# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2017

####################################################################### 
# 
# 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. 
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data_1(Tb)
_database_code_depnum_ccdc_archive 'CCDC 1574339'
_audit_update_record             
;
2017-11-16 deposited with the CCDC.
2017-11-17 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C33 H38 N5 O10 Tb, 2(N O3), C2 H3 N'
_chemical_formula_sum            'C35 H41 N8 O16 Tb'
_chemical_formula_weight         988.68

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           11
_space_group_name_H-M_alt        'P 21/m'
_space_group_name_Hall           '-P 2yb'

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

_cell_length_a                   10.0065(6)
_cell_length_b                   17.7675(10)
_cell_length_c                   11.8168(8)
_cell_angle_alpha                90
_cell_angle_beta                 109.875(4)
_cell_angle_gamma                90
_cell_volume                     1975.8(2)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    1968
_cell_measurement_theta_min      2.45
_cell_measurement_theta_max      26.685

_exptl_crystal_description       plate
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.662
_exptl_crystal_F_000             1000
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.160
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.060
_exptl_absorpt_coefficient_mu    1.873
_shelx_estimated_absorpt_T_min   0.754
_shelx_estimated_absorpt_T_max   0.896
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6620
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_process_details   'SADABS-2014/5 (Bruker, 2014)'
_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 Kappa APEXII CCD'
_diffrn_measurement_method       'omega and phi scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            73699
_diffrn_reflns_av_unetI/netI     0.0303
_diffrn_reflns_av_R_equivalents  0.0648
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         2.162
_diffrn_reflns_theta_max         28.282
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             5058
_reflns_number_gt                4732
_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 APEX2'
_computing_data_reduction        ?
_computing_structure_solution    'SHELXS-2014/7 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Wingx 2014.1 (Farrugia, 2012)'
_computing_publication_material  'Wingx 2014.1 (Farrugia, 2012)'
_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)+6.5252P] 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         5058
_refine_ls_number_parameters     329
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0340
_refine_ls_R_factor_gt           0.0307
_refine_ls_wR_factor_ref         0.0693
_refine_ls_wR_factor_gt          0.0683
_refine_ls_goodness_of_fit_ref   1.201
_refine_ls_restrained_S_all      1.201
_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
Tb1 Tb 0.10342(2) 0.2500 0.39954(2) 0.00918(6) Uani 1 2 d S T P . .
O1W O 0.3326(4) 0.2500 0.5529(3) 0.0184(7) Uani 1 2 d S T P . .
O10 O 0.0733(3) 0.18927(13) 0.5828(2) 0.0209(5) Uani 1 1 d . . . . .
O1 O 0.0329(3) 0.12278(14) 0.3731(2) 0.0319(7) Uani 1 1 d . . . . .
O2 O 0.2611(2) 0.17495(13) 0.3204(2) 0.0202(5) Uani 1 1 d . . . . .
O3 O -0.1388(3) 0.2500 0.3593(3) 0.0349(10) Uani 1 2 d S T P . .
O4 O -0.0048(3) 0.2500 0.1863(3) 0.0191(7) Uani 1 2 d S T P . .
N10 N 0.0714(4) 0.2500 0.6387(3) 0.0158(8) Uani 1 2 d S T P . .
O11 O 0.0666(4) 0.2500 0.7411(3) 0.0239(8) Uani 1 2 d S T P . .
C1 C 0.0368(4) 0.06639(18) 0.3058(3) 0.0218(7) Uani 1 1 d . . . . .
C2 C 0.1355(4) 0.06144(18) 0.2430(3) 0.0187(7) Uani 1 1 d . . . . .
C2A C 0.2446(3) 0.11715(19) 0.2595(3) 0.0199(7) Uani 1 1 d . . . . .
H2A H 0.3109 0.1085 0.2193 0.024 Uiso 1 1 calc R U . . .
C3 C 0.1353(4) -0.00136(19) 0.1711(3) 0.0208(7) Uani 1 1 d . . . . .
H3 H 0.2022 -0.0031 0.1303 0.025 Uiso 1 1 calc R U . . .
C4 C 0.0418(4) -0.06107(19) 0.1569(3) 0.0215(7) Uani 1 1 d . . . . .
C4A C 0.0457(4) -0.1280(2) 0.0792(3) 0.0284(8) Uani 1 1 d . . . . .
H4A1 H -0.0049 -0.1157 -0.0055 0.043 Uiso 1 1 calc R U . . .
H4A2 H -0.0002 -0.1712 0.1025 0.043 Uiso 1 1 calc R U . . .
H4A3 H 0.1446 -0.1406 0.0900 0.043 Uiso 1 1 calc R U . . .
C5 C -0.0522(4) -0.05779(18) 0.2204(3) 0.0215(7) Uani 1 1 d . . . . .
H5 H -0.1161 -0.0985 0.2134 0.026 Uiso 1 1 calc R U . . .
C6 C -0.0565(4) 0.00333(18) 0.2946(3) 0.0210(7) Uani 1 1 d . . . . .
C7 C -0.1536(4) 0.00005(18) 0.3591(3) 0.0210(7) Uani 1 1 d . . . . .
H7 H -0.2122 -0.0433 0.3490 0.025 Uiso 1 1 calc R U . . .
N1 N -0.1671(4) 0.05270(16) 0.4310(3) 0.0246(7) Uani 1 1 d . . . . .
C8 C -0.2707(4) 0.05009(19) 0.4937(3) 0.0233(7) Uani 1 1 d . . . . .
H8A H -0.2213 0.0561 0.5813 0.028 Uiso 1 1 calc R U . . .
H8B H -0.3195 0.0007 0.4797 0.028 Uiso 1 1 calc R U . . .
C9 C -0.3785(4) 0.11233(18) 0.4480(3) 0.0248(8) Uani 1 1 d . . . . .
H9A H -0.4212 0.1091 0.3593 0.030 Uiso 1 1 calc R U . . .
H9B H -0.4555 0.1062 0.4822 0.030 Uiso 1 1 calc R U . . .
N2 N -0.3107(3) 0.18699(15) 0.4824(2) 0.0177(6) Uani 1 1 d . . . . .
H2 H -0.2179 0.1855 0.4681 0.021 Uiso 0.5 1 d R U P . .
C10 C -0.2796(4) 0.20772(18) 0.6110(3) 0.0207(7) Uani 1 1 d . . . . .
H10A H -0.1860 0.1878 0.6618 0.025 Uiso 1 1 calc R U . . .
H10B H -0.3536 0.1878 0.6412 0.025 Uiso 1 1 calc R U . . .
C12 C -0.3933(4) 0.2500 0.4108(4) 0.0117(8) Uani 1 2 d S T P . .
H12 H -0.4934 0.2500 0.4104 0.014 Uiso 1 2 calc R U P . .
C13 C -0.3880(5) 0.2500 0.2858(4) 0.0170(9) Uani 1 2 d S T P . .
C14 C -0.2543(4) 0.2500 0.2671(4) 0.0118(8) Uani 1 2 d S T P A .
C15 C -0.2551(5) 0.2500 0.1481(4) 0.0257(11) Uani 1 2 d S T P . .
C15A C -0.1289(5) 0.2500 0.1171(4) 0.0166(9) Uani 1 2 d S T P A .
H15A H -0.1422 0.2500 0.0336 0.020 Uiso 1 2 calc R U P . .
C16 C -0.3832(7) 0.2283(4) 0.0524(5) 0.0229(18) Uani 0.5 1 d . . P A -1
H16 H -0.3786 0.2170 -0.0248 0.027 Uiso 0.5 1 calc R U P A -1
C17 C -0.5123(7) 0.2234(4) 0.0702(6) 0.0245(16) Uani 0.5 1 d . . P A -1
C17A C -0.6510(8) 0.2108(5) -0.0310(6) 0.039(2) Uani 0.5 1 d . . P A -1
H17A H -0.7289 0.2091 0.0015 0.059 Uiso 0.5 1 calc R U P A -1
H17B H -0.6672 0.2520 -0.0892 0.059 Uiso 0.5 1 calc R U P A -1
H17C H -0.6469 0.1629 -0.0710 0.059 Uiso 0.5 1 calc R U P A -1
C18 C -0.5111(6) 0.2328(3) 0.1888(5) 0.0171(19) Uani 0.5 1 d . . P A -1
H18 H -0.5980 0.2272 0.2038 0.021 Uiso 0.5 1 calc R U P A -1
H1A H -0.114(4) 0.091(2) 0.434(3) 0.024(10) Uiso 1 1 d . . . . .
H1W1 H 0.361(4) 0.215(2) 0.588(4) 0.035(13) Uiso 1 1 d . . . . .
N20 N 0.5048(3) 0.08592(18) 0.7308(3) 0.0300(7) Uani 1 1 d . . . . .
O20 O 0.4122(4) 0.11165(16) 0.6373(3) 0.0569(10) Uani 1 1 d . . . . .
O21 O 0.5111(4) 0.01725(18) 0.7440(4) 0.0645(11) Uani 1 1 d . . . . .
O22 O 0.5858(4) 0.12798(19) 0.8061(3) 0.0482(8) Uani 1 1 d . . . . .
N1S N -0.6513(9) 0.0946(6) 0.0020(7) 0.055(2) Uani 0.5 1 d . . P B -2
C1S C -0.5401(12) 0.0698(11) 0.0248(9) 0.088(5) Uani 0.5 1 d . . P B -2
C2S C -0.3979(13) 0.0430(14) 0.0590(13) 0.155(11) Uani 0.5 1 d . . P B -2
H2S1 H -0.3484 0.0686 0.0112 0.232 Uiso 0.5 1 calc R U P B -2
H2S2 H -0.3985 -0.0114 0.0448 0.232 Uiso 0.5 1 calc R U P B -2
H2S3 H -0.3487 0.0534 0.1446 0.232 Uiso 0.5 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
Tb1 O3 2.306(3) . ?
Tb1 O1 2.357(2) 4_565 ?
Tb1 O1 2.357(2) . ?
Tb1 O4 2.380(3) . ?
Tb1 O1W 2.391(3) . ?
Tb1 O2 2.479(2) . ?
Tb1 O2 2.479(2) 4_565 ?
Tb1 O10 2.527(2) 4_565 ?
Tb1 O10 2.527(2) . ?
Tb1 N10 2.950(4) . ?
O1W H1W1 0.76(4) . ?
O10 N10 1.269(3) . ?
O1 C1 1.288(4) . ?
O2 C2A 1.232(4) . ?
O3 C14 1.291(5) . ?
O4 C15A 1.233(5) . ?
N10 O11 1.227(5) . ?
N10 O10 1.269(3) 4_565 ?
C1 C2 1.427(5) . ?
C1 C6 1.435(5) . ?
C2 C3 1.402(4) . ?
C2 C2A 1.437(5) . ?
C2A H2A 0.9500 . ?
C3 C4 1.386(5) . ?
C3 H3 0.9500 . ?
C4 C5 1.390(5) . ?
C4 C4A 1.511(4) . ?
C4A H4A1 0.9800 . ?
C4A H4A2 0.9800 . ?
C4A H4A3 0.9800 . ?
C5 C6 1.405(4) . ?
C5 H5 0.9500 . ?
C6 C7 1.426(5) . ?
C7 N1 1.301(4) . ?
C7 H7 0.9500 . ?
N1 C8 1.465(4) . ?
N1 H1A 0.86(4) . ?
C8 C9 1.511(5) . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C9 N2 1.482(4) . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
N2 C12 1.475(4) . ?
N2 C10 1.490(4) . ?
N2 H2 1.0000 . ?
C10 C10 1.502(6) 4_565 ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C12 N2 1.475(4) 4_565 ?
C12 C13 1.495(6) . ?
C12 H12 1.0000 . ?
C13 C18 1.402(7) . ?
C13 C14 1.428(6) . ?
C14 C15 1.404(6) . ?
C15 C15A 1.429(6) . ?
C15 C16 1.444(7) . ?
C15A H15A 0.9500 . ?
C16 C17 1.380(9) . ?
C16 H16 0.9500 . ?
C17 C18 1.407(8) . ?
C17 C17A 1.509(9) . ?
C17A H17A 0.9800 . ?
C17A H17B 0.9800 . ?
C17A H17C 0.9800 . ?
C18 H18 0.9500 . ?
N20 O21 1.229(4) . ?
N20 O22 1.232(4) . ?
N20 O20 1.262(4) . ?
N1S C1S 1.141(13) . ?
C1S C2S 1.423(15) . ?
C2S H2S1 0.9800 . ?
C2S H2S2 0.9800 . ?
C2S H2S3 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
O3 Tb1 O1 74.11(7) . 4_565 ?
O3 Tb1 O1 74.11(7) . . ?
O1 Tb1 O1 147.07(15) 4_565 . ?
O3 Tb1 O4 73.36(11) . . ?
O1 Tb1 O4 81.46(7) 4_565 . ?
O1 Tb1 O4 81.47(7) . . ?
O3 Tb1 O1W 145.71(12) . . ?
O1 Tb1 O1W 105.51(8) 4_565 . ?
O1 Tb1 O1W 105.51(8) . . ?
O4 Tb1 O1W 140.93(11) . . ?
O3 Tb1 O2 132.95(8) . . ?
O1 Tb1 O2 131.78(8) 4_565 . ?
O1 Tb1 O2 68.56(8) . . ?
O4 Tb1 O2 73.72(8) . . ?
O1W Tb1 O2 73.54(9) . . ?
O3 Tb1 O2 132.95(8) . 4_565 ?
O1 Tb1 O2 68.56(8) 4_565 4_565 ?
O1 Tb1 O2 131.78(8) . 4_565 ?
O4 Tb1 O2 73.72(8) . 4_565 ?
O1W Tb1 O2 73.54(9) . 4_565 ?
O2 Tb1 O2 65.09(11) . 4_565 ?
O3 Tb1 O10 75.73(9) . 4_565 ?
O1 Tb1 O10 65.58(8) 4_565 4_565 ?
O1 Tb1 O10 113.92(8) . 4_565 ?
O4 Tb1 O10 139.73(8) . 4_565 ?
O1W Tb1 O10 73.35(9) . 4_565 ?
O2 Tb1 O10 146.04(8) . 4_565 ?
O2 Tb1 O10 111.72(8) 4_565 4_565 ?
O3 Tb1 O10 75.73(9) . . ?
O1 Tb1 O10 113.92(8) 4_565 . ?
O1 Tb1 O10 65.58(8) . . ?
O4 Tb1 O10 139.73(8) . . ?
O1W Tb1 O10 73.35(9) . . ?
O2 Tb1 O10 111.72(8) . . ?
O2 Tb1 O10 146.04(8) 4_565 . ?
O10 Tb1 O10 50.55(10) 4_565 . ?
O3 Tb1 N10 75.45(11) . . ?
O1 Tb1 N10 90.11(6) 4_565 . ?
O1 Tb1 N10 90.11(6) . . ?
O4 Tb1 N10 148.81(10) . . ?
O1W Tb1 N10 70.26(11) . . ?
O2 Tb1 N10 130.66(7) . . ?
O2 Tb1 N10 130.66(7) 4_565 . ?
O10 Tb1 N10 25.30(5) 4_565 . ?
O10 Tb1 N10 25.30(5) . . ?
Tb1 O1W H1W1 120(3) . . ?
N10 O10 Tb1 96.34(19) . . ?
C1 O1 Tb1 139.3(2) . . ?
C2A O2 Tb1 133.9(2) . . ?
C14 O3 Tb1 138.7(3) . . ?
C15A O4 Tb1 134.1(3) . . ?
O11 N10 O10 121.75(18) . 4_565 ?
O11 N10 O10 121.75(18) . . ?
O10 N10 O10 116.5(4) 4_565 . ?
O11 N10 Tb1 176.3(3) . . ?
O10 N10 Tb1 58.35(18) 4_565 . ?
O10 N10 Tb1 58.35(18) . . ?
O1 C1 C2 122.7(3) . . ?
O1 C1 C6 120.6(3) . . ?
C2 C1 C6 116.6(3) . . ?
C3 C2 C1 120.4(3) . . ?
C3 C2 C2A 118.4(3) . . ?
C1 C2 C2A 121.0(3) . . ?
O2 C2A C2 126.7(3) . . ?
O2 C2A H2A 116.6 . . ?
C2 C2A H2A 116.6 . . ?
C4 C3 C2 123.0(3) . . ?
C4 C3 H3 118.5 . . ?
C2 C3 H3 118.5 . . ?
C3 C4 C5 117.1(3) . . ?
C3 C4 C4A 121.4(3) . . ?
C5 C4 C4A 121.5(3) . . ?
C4 C4A H4A1 109.5 . . ?
C4 C4A H4A2 109.5 . . ?
H4A1 C4A H4A2 109.5 . . ?
C4 C4A H4A3 109.5 . . ?
H4A1 C4A H4A3 109.5 . . ?
H4A2 C4A H4A3 109.5 . . ?
C4 C5 C6 122.6(3) . . ?
C4 C5 H5 118.7 . . ?
C6 C5 H5 118.7 . . ?
C5 C6 C7 118.2(3) . . ?
C5 C6 C1 120.3(3) . . ?
C7 C6 C1 121.5(3) . . ?
N1 C7 C6 124.1(3) . . ?
N1 C7 H7 118.0 . . ?
C6 C7 H7 118.0 . . ?
C7 N1 C8 123.7(3) . . ?
C7 N1 H1A 114(3) . . ?
C8 N1 H1A 122(3) . . ?
N1 C8 C9 109.8(3) . . ?
N1 C8 H8A 109.7 . . ?
C9 C8 H8A 109.7 . . ?
N1 C8 H8B 109.7 . . ?
C9 C8 H8B 109.7 . . ?
H8A C8 H8B 108.2 . . ?
N2 C9 C8 110.6(3) . . ?
N2 C9 H9A 109.5 . . ?
C8 C9 H9A 109.5 . . ?
N2 C9 H9B 109.5 . . ?
C8 C9 H9B 109.5 . . ?
H9A C9 H9B 108.1 . . ?
C12 N2 C9 114.0(2) . . ?
C12 N2 C10 106.2(3) . . ?
C9 N2 C10 114.7(3) . . ?
C12 N2 H2 107.2 . . ?
C9 N2 H2 107.1 . . ?
C10 N2 H2 107.1 . . ?
N2 C10 C10 104.31(16) . 4_565 ?
N2 C10 H10A 110.9 . . ?
C10 C10 H10A 110.9 4_565 . ?
N2 C10 H10B 110.9 . . ?
C10 C10 H10B 110.9 4_565 . ?
H10A C10 H10B 108.9 . . ?
N2 C12 N2 98.7(3) . 4_565 ?
N2 C12 C13 111.4(2) . . ?
N2 C12 C13 111.4(2) 4_565 . ?
N2 C12 H12 111.5 . . ?
N2 C12 H12 111.5 4_565 . ?
C13 C12 H12 111.5 . . ?
C18 C13 C14 118.8(4) . . ?
C18 C13 C12 119.4(4) . . ?
C14 C13 C12 120.2(4) . . ?
O3 C14 C15 123.0(4) . . ?
O3 C14 C13 119.1(4) . . ?
C15 C14 C13 117.9(4) . . ?
C14 C15 C15A 123.5(4) . . ?
C14 C15 C16 119.0(4) . . ?
C15A C15 C16 115.2(4) . . ?
O4 C15A C15 127.5(4) . . ?
O4 C15A H15A 116.3 . . ?
C15 C15A H15A 116.3 . . ?
C17 C16 C15 121.7(5) . . ?
C17 C16 H16 119.2 . . ?
C15 C16 H16 119.2 . . ?
C16 C17 C18 116.9(6) . . ?
C16 C17 C17A 123.0(6) . . ?
C18 C17 C17A 120.1(6) . . ?
C17 C17A H17A 109.5 . . ?
C17 C17A H17B 109.5 . . ?
H17A C17A H17B 109.5 . . ?
C17 C17A H17C 109.5 . . ?
H17A C17A H17C 109.5 . . ?
H17B C17A H17C 109.5 . . ?
C13 C18 C17 123.2(5) . . ?
C13 C18 H18 118.4 . . ?
C17 C18 H18 118.4 . . ?
O21 N20 O22 121.2(4) . . ?
O21 N20 O20 117.5(4) . . ?
O22 N20 O20 121.3(3) . . ?
N1S C1S C2S 176(2) . . ?
C1S C2S H2S1 109.5 . . ?
C1S C2S H2S2 109.5 . . ?
H2S1 C2S H2S2 109.5 . . ?
C1S C2S H2S3 109.5 . . ?
H2S1 C2S H2S3 109.5 . . ?
H2S2 C2S H2S3 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
Tb1 O10 N10 O11 -175.6(3) . . . . ?
Tb1 O10 N10 O10 5.1(4) . . . 4_565 ?
Tb1 O1 C1 C2 21.5(6) . . . . ?
Tb1 O1 C1 C6 -161.0(3) . . . . ?
O1 C1 C2 C3 179.9(3) . . . . ?
C6 C1 C2 C3 2.2(5) . . . . ?
O1 C1 C2 C2A 5.1(5) . . . . ?
C6 C1 C2 C2A -172.5(3) . . . . ?
Tb1 O2 C2A C2 -19.8(5) . . . . ?
C3 C2 C2A O2 -179.2(3) . . . . ?
C1 C2 C2A O2 -4.3(5) . . . . ?
C1 C2 C3 C4 0.0(5) . . . . ?
C2A C2 C3 C4 174.9(3) . . . . ?
C2 C3 C4 C5 -1.7(5) . . . . ?
C2 C3 C4 C4A -179.6(3) . . . . ?
C3 C4 C5 C6 1.2(5) . . . . ?
C4A C4 C5 C6 179.1(3) . . . . ?
C4 C5 C6 C7 -177.9(3) . . . . ?
C4 C5 C6 C1 1.0(5) . . . . ?
O1 C1 C6 C5 179.6(3) . . . . ?
C2 C1 C6 C5 -2.7(5) . . . . ?
O1 C1 C6 C7 -1.5(5) . . . . ?
C2 C1 C6 C7 176.2(3) . . . . ?
C5 C6 C7 N1 179.6(3) . . . . ?
C1 C6 C7 N1 0.7(5) . . . . ?
C6 C7 N1 C8 177.7(3) . . . . ?
C7 N1 C8 C9 -114.5(4) . . . . ?
N1 C8 C9 N2 -66.9(4) . . . . ?
C8 C9 N2 C12 161.3(3) . . . . ?
C8 C9 N2 C10 -75.9(4) . . . . ?
C12 N2 C10 C10 -27.1(2) . . . 4_565 ?
C9 N2 C10 C10 -154.1(2) . . . 4_565 ?
C9 N2 C12 N2 170.1(2) . . . 4_565 ?
C10 N2 C12 N2 42.7(4) . . . 4_565 ?
C9 N2 C12 C13 -72.7(4) . . . . ?
C10 N2 C12 C13 159.9(3) . . . . ?
N2 C12 C13 C18 110.9(4) . . . . ?
N2 C12 C13 C18 -139.9(3) 4_565 . . . ?
N2 C12 C13 C14 -54.6(2) . . . . ?
N2 C12 C13 C14 54.6(2) 4_565 . . . ?
Tb1 O3 C14 C15 0.000(1) . . . . ?
Tb1 O3 C14 C13 180.000(1) . . . . ?
C18 C13 C14 O3 -165.6(3) . . . . ?
C12 C13 C14 O3 0.000(1) . . . . ?
C18 C13 C14 C15 14.4(3) . . . . ?
C12 C13 C14 C15 180.000(1) . . . . ?
O3 C14 C15 C15A 0.000(1) . . . . ?
C13 C14 C15 C15A 180.000(1) . . . . ?
O3 C14 C15 C16 162.2(3) . . . . ?
C13 C14 C15 C16 -17.8(3) . . . . ?
Tb1 O4 C15A C15 0.000(1) . . . . ?
C14 C15 C15A O4 0.000(1) . . . . ?
C16 C15 C15A O4 -162.8(3) . . . . ?
C14 C15 C16 C17 14.3(7) . . . . ?
C15A C15 C16 C17 177.9(5) . . . . ?
C15 C16 C17 C18 -6.5(10) . . . . ?
C15 C16 C17 C17A 171.8(6) . . . . ?
C14 C13 C18 C17 -7.1(7) . . . . ?
C12 C13 C18 C17 -172.8(5) . . . . ?
C16 C17 C18 C13 3.0(9) . . . . ?
C17A C17 C18 C13 -175.3(6) . . . . ?

