# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2019

####################################################################### 
# 
# 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_mz
_database_code_depnum_ccdc_archive 'CCDC 1902974'
_audit_update_record             
;
2019-03-13 deposited with the CCDC.	2019-10-31 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C23 H21 N7 O6'
_chemical_formula_weight         491.47

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'

_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                   4.6284(2)
_cell_length_b                   18.7941(10)
_cell_length_c                   26.5269(14)
_cell_angle_alpha                90
_cell_angle_beta                 93.527(2)
_cell_angle_gamma                90
_cell_volume                     2303.1(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    7795
_cell_measurement_theta_min      2.31
_cell_measurement_theta_max      25.86

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.417
_exptl_crystal_F_000             1024
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.380
_exptl_crystal_size_mid          0.320
_exptl_crystal_size_min          0.280
_exptl_absorpt_coefficient_mu    0.106
_shelx_estimated_absorpt_T_min   0.961
_shelx_estimated_absorpt_T_max   0.971
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.28
_exptl_absorpt_correction_T_max  0.38
_exptl_absorpt_process_details   sadabs
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            24932
_diffrn_reflns_av_unetI/netI     0.0328
_diffrn_reflns_av_R_equivalents  0.0526
_diffrn_reflns_limit_h_min       -5
_diffrn_reflns_limit_h_max       5
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_theta_min         2.300
_diffrn_reflns_theta_max         25.010
_diffrn_reflns_theta_full        25.010
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             4070
_reflns_number_gt                2919
_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 SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0931P)²+1.8002P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         4070
_refine_ls_number_parameters     328
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0818
_refine_ls_R_factor_gt           0.0553
_refine_ls_wR_factor_ref         0.1661
_refine_ls_wR_factor_gt          0.1422
_refine_ls_goodness_of_fit_ref   1.017
_refine_ls_restrained_S_all      1.017
_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
C21 C 1.5911(7) 0.41650(17) 0.46120(13) 0.0492(8) Uani 1 1 d . . . . .
H21A H 1.764680 0.403714 0.443851 0.074 Uiso 1 1 calc R U . . .
H21B H 1.644385 0.425890 0.496909 0.074 Uiso 1 1 calc R U . . .
H21C H 1.503319 0.459229 0.445614 0.074 Uiso 1 1 calc R U . . .
C20 C 1.0700(6) 0.28772(14) 0.40853(10) 0.0301(6) Uani 1 1 d . . . . .
C19 C 1.2734(6) 0.34297(14) 0.40997(10) 0.0329(6) Uani 1 1 d . . . . .
C18 C 1.3425(6) 0.37671(15) 0.36599(11) 0.0376(7) Uani 1 1 d . . . . .
H18 H 1.481813 0.413884 0.367223 0.045 Uiso 1 1 calc R U . . .
C17 C 1.2076(7) 0.35614(16) 0.31982(11) 0.0427(7) Uani 1 1 d . . . . .
H17 H 1.257771 0.378743 0.289541 0.051 Uiso 1 1 calc R U . . .
C16 C 1.0022(6) 0.30325(15) 0.31805(11) 0.0386(7) Uani 1 1 d . . . . .
H16 H 0.907956 0.290349 0.286544 0.046 Uiso 1 1 calc R U . . .
C15 C 0.9299(6) 0.26806(14) 0.36220(9) 0.0289(6) Uani 1 1 d . . . . .
C14 C 0.7105(5) 0.21334(13) 0.35861(9) 0.0281(6) Uani 1 1 d . . . . .
C13 C 0.3982(5) 0.07885(13) 0.42677(9) 0.0255(5) Uani 1 1 d . . . . .
C1 C -0.0857(6) -0.06854(14) 0.43175(9) 0.0295(6) Uani 1 1 d . . . . .
H1 H -0.154462 -0.108470 0.449415 0.035 Uiso 1 1 calc R U . . .
C12 C 0.1728(5) 0.02481(12) 0.41438(9) 0.0239(5) Uani 1 1 d . . . . .
C2 C -0.0305(5) 0.01028(13) 0.37534(9) 0.0253(5) Uani 1 1 d . . . . .
