# 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_1
_database_code_depnum_ccdc_archive 'CCDC 1942683'
loop_
_audit_author_name
_audit_author_address
'Ana M. Garcia-Deibe'
;Universidade de Santiago de Compostela
Spain
;
_audit_update_record             
;
2020-06-04 deposited with the CCDC.	2020-06-05 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/1
_shelx_SHELXL_version_number     2018/1
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C19 H14 Dy N5 O8, 1.15(C5 H5 N), 0.3(C7 H8)'
_chemical_formula_sum            'C26.85 H22.15 Dy N6.15 O8'
_chemical_formula_weight         721.46

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

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

_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, -z'

_cell_length_a                   9.8073(10)
_cell_length_b                   10.4055(12)
_cell_length_c                   13.9823(15)
_cell_angle_alpha                86.328(4)
_cell_angle_beta                 82.101(4)
_cell_angle_gamma                74.962(4)
_cell_volume                     1364.4(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    1962
_cell_measurement_theta_min      2.54
_cell_measurement_theta_max      27.98

_exptl_crystal_description       plate
_exptl_crystal_colour            red
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.756
_exptl_crystal_F_000             713
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.180
_exptl_crystal_size_mid          0.040
_exptl_crystal_size_min          0.020
_exptl_absorpt_coefficient_mu    2.800
_shelx_estimated_absorpt_T_min   0.633
_shelx_estimated_absorpt_T_max   0.946
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6237
_exptl_absorpt_correction_T_max  0.6750
_exptl_absorpt_process_details   
;
 SADABS 2016/2: Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D.,
 J. Appl. Cryst. 48 (2015) 3-10
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            74232
_diffrn_reflns_av_unetI/netI     0.0248
_diffrn_reflns_av_R_equivalents  0.0501
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         2.462
_diffrn_reflns_theta_max         28.332
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measured_fraction_theta_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_point_group_measured_fraction_full 0.997
_reflns_number_total             6798
_reflns_number_gt                6203
_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 APEX3'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXT-2014/1 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2018/1 (Sheldrick, 2018)'
_computing_molecular_graphics    'SHELXT-2018/1 (Sheldrick, 2018)'
_computing_publication_material  'WinGX 2018.3 (Farrugia, 2012)'
_refine_special_details          
;
Details:
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 N2S_1-C6S_1 = N2S_1-C10S_1
 1.33 with sigma of 0.02
 C6S_1-C7S_1 = C8S_1-C9S_1
 1.37 with sigma of 0.02
 C8S_1-C10S_1
 2.38 with sigma of 0.04
 N2S_1-C7S_1
 2.4 with sigma of 0.04
 N2S_1-C9S_1
 2.38 with sigma of 0.04
 C6S_1-C8S_1
 2.38 with sigma of 0.04
 C6S_1-C7S_1 ? C7S_1-C8S_1 ? C8S_1-C9S_1 ? C9S_1-C10S_1
 with sigma of 0.02
 C8S_1-C10S_1 ? C8S_1-C6S_1 ? C9S_1-C7S_1 ? C10S_1-C6S_1
 with sigma of 0.04
 N2S_1-C6S_1 ? N2S_1-C10S_1
 with sigma of 0.02
3. Restrained planarity
 N2S_1, C6S_1, C7S_1, C8S_1, C9S_1, C10S_1
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 1A with sigma of 0.04 and sigma
for terminal atoms of 0.08
5. Rigid body (RIGU) restrains
 C11S, C12S, C13S, C14S, C15S, C16S, C17S
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 N2S_1, C6S_1, C7S_1, C8S_1, C9S_1, C10S_1
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 Fixed Sof: C11S(0.3) C12S(0.3) H12S(0.3) C13S(0.3) H13S(0.3) C14S(0.3)
 H14S(0.3) C15S(0.3) H15S(0.3) C16S(0.3) H16S(0.3) C17S(0.3) H17a(0.3)
 H17b(0.3) H17c(0.3) N2S(0.15) C6S(0.15) H6S(0.15) C7S(0.15) H7S(0.15)
 C8S(0.15) H8S(0.15) C9S(0.15) H9S(0.15) C10S(0.15) H10S(0.15)
 Fixed Uiso: N2S(0.04) C6S(0.04) H6S(0.04) C7S(0.04) H7S(0.04) C8S(0.04)
 H8S(0.04) C9S(0.04) H9S(0.04) C10S(0.04) H10S(0.04)
7.a Riding coordinates:
 O2(H2)
7.b Aromatic/amide H refined with riding coordinates:
 C2(H2a), C3(H3), C4(H4), C5(H5), C7(H7), C9(H9), C10(H10), C11(H11), C13(H13),
  C15(H15), C16(H16), C17(H17), C18(H18), C1S(H1S), C2S(H2S), C3S(H3S),
 C4S(H4S), C5S(H5S), C12S(H12S), C13S(H13S), C14S(H14S), C15S(H15S), C16S(H16S),
  C6S(H6S), C7S(H7S), C8S(H8S), C9S(H9S), C10S(H10S)
7.c Fitted hexagon refined as free rotating group:
 C11S(C12S,C13S,C14S,C15S,C16S)
7.d Idealised Me refined as rotating group:
 C17S(H17a,H17b,H17c)
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0166P)²+1.3172P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         6798
_refine_ls_number_parameters     423
_refine_ls_number_restraints     127
_refine_ls_R_factor_all          0.0277
_refine_ls_R_factor_gt           0.0224
_refine_ls_wR_factor_ref         0.0486
_refine_ls_wR_factor_gt          0.0462
_refine_ls_goodness_of_fit_ref   1.083
_refine_ls_restrained_S_all      1.075
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Dy1 Dy 0.67605(2) 0.70084(2) 0.66854(2) 0.01931(4) Uani 1 1 d . . . . .
O1 O 0.78289(17) 0.56593(18) 0.78243(12) 0.0258(4) Uani 1 1 d . . . . .
O2 O 0.45383(16) 0.80703(17) 0.75390(12) 0.0228(3) Uani 1 1 d . . . . .
H2P H 0.437700 0.796592 0.818008 0.065(14) Uiso 1 1 d R . . . .
N1 N 0.9372(2) 0.63545(19) 0.62602(14) 0.0213(4) Uani 1 1 d . . . . .
N2 N 0.7640(2) 0.73961(19) 0.49639(14) 0.0211(4) Uani 1 1 d . . . . .
N3 N 0.4885(2) 0.80387(19) 0.56290(14) 0.0200(4) Uani 1 1 d . . . . .
O11 O 0.53141(18) 0.53958(17) 0.69462(12) 0.0268(4) Uani 1 1 d . . . . .
O12 O 0.70675(18) 0.49654(18) 0.58022(13) 0.0286(4) Uani 1 1 d . . . . .
O21 O 0.68994(19) 0.93271(17) 0.63868(13) 0.0285(4) Uani 1 1 d . . . . .
O22 O 0.72691(19) 0.85339(18) 0.78170(13) 0.0302(4) Uani 1 1 d . . . . .
C1 C 0.9215(2) 0.5445(2) 0.78496(18) 0.0237(5) Uani 1 1 d . . . . .
C2 C 0.9866(3) 0.4865(3) 0.86604(19) 0.0295(6) Uani 1 1 d . . . . .
H2 H 0.930321 0.462515 0.921746 0.035 Uiso 1 1 calc R U . . .
C3 C 1.1324(3) 0.4640(3) 0.8656(2) 0.0319(6) Uani 1 1 d . . . . .
H3 H 1.174466 0.424157 0.921144 0.038 Uiso 1 1 calc R U . . .
C4 C 1.2181(3) 0.4983(3) 0.7860(2) 0.0299(6) Uani 1 1 d . . . . .
H4 H 1.317618 0.482980 0.787287 0.036 Uiso 1 1 calc R U . . .
C5 C 1.1579(3) 0.5546(2) 0.70497(19) 0.0255(5) Uani 1 1 d . . . . .
H5 H 1.215971 0.577478 0.649792 0.031 Uiso 1 1 calc R U . . .
C6 C 1.0109(2) 0.5782(2) 0.70401(17) 0.0215(5) Uani 1 1 d . . . . .
C7 C 0.9966(2) 0.6503(2) 0.53987(17) 0.0226(5) Uani 1 1 d . . . . .
H7 H 1.097157 0.624479 0.524552 0.027 Uiso 1 1 calc R U . . .
C8 C 0.9047(3) 0.7084(2) 0.46583(17) 0.0219(5) Uani 1 1 d . . . . .
C9 C 0.9578(3) 0.7295(2) 0.36996(18) 0.0264(5) Uani 1 1 d . . . . .
H9 H 1.057339 0.706269 0.349588 0.032 Uiso 1 1 calc R U . . .
C10 C 0.8624(3) 0.7850(2) 0.30518(18) 0.0272(5) Uani 1 1 d . . . . .
H10 H 0.896005 0.800153 0.239488 0.033 Uiso 1 1 calc R U . . .
C11 C 0.7177(3) 0.8183(2) 0.33655(17) 0.0247(5) Uani 1 1 d . . . . .
H11 H 0.650877 0.856853 0.293049 0.030 Uiso 1 1 calc R U . . .
C12 C 0.6724(3) 0.7939(2) 0.43327(16) 0.0216(5) Uani 1 1 d . . . . .
C13 C 0.5213(3) 0.8296(2) 0.47309(17) 0.0223(5) Uani 1 1 d . . . . .
H13 H 0.449833 0.870679 0.433385 0.027 Uiso 1 1 calc R U . . .
C14 C 0.3461(2) 0.8398(2) 0.60923(17) 0.0203(5) Uani 1 1 d . . . . .
C15 C 0.2248(3) 0.8742(2) 0.56221(18) 0.0234(5) Uani 1 1 d . . . . .
H15 H 0.233570 0.874696 0.493678 0.028 Uiso 1 1 calc R U . . .
C16 C 0.0911(3) 0.9076(2) 0.61554(19) 0.0249(5) Uani 1 1 d . . . . .
H16 H 0.008157 0.932102 0.583695 0.030 Uiso 1 1 calc R U . . .
C17 C 0.0792(3) 0.9052(2) 0.71570(19) 0.0257(5) Uani 1 1 d . . . . .
H17 H -0.012622 0.926619 0.752004 0.031 Uiso 1 1 calc R U . . .
C18 C 0.1983(3) 0.8722(2) 0.76347(18) 0.0237(5) Uani 1 1 d . . . . .
H18 H 0.188283 0.872356 0.832015 0.028 Uiso 1 1 calc R U . . .
C19 C 0.3337(2) 0.8385(2) 0.71059(17) 0.0202(5) Uani 1 1 d . . . . .
N10 N 0.6069(2) 0.4585(2) 0.63231(15) 0.0254(4) Uani 1 1 d . . . . .
O10 O 0.5858(2) 0.3497(2) 0.62373(15) 0.0427(5) Uani 1 1 d . . . . .
N20 N 0.7076(2) 0.9541(2) 0.72356(17) 0.0307(5) Uani 1 1 d . . . . .
O20 O 0.7089(3) 1.0645(2) 0.74706(18) 0.0577(7) Uani 1 1 d . . . . .
N1S N 0.4416(2) 0.7523(2) 0.93208(15) 0.0284(5) Uani 1 1 d . . . . .
C1S C 0.3723(3) 0.6684(3) 0.9802(2) 0.0365(6) Uani 1 1 d . . . . .
H1SA H 0.318611 0.626843 0.946226 0.044 Uiso 1 1 calc R U . . .
C2S C 0.3764(3) 0.6401(3) 1.0781(2) 0.0403(7) Uani 1 1 d . . . . .
H2S H 0.327599 0.579145 1.110998 0.048 Uiso 1 1 calc R U . . .
C3S C 0.4530(3) 0.7025(3) 1.1266(2) 0.0414(7) Uani 1 1 d . . . . .
H3S H 0.455455 0.687119 1.194088 0.050 Uiso 1 1 calc R U . . .
C4S C 0.5257(4) 0.7870(4) 1.0767(2) 0.0463(8) Uani 1 1 d . . . . .
H4S H 0.580627 0.829212 1.108976 0.056 Uiso 1 1 calc R U . . .
C5S C 0.5184(3) 0.8100(3) 0.9789(2) 0.0403(7) Uani 1 1 d . . . . .
H5S H 0.569160 0.868264 0.944291 0.048 Uiso 1 1 calc R U . . .
C11S C 0.9570(8) 0.9280(6) 0.9917(6) 0.0292(18) Uani 0.3 1 d G U P A -1
C12S C 1.0693(8) 0.9124(7) 1.0458(5) 0.035(2) Uani 0.3 1 d G U P A -1
H1S2 H 1.105136 0.829522 1.077678 0.042 Uiso 0.3 1 calc R U P A -1
C13S C 1.1292(8) 1.0181(9) 1.0533(6) 0.041(2) Uani 0.3 1 d G U P A -1
H13S H 1.205937 1.007465 1.090223 0.049 Uiso 0.3 1 calc R U P A -1
C14S C 1.0767(9) 1.1394(7) 1.0066(8) 0.053(3) Uani 0.3 1 d G U P A -1
H14S H 1.117634 1.211637 1.011742 0.064 Uiso 0.3 1 calc R U P A -1
C15S C 0.9644(10) 1.1550(7) 0.9526(9) 0.039(2) Uani 0.3 1 d G U P A -1
H15S H 0.928528 1.237869 0.920717 0.047 Uiso 0.3 1 calc R U P A -1
C16S C 0.9045(9) 1.0493(8) 0.9451(8) 0.034(3) Uani 0.3 1 d G U P A -1
H16S H 0.827725 1.059927 0.908172 0.041 Uiso 0.3 1 calc R U P A -1
C17S C 0.8922(15) 0.8291(13) 0.9810(9) 0.044(3) Uani 0.3 1 d . . P A -1
H17A H 0.960624 0.755726 0.946319 0.066 Uiso 0.3 1 calc R U P A -1
H17B H 0.811589 0.864104 0.944252 0.066 Uiso 0.3 1 calc R U P A -1
H17C H 0.858013 0.796529 1.044791 0.066 Uiso 0.3 1 calc R U P A -1
N2S_1 N 0.921(3) 1.066(2) 0.941(2) 0.040 Uiso 0.15 1 d D U P B -2
C6S_1 C 0.998(3) 1.145(2) 0.9647(19) 0.040 Uiso 0.15 1 d D U P B -2
H6S_1 H 0.985642 1.233200 0.939480 0.040 Uiso 0.15 1 calc R U P B -2
C7S_1 C 1.097(2) 1.092(2) 1.0271(17) 0.040 Uiso 0.15 1 d D U P B -2
H7S_1 H 1.155306 1.143345 1.045921 0.040 Uiso 0.15 1 calc R U P B -2
C8S_1 C 1.110(3) 0.963(2) 1.062(2) 0.040 Uiso 0.15 1 d D U P B -2
H8S_1 H 1.177692 0.926862 1.105167 0.040 Uiso 0.15 1 calc R U P B -2
C9S_1 C 1.029(3) 0.885(2) 1.035(2) 0.040 Uiso 0.15 1 d D U P B -2
H9S_1 H 1.043318 0.794653 1.056688 0.040 Uiso 0.15 1 calc R U P B -2
C10S_1 C 0.925(3) 0.942(2) 0.976(2) 0.040 Uiso 0.15 1 d D U P B -2
H10S_1 H 0.860250 0.895294 0.960659 0.040 Uiso 0.15 1 calc R U P B -2