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
C7 H7 O20 0.95 2.39 3.273(5) 153.7 3_556
C8 H8B O20 0.99 2.43 3.342(5) 153.6 3_556
C9 H9A O21 0.99 2.57 3.188(5) 120.6 3_556
C9 H9B O20 0.99 2.60 3.546(6) 159.4 1_455
N2 H2 O3 1.00 2.07 2.834(4) 131.6 .
C10 H10A O11 0.99 2.62 3.362(5) 131.7 .
C10 H10B O22 0.99 2.47 3.353(5) 148.5 1_455
N1 H1A O1 0.86(4) 1.93(4) 2.637(4) 139(4) .
O1W H1W1 O20 0.76(4) 1.93(4) 2.670(3) 165(5) .
C2S H2S1 O22 0.98 2.52 3.303(14) 137.0 1_454

_refine_diff_density_max         0.781
_refine_diff_density_min         -1.218
_refine_diff_density_rms         0.110


_exptl_crystal_preparation       'Magnetic properties'
####################################################################### 
# 
# 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_[Er(H3L)(H2O)(NO3)](NO3)2
_database_code_depnum_ccdc_archive 'CCDC 1574342'
_audit_update_record             
;
2017-11-01 deposited with the CCDC.
2017-11-17 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C33 H38 Er N5 O10, 2(N O3)'
_chemical_formula_sum            'C33 H38 Er N7 O16'
_chemical_formula_weight         955.96

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'
Er Er -0.2586 4.9576 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           11
_space_group_name_H-M_alt        'P 21/m'
_space_group_name_Hall           '-P 2yb'

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

_cell_length_a                   10.0570(6)
_cell_length_b                   17.6505(12)
_cell_length_c                   11.8657(8)
_cell_angle_alpha                90
_cell_angle_beta                 110.362(4)
_cell_angle_gamma                90
_cell_volume                     1974.7(2)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    1965
_cell_measurement_theta_min      2.295
_cell_measurement_theta_max      20.835