C3 C -0.0847(5) 0.04651(13) 0.32643(9) 0.0258(6) Uani 1 1 d . . . . .
C4 C -0.5796(6) 0.03001(14) 0.22207(10) 0.0318(6) Uani 1 1 d . . . . .
C5 C -0.6483(6) 0.06596(14) 0.17400(10) 0.0293(6) Uani 1 1 d . . . . .
C6 C -0.8591(6) 0.03682(15) 0.14023(10) 0.0361(7) Uani 1 1 d . . . . .
H6 H -0.958878 -0.005003 0.149288 0.043 Uiso 1 1 calc R U . . .
C7 C -0.9243(6) 0.06792(16) 0.09397(11) 0.0399(7) Uani 1 1 d . . . . .
H7 H -1.065981 0.046915 0.071168 0.048 Uiso 1 1 calc R U . . .
C8 C -0.7846(6) 0.12982(16) 0.08034(10) 0.0372(7) Uani 1 1 d . . . . .
H8 H -0.830755 0.151027 0.048346 0.045 Uiso 1 1 calc R U . . .
C9 C -0.5782(6) 0.16047(14) 0.11341(10) 0.0329(6) Uani 1 1 d . . . . .
C10 C -0.5073(6) 0.12884(15) 0.16057(10) 0.0321(6) Uani 1 1 d . . . . .
C11 C -0.4849(8) 0.25548(18) 0.05639(12) 0.0534(9) Uani 1 1 d . . . . .
H11A H -0.421365 0.224095 0.029727 0.080 Uiso 1 1 calc R U . . .
H11B H -0.378211 0.300481 0.055768 0.080 Uiso 1 1 calc R U . . .
H11C H -0.692691 0.264842 0.050761 0.080 Uiso 1 1 calc R U . . .
C22 C 0.8895(6) 0.34951(15) 0.18998(10) 0.0363(7) Uani 1 1 d . . . . .
C23 C 1.0985(6) 0.29722(15) 0.17564(12) 0.0426(7) Uani 1 1 d . . . . .
H23A H 1.240169 0.319940 0.154860 0.064 Uiso 1 1 calc R U . . .
H23B H 0.998839 0.259115 0.156286 0.064 Uiso 1 1 calc R U . . .
H23C H 1.198266 0.277179 0.206067 0.064 Uiso 1 1 calc R U . . .
N6 N 0.6509(4) 0.17735(11) 0.39784(8) 0.0271(5) Uani 1 1 d . . . . .
N5 N 0.4387(4) 0.12646(11) 0.39017(7) 0.0261(5) Uani 1 1 d . . . . .
H5 H 0.331071 0.125189 0.361660 0.031 Uiso 1 1 calc R U . . .
N2 N 0.1317(4) -0.02669(11) 0.44952(8) 0.0269(5) Uani 1 1 d . . . . .
H2 H 0.230678 -0.031542 0.478721 0.032 Uiso 1 1 calc R U . . .
N1 N -0.1933(5) -0.04796(11) 0.38695(8) 0.0287(5) Uani 1 1 d . . . . .
N3 N -0.3061(5) 0.01999(12) 0.29674(8) 0.0293(5) Uani 1 1 d . . . . .
H3 H -0.406185 -0.017080 0.306012 0.035 Uiso 1 1 calc R U . . .
N4 N -0.3684(5) 0.05360(12) 0.25127(8) 0.0308(5) Uani 1 1 d . . . . .
N7 N 0.7257(6) 0.39127(14) 0.20166(9) 0.0438(6) Uani 1 1 d . . . . .
O6 O 1.3888(4) 0.35926(11) 0.45717(7) 0.0457(5) Uani 1 1 d . . . . .
O5 O 1.0157(4) 0.25583(11) 0.45284(7) 0.0391(5) Uani 1 1 d . . . . .
H5A H 0.891266 0.223718 0.447515 0.059 Uiso 1 1 calc R U . . .
O4 O 0.5341(4) 0.07866(9) 0.46821(6) 0.0317(4) Uani 1 1 d . . . . .
O1 O 0.0608(4) 0.09770(9) 0.31275(6) 0.0310(4) Uani 1 1 d . . . . .
O2 O -0.3037(4) 0.16180(10) 0.19129(7) 0.0409(5) Uani 1 1 d . . . . .
H2A H -0.277916 0.138711 0.218307 0.061 Uiso 1 1 calc R U . . .
O3 O -0.4301(5) 0.22195(10) 0.10444(7) 0.0426(5) Uani 1 1 d . . . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C21 O6 1.426(4) . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C20 O5 1.357(3) . ?
C20 C19 1.401(4) . ?
C20 C15 1.403(4) . ?
C19 O6 1.366(3) . ?
C19 C18 1.382(4) . ?
C18 C17 1.395(4) . ?
C18 H18 0.9500 . ?
C17 C16 1.374(4) . ?
C17 H17 0.9500 . ?
C16 C15 1.403(4) . ?
C16 H16 0.9500 . ?
C15 C14 1.444(4) . ?
C14 N6 1.285(3) . ?
C13 O4 1.233(3) . ?
C13 N5 1.342(3) . ?
C13 C12 1.478(4) . ?
C1 N1 1.318(3) . ?
C1 N2 1.340(3) . ?
C1 H1 0.9500 . ?
C12 N2 1.365(3) . ?
C12 C2 1.383(3) . ?
C2 N1 1.374(3) . ?
C2 C3 1.473(3) . ?
C3 O1 1.241(3) . ?
C3 N3 1.349(3) . ?
C4 N4 1.288(3) . ?
C4 C5 1.461(4) . ?
C5 C6 1.395(4) . ?
C5 C10 1.407(4) . ?
C6 C7 1.376(4) . ?
C6 H6 0.9500 . ?
C7 C8 1.390(4) . ?
C7 H7 0.9500 . ?
C8 C9 1.382(4) . ?
C8 H8 0.9500 . ?
C9 O3 1.372(3) . ?
C9 C10 1.406(4) . ?
C10 O2 1.357(3) . ?
C11 O3 1.430(4) . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C22 N7 1.147(4) . ?
C22 C23 1.446(4) . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 H23C 0.9800 . ?
N6 N5 1.377(3) . ?
N5 H5 0.8800 . ?
N2 H2 0.8800 . ?
N3 N4 1.376(3) . ?
N3 H3 0.8800 . ?
O5 H5A 0.8400 . ?
O2 H2A 0.8400 . ?