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Dy1 O1 2.2391(16) . ?
Dy1 O2 2.3663(16) . ?
Dy1 O11 2.4445(17) . ?
Dy1 O12 2.4570(18) . ?
Dy1 O21 2.4576(18) . ?
Dy1 N1 2.4713(19) . ?
Dy1 N2 2.4872(19) . ?
Dy1 O22 2.4944(18) . ?
Dy1 N3 2.4971(19) . ?
O1 C1 1.325(3) . ?
O2 C19 1.354(3) . ?
O2 H2P 0.8932 . ?
N1 C7 1.282(3) . ?
N1 C6 1.406(3) . ?
N2 C12 1.340(3) . ?
N2 C8 1.347(3) . ?
N3 C13 1.282(3) . ?
N3 C14 1.422(3) . ?
O11 N10 1.270(3) . ?
O12 N10 1.270(3) . ?
O21 N20 1.264(3) . ?
O22 N20 1.275(3) . ?
C1 C2 1.403(3) . ?
C1 C6 1.417(3) . ?
C2 C3 1.387(4) . ?
C2 H2 0.9500 . ?
C3 C4 1.386(4) . ?
C3 H3 0.9500 . ?
C4 C5 1.376(4) . ?
C4 H4 0.9500 . ?
C5 C6 1.400(3) . ?
C5 H5 0.9500 . ?
C7 C8 1.464(3) . ?
C7 H7 0.9500 . ?
C8 C9 1.395(3) . ?
C9 C10 1.384(4) . ?
C9 H9 0.9500 . ?
C10 C11 1.386(4) . ?
C10 H10 0.9500 . ?
C11 C12 1.393(3) . ?
C11 H11 0.9500 . ?
C12 C13 1.469(3) . ?
C13 H13 0.9500 . ?
C14 C15 1.393(3) . ?
C14 C19 1.405(3) . ?
C15 C16 1.387(3) . ?
C15 H15 0.9500 . ?
C16 C17 1.388(4) . ?
C16 H16 0.9500 . ?
C17 C18 1.380(3) . ?
C17 H17 0.9500 . ?
C18 C19 1.398(3) . ?
C18 H18 0.9500 . ?
N10 O10 1.219(3) . ?
N20 O20 1.219(3) . ?
N1S C5S 1.333(4) . ?
N1S C1S 1.336(4) . ?
C1S C2S 1.386(4) . ?
C1S H1SA 0.9500 . ?
C2S C3S 1.376(5) . ?
C2S H2S 0.9500 . ?
C3S C4S 1.370(5) . ?
C3S H3S 0.9500 . ?
C4S C5S 1.381(4) . ?
C4S H4S 0.9500 . ?
C5S H5S 0.9500 . ?
C11S C17S 1.368(14) . ?
C11S C12S 1.3900 . ?
C11S C16S 1.3900 . ?
C12S C13S 1.3900 . ?
C12S H1S2 0.9500 . ?
C13S C14S 1.3900 . ?
C13S H13S 0.9500 . ?
C14S C15S 1.3900 . ?
C14S H14S 0.9500 . ?
C15S C16S 1.3900 . ?
C15S H15S 0.9500 . ?
C16S H16S 0.9500 . ?
C17S H17A 0.9800 . ?
C17S H17B 0.9800 . ?
C17S H17C 0.9800 . ?
N2S_1 C6S_1 1.331(13) . ?
N2S_1 C10S_1 1.341(12) . ?
C6S_1 C7S_1 1.379(10) . ?
C6S_1 H6S_1 0.9500 . ?
C7S_1 C8S_1 1.373(15) . ?
C7S_1 H7S_1 0.9500 . ?
C8S_1 C9S_1 1.373(10) . ?
C8S_1 H8S_1 0.9500 . ?
C9S_1 C10S_1 1.388(15) . ?
C9S_1 H9S_1 0.9500 . ?
C10S_1 H10S_1 0.9500 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Dy1 O2 102.42(6) . . ?
O1 Dy1 O11 78.95(6) . . ?
O2 Dy1 O11 72.18(6) . . ?
O1 Dy1 O12 85.54(6) . . ?
O2 Dy1 O12 121.31(6) . . ?
O11 Dy1 O12 52.22(6) . . ?
O1 Dy1 O21 123.65(6) . . ?
O2 Dy1 O21 81.62(6) . . ?
O11 Dy1 O21 149.05(6) . . ?
O12 Dy1 O21 140.12(6) . . ?
O1 Dy1 N1 68.44(6) . . ?
O2 Dy1 N1 157.97(6) . . ?
O11 Dy1 N1 122.90(6) . . ?
O12 Dy1 N1 78.97(6) . . ?
O21 Dy1 N1 87.14(6) . . ?
O1 Dy1 N2 130.28(6) . . ?
O2 Dy1 N2 127.28(6) . . ?
O11 Dy1 N2 114.51(6) . . ?
O12 Dy1 N2 71.09(6) . . ?
O21 Dy1 N2 69.18(6) . . ?
N1 Dy1 N2 64.42(6) . . ?
O1 Dy1 O22 75.26(6) . . ?
O2 Dy1 O22 73.85(6) . . ?
O11 Dy1 O22 131.14(6) . . ?
O12 Dy1 O22 158.18(6) . . ?
O21 Dy1 O22 51.59(6) . . ?
N1 Dy1 O22 84.31(6) . . ?
N2 Dy1 O22 113.88(6) . . ?
O1 Dy1 N3 158.34(6) . . ?
O2 Dy1 N3 65.88(6) . . ?
O11 Dy1 N3 80.03(6) . . ?
O12 Dy1 N3 85.73(6) . . ?
O21 Dy1 N3 74.31(6) . . ?
N1 Dy1 N3 128.87(6) . . ?
N2 Dy1 N3 64.45(6) . . ?
O22 Dy1 N3 115.84(6) . . ?
O1 Dy1 N10 79.67(6) . . ?
O2 Dy1 N10 97.37(6) . . ?
O11 Dy1 N10 26.14(6) . . ?
O12 Dy1 N10 26.18(6) . . ?
O21 Dy1 N10 156.46(6) . . ?
N1 Dy1 N10 100.41(6) . . ?
N2 Dy1 N10 93.84(6) . . ?
O22 Dy1 N10 150.71(6) . . ?
N3 Dy1 N10 83.78(6) . . ?
O1 Dy1 N20 100.38(7) . . ?
O2 Dy1 N20 74.51(6) . . ?
O11 Dy1 N20 145.63(6) . . ?
O12 Dy1 N20 161.82(6) . . ?
O21 Dy1 N20 25.70(6) . . ?
N1 Dy1 N20 87.18(6) . . ?
N2 Dy1 N20 92.37(7) . . ?
O22 Dy1 N20 26.02(6) . . ?
N3 Dy1 N20 94.02(6) . . ?
N10 Dy1 N20 171.74(6) . . ?
C1 O1 Dy1 120.72(15) . . ?
C19 O2 Dy1 121.09(14) . . ?
C19 O2 H2P 113.4 . . ?
Dy1 O2 H2P 120.5 . . ?
C7 N1 C6 124.5(2) . . ?
C7 N1 Dy1 121.96(16) . . ?
C6 N1 Dy1 113.47(14) . . ?
C12 N2 C8 119.2(2) . . ?
C12 N2 Dy1 120.51(15) . . ?
C8 N2 Dy1 120.31(15) . . ?
C13 N3 C14 122.4(2) . . ?
C13 N3 Dy1 121.10(16) . . ?
C14 N3 Dy1 116.33(14) . . ?
N10 O11 Dy1 95.85(13) . . ?
N10 O12 Dy1 95.24(13) . . ?
N20 O21 Dy1 96.86(14) . . ?
N20 O22 Dy1 94.82(14) . . ?
O1 C1 C2 122.2(2) . . ?
O1 C1 C6 120.6(2) . . ?
C2 C1 C6 117.2(2) . . ?
C3 C2 C1 120.6(2) . . ?
C3 C2 H2 119.7 . . ?
C1 C2 H2 119.7 . . ?
C4 C3 C2 121.4(2) . . ?
C4 C3 H3 119.3 . . ?
C2 C3 H3 119.3 . . ?
C5 C4 C3 119.5(2) . . ?
C5 C4 H4 120.2 . . ?
C3 C4 H4 120.2 . . ?
C4 C5 C6 119.9(2) . . ?
C4 C5 H5 120.1 . . ?
C6 C5 H5 120.1 . . ?
C5 C6 N1 125.1(2) . . ?
C5 C6 C1 121.4(2) . . ?
N1 C6 C1 113.5(2) . . ?
N1 C7 C8 118.0(2) . . ?
N1 C7 H7 121.0 . . ?
C8 C7 H7 121.0 . . ?
N2 C8 C9 121.9(2) . . ?
N2 C8 C7 115.3(2) . . ?
C9 C8 C7 122.8(2) . . ?
C10 C9 C8 118.6(2) . . ?
C10 C9 H9 120.7 . . ?
C8 C9 H9 120.7 . . ?
C9 C10 C11 119.7(2) . . ?
C9 C10 H10 120.1 . . ?
C11 C10 H10 120.1 . . ?
C10 C11 C12 118.5(2) . . ?
C10 C11 H11 120.7 . . ?
C12 C11 H11 120.7 . . ?
N2 C12 C11 122.2(2) . . ?
N2 C12 C13 115.8(2) . . ?
C11 C12 C13 122.0(2) . . ?
N3 C13 C12 118.1(2) . . ?
N3 C13 H13 120.9 . . ?
C12 C13 H13 120.9 . . ?
C15 C14 C19 120.3(2) . . ?
C15 C14 N3 125.3(2) . . ?
C19 C14 N3 114.4(2) . . ?
C16 C15 C14 119.9(2) . . ?
C16 C15 H15 120.0 . . ?
C14 C15 H15 120.0 . . ?
C15 C16 C17 119.7(2) . . ?
C15 C16 H16 120.2 . . ?
C17 C16 H16 120.2 . . ?
C18 C17 C16 121.2(2) . . ?
C18 C17 H17 119.4 . . ?
C16 C17 H17 119.4 . . ?
C17 C18 C19 119.7(2) . . ?
C17 C18 H18 120.1 . . ?
C19 C18 H18 120.1 . . ?
O2 C19 C18 122.1(2) . . ?
O2 C19 C14 118.7(2) . . ?
C18 C19 C14 119.2(2) . . ?
O10 N10 O11 121.8(2) . . ?
O10 N10 O12 121.9(2) . . ?
O11 N10 O12 116.2(2) . . ?
O10 N10 Dy1 173.68(18) . . ?
O11 N10 Dy1 58.01(11) . . ?
O12 N10 Dy1 58.58(11) . . ?
O20 N20 O21 121.4(2) . . ?
O20 N20 O22 122.5(2) . . ?
O21 N20 O22 116.2(2) . . ?
O20 N20 Dy1 174.66(19) . . ?
O21 N20 Dy1 57.44(12) . . ?
O22 N20 Dy1 59.16(12) . . ?
C5S N1S C1S 119.4(2) . . ?
N1S C1S C2S 122.0(3) . . ?
N1S C1S H1SA 119.0 . . ?
C2S C1S H1SA 119.0 . . ?
C3S C2S C1S 118.3(3) . . ?
C3S C2S H2S 120.8 . . ?
C1S C2S H2S 120.8 . . ?
C4S C3S C2S 119.5(3) . . ?
C4S C3S H3S 120.2 . . ?
C2S C3S H3S 120.2 . . ?
C3S C4S C5S 119.3(3) . . ?
C3S C4S H4S 120.3 . . ?
C5S C4S H4S 120.3 . . ?
N1S C5S C4S 121.4(3) . . ?
N1S C5S H5S 119.3 . . ?
C4S C5S H5S 119.3 . . ?
C17S C11S C12S 123.6(7) . . ?
C17S C11S C16S 116.4(7) . . ?
C12S C11S C16S 120.0 . . ?
C11S C12S C13S 120.0 . . ?
C11S C12S H1S2 120.0 . . ?
C13S C12S H1S2 120.0 . . ?
C14S C13S C12S 120.0 . . ?
C14S C13S H13S 120.0 . . ?
C12S C13S H13S 120.0 . . ?
C13S C14S C15S 120.0 . . ?
C13S C14S H14S 120.0 . . ?
C15S C14S H14S 120.0 . . ?
C16S C15S C14S 120.0 . . ?
C16S C15S H15S 120.0 . . ?
C14S C15S H15S 120.0 . . ?
C15S C16S C11S 120.0 . . ?
C15S C16S H16S 120.0 . . ?
C11S C16S H16S 120.0 . . ?
C11S C17S H17A 109.5 . . ?
C11S C17S H17B 109.5 . . ?
H17A C17S H17B 109.5 . . ?
C11S C17S H17C 109.5 . . ?
H17A C17S H17C 109.5 . . ?
H17B C17S H17C 109.5 . . ?
C6S_1 N2S_1 C10S_1 126.1(16) . . ?
N2S_1 C6S_1 C7S_1 117.3(14) . . ?
N2S_1 C6S_1 H6S_1 121.4 . . ?
C7S_1 C6S_1 H6S_1 121.4 . . ?
C8S_1 C7S_1 C6S_1 118.9(14) . . ?
C8S_1 C7S_1 H7S_1 120.6 . . ?
C6S_1 C7S_1 H7S_1 120.6 . . ?
C7S_1 C8S_1 C9S_1 122.1(13) . . ?
C7S_1 C8S_1 H8S_1 119.0 . . ?
C9S_1 C8S_1 H8S_1 119.0 . . ?
C8S_1 C9S_1 C10S_1 118.1(14) . . ?
C8S_1 C9S_1 H9S_1 121.0 . . ?
C10S_1 C9S_1 H9S_1 121.0 . . ?
N2S_1 C10S_1 C9S_1 117.2(14) . . ?
N2S_1 C10S_1 H10S_1 121.4 . . ?
C9S_1 C10S_1 H10S_1 121.4 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Dy1 O1 C1 C2 165.16(19) . . . . ?
Dy1 O1 C1 C6 -15.7(3) . . . . ?
O1 C1 C2 C3 179.1(2) . . . . ?
C6 C1 C2 C3 0.0(4) . . . . ?
C1 C2 C3 C4 0.4(4) . . . . ?
C2 C3 C4 C5 -0.7(4) . . . . ?
C3 C4 C5 C6 0.7(4) . . . . ?
C4 C5 C6 N1 179.7(2) . . . . ?
C4 C5 C6 C1 -0.4(4) . . . . ?
C7 N1 C6 C5 14.0(4) . . . . ?
Dy1 N1 C6 C5 -167.83(19) . . . . ?
C7 N1 C6 C1 -166.0(2) . . . . ?
Dy1 N1 C6 C1 12.2(2) . . . . ?
O1 C1 C6 C5 -179.2(2) . . . . ?
C2 C1 C6 C5 0.0(4) . . . . ?
O1 C1 C6 N1 0.8(3) . . . . ?
C2 C1 C6 N1 179.9(2) . . . . ?
C6 N1 C7 C8 178.3(2) . . . . ?
Dy1 N1 C7 C8 0.2(3) . . . . ?
C12 N2 C8 C9 -0.8(3) . . . . ?
Dy1 N2 C8 C9 -179.62(17) . . . . ?
C12 N2 C8 C7 179.6(2) . . . . ?
Dy1 N2 C8 C7 0.8(3) . . . . ?
N1 C7 C8 N2 -0.7(3) . . . . ?
N1 C7 C8 C9 179.8(2) . . . . ?
N2 C8 C9 C10 0.5(4) . . . . ?
C7 C8 C9 C10 180.0(2) . . . . ?
C8 C9 C10 C11 0.1(4) . . . . ?
C9 C10 C11 C12 -0.3(4) . . . . ?
C8 N2 C12 C11 0.6(3) . . . . ?
Dy1 N2 C12 C11 179.40(17) . . . . ?
C8 N2 C12 C13 -177.8(2) . . . . ?
Dy1 N2 C12 C13 1.0(3) . . . . ?
C10 C11 C12 N2 0.0(4) . . . . ?
C10 C11 C12 C13 178.3(2) . . . . ?
C14 N3 C13 C12 177.2(2) . . . . ?
Dy1 N3 C13 C12 1.4(3) . . . . ?
N2 C12 C13 N3 -1.6(3) . . . . ?
C11 C12 C13 N3 -180.0(2) . . . . ?
C13 N3 C14 C15 17.1(4) . . . . ?
Dy1 N3 C14 C15 -167.00(18) . . . . ?
C13 N3 C14 C19 -163.0(2) . . . . ?
Dy1 N3 C14 C19 12.9(2) . . . . ?
C19 C14 C15 C16 0.2(4) . . . . ?
N3 C14 C15 C16 -179.9(2) . . . . ?
C14 C15 C16 C17 -0.7(4) . . . . ?
C15 C16 C17 C18 1.1(4) . . . . ?
C16 C17 C18 C19 -1.0(4) . . . . ?
Dy1 O2 C19 C18 164.89(17) . . . . ?
Dy1 O2 C19 C14 -16.5(3) . . . . ?
C17 C18 C19 O2 179.1(2) . . . . ?
C17 C18 C19 C14 0.5(4) . . . . ?
C15 C14 C19 O2 -178.8(2) . . . . ?
N3 C14 C19 O2 1.3(3) . . . . ?
C15 C14 C19 C18 -0.1(3) . . . . ?
N3 C14 C19 C18 -180.0(2) . . . . ?
Dy1 O11 N10 O10 172.6(2) . . . . ?
Dy1 O11 N10 O12 -6.7(2) . . . . ?
Dy1 O12 N10 O10 -172.6(2) . . . . ?
Dy1 O12 N10 O11 6.6(2) . . . . ?
Dy1 O21 N20 O20 -173.9(2) . . . . ?
Dy1 O21 N20 O22 7.6(2) . . . . ?
Dy1 O22 N20 O20 174.0(2) . . . . ?
Dy1 O22 N20 O21 -7.5(2) . . . . ?
C5S N1S C1S C2S 0.7(4) . . . . ?
N1S C1S C2S C3S 0.9(4) . . . . ?
C1S C2S C3S C4S -1.9(4) . . . . ?
C2S C3S C4S C5S 1.3(5) . . . . ?
C1S N1S C5S C4S -1.3(4) . . . . ?
C3S C4S C5S N1S 0.3(5) . . . . ?
C17S C11S C12S C13S -179.9(13) . . . . ?
C16S C11S C12S C13S 0.0 . . . . ?
C11S C12S C13S C14S 0.0 . . . . ?
C12S C13S C14S C15S 0.0 . . . . ?
C13S C14S C15S C16S 0.0 . . . . ?
C14S C15S C16S C11S 0.0 . . . . ?
C17S C11S C16S C15S 179.9(12) . . . . ?
C12S C11S C16S C15S 0.0 . . . . ?
C10S_1 N2S_1 C6S_1 C7S_1 3(2) . . . . ?
N2S_1 C6S_1 C7S_1 C8S_1 0(2) . . . . ?
C6S_1 C7S_1 C8S_1 C9S_1 1(4) . . . . ?
C7S_1 C8S_1 C9S_1 C10S_1 -4(4) . . . . ?
C6S_1 N2S_1 C10S_1 C9S_1 -6(4) . . . . ?
C8S_1 C9S_1 C10S_1 N2S_1 6(4) . . . . ?