_exptl_crystal_description       needle
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.608
_exptl_crystal_F_000             962
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.060
_exptl_crystal_size_min          0.040
_exptl_absorpt_coefficient_mu    2.204
_shelx_estimated_absorpt_T_min   0.667
_shelx_estimated_absorpt_T_max   0.917
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.653
_exptl_absorpt_correction_T_max  0.917
_exptl_absorpt_process_details   'SADABS-2014/5, (Bruker AXS, 2014)'
_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 Kappa APEXII CCD'
_diffrn_measurement_method       'omega and phi scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            29223
_diffrn_reflns_av_unetI/netI     0.0807
_diffrn_reflns_av_R_equivalents  0.1312
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         1.831
_diffrn_reflns_theta_max         25.348
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             3748
_reflns_number_gt                2990
_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 APEX2'
_computing_data_reduction        ?
_computing_structure_solution    'SHELXT-2014/7 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1455P)²] 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         3748
_refine_ls_number_parameters     304
_refine_ls_number_restraints     64
_refine_ls_R_factor_all          0.1011
_refine_ls_R_factor_gt           0.0789
_refine_ls_wR_factor_ref         0.2152
_refine_ls_wR_factor_gt          0.1949
_refine_ls_goodness_of_fit_ref   1.107
_refine_ls_restrained_S_all      1.106
_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
Er1 Er 0.59640(5) 0.2500 0.89453(5) 0.0284(3) Uani 1 2 d S T P . .
O1 O 0.5264(9) 0.1244(4) 0.8681(7) 0.052(2) Uani 1 1 d . . . . .
O2 O 0.7527(7) 0.1757(4) 0.8169(7) 0.0436(17) Uani 1 1 d . . . . .
O3 O 0.3596(11) 0.2500 0.8577(9) 0.044(2) Uani 1 2 d S TU P . .
O4 O 0.4896(11) 0.2500 0.6856(9) 0.043(2) Uani 1 2 d S T P . .
O1W O 0.8221(10) 0.2500 1.0453(9) 0.041(2) Uani 1 2 d S T P . .
H1W1 H 0.8572 0.2036 1.0876 0.062 Uiso 1 1 d R U . . .
O10 O 0.5720(8) 0.1893(4) 1.0764(6) 0.0400(16) Uani 1 1 d . . . . .
N10 N 0.5699(11) 0.2500 1.1322(10) 0.034(3) Uani 1 2 d S T P . .
O11 O 0.5715(11) 0.2500 1.2354(9) 0.049(3) Uani 1 2 d S T P . .
C1 C 0.5306(13) 0.0674(6) 0.8031(9) 0.043(3) Uani 1 1 d . . . . .
C2 C 0.6311(11) 0.0618(5) 0.7410(8) 0.035(2) Uani 1 1 d . . . . .
C2A C 0.7381(11) 0.1187(6) 0.7586(9) 0.039(2) Uani 1 1 d . . . . .
H2A H 0.8050 0.1103 0.7197 0.047 Uiso 1 1 calc R U . . .
C3 C 0.6301(13) -0.0022(6) 0.6702(10) 0.047(3) Uani 1 1 d . . . . .
H3 H 0.6971 -0.0041 0.6303 0.056 Uiso 1 1 calc R U . . .
C4 C 0.5392(13) -0.0617(6) 0.6552(9) 0.043(3) Uani 1 1 d . . . . .
C4A C 0.5417(15) -0.1298(7) 0.5800(10) 0.058(3) Uani 1 1 d . . . . .
H4A1 H 0.6393 -0.1397 0.5845 0.087 Uiso 1 1 calc R U . . .
H4A2 H 0.4821 -0.1203 0.4963 0.087 Uiso 1 1 calc R U . . .
H4A3 H 0.5053 -0.1739 0.6102 0.087 Uiso 1 1 calc R U . . .
C5 C 0.4430(13) -0.0578(6) 0.7173(9) 0.044(3) Uani 1 1 d . . . . .
H5 H 0.3778 -0.0982 0.7087 0.053 Uiso 1 1 calc R U . . .
C6 C 0.4398(13) 0.0032(6) 0.7911(9) 0.045(3) Uani 1 1 d . . . . .
C7 C 0.3459(12) -0.0006(6) 0.8573(10) 0.046(3) Uani 1 1 d . . . . .
H7 H 0.2892 -0.0448 0.8482 0.055 Uiso 1 1 calc R U . . .
N1 N 0.3324(11) 0.0511(5) 0.9281(8) 0.051(2) Uani 1 1 d . . . . .
H1A H 0.3887 0.0907 0.9405 0.061 Uiso 1 1 d R U . . .
C8 C 0.2259(13) 0.0488(6) 0.9915(10) 0.047(3) Uani 1 1 d . . . . .
H8A H 0.1765 -0.0007 0.9772 0.056 Uiso 1 1 calc R U . . .
H8B H 0.2751 0.0549 1.0792 0.056 Uiso 1 1 calc R U . . .
C9 C 0.1223(12) 0.1103(6) 0.9456(10) 0.047(3) Uani 1 1 d . . . . .
H9A H 0.0439 0.1038 0.9771 0.056 Uiso 1 1 calc R U . . .
H9B H 0.0818 0.1072 0.8569 0.056 Uiso 1 1 calc R U . . .
N2 N 0.1882(9) 0.1877(4) 0.9815(6) 0.0346(18) Uani 1 1 d . . . . .
H2 H 0.2816 0.1867 0.9691 0.042 Uiso 0.5 1 d R U P . .
C10 C 0.1081(13) 0.2500 0.9092(11) 0.031(3) Uani 1 2 d S TU P . .
H10 H 0.0080 0.2500 0.9076 0.037 Uiso 1 2 calc R U P . .
C11 C 0.1126(15) 0.2500 0.7870(12) 0.033(3) Uani 1 2 d S TU P . .
C12 C 0.2428(13) 0.2500 0.7666(11) 0.027(3) Uani 1 2 d S T P . .
C13 C 0.2367(14) 0.2500 0.6453(11) 0.031(3) Uani 1 2 d S T P . .
C13A C 0.3630(15) 0.2500 0.6153(11) 0.033(3) Uani 1 2 d S T P . .
H13A H 0.3492 0.2500 0.5320 0.040 Uiso 1 2 calc R U P . .
C14 C 0.115(2) 0.2500 0.5519(15) 0.075(6) Uani 1 2 d S T P . .
H14 H 0.1166 0.2634 0.4749 0.090 Uiso 0.5 1 calc R U P . .
C15 C -0.016(2) 0.2309(10) 0.5632(17) 0.043(4) Uani 0.5 1 d . U P . .
C15A C -0.164(3) 0.2202(13) 0.466(2) 0.059(5) Uani 0.5 1 d . U P . .
H15A H -0.2330 0.2070 0.5037 0.089 Uiso 0.5 1 calc R U P . .
H15B H -0.1929 0.2674 0.4201 0.089 Uiso 0.5 1 calc R U P . .
H15C H -0.1595 0.1795 0.4108 0.089 Uiso 0.5 1 calc R U P . .
C16 C -0.017(2) 0.2500 0.6883(15) 0.055(4) Uani 1 2 d S TU P . .
H16 H -0.1039 0.2617 0.6999 0.066 Uiso 0.5 1 calc R U P . .
C17 C 0.2200(13) 0.2076(6) 1.1088(9) 0.046(3) Uani 1 1 d . . . . .
H17A H 0.3136 0.1875 1.1595 0.056 Uiso 1 1 calc R U . . .
H17B H 0.1464 0.1875 1.1386 0.056 Uiso 1 1 calc R U . . .
N20 N 0.0005(13) 0.0909(8) 0.2265(15) 0.064(4) Uani 0.814(12) 1 d . . P A 1
O20 O 0.0175(19) 0.0222(10) 0.2329(18) 0.149(9) Uani 0.814(12) 1 d . . P A 1
O21 O 0.077(2) 0.1296(9) 0.3031(13) 0.116(6) Uani 0.814(12) 1 d . . P A 1
O22 O -0.0847(15) 0.1148(7) 0.1393(17) 0.115(7) Uani 0.814(12) 1 d . . P A 1
N20' N -0.008(9) -0.058(3) 0.436(7) 0.19(6) Uiso 0.186(12) 1 d D . P A 2
O20' O -0.092(8) -0.026(4) 0.469(6) 0.12(3) Uiso 0.186(12) 1 d D . P A 2
O21' O -0.063(10) -0.077(5) 0.328(7) 0.17(4) Uiso 0.186(12) 1 d D . P A 2
O22' O 0.116(9) -0.075(5) 0.488(8) 0.16(4) Uiso 0.186(12) 1 d D . P A 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
Er1 O3 2.266(10) . ?
Er1 O1 2.314(7) . ?
Er1 O1 2.314(7) 4_565 ?
Er1 O4 2.334(10) . ?
Er1 O1W 2.351(9) . ?
Er1 O2 2.460(7) 4_565 ?
Er1 O2 2.460(7) . ?
Er1 O10 2.496(7) . ?
Er1 O10 2.497(7) 4_565 ?
Er1 N10 2.923(12) . ?
O1 C1 1.277(12) . ?
O2 C2A 1.200(11) . ?
O3 C12 1.290(15) . ?
O4 C13A 1.256(16) . ?
O1W H1W1 0.9612 . ?
O10 N10 1.263(9) . ?
N10 O11 1.219(14) . ?
N10 O10 1.263(9) 4_565 ?
C1 C6 1.431(15) . ?
C1 C2 1.447(15) . ?
C2 C3 1.405(14) . ?
C2 C2A 1.433(14) . ?
C2A H2A 0.9500 . ?
C3 C4 1.363(16) . ?
C3 H3 0.9500 . ?
C4 C5 1.408(16) . ?
C4 C4A 1.503(15) . ?
C4A H4A1 0.9800 . ?
C4A H4A2 0.9800 . ?
C4A H4A3 0.9800 . ?
C5 C6 1.394(15) . ?
C5 H5 0.9500 . ?
C6 C7 1.425(16) . ?
C7 N1 1.279(14) . ?
C7 H7 0.9500 . ?
N1 C8 1.508(15) . ?
N1 H1A 0.8800 . ?
C8 C9 1.472(14) . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C9 N2 1.513(13) . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
N2 C10 1.454(11) . ?
N2 C17 1.473(12) . ?
N2 H2 1.0000 . ?
C10 N2 1.454(11) 4_565 ?
C10 C11 1.466(17) . ?
C10 H10 1.0000 . ?
C11 C12 1.412(18) . ?
C11 C16 1.42(2) . ?
C12 C13 1.419(17) . ?
C13 C14 1.33(2) . ?
C13 C13A 1.433(18) . ?
C13A H13A 0.9500 . ?
C14 C15 1.41(3) . ?
C14 H14 0.9500 . ?
C15 C16 1.53(3) . ?
C15 C15A 1.55(3) . ?
C15A H15A 0.9800 . ?
C15A H15B 0.9800 . ?
C15A H15C 0.9800 . ?
C16 H16 0.9500 . ?
C17 C17 1.50(2) 4_565 ?
C17 H17A 0.9900 . ?
C17 H17B 0.9900 . ?
N20 O22 1.169(18) . ?
N20 O21 1.183(18) . ?
N20 O20 1.224(19) . ?
N20' O20' 1.19(5) . ?
N20' O22' 1.22(5) . ?
N20' O21' 1.26(5) . ?

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
O3 Er1 O1 74.0(2) . . ?
O3 Er1 O1 74.0(2) . 4_565 ?
O1 Er1 O1 146.7(5) . 4_565 ?
O3 Er1 O4 74.4(3) . . ?
O1 Er1 O4 81.4(2) . . ?
O1 Er1 O4 81.4(2) 4_565 . ?
O3 Er1 O1W 144.9(4) . . ?
O1 Er1 O1W 105.7(2) . . ?
O1 Er1 O1W 105.7(2) 4_565 . ?
O4 Er1 O1W 140.7(3) . . ?
O3 Er1 O2 133.9(2) . 4_565 ?
O1 Er1 O2 131.6(3) . 4_565 ?
O1 Er1 O2 69.0(3) 4_565 4_565 ?
O4 Er1 O2 73.7(3) . 4_565 ?
O1W Er1 O2 73.2(3) . 4_565 ?
O3 Er1 O2 133.9(2) . . ?
O1 Er1 O2 69.0(3) . . ?
O1 Er1 O2 131.6(3) 4_565 . ?
O4 Er1 O2 73.7(3) . . ?
O1W Er1 O2 73.2(3) . . ?
O2 Er1 O2 64.5(3) 4_565 . ?
O3 Er1 O10 75.8(3) . . ?
O1 Er1 O10 65.8(2) . . ?
O1 Er1 O10 114.3(2) 4_565 . ?
O4 Er1 O10 140.4(2) . . ?
O1W Er1 O10 72.6(3) . . ?
O2 Er1 O10 145.1(2) 4_565 . ?
O2 Er1 O10 111.3(2) . . ?
O3 Er1 O10 75.8(3) . 4_565 ?
O1 Er1 O10 114.3(2) . 4_565 ?
O1 Er1 O10 65.8(2) 4_565 4_565 ?
O4 Er1 O10 140.4(2) . 4_565 ?
O1W Er1 O10 72.6(3) . 4_565 ?
O2 Er1 O10 111.3(2) 4_565 4_565 ?
O2 Er1 O10 145.1(2) . 4_565 ?
O10 Er1 O10 50.8(3) . 4_565 ?
O3 Er1 N10 75.2(3) . . ?
O1 Er1 N10 90.30(19) . . ?
O1 Er1 N10 90.30(19) 4_565 . ?
O4 Er1 N10 149.5(3) . . ?
O1W Er1 N10 69.8(3) . . ?
O2 Er1 N10 130.2(2) 4_565 . ?
O2 Er1 N10 130.2(2) . . ?
O10 Er1 N10 25.42(16) . . ?
O10 Er1 N10 25.42(16) 4_565 . ?
C1 O1 Er1 139.8(7) . . ?
C2A O2 Er1 134.2(7) . . ?
C12 O3 Er1 138.7(9) . . ?
C13A O4 Er1 133.7(9) . . ?
Er1 O1W H1W1 118.7 . . ?
N10 O10 Er1 96.5(6) . . ?
O11 N10 O10 122.0(6) . . ?
O11 N10 O10 122.0(6) . 4_565 ?
O10 N10 O10 116.0(11) . 4_565 ?
O11 N10 Er1 174.4(9) . . ?
O10 N10 Er1 58.0(6) . . ?
O10 N10 Er1 58.0(6) 4_565 . ?
O1 C1 C6 122.0(10) . . ?
O1 C1 C2 122.5(9) . . ?
C6 C1 C2 115.4(9) . . ?
C3 C2 C2A 119.9(10) . . ?
C3 C2 C1 119.9(10) . . ?
C2A C2 C1 120.0(9) . . ?
O2 C2A C2 127.3(10) . . ?
O2 C2A H2A 116.3 . . ?
C2 C2A H2A 116.3 . . ?
C4 C3 C2 124.2(11) . . ?
C4 C3 H3 117.9 . . ?
C2 C3 H3 117.9 . . ?
C3 C4 C5 116.5(10) . . ?
C3 C4 C4A 123.1(11) . . ?
C5 C4 C4A 120.4(11) . . ?
C4 C4A H4A1 109.5 . . ?
C4 C4A H4A2 109.5 . . ?
H4A1 C4A H4A2 109.5 . . ?
C4 C4A H4A3 109.5 . . ?
H4A1 C4A H4A3 109.5 . . ?
H4A2 C4A H4A3 109.5 . . ?
C6 C5 C4 122.4(10) . . ?
C6 C5 H5 118.8 . . ?
C4 C5 H5 118.8 . . ?
C5 C6 C7 118.3(10) . . ?
C5 C6 C1 121.4(10) . . ?
C7 C6 C1 120.3(10) . . ?
N1 C7 C6 124.9(10) . . ?
N1 C7 H7 117.6 . . ?
C6 C7 H7 117.6 . . ?
C7 N1 C8 124.4(10) . . ?
C7 N1 H1A 117.8 . . ?
C8 N1 H1A 117.8 . . ?
C9 C8 N1 109.3(9) . . ?
C9 C8 H8A 109.8 . . ?
N1 C8 H8A 109.8 . . ?
C9 C8 H8B 109.8 . . ?
N1 C8 H8B 109.8 . . ?
H8A C8 H8B 108.3 . . ?
C8 C9 N2 112.2(9) . . ?
C8 C9 H9A 109.2 . . ?
N2 C9 H9A 109.2 . . ?
C8 C9 H9B 109.2 . . ?
N2 C9 H9B 109.2 . . ?
H9A C9 H9B 107.9 . . ?
C10 N2 C17 107.7(8) . . ?
C10 N2 C9 114.7(7) . . ?
C17 N2 C9 114.9(8) . . ?
C10 N2 H2 106.4 . . ?
C17 N2 H2 106.0 . . ?
C9 N2 H2 106.5 . . ?
N2 C10 N2 98.3(9) . 4_565 ?
N2 C10 C11 112.5(8) . . ?
N2 C10 C11 112.5(8) 4_565 . ?
N2 C10 H10 111.0 . . ?
N2 C10 H10 111.0 4_565 . ?
C11 C10 H10 111.0 . . ?
C12 C11 C16 120.0(13) . . ?
C12 C11 C10 121.3(12) . . ?
C16 C11 C10 118.6(13) . . ?
O3 C12 C11 119.0(12) . . ?
O3 C12 C13 123.7(12) . . ?
C11 C12 C13 117.3(11) . . ?
C14 C13 C12 123.0(13) . . ?
C14 C13 C13A 115.5(12) . . ?
C12 C13 C13A 121.5(11) . . ?
O4 C13A C13 128.1(11) . . ?
O4 C13A H13A 116.0 . . ?
C13 C13A H13A 116.0 . . ?
C13 C14 C15 122.6(15) . . ?
C13 C14 H14 118.7 . . ?
C15 C14 H14 118.7 . . ?
C14 C15 C16 111.3(15) . . ?
C14 C15 C15A 130.1(18) . . ?
C16 C15 C15A 115.2(18) . . ?
C15 C15A H15A 109.5 . . ?
C15 C15A H15B 109.5 . . ?
H15A C15A H15B 109.5 . . ?
C15 C15A H15C 109.5 . . ?
H15A C15A H15C 109.5 . . ?
H15B C15A H15C 109.5 . . ?
C11 C16 C15 119.0(16) . . ?
C11 C16 H16 120.5 . . ?
C15 C16 H16 120.5 . . ?
N2 C17 C17 103.8(5) . 4_565 ?
N2 C17 H17A 111.0 . . ?
C17 C17 H17A 111.0 4_565 . ?
N2 C17 H17B 111.0 . . ?
C17 C17 H17B 111.0 4_565 . ?
H17A C17 H17B 109.0 . . ?
O22 N20 O21 123.6(17) . . ?
O22 N20 O20 117.1(17) . . ?
O21 N20 O20 119.0(17) . . ?
O20' N20' O22' 132(8) . . ?
O20' N20' O21' 111(7) . . ?
O22' N20' O21' 117(7) . . ?

