_refine_ls_number_parameters     327
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0884
_refine_ls_R_factor_gt           0.0537
_refine_ls_wR_factor_ref         0.1660
_refine_ls_wR_factor_gt          0.1431
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_restrained_S_all      1.037
_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 0.7550(8) 0.8537(14) 0.1134(6) 0.061(3) Uani 1 1 d . . . . .
H1 H 0.742719 0.846162 0.064959 0.073 Uiso 1 1 calc R U . . .
C2 C 0.6902(7) 0.9032(15) 0.1575(5) 0.063(3) Uani 1 1 d . . . . .
H2 H 0.636097 0.928307 0.139370 0.075 Uiso 1 1 calc R U . . .
C3 C 0.7100(7) 0.9136(13) 0.2303(5) 0.055(3) Uani 1 1 d . . . . .
H3 H 0.668101 0.944478 0.261440 0.066 Uiso 1 1 calc R U . . .
C4 C 0.7914(7) 0.8785(13) 0.2567(5) 0.047(3) Uani 1 1 d . . . . .
C5 C 0.8529(6) 0.8267(11) 0.2071(5) 0.043(2) Uani 1 1 d . . . . .
C6 C 0.9391(6) 0.7861(11) 0.2304(5) 0.045(2) Uani 1 1 d . . . . .
C7 C 1.0737(7) 0.6990(13) 0.1999(6) 0.056(3) Uani 1 1 d . . . . .
H7 H 1.111977 0.670340 0.165407 0.067 Uiso 1 1 calc R U . . .
C8 C 1.1000(7) 0.6923(13) 0.2704(6) 0.059(3) Uani 1 1 d . . . . .
H8 H 1.155006 0.658545 0.282594 0.071 Uiso 1 1 calc R U . . .
C9 C 1.0446(8) 0.7359(14) 0.3232(5) 0.056(3) Uani 1 1 d . . . . .
H9 H 1.062367 0.732268 0.370644 0.067 Uiso 1 1 calc R U . . .
C10 C 0.9619(7) 0.7852(13) 0.3043(5) 0.049(3) Uani 1 1 d . . . . .
C11 C 0.8988(7) 0.8357(12) 0.3519(5) 0.050(3) Uani 1 1 d . . . . .
C12 C 0.8177(6) 0.8806(13) 0.3276(5) 0.045(2) Uani 1 1 d . . . . .
C13 C 0.8324(7) 0.9026(14) 0.4452(5) 0.051(3) Uani 1 1 d . . . . .
C14 C 0.6893(7) 0.4350(13) -0.0195(5) 0.052(3) Uani 1 1 d . . . . .
C15 C 0.7665(7) 0.5255(12) -0.0357(5) 0.050(3) Uani 1 1 d . . . . .
C16 C 0.7804(8) 0.5545(15) -0.1097(5) 0.060(3) Uani 1 1 d . . . . .
H16 H 0.826615 0.619052 -0.122599 0.072 Uiso 1 1 calc R U . . .
C17 C 0.7279(8) 0.4904(16) -0.1610(6) 0.063(3) Uani 1 1 d . . . . .
H17 H 0.740224 0.506681 -0.208416 0.076 Uiso 1 1 calc R U . . .
C18 C 0.6565(8) 0.4012(17) -0.1439(5) 0.067(3) Uani 1 1 d . . . . .
C19 C 0.6345(8) 0.3746(15) -0.0725(5) 0.062(3) Uani 1 1 d . . . . .
H19 H 0.584897 0.318330 -0.061547 0.075 Uiso 1 1 calc R U . . .
C20 C 1.1184(7) 0.9396(12) 0.0410(5) 0.045(2) Uani 1 1 d . . . . .
C21 C 1.2000(8) 0.9570(16) 0.0849(7) 0.086(4) Uani 1 1 d . . . . .
H21A H 1.247563 0.940788 0.055037 0.129 Uiso 1 1 calc R U . . .
H21B H 1.201375 0.873654 0.121785 0.129 Uiso 1 1 calc R U . . .
H21C H 1.202826 1.067449 0.105555 0.129 Uiso 1 1 calc R U . . .
C22 C 0.9596(6) 0.3599(12) 0.1090(5) 0.041(2) Uani 1 1 d . . . . .
C23 C 0.9654(8) 0.1821(12) 0.1357(6) 0.060(3) Uani 1 1 d . . . . .
H23A H 1.022638 0.158799 0.151761 0.090 Uiso 1 1 calc R U . . .
H23B H 0.949478 0.105717 0.098140 0.090 Uiso 1 1 calc R U . . .
H23C H 0.927896 0.167792 0.174365 0.090 Uiso 1 1 calc R U . . .
N1 N 0.8335(5) 0.8165(9) 0.1364(4) 0.0441(19) Uani 1 1 d . . . . .
N2 N 0.9950(6) 0.7453(10) 0.1798(4) 0.048(2) Uani 1 1 d . . . . .
N3 N 0.9071(6) 0.8500(11) 0.4247(4) 0.053(2) Uani 1 1 d . . . . .
N4 N 0.7770(6) 0.9228(10) 0.3886(4) 0.051(2) Uani 1 1 d . . . . .
H4 H 0.725317 0.956475 0.390730 0.061 Uiso 1 1 calc R U . . .
N5 N 0.6031(10) 0.3152(18) -0.1985(6) 0.099(4) Uani 1 1 d . . . . .
O1 O 0.8190(5) 0.5788(8) 0.0124(3) 0.0527(18) Uani 1 1 d . . . . .
O2 O 0.6341(8) 0.3131(19) -0.2585(5) 0.148(6) Uani 1 1 d . . . . .
O3 O 0.5325(9) 0.261(2) -0.1819(6) 0.138(5) Uani 1 1 d . . . . .
O4 O 1.0777(5) 0.8080(8) 0.0461(4) 0.0518(18) Uani 1 1 d . . . . .
O5 O 0.9006(4) 0.9360(8) -0.0034(3) 0.0542(18) Uani 1 1 d . . . . .
O6 O 1.0106(4) 0.4087(8) 0.0617(3) 0.0439(16) Uani 1 1 d . . . . .
O7 O 0.9077(4) 0.4602(8) 0.1322(3) 0.0525(18) Uani 1 1 d . . . . .
Tb1 Tb 0.94186(3) 0.69381(5) 0.05135(2) 0.0428(2) 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 N1 1.331(14) . ?
C1 C2 1.395(14) . ?
C2 C3 1.402(14) . ?
C3 C4 1.390(14) . ?
C4 C12 1.388(13) . ?
C4 C5 1.428(13) . ?
C5 N1 1.362(12) . ?
C5 C6 1.451(14) . ?
C6 N2 1.359(12) . ?
C6 C10 1.430(14) . ?
C7 N2 1.338(13) . ?
C7 C8 1.381(15) . ?
C8 C9 1.388(14) . ?
C9 C10 1.396(15) . ?
C10 C11 1.420(14) . ?
C11 N3 1.380(12) . ?
C11 C12 1.391(14) . ?
C12 N4 1.376(11) . ?
C13 N3 1.320(13) . ?
C13 N4 1.367(12) . ?
C13 C14 1.477(12) 2_655 ?
C14 C19 1.385(15) . ?
C14 C15 1.454(14) . ?
C15 O1 1.280(12) . ?
C15 C16 1.438(13) . ?
C16 C17 1.353(15) . ?
C17 C18 1.377(16) . ?
C18 C19 1.417(14) . ?
C18 N5 1.477(17) . ?
C20 O4 1.230(11) . ?
C20 O5 1.247(11) 3_775 ?
C20 C21 1.513(15) . ?
C22 O7 1.231(11) . ?
C22 O6 1.280(10) . ?
C22 C23 1.500(13) . ?
C22 Tb1 2.874(9) . ?
N1 Tb1 2.572(8) . ?
N2 Tb1 2.572(8) . ?
N5 O3 1.243(17) . ?
N5 O2 1.247(16) . ?
O1 Tb1 2.244(7) . ?
O4 Tb1 2.330(7) . ?
O5 Tb1 2.267(7) . ?
O6 Tb1 2.423(5) 3_765 ?
O6 Tb1 2.513(6) . ?
O7 Tb1 2.470(6) . ?