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
C7 H7 O12 0.95 2.37 3.209(3) 146.5 2_766 yes
C13 H13 O21 0.95 2.40 3.253(3) 150.0 2_676 yes
O2 H2P N1S 0.89 1.63 2.513(3) 167.3 . yes
C2S H2S O1 0.95 2.41 3.347(3) 170.6 2_667 yes
C5S H5S O22 0.95 2.56 3.280(4) 133.1 . yes

_refine_diff_density_max         0.833
_refine_diff_density_min         -0.408
_refine_diff_density_rms         0.088

####################################################################### 
# 
# 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_3
_database_code_depnum_ccdc_archive 'CCDC 1957820'
loop_
_audit_author_name
_audit_author_address
'Ana M. Garcia-Deibe'
;Universidade de Santiago de Compostela
Spain
;
_audit_update_record             
;
2020-06-03 deposited with the CCDC.	2020-06-05 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/1
_shelx_SHELXL_version_number     2018/1
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C28 H26 Dy N4 O6, C19 H13 Cl2 Dy N3 O2'
_chemical_formula_sum            'C47 H39 Cl2 Dy2 N7 O8'
_chemical_formula_weight         1225.75

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

_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 2/c'
_space_group_name_Hall           '-C 2yc'

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

_cell_length_a                   19.188(4)
_cell_length_b                   18.419(4)
_cell_length_c                   12.866(3)
_cell_angle_alpha                90
_cell_angle_beta                 102.517(7)
_cell_angle_gamma                90
_cell_volume                     4439.2(16)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    2900
_cell_measurement_theta_min      3.1
_cell_measurement_theta_max      28.275

_exptl_crystal_description       plate
_exptl_crystal_colour            red
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.834
_exptl_crystal_F_000             2400
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.150
_exptl_crystal_size_mid          0.084
_exptl_crystal_size_min          0.040
_exptl_absorpt_coefficient_mu    3.525
_shelx_estimated_absorpt_T_min   0.620
_shelx_estimated_absorpt_T_max   0.872
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.337817
_exptl_absorpt_correction_T_max  0.959344
_exptl_absorpt_process_details   'TWINABS 2012.1 (Bruker AXS,2012)'
_exptl_absorpt_special_details   
;
4 twin components present. Reflections merged according to point-group 2/m   
 Single reflections that also occur in composites omitted
;
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'microfocus sealed tube'
_diffrn_measurement_device_type  'Bruker D8 VENTURE PHOTON III-14'
_diffrn_measurement_method       'omega and phi'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            13092
_diffrn_reflns_av_unetI/netI     0.0861
_diffrn_reflns_av_R_equivalents  0.0843