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
Er1 O10 N10 O11 -173.3(10) . . . . ?
Er1 O10 N10 O10 3.7(11) . . . 4_565 ?
Er1 O1 C1 C6 -162.2(8) . . . . ?
Er1 O1 C1 C2 20.7(19) . . . . ?
O1 C1 C2 C3 -179.7(10) . . . . ?
C6 C1 C2 C3 3.0(14) . . . . ?
O1 C1 C2 C2A 4.8(15) . . . . ?
C6 C1 C2 C2A -172.5(9) . . . . ?
Er1 O2 C2A C2 -19.0(16) . . . . ?
C3 C2 C2A O2 -179.5(10) . . . . ?
C1 C2 C2A O2 -4.0(16) . . . . ?
C2A C2 C3 C4 175.2(10) . . . . ?
C1 C2 C3 C4 -0.3(16) . . . . ?
C2 C3 C4 C5 -1.2(16) . . . . ?
C2 C3 C4 C4A -179.3(10) . . . . ?
C3 C4 C5 C6 -0.2(16) . . . . ?
C4A C4 C5 C6 177.9(10) . . . . ?
C4 C5 C6 C7 -175.4(10) . . . . ?
C4 C5 C6 C1 3.1(17) . . . . ?
O1 C1 C6 C5 178.3(11) . . . . ?
C2 C1 C6 C5 -4.4(16) . . . . ?
O1 C1 C6 C7 -3.2(17) . . . . ?
C2 C1 C6 C7 174.1(10) . . . . ?
C5 C6 C7 N1 180.0(11) . . . . ?
C1 C6 C7 N1 1.5(18) . . . . ?
C6 C7 N1 C8 175.8(11) . . . . ?
C7 N1 C8 C9 -114.3(12) . . . . ?
N1 C8 C9 N2 -68.1(12) . . . . ?
C8 C9 N2 C10 160.8(9) . . . . ?
C8 C9 N2 C17 -73.7(12) . . . . ?
C17 N2 C10 N2 41.5(12) . . . 4_565 ?
C9 N2 C10 N2 170.7(6) . . . 4_565 ?
C17 N2 C10 C11 160.0(9) . . . . ?
C9 N2 C10 C11 -70.8(12) . . . . ?
N2 C10 C11 C12 -54.9(7) . . . . ?
N2 C10 C11 C12 54.9(7) 4_565 . . . ?
N2 C10 C11 C16 125.1(7) . . . . ?
N2 C10 C11 C16 -125.1(7) 4_565 . . . ?
Er1 O3 C12 C11 180.000(6) . . . . ?
Er1 O3 C12 C13 0.000(8) . . . . ?
C16 C11 C12 O3 180.000(5) . . . . ?
C10 C11 C12 O3 0.000(7) . . . . ?
C16 C11 C12 C13 0.000(6) . . . . ?
C10 C11 C12 C13 180.000(6) . . . . ?
O3 C12 C13 C14 180.000(6) . . . . ?
C11 C12 C13 C14 0.000(7) . . . . ?
O3 C12 C13 C13A 0.000(6) . . . . ?
C11 C12 C13 C13A 180.000(5) . . . . ?
Er1 O4 C13A C13 0.000(7) . . . . ?
C14 C13 C13A O4 180.000(5) . . . . ?
C12 C13 C13A O4 0.000(6) . . . . ?
C12 C13 C14 C15 -16.5(9) . . . . ?
C13A C13 C14 C15 163.5(9) . . . . ?
C13 C14 C15 C16 28.9(15) . . . . ?
C13 C14 C15 C15A -173.4(15) . . . . ?
C12 C11 C16 C15 14.7(8) . . . . ?
C10 C11 C16 C15 -165.3(8) . . . . ?
C14 C15 C16 C11 -27.8(15) . . . . ?
C15A C15 C16 C11 171.0(12) . . . . ?
C10 N2 C17 C17 -26.5(8) . . . 4_565 ?
C9 N2 C17 C17 -155.6(6) . . . 4_565 ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O1W H1W1 N20 0.96 2.66 3.611(15) 168.7 1_656
O1W H1W1 O22 0.96 1.71 2.663(14) 170.2 1_656
C7 H7 O22 0.95 2.45 3.322(18) 153.1 3_556
N1 H1A O1 0.88 1.96 2.638(12) 132.9 .
N1 H1A O10 0.88 2.64 3.451(12) 154.0 .
C8 H8A O20 0.99 2.60 3.18(2) 117.2 3_556
C8 H8A O22 0.99 2.44 3.351(19) 153.6 3_556
C9 H9B O20 0.99 2.57 3.14(2) 116.6 3_556
C9 H9B O21' 0.99 2.19 3.14(8) 159.4 3_556
N2 H2 O3 1.00 2.08 2.847(12) 131.6 .
C17 H17B N20 0.99 2.69 3.634(18) 160.6 1_556
C17 H17B O21 0.99 2.51 3.402(19) 150.3 1_556
C17 H17B O22 0.99 2.66 3.60(2) 159.6 1_556

_refine_diff_density_max         3.122
_refine_diff_density_min         -3.797
_refine_diff_density_rms         0.286

####################################################################### 
# 
# 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_Zn2Dy(4)
_database_code_depnum_ccdc_archive 'CCDC 1574343'
_audit_update_record             
;
2017-11-04 deposited with the CCDC.
2017-11-17 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2016/4
_shelx_SHELXL_version_number     2016/4
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C33 H34 Dy N7 O16 Zn2, C3 H6 O'
_chemical_formula_sum            'C36 H40 Dy N7 O17 Zn2'
_chemical_formula_weight         1135.99

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'
Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Dy Dy -0.1892 4.4098 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           62
_space_group_name_H-M_alt        'P n m a'
_space_group_name_Hall           '-P 2ac 2n'

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

_cell_length_a                   22.6952(7)
_cell_length_b                   17.2196(5)
_cell_length_c                   10.1931(2)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     3983.49(19)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    1894
_cell_measurement_theta_min      2.19
_cell_measurement_theta_max      22.67

_exptl_crystal_description       needle
_exptl_crystal_colour            green
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.894
_exptl_crystal_F_000             2268
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.240
_exptl_crystal_size_mid          0.050
_exptl_crystal_size_min          0.020
_exptl_absorpt_coefficient_mu    3.138
_shelx_estimated_absorpt_T_min   0.520
_shelx_estimated_absorpt_T_max   0.940
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.7101
_exptl_absorpt_correction_T_max  0.7897
_exptl_absorpt_process_details   'SADABS (Bruker, 2014)'
_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 Kappa APEXII CCD'
_diffrn_measurement_method       'omega and phi scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            58780
_diffrn_reflns_av_unetI/netI     0.0570
_diffrn_reflns_av_R_equivalents  0.1043
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_theta_min         2.149
_diffrn_reflns_theta_max         26.423
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             4226
_reflns_number_gt                3125
_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 APEX2'
_computing_data_reduction        ?
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2016/4 (Sheldrick, 2016)'
_computing_molecular_graphics    'Wingx (Farrugia, 1999)'
_computing_publication_material  'Wingx (Farrugia, 1993)'
_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)+(0.0091P)²+23.1547P] 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         4226
_refine_ls_number_parameters     329
_refine_ls_number_restraints     36
_refine_ls_R_factor_all          0.0745
_refine_ls_R_factor_gt           0.0429
_refine_ls_wR_factor_ref         0.0799
_refine_ls_wR_factor_gt          0.0694
_refine_ls_goodness_of_fit_ref   1.068
_refine_ls_restrained_S_all      1.064
_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 0.18787(2) 0.250000 0.03343(3) 0.01731(10) Uani 1 2 d S T P . .
ZN1 Zn 0.23581(3) 0.15454(4) 0.28073(6) 0.02328(16) Uani 1 1 d . . . . .
N1 N 0.2072(2) 0.0521(3) 0.3571(4) 0.0333(13) Uani 1 1 d . . . . .
N2 N 0.2385(2) 0.1828(3) 0.4945(4) 0.0317(12) Uani 1 1 d . . . . .
O1H O 0.2672(2) 0.250000 0.1835(4) 0.0215(12) Uani 1 2 d S T P . .
H1H H 0.310974 0.250000 0.165186 0.026 Uiso 1 2 d R U P . .
O1 O 0.18306(16) 0.1243(2) 0.1127(3) 0.0212(8) Uani 1 1 d . . . . .
O2 O 0.14750(17) 0.1721(2) -0.1345(3) 0.0251(9) Uani 1 1 d . . . . .
O3 O 0.1703(2) 0.250000 0.2695(4) 0.0214(12) Uani 1 2 d S T P . .
O4 O 0.0837(2) 0.250000 0.0804(5) 0.0266(13) Uani 1 2 d S T P . .
O10 O 0.27001(18) 0.1877(3) -0.0886(4) 0.0400(11) Uani 1 1 d . . . . .
N10 N 0.2965(3) 0.250000 -0.1198(7) 0.041(2) Uani 1 2 d S T P . .
O11 O 0.3436(3) 0.250000 -0.1767(6) 0.057(2) Uani 1 2 d S T P . .
O20 O 0.31045(19) 0.0860(3) 0.2418(4) 0.0416(11) Uani 1 1 d . . . . .
N20 N 0.3580(3) 0.1041(4) 0.1894(7) 0.0559(17) Uani 1 1 d . . . . .
O21 O 0.3847(2) 0.0529(4) 0.1250(6) 0.0780(18) Uani 1 1 d . . . . .
O22 O 0.3785(2) 0.1674(4) 0.2062(9) 0.121(3) Uani 1 1 d . . . . .
C1 C 0.1494(2) 0.0639(3) 0.0925(5) 0.0214(12) Uani 1 1 d . . . . .
C2 C 0.1178(2) 0.0551(3) -0.0285(6) 0.0234(12) Uani 1 1 d . . . . .
C3 C 0.0828(3) -0.0101(3) -0.0503(6) 0.0355(15) Uani 1 1 d . . . . .
H3 H 0.062739 -0.014944 -0.131712 0.043 Uiso 1 1 calc R U . . .
C4 C 0.0762(3) -0.0678(3) 0.0420(7) 0.0406(16) Uani 1 1 d . . . . .
C4A C 0.0381(3) -0.1383(4) 0.0145(8) 0.067(2) Uani 1 1 d . . . . .
H4A1 H 0.063388 -0.183071 -0.004491 0.100 Uiso 1 1 calc R U . . .
H4A2 H 0.012701 -0.127852 -0.061159 0.100 Uiso 1 1 calc R U . . .
H4A3 H 0.013683 -0.149612 0.091463 0.100 Uiso 1 1 calc R U . . .
C5 C 0.1064(3) -0.0596(3) 0.1574(6) 0.0371(16) Uani 1 1 d . . . . .
H5 H 0.102067 -0.098992 0.221859 0.045 Uiso 1 1 calc R U . . .
C6 C 0.1427(2) 0.0025(3) 0.1857(5) 0.0240(13) Uani 1 1 d . . . . .
C7 C 0.1730(3) 0.0004(4) 0.3120(6) 0.0327(15) Uani 1 1 d . . . . .
H7 H 0.166456 -0.043931 0.365507 0.039 Uiso 1 1 calc R U . . .
C8 C 0.2340(3) 0.0407(4) 0.4864(6) 0.0432(18) Uani 1 1 d . . . . .
H8A H 0.277293 0.035392 0.478284 0.052 Uiso 1 1 calc R U . . .
H8B H 0.218191 -0.006762 0.528488 0.052 Uiso 1 1 calc R U . . .
C9 C 0.2187(3) 0.1108(4) 0.5652(5) 0.0440(18) Uani 1 1 d . . . . .
H9A H 0.238127 0.107957 0.651977 0.053 Uiso 1 1 calc R U . . .
H9B H 0.175565 0.112830 0.579310 0.053 Uiso 1 1 calc R U . . .
C10 C 0.3004(2) 0.2059(4) 0.5240(7) 0.058(2) Uani 1 1 d . . . . .
H10A H 0.327553 0.185582 0.456251 0.070 Uiso 1 1 calc R U . . .
H10B H 0.312703 0.185582 0.610667 0.070 Uiso 1 1 calc R U . . .
C11 C 0.2029(3) 0.250000 0.5392(8) 0.0277(19) Uani 1 2 d S T P . .
H11 H 0.202272 0.250000 0.637342 0.033 Uiso 1 2 calc R U P . .
C12 C 0.1397(3) 0.250000 0.4901(7) 0.0199(17) Uani 1 2 d S T P . .
C13 C 0.1273(3) 0.250000 0.3555(7) 0.0164(16) Uani 1 2 d S T P . .
C13A C 0.1225(2) 0.1086(3) -0.1343(5) 0.0247(13) Uani 1 1 d . . . . .
H13A H 0.104220 0.093526 -0.214247 0.030 Uiso 1 1 calc R U . . .
C14 C 0.0677(3) 0.250000 0.3142(7) 0.0237(18) Uani 1 2 d S T P . .
C14A C 0.0515(4) 0.250000 0.1775(8) 0.029(2) Uani 1 2 d S T P . .
H14A H 0.010390 0.250000 0.159995 0.034 Uiso 1 2 calc R U P . .
C15 C 0.0222(4) 0.250000 0.4085(8) 0.036(2) Uani 1 2 d S T P . .
H15 H -0.017651 0.250000 0.380230 0.043 Uiso 1 2 calc R U P . .
C17 C 0.0939(4) 0.250000 0.5799(7) 0.027(2) Uani 1 2 d S T P . .
H17 H 0.102945 0.250000 0.670855 0.033 Uiso 1 2 calc R U P . .
C16 C 0.0346(3) 0.250000 0.5414(8) 0.031(2) Uani 1 2 d S T P . .
C16A C -0.0141(4) 0.250000 0.6412(9) 0.062(3) Uani 1 2 d S T P . .
H16A H -0.022582 0.196508 0.668098 0.093 Uiso 0.5 1 calc R U P . .
H16B H -0.049608 0.273105 0.602639 0.093 Uiso 0.5 1 calc R U P . .
H16C H -0.002034 0.280387 0.717870 0.093 Uiso 0.5 1 calc R U P . .
O1S O 0.4840(5) -0.0686(6) 0.1641(9) 0.059(3) Uani 0.5 1 d . U P A -1
C1S C 0.4919(6) -0.0276(8) 0.0655(12) 0.042(3) Uani 0.5 1 d . U P A -1
C2S C 0.4757(16) -0.051(2) -0.083(2) 0.047(5) Uani 0.5 1 d . U P A -1
H2SA H 0.441572 -0.086092 -0.082322 0.070 Uiso 0.5 1 calc R U P A -1
H2SB H 0.509348 -0.077501 -0.123143 0.070 Uiso 0.5 1 calc R U P A -1
H2SC H 0.466143 -0.004278 -0.132857 0.070 Uiso 0.5 1 calc R U P A -1
C3S C 0.5291(18) 0.045(2) 0.051(2) 0.053(6) Uani 0.5 1 d . U P A -1
H3SA H 0.503801 0.088513 0.027594 0.079 Uiso 0.5 1 calc R U P A -1
H3SB H 0.558579 0.036439 -0.017521 0.079 Uiso 0.5 1 calc R U P A -1
H3SC H 0.548929 0.055554 0.134614 0.079 Uiso 0.5 1 calc R U P A -1