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
N1 C1 C2 123.9(10) . . ?
C1 C2 C3 117.2(11) . . ?
C4 C3 C2 120.9(9) . . ?
C12 C4 C3 125.9(9) . . ?
C12 C4 C5 116.5(10) . . ?
C3 C4 C5 117.4(9) . . ?
N1 C5 C4 121.6(9) . . ?
N1 C5 C6 117.5(8) . . ?
C4 C5 C6 120.9(9) . . ?
N2 C6 C10 122.4(9) . . ?
N2 C6 C5 117.6(9) . . ?
C10 C6 C5 120.1(9) . . ?
N2 C7 C8 122.1(9) . . ?
C7 C8 C9 120.3(10) . . ?
C8 C9 C10 119.3(10) . . ?
C9 C10 C11 125.8(9) . . ?
C9 C10 C6 117.1(9) . . ?
C11 C10 C6 117.1(10) . . ?
N3 C11 C12 111.4(9) . . ?
N3 C11 C10 127.3(10) . . ?
C12 C11 C10 121.3(9) . . ?
N4 C12 C4 132.5(10) . . ?
N4 C12 C11 103.5(8) . . ?
C4 C12 C11 123.9(9) . . ?
N3 C13 N4 111.2(8) . . ?
N3 C13 C14 124.6(10) . 2_655 ?
N4 C13 C14 124.1(9) . 2_655 ?
C19 C14 C15 121.8(9) . . ?
C19 C14 C13 117.9(10) . 2_645 ?
C15 C14 C13 120.3(9) . 2_645 ?
O1 C15 C16 121.4(10) . . ?
O1 C15 C14 122.8(8) . . ?
C16 C15 C14 115.8(10) . . ?
C17 C16 C15 121.8(12) . . ?
C16 C17 C18 120.7(10) . . ?
C17 C18 C19 121.7(11) . . ?
C17 C18 N5 121.7(11) . . ?
C19 C18 N5 116.4(12) . . ?
C14 C19 C18 118.0(11) . . ?
O4 C20 O5 126.8(10) . 3_775 ?
O4 C20 C21 118.1(9) . . ?
O5 C20 C21 115.1(10) 3_775 . ?
O7 C22 O6 119.4(8) . . ?
O7 C22 C23 121.5(9) . . ?
O6 C22 C23 119.1(9) . . ?
O7 C22 Tb1 58.7(5) . . ?
O6 C22 Tb1 60.9(5) . . ?
C23 C22 Tb1 176.6(7) . . ?
C1 N1 C5 119.0(8) . . ?
C1 N1 Tb1 120.6(6) . . ?
C5 N1 Tb1 120.1(6) . . ?
C7 N2 C6 118.8(9) . . ?
C7 N2 Tb1 119.7(6) . . ?
C6 N2 Tb1 120.1(7) . . ?
C13 N3 C11 105.0(9) . . ?
C13 N4 C12 108.8(8) . . ?
O3 N5 O2 127.1(14) . . ?
O3 N5 C18 118.7(12) . . ?
O2 N5 C18 114.1(14) . . ?
C15 O1 Tb1 153.9(6) . . ?
C20 O4 Tb1 144.6(7) . . ?
C20 O5 Tb1 172.2(6) 3_775 . ?
C22 O6 Tb1 137.0(6) . 3_765 ?
C22 O6 Tb1 92.7(5) . . ?
Tb1 O6 Tb1 112.2(2) 3_765 . ?
C22 O7 Tb1 96.1(5) . . ?
O1 Tb1 O5 87.9(2) . . ?
O1 Tb1 O4 158.3(2) . . ?
O5 Tb1 O4 84.4(2) . . ?
O1 Tb1 O6 82.1(2) . 3_765 ?
O5 Tb1 O6 88.6(2) . 3_765 ?
O4 Tb1 O6 77.5(2) . 3_765 ?
O1 Tb1 O7 72.2(2) . . ?
O5 Tb1 O7 148.4(2) . . ?
O4 Tb1 O7 122.4(2) . . ?
O6 Tb1 O7 111.8(2) 3_765 . ?
O1 Tb1 O6 91.5(2) . . ?
O5 Tb1 O6 156.2(2) . . ?
O4 Tb1 O6 87.6(2) . . ?
O6 Tb1 O6 67.8(2) 3_765 . ?
O7 Tb1 O6 51.6(2) . . ?
O1 Tb1 N2 128.7(2) . . ?
O5 Tb1 N2 112.0(3) . . ?
O4 Tb1 N2 72.9(3) . . ?
O6 Tb1 N2 141.5(2) 3_765 . ?
O7 Tb1 N2 66.9(2) . . ?
O6 Tb1 N2 86.7(2) . . ?
O1 Tb1 N1 77.0(2) . . ?
O5 Tb1 N1 77.1(2) . . ?
O4 Tb1 N1 120.6(2) . . ?
O6 Tb1 N1 155.0(2) 3_765 . ?
O7 Tb1 N1 74.7(2) . . ?
O6 Tb1 N1 125.8(2) . . ?
N2 Tb1 N1 63.6(3) . . ?
O1 Tb1 C22 79.8(3) . . ?
O5 Tb1 C22 167.6(3) . . ?
O4 Tb1 C22 107.2(3) . . ?
O6 Tb1 C22 89.7(2) 3_765 . ?
O7 Tb1 C22 25.2(2) . . ?
O6 Tb1 C22 26.4(2) . . ?
N2 Tb1 C22 76.4(3) . . ?
N1 Tb1 C22 99.8(3) . . ?