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
O6 C21 H21A 109.5 . . ?
O6 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
O6 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
O5 C20 C19 117.7(2) . . ?
O5 C20 C15 122.8(2) . . ?
C19 C20 C15 119.5(2) . . ?
O6 C19 C18 125.0(3) . . ?
O6 C19 C20 114.6(2) . . ?
C18 C19 C20 120.5(2) . . ?
C19 C18 C17 120.0(3) . . ?
C19 C18 H18 120.0 . . ?
C17 C18 H18 120.0 . . ?
C16 C17 C18 120.1(3) . . ?
C16 C17 H17 119.9 . . ?
C18 C17 H17 119.9 . . ?
C17 C16 C15 120.8(3) . . ?
C17 C16 H16 119.6 . . ?
C15 C16 H16 119.6 . . ?
C16 C15 C20 119.1(2) . . ?
C16 C15 C14 118.9(2) . . ?
C20 C15 C14 122.0(2) . . ?
N6 C14 C15 120.4(2) . . ?
O4 C13 N5 124.1(2) . . ?
O4 C13 C12 120.7(2) . . ?
N5 C13 C12 115.2(2) . . ?
N1 C1 N2 112.3(2) . . ?
N1 C1 H1 123.9 . . ?
N2 C1 H1 123.9 . . ?
N2 C12 C2 104.7(2) . . ?
N2 C12 C13 117.5(2) . . ?
C2 C12 C13 137.8(2) . . ?
N1 C2 C12 110.3(2) . . ?
N1 C2 C3 120.0(2) . . ?
C12 C2 C3 129.7(2) . . ?
O1 C3 N3 121.5(2) . . ?
O1 C3 C2 123.4(2) . . ?
N3 C3 C2 115.2(2) . . ?
N4 C4 C5 118.8(2) . . ?
C6 C5 C10 119.0(2) . . ?
C6 C5 C4 119.0(2) . . ?
C10 C5 C4 122.0(2) . . ?
C7 C6 C5 120.8(3) . . ?
C7 C6 H6 119.6 . . ?
C5 C6 H6 119.6 . . ?
C6 C7 C8 120.5(3) . . ?
C6 C7 H7 119.8 . . ?
C8 C7 H7 119.8 . . ?
C9 C8 C7 119.9(3) . . ?
C9 C8 H8 120.1 . . ?
C7 C8 H8 120.1 . . ?
O3 C9 C8 125.0(2) . . ?
O3 C9 C10 114.8(2) . . ?
C8 C9 C10 120.2(3) . . ?
O2 C10 C9 117.2(2) . . ?
O2 C10 C5 123.2(2) . . ?
C9 C10 C5 119.6(2) . . ?
O3 C11 H11A 109.5 . . ?
O3 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
O3 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
N7 C22 C23 179.4(3) . . ?
C22 C23 H23A 109.5 . . ?
C22 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
C22 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C14 N6 N5 115.6(2) . . ?
C13 N5 N6 119.1(2) . . ?
C13 N5 H5 120.4 . . ?
N6 N5 H5 120.4 . . ?
C1 N2 C12 108.0(2) . . ?
C1 N2 H2 126.0 . . ?
C12 N2 H2 126.0 . . ?
C1 N1 C2 104.7(2) . . ?
C3 N3 N4 116.9(2) . . ?
C3 N3 H3 121.5 . . ?
N4 N3 H3 121.5 . . ?
C4 N4 N3 118.6(2) . . ?
C19 O6 C21 117.1(2) . . ?
C20 O5 H5A 109.5 . . ?
C10 O2 H2A 109.5 . . ?
C9 O3 C11 117.6(2) . . ?