_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 2.312(3) . ?
DY1 O1 2.312(3) 7_565 ?
DY1 O2 2.360(3) . ?
DY1 O2 2.360(3) 7_565 ?
DY1 O1H 2.362(5) . ?
DY1 O4 2.411(5) . ?
DY1 O3 2.439(5) . ?
DY1 O10 2.485(4) 7_565 ?
DY1 O10 2.485(4) . ?
DY1 N10 2.919(8) . ?
DY1 ZN1 3.2000(7) . ?
DY1 ZN1 3.2000(7) 7_565 ?
ZN1 N1 2.034(5) . ?
ZN1 O1H 2.048(3) . ?
ZN1 O20 2.103(4) . ?
ZN1 O1 2.154(3) . ?
ZN1 O3 2.219(3) . ?
ZN1 N2 2.234(4) . ?
N1 C7 1.267(8) . ?
N1 C8 1.465(7) . ?
N2 C11 1.482(6) . ?
N2 C10 1.490(7) . ?
N2 C9 1.502(8) . ?
O1H ZN1 2.048(3) 7_565 ?
O1H H1H 1.0105 . ?
O1 C1 1.307(6) . ?
O2 C13A 1.233(6) . ?
O3 C13 1.313(8) . ?
O3 ZN1 2.219(3) 7_565 ?
O4 C14A 1.231(9) . ?
O10 N10 1.271(6) . ?
N10 O11 1.215(9) . ?
N10 O10 1.271(6) 7_565 ?
O20 N20 1.244(7) . ?
N20 O22 1.198(8) . ?
N20 O21 1.255(7) . ?
C1 C6 1.430(7) . ?
C1 C2 1.435(7) . ?
C2 C3 1.394(7) . ?
C2 C13A 1.422(8) . ?
C3 C4 1.376(9) . ?
C3 H3 0.9500 . ?
C4 C5 1.368(9) . ?
C4 C4A 1.516(8) . ?
C4A H4A1 0.9800 . ?
C4A H4A2 0.9800 . ?
C4A H4A3 0.9800 . ?
C5 C6 1.380(8) . ?
C5 H5 0.9500 . ?
C6 C7 1.460(8) . ?
C7 H7 0.9500 . ?
C8 C9 1.492(9) . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C10 C10 1.520(15) 7_565 ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C11 N2 1.482(6) 7_565 ?
C11 C12 1.520(10) . ?
C11 H11 1.0000 . ?
C12 C17 1.385(10) . ?
C12 C13 1.401(10) . ?
C13 C14 1.416(10) . ?
C13A H13A 0.9500 . ?
C14 C15 1.410(11) . ?
C14 C14A 1.440(10) . ?
C14A H14A 0.9500 . ?
C15 C16 1.383(11) . ?
C15 H15 0.9500 . ?
C17 C16 1.401(11) . ?
C17 H17 0.9500 . ?
C16 C16A 1.503(11) . ?
C16A H16A 0.9800 . ?
C16A H16B 0.9800 . ?
C16A H16C 0.9800 . ?
O1S C1S 1.242(15) . ?
C1S C3S 1.51(4) . ?
C1S C2S 1.61(3) . ?
C2S H2SA 0.9800 . ?
C2S H2SB 0.9800 . ?
C2S H2SC 0.9800 . ?
C3S H3SA 0.9800 . ?
C3S H3SB 0.9800 . ?
C3S H3SC 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
O1 DY1 O1 138.71(16) . 7_565 ?
O1 DY1 O2 72.73(12) . . ?
O1 DY1 O2 140.08(12) 7_565 . ?
O1 DY1 O2 140.08(12) . 7_565 ?
O1 DY1 O2 72.73(12) 7_565 7_565 ?
O2 DY1 O2 69.27(17) . 7_565 ?
O1 DY1 O1H 79.04(9) . . ?
O1 DY1 O1H 79.04(9) 7_565 . ?
O2 DY1 O1H 139.96(10) . . ?
O2 DY1 O1H 139.96(10) 7_565 . ?
O1 DY1 O4 83.35(10) . . ?
O1 DY1 O4 83.35(10) 7_565 . ?
O2 DY1 O4 76.32(13) . . ?
O2 DY1 O4 76.32(13) 7_565 . ?
O1H DY1 O4 128.20(17) . . ?
O1 DY1 O3 69.37(8) . . ?
O1 DY1 O3 69.37(8) 7_565 . ?
O2 DY1 O3 130.70(12) . . ?
O2 DY1 O3 130.70(12) 7_565 . ?
O1H DY1 O3 59.06(16) . . ?
O4 DY1 O3 69.14(16) . . ?
O1 DY1 O10 127.92(14) . 7_565 ?
O1 DY1 O10 78.82(14) 7_565 7_565 ?
O2 DY1 O10 100.01(14) . 7_565 ?
O2 DY1 O10 71.50(13) 7_565 7_565 ?
O1H DY1 O10 75.66(14) . 7_565 ?
O4 DY1 O10 146.59(12) . 7_565 ?
O3 DY1 O10 128.06(14) . 7_565 ?
O1 DY1 O10 78.82(14) . . ?
O1 DY1 O10 127.92(14) 7_565 . ?
O2 DY1 O10 71.50(13) . . ?
O2 DY1 O10 100.01(14) 7_565 . ?
O1H DY1 O10 75.66(14) . . ?
O4 DY1 O10 146.59(12) . . ?
O3 DY1 O10 128.06(14) . . ?
O10 DY1 O10 51.2(2) 7_565 . ?
O1 DY1 N10 103.11(10) . . ?
O1 DY1 N10 103.11(10) 7_565 . ?
O2 DY1 N10 86.56(15) . . ?
O2 DY1 N10 86.56(15) 7_565 . ?
O1H DY1 N10 72.69(18) . . ?
O4 DY1 N10 159.11(18) . . ?
O3 DY1 N10 131.75(18) . . ?
O10 DY1 N10 25.63(11) 7_565 . ?
O10 DY1 N10 25.62(11) . . ?
O1 DY1 ZN1 42.28(8) . . ?
O1 DY1 ZN1 102.80(8) 7_565 . ?
O2 DY1 ZN1 114.30(9) . . ?
O2 DY1 ZN1 174.49(9) 7_565 . ?
O1H DY1 ZN1 39.73(7) . . ?
O4 DY1 ZN1 100.17(10) . . ?
O3 DY1 ZN1 43.81(8) . . ?
O10 DY1 ZN1 111.17(10) 7_565 . ?
O10 DY1 ZN1 85.26(10) . . ?
N10 DY1 ZN1 97.72(12) . . ?
O1 DY1 ZN1 102.80(8) . 7_565 ?
O1 DY1 ZN1 42.28(8) 7_565 7_565 ?
O2 DY1 ZN1 174.49(9) . 7_565 ?
O2 DY1 ZN1 114.30(9) 7_565 7_565 ?
O1H DY1 ZN1 39.73(7) . 7_565 ?
O4 DY1 ZN1 100.18(10) . 7_565 ?
O3 DY1 ZN1 43.81(8) . 7_565 ?
O10 DY1 ZN1 85.26(10) 7_565 7_565 ?
O10 DY1 ZN1 111.17(10) . 7_565 ?
N10 DY1 ZN1 97.72(12) . 7_565 ?
ZN1 DY1 ZN1 61.82(2) . 7_565 ?
N1 ZN1 O1H 172.92(18) . . ?
N1 ZN1 O20 80.97(18) . . ?
O1H ZN1 O20 94.53(17) . . ?
N1 ZN1 O1 85.26(17) . . ?
O1H ZN1 O1 90.12(15) . . ?
O20 ZN1 O1 99.34(15) . . ?
N1 ZN1 O3 116.61(17) . . ?
O1H ZN1 O3 67.26(16) . . ?
O20 ZN1 O3 161.05(16) . . ?
O1 ZN1 O3 76.43(14) . . ?
N1 ZN1 N2 79.9(2) . . ?
O1H ZN1 N2 106.75(18) . . ?
O20 ZN1 N2 106.53(16) . . ?
O1 ZN1 N2 147.53(16) . . ?
O3 ZN1 N2 84.68(17) . . ?
N1 ZN1 DY1 129.65(14) . . ?
O1H ZN1 DY1 47.51(13) . . ?
O20 ZN1 DY1 114.44(11) . . ?
O1 ZN1 DY1 46.25(9) . . ?
O3 ZN1 DY1 49.53(12) . . ?
N2 ZN1 DY1 131.75(13) . . ?
C7 N1 C8 119.1(5) . . ?
C7 N1 ZN1 131.8(4) . . ?
C8 N1 ZN1 109.1(4) . . ?
C11 N2 C10 104.1(5) . . ?
C11 N2 C9 109.5(4) . . ?
C10 N2 C9 113.9(5) . . ?
C11 N2 ZN1 117.1(4) . . ?
C10 N2 ZN1 106.3(3) . . ?
C9 N2 ZN1 106.2(3) . . ?
ZN1 O1H ZN1 106.8(2) 7_565 . ?
ZN1 O1H DY1 92.76(16) 7_565 . ?
ZN1 O1H DY1 92.76(16) . . ?
ZN1 O1H H1H 115.5 7_565 . ?
ZN1 O1H H1H 115.6 . . ?
DY1 O1H H1H 129.0 . . ?
C1 O1 ZN1 130.0(3) . . ?
C1 O1 DY1 135.8(3) . . ?
ZN1 O1 DY1 91.47(13) . . ?
C13A O2 DY1 133.0(3) . . ?
C13 O3 ZN1 117.6(2) . . ?
C13 O3 ZN1 117.6(2) . 7_565 ?
ZN1 O3 ZN1 95.59(18) . 7_565 ?
C13 O3 DY1 141.3(4) . . ?
ZN1 O3 DY1 86.66(14) . . ?
ZN1 O3 DY1 86.66(14) 7_565 . ?
C14A O4 DY1 137.9(5) . . ?
N10 O10 DY1 96.7(4) . . ?
O11 N10 O10 122.4(4) . . ?
O11 N10 O10 122.4(4) . 7_565 ?
O10 N10 O10 115.2(7) . 7_565 ?
O11 N10 DY1 176.1(5) . . ?
O10 N10 DY1 57.7(4) . . ?
O10 N10 DY1 57.7(4) 7_565 . ?
N20 O20 ZN1 129.8(4) . . ?
O22 N20 O20 120.2(7) . . ?
O22 N20 O21 121.9(7) . . ?
O20 N20 O21 117.9(7) . . ?
O1 C1 C6 123.1(5) . . ?
O1 C1 C2 120.8(5) . . ?
C6 C1 C2 116.1(5) . . ?
C3 C2 C13A 116.3(5) . . ?
C3 C2 C1 120.5(5) . . ?
C13A C2 C1 123.1(5) . . ?
C4 C3 C2 122.3(6) . . ?
C4 C3 H3 118.8 . . ?
C2 C3 H3 118.8 . . ?
C5 C4 C3 117.3(6) . . ?
C5 C4 C4A 121.8(6) . . ?
C3 C4 C4A 120.9(7) . . ?
C4 C4A H4A1 109.5 . . ?
C4 C4A H4A2 109.5 . . ?
H4A1 C4A H4A2 109.5 . . ?
C4 C4A H4A3 109.5 . . ?
H4A1 C4A H4A3 109.5 . . ?
H4A2 C4A H4A3 109.5 . . ?
C4 C5 C6 124.0(6) . . ?
C4 C5 H5 118.0 . . ?
C6 C5 H5 118.0 . . ?
C5 C6 C1 119.8(5) . . ?
C5 C6 C7 116.5(5) . . ?
C1 C6 C7 123.6(5) . . ?
N1 C7 C6 126.2(5) . . ?
N1 C7 H7 116.9 . . ?
C6 C7 H7 116.9 . . ?
N1 C8 C9 106.1(5) . . ?
N1 C8 H8A 110.5 . . ?
C9 C8 H8A 110.5 . . ?
N1 C8 H8B 110.5 . . ?
C9 C8 H8B 110.5 . . ?
H8A C8 H8B 108.7 . . ?
C8 C9 N2 109.9(5) . . ?
C8 C9 H9A 109.7 . . ?
N2 C9 H9A 109.7 . . ?
C8 C9 H9B 109.7 . . ?
N2 C9 H9B 109.7 . . ?
H9A C9 H9B 108.2 . . ?
N2 C10 C10 105.4(4) . 7_565 ?
N2 C10 H10A 110.7 . . ?
C10 C10 H10A 110.7 7_565 . ?
N2 C10 H10B 110.7 . . ?
C10 C10 H10B 110.7 7_565 . ?
H10A C10 H10B 108.8 . . ?
N2 C11 N2 102.6(6) . 7_565 ?
N2 C11 C12 114.4(4) . . ?
N2 C11 C12 114.4(4) 7_565 . ?
N2 C11 H11 108.4 . . ?
N2 C11 H11 108.4 7_565 . ?
C12 C11 H11 108.4 . . ?
C17 C12 C13 119.7(7) . . ?
C17 C12 C11 119.4(6) . . ?
C13 C12 C11 120.9(6) . . ?
O3 C13 C12 120.3(6) . . ?
O3 C13 C14 120.8(6) . . ?
C12 C13 C14 118.9(7) . . ?
O2 C13A C2 127.6(5) . . ?
O2 C13A H13A 116.2 . . ?
C2 C13A H13A 116.2 . . ?
C15 C14 C13 119.7(7) . . ?
C15 C14 C14A 118.2(7) . . ?
C13 C14 C14A 122.0(7) . . ?
O4 C14A C14 128.8(7) . . ?
O4 C14A H14A 115.6 . . ?
C14 C14A H14A 115.6 . . ?
C16 C15 C14 121.3(8) . . ?
C16 C15 H15 119.4 . . ?
C14 C15 H15 119.4 . . ?
C12 C17 C16 122.4(7) . . ?
C12 C17 H17 118.8 . . ?
C16 C17 H17 118.8 . . ?
C15 C16 C17 118.0(7) . . ?
C15 C16 C16A 120.9(8) . . ?
C17 C16 C16A 121.1(8) . . ?
C16 C16A H16A 109.5 . . ?
C16 C16A H16B 109.5 . . ?
H16A C16A H16B 109.5 . . ?
C16 C16A H16C 109.5 . . ?
H16A C16A H16C 109.5 . . ?
H16B C16A H16C 109.5 . . ?
O1S C1S C3S 128.8(16) . . ?
O1S C1S C2S 125.7(18) . . ?
C3S C1S C2S 104.3(19) . . ?
C1S C2S H2SA 109.5 . . ?
C1S C2S H2SB 109.5 . . ?
H2SA C2S H2SB 109.5 . . ?
C1S C2S H2SC 109.5 . . ?
H2SA C2S H2SC 109.5 . . ?
H2SB C2S H2SC 109.5 . . ?
C1S C3S H3SA 109.5 . . ?
C1S C3S H3SB 109.5 . . ?
H3SA C3S H3SB 109.5 . . ?
C1S C3S H3SC 109.5 . . ?
H3SA C3S H3SC 109.5 . . ?
H3SB C3S H3SC 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
DY1 O10 N10 O11 175.4(6) . . . . ?
DY1 O10 N10 O10 -5.3(7) . . . 7_565 ?
ZN1 O20 N20 O22 34.5(11) . . . . ?
ZN1 O20 N20 O21 -149.1(5) . . . . ?
ZN1 O1 C1 C6 -1.5(7) . . . . ?
DY1 O1 C1 C6 -157.1(4) . . . . ?
ZN1 O1 C1 C2 -179.9(3) . . . . ?
DY1 O1 C1 C2 24.5(7) . . . . ?
O1 C1 C2 C3 178.9(5) . . . . ?
C6 C1 C2 C3 0.3(7) . . . . ?
O1 C1 C2 C13A 2.4(8) . . . . ?
C6 C1 C2 C13A -176.1(5) . . . . ?
C13A C2 C3 C4 177.6(5) . . . . ?
C1 C2 C3 C4 0.9(9) . . . . ?
C2 C3 C4 C5 -1.0(9) . . . . ?
C2 C3 C4 C4A -179.5(6) . . . . ?
C3 C4 C5 C6 -0.1(10) . . . . ?
C4A C4 C5 C6 178.3(6) . . . . ?
C4 C5 C6 C1 1.4(9) . . . . ?
C4 C5 C6 C7 -178.0(6) . . . . ?
O1 C1 C6 C5 -179.9(5) . . . . ?
C2 C1 C6 C5 -1.4(7) . . . . ?
O1 C1 C6 C7 -0.5(8) . . . . ?
C2 C1 C6 C7 177.9(5) . . . . ?
C8 N1 C7 C6 180.0(5) . . . . ?
ZN1 N1 C7 C6 -1.3(9) . . . . ?
C5 C6 C7 N1 -178.6(6) . . . . ?
C1 C6 C7 N1 2.0(9) . . . . ?
C7 N1 C8 C9 -125.4(6) . . . . ?
ZN1 N1 C8 C9 55.6(6) . . . . ?
N1 C8 C9 N2 -55.4(7) . . . . ?
C11 N2 C9 C8 156.2(5) . . . . ?
C10 N2 C9 C8 -87.8(6) . . . . ?
ZN1 N2 C9 C8 28.8(6) . . . . ?
C11 N2 C10 C10 -25.3(4) . . . 7_565 ?
C9 N2 C10 C10 -144.5(4) . . . 7_565 ?
ZN1 N2 C10 C10 98.9(2) . . . 7_565 ?
C10 N2 C11 N2 41.2(7) . . . 7_565 ?
C9 N2 C11 N2 163.3(4) . . . 7_565 ?
ZN1 N2 C11 N2 -75.7(6) . . . 7_565 ?
C10 N2 C11 C12 165.7(5) . . . . ?
C9 N2 C11 C12 -72.2(6) . . . . ?
ZN1 N2 C11 C12 48.7(6) . . . . ?
N2 C11 C12 C17 121.0(5) . . . . ?
N2 C11 C12 C17 -121.0(5) 7_565 . . . ?
N2 C11 C12 C13 -59.0(5) . . . . ?
N2 C11 C12 C13 59.0(5) 7_565 . . . ?
ZN1 O3 C13 C12 56.7(2) . . . . ?
ZN1 O3 C13 C12 -56.7(2) 7_565 . . . ?
DY1 O3 C13 C12 180.000(1) . . . . ?
ZN1 O3 C13 C14 -123.3(2) . . . . ?
ZN1 O3 C13 C14 123.3(2) 7_565 . . . ?
DY1 O3 C13 C14 0.000(1) . . . . ?
C17 C12 C13 O3 180.000(1) . . . . ?
C11 C12 C13 O3 0.000(1) . . . . ?
C17 C12 C13 C14 0.000(1) . . . . ?
C11 C12 C13 C14 180.000(1) . . . . ?
DY1 O2 C13A C2 -10.4(9) . . . . ?
C3 C2 C13A O2 174.7(5) . . . . ?
C1 C2 C13A O2 -8.7(9) . . . . ?
O3 C13 C14 C15 180.000(1) . . . . ?
C12 C13 C14 C15 0.000(1) . . . . ?
O3 C13 C14 C14A 0.000(1) . . . . ?
C12 C13 C14 C14A 180.000(1) . . . . ?
DY1 O4 C14A C14 0.000(1) . . . . ?
C15 C14 C14A O4 180.000(1) . . . . ?
C13 C14 C14A O4 0.000(1) . . . . ?
C13 C14 C15 C16 0.000(1) . . . . ?
C14A C14 C15 C16 180.000(1) . . . . ?
C13 C12 C17 C16 0.000(1) . . . . ?
C11 C12 C17 C16 180.000(1) . . . . ?
C14 C15 C16 C17 0.000(1) . . . . ?
C14 C15 C16 C16A 180.000(1) . . . . ?
C12 C17 C16 C15 0.000(1) . . . . ?
C12 C17 C16 C16A 180.000(1) . . . . ?