_refine_diff_density_max         2.047
_refine_diff_density_min         -0.544
_refine_diff_density_rms         0.174



####################################################################### 
# 
# 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_shelx_CCDC2
_database_code_depnum_ccdc_archive 'CCDC 1860536'
_audit_update_record             
;
2018-08-06 deposited with the CCDC.
2018-10-30 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            'C50 H42 N8 O14 Tb2'
_chemical_formula_weight         1296.75

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

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/c'
_space_group_name_Hall           '-P 2ybc'

_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, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   11.4496(19)
_cell_length_b                   16.139(3)
_cell_length_c                   13.595(2)
_cell_angle_alpha                90
_cell_angle_beta                 103.261(3)
_cell_angle_gamma                90
_cell_volume                     2445.2(7)
_cell_formula_units_Z            2
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    1935
_cell_measurement_theta_min      2.45
_cell_measurement_theta_max      19.51

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.761
_exptl_crystal_F_000             1280
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.230
_exptl_crystal_size_mid          0.220
_exptl_crystal_size_min          0.210
_exptl_absorpt_coefficient_mu    2.946
_shelx_estimated_absorpt_T_min   0.551
_shelx_estimated_absorpt_T_max   0.577
_exptl_absorpt_correction_type   none
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'sealed tube'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            12405
_diffrn_reflns_av_unetI/netI     0.0655
_diffrn_reflns_av_R_equivalents  0.0541
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         1.990
_diffrn_reflns_theta_max         25.247
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             4427
_reflns_number_gt                2876
_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 APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_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)+(0.0394P)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         4427
_refine_ls_number_parameters     338
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0757
_refine_ls_R_factor_gt           0.0415
_refine_ls_wR_factor_ref         0.0975
_refine_ls_wR_factor_gt          0.0843
_refine_ls_goodness_of_fit_ref   0.996
_refine_ls_restrained_S_all      0.996
_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 0.5088(6) -0.0943(4) 0.1615(5) 0.0620(18) Uani 1 1 d . . . . .
H1 H 0.454657 -0.117869 0.194941 0.074 Uiso 1 1 calc R U . . .
C2 C 0.5125(6) -0.1255(4) 0.0669(5) 0.067(2) Uani 1 1 d . . . . .
H2 H 0.463159 -0.169206 0.038489 0.080 Uiso 1 1 calc R U . . .
C3 C 0.5900(6) -0.0904(4) 0.0172(5) 0.0674(19) Uani 1 1 d . . . . .
H3 H 0.592065 -0.108548 -0.047351 0.081 Uiso 1 1 calc R U . . .
C4 C 0.6663(6) -0.0275(4) 0.0624(5) 0.0561(17) Uani 1 1 d . . . . .
C5 C 0.6597(6) -0.0010(4) 0.1608(5) 0.0590(18) Uani 1 1 d . . . . .
C6 C 0.7409(6) 0.0621(4) 0.2152(5) 0.0538(17) Uani 1 1 d . . . . .
C7 C 0.8045(7) 0.1367(4) 0.3606(6) 0.075(2) Uani 1 1 d . . . . .
H7 H 0.795489 0.152264 0.424290 0.090 Uiso 1 1 calc R U . . .
C8 C 0.8995(7) 0.1708(4) 0.3258(6) 0.072(2) Uani 1 1 d . . . . .
H8 H 0.953605 0.206767 0.366045 0.086 Uiso 1 1 calc R U . . .
C9 C 0.9113(6) 0.1500(4) 0.2308(6) 0.0645(19) Uani 1 1 d . . . . .
H9 H 0.973138 0.172759 0.205545 0.077 Uiso 1 1 calc R U . . .
C10 C 0.8316(6) 0.0954(4) 0.1726(5) 0.0578(17) Uani 1 1 d . . . . .
C11 C 0.8327(6) 0.0711(4) 0.0718(5) 0.0586(18) Uani 1 1 d . . . . .
C12 C 0.7529(6) 0.0142(4) 0.0205(5) 0.0574(18) Uani 1 1 d . . . . .
C13 C 0.8731(7) 0.0585(5) -0.0736(6) 0.067(2) Uani 1 1 d . . . . .
C14 C 0.9288(7) 0.0692(4) -0.1594(6) 0.066(2) Uani 1 1 d . . . . .