_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         2.408
_diffrn_reflns_theta_max         28.390
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.972
_diffrn_measured_fraction_theta_full 0.987
_diffrn_reflns_Laue_measured_fraction_max 0.972
_diffrn_reflns_Laue_measured_fraction_full 0.987
_diffrn_reflns_point_group_measured_fraction_max 0.972
_diffrn_reflns_point_group_measured_fraction_full 0.987
_reflns_number_total             6438
_reflns_number_gt                4622
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 _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 APEX3'
_computing_cell_refinement       'BRUKER APEX3'
_computing_data_reduction        'BRUKER SAINT'
_computing_structure_solution    'SHELXT-2014/1 (Sheldrick, 2018)'
_computing_structure_refinement  'SHELXL-2018/1 (Sheldrick, 2018)'
_computing_molecular_graphics    'WinGX 2020.1 (Farrugia, 2012)'
_computing_publication_material  'WinGX 2020.1 (Farrugia, 2012)'
_refine_special_details          
;1. Twinned data refinement
 Scales: 0.396(6)
 0.302(3) 0.186(4) 0.116(4)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All O(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3. Uiso/Uaniso restraints and constraints
Uanis(C108) ∼ Ueq, Uanis(C109) ∼ Ueq: with sigma of 0.1 and sigma for
terminal atoms of 0.2
4.a Riding coordinates:
 O12(H12)
4.b Ternary CH refined with riding coordinates:
 C113(H113)
4.c Aromatic/amide H refined with riding coordinates:
 C102(H102), C103(H103), C104(H104), C105(H105), C107(H107), C109(H109),
 C110(H110), C111(H111), C202(H202), C203(H203), C204(H204), C205(H205),
 C207(H207), C209(H209), C210(H210)
4.d Idealised Me refined as rotating group:
 C114(H11a,H11b,H11c),Twin
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1074P)²+43.6418P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         6438
_refine_ls_number_parameters     305
_refine_ls_number_restraints     12
_refine_ls_R_factor_all          0.1120
_refine_ls_R_factor_gt           0.0761
_refine_ls_wR_factor_ref         0.2123
_refine_ls_wR_factor_gt          0.1930
_refine_ls_goodness_of_fit_ref   1.066
_refine_ls_restrained_S_all      1.065
_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
Dy1 Dy 0.500000 0.91946(5) 0.750000 0.0338(3) Uani 1 2 d S T P . .
O11 O 0.5839(5) 1.0007(5) 0.8133(6) 0.040(2) Uani 1 1 d . . . . .
N11 N 0.5684(7) 0.9542(7) 0.6175(8) 0.046(3) Uani 1 1 d . . . . .
N12 N 0.4591(7) 0.8635(6) 0.5711(7) 0.045(3) Uani 1 1 d . . . . .
C101 C 0.6318(8) 1.0211(8) 0.7628(10) 0.044(3) Uani 1 1 d . . . . .
C102 C 0.6910(9) 1.0659(10) 0.8075(12) 0.063(5) Uani 1 1 d . . . . .
H102 H 0.697836 1.079315 0.880278 0.075 Uiso 1 1 calc R U . . .
C103 C 0.7378(9) 1.0901(14) 0.7514(15) 0.079(6) Uani 1 1 d . . . . .
H103 H 0.775227 1.122396 0.782049 0.094 Uiso 1 1 calc R U . . .
C104 C 0.7286(12) 1.0644(14) 0.6384(16) 0.089(7) Uani 1 1 d . . . . .
H104 H 0.762330 1.078460 0.597891 0.106 Uiso 1 1 calc R U . . .
C105 C 0.6753(9) 1.0231(11) 0.5954(14) 0.065(5) Uani 1 1 d . . . . .
H105 H 0.669638 1.009258 0.522913 0.077 Uiso 1 1 calc R U . . .
C106 C 0.6264(8) 0.9988(9) 0.6524(10) 0.049(4) Uani 1 1 d . . . . .
C107 C 0.5530(10) 0.9305(8) 0.5202(10) 0.055(4) Uani 1 1 d . . . . .
H107 H 0.579559 0.945122 0.469519 0.066 Uiso 1 1 calc R U . . .
C108 C 0.4931(9) 0.8807(8) 0.4926(9) 0.048(4) Uani 1 1 d . U . . .
C109 C 0.4686(13) 0.8542(10) 0.3896(10) 0.075(7) Uani 1 1 d . U . . .
H109 H 0.491778 0.867004 0.334015 0.089 Uiso 1 1 calc R U . . .
C110 C 0.4092(12) 0.8086(9) 0.3699(11) 0.071(6) Uani 1 1 d . . . . .
H110 H 0.391827 0.790214 0.300130 0.085 Uiso 1 1 calc R U . . .
C111 C 0.3762(12) 0.7902(8) 0.4478(11) 0.063(5) Uani 1 1 d . . . . .
H111 H 0.336196 0.758582 0.435227 0.076 Uiso 1 1 calc R U . . .
C112 C 0.4043(9) 0.8207(8) 0.5514(9) 0.049(4) Uani 1 1 d . . . . .
C113 C 0.3664(8) 0.8049(9) 0.6396(11) 0.051(4) Uani 1 1 d . . . . .
H113 H 0.351916 0.752715 0.638658 0.061 Uiso 1 1 calc R U . . .
C114 C 0.2665(9) 0.8439(14) 0.6998(18) 0.082(6) Uani 1 1 d . . . . .
H11A H 0.258923 0.792428 0.712973 0.124 Uiso 1 1 calc R U . . .
H11B H 0.220322 0.867789 0.674543 0.124 Uiso 1 1 calc R U . . .
H11C H 0.291652 0.866995 0.766042 0.124 Uiso 1 1 calc R U . . .
Dy2 Dy 0.500000 0.62161(5) 0.750000 0.0356(3) Uani 1 2 d S T P . .
Cl2 Cl 0.39427(19) 0.61762(19) 0.5834(3) 0.0430(8) Uani 1 1 d . . . . .
N21 N 0.4329(6) 0.5640(6) 0.8750(8) 0.036(2) Uani 1 1 d . . . . .
N22 N 0.500000 0.4869(8) 0.750000 0.037(3) Uani 1 2 d S T P . .
O12 O 0.4139(5) 0.8230(5) 0.7382(6) 0.042(2) Uani 1 1 d . . . . .
H12 H 0.422441 0.791154 0.765833 0.051 Uiso 1 1 d R U . . .
O21 O 0.4416(5) 0.7038(5) 0.8340(7) 0.040(2) Uani 1 1 d . . . . .
O13 O 0.3068(7) 0.8503(8) 0.6241(9) 0.073(4) Uani 1 1 d . . . . .
C201 C 0.4092(7) 0.6869(7) 0.9096(8) 0.031(3) Uani 1 1 d . . . . .
C202 C 0.3768(7) 0.7374(8) 0.9641(11) 0.041(3) Uani 1 1 d . . . . .
H202 H 0.380417 0.787435 0.948324 0.050 Uiso 1 1 calc R U . . .
C203 C 0.3389(8) 0.7173(9) 1.0414(11) 0.052(4) Uani 1 1 d . . . . .
H203 H 0.317086 0.753253 1.076762 0.062 Uiso 1 1 calc R U . . .
C204 C 0.3337(7) 0.6437(9) 1.0658(10) 0.044(3) Uani 1 1 d . . . . .
H204 H 0.309703 0.629580 1.119797 0.053 Uiso 1 1 calc R U . . .
C205 C 0.3633(8) 0.5920(8) 1.0117(10) 0.043(3) Uani 1 1 d . . . . .
H205 H 0.358400 0.541887 1.026342 0.052 Uiso 1 1 calc R U . . .
C206 C 0.4006(7) 0.6135(7) 0.9351(10) 0.036(3) Uani 1 1 d . . . . .
C207 C 0.4312(8) 0.4955(8) 0.8855(11) 0.042(3) Uani 1 1 d . . . . .
H207 H 0.408607 0.473795 0.936609 0.050 Uiso 1 1 calc R U . . .
C208 C 0.4658(7) 0.4505(7) 0.8151(10) 0.041(3) Uani 1 1 d . . . . .
C209 C 0.4671(8) 0.3751(8) 0.8165(13) 0.050(4) Uani 1 1 d . . . . .
H209 H 0.444678 0.350063 0.864858 0.060 Uiso 1 1 calc R U . . .
C210 C 0.500000 0.3354(11) 0.750000 0.042(4) Uani 1 2 d S T P . .
H210 H 0.500001 0.283857 0.749998 0.051 Uiso 1 2 calc R U P . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Dy1 O11 2.218(9) . ?
Dy1 O11 2.218(9) 2_656 ?
Dy1 O12 2.409(10) . ?
Dy1 O12 2.409(9) 2_656 ?
Dy1 N11 2.451(11) 2_656 ?
Dy1 N11 2.451(11) . ?
Dy1 N12 2.488(10) 2_656 ?
Dy1 N12 2.488(10) . ?
O11 C101 1.293(16) . ?
N11 C107 1.297(17) . ?
N11 C106 1.38(2) . ?
N12 C112 1.30(2) . ?
N12 C108 1.353(18) . ?
C101 C102 1.42(2) . ?
C101 C106 1.459(18) . ?
C102 C103 1.34(2) . ?
C103 C104 1.50(3) . ?
C104 C105 1.30(3) . ?
C105 C106 1.38(2) . ?
C107 C108 1.45(2) . ?
C108 C109 1.396(19) . ?
C109 C110 1.39(3) . ?
C110 C111 1.34(3) . ?
C111 C112 1.439(18) . ?
C112 C113 1.50(2) . ?
C113 O13 1.40(2) . ?
C113 O12 1.431(15) . ?
C114 O13 1.37(2) . ?
Dy2 O21 2.289(9) . ?
Dy2 O21 2.289(9) 2_656 ?
Dy2 N22 2.482(15) . ?
Dy2 N21 2.504(10) 2_656 ?
Dy2 N21 2.504(10) . ?
Dy2 Cl2 2.613(3) . ?
Dy2 Cl2 2.613(3) 2_656 ?
N21 C207 1.269(17) . ?
N21 C206 1.422(16) . ?
N22 C208 1.348(15) 2_656 ?
N22 C208 1.349(15) . ?
O21 C201 1.300(14) . ?
C201 C202 1.389(17) . ?
C201 C206 1.410(18) . ?
C202 C203 1.40(2) . ?
C203 C204 1.40(2) . ?
C204 C205 1.374(19) . ?
C205 C206 1.395(17) . ?
C207 C208 1.49(2) . ?
C208 C209 1.390(19) . ?
C209 C210 1.377(19) . ?

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
O11 Dy1 O11 95.2(5) . 2_656 ?
O11 Dy1 O12 162.5(3) . . ?
O11 Dy1 O12 92.4(3) 2_656 . ?
O11 Dy1 O12 92.4(3) . 2_656 ?
O11 Dy1 O12 162.5(3) 2_656 2_656 ?
O12 Dy1 O12 84.9(5) . 2_656 ?
O11 Dy1 N11 91.4(3) . 2_656 ?
O11 Dy1 N11 67.9(4) 2_656 2_656 ?
O12 Dy1 N11 76.9(3) . 2_656 ?
O12 Dy1 N11 127.7(4) 2_656 2_656 ?
O11 Dy1 N11 67.9(4) . . ?
O11 Dy1 N11 91.4(3) 2_656 . ?
O12 Dy1 N11 127.7(4) . . ?
O12 Dy1 N11 76.9(3) 2_656 . ?
N11 Dy1 N11 149.7(6) 2_656 . ?
O11 Dy1 N12 83.2(3) . 2_656 ?
O11 Dy1 N12 132.6(4) 2_656 2_656 ?
O12 Dy1 N12 80.0(3) . 2_656 ?
O12 Dy1 N12 64.0(3) 2_656 2_656 ?
N11 Dy1 N12 64.8(5) 2_656 2_656 ?
N11 Dy1 N12 130.0(4) . 2_656 ?
O11 Dy1 N12 132.6(4) . . ?
O11 Dy1 N12 83.2(3) 2_656 . ?
O12 Dy1 N12 64.0(3) . . ?
O12 Dy1 N12 80.0(3) 2_656 . ?
N11 Dy1 N12 130.0(4) 2_656 . ?
N11 Dy1 N12 64.8(5) . . ?
N12 Dy1 N12 131.1(5) 2_656 . ?
C101 O11 Dy1 123.4(9) . . ?
C107 N11 C106 120.9(13) . . ?
C107 N11 Dy1 122.6(12) . . ?
C106 N11 Dy1 116.4(8) . . ?
C112 N12 C108 119.9(12) . . ?
C112 N12 Dy1 120.9(9) . . ?
C108 N12 Dy1 119.2(10) . . ?
O11 C101 C102 124.0(13) . . ?
O11 C101 C106 119.9(14) . . ?
C102 C101 C106 116.1(14) . . ?
C103 C102 C101 122.9(17) . . ?
C102 C103 C104 117.6(19) . . ?
C105 C104 C103 120.8(17) . . ?
C104 C105 C106 121.7(18) . . ?
N11 C106 C105 127.8(14) . . ?
N11 C106 C101 111.5(12) . . ?
C105 C106 C101 120.7(16) . . ?
N11 C107 C108 116.8(13) . . ?
N12 C108 C109 120.6(18) . . ?
N12 C108 C107 116.6(11) . . ?
C109 C108 C107 122.7(15) . . ?
C110 C109 C108 118.5(16) . . ?
C111 C110 C109 121.1(14) . . ?
C110 C111 C112 116.9(18) . . ?
N12 C112 C111 123.0(15) . . ?
N12 C112 C113 118.4(12) . . ?
C111 C112 C113 118.6(16) . . ?
O13 C113 O12 109.3(12) . . ?
O13 C113 C112 107.0(13) . . ?
O12 C113 C112 107.8(12) . . ?
O21 Dy2 O21 97.2(5) . 2_656 ?
O21 Dy2 N22 131.4(2) . . ?
O21 Dy2 N22 131.4(2) 2_656 . ?
O21 Dy2 N21 163.0(3) . 2_656 ?
O21 Dy2 N21 66.7(3) 2_656 2_656 ?
N22 Dy2 N21 64.9(3) . 2_656 ?
O21 Dy2 N21 66.7(3) . . ?
O21 Dy2 N21 163.0(3) 2_656 . ?
N22 Dy2 N21 64.9(3) . . ?
N21 Dy2 N21 129.8(5) 2_656 . ?
O21 Dy2 Cl2 91.9(2) . . ?
O21 Dy2 Cl2 90.2(2) 2_656 . ?
N22 Dy2 Cl2 88.39(8) . . ?
N21 Dy2 Cl2 82.9(3) 2_656 . ?
N21 Dy2 Cl2 95.7(3) . . ?
O21 Dy2 Cl2 90.2(2) . 2_656 ?
O21 Dy2 Cl2 91.9(2) 2_656 2_656 ?
N22 Dy2 Cl2 88.39(8) . 2_656 ?
N21 Dy2 Cl2 95.7(3) 2_656 2_656 ?
N21 Dy2 Cl2 82.9(3) . 2_656 ?
Cl2 Dy2 Cl2 176.77(16) . 2_656 ?
C207 N21 C206 123.7(11) . . ?
C207 N21 Dy2 121.2(9) . . ?
C206 N21 Dy2 115.0(8) . . ?
C208 N22 C208 120.4(17) 2_656 . ?
C208 N22 Dy2 119.8(8) 2_656 . ?
C208 N22 Dy2 119.8(8) . . ?
C113 O12 Dy1 121.6(9) . . ?
C201 O21 Dy2 123.9(8) . . ?
C114 O13 C113 114.6(15) . . ?
O21 C201 C202 123.8(12) . . ?
O21 C201 C206 120.1(11) . . ?
C202 C201 C206 115.9(11) . . ?
C201 C202 C203 122.7(14) . . ?
C204 C203 C202 119.1(14) . . ?
C205 C204 C203 120.1(12) . . ?
C204 C205 C206 119.4(13) . . ?
C205 C206 C201 122.8(12) . . ?
C205 C206 N21 123.5(12) . . ?
C201 C206 N21 113.7(10) . . ?
N21 C207 C208 117.6(12) . . ?
N22 C208 C209 119.6(14) . . ?
N22 C208 C207 116.3(12) . . ?
C209 C208 C207 124.0(13) . . ?
C210 C209 C208 122.2(14) . . ?
C209 C210 C209 115.9(18) 2_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
C107 H107 O11 0.95 2.26 3.120(16) 149.7 6_575 yes
C113 H113 Cl2 1.00 2.76 3.588(17) 140.6 . yes
O12 H12 O21 0.69 1.83 2.518(13) 176.9 . yes
C207 H207 Cl2 0.95 2.59 3.479(13) 156.2 6_566 yes

_refine_diff_density_max         3.352
_refine_diff_density_min         -2.279
_refine_diff_density_rms         0.242

####################################################################### 
# 
# 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_2
_database_code_depnum_ccdc_archive 'CCDC 1942684'
loop_
_audit_author_name
_audit_author_address
'Ana M. Garcia-Deibe'
;Universidade de Santiago de Compostela
Spain
;
_audit_update_record             
;
2020-06-03 deposited with the CCDC.	2020-06-05 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/1
_shelx_SHELXL_version_number     2018/1
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C21 H21 Dy N4 O7, 2(H2 O)'
_chemical_formula_sum            'C21 H25 Dy N4 O9'
_chemical_formula_weight         639.95

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'
Dy Dy -0.1892 4.4098 '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'

_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                   13.9344(8)
_cell_length_b                   8.2685(5)
_cell_length_c                   20.4164(11)
_cell_angle_alpha                90
_cell_angle_beta                 100.009(2)
_cell_angle_gamma                90
_cell_volume                     2316.5(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9235
_cell_measurement_theta_min      2.875
_cell_measurement_theta_max      30.49