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
O1H H1H O22 1.01 2.13 2.907(7) 132.1 .
O1H H1H O22_$2 1.01 2.13 2.907(7) 132.1 7_565
C8 H8B O20_$1 0.99 2.65 3.543(8) 150.5 4
C8 H8B O21_$1 0.99 2.65 3.441(9) 136.6 4
C10 H10B O11_$3 0.99 2.53 3.294(8) 133.4 1_556
C13A H13A O1S_$5 0.95 2.39 3.246(11) 149.1 4_554
C2S H2SB O21_$4 0.98 2.44 3.20(4) 133.7 5_655
C3S H3SB O21_$4 0.98 2.29 3.14(3) 145.5 5_655

_refine_diff_density_max         1.015
_refine_diff_density_min         -1.022
_refine_diff_density_rms         0.157


_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: Acetone/methanol'
####################################################################### 
# 
# 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(Dy)
_database_code_depnum_ccdc_archive 'CCDC 1574341'
_audit_update_record             
;
2017-11-16 deposited with the CCDC.
2017-11-17 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C33 H38 Dy N5 O10, 2(N O3), 0.5(C2 H3 N)'
_chemical_formula_sum            'C34 H39.50 Dy N7.50 O16'
_chemical_formula_weight         971.73

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           4
_space_group_name_H-M_alt        'P 21'
_space_group_name_Hall           'P 2yb'

_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'

_cell_length_a                   9.9976(12)
_cell_length_b                   17.7134(19)
_cell_length_c                   11.8299(14)
_cell_angle_alpha                90
_cell_angle_beta                 110.076(8)
_cell_angle_gamma                90
_cell_volume                     1967.7(4)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    1921
_cell_measurement_theta_min      2.455
_cell_measurement_theta_max      31.965

_exptl_crystal_description       needle
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.640
_exptl_crystal_F_000             980
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.270
_exptl_crystal_size_mid          0.080
_exptl_crystal_size_min          0.040
_exptl_absorpt_coefficient_mu    1.980
_shelx_estimated_absorpt_T_min   0.617
_shelx_estimated_absorpt_T_max   0.925
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.808
_exptl_absorpt_correction_T_max  0.925
_exptl_absorpt_process_details   'SADABS-2014/5 (Bruker AXS, 2014)'
_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 Kappa APEXII CCD'
_diffrn_measurement_method       'omega and phi scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            58167
_diffrn_reflns_av_unetI/netI     0.0622
_diffrn_reflns_av_R_equivalents  0.0565
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         1.833
_diffrn_reflns_theta_max         33.141
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             15013
_reflns_number_gt                12901
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.945
_reflns_Friedel_fraction_max     0.999
_reflns_Friedel_fraction_full    1.000