C15 C 1.0317(8) 0.1181(5) -0.1492(7) 0.079(2) Uani 1 1 d . . . . .
C16 C 1.0870(8) 0.1288(5) -0.2280(8) 0.095(3) Uani 1 1 d . . . . .
H16 H 1.154764 0.162181 -0.219793 0.114 Uiso 1 1 calc R U . . .
C17 C 1.0416(10) 0.0898(6) -0.3199(8) 0.109(3) Uani 1 1 d . . . . .
H17 H 1.081047 0.096161 -0.372056 0.130 Uiso 1 1 calc R U . . .
C18 C 0.9360(9) 0.0402(6) -0.3360(8) 0.102(3) Uani 1 1 d . . . . .
H18 H 0.904088 0.015296 -0.398008 0.122 Uiso 1 1 calc R U . . .
C19 C 0.8827(8) 0.0308(5) -0.2535(7) 0.088(3) Uani 1 1 d . . . . .
H19 H 0.814378 -0.001906 -0.261208 0.106 Uiso 1 1 calc R U . . .
C20 C 0.4073(8) 0.1531(5) 0.2487(6) 0.071(2) Uani 1 1 d . . . . .
C21 C 0.3337(9) 0.2204(5) 0.1890(6) 0.108(3) Uani 1 1 d . . . . .
H21A H 0.335712 0.268613 0.230733 0.162 Uiso 1 1 calc R U . . .
H21B H 0.252280 0.201890 0.166184 0.162 Uiso 1 1 calc R U . . .
H21C H 0.365764 0.234020 0.131644 0.162 Uiso 1 1 calc R U . . .
C22 C 0.6825(6) -0.0942(4) 0.5040(5) 0.0574(17) Uani 1 1 d . . . . .
C23 C 0.7520(7) -0.1644(5) 0.5647(6) 0.091(3) Uani 1 1 d . . . . .
H23A H 0.697753 -0.208289 0.571519 0.136 Uiso 1 1 calc R U . . .
H23B H 0.791423 -0.144541 0.630532 0.136 Uiso 1 1 calc R U . . .
H23C H 0.810819 -0.184921 0.530617 0.136 Uiso 1 1 calc R U . . .
C24 C 0.6343(6) 0.1286(4) 0.5967(6) 0.0648(19) Uani 1 1 d . . . . .
C25 C 0.6955(7) 0.2043(4) 0.6470(5) 0.088(3) Uani 1 1 d . . . . .
H25A H 0.741901 0.190049 0.713014 0.132 Uiso 1 1 calc R U . . .
H25B H 0.636489 0.245007 0.652978 0.132 Uiso 1 1 calc R U . . .
H25C H 0.747596 0.226371 0.607272 0.132 Uiso 1 1 calc R U . . .
N1 N 0.5776(5) -0.0331(3) 0.2071(4) 0.0533(13) Uani 1 1 d . . . . .
N2 N 0.7272(5) 0.0839(3) 0.3085(4) 0.0595(14) Uani 1 1 d . . . . .
N3 N 0.9093(5) 0.0981(3) 0.0135(5) 0.0656(15) Uani 1 1 d . . . . .
N4 N 0.7788(5) 0.0075(4) -0.0733(4) 0.0664(16) Uani 1 1 d . . . . .
H4 H 0.742134 -0.023273 -0.122431 0.080 Uiso 1 1 calc R U . . .
O1 O 1.0812(5) 0.1580(4) -0.0604(5) 0.0972(17) Uani 1 1 d . . . . .
H1H H 1.037573 0.152145 -0.020796 0.146 Uiso 1 1 calc R U . . .
O2 O 0.3767(5) 0.0790(3) 0.2327(3) 0.0745(14) Uani 1 1 d . . . . .
O3 O 0.5007(5) 0.1725(3) 0.3129(4) 0.0824(15) Uani 1 1 d . . . . .
O4 O 0.4015(4) 0.0616(3) 0.4638(3) 0.0612(12) Uani 1 1 d . . . . .
O5 O 0.7067(4) -0.0721(3) 0.4244(3) 0.0720(14) Uani 1 1 d . . . . .
O6 O 0.4231(4) -0.0861(3) 0.3530(3) 0.0630(12) Uani 1 1 d . . . . .
O7 O 0.6467(4) 0.1103(3) 0.5101(3) 0.0697(13) Uani 1 1 d . . . . .
Tb1 Tb 0.54637(3) 0.03056(2) 0.37467(2) 0.05280(14) 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 N1 1.324(7) . ?
C1 C2 1.392(9) . ?
C1 H1 0.9300 . ?
C2 C3 1.357(9) . ?
C2 H2 0.9300 . ?
C3 C4 1.388(8) . ?
C3 H3 0.9300 . ?
C4 C12 1.422(9) . ?
C4 C5 1.422(9) . ?
C5 N1 1.350(8) . ?
C5 C6 1.461(9) . ?
C6 N2 1.360(8) . ?
C6 C10 1.407(9) . ?
C7 N2 1.313(8) . ?
C7 C8 1.395(10) . ?
C7 H7 0.9300 . ?
C8 C9 1.370(9) . ?
C8 H8 0.9300 . ?
C9 C10 1.380(9) . ?
C9 H9 0.9300 . ?
C10 C11 1.428(9) . ?
C11 C12 1.368(9) . ?
C11 N3 1.381(8) . ?
C12 N4 1.379(8) . ?
C13 N3 1.325(9) . ?
C13 N4 1.359(9) . ?
C13 C14 1.463(10) . ?
C14 C15 1.398(10) . ?
C14 C19 1.410(10) . ?
C15 O1 1.371(9) . ?
C15 C16 1.374(11) . ?
C16 C17 1.389(12) . ?
C16 H16 0.9300 . ?
C17 C18 1.424(12) . ?
C17 H17 0.9300 . ?
C18 C19 1.402(11) . ?
C18 H18 0.9300 . ?
C19 H19 0.9300 . ?
C20 O2 1.251(9) . ?
C20 O3 1.255(8) . ?
C20 C21 1.496(9) . ?
C20 Tb1 2.851(7) . ?
C21 H21A 0.9600 . ?
C21 H21B 0.9600 . ?
C21 H21C 0.9600 . ?
C22 O5 1.230(7) . ?
C22 O4 1.259(8) 3_656 ?
C22 C23 1.517(9) . ?
C22 Tb1 2.883(7) . ?
C23 H23A 0.9600 . ?
C23 H23B 0.9600 . ?
C23 H23C 0.9600 . ?
C24 O7 1.254(8) . ?
C24 O6 1.254(8) 3_656 ?
C24 C25 1.493(9) . ?
C25 H25A 0.9600 . ?
C25 H25B 0.9600 . ?
C25 H25C 0.9600 . ?
N1 Tb1 2.598(5) . ?
N2 Tb1 2.587(6) . ?
N4 H4 0.8600 . ?
O1 H1H 0.8200 . ?
O2 Tb1 2.527(5) . ?
O3 Tb1 2.455(5) . ?
O4 Tb1 2.322(5) . ?
O4 Tb1 2.606(4) 3_656 ?
O5 Tb1 2.450(5) . ?
O6 Tb1 2.332(4) . ?
O7 Tb1 2.323(4) . ?
Tb1 Tb1 3.9211(8) 3_656 ?