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
O5 C20 C19 O6 -1.6(3) . . . . ?
C15 C20 C19 O6 177.8(2) . . . . ?
O5 C20 C19 C18 178.8(2) . . . . ?
C15 C20 C19 C18 -1.8(4) . . . . ?
O6 C19 C18 C17 -179.1(3) . . . . ?
C20 C19 C18 C17 0.5(4) . . . . ?
C19 C18 C17 C16 1.2(5) . . . . ?
C18 C17 C16 C15 -1.5(5) . . . . ?
C17 C16 C15 C20 0.2(4) . . . . ?
C17 C16 C15 C14 179.3(3) . . . . ?
O5 C20 C15 C16 -179.1(2) . . . . ?
C19 C20 C15 C16 1.5(4) . . . . ?
O5 C20 C15 C14 1.7(4) . . . . ?
C19 C20 C15 C14 -177.6(2) . . . . ?
C16 C15 C14 N6 176.0(2) . . . . ?
C20 C15 C14 N6 -4.8(4) . . . . ?
O4 C13 C12 N2 -3.0(3) . . . . ?
N5 C13 C12 N2 177.3(2) . . . . ?
O4 C13 C12 C2 174.9(3) . . . . ?
N5 C13 C12 C2 -4.9(4) . . . . ?
N2 C12 C2 N1 0.9(3) . . . . ?
C13 C12 C2 N1 -177.2(3) . . . . ?
N2 C12 C2 C3 -178.1(2) . . . . ?
C13 C12 C2 C3 3.8(5) . . . . ?
N1 C2 C3 O1 -177.3(2) . . . . ?
C12 C2 C3 O1 1.6(4) . . . . ?
N1 C2 C3 N3 2.5(3) . . . . ?
C12 C2 C3 N3 -178.6(2) . . . . ?
N4 C4 C5 C6 174.2(2) . . . . ?
N4 C4 C5 C10 -5.4(4) . . . . ?
C10 C5 C6 C7 1.5(4) . . . . ?
C4 C5 C6 C7 -178.1(3) . . . . ?
C5 C6 C7 C8 -1.1(4) . . . . ?
C6 C7 C8 C9 0.0(4) . . . . ?
C7 C8 C9 O3 -178.9(3) . . . . ?
C7 C8 C9 C10 0.6(4) . . . . ?
O3 C9 C10 O2 -0.2(4) . . . . ?
C8 C9 C10 O2 -179.8(2) . . . . ?
O3 C9 C10 C5 179.3(2) . . . . ?
C8 C9 C10 C5 -0.3(4) . . . . ?
C6 C5 C10 O2 178.7(2) . . . . ?
C4 C5 C10 O2 -1.7(4) . . . . ?
C6 C5 C10 C9 -0.8(4) . . . . ?
C4 C5 C10 C9 178.8(2) . . . . ?
C15 C14 N6 N5 -179.9(2) . . . . ?
O4 C13 N5 N6 2.3(4) . . . . ?
C12 C13 N5 N6 -177.9(2) . . . . ?
C14 N6 N5 C13 168.8(2) . . . . ?
N1 C1 N2 C12 -0.3(3) . . . . ?
C2 C12 N2 C1 -0.4(3) . . . . ?
C13 C12 N2 C1 178.2(2) . . . . ?
N2 C1 N1 C2 0.8(3) . . . . ?
C12 C2 N1 C1 -1.0(3) . . . . ?
C3 C2 N1 C1 178.1(2) . . . . ?
O1 C3 N3 N4 -1.8(3) . . . . ?
C2 C3 N3 N4 178.4(2) . . . . ?
C5 C4 N4 N3 179.4(2) . . . . ?
C3 N3 N4 C4 -179.6(2) . . . . ?
C18 C19 O6 C21 1.4(4) . . . . ?
C20 C19 O6 C21 -178.2(2) . . . . ?
C8 C9 O3 C11 -2.6(4) . . . . ?
C10 C9 O3 C11 177.9(3) . . . . ?