_exptl_crystal_description       plate
_exptl_crystal_colour            red
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.835
_exptl_crystal_F_000             1268
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.190
_exptl_crystal_size_mid          0.140
_exptl_crystal_size_min          0.080
_exptl_absorpt_coefficient_mu    3.286
_shelx_estimated_absorpt_T_min   0.574
_shelx_estimated_absorpt_T_max   0.779
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6257
_exptl_absorpt_correction_T_max  0.7251
_exptl_absorpt_process_details   'SADABS 2016/2 (Bruker, 2016)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker D8 VENTURE PHOTON III-14'
_diffrn_measurement_method       'omega and phi'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            179276
_diffrn_reflns_av_unetI/netI     0.0109
_diffrn_reflns_av_R_equivalents  0.0367
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_theta_min         2.876
_diffrn_reflns_theta_max         30.506
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 0.997
_reflns_number_total             7050
_reflns_number_gt                6908
_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 APEX3'
_computing_cell_refinement       'BRUKER SAINT'
_computing_data_reduction        'BRUKER SAINT'
_computing_structure_solution    'SHELXT-2014/1 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2018/1 (Sheldrick, 2018)'
_computing_molecular_graphics    'WinGX 2020.1 (Farrugia, 2012)'
_computing_publication_material  'WinGX 2020.1 (Farrugia, 2012)'
_refine_special_details          
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All O(H) groups, All O(H,H,H) groups
 At 1.5 times of:
  All C(H,H,H,H,H,H) groups
2. Uiso/Uaniso restraints and constraints
O1S': within 2.2A with sigma of 0.01 and sigma for terminal atoms of 0.01
Uanis(O1S') ? Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.01
3. Rigid body (RIGU) restrains
 O1S'
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Others
 Fixed Sof: O1S(0.5) H1S(0.5) C1S(0.5) H1SA(0.5) H1SB(0.5) O1S'(0.5) H1S'(0.5)
 C1S'(0.5) H1SC(0.5) H1SD(0.5) HB(0.5) HC(0.5) HD(0.5) HE(0.5) HF(0.5) HG(0.5)
 H2W2(0.5) H2W3(0.5) H3W2(0.5) H3W3(0.5)
5.a Riding coordinates:
 O1S(H1S), O1S'(H1S'), C2S(HB,HC,HD,HE,HF,HG), O2W(H2W1,H2W2,H2W3), O3W(H3W1,
 H3W2,H3W3)
5.b Secondary CH2 refined with riding coordinates:
 C1S(H1SA,H1SB), C1S'(H1SC,H1SD)
5.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C7(H7), C9(H9), C10(H10), C11(H11), C13(H13),
 C15(H15), C16(H16), C17(H17), C18(H18)
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+5.8723P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         7050
_refine_ls_number_parameters     343
_refine_ls_number_restraints     6
_refine_ls_R_factor_all          0.0221
_refine_ls_R_factor_gt           0.0216
_refine_ls_wR_factor_ref         0.0537
_refine_ls_wR_factor_gt          0.0535
_refine_ls_goodness_of_fit_ref   1.446
_refine_ls_restrained_S_all      1.446
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Dy1 Dy 0.30196(2) 0.55447(2) 0.64041(2) 0.00838(3) Uani 1 1 d . . . . .
N1 N 0.14088(15) 0.4315(2) 0.58745(10) 0.0110(4) Uani 1 1 d . . . . .
N3 N 0.46755(15) 0.4307(3) 0.63642(10) 0.0128(4) Uani 1 1 d . . . . .
N2 N 0.30802(15) 0.3405(3) 0.55453(10) 0.0131(4) Uani 1 1 d . . . . .
O1 O 0.17449(12) 0.6586(2) 0.68211(9) 0.0132(3) Uani 1 1 d . . . . .
O2 O 0.41283(13) 0.5872(2) 0.73613(8) 0.0130(3) Uani 1 1 d . . . . .
O11 O 0.22438(14) 0.7006(2) 0.53627(9) 0.0181(4) Uani 1 1 d . . . . .
O12 O 0.38001(14) 0.6693(3) 0.54518(9) 0.0185(4) Uani 1 1 d . . . . .
N10 N 0.30083(16) 0.7174(3) 0.51074(11) 0.0153(4) Uani 1 1 d . . . . .
O10 O 0.29726(16) 0.7758(3) 0.45517(10) 0.0237(4) Uani 1 1 d . . . . .
O1W O 0.27565(14) 0.3180(2) 0.70069(9) 0.0137(3) Uani 1 1 d . . . . .
O1S O 0.3410(7) 0.8536(14) 0.6691(4) 0.0143(14) Uani 0.5 1 d . . P A 1
H1S H 0.372425 0.832783 0.707573 0.017 Uiso 0.5 1 d R U P A 1
C1S C 0.3988(4) 0.9774(6) 0.6448(3) 0.0172(10) Uani 0.5 1 d . . P A 1
H1SA H 0.377172 0.991175 0.596287 0.021 Uiso 0.5 1 calc R U P A 1
H1SB H 0.389323 1.081478 0.666714 0.021 Uiso 0.5 1 calc R U P A 1
O1S' O 0.3249(7) 0.8459(14) 0.6512(4) 0.0133(13) Uani 0.5 1 d . U P A 2
H1S' H 0.272287 0.878105 0.654182 0.016 Uiso 0.5 1 d R U P A 2
C1S' C 0.4045(3) 0.9368(6) 0.6892(2) 0.0128(8) Uani 0.5 1 d . . P A 2
H1SC H 0.419631 0.891400 0.734667 0.015 Uiso 0.5 1 calc R U P A 2
H1SD H 0.383376 1.050283 0.692951 0.015 Uiso 0.5 1 calc R U P A 2
C2S C 0.4991(2) 0.9351(4) 0.65776(14) 0.0219(5) Uani 1 1 d . . . . .
HB H 0.535184 1.036469 0.667982 0.033 Uiso 0.5 1 d R U P A 1
HC H 0.530843 0.848961 0.686669 0.033 Uiso 0.5 1 d R U P A 1
HD H 0.498763 0.906100 0.611150 0.033 Uiso 0.5 1 d R U P A 1
HE H 0.546193 1.012310 0.681290 0.033 Uiso 0.5 1 d R U P A 2
HF H 0.527503 0.826360 0.661341 0.033 Uiso 0.5 1 d R U P A 2
HG H 0.482634 0.965800 0.610792 0.033 Uiso 0.5 1 d R U P A 2
C1 C 0.08332(17) 0.6121(3) 0.66218(12) 0.0125(4) Uani 1 1 d . . . . .
C2 C 0.00622(18) 0.6798(3) 0.68934(13) 0.0151(4) Uani 1 1 d . . . . .
H2 H 0.019556 0.761392 0.722449 0.018 Uiso 1 1 calc R U . . .
C3 C -0.08855(18) 0.6291(3) 0.66844(13) 0.0165(5) Uani 1 1 d . . . . .
H3 H -0.139477 0.676345 0.687443 0.020 Uiso 1 1 calc R U . . .
C4 C -0.11094(18) 0.5093(3) 0.61979(13) 0.0170(5) Uani 1 1 d . . . . .
H4 H -0.176382 0.474759 0.606152 0.020 Uiso 1 1 calc R U . . .
C5 C -0.03666(18) 0.4417(3) 0.59172(12) 0.0150(4) Uani 1 1 d . . . . .
H5 H -0.051221 0.360902 0.558375 0.018 Uiso 1 1 calc R U . . .
C6 C 0.05981(17) 0.4919(3) 0.61235(12) 0.0116(4) Uani 1 1 d . . . . .
C7 C 0.13492(18) 0.3324(3) 0.53842(12) 0.0128(4) Uani 1 1 d . . . . .
H7 H 0.073670 0.293505 0.516253 0.015 Uiso 1 1 calc R U . . .
C8 C 0.22588(18) 0.2816(3) 0.51799(12) 0.0131(4) Uani 1 1 d . . . . .
C9 C 0.2272(2) 0.1796(3) 0.46371(12) 0.0167(5) Uani 1 1 d . . . . .
H9 H 0.168338 0.136716 0.439478 0.020 Uiso 1 1 calc R U . . .
C10 C 0.3163(2) 0.1419(4) 0.44577(13) 0.0208(5) Uani 1 1 d . . . . .
H10 H 0.318780 0.077722 0.407498 0.025 Uiso 1 1 calc R U . . .
C11 C 0.4015(2) 0.1987(4) 0.48426(13) 0.0210(5) Uani 1 1 d . . . . .
H11 H 0.463265 0.171982 0.473540 0.025 Uiso 1 1 calc R U . . .
C12 C 0.39454(19) 0.2962(3) 0.53909(12) 0.0157(5) Uani 1 1 d . . . . .
C13 C 0.48088(18) 0.3492(3) 0.58555(12) 0.0165(5) Uani 1 1 d . . . . .
H13 H 0.544633 0.323872 0.578156 0.020 Uiso 1 1 calc R U . . .
C14 C 0.54209(18) 0.4785(3) 0.68824(12) 0.0127(4) Uani 1 1 d . . . . .
C15 C 0.64203(18) 0.4456(4) 0.69231(13) 0.0190(5) Uani 1 1 d . . . . .
H15 H 0.664299 0.388065 0.657543 0.023 Uiso 1 1 calc R U . . .
C16 C 0.70780(19) 0.4971(4) 0.74707(14) 0.0212(5) Uani 1 1 d . . . . .
H16 H 0.775319 0.474726 0.750213 0.025 Uiso 1 1 calc R U . . .
C17 C 0.67413(19) 0.5823(3) 0.79775(14) 0.0192(5) Uani 1 1 d . . . . .
H17 H 0.719549 0.619185 0.834922 0.023 Uiso 1 1 calc R U . . .
C18 C 0.57614(19) 0.6140(3) 0.79480(13) 0.0164(5) Uani 1 1 d . . . . .
H18 H 0.554904 0.671498 0.829949 0.020 Uiso 1 1 calc R U . . .
C19 C 0.50753(17) 0.5614(3) 0.73997(12) 0.0123(4) Uani 1 1 d . . . . .
O2W O 0.33302(14) 0.5500(2) 0.84499(9) 0.0173(4) Uani 1 1 d . . . . .
H2W1 H 0.365057 0.556506 0.810902 0.021 Uiso 1 1 d R U . B 2
H2W2 H 0.372267 0.505935 0.876929 0.021 Uiso 0.5 1 d R U P B 2
H2W3 H 0.292097 0.478830 0.824593 0.021 Uiso 0.5 1 d R U P C 1
O3W O 0.06112(16) 0.9095(3) 0.54406(11) 0.0279(5) Uani 1 1 d . . . . .
H3W1 H 0.111945 0.864225 0.531241 0.034 Uiso 1 1 d R U . . .
H3W2 H 0.085785 0.955375 0.584071 0.034 Uiso 0.5 1 d R U P D 1
H3W3 H 0.041135 0.959985 0.509841 0.034 Uiso 0.5 1 d R U P E 2
H1W1 H 0.295(3) 0.285(5) 0.738(2) 0.037(12) Uiso 1 1 d . . . . .
H1W2 H 0.240(3) 0.236(6) 0.680(2) 0.041(12) Uiso 1 1 d . . . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Dy1 O1 2.2689(17) . ?
Dy1 O2 2.2869(17) . ?
Dy1 O1W 2.3723(18) . ?
Dy1 O1S' 2.436(12) . ?
Dy1 N2 2.503(2) . ?
Dy1 O11 2.5201(19) . ?
Dy1 N1 2.529(2) . ?
Dy1 N3 2.538(2) . ?
Dy1 O12 2.5691(19) . ?
Dy1 O1S 2.578(11) . ?
N1 C7 1.285(3) . ?
N1 C6 1.408(3) . ?
N3 C13 1.279(3) . ?
N3 C14 1.404(3) . ?
N2 C8 1.344(3) . ?
N2 C12 1.349(3) . ?
O1 C1 1.322(3) . ?
O2 C19 1.325(3) . ?
O11 N10 1.272(3) . ?
O12 N10 1.265(3) . ?
N10 O10 1.226(3) . ?
O1W H1W1 0.80(4) . ?
O1W H1W2 0.91(5) . ?
O1S C1S 1.443(12) . ?
O1S H1S 0.8478 . ?
C1S C2S 1.419(6) . ?
C1S H1SA 0.9900 . ?
C1S H1SB 0.9900 . ?
O1S' C1S' 1.447(9) . ?
O1S' H1S' 0.7925 . ?
C1S' C2S 1.563(5) . ?
C1S' H1SC 0.9900 . ?
C1S' H1SD 0.9900 . ?
C2S HB 0.9815 . ?
C2S HC 0.9801 . ?
C2S HD 0.9807 . ?
C2S HE 0.9800 . ?
C2S HF 0.9800 . ?
C2S HG 0.9800 . ?
C1 C2 1.408(3) . ?
C1 C6 1.419(3) . ?
C2 C3 1.381(3) . ?
C2 H2 0.9500 . ?
C3 C4 1.399(4) . ?
C3 H3 0.9500 . ?
C4 C5 1.385(4) . ?
C4 H4 0.9500 . ?
C5 C6 1.400(3) . ?
C5 H5 0.9500 . ?
C7 C8 1.463(3) . ?
C7 H7 0.9500 . ?
C8 C9 1.395(3) . ?
C9 C10 1.389(4) . ?
C9 H9 0.9500 . ?
C10 C11 1.388(4) . ?
C10 H10 0.9500 . ?
C11 C12 1.396(3) . ?
C11 H11 0.9500 . ?
C12 C13 1.464(4) . ?
C13 H13 0.9500 . ?
C14 C15 1.407(3) . ?
C14 C19 1.412(3) . ?
C15 C16 1.384(4) . ?
C15 H15 0.9500 . ?
C16 C17 1.399(4) . ?
C16 H16 0.9500 . ?
C17 C18 1.381(4) . ?
C17 H17 0.9500 . ?
C18 C19 1.409(3) . ?
C18 H18 0.9500 . ?
O2W H2W1 0.8914 . ?
O2W H2W2 0.8564 . ?
O2W H2W3 0.8734 . ?
O3W H3W1 0.8801 . ?
O3W H3W2 0.9119 . ?
O3W H3W3 0.8199 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Dy1 O2 95.22(6) . . ?
O1 Dy1 O1W 85.21(7) . . ?
O2 Dy1 O1W 78.27(6) . . ?
O1 Dy1 O1S' 71.9(3) . . ?
O2 Dy1 O1S' 75.32(16) . . ?
O1W Dy1 O1S' 142.9(2) . . ?
O1 Dy1 N2 130.93(7) . . ?
O2 Dy1 N2 125.62(7) . . ?
O1W Dy1 N2 78.93(7) . . ?
O1S' Dy1 N2 138.0(2) . . ?
O1 Dy1 O11 83.43(6) . . ?
O2 Dy1 O11 142.30(7) . . ?
O1W Dy1 O11 138.64(6) . . ?
O1S' Dy1 O11 68.44(15) . . ?
N2 Dy1 O11 79.03(7) . . ?
O1 Dy1 N1 67.57(6) . . ?
O2 Dy1 N1 146.15(6) . . ?
O1W Dy1 N1 71.63(6) . . ?
O1S' Dy1 N1 122.0(2) . . ?
N2 Dy1 N1 63.37(7) . . ?
O11 Dy1 N1 67.25(6) . . ?
O1 Dy1 N3 160.12(6) . . ?
O2 Dy1 N3 65.94(6) . . ?
O1W Dy1 N3 84.71(7) . . ?
O1S' Dy1 N3 107.2(3) . . ?
N2 Dy1 N3 63.32(7) . . ?
O11 Dy1 N3 115.17(6) . . ?
N1 Dy1 N3 124.64(7) . . ?
O1 Dy1 O12 127.28(7) . . ?
O2 Dy1 O12 106.92(6) . . ?
O1W Dy1 O12 145.21(7) . . ?
O1S' Dy1 O12 68.7(2) . . ?
N2 Dy1 O12 70.17(7) . . ?
O11 Dy1 O12 50.22(6) . . ?
N1 Dy1 O12 106.62(6) . . ?
N3 Dy1 O12 67.54(6) . . ?
O1 Dy1 O1S 72.5(3) . . ?
O2 Dy1 O1S 66.90(17) . . ?
O1W Dy1 O1S 135.9(2) . . ?
N2 Dy1 O1S 143.7(2) . . ?
O11 Dy1 O1S 76.95(17) . . ?
N1 Dy1 O1S 128.3(2) . . ?
N3 Dy1 O1S 103.7(2) . . ?
O12 Dy1 O1S 73.5(2) . . ?
C7 N1 C6 124.1(2) . . ?
C7 N1 Dy1 121.45(16) . . ?
C6 N1 Dy1 114.27(15) . . ?
C13 N3 C14 124.6(2) . . ?
C13 N3 Dy1 119.99(17) . . ?
C14 N3 Dy1 114.82(15) . . ?
C8 N2 C12 118.8(2) . . ?
C8 N2 Dy1 121.06(16) . . ?
C12 N2 Dy1 119.74(17) . . ?
C1 O1 Dy1 123.18(15) . . ?
C19 O2 Dy1 123.31(15) . . ?
N10 O11 Dy1 97.53(14) . . ?
N10 O12 Dy1 95.38(14) . . ?
O10 N10 O12 122.0(2) . . ?
O10 N10 O11 121.3(2) . . ?
O12 N10 O11 116.7(2) . . ?
Dy1 O1W H1W1 135(3) . . ?
Dy1 O1W H1W2 120(3) . . ?
H1W1 O1W H1W2 105(4) . . ?
C1S O1S Dy1 135.3(6) . . ?
C1S O1S H1S 103.5 . . ?
Dy1 O1S H1S 94.1 . . ?
C2S C1S O1S 110.5(5) . . ?
C2S C1S H1SA 109.5 . . ?
O1S C1S H1SA 109.5 . . ?
C2S C1S H1SB 109.5 . . ?
O1S C1S H1SB 109.5 . . ?
H1SA C1S H1SB 108.1 . . ?
C1S' O1S' Dy1 129.7(6) . . ?
C1S' O1S' H1S' 114.7 . . ?
Dy1 O1S' H1S' 103.3 . . ?
O1S' C1S' C2S 113.4(5) . . ?
O1S' C1S' H1SC 108.9 . . ?
C2S C1S' H1SC 108.9 . . ?
O1S' C1S' H1SD 108.9 . . ?
C2S C1S' H1SD 108.9 . . ?
H1SC C1S' H1SD 107.7 . . ?
C1S C2S HB 106.3 . . ?
C1S C2S HC 128.2 . . ?
HB C2S HC 109.3 . . ?
C1S C2S HD 92.3 . . ?
HB C2S HD 109.3 . . ?
HC C2S HD 109.4 . . ?
C1S' C2S HE 109.5 . . ?
C1S' C2S HF 109.7 . . ?
HE C2S HF 109.5 . . ?
C1S' C2S HG 109.2 . . ?
HE C2S HG 109.5 . . ?
HF C2S HG 109.5 . . ?
O1 C1 C2 121.4(2) . . ?
O1 C1 C6 120.9(2) . . ?
C2 C1 C6 117.6(2) . . ?
C3 C2 C1 120.8(2) . . ?
C3 C2 H2 119.6 . . ?
C1 C2 H2 119.6 . . ?
C2 C3 C4 121.2(2) . . ?
C2 C3 H3 119.4 . . ?
C4 C3 H3 119.4 . . ?
C5 C4 C3 119.3(2) . . ?
C5 C4 H4 120.4 . . ?
C3 C4 H4 120.4 . . ?
C4 C5 C6 120.2(2) . . ?
C4 C5 H5 119.9 . . ?
C6 C5 H5 119.9 . . ?
C5 C6 N1 125.1(2) . . ?
C5 C6 C1 120.9(2) . . ?
N1 C6 C1 114.0(2) . . ?
N1 C7 C8 117.6(2) . . ?
N1 C7 H7 121.2 . . ?
C8 C7 H7 121.2 . . ?
N2 C8 C9 122.2(2) . . ?
N2 C8 C7 115.7(2) . . ?
C9 C8 C7 122.1(2) . . ?
C10 C9 C8 118.8(2) . . ?
C10 C9 H9 120.6 . . ?
C8 C9 H9 120.6 . . ?
C11 C10 C9 119.4(2) . . ?
C11 C10 H10 120.3 . . ?
C9 C10 H10 120.3 . . ?
C10 C11 C12 118.5(3) . . ?
C10 C11 H11 120.7 . . ?
C12 C11 H11 120.7 . . ?
N2 C12 C11 122.3(2) . . ?
N2 C12 C13 115.8(2) . . ?
C11 C12 C13 121.9(2) . . ?
N3 C13 C12 117.7(2) . . ?
N3 C13 H13 121.1 . . ?
C12 C13 H13 121.1 . . ?
N3 C14 C15 125.8(2) . . ?
N3 C14 C19 113.3(2) . . ?
C15 C14 C19 120.8(2) . . ?
C16 C15 C14 119.8(3) . . ?
C16 C15 H15 120.1 . . ?
C14 C15 H15 120.1 . . ?
C15 C16 C17 119.5(2) . . ?
C15 C16 H16 120.2 . . ?
C17 C16 H16 120.2 . . ?
C18 C17 C16 121.3(2) . . ?
C18 C17 H17 119.4 . . ?
C16 C17 H17 119.4 . . ?
C17 C18 C19 120.4(2) . . ?
C17 C18 H18 119.8 . . ?
C19 C18 H18 119.8 . . ?
O2 C19 C18 121.9(2) . . ?
O2 C19 C14 120.0(2) . . ?
C18 C19 C14 118.1(2) . . ?
H2W1 O2W H2W2 106.2 . . ?
H3W1 O3W H3W2 104.2 . . ?
H3W1 O3W H3W3 97.8 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Dy1 O12 N10 O10 -175.3(2) . . . . ?
Dy1 O12 N10 O11 3.9(2) . . . . ?
Dy1 O11 N10 O10 175.2(2) . . . . ?
Dy1 O11 N10 O12 -4.0(2) . . . . ?
Dy1 O1S C1S C2S -64.7(7) . . . . ?
Dy1 O1S' C1S' C2S 74.1(8) . . . . ?
Dy1 O1 C1 C2 179.99(18) . . . . ?
Dy1 O1 C1 C6 -0.1(3) . . . . ?
O1 C1 C2 C3 -179.4(2) . . . . ?
C6 C1 C2 C3 0.7(4) . . . . ?
C1 C2 C3 C4 0.0(4) . . . . ?
C2 C3 C4 C5 -0.6(4) . . . . ?
C3 C4 C5 C6 0.5(4) . . . . ?
C4 C5 C6 N1 179.9(2) . . . . ?
C4 C5 C6 C1 0.1(4) . . . . ?
C7 N1 C6 C5 6.3(4) . . . . ?
Dy1 N1 C6 C5 -179.1(2) . . . . ?
C7 N1 C6 C1 -173.9(2) . . . . ?
Dy1 N1 C6 C1 0.6(3) . . . . ?
O1 C1 C6 C5 179.4(2) . . . . ?
C2 C1 C6 C5 -0.7(4) . . . . ?
O1 C1 C6 N1 -0.4(3) . . . . ?
C2 C1 C6 N1 179.5(2) . . . . ?
C6 N1 C7 C8 179.5(2) . . . . ?
Dy1 N1 C7 C8 5.3(3) . . . . ?
C12 N2 C8 C9 -1.7(4) . . . . ?
Dy1 N2 C8 C9 170.80(19) . . . . ?
C12 N2 C8 C7 178.9(2) . . . . ?
Dy1 N2 C8 C7 -8.7(3) . . . . ?
N1 C7 C8 N2 2.1(3) . . . . ?
N1 C7 C8 C9 -177.3(2) . . . . ?
N2 C8 C9 C10 -2.0(4) . . . . ?
C7 C8 C9 C10 177.5(2) . . . . ?
C8 C9 C10 C11 3.6(4) . . . . ?
C9 C10 C11 C12 -1.7(4) . . . . ?
C8 N2 C12 C11 3.7(4) . . . . ?
Dy1 N2 C12 C11 -168.8(2) . . . . ?
C8 N2 C12 C13 -173.0(2) . . . . ?
Dy1 N2 C12 C13 14.4(3) . . . . ?
C10 C11 C12 N2 -2.1(4) . . . . ?
C10 C11 C12 C13 174.5(3) . . . . ?
C14 N3 C13 C12 174.4(2) . . . . ?
Dy1 N3 C13 C12 -15.1(3) . . . . ?
N2 C12 C13 N3 0.5(4) . . . . ?
C11 C12 C13 N3 -176.2(3) . . . . ?
C13 N3 C14 C15 0.3(4) . . . . ?
Dy1 N3 C14 C15 -170.6(2) . . . . ?
C13 N3 C14 C19 -177.4(3) . . . . ?
Dy1 N3 C14 C19 11.6(3) . . . . ?
N3 C14 C15 C16 -178.6(3) . . . . ?
C19 C14 C15 C16 -1.1(4) . . . . ?
C14 C15 C16 C17 -0.3(4) . . . . ?
C15 C16 C17 C18 1.1(4) . . . . ?
C16 C17 C18 C19 -0.4(4) . . . . ?
Dy1 O2 C19 C18 166.51(18) . . . . ?
Dy1 O2 C19 C14 -13.8(3) . . . . ?
C17 C18 C19 O2 178.8(2) . . . . ?
C17 C18 C19 C14 -1.0(4) . . . . ?
N3 C14 C19 O2 -0.2(3) . . . . ?
C15 C14 C19 O2 -178.0(2) . . . . ?
N3 C14 C19 C18 179.6(2) . . . . ?
C15 C14 C19 C18 1.7(4) . . . . ?