_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 APEX2'
_computing_data_reduction        ?
_computing_structure_solution    'SHELXS-2014/7 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Wingx 2014.1 (Farrugia, 2012)'
_computing_publication_material  'Wingx 2014.1 (Farrugia, 2012)'
_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)+(0.0466P)²+1.5837P] 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_abs_structure_details 
;
 Flack x determined using 5453 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.474(8)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         15013
_refine_ls_number_parameters     546
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0528
_refine_ls_R_factor_gt           0.0416
_refine_ls_wR_factor_ref         0.0997
_refine_ls_wR_factor_gt          0.0940
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_restrained_S_all      1.054
_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
Dy1 Dy 1.60026(2) 0.31324(5) 1.39664(2) 0.01108(5) Uani 1 1 d . . . . .
N1 N 1.3511(8) 0.1142(4) 1.4345(8) 0.0185(15) Uani 1 1 d . . . . .
H1A H 1.3883 0.1632 1.4282 0.022 Uiso 1 1 d R U . . .
N2 N 1.3154(8) 0.5099(4) 1.4272(8) 0.0190(15) Uani 1 1 d . . . . .
H2A H 1.3985 0.4722 1.4412 0.08(4) Uiso 1 1 d R . . . .
N3 N 1.1975(8) 0.2510(5) 1.4815(7) 0.0141(14) Uani 1 1 d . . . . .
N4 N 1.1798(9) 0.3778(4) 1.4828(8) 0.0179(16) Uani 1 1 d . . . . .
H4A H 1.2635 0.3735 1.4455 0.02(2) Uiso 1 1 d R . . . .
O1 O 1.5093(6) 0.4367(3) 1.3609(6) 0.0193(13) Uani 1 1 d . . . . .
O2 O 1.7525(8) 0.3918(4) 1.3203(8) 0.0210(15) Uani 1 1 d . . . . .
O3 O 1.5525(6) 0.1832(3) 1.3814(6) 0.0181(12) Uani 1 1 d . . . . .
O4 O 1.7626(7) 0.2423(4) 1.3162(8) 0.0196(14) Uani 1 1 d . . . . .
O5 O 1.3595(4) 0.3023(4) 1.3577(3) 0.0212(14) Uani 1 1 d . . . . .
O6 O 1.4924(4) 0.3101(6) 1.1849(3) 0.0191(7) Uani 1 1 d . . . . .
O1W O 1.8289(4) 0.3105(6) 1.5493(3) 0.0199(7) Uani 1 1 d . . . . .
H1W2 H 1.8779 0.3518 1.5871 0.030 Uiso 1 1 d R U . . .
H1W1 H 1.8608 0.2694 1.5693 0.030 Uiso 1 1 d R U . . .
O10 O 1.5666(8) 0.2556(4) 1.5798(7) 0.0181(15) Uani 1 1 d . . . . .
O11 O 1.5786(8) 0.3770(5) 1.5784(8) 0.0200(15) Uani 1 1 d . . . . .
N10 N 1.5715(4) 0.3161(7) 1.6355(4) 0.0166(8) Uani 1 1 d . . . . .
O12 O 1.5684(4) 0.3175(6) 1.7378(3) 0.0234(9) Uani 1 1 d . . . . .
C1 C 1.5509(9) 0.1283(5) 1.3076(9) 0.0155(16) Uani 1 1 d . . . . .
C2 C 1.6454(11) 0.1253(6) 1.2420(10) 0.0178(18) Uani 1 1 d . . . . .
C2A C 1.7485(11) 0.1833(6) 1.2550(11) 0.0200(19) Uani 1 1 d . . . . .
H2B H 1.8131 0.1765 1.2128 0.024 Uiso 1 1 calc R U . . .
C3 C 1.6440(11) 0.0642(6) 1.1727(10) 0.0186(18) Uani 1 1 d . . . . .
H3 H 1.7115 0.0630 1.1325 0.022 Uiso 1 1 calc R U . . .
C4A C 1.5586(13) -0.0636(6) 1.0801(11) 0.028(2) Uani 1 1 d . . . . .
H4A1 H 1.4980 -0.1039 1.0926 0.042 Uiso 1 1 calc R U . . .
H4A2 H 1.6571 -0.0816 1.1034 0.042 Uiso 1 1 calc R U . . .
H4A3 H 1.5248 -0.0491 0.9950 0.042 Uiso 1 1 calc R U . . .
C4 C 1.5525(10) 0.0036(5) 1.1556(9) 0.0170(17) Uani 1 1 d . . . . .
C5 C 1.4595(11) 0.0049(6) 1.2214(10) 0.0208(19) Uani 1 1 d . . . . .
H5 H 1.3963 -0.0362 1.2149 0.025 Uiso 1 1 calc R U . . .
C6 C 1.4582(9) 0.0654(6) 1.2962(10) 0.0174(17) Uani 1 1 d . . . . .
C7 C 1.3609(9) 0.0626(5) 1.3620(9) 0.0160(16) Uani 1 1 d . . . . .
H7 H 1.3003 0.0198 1.3510 0.019 Uiso 1 1 calc R U . . .
C8 C 1.2478(9) 0.1145(4) 1.4958(9) 0.0157(15) Uani 1 1 d . . . . .
H8A H 1.2971 0.1236 1.5828 0.019 Uiso 1 1 calc R U . . .
H8B H 1.2007 0.0645 1.4864 0.019 Uiso 1 1 calc R U . . .
C9 C 1.1362(9) 0.1753(5) 1.4447(9) 0.0196(17) Uani 1 1 d . . . . .
H9A H 1.0994 0.1719 1.3557 0.024 Uiso 1 1 calc R U . . .
H9B H 1.0555 0.1673 1.4737 0.024 Uiso 1 1 calc R U . . .
C10 C 1.2306(13) 0.2705(7) 1.6102(11) 0.023(2) Uani 1 1 d . . . . .
H10A H 1.3295 0.2562 1.6583 0.028 Uiso 1 1 calc R U . . .
H10B H 1.1644 0.2447 1.6435 0.028 Uiso 1 1 calc R U . . .
C11 C 1.2112(13) 0.3553(7) 1.6098(10) 0.020(2) Uani 1 1 d . . . . .
H11A H 1.1314 0.3689 1.6374 0.024 Uiso 1 1 calc R U . . .
H11B H 1.2990 0.3803 1.6627 0.024 Uiso 1 1 calc R U . . .
C12 C 1.1056(9) 0.4511(5) 1.4508(9) 0.0178(16) Uani 1 1 d . . . . .
H12A H 1.0337 0.4560 1.4907 0.021 Uiso 1 1 calc R U . . .
H12B H 1.0556 0.4536 1.3627 0.021 Uiso 1 1 calc R U . . .
C13 C 1.2123(9) 0.5152(5) 1.4902(9) 0.0191(17) Uani 1 1 d . . . . .
H13A H 1.1619 0.5642 1.4718 0.023 Uiso 1 1 calc R U . . .
H13B H 1.2628 0.5124 1.5782 0.023 Uiso 1 1 calc R U . . .
C14 C 1.3286(10) 0.5634(5) 1.3552(9) 0.0184(17) Uani 1 1 d . . . . .
H14 H 1.2696 0.6068 1.3446 0.022 Uiso 1 1 calc R U . . .
C15 C 1.4261(10) 0.5600(5) 1.2924(9) 0.0154(16) Uani 1 1 d . . . . .
C16 C 1.5180(10) 0.4963(5) 1.3015(9) 0.0162(16) Uani 1 1 d . . . . .
C17 C 1.6211(10) 0.5031(5) 1.2418(10) 0.0149(16) Uani 1 1 d . . . . .
C17A C 1.7344(11) 0.4491(6) 1.2589(10) 0.0192(19) Uani 1 1 d . . . . .
H17A H 1.8006 0.4588 1.2192 0.023 Uiso 1 1 calc R U . . .
C18 C 1.6205(11) 0.5685(6) 1.1673(10) 0.022(2) Uani 1 1 d . . . . .
H18 H 1.6849 0.5707 1.1242 0.026 Uiso 1 1 calc R U . . .
C19 C 1.5261(11) 0.6278(6) 1.1587(10) 0.0203(18) Uani 1 1 d . . . . .
C19' C 1.5297(12) 0.6955(6) 1.0788(11) 0.026(2) Uani 1 1 d . . . . .
H19A H 1.4320 0.7111 1.0327 0.038 Uiso 1 1 calc R U . . .
H19B H 1.5789 0.6811 1.0232 0.038 Uiso 1 1 calc R U . . .
H19C H 1.5803 0.7375 1.1293 0.038 Uiso 1 1 calc R U . . .
C20 C 1.4331(11) 0.6229(6) 1.2193(10) 0.0195(18) Uani 1 1 d . . . . .
H20 H 1.3691 0.6637 1.2126 0.023 Uiso 1 1 calc R U . . .
C21 C 1.1060(4) 0.3158(9) 1.4100(4) 0.0126(8) Uani 1 1 d . . . . .
H21 H 1.0059 0.3121 1.4093 0.015 Uiso 1 1 calc R U . . .
C22 C 1.1102(5) 0.3173(8) 1.2854(4) 0.0150(10) Uani 1 1 d . . . . .
C23 C 1.2439(4) 0.3147(7) 1.2675(4) 0.0119(7) Uani 1 1 d . . . . .
C24 C 1.2417(6) 0.3202(8) 1.1476(5) 0.0200(16) Uani 1 1 d . . . . .
C24A C 1.3678(5) 0.3141(8) 1.1160(4) 0.0156(8) Uani 1 1 d . . . . .
H24A H 1.3536 0.3129 1.0324 0.019 Uiso 1 1 calc R U . . .
C25 C 1.1131(7) 0.3341(4) 1.0525(6) 0.0254(15) Uani 1 1 d . . . . .
H25 H 1.1152 0.3401 0.9733 0.030 Uiso 1 1 calc R U . . .
C26 C 0.9837(7) 0.3392(4) 1.0708(6) 0.0276(14) Uani 1 1 d . . . . .
C26A C 0.8449(9) 0.3519(6) 0.9687(7) 0.049(2) Uani 1 1 d . . . . .
H26A H 0.8647 0.3661 0.8960 0.073 Uiso 1 1 calc R U . . .
H26B H 0.7916 0.3925 0.9904 0.073 Uiso 1 1 calc R U . . .
H26C H 0.7884 0.3054 0.9537 0.073 Uiso 1 1 calc R U . . .
C27 C 0.9849(6) 0.3305(3) 1.1890(5) 0.0202(14) Uani 1 1 d . . . . .
H27 H 0.8975 0.3338 1.2039 0.024 Uiso 1 1 calc R U . . .
N20 N 0.9969(9) 0.4785(4) 0.7243(9) 0.0240(17) Uani 1 1 d . . . . .
O20 O 1.0697(12) 0.4367(7) 0.8029(10) 0.058(3) Uani 1 1 d . . . . .
O21 O 0.8909(7) 0.4509(5) 0.6407(10) 0.050(2) Uani 1 1 d . . . . .
O22 O 1.0121(13) 0.5462(6) 0.7233(13) 0.091(5) Uani 1 1 d . . . . .
N30 N 0.9917(14) 0.6553(7) 1.2655(12) 0.058(4) Uani 1 1 d . . . . .
O30 O 0.9027(12) 0.6949(7) 1.1918(10) 0.053(3) Uani 1 1 d . . . . .
O31 O 1.0647(8) 0.6773(5) 1.3661(8) 0.0412(18) Uani 1 1 d . . . . .
O32 O 0.9818(10) 0.5830(5) 1.2453(10) 0.057(3) Uani 1 1 d . . . . .
N1S N 1.1474(18) 0.6569(10) 0.9970(13) 0.049(4) Uani 0.5 1 d . . P A -1
C1S C 1.043(2) 0.6265(17) 0.9784(16) 0.076(9) Uani 0.5 1 d . . P A -1
C2S C 0.895(2) 0.6107(17) 0.9410(19) 0.071(8) Uani 0.5 1 d . . P A -1
H2S1 H 0.8474 0.6493 0.9731 0.107 Uiso 0.5 1 calc R U P A -1
H2S2 H 0.8802 0.5610 0.9712 0.107 Uiso 0.5 1 calc R U P A -1
H2S3 H 0.8545 0.6109 0.8529 0.107 Uiso 0.5 1 calc R U P A -1