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
O2 H2A N4 0.84 1.88 2.611(3) 144.2 . yes
O5 H5A N6 0.84 1.88 2.618(3) 145.0 . yes
N3 H3 N7 0.88 2.27 3.104(4) 157.9 2_545 yes
N2 H2 O4 0.88 1.94 2.774(3) 157.6 3_656 yes
N5 H5 O1 0.88 1.82 2.670(3) 161.4 . yes
C23 H23B O3 0.98 2.45 3.315(4) 147.4 1_655 yes
C23 H23B O2 0.98 2.52 3.195(4) 126.4 1_655 yes
C11 H11A O6 0.98 2.59 3.425(4) 142.8 4_365 yes
N2 H2 O4 0.88 2.53 2.742(3) 94.6 . yes
C11 H11A O6 0.98 2.59 3.425(4) 142.8 4_365 yes
C23 H23B O2 0.98 2.52 3.195(4) 126.4 1_655 yes
C23 H23B O3 0.98 2.45 3.315(4) 147.4 1_655 yes
N5 H5 O1 0.88 1.82 2.670(3) 161.4 . yes
N2 H2 O4 0.88 1.94 2.774(3) 157.6 3_656 yes
N3 H3 N7 0.88 2.27 3.104(4) 157.9 2_545 yes
O5 H5A N6 0.84 1.88 2.618(3) 145.0 . yes
O2 H2A N4 0.84 1.88 2.611(3) 144.2 . yes

_refine_diff_density_max         0.752
_refine_diff_density_min         -0.287
_refine_diff_density_rms         0.062

####################################################################### 
# 
# 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_Compound-3
_database_code_depnum_ccdc_archive 'CCDC 1902977'
_audit_update_record             
;
2019-03-13 deposited with the CCDC.	2019-10-31 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C63 H99 Dy12 N27 O78, C6 H15 N [+ solvent]'
_chemical_formula_sum            'C69 H114 Dy12 N28 O78 [+ solvent]'
_chemical_formula_weight         4533.88

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      trigonal
_space_group_IT_number           167
_space_group_name_H-M_alt        'R -3 c :H'
_space_group_name_Hall           '-R 3 2"c'

_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'
'-y, x-y, z'
'-x+y, -x, z'
'y, x, -z+1/2'
'x-y, -y, -z+1/2'
'-x, -x+y, -z+1/2'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'y+2/3, x+1/3, -z+5/6'
'x-y+2/3, -y+1/3, -z+5/6'
'-x+2/3, -x+y+1/3, -z+5/6'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'y+1/3, x+2/3, -z+7/6'
'x-y+1/3, -y+2/3, -z+7/6'
'-x+1/3, -x+y+2/3, -z+7/6'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-y, -x, z-1/2'
'-x+y, y, z-1/2'
'x, x-y, z-1/2'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-y+2/3, -x+1/3, z-1/6'
'-x+y+2/3, y+1/3, z-1/6'
'x+2/3, x-y+1/3, z-1/6'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'
'-y+1/3, -x+2/3, z+1/6'
'-x+y+1/3, y+2/3, z+1/6'
'x+1/3, x-y+2/3, z+1/6'

_cell_length_a                   30.9262(8)
_cell_length_b                   30.9262(8)
_cell_length_c                   60.130(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     49805(4)
_cell_formula_units_Z            12
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    3793
_cell_measurement_theta_min      2.01
_cell_measurement_theta_max      25.12

_exptl_crystal_description       block
_exptl_crystal_colour            orange-yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.814
_exptl_crystal_F_000             25680
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.220
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.180
_exptl_absorpt_coefficient_mu    5.415
_shelx_estimated_absorpt_T_min   0.382
_shelx_estimated_absorpt_T_max   0.442
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.39
_exptl_absorpt_correction_T_max  0.44
_exptl_absorpt_process_details   'SADABS; Bruker, 2008'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            120473
_diffrn_reflns_av_unetI/netI     0.0495
_diffrn_reflns_av_R_equivalents  0.0541
_diffrn_reflns_limit_h_min       -37
_diffrn_reflns_limit_h_max       37
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_k_max       34
_diffrn_reflns_limit_l_min       -72
_diffrn_reflns_limit_l_max       72
_diffrn_reflns_theta_min         2.281
_diffrn_reflns_theta_max         25.401
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             10171
_reflns_number_gt                6995
_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.
 