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
O1W H1W1 O1 0.80(4) 1.93(5) 2.714(2) 166(4) 2_546 yes
O1W H1W2 O2W 0.91(5) 1.86(5) 2.754(3) 168(4) 2_546 yes
O1S^a H1S^a O2 0.85 2.16 2.692(11) 120.6 . yes
O1S'^b H1S'^b O2W 0.79 2.05 2.785(11) 155.4 2_556 yes
C1S'^b H1SC^b O2 0.99 2.52 3.041(5) 112.8 . yes
C13 H13 O10 0.95 2.55 3.494(3) 171.0 3_666 yes
O2W H2W1^b O2 0.89 1.79 2.670(3) 170.9 . yes
O2W H2W2^b O3W 0.86 1.89 2.738(3) 169.3 2_546 yes
O2W H2W3^a O1S^a 0.87 2.15 2.891(11) 142.7 2_546 yes
O3W H3W1 O11 0.88 2.06 2.883(3) 155.4 . yes
O3W H3W2^a O2W 0.91 1.85 2.738(3) 164.0 2_556 yes
O3W H3W3^b O3W 0.82 1.96 2.704(5) 149.6 3_576 yes

_refine_diff_density_max         0.553
_refine_diff_density_min         -0.998
_refine_diff_density_rms         0.101

####################################################################### 
# 
# 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_4
_database_code_depnum_ccdc_archive 'CCDC 1942685'
loop_
_audit_author_name
_audit_author_address
'Ana M. Garcia-Deibe'
;Universidade de Santiago de Compostela
Spain
;
_audit_update_record             
;
2020-06-03 deposited with the CCDC.	2020-06-05 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/1
_shelx_SHELXL_version_number     2018/1
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C19 H13 Dy0.09 N5 O8 Y0.91, C6 H16 N'
_chemical_formula_sum            'C25 H29 Dy0.09 N6 O8 Y0.91'
_chemical_formula_weight         637.44

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'
Y Y -2.7962 3.5667 '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                   10.3588(6)
_cell_length_b                   14.8159(10)
_cell_length_c                   17.2043(11)
_cell_angle_alpha                90
_cell_angle_beta                 94.679(3)
_cell_angle_gamma                90
_cell_volume                     2631.6(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    1918
_cell_measurement_theta_min      2.4
_cell_measurement_theta_max      27.78