_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 O5 2.299(4) . ?
Dy1 O3 2.346(6) . ?
Dy1 O1 2.350(6) . ?
Dy1 O6 2.363(3) . ?
Dy1 O1W 2.378(3) . ?
Dy1 O2 2.452(7) . ?
Dy1 O4 2.485(7) . ?
Dy1 O11 2.503(8) . ?
Dy1 O10 2.520(8) . ?
Dy1 N10 2.938(4) . ?
N1 C7 1.280(13) . ?
N1 C8 1.452(12) . ?
N1 H1A 0.9568 . ?
N2 C14 1.312(13) . ?
N2 C13 1.467(11) . ?
N2 H2A 1.0346 . ?
N3 C9 1.476(13) . ?
N3 C10 1.484(15) . ?
N3 C21 1.529(15) . ?
N4 C21 1.434(15) . ?
N4 C12 1.479(12) . ?
N4 C11 1.480(15) . ?
N4 H4A 1.0741 . ?
O1 C16 1.288(11) . ?
O2 C17A 1.224(13) . ?
O3 C1 1.305(11) . ?
O4 C2A 1.252(13) . ?
O5 C23 1.295(6) . ?
O6 C24A 1.235(5) . ?
O1W H1W2 0.9082 . ?
O1W H1W1 0.7974 . ?
O10 N10 1.249(13) . ?
O11 N10 1.288(13) . ?
N10 O12 1.221(5) . ?
C1 C2 1.414(14) . ?
C1 C6 1.426(12) . ?
C2 C3 1.356(15) . ?
C2 C2A 1.425(15) . ?
C2A H2B 0.9500 . ?
C3 C4 1.380(13) . ?
C3 H3 0.9500 . ?
C4A C4 1.501(14) . ?
C4A H4A1 0.9800 . ?
C4A H4A2 0.9800 . ?
C4A H4A3 0.9800 . ?
C4 C5 1.403(14) . ?
C5 C6 1.392(15) . ?
C5 H5 0.9500 . ?
C6 C7 1.441(14) . ?
C7 H7 0.9500 . ?
C8 C9 1.520(12) . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C10 C11 1.515(8) . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C12 C13 1.518(13) . ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
C13 H13A 0.9900 . ?
C13 H13B 0.9900 . ?
C14 C15 1.415(14) . ?
C14 H14 0.9500 . ?
C15 C20 1.427(14) . ?
C15 C16 1.436(13) . ?
C16 C17 1.441(13) . ?
C17 C17A 1.443(15) . ?
C17 C18 1.453(14) . ?
C17A H17A 0.9500 . ?
C18 C19 1.393(14) . ?
C18 H18 0.9500 . ?
C19 C20 1.357(15) . ?
C19 C19' 1.536(15) . ?
C19' H19A 0.9800 . ?
C19' H19B 0.9800 . ?
C19' H19C 0.9800 . ?
C20 H20 0.9500 . ?
C21 C22 1.490(6) . ?
C21 H21 1.0000 . ?
C22 C27 1.394(8) . ?
C22 C23 1.423(6) . ?
C23 C24 1.414(7) . ?
C24 C25 1.409(8) . ?
C24 C24A 1.437(7) . ?
C24A H24A 0.9500 . ?
C25 C26 1.387(9) . ?
C25 H25 0.9500 . ?
C26 C27 1.403(9) . ?
C26 C26A 1.511(10) . ?
C26A H26A 0.9800 . ?
C26A H26B 0.9800 . ?
C26A H26C 0.9800 . ?
C27 H27 0.9500 . ?
N20 O22 1.210(12) . ?
N20 O20 1.215(12) . ?
N20 O21 1.273(12) . ?
N30 O31 1.227(15) . ?
N30 O30 1.230(15) . ?
N30 O32 1.300(14) . ?
N1S C1S 1.13(3) . ?
C1S C2S 1.42(3) . ?
C2S H2S1 0.9800 . ?
C2S H2S2 0.9800 . ?
C2S H2S3 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
O5 Dy1 O3 74.4(2) . . ?
O5 Dy1 O1 74.2(2) . . ?
O3 Dy1 O1 147.5(2) . . ?
O5 Dy1 O6 73.76(12) . . ?
O3 Dy1 O6 83.6(3) . . ?
O1 Dy1 O6 79.8(3) . . ?
O5 Dy1 O1W 144.88(14) . . ?
O3 Dy1 O1W 98.9(3) . . ?
O1 Dy1 O1W 111.6(3) . . ?
O6 Dy1 O1W 140.75(12) . . ?
O5 Dy1 O2 135.5(2) . . ?
O3 Dy1 O2 131.7(2) . . ?
O1 Dy1 O2 69.9(2) . . ?
O6 Dy1 O2 74.8(3) . . ?
O1W Dy1 O2 74.6(3) . . ?
O5 Dy1 O4 131.1(2) . . ?
O3 Dy1 O4 67.5(2) . . ?
O1 Dy1 O4 131.7(2) . . ?
O6 Dy1 O4 72.7(2) . . ?
O1W Dy1 O4 72.3(2) . . ?
O2 Dy1 O4 64.97(15) . . ?
O5 Dy1 O11 79.4(2) . . ?
O3 Dy1 O11 115.7(2) . . ?
O1 Dy1 O11 66.0(2) . . ?
O6 Dy1 O11 141.1(3) . . ?
O1W Dy1 O11 72.6(2) . . ?
O2 Dy1 O11 107.9(3) . . ?
O4 Dy1 O11 144.8(3) . . ?
O5 Dy1 O10 72.4(2) . . ?
O3 Dy1 O10 65.5(2) . . ?
O1 Dy1 O10 112.0(2) . . ?
O6 Dy1 O10 139.0(3) . . ?
O1W Dy1 O10 73.5(2) . . ?
O2 Dy1 O10 146.1(3) . . ?
O4 Dy1 O10 115.0(3) . . ?
O11 Dy1 O10 50.77(13) . . ?
O5 Dy1 N10 75.66(12) . . ?
O3 Dy1 N10 90.3(3) . . ?
O1 Dy1 N10 89.9(3) . . ?
O6 Dy1 N10 149.33(11) . . ?
O1W Dy1 N10 69.87(12) . . ?
O2 Dy1 N10 128.5(3) . . ?
O4 Dy1 N10 132.0(3) . . ?
O11 Dy1 N10 25.8(3) . . ?
O10 Dy1 N10 25.0(3) . . ?
C7 N1 C8 124.6(8) . . ?
C7 N1 H1A 118.4 . . ?
C8 N1 H1A 113.4 . . ?
C14 N2 C13 121.9(8) . . ?
C14 N2 H2A 108.4 . . ?
C13 N2 H2A 128.7 . . ?
C9 N3 C10 116.0(9) . . ?
C9 N3 C21 114.1(8) . . ?
C10 N3 C21 105.9(8) . . ?
C21 N4 C12 114.1(8) . . ?
C21 N4 C11 106.9(8) . . ?
C12 N4 C11 114.1(8) . . ?
C21 N4 H4A 90.7 . . ?
C12 N4 H4A 110.4 . . ?
C11 N4 H4A 118.3 . . ?
C16 O1 Dy1 140.1(6) . . ?
C17A O2 Dy1 134.8(7) . . ?
C1 O3 Dy1 137.7(6) . . ?
C2A O4 Dy1 133.3(7) . . ?
C23 O5 Dy1 136.7(4) . . ?
C24A O6 Dy1 133.5(3) . . ?
Dy1 O1W H1W2 124.9 . . ?
Dy1 O1W H1W1 115.2 . . ?
H1W2 O1W H1W1 119.7 . . ?
N10 O10 Dy1 96.6(5) . . ?
N10 O11 Dy1 96.3(6) . . ?
O12 N10 O10 122.1(12) . . ?
O12 N10 O11 121.9(12) . . ?
O10 N10 O11 116.1(4) . . ?
O12 N10 Dy1 176.1(3) . . ?
O10 N10 Dy1 58.4(4) . . ?
O11 N10 Dy1 57.9(4) . . ?
O3 C1 C2 122.5(8) . . ?
O3 C1 C6 120.3(8) . . ?
C2 C1 C6 117.0(9) . . ?
C3 C2 C1 119.4(10) . . ?
C3 C2 C2A 119.9(10) . . ?
C1 C2 C2A 120.6(10) . . ?
O4 C2A C2 126.7(10) . . ?
O4 C2A H2B 116.7 . . ?
C2 C2A H2B 116.7 . . ?
C2 C3 C4 125.4(10) . . ?
C2 C3 H3 117.3 . . ?
C4 C3 H3 117.3 . . ?
C4 C4A H4A1 109.5 . . ?
C4 C4A H4A2 109.5 . . ?
H4A1 C4A H4A2 109.5 . . ?
C4 C4A H4A3 109.5 . . ?
H4A1 C4A H4A3 109.5 . . ?
H4A2 C4A H4A3 109.5 . . ?
C3 C4 C5 116.0(10) . . ?
C3 C4 C4A 122.9(9) . . ?
C5 C4 C4A 120.9(9) . . ?
C6 C5 C4 121.2(9) . . ?
C6 C5 H5 119.4 . . ?
C4 C5 H5 119.4 . . ?
C5 C6 C1 120.9(9) . . ?
C5 C6 C7 118.2(9) . . ?
C1 C6 C7 120.9(9) . . ?
N1 C7 C6 123.9(9) . . ?
N1 C7 H7 118.0 . . ?
C6 C7 H7 118.0 . . ?
N1 C8 C9 110.7(8) . . ?
N1 C8 H8A 109.5 . . ?
C9 C8 H8A 109.5 . . ?
N1 C8 H8B 109.5 . . ?
C9 C8 H8B 109.5 . . ?
H8A C8 H8B 108.1 . . ?
N3 C9 C8 110.7(7) . . ?
N3 C9 H9A 109.5 . . ?
C8 C9 H9A 109.5 . . ?
N3 C9 H9B 109.5 . . ?
C8 C9 H9B 109.5 . . ?
H9A C9 H9B 108.1 . . ?
N3 C10 C11 104.1(11) . . ?
N3 C10 H10A 110.9 . . ?
C11 C10 H10A 110.9 . . ?
N3 C10 H10B 110.9 . . ?
C11 C10 H10B 110.9 . . ?
H10A C10 H10B 108.9 . . ?
N4 C11 C10 104.6(11) . . ?
N4 C11 H11A 110.8 . . ?
C10 C11 H11A 110.8 . . ?
N4 C11 H11B 110.8 . . ?
C10 C11 H11B 110.8 . . ?
H11A C11 H11B 108.9 . . ?
N4 C12 C13 109.9(7) . . ?
N4 C12 H12A 109.7 . . ?
C13 C12 H12A 109.7 . . ?
N4 C12 H12B 109.7 . . ?
C13 C12 H12B 109.7 . . ?
H12A C12 H12B 108.2 . . ?
N2 C13 C12 109.8(8) . . ?
N2 C13 H13A 109.7 . . ?
C12 C13 H13A 109.7 . . ?
N2 C13 H13B 109.7 . . ?
C12 C13 H13B 109.7 . . ?
H13A C13 H13B 108.2 . . ?
N2 C14 C15 123.5(9) . . ?
N2 C14 H14 118.2 . . ?
C15 C14 H14 118.2 . . ?
C14 C15 C20 118.1(9) . . ?
C14 C15 C16 122.1(8) . . ?
C20 C15 C16 119.7(9) . . ?
O1 C16 C15 121.6(8) . . ?
O1 C16 C17 122.0(9) . . ?
C15 C16 C17 116.4(8) . . ?
C16 C17 C17A 122.4(9) . . ?
C16 C17 C18 120.6(9) . . ?
C17A C17 C18 116.9(9) . . ?
O2 C17A C17 125.6(9) . . ?
O2 C17A H17A 117.2 . . ?
C17 C17A H17A 117.2 . . ?
C19 C18 C17 120.5(10) . . ?
C19 C18 H18 119.8 . . ?
C17 C18 H18 119.8 . . ?
C20 C19 C18 118.9(10) . . ?
C20 C19 C19' 122.7(9) . . ?
C18 C19 C19' 118.4(9) . . ?
C19 C19' H19A 109.5 . . ?
C19 C19' H19B 109.5 . . ?
H19A C19' H19B 109.5 . . ?
C19 C19' H19C 109.5 . . ?
H19A C19' H19C 109.5 . . ?
H19B C19' H19C 109.5 . . ?
C19 C20 C15 123.7(10) . . ?
C19 C20 H20 118.2 . . ?
C15 C20 H20 118.2 . . ?
N4 C21 C22 113.4(10) . . ?
N4 C21 N3 98.9(3) . . ?
C22 C21 N3 110.3(9) . . ?
N4 C21 H21 111.2 . . ?
C22 C21 H21 111.2 . . ?
N3 C21 H21 111.2 . . ?
C27 C22 C23 120.7(5) . . ?
C27 C22 C21 119.3(5) . . ?
C23 C22 C21 119.6(4) . . ?
O5 C23 C24 122.7(4) . . ?
O5 C23 C22 120.1(4) . . ?
C24 C23 C22 117.0(4) . . ?
C25 C24 C23 120.6(5) . . ?
C25 C24 C24A 116.5(5) . . ?
C23 C24 C24A 122.9(5) . . ?
O6 C24A C24 127.5(4) . . ?
O6 C24A H24A 116.3 . . ?
C24 C24A H24A 116.3 . . ?
C26 C25 C24 122.1(6) . . ?
C26 C25 H25 118.9 . . ?
C24 C25 H25 118.9 . . ?
C25 C26 C27 117.3(6) . . ?
C25 C26 C26A 122.4(6) . . ?
C27 C26 C26A 120.3(6) . . ?
C26 C26A H26A 109.5 . . ?
C26 C26A H26B 109.5 . . ?
H26A C26A H26B 109.5 . . ?
C26 C26A H26C 109.5 . . ?
H26A C26A H26C 109.5 . . ?
H26B C26A H26C 109.5 . . ?
C22 C27 C26 122.1(5) . . ?
C22 C27 H27 119.0 . . ?
C26 C27 H27 119.0 . . ?
O22 N20 O20 124.5(11) . . ?
O22 N20 O21 116.5(10) . . ?
O20 N20 O21 118.8(10) . . ?
O31 N30 O30 123.5(13) . . ?
O31 N30 O32 118.2(12) . . ?
O30 N30 O32 116.1(13) . . ?
N1S C1S C2S 162(3) . . ?
C1S C2S H2S1 109.5 . . ?
C1S C2S H2S2 109.5 . . ?
H2S1 C2S H2S2 109.5 . . ?
C1S C2S H2S3 109.5 . . ?
H2S1 C2S H2S3 109.5 . . ?
H2S2 C2S H2S3 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
Dy1 O10 N10 O12 -175.4(4) . . . . ?
Dy1 O10 N10 O11 5.2(4) . . . . ?
Dy1 O11 N10 O12 175.4(4) . . . . ?
Dy1 O11 N10 O10 -5.3(4) . . . . ?
Dy1 O3 C1 C2 33.0(14) . . . . ?
Dy1 O3 C1 C6 -151.3(7) . . . . ?
O3 C1 C2 C3 175.9(9) . . . . ?
C6 C1 C2 C3 0.0(14) . . . . ?
O3 C1 C2 C2A 0.4(15) . . . . ?
C6 C1 C2 C2A -175.5(10) . . . . ?
Dy1 O4 C2A C2 -20.6(18) . . . . ?
C3 C2 C2A O4 -179.6(11) . . . . ?
C1 C2 C2A O4 -4.2(18) . . . . ?
C1 C2 C3 C4 2.6(17) . . . . ?
C2A C2 C3 C4 178.1(10) . . . . ?
C2 C3 C4 C5 -3.5(16) . . . . ?
C2 C3 C4 C4A -178.4(11) . . . . ?
C3 C4 C5 C6 1.9(15) . . . . ?
C4A C4 C5 C6 176.8(10) . . . . ?
C4 C5 C6 C1 0.4(16) . . . . ?
C4 C5 C6 C7 -179.4(10) . . . . ?
O3 C1 C6 C5 -177.4(9) . . . . ?
C2 C1 C6 C5 -1.4(15) . . . . ?
O3 C1 C6 C7 2.4(15) . . . . ?
C2 C1 C6 C7 178.4(9) . . . . ?
C8 N1 C7 C6 176.0(9) . . . . ?
C5 C6 C7 N1 179.1(10) . . . . ?
C1 C6 C7 N1 -0.7(16) . . . . ?
C7 N1 C8 C9 -109.3(11) . . . . ?
C10 N3 C9 C8 -71.1(10) . . . . ?
C21 N3 C9 C8 165.4(7) . . . . ?
N1 C8 C9 N3 -72.0(10) . . . . ?
C9 N3 C10 C11 -149.8(10) . . . . ?
C21 N3 C10 C11 -22.1(13) . . . . ?
C21 N4 C11 C10 31.2(13) . . . . ?
C12 N4 C11 C10 158.4(10) . . . . ?
N3 C10 C11 N4 -4.2(15) . . . . ?
C21 N4 C12 C13 -155.5(8) . . . . ?
C11 N4 C12 C13 81.1(10) . . . . ?
C14 N2 C13 C12 118.3(10) . . . . ?
N4 C12 C13 N2 61.7(11) . . . . ?
C13 N2 C14 C15 -179.6(9) . . . . ?
N2 C14 C15 C20 -178.3(10) . . . . ?
N2 C14 C15 C16 0.9(15) . . . . ?
Dy1 O1 C16 C15 171.8(7) . . . . ?
Dy1 O1 C16 C17 -8.9(16) . . . . ?
C14 C15 C16 O1 4.9(15) . . . . ?
C20 C15 C16 O1 -175.9(9) . . . . ?
C14 C15 C16 C17 -174.5(9) . . . . ?
C20 C15 C16 C17 4.7(14) . . . . ?
O1 C16 C17 C17A -9.4(16) . . . . ?
C15 C16 C17 C17A 170.0(9) . . . . ?
O1 C16 C17 C18 174.9(9) . . . . ?
C15 C16 C17 C18 -5.8(14) . . . . ?
Dy1 O2 C17A C17 21.1(18) . . . . ?
C16 C17 C17A O2 2.8(17) . . . . ?
C18 C17 C17A O2 178.7(10) . . . . ?
C16 C17 C18 C19 4.2(16) . . . . ?
C17A C17 C18 C19 -171.8(10) . . . . ?
C17 C18 C19 C20 -1.2(16) . . . . ?
C17 C18 C19 C19' -180.0(10) . . . . ?
C18 C19 C20 C15 0.1(17) . . . . ?
C19' C19 C20 C15 178.8(10) . . . . ?
C14 C15 C20 C19 177.2(10) . . . . ?
C16 C15 C20 C19 -2.0(16) . . . . ?
C12 N4 C21 C22 72.6(10) . . . . ?
C11 N4 C21 C22 -160.2(8) . . . . ?
C12 N4 C21 N3 -170.6(8) . . . . ?
C11 N4 C21 N3 -43.4(7) . . . . ?
C9 N3 C21 N4 169.1(8) . . . . ?
C10 N3 C21 N4 40.3(8) . . . . ?
C9 N3 C21 C22 -71.8(10) . . . . ?
C10 N3 C21 C22 159.4(9) . . . . ?
N4 C21 C22 C27 -112.1(10) . . . . ?
N3 C21 C22 C27 138.0(9) . . . . ?
N4 C21 C22 C23 60.2(16) . . . . ?
N3 C21 C22 C23 -49.7(15) . . . . ?
Dy1 O5 C23 C24 19.3(19) . . . . ?
Dy1 O5 C23 C22 -165.6(8) . . . . ?
C27 C22 C23 O5 -180.0(10) . . . . ?
C21 C22 C23 O5 7.8(19) . . . . ?
C27 C22 C23 C24 -4.7(18) . . . . ?
C21 C22 C23 C24 -176.9(13) . . . . ?
O5 C23 C24 C25 -179.7(10) . . . . ?
C22 C23 C24 C25 5.1(19) . . . . ?
O5 C23 C24 C24A -1(2) . . . . ?
C22 C23 C24 C24A -176.4(13) . . . . ?
Dy1 O6 C24A C24 -2(2) . . . . ?
C25 C24 C24A O6 171.7(12) . . . . ?
C23 C24 C24A O6 -7(2) . . . . ?
C23 C24 C25 C26 -3.2(16) . . . . ?
C24A C24 C25 C26 178.3(10) . . . . ?
C24 C25 C26 C27 0.5(11) . . . . ?
C24 C25 C26 C26A -178.3(9) . . . . ?
C23 C22 C27 C26 2.2(15) . . . . ?
C21 C22 C27 C26 174.4(10) . . . . ?
C25 C26 C27 C22 0.0(11) . . . . ?
C26A C26 C27 C22 178.8(9) . . . . ?

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
N1 H1A O3 0.96 1.94 2.610(10) 125.3 .
N1 H1A O5 0.96 2.59 3.462(11) 152.4 .
N1 H1A O10 0.96 2.62 3.365(11) 134.8 .
N2 H2A O1 1.03 1.80 2.665(10) 138.2 .
N2 H2A O11 1.03 2.59 3.527(12) 150.3 .
N4 H4A O5 1.07 2.07 3.004(10) 144.1 .
O1W H1W2 O21 0.91 1.86 2.698(13) 153.2 1_656
O1W H1W1 O31 0.80 1.85 2.640(13) 173.2 2_848
C2A H2B N1S 0.95 2.67 3.509(19) 148.2 2_847
C7 H7 O21 0.95 2.30 3.193(12) 156.6 2_747
C8 H8B O21 0.99 2.49 3.374(13) 148.4 2_747
C9 H9A O22 0.99 2.52 3.059(15) 113.8 2_747
C9 H9B O31 0.99 2.57 3.483(12) 152.6 2_748
C10 H10A O12 0.99 2.49 3.298(14) 138.0 .
C10 H10B N30 0.99 2.69 3.675(18) 171.2 2_748
C10 H10B O30 0.99 2.43 3.346(17) 153.0 2_748
C10 H10B O31 0.99 2.55 3.477(15) 155.6 2_748
C11 H11A O20 0.99 2.55 3.394(16) 143.4 1_556
C12 H12A O21 0.99 2.63 3.601(14) 165.7 1_556
C12 H12B O32 0.99 2.65 3.292(15) 122.7 .
C13 H13A O31 0.99 2.38 3.330(13) 159.6 .
C14 H14 O31 0.95 2.49 3.359(12) 152.7 .
C21 H21 O4 1.00 2.61 3.478(10) 145.0 1_455
C2S H2S1 O30 0.98 2.58 3.30(2) 129.9 .

_refine_diff_density_max         1.306
_refine_diff_density_min         -1.025
_refine_diff_density_rms         0.141


_exptl_crystal_preparation       'Magnetic properties'