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
N1 C1 C2 124.2(7) . . ?
N1 C1 H1 117.9 . . ?
C2 C1 H1 117.9 . . ?
C3 C2 C1 118.1(7) . . ?
C3 C2 H2 120.9 . . ?
C1 C2 H2 120.9 . . ?
C2 C3 C4 120.1(7) . . ?
C2 C3 H3 119.9 . . ?
C4 C3 H3 119.9 . . ?
C3 C4 C12 126.5(6) . . ?
C3 C4 C5 118.3(6) . . ?
C12 C4 C5 115.3(6) . . ?
N1 C5 C4 121.0(6) . . ?
N1 C5 C6 117.5(6) . . ?
C4 C5 C6 121.4(6) . . ?
N2 C6 C10 122.7(6) . . ?
N2 C6 C5 117.2(6) . . ?
C10 C6 C5 120.1(6) . . ?
N2 C7 C8 123.7(7) . . ?
N2 C7 H7 118.2 . . ?
C8 C7 H7 118.2 . . ?
C9 C8 C7 118.5(7) . . ?
C9 C8 H8 120.8 . . ?
C7 C8 H8 120.8 . . ?
C8 C9 C10 120.1(7) . . ?
C8 C9 H9 119.9 . . ?
C10 C9 H9 119.9 . . ?
C9 C10 C6 117.4(7) . . ?
C9 C10 C11 125.1(7) . . ?
C6 C10 C11 117.4(6) . . ?
C12 C11 N3 111.0(6) . . ?
C12 C11 C10 121.4(7) . . ?
N3 C11 C10 127.6(7) . . ?
C11 C12 N4 105.3(6) . . ?
C11 C12 C4 124.0(6) . . ?
N4 C12 C4 130.6(7) . . ?
N3 C13 N4 112.1(7) . . ?
N3 C13 C14 123.4(7) . . ?
N4 C13 C14 124.4(7) . . ?
C15 C14 C19 118.0(8) . . ?
C15 C14 C13 119.9(8) . . ?
C19 C14 C13 122.1(7) . . ?
O1 C15 C16 117.1(9) . . ?
O1 C15 C14 121.4(8) . . ?
C16 C15 C14 121.5(9) . . ?
C15 C16 C17 120.0(10) . . ?
C15 C16 H16 120.0 . . ?
C17 C16 H16 120.0 . . ?
C16 C17 C18 121.5(9) . . ?
C16 C17 H17 119.3 . . ?
C18 C17 H17 119.3 . . ?
C19 C18 C17 116.6(10) . . ?
C19 C18 H18 121.7 . . ?
C17 C18 H18 121.7 . . ?
C18 C19 C14 122.5(9) . . ?
C18 C19 H19 118.8 . . ?
C14 C19 H19 118.8 . . ?
O2 C20 O3 121.3(7) . . ?
O2 C20 C21 120.0(8) . . ?
O3 C20 C21 118.7(8) . . ?
O2 C20 Tb1 62.4(4) . . ?
O3 C20 Tb1 59.1(4) . . ?
C21 C20 Tb1 176.1(6) . . ?
C20 C21 H21A 109.5 . . ?
C20 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
C20 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
O5 C22 O4 122.0(7) . 3_656 ?
O5 C22 C23 120.0(7) . . ?
O4 C22 C23 118.0(7) 3_656 . ?
O5 C22 Tb1 57.4(4) . . ?
O4 C22 Tb1 64.7(4) 3_656 . ?
C23 C22 Tb1 175.4(5) . . ?
C22 C23 H23A 109.5 . . ?
C22 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
C22 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
O7 C24 O6 124.8(7) . 3_656 ?
O7 C24 C25 118.7(7) . . ?
O6 C24 C25 116.5(7) 3_656 . ?
C24 C25 H25A 109.5 . . ?
C24 C25 H25B 109.5 . . ?
H25A C25 H25B 109.5 . . ?
C24 C25 H25C 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
C1 N1 C5 118.1(6) . . ?
C1 N1 Tb1 121.2(4) . . ?
C5 N1 Tb1 120.5(4) . . ?
C7 N2 C6 117.6(6) . . ?
C7 N2 Tb1 121.6(5) . . ?
C6 N2 Tb1 120.7(4) . . ?
C13 N3 C11 104.5(6) . . ?
C13 N4 C12 107.1(6) . . ?
C13 N4 H4 126.5 . . ?
C12 N4 H4 126.5 . . ?
C15 O1 H1H 109.5 . . ?
C20 O2 Tb1 91.6(4) . . ?
C20 O3 Tb1 94.9(5) . . ?
C22 O4 Tb1 164.9(5) 3_656 . ?
C22 O4 Tb1 89.4(4) 3_656 3_656 ?
Tb1 O4 Tb1 105.27(17) . 3_656 ?
C22 O5 Tb1 97.6(4) . . ?
C24 O6 Tb1 138.6(4) 3_656 . ?
C24 O7 Tb1 137.1(5) . . ?
O4 Tb1 O7 75.50(16) . . ?
O4 Tb1 O6 75.87(15) . . ?
O7 Tb1 O6 136.29(15) . . ?
O4 Tb1 O5 125.57(15) . . ?
O7 Tb1 O5 87.32(16) . . ?
O6 Tb1 O5 83.23(17) . . ?
O4 Tb1 O3 81.67(16) . . ?
O7 Tb1 O3 77.39(17) . . ?
O6 Tb1 O3 129.44(17) . . ?
O5 Tb1 O3 144.39(18) . . ?
O4 Tb1 O2 79.37(16) . . ?
O7 Tb1 O2 125.97(17) . . ?
O6 Tb1 O2 79.42(16) . . ?
O5 Tb1 O2 144.67(16) . . ?
O3 Tb1 O2 51.97(16) . . ?
O4 Tb1 N2 146.50(17) . . ?
O7 Tb1 N2 78.52(17) . . ?
O6 Tb1 N2 137.30(17) . . ?
O5 Tb1 N2 73.29(16) . . ?
O3 Tb1 N2 72.25(17) . . ?
O2 Tb1 N2 99.67(17) . . ?
O4 Tb1 N1 143.27(16) . . ?
O7 Tb1 N1 140.51(17) . . ?
O6 Tb1 N1 76.76(16) . . ?
O5 Tb1 N1 74.29(15) . . ?
O3 Tb1 N1 97.51(17) . . ?
O2 Tb1 N1 71.90(15) . . ?
N2 Tb1 N1 62.92(17) . . ?
O4 Tb1 O4 74.73(17) . 3_656 ?
O7 Tb1 O4 70.89(15) . 3_656 ?
O6 Tb1 O4 70.14(14) . 3_656 ?
O5 Tb1 O4 50.88(15) . 3_656 ?
O3 Tb1 O4 144.17(16) . 3_656 ?
O2 Tb1 O4 143.83(16) . 3_656 ?
N2 Tb1 O4 115.86(16) . 3_656 ?
N1 Tb1 O4 117.52(15) . 3_656 ?
O4 Tb1 C20 78.25(18) . . ?
O7 Tb1 C20 101.4(2) . . ?
O6 Tb1 C20 104.2(2) . . ?
O5 Tb1 C20 156.16(19) . . ?
O3 Tb1 C20 26.01(19) . . ?
O2 Tb1 C20 26.02(19) . . ?
N2 Tb1 C20 86.6(2) . . ?
N1 Tb1 C20 85.28(19) . . ?
O4 Tb1 C20 152.96(18) 3_656 . ?
O4 Tb1 C22 100.6(2) . . ?
O7 Tb1 C22 78.69(17) . . ?
O6 Tb1 C22 74.93(17) . . ?
O5 Tb1 C22 25.01(17) . . ?
O3 Tb1 C22 154.57(18) . . ?
O2 Tb1 C22 153.46(17) . . ?
N2 Tb1 C22 94.63(19) . . ?
N1 Tb1 C22 95.43(18) . . ?
O4 Tb1 C22 25.88(16) 3_656 . ?
C20 Tb1 C22 178.7(2) . . ?
O4 Tb1 Tb1 39.89(11) . 3_656 ?
O7 Tb1 Tb1 68.53(11) . 3_656 ?
O6 Tb1 Tb1 68.26(11) . 3_656 ?
O5 Tb1 Tb1 85.71(11) . 3_656 ?
O3 Tb1 Tb1 116.95(13) . 3_656 ?
O2 Tb1 Tb1 115.30(12) . 3_656 ?
N2 Tb1 Tb1 141.61(12) . 3_656 ?
N1 Tb1 Tb1 141.43(11) . 3_656 ?
O4 Tb1 Tb1 34.85(10) 3_656 3_656 ?
C20 Tb1 Tb1 118.13(15) . 3_656 ?
C22 Tb1 Tb1 60.70(15) . 3_656 ?