_exptl_crystal_description       prism
_exptl_crystal_colour            orange
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.609
_exptl_crystal_F_000             1306
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.080
_exptl_crystal_size_mid          0.060
_exptl_crystal_size_min          0.020
_exptl_absorpt_coefficient_mu    2.337
_shelx_estimated_absorpt_T_min   0.835
_shelx_estimated_absorpt_T_max   0.955
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.8297
_exptl_absorpt_correction_T_max  0.9143
_exptl_absorpt_process_details   'SADABS-2016/2(Bruker, 2016)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker D8 VENTURE PHOTON III-14'
_diffrn_measurement_method       'omega and phi scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            61528
_diffrn_reflns_av_unetI/netI     0.0500
_diffrn_reflns_av_R_equivalents  0.1012
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         2.404
_diffrn_reflns_theta_max         28.280
_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             6517
_reflns_number_gt                5126
_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 APEX3'
_computing_cell_refinement       'BRUKER APEX3'
_computing_data_reduction        'BRUKER SAINT'
_computing_structure_solution    'SHELXT-2014/1 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2018/1 (Sheldrick, 2018)'
_computing_molecular_graphics    'WinGX 2020.1 (Farrugia, 2012)'
_computing_publication_material  'WinGX 2020.1 (Farrugia, 2012)'
_refine_special_details          
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Others
 Sof(Dy1)=1-FVAR(1)
 Sof(Y1)=FVAR(1)
3.a Riding coordinates:
 N30(H30)
3.b Secondary CH2 refined with riding coordinates:
 C30(H30a,H30b), C32(H32a,H32b), C34(H34a,H34b)
3.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C7(H7), C9(H9), C10(H10), C11(H11), C13(H13),
 C15(H15), C16(H16), C17(H17), C18(H18)
3.d Idealised Me refined as rotating group:
 C31(H31a,H31b,H31c), C33(H33a,H33b,H33c), C35(H35a,H35b,H35c)
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0164P)²+1.9086P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         6517
_refine_ls_number_parameters     369
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0581
_refine_ls_R_factor_gt           0.0355
_refine_ls_wR_factor_ref         0.0682
_refine_ls_wR_factor_gt          0.0602
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_restrained_S_all      1.055
_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
Y1 Y 0.6733(3) 0.65634(18) 0.28808(14) 0.0129(3) Uani 0.9063(17) 1 d . . P . .
Dy1 Dy 0.6794(12) 0.6586(9) 0.2947(7) 0.0090(10) Uiso 0.0937(17) 1 d . . P . .
O1 O 0.83453(15) 0.60364(10) 0.21684(10) 0.0180(4) Uani 1 1 d . . . . .
O2 O 0.69235(16) 0.80705(11) 0.27694(9) 0.0191(4) Uani 1 1 d . . . . .
N1 N 0.63457(18) 0.49775(13) 0.24651(11) 0.0171(4) Uani 1 1 d . . . . .
N2 N 0.51392(18) 0.57047(13) 0.36158(11) 0.0167(4) Uani 1 1 d . . . . .
N3 N 0.58030(18) 0.73865(13) 0.39694(11) 0.0160(4) Uani 1 1 d . . . . .
O11 O 0.79299(16) 0.56865(12) 0.39273(10) 0.0231(4) Uani 1 1 d . . . . .
O12 O 0.87447(16) 0.69843(11) 0.36602(10) 0.0217(4) Uani 1 1 d . . . . .
O21 O 0.45158(16) 0.69581(12) 0.23507(10) 0.0224(4) Uani 1 1 d . . . . .
O22 O 0.59652(16) 0.68454(12) 0.15229(10) 0.0231(4) Uani 1 1 d . . . . .
C1 C 0.8236(2) 0.52511(16) 0.17995(14) 0.0171(5) Uani 1 1 d . . . . .
C2 C 0.9172(2) 0.49489(17) 0.13125(14) 0.0217(5) Uani 1 1 d . . . . .
H2 H 0.990267 0.531763 0.123895 0.026 Uiso 1 1 calc R U . . .
C3 C 0.9047(2) 0.41237(17) 0.09390(15) 0.0232(6) Uani 1 1 d . . . . .
H3 H 0.969335 0.393438 0.061280 0.028 Uiso 1 1 calc R U . . .
C4 C 0.7988(2) 0.35646(17) 0.10334(15) 0.0247(6) Uani 1 1 d . . . . .
H4 H 0.789773 0.300771 0.076066 0.030 Uiso 1 1 calc R U . . .
C5 C 0.7069(2) 0.38304(17) 0.15296(14) 0.0211(5) Uani 1 1 d . . . . .
H5 H 0.635760 0.344621 0.160887 0.025 Uiso 1 1 calc R U . . .
C6 C 0.7186(2) 0.46619(16) 0.19137(14) 0.0183(5) Uani 1 1 d . . . . .
C7 C 0.5519(2) 0.44730(16) 0.27754(14) 0.0192(5) Uani 1 1 d . . . . .
H7 H 0.537836 0.386721 0.260840 0.023 Uiso 1 1 calc R U . . .
C8 C 0.4795(2) 0.48626(16) 0.33990(14) 0.0184(5) Uani 1 1 d . . . . .
C9 C 0.3849(2) 0.43833(17) 0.37562(15) 0.0222(5) Uani 1 1 d . . . . .
H9 H 0.361912 0.378832 0.359246 0.027 Uiso 1 1 calc R U . . .
C10 C 0.3251(2) 0.47942(17) 0.43572(15) 0.0243(6) Uani 1 1 d . . . . .
H10 H 0.259133 0.448616 0.460383 0.029 Uiso 1 1 calc R U . . .
C11 C 0.3620(2) 0.56525(17) 0.45938(15) 0.0219(5) Uani 1 1 d . . . . .
H11 H 0.323453 0.593614 0.501291 0.026 Uiso 1 1 calc R U . . .
C12 C 0.4566(2) 0.60963(16) 0.42081(14) 0.0179(5) Uani 1 1 d . . . . .
C13 C 0.4984(2) 0.70201(16) 0.43953(14) 0.0186(5) Uani 1 1 d . . . . .
H13 H 0.466070 0.733859 0.481770 0.022 Uiso 1 1 calc R U . . .
C14 C 0.6214(2) 0.82884(15) 0.40370(14) 0.0168(5) Uani 1 1 d . . . . .
C15 C 0.6054(2) 0.88489(17) 0.46744(15) 0.0210(5) Uani 1 1 d . . . . .
H15 H 0.562971 0.862836 0.510502 0.025 Uiso 1 1 calc R U . . .
C16 C 0.6513(2) 0.97221(17) 0.46787(15) 0.0247(6) Uani 1 1 d . . . . .
H16 H 0.642367 1.010309 0.511520 0.030 Uiso 1 1 calc R U . . .
C17 C 0.7107(3) 1.00382(18) 0.40363(16) 0.0273(6) Uani 1 1 d . . . . .
H17 H 0.741262 1.064283 0.403799 0.033 Uiso 1 1 calc R U . . .
C18 C 0.7267(2) 0.95023(17) 0.33973(15) 0.0233(6) Uani 1 1 d . . . . .
H18 H 0.767903 0.974069 0.296861 0.028 Uiso 1 1 calc R U . . .
C19 C 0.6823(2) 0.86031(16) 0.33747(14) 0.0180(5) Uani 1 1 d . . . . .
N10 N 0.8867(2) 0.62421(15) 0.40369(12) 0.0230(5) Uani 1 1 d . . . . .
O10 O 0.98229(18) 0.60814(13) 0.44834(11) 0.0337(5) Uani 1 1 d . . . . .
N20 N 0.4822(2) 0.70669(14) 0.16551(12) 0.0203(4) Uani 1 1 d . . . . .
O20 O 0.40567(17) 0.73853(13) 0.11456(10) 0.0293(4) Uani 1 1 d . . . . .
N30 N 1.01341(19) 0.73014(14) 0.17405(11) 0.0189(4) Uani 1 1 d . . . . .
H30 H 0.952698 0.681863 0.192687 0.023 Uiso 1 1 d R U . . .
C30 C 1.1489(2) 0.70893(19) 0.20850(15) 0.0265(6) Uani 1 1 d . . . . .
H30A H 1.194525 0.673492 0.170380 0.032 Uiso 1 1 calc R U . . .
H30B H 1.197011 0.766032 0.218515 0.032 Uiso 1 1 calc R U . . .
C31 C 1.1483(2) 0.65670(19) 0.28314(16) 0.0284(6) Uani 1 1 d . . . . .
H31A H 1.104338 0.691954 0.321316 0.043 Uiso 1 1 calc R U . . .
H31B H 1.237669 0.644579 0.303651 0.043 Uiso 1 1 calc R U . . .
H31C H 1.102539 0.599439 0.273229 0.043 Uiso 1 1 calc R U . . .
C32 C 0.9655(3) 0.81763(17) 0.20501(15) 0.0255(6) Uani 1 1 d . . . . .
H32A H 0.989014 0.820179 0.261912 0.031 Uiso 1 1 calc R U . . .
H32B H 0.869824 0.818933 0.196768 0.031 Uiso 1 1 calc R U . . .
C33 C 1.0196(3) 0.90095(18) 0.16720(17) 0.0302(6) Uani 1 1 d . . . . .
H33A H 1.114240 0.896622 0.169264 0.045 Uiso 1 1 calc R U . . .
H33B H 0.995194 0.955052 0.195309 0.045 Uiso 1 1 calc R U . . .
H33C H 0.984233 0.904763 0.112710 0.045 Uiso 1 1 calc R U . . .
C34 C 1.0049(2) 0.72617(18) 0.08659(14) 0.0237(6) Uani 1 1 d . . . . .
H34A H 1.043244 0.668834 0.069953 0.028 Uiso 1 1 calc R U . . .
H34B H 1.055470 0.776496 0.066476 0.028 Uiso 1 1 calc R U . . .
C35 C 0.8658(3) 0.73243(19) 0.05220(16) 0.0295(6) Uani 1 1 d . . . . .
H35A H 0.813833 0.685992 0.075584 0.044 Uiso 1 1 calc R U . . .
H35B H 0.862574 0.723131 -0.004327 0.044 Uiso 1 1 calc R U . . .
H35C H 0.831029 0.792215 0.063079 0.044 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
Y1 O2 2.251(3) . ?
Y1 O1 2.288(3) . ?
Y1 O22 2.442(3) . ?
Y1 O12 2.465(3) . ?
Y1 O11 2.470(3) . ?
Y1 O21 2.471(3) . ?
Y1 N1 2.479(3) . ?
Y1 N3 2.493(3) . ?
Y1 N2 2.507(3) . ?
Dy1 O2 2.226(13) . ?
Dy1 O1 2.322(13) . ?
Dy1 O12 2.352(12) . ?
Dy1 O11 2.384(12) . ?
Dy1 N3 2.418(13) . ?
Dy1 N2 2.508(13) . ?
Dy1 N1 2.554(13) . ?
Dy1 O21 2.556(12) . ?
Dy1 O22 2.558(12) . ?
O1 C1 1.326(3) . ?
O2 C19 1.317(3) . ?
N1 C7 1.285(3) . ?
N1 C6 1.418(3) . ?
N2 C8 1.342(3) . ?
N2 C12 1.351(3) . ?
N3 C13 1.286(3) . ?
N3 C14 1.405(3) . ?
O11 N10 1.275(3) . ?
O12 N10 1.278(3) . ?
O21 N20 1.273(2) . ?
O22 N20 1.267(2) . ?
C1 C2 1.406(3) . ?
C1 C6 1.421(3) . ?
C2 C3 1.382(3) . ?
C2 H2 0.9500 . ?
C3 C4 1.395(4) . ?
C3 H3 0.9500 . ?
C4 C5 1.387(3) . ?
C4 H4 0.9500 . ?
C5 C6 1.399(3) . ?
C5 H5 0.9500 . ?
C7 C8 1.476(3) . ?
C7 H7 0.9500 . ?
C8 C9 1.393(3) . ?
C9 C10 1.389(3) . ?
C9 H9 0.9500 . ?
C10 C11 1.380(3) . ?
C10 H10 0.9500 . ?
C11 C12 1.393(3) . ?
C11 H11 0.9500 . ?
C12 C13 1.464(3) . ?
C13 H13 0.9500 . ?
C14 C15 1.396(3) . ?
C14 C19 1.425(3) . ?
C15 C16 1.378(3) . ?
C15 H15 0.9500 . ?
C16 C17 1.389(4) . ?
C16 H16 0.9500 . ?
C17 C18 1.377(4) . ?
C17 H17 0.9500 . ?
C18 C19 1.409(3) . ?
C18 H18 0.9500 . ?
N10 O10 1.226(3) . ?
N20 O20 1.227(3) . ?
N30 C32 1.501(3) . ?
N30 C34 1.501(3) . ?
N30 C30 1.511(3) . ?
N30 H30 1.0212 . ?
C30 C31 1.500(4) . ?
C30 H30A 0.9900 . ?
C30 H30B 0.9900 . ?
C31 H31A 0.9800 . ?
C31 H31B 0.9800 . ?
C31 H31C 0.9800 . ?
C32 C33 1.523(4) . ?
C32 H32A 0.9900 . ?
C32 H32B 0.9900 . ?
C33 H33A 0.9800 . ?
C33 H33B 0.9800 . ?
C33 H33C 0.9800 . ?
C34 C35 1.515(3) . ?
C34 H34A 0.9900 . ?
C34 H34B 0.9900 . ?
C35 H35A 0.9800 . ?
C35 H35B 0.9800 . ?
C35 H35C 0.9800 . ?