 Structure factors included contributions from the .fab file.
 
 _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       'SMART (Bruker, 2008)'
_computing_cell_refinement       SMART
_computing_data_reduction        'SAINT (Bruker, 2008)'
_computing_structure_solution    'SHELXTL (Bruker, 2008)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    'SHELXTL (Bruker, 2008)'
_computing_publication_material  'SHELXTL (Bruker, 2008)'
_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)+(0.04P)²+1.22P] 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         10171
_refine_ls_number_parameters     565
_refine_ls_number_restraints     3
_refine_ls_R_factor_all          0.0644
_refine_ls_R_factor_gt           0.0370
_refine_ls_wR_factor_ref         0.0797
_refine_ls_wR_factor_gt          0.0753
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_restrained_S_all      1.026
_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
C1 C 0.3575(2) 0.7397(2) 0.08636(10) 0.0401(15) Uani 1 1 d . . . . .
H1 H 0.351581 0.719820 0.099292 0.048 Uiso 1 1 calc R U . . .
C2 C 0.3946(2) 0.7898(2) 0.05961(10) 0.0409(16) Uani 1 1 d . . . . .
C3 C 0.4393(3) 0.8208(2) 0.04627(11) 0.0469(17) Uani 1 1 d . . . . .
C4 C 0.4769(2) 0.9043(2) 0.00247(11) 0.0520(18) Uani 1 1 d . . . . .
H4 H 0.444752 0.899597 -0.000624 0.062 Uiso 1 1 calc R U . . .
C5 C 0.5203(2) 0.9415(2) -0.01165(11) 0.0529(18) Uani 1 1 d . U . . .
C6 C 0.5121(3) 0.9768(2) -0.02359(11) 0.0580(19) Uani 1 1 d . U . . .
H6 H 0.480144 0.974243 -0.023337 0.070 Uiso 1 1 calc R U . . .
C7 C 0.5500(3) 1.0140(2) -0.03528(12) 0.060(2) Uani 1 1 d . . . . .
H7 H 0.544347 1.036592 -0.043783 0.072 Uiso 1 1 calc R U . . .
C8 C 0.5966(3) 1.0188(2) -0.03476(11) 0.0538(18) Uani 1 1 d . . . . .
H8 H 0.623454 1.045680 -0.042416 0.065 Uiso 1 1 calc R U . . .
C9 C 0.6051(3) 0.9842(2) -0.02299(11) 0.0532(18) Uani 1 1 d . . . . .
C10 C 0.5672(3) 0.9443(3) -0.01157(11) 0.0522(18) Uani 1 1 d . . . . .
C11 C 0.6949(3) 1.0278(3) -0.03168(15) 0.086(3) Uani 1 1 d . U . . .
H11A H 0.692784 1.025035 -0.047925 0.129 Uiso 1 1 calc R U . . .
H11B H 0.724662 1.027230 -0.026553 0.129 Uiso 1 1 calc R U . . .
H11C H 0.696948 1.059203 -0.027128 0.129 Uiso 1 1 calc R U . . .
C12 C 0.4332(2) 0.6544(2) 0.05969(10) 0.0422(16) Uani 1 1 d . . . . .
C13 C 0.4778(2) 0.6832(3) 0.04584(11) 0.0442(16) Uani 1 1 d . . . . .
C14 C 0.5417(2) 0.6714(3) 0.00282(12) 0.0549(19) Uani 1 1 d . . . . .
H14 H 0.525426 0.635951 0.003120 0.066 Uiso 1 1 calc R U . . .
C15 C 0.5760(2) 0.6966(3) -0.01470(11) 0.0511(18) Uani 1 1 d . . . . .
C16 C 0.5863(3) 0.6671(3) -0.02866(12) 0.068(2) Uani 1 1 d . . . . .
H16 H 0.574996 0.633270 -0.024969 0.081 Uiso 1 1 calc R U . . .