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
_geom_hbond_publ_flag
O1 H1H N3 0.82 1.86 2.593(8) 148.8 . yes
N4 H4 O2 0.86 1.99 2.836(8) 166.4 3_655 yes

_refine_diff_density_max         0.744
_refine_diff_density_min         -0.702
_refine_diff_density_rms         0.098



####################################################################### 
# 
# 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_shelx_CCDC3
_database_code_depnum_ccdc_archive 'CCDC 1860537'
_audit_update_record             
;
2018-08-06 deposited with the CCDC.
2018-10-30 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            'C50 H42 Dy2 N8 O14'
_chemical_formula_weight         1303.91

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

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/c'
_space_group_name_Hall           '-P 2ybc'

_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, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   11.4127(19)
_cell_length_b                   16.033(3)
_cell_length_c                   13.543(2)
_cell_angle_alpha                90
_cell_angle_beta                 103.302(3)
_cell_angle_gamma                90
_cell_volume                     2411.7(7)
_cell_formula_units_Z            2
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    2018
_cell_measurement_theta_min      2.46
_cell_measurement_theta_max      19.59

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.796
_exptl_crystal_F_000             1284
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.220
_exptl_crystal_size_mid          0.210
_exptl_crystal_size_min          0.190
_exptl_absorpt_coefficient_mu    3.152
_shelx_estimated_absorpt_T_min   0.544
_shelx_estimated_absorpt_T_max   0.586
_exptl_absorpt_correction_type   none
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'sealed tube'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            12258
_diffrn_reflns_av_unetI/netI     0.0672
_diffrn_reflns_av_R_equivalents  0.0559
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         1.834
_diffrn_reflns_theta_max         25.249
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             4371
_reflns_number_gt                2923
_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 APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_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)+(0.0455P)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         4371
_refine_ls_number_parameters     338
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0730
_refine_ls_R_factor_gt           0.0416
_refine_ls_wR_factor_ref         0.1017
_refine_ls_wR_factor_gt          0.0876
_refine_ls_goodness_of_fit_ref   0.982
_refine_ls_restrained_S_all      0.982
_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 0.0075(6) -0.0961(4) 0.6617(5) 0.0481(17) Uani 1 1 d . . . . .
H1 H -0.046587 -0.120426 0.694976 0.058 Uiso 1 1 calc R U . . .
C2 C 0.0123(6) -0.1266(5) 0.5665(5) 0.058(2) Uani 1 1 d . . . . .
H2 H -0.036929 -0.170427 0.537181 0.069 Uiso 1 1 calc R U . . .
C3 C 0.0908(6) -0.0908(4) 0.5172(5) 0.0534(19) Uani 1 1 d . . . . .
H3 H 0.093759 -0.109445 0.452834 0.064 Uiso 1 1 calc R U . . .
C4 C 0.1657(6) -0.0273(5) 0.5614(5) 0.0496(18) Uani 1 1 d . . . . .
C5 C 0.1590(6) -0.0008(5) 0.6609(5) 0.0493(18) Uani 1 1 d . . . . .
C6 C 0.2425(6) 0.0615(4) 0.7166(5) 0.0443(17) Uani 1 1 d . . . . .
C7 C 0.3067(7) 0.1360(5) 0.8625(6) 0.058(2) Uani 1 1 d . . . . .
H7 H 0.300020 0.150070 0.927565 0.070 Uiso 1 1 calc R U . . .
C8 C 0.4002(7) 0.1707(5) 0.8254(6) 0.061(2) Uani 1 1 d . . . . .
H8 H 0.453327 0.208085 0.864938 0.073 Uiso 1 1 calc R U . . .
C9 C 0.4131(6) 0.1500(5) 0.7324(5) 0.0552(19) Uani 1 1 d . . . . .
H9 H 0.475743 0.172426 0.707571 0.066 Uiso 1 1 calc R U . . .
C10 C 0.3325(6) 0.0951(4) 0.6738(5) 0.0463(17) Uani 1 1 d . . . . .
C11 C 0.3330(6) 0.0710(5) 0.5711(5) 0.0497(18) Uani 1 1 d . . . . .
C12 C 0.2532(6) 0.0135(4) 0.5195(5) 0.0449(17) Uani 1 1 d . . . . .
C13 C 0.3727(6) 0.0585(5) 0.4256(6) 0.0548(19) Uani 1 1 d . . . . .