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
O2 Y1 O1 102.71(12) . . ?
O2 Y1 O22 76.87(10) . . ?
O1 Y1 O22 74.98(9) . . ?
O2 Y1 O12 73.69(10) . . ?
O1 Y1 O12 75.87(10) . . ?
O22 Y1 O12 132.24(13) . . ?
O2 Y1 O11 122.78(12) . . ?
O1 Y1 O11 82.30(10) . . ?
O22 Y1 O11 153.16(13) . . ?
O12 Y1 O11 52.02(7) . . ?
O2 Y1 O21 79.58(10) . . ?
O1 Y1 O21 125.46(12) . . ?
O22 Y1 O21 52.12(7) . . ?
O12 Y1 O21 149.33(13) . . ?
O11 Y1 O21 142.14(13) . . ?
O2 Y1 N1 158.24(13) . . ?
O1 Y1 N1 68.29(9) . . ?
O22 Y1 N1 81.59(10) . . ?
O12 Y1 N1 120.43(12) . . ?
O11 Y1 N1 76.80(10) . . ?
O21 Y1 N1 89.67(10) . . ?
O2 Y1 N3 67.71(9) . . ?
O1 Y1 N3 155.90(13) . . ?
O22 Y1 N3 121.29(12) . . ?
O12 Y1 N3 80.15(9) . . ?
O11 Y1 N3 84.92(10) . . ?
O21 Y1 N3 75.95(10) . . ?
N1 Y1 N3 128.09(13) . . ?
O2 Y1 N2 127.76(13) . . ?
O1 Y1 N2 129.54(13) . . ?
O22 Y1 N2 113.14(11) . . ?
O12 Y1 N2 114.61(11) . . ?
O11 Y1 N2 71.19(9) . . ?
O21 Y1 N2 71.08(9) . . ?
N1 Y1 N2 64.33(9) . . ?
N3 Y1 N2 63.81(9) . . ?
O2 Dy1 O1 102.4(5) . . ?
O2 Dy1 O12 76.4(4) . . ?
O1 Dy1 O12 77.5(4) . . ?
O2 Dy1 O11 128.2(5) . . ?
O1 Dy1 O11 83.5(4) . . ?
O12 Dy1 O11 54.4(3) . . ?
O2 Dy1 N3 69.5(4) . . ?
O1 Dy1 N3 161.2(6) . . ?
O12 Dy1 N3 84.0(4) . . ?
O11 Dy1 N3 88.5(4) . . ?
O2 Dy1 N2 129.0(6) . . ?
O1 Dy1 N2 127.8(5) . . ?
O12 Dy1 N2 118.8(5) . . ?
O11 Dy1 N2 72.6(4) . . ?
N3 Dy1 N2 64.9(3) . . ?
O2 Dy1 N1 152.7(6) . . ?
O1 Dy1 N1 66.5(3) . . ?
O12 Dy1 N1 121.9(5) . . ?
O11 Dy1 N1 76.9(4) . . ?
N3 Dy1 N1 128.1(5) . . ?
N2 Dy1 N1 63.2(3) . . ?
O2 Dy1 O21 78.2(4) . . ?
O1 Dy1 O21 120.2(5) . . ?
O12 Dy1 O21 151.8(6) . . ?
O11 Dy1 O21 142.3(6) . . ?
N3 Dy1 O21 75.7(4) . . ?
N2 Dy1 O21 69.7(3) . . ?
N1 Dy1 O21 86.2(4) . . ?
O2 Dy1 O22 74.9(4) . . ?
O1 Dy1 O22 72.2(3) . . ?
O12 Dy1 O22 132.0(6) . . ?
O11 Dy1 O22 150.4(6) . . ?
N3 Dy1 O22 119.6(5) . . ?
N2 Dy1 O22 109.2(4) . . ?
N1 Dy1 O22 77.9(3) . . ?
O21 Dy1 O22 49.9(2) . . ?
O2 Dy1 N10 102.8(4) . . ?
O1 Dy1 N10 78.0(4) . . ?
O12 Dy1 N10 27.22(14) . . ?
O11 Dy1 N10 27.23(14) . . ?
N3 Dy1 N10 87.1(4) . . ?
N2 Dy1 N10 96.6(4) . . ?
N1 Dy1 N10 99.1(4) . . ?
O21 Dy1 N10 161.4(5) . . ?
O22 Dy1 N10 148.6(5) . . ?
C1 O1 Y1 121.22(16) . . ?
C1 O1 Dy1 123.2(3) . . ?
C19 O2 Dy1 118.3(3) . . ?
C19 O2 Y1 120.91(15) . . ?
C7 N1 C6 123.5(2) . . ?
C7 N1 Y1 121.94(17) . . ?
C6 N1 Y1 114.32(16) . . ?
C7 N1 Dy1 121.2(3) . . ?
C6 N1 Dy1 114.8(3) . . ?
C8 N2 C12 119.0(2) . . ?
C8 N2 Y1 120.17(16) . . ?
C12 N2 Y1 120.70(16) . . ?
C8 N2 Dy1 122.2(3) . . ?
C12 N2 Dy1 118.8(3) . . ?
C13 N3 C14 124.4(2) . . ?
C13 N3 Dy1 123.1(3) . . ?
C14 N3 Dy1 112.5(3) . . ?
C13 N3 Y1 122.34(17) . . ?
C14 N3 Y1 113.22(15) . . ?
N10 O11 Dy1 94.0(3) . . ?
N10 O11 Y1 95.69(15) . . ?
N10 O12 Dy1 95.4(3) . . ?
N10 O12 Y1 95.91(15) . . ?
N20 O21 Y1 94.66(14) . . ?
N20 O21 Dy1 96.4(3) . . ?
N20 O22 Y1 96.24(14) . . ?
N20 O22 Dy1 96.5(3) . . ?
O1 C1 C2 121.9(2) . . ?
O1 C1 C6 120.6(2) . . ?
C2 C1 C6 117.4(2) . . ?
C3 C2 C1 121.1(2) . . ?
C3 C2 H2 119.5 . . ?
C1 C2 H2 119.5 . . ?
C2 C3 C4 121.1(2) . . ?
C2 C3 H3 119.5 . . ?
C4 C3 H3 119.5 . . ?
C5 C4 C3 119.3(2) . . ?
C5 C4 H4 120.4 . . ?
C3 C4 H4 120.4 . . ?
C4 C5 C6 120.3(2) . . ?
C4 C5 H5 119.9 . . ?
C6 C5 H5 119.9 . . ?
C5 C6 N1 124.9(2) . . ?
C5 C6 C1 120.9(2) . . ?
N1 C6 C1 114.1(2) . . ?
N1 C7 C8 118.0(2) . . ?
N1 C7 H7 121.0 . . ?
C8 C7 H7 121.0 . . ?
N2 C8 C9 122.1(2) . . ?
N2 C8 C7 115.2(2) . . ?
C9 C8 C7 122.6(2) . . ?
C10 C9 C8 118.5(2) . . ?
C10 C9 H9 120.7 . . ?
C8 C9 H9 120.7 . . ?
C11 C10 C9 119.6(2) . . ?
C11 C10 H10 120.2 . . ?
C9 C10 H10 120.2 . . ?
C10 C11 C12 118.9(2) . . ?
C10 C11 H11 120.6 . . ?
C12 C11 H11 120.6 . . ?
N2 C12 C11 121.8(2) . . ?
N2 C12 C13 115.3(2) . . ?
C11 C12 C13 122.9(2) . . ?
N3 C13 C12 117.8(2) . . ?
N3 C13 H13 121.1 . . ?
C12 C13 H13 121.1 . . ?
C15 C14 N3 125.2(2) . . ?
C15 C14 C19 121.5(2) . . ?
N3 C14 C19 113.3(2) . . ?
C16 C15 C14 120.0(2) . . ?
C16 C15 H15 120.0 . . ?
C14 C15 H15 120.0 . . ?
C15 C16 C17 119.1(2) . . ?
C15 C16 H16 120.4 . . ?
C17 C16 H16 120.4 . . ?
C18 C17 C16 122.0(2) . . ?
C18 C17 H17 119.0 . . ?
C16 C17 H17 119.0 . . ?
C17 C18 C19 120.5(2) . . ?
C17 C18 H18 119.8 . . ?
C19 C18 H18 119.8 . . ?
O2 C19 C18 122.8(2) . . ?
O2 C19 C14 120.3(2) . . ?
C18 C19 C14 116.9(2) . . ?
O10 N10 O11 122.2(2) . . ?
O10 N10 O12 121.8(2) . . ?
O11 N10 O12 115.9(2) . . ?
O10 N10 Dy1 176.4(3) . . ?
O11 N10 Dy1 58.8(3) . . ?
O12 N10 Dy1 57.4(3) . . ?
O10 N10 Y1 175.24(17) . . ?
O11 N10 Y1 58.27(13) . . ?
O12 N10 Y1 58.01(12) . . ?
O20 N20 O22 122.0(2) . . ?
O20 N20 O21 121.6(2) . . ?
O22 N20 O21 116.38(19) . . ?
O20 N20 Y1 172.39(18) . . ?
O22 N20 Y1 57.73(12) . . ?
O21 N20 Y1 59.10(12) . . ?
C32 N30 C34 113.3(2) . . ?
C32 N30 C30 111.3(2) . . ?
C34 N30 C30 111.22(18) . . ?
C32 N30 H30 105.3 . . ?
C34 N30 H30 107.4 . . ?
C30 N30 H30 107.9 . . ?
C31 C30 N30 112.0(2) . . ?
C31 C30 H30A 109.2 . . ?
N30 C30 H30A 109.2 . . ?
C31 C30 H30B 109.2 . . ?
N30 C30 H30B 109.2 . . ?
H30A C30 H30B 107.9 . . ?
C30 C31 H31A 109.5 . . ?
C30 C31 H31B 109.5 . . ?
H31A C31 H31B 109.5 . . ?
C30 C31 H31C 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
N30 C32 C33 113.9(2) . . ?
N30 C32 H32A 108.8 . . ?
C33 C32 H32A 108.8 . . ?
N30 C32 H32B 108.8 . . ?
C33 C32 H32B 108.8 . . ?
H32A C32 H32B 107.7 . . ?
C32 C33 H33A 109.5 . . ?
C32 C33 H33B 109.5 . . ?
H33A C33 H33B 109.5 . . ?
C32 C33 H33C 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
N30 C34 C35 111.4(2) . . ?
N30 C34 H34A 109.3 . . ?
C35 C34 H34A 109.3 . . ?
N30 C34 H34B 109.3 . . ?
C35 C34 H34B 109.3 . . ?
H34A C34 H34B 108.0 . . ?
C34 C35 H35A 109.5 . . ?
C34 C35 H35B 109.5 . . ?
H35A C35 H35B 109.5 . . ?
C34 C35 H35C 109.5 . . ?
H35A C35 H35C 109.5 . . ?
H35B C35 H35C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Y1 O1 C1 C2 175.14(19) . . . . ?
Dy1 O1 C1 C2 178.0(4) . . . . ?
Y1 O1 C1 C6 -7.8(3) . . . . ?
Dy1 O1 C1 C6 -5.0(5) . . . . ?
O1 C1 C2 C3 179.3(2) . . . . ?
C6 C1 C2 C3 2.2(4) . . . . ?
C1 C2 C3 C4 0.0(4) . . . . ?
C2 C3 C4 C5 -2.1(4) . . . . ?
C3 C4 C5 C6 1.8(4) . . . . ?
C4 C5 C6 N1 -176.3(2) . . . . ?
C4 C5 C6 C1 0.5(4) . . . . ?
C7 N1 C6 C5 12.6(4) . . . . ?
Y1 N1 C6 C5 -172.7(2) . . . . ?
Dy1 N1 C6 C5 -175.3(3) . . . . ?
C7 N1 C6 C1 -164.4(2) . . . . ?
Y1 N1 C6 C1 10.3(3) . . . . ?
Dy1 N1 C6 C1 7.7(4) . . . . ?
O1 C1 C6 C5 -179.6(2) . . . . ?
C2 C1 C6 C5 -2.5(4) . . . . ?
O1 C1 C6 N1 -2.5(3) . . . . ?
C2 C1 C6 N1 174.6(2) . . . . ?
C6 N1 C7 C8 174.0(2) . . . . ?
Y1 N1 C7 C8 -0.3(3) . . . . ?
Dy1 N1 C7 C8 2.4(4) . . . . ?
C12 N2 C8 C9 1.1(4) . . . . ?
Y1 N2 C8 C9 -175.58(19) . . . . ?
Dy1 N2 C8 C9 -178.1(4) . . . . ?
C12 N2 C8 C7 -177.0(2) . . . . ?
Y1 N2 C8 C7 6.4(3) . . . . ?
Dy1 N2 C8 C7 3.8(4) . . . . ?
N1 C7 C8 N2 -4.0(3) . . . . ?
N1 C7 C8 C9 177.9(2) . . . . ?
N2 C8 C9 C10 -0.2(4) . . . . ?
C7 C8 C9 C10 177.7(2) . . . . ?
C8 C9 C10 C11 -1.2(4) . . . . ?
C9 C10 C11 C12 1.6(4) . . . . ?
C8 N2 C12 C11 -0.6(3) . . . . ?
Y1 N2 C12 C11 176.01(19) . . . . ?
Dy1 N2 C12 C11 178.6(4) . . . . ?
C8 N2 C12 C13 -179.0(2) . . . . ?
Y1 N2 C12 C13 -2.3(3) . . . . ?
Dy1 N2 C12 C13 0.3(4) . . . . ?
C10 C11 C12 N2 -0.7(4) . . . . ?
C10 C11 C12 C13 177.5(2) . . . . ?
C14 N3 C13 C12 174.7(2) . . . . ?
Dy1 N3 C13 C12 -4.8(4) . . . . ?
Y1 N3 C13 C12 -2.0(3) . . . . ?
N2 C12 C13 N3 2.8(3) . . . . ?
C11 C12 C13 N3 -175.5(2) . . . . ?
C13 N3 C14 C15 16.2(4) . . . . ?
Dy1 N3 C14 C15 -164.3(4) . . . . ?
Y1 N3 C14 C15 -166.9(2) . . . . ?
C13 N3 C14 C19 -163.3(2) . . . . ?
Dy1 N3 C14 C19 16.2(4) . . . . ?
Y1 N3 C14 C19 13.6(2) . . . . ?
N3 C14 C15 C16 179.3(2) . . . . ?
C19 C14 C15 C16 -1.3(4) . . . . ?
C14 C15 C16 C17 1.3(4) . . . . ?
C15 C16 C17 C18 -0.8(4) . . . . ?
C16 C17 C18 C19 0.1(4) . . . . ?
Dy1 O2 C19 C18 160.3(4) . . . . ?
Y1 O2 C19 C18 162.6(2) . . . . ?
Dy1 O2 C19 C14 -21.4(5) . . . . ?
Y1 O2 C19 C14 -19.2(3) . . . . ?
C17 C18 C19 O2 178.3(2) . . . . ?
C17 C18 C19 C14 0.0(4) . . . . ?
C15 C14 C19 O2 -177.7(2) . . . . ?
N3 C14 C19 O2 1.8(3) . . . . ?
C15 C14 C19 C18 0.6(3) . . . . ?
N3 C14 C19 C18 -179.9(2) . . . . ?
C32 N30 C30 C31 88.7(3) . . . . ?
C34 N30 C30 C31 -143.9(2) . . . . ?
C34 N30 C32 C33 -48.0(3) . . . . ?
C30 N30 C32 C33 78.3(3) . . . . ?
C32 N30 C34 C35 -62.9(3) . . . . ?
C30 N30 C34 C35 170.9(2) . . . . ?

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
C9 H9 O2 0.95 2.59 3.312(3) 132.8 2_645 yes
C13 H13 O20 0.95 2.45 3.352(3) 158.2 4_576 yes
C15 H15 O22 0.95 2.53 3.351(3) 144.1 4_576 yes
N30 H30 O1 1.02 1.76 2.777(3) 173.4 . yes
C31 H31A O12 0.98 2.56 3.335(3) 135.6 . yes
C32 H32B O2 0.99 2.39 3.183(3) 136.3 . yes
C35 H35B O12 0.98 2.53 3.371(3) 144.2 4_575 yes

_refine_diff_density_max         0.453
_refine_diff_density_min         -0.471
_refine_diff_density_rms         0.087