C17 C 0.6144(3) 0.6885(3) -0.04895(12) 0.072(2) Uani 1 1 d . . . . .
H17 H 0.619644 0.668265 -0.059250 0.086 Uiso 1 1 calc R U . . .
C18 C 0.6336(3) 0.7390(3) -0.05304(13) 0.070(2) Uani 1 1 d . . . . .
H18 H 0.654725 0.754616 -0.065453 0.084 Uiso 1 1 calc R U . . .
C19 C 0.6212(3) 0.7661(3) -0.03866(12) 0.0555(19) Uani 1 1 d . . . . .
C20 C 0.5954(2) 0.7474(2) -0.01884(11) 0.0485(17) Uani 1 1 d . . . . .
C21 C 0.6684(3) 0.8413(2) -0.06071(12) 0.070(2) Uani 1 1 d . . . . .
H21A H 0.680945 0.877215 -0.059553 0.105 Uiso 1 1 calc R U . . .
H21B H 0.649799 0.828643 -0.074648 0.105 Uiso 1 1 calc R U . . .
H21C H 0.696502 0.835067 -0.060513 0.105 Uiso 1 1 calc R U . . .
C22 C 0.3294(4) 0.6178(4) 0.0316(2) 0.156(5) Uani 1 1 d . U . . .
H22A H 0.304830 0.593943 0.042356 0.187 Uiso 1 1 calc R U . . .
H22B H 0.362063 0.621682 0.035974 0.187 Uiso 1 1 calc R U . . .
C23 C 0.3161(5) 0.5889(4) 0.00869(16) 0.135(5) Uani 1 1 d . U . . .
H23A H 0.285252 0.586059 0.002789 0.203 Uiso 1 1 calc R U . . .
H23B H 0.311442 0.555457 0.010984 0.203 Uiso 1 1 calc R U . . .
H23C H 0.343365 0.607270 -0.001906 0.203 Uiso 1 1 calc R U . . .
Dy1 Dy 0.55799(2) 0.88118(2) 0.03476(2) 0.04494(10) Uani 1 1 d . . . . .
Dy2 Dy 0.48543(2) 0.77148(2) 0.08018(2) 0.04345(10) Uani 1 1 d . . . . .
Dy3 Dy 0.58059(2) 0.78140(2) 0.03275(2) 0.04651(10) Uani 1 1 d . . . . .
Dy4 Dy 0.58449(2) 0.84560(2) -0.01678(2) 0.04843(10) Uani 1 1 d . . . . .
N1 N 0.40078(19) 0.76327(18) 0.07679(8) 0.0414(13) Uani 1 1 d . . . . .
N2 N 0.42386(18) 0.67853(19) 0.07664(8) 0.0426(13) Uani 1 1 d . . . . .
N3 N 0.43666(19) 0.84934(18) 0.02996(8) 0.0471(14) Uani 1 1 d . . . . .
H3A H 0.426773 0.870168 0.036213 0.057 Uiso 1 1 d R U . . .
N4 N 0.48085(19) 0.87889(19) 0.01818(9) 0.0473(14) Uani 1 1 d . . . . .
N5 N 0.4891(2) 0.65990(19) 0.03130(9) 0.0479(14) Uani 1 1 d . . . . .
H5A H 0.462171 0.641874 0.022090 0.057 Uiso 1 1 d R U . . .
N6 N 0.53142(19) 0.69328(19) 0.01821(9) 0.0472(14) Uani 1 1 d . . . . .
N7 N 0.5552(2) 0.9650(2) 0.05429(9) 0.0516(15) Uani 1 1 d . . . . .
N8 N 0.5511(3) 0.7537(3) 0.10939(11) 0.0696(18) Uani 1 1 d . . . . .
N9 N 0.4910(2) 0.7894(2) -0.04022(10) 0.0594(17) Uani 1 1 d . . . . .
N10 N 0.333333 0.666667 0.03682(16) 0.047(2) Uani 1 3 d S T P . .
O1 O 0.47831(15) 0.81996(15) 0.05050(6) 0.0430(11) Uani 1 1 d . . . . .
O2 O 0.57591(15) 0.91093(15) -0.00158(7) 0.0478(11) Uani 1 1 d . . . . .
O3 O 0.65117(18) 0.98658(16) -0.02204(8) 0.0632(14) Uani 1 1 d . U . . .
O4 O 0.50163(15) 0.73114(15) 0.04946(7) 0.0434(11) Uani 1 1 d . . . . .
O5 O 0.58840(15) 0.77679(14) -0.00534(7) 0.0457(11) Uani 1 1 d . . . . .
O6 O 0.63496(17) 0.81536(17) -0.04172(8) 0.0623(13) Uani 1 1 d . . . . .