C14 C 0.4272(7) 0.0693(5) 0.3392(6) 0.058(2) Uani 1 1 d . . . . .
C15 C 0.5309(7) 0.1180(5) 0.3498(6) 0.066(2) Uani 1 1 d . . . . .
C16 C 0.5877(8) 0.1286(6) 0.2699(7) 0.079(3) Uani 1 1 d . . . . .
H16 H 0.657361 0.160497 0.278311 0.095 Uiso 1 1 calc R U . . .
C17 C 0.5389(9) 0.0909(6) 0.1785(8) 0.087(3) Uani 1 1 d . . . . .
H17 H 0.575108 0.098890 0.124331 0.105 Uiso 1 1 calc R U . . .
C18 C 0.4381(8) 0.0419(6) 0.1655(7) 0.081(3) Uani 1 1 d . . . . .
H18 H 0.407724 0.015829 0.103538 0.097 Uiso 1 1 calc R U . . .
C19 C 0.3818(7) 0.0312(5) 0.2447(6) 0.069(2) Uani 1 1 d . . . . .
H19 H 0.313019 -0.001694 0.235352 0.083 Uiso 1 1 calc R U . . .
C20 C -0.0906(8) 0.1548(6) 0.7485(6) 0.061(2) Uani 1 1 d . . . . .
C21 C -0.1632(8) 0.2214(5) 0.6898(6) 0.083(3) Uani 1 1 d . . . . .
H21A H -0.188348 0.259767 0.735247 0.124 Uiso 1 1 calc R U . . .
H21B H -0.232793 0.197518 0.645144 0.124 Uiso 1 1 calc R U . . .
H21C H -0.115935 0.250386 0.650548 0.124 Uiso 1 1 calc R U . . .
C22 C 0.1834(6) -0.0953(5) 1.0046(5) 0.0495(18) Uani 1 1 d . . . . .
C23 C 0.2530(7) -0.1637(5) 1.0657(6) 0.075(2) Uani 1 1 d . . . . .
H23A H 0.200282 -0.209656 1.069382 0.113 Uiso 1 1 calc R U . . .
H23B H 0.287818 -0.143801 1.132910 0.113 Uiso 1 1 calc R U . . .
H23C H 0.315903 -0.181764 1.034196 0.113 Uiso 1 1 calc R U . . .
C24 C -0.1357(6) -0.1281(5) 0.9030(6) 0.0517(18) Uani 1 1 d . . . . .
C25 C -0.1947(8) -0.2056(5) 0.8546(6) 0.077(3) Uani 1 1 d . . . . .
H25A H -0.265922 -0.191124 0.804436 0.115 Uiso 1 1 calc R U . . .
H25B H -0.216052 -0.240414 0.905328 0.115 Uiso 1 1 calc R U . . .
H25C H -0.140027 -0.235035 0.822746 0.115 Uiso 1 1 calc R U . . .
N1 N 0.0768(5) -0.0338(3) 0.7077(4) 0.0480(14) Uani 1 1 d . . . . .
N2 N 0.2268(5) 0.0834(4) 0.8084(4) 0.0503(15) Uani 1 1 d . . . . .
N3 N 0.4097(5) 0.0982(4) 0.5127(5) 0.0579(16) Uani 1 1 d . . . . .
N4 N 0.2782(5) 0.0070(4) 0.4254(4) 0.0512(15) Uani 1 1 d . . . . .
H4 H 0.241235 -0.023663 0.375864 0.061 Uiso 1 1 calc R U . . .
O1 O 0.5827(5) 0.1578(4) 0.4387(5) 0.0802(17) Uani 1 1 d . . . . .
H1H H 0.546001 0.145801 0.482128 0.120 Uiso 1 1 calc R U . . .
O2 O -0.1227(5) 0.0785(3) 0.7329(3) 0.0609(13) Uani 1 1 d . . . . .
O3 O 0.0014(5) 0.1721(3) 0.8143(4) 0.0716(15) Uani 1 1 d . . . . .
O4 O -0.0990(4) 0.0621(3) 0.9631(3) 0.0505(12) Uani 1 1 d . . . . .
O5 O 0.2065(4) -0.0713(3) 0.9249(4) 0.0587(13) Uani 1 1 d . . . . .
O6 O -0.0747(4) -0.0867(3) 0.8535(3) 0.0532(12) Uani 1 1 d . . . . .
O7 O 0.1477(4) 0.1100(3) 1.0097(3) 0.0583(13) Uani 1 1 d . . . . .
Dy1 Dy 0.04709(3) 0.03033(2) 0.87485(2) 0.04405(14) 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 N1 1.337(8) . ?
C1 C2 1.391(9) . ?
C1 H1 0.9300 . ?
C2 C3 1.361(9) . ?
C2 H2 0.9300 . ?
C3 C4 1.375(9) . ?
C3 H3 0.9300 . ?
C4 C12 1.418(9) . ?
C4 C5 1.432(9) . ?
C5 N1 1.354(8) . ?
C5 C6 1.465(10) . ?
C6 N2 1.343(8) . ?
C6 C10 1.398(9) . ?
C7 N2 1.330(8) . ?
C7 C8 1.395(10) . ?
C7 H7 0.9300 . ?
C8 C9 1.343(9) . ?
C8 H8 0.9300 . ?
C9 C10 1.384(9) . ?
C9 H9 0.9300 . ?
C10 C11 1.444(9) . ?
C11 C12 1.369(9) . ?
C11 N3 1.379(8) . ?
C12 N4 1.372(8) . ?
C13 N3 1.321(9) . ?
C13 N4 1.357(9) . ?
C13 C14 1.457(10) . ?
C14 C15 1.398(10) . ?
C14 C19 1.405(11) . ?
C15 O1 1.369(9) . ?
C15 C16 1.393(10) . ?
C16 C17 1.375(12) . ?
C16 H16 0.9300 . ?
C17 C18 1.371(12) . ?
C17 H17 0.9300 . ?
C18 C19 1.382(10) . ?
C18 H18 0.9300 . ?
C19 H19 0.9300 . ?
C20 O3 1.243(9) . ?
C20 O2 1.280(9) . ?
C20 C21 1.468(10) . ?
C20 Dy1 2.854(8) . ?
C21 H21A 0.9600 . ?
C21 H21B 0.9600 . ?
C21 H21C 0.9600 . ?
C22 O5 1.230(8) . ?
C22 O4 1.263(7) 3_557 ?
C22 C23 1.489(9) . ?
C22 Dy1 2.882(7) . ?
C23 H23A 0.9600 . ?
C23 H23B 0.9600 . ?
C23 H23C 0.9600 . ?
C24 O7 1.255(8) 3_557 ?
C24 O6 1.260(8) . ?
C24 C25 1.492(9) . ?
C25 H25A 0.9600 . ?
C25 H25B 0.9600 . ?
C25 H25C 0.9600 . ?
N1 Dy1 2.578(5) . ?
N2 Dy1 2.567(5) . ?
N4 H4 0.8600 . ?
O1 H1H 0.8200 . ?
O2 Dy1 2.516(5) . ?
O3 Dy1 2.432(5) . ?
O4 Dy1 2.321(4) . ?
O4 Dy1 2.601(4) 3_557 ?
O5 Dy1 2.419(5) . ?
O6 Dy1 2.314(5) . ?
O7 Dy1 2.307(4) . ?
Dy1 Dy1 3.9075(8) 3_557 ?

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
N1 C1 C2 123.3(6) . . ?
N1 C1 H1 118.3 . . ?
C2 C1 H1 118.3 . . ?
C3 C2 C1 118.5(7) . . ?
C3 C2 H2 120.8 . . ?
C1 C2 H2 120.8 . . ?
C2 C3 C4 120.8(6) . . ?
C2 C3 H3 119.6 . . ?
C4 C3 H3 119.6 . . ?
C3 C4 C12 126.3(6) . . ?
C3 C4 C5 117.8(6) . . ?
C12 C4 C5 115.8(7) . . ?
N1 C5 C4 121.2(7) . . ?
N1 C5 C6 117.7(6) . . ?
C4 C5 C6 121.1(6) . . ?
N2 C6 C10 123.4(6) . . ?
N2 C6 C5 116.4(6) . . ?
C10 C6 C5 120.2(6) . . ?
N2 C7 C8 122.6(7) . . ?
N2 C7 H7 118.7 . . ?
C8 C7 H7 118.7 . . ?
C9 C8 C7 119.8(7) . . ?
C9 C8 H8 120.1 . . ?
C7 C8 H8 120.1 . . ?
C8 C9 C10 119.6(7) . . ?
C8 C9 H9 120.2 . . ?
C10 C9 H9 120.2 . . ?
C9 C10 C6 117.5(6) . . ?
C9 C10 C11 125.0(6) . . ?
C6 C10 C11 117.6(6) . . ?
C12 C11 N3 110.8(6) . . ?
C12 C11 C10 121.5(6) . . ?
N3 C11 C10 127.7(7) . . ?
C11 C12 N4 105.6(6) . . ?
C11 C12 C4 123.6(6) . . ?
N4 C12 C4 130.8(7) . . ?
N3 C13 N4 112.7(6) . . ?
N3 C13 C14 123.5(7) . . ?
N4 C13 C14 123.8(7) . . ?
C15 C14 C19 117.6(7) . . ?
C15 C14 C13 119.4(8) . . ?
C19 C14 C13 123.0(7) . . ?
O1 C15 C16 116.2(8) . . ?
O1 C15 C14 122.3(7) . . ?
C16 C15 C14 121.4(9) . . ?
C17 C16 C15 118.8(9) . . ?
C17 C16 H16 120.6 . . ?
C15 C16 H16 120.6 . . ?
C18 C17 C16 121.4(8) . . ?
C18 C17 H17 119.3 . . ?
C16 C17 H17 119.3 . . ?
C17 C18 C19 119.8(9) . . ?
C17 C18 H18 120.1 . . ?
C19 C18 H18 120.1 . . ?
C18 C19 C14 120.9(8) . . ?
C18 C19 H19 119.6 . . ?
C14 C19 H19 119.6 . . ?
O3 C20 O2 119.6(7) . . ?
O3 C20 C21 120.3(8) . . ?
O2 C20 C21 120.1(8) . . ?
O3 C20 Dy1 57.9(4) . . ?
O2 C20 Dy1 61.8(4) . . ?
C21 C20 Dy1 176.1(5) . . ?
C20 C21 H21A 109.5 . . ?
C20 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
C20 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
O5 C22 O4 120.4(7) . 3_557 ?
O5 C22 C23 121.6(6) . . ?
O4 C22 C23 118.1(7) 3_557 . ?
O5 C22 Dy1 56.0(4) . . ?
O4 C22 Dy1 64.5(4) 3_557 . ?
C23 C22 Dy1 176.3(5) . . ?
C22 C23 H23A 109.5 . . ?
C22 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
C22 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
O7 C24 O6 125.0(7) 3_557 . ?
O7 C24 C25 118.0(7) 3_557 . ?
O6 C24 C25 116.9(7) . . ?
C24 C25 H25A 109.5 . . ?
C24 C25 H25B 109.5 . . ?
H25A C25 H25B 109.5 . . ?
C24 C25 H25C 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
C1 N1 C5 118.2(6) . . ?
C1 N1 Dy1 121.6(4) . . ?
C5 N1 Dy1 120.0(5) . . ?
C7 N2 C6 117.0(6) . . ?
C7 N2 Dy1 121.2(4) . . ?
C6 N2 Dy1 121.7(5) . . ?
C13 N3 C11 104.2(6) . . ?
C13 N4 C12 106.6(6) . . ?
C13 N4 H4 126.7 . . ?
C12 N4 H4 126.7 . . ?
C15 O1 H1H 109.5 . . ?
C20 O2 Dy1 91.5(4) . . ?
C20 O3 Dy1 96.5(5) . . ?
C22 O4 Dy1 165.0(5) 3_557 . ?
C22 O4 Dy1 89.5(4) 3_557 3_557 ?
Dy1 O4 Dy1 104.98(17) . 3_557 ?
C22 O5 Dy1 99.1(4) . . ?
C24 O6 Dy1 138.6(4) . . ?
C24 O7 Dy1 136.9(4) 3_557 . ?
O7 Dy1 O6 136.34(15) . . ?
O7 Dy1 O4 75.89(16) . . ?
O6 Dy1 O4 76.14(16) . . ?
O7 Dy1 O5 86.89(17) . . ?
O6 Dy1 O5 83.11(18) . . ?
O4 Dy1 O5 125.89(15) . . ?
O7 Dy1 O3 77.17(18) . . ?
O6 Dy1 O3 129.81(18) . . ?
O4 Dy1 O3 81.06(17) . . ?
O5 Dy1 O3 144.37(18) . . ?
O7 Dy1 O2 126.16(18) . . ?
O6 Dy1 O2 79.58(17) . . ?
O4 Dy1 O2 78.92(15) . . ?
O5 Dy1 O2 144.88(16) . . ?
O3 Dy1 O2 52.25(17) . . ?
O7 Dy1 N2 78.54(17) . . ?
O6 Dy1 N2 136.95(17) . . ?
O4 Dy1 N2 146.53(18) . . ?
O5 Dy1 N2 73.25(17) . . ?
O3 Dy1 N2 72.45(18) . . ?
O2 Dy1 N2 99.63(17) . . ?
O7 Dy1 N1 140.68(17) . . ?
O6 Dy1 N1 76.33(16) . . ?
O4 Dy1 N1 142.66(17) . . ?
O5 Dy1 N1 74.67(16) . . ?
O3 Dy1 N1 97.93(18) . . ?
O2 Dy1 N1 71.67(16) . . ?
N2 Dy1 N1 63.09(18) . . ?
O7 Dy1 O4 70.89(16) . 3_557 ?
O6 Dy1 O4 69.90(15) . 3_557 ?
O4 Dy1 O4 75.02(17) . 3_557 ?
O5 Dy1 O4 50.90(14) . 3_557 ?
O3 Dy1 O4 143.76(16) . 3_557 ?
O2 Dy1 O4 143.63(16) . 3_557 ?
N2 Dy1 O4 116.08(16) . 3_557 ?
N1 Dy1 O4 117.59(16) . 3_557 ?
O7 Dy1 C20 101.1(2) . . ?
O6 Dy1 C20 105.1(2) . . ?
O4 Dy1 C20 78.08(18) . . ?
O5 Dy1 C20 156.03(18) . . ?
O3 Dy1 C20 25.6(2) . . ?
O2 Dy1 C20 26.6(2) . . ?
N2 Dy1 C20 86.1(2) . . ?
N1 Dy1 C20 85.29(19) . . ?
O4 Dy1 C20 153.06(17) 3_557 . ?
O7 Dy1 C22 78.68(18) . . ?
O6 Dy1 C22 74.55(18) . . ?
O4 Dy1 C22 100.97(19) . . ?
O5 Dy1 C22 24.93(16) . . ?
O3 Dy1 C22 154.48(19) . . ?
O2 Dy1 C22 153.27(19) . . ?
N2 Dy1 C22 94.75(19) . . ?
N1 Dy1 C22 95.47(18) . . ?
O4 Dy1 C22 25.99(16) 3_557 . ?
C20 Dy1 C22 179.0(2) . . ?
O7 Dy1 Dy1 68.74(11) . 3_557 ?
O6 Dy1 Dy1 68.22(11) . 3_557 ?
O4 Dy1 Dy1 40.01(11) . 3_557 ?
O5 Dy1 Dy1 85.89(11) . 3_557 ?
O3 Dy1 Dy1 116.39(13) . 3_557 ?
O2 Dy1 Dy1 114.95(11) . 3_557 ?
N2 Dy1 Dy1 142.00(12) . 3_557 ?
N1 Dy1 Dy1 141.30(13) . 3_557 ?
O4 Dy1 Dy1 35.01(10) 3_557 3_557 ?
C20 Dy1 Dy1 118.08(14) . 3_557 ?
C22 Dy1 Dy1 60.97(14) . 3_557 ?

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
_geom_hbond_publ_flag
O1 H1H N3 0.82 1.86 2.593(8) 147.8 . yes
N4 H4 O2 0.86 1.96 2.807(8) 166.1 3_556 yes

_refine_diff_density_max         1.107
_refine_diff_density_min         -0.896
_refine_diff_density_rms         0.118