O7 O 0.61779(15) 0.86254(15) 0.02005(7) 0.0488(11) Uani 1 1 d . . . . .
O8 O 0.53056(14) 0.80834(14) 0.01403(7) 0.0424(10) Uani 1 1 d . . . . .
O9 O 0.56085(14) 0.82470(14) 0.06095(6) 0.0424(10) Uani 1 1 d . . . . .
O10 O 0.53272(16) 0.92174(17) 0.06364(7) 0.0543(12) Uani 1 1 d . . . . .
O11 O 0.55472(18) 1.00091(17) 0.06275(8) 0.0620(13) Uani 1 1 d . . . . .
O12 O 0.57362(17) 0.96865(15) 0.03591(8) 0.0553(12) Uani 1 1 d . . . . .
O13 O 0.51975(18) 0.72260(18) 0.09663(8) 0.0606(13) Uani 1 1 d . . . . .
O14 O 0.5741(2) 0.7417(2) 0.12295(11) 0.102(2) Uani 1 1 d . . . . .
O15 O 0.55689(18) 0.79721(19) 0.10787(8) 0.0657(14) Uani 1 1 d . . . . .
O16 O 0.49979(17) 0.82738(18) -0.02897(8) 0.0600(13) Uani 1 1 d . . . . .
O17 O 0.4528(2) 0.76596(19) -0.05046(9) 0.0757(16) Uani 1 1 d . . . . .
O18 O 0.5235(2) 0.77704(17) -0.04070(8) 0.0654(14) Uani 1 1 d . . . . .
O1W O 0.63368(18) 0.93204(17) 0.05825(9) 0.0814(17) Uani 1 1 d . . . . .
H1X H 0.652925 0.925583 0.050655 0.098 Uiso 1 1 d R U . . .
H1Y H 0.634887 0.959933 0.056609 0.098 Uiso 1 1 d R U . . .
O2W O 0.50192(16) 0.84856(15) 0.09715(7) 0.0541(12) Uani 1 1 d . . . . .
H2X H 0.530589 0.862440 0.103196 0.065 Uiso 1 1 d R U . . .
H2Y H 0.501139 0.867800 0.087256 0.065 Uiso 1 1 d R U . . .
O3W O 0.44930(16) 0.74059(19) 0.11631(7) 0.0744(15) Uani 1 1 d . . . . .
H3X H 0.454951 0.716398 0.115758 0.089 Uiso 1 1 d R U . . .
H3Y H 0.470975 0.763258 0.124672 0.089 Uiso 1 1 d R U . . .
O4W O 0.6376(3) 0.8262(3) 0.06576(10) 0.155(3) Uani 1 1 d . . . . .
H4X H 0.663178 0.823733 0.063198 0.186 Uiso 1 1 d R U . . .
H4Y H 0.616422 0.808536 0.075654 0.186 Uiso 1 1 d R U . . .
O5W O 0.59156(18) 0.72713(18) 0.06086(8) 0.0718(15) Uani 1 1 d . . . . .
H5X H 0.572735 0.729179 0.070607 0.086 Uiso 1 1 d R U . . .
H5Y H 0.621710 0.743703 0.065203 0.086 Uiso 1 1 d R U . . .
O6W O 0.66439(16) 0.79852(18) 0.02515(8) 0.0691(14) Uani 1 1 d . . . . .
H6X H 0.674802 0.827686 0.020007 0.083 Uiso 1 1 d R U . . .
H6Y H 0.658027 0.778550 0.014319 0.083 Uiso 1 1 d R U . . .
O7W O 0.67042(15) 0.91035(16) -0.02050(7) 0.0626(13) Uani 1 1 d . . . . .
H7X H 0.688687 0.897097 -0.021434 0.075 Uiso 1 1 d R U . . .
H7Y H 0.673811 0.927229 -0.032194 0.075 Uiso 1 1 d R U . . .
O8W O 0.59234(18) 0.88651(16) -0.05209(7) 0.0678(14) Uani 1 1 d . . . . .
H8X H 0.580880 0.859773 -0.059641 0.081 Uiso 1 1 d R U . . .
H8Y H 0.570844 0.895318 -0.049496 0.081 Uiso 1 1 d 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
C1 N1 1.297(7) . ?
C1 N2 1.344(7) 2_665 ?
C1 H1 0.9500 . ?
C2 C12 1.376(8) 2_665 ?
C2 N1 1.390(7) . ?
C2 C3 1.466(8) . ?
C3 O1 1.247(7) . ?
C3 N3 1.348(8) . ?
C4 N4 1.272(8) . ?
C4 C5 1.517(8) . ?
C4 H4 0.9500 . ?
C5 C10 1.410(9) . ?
C5 C6 1.432(9) . ?
C6 C7 1.358(9) . ?
C6 H6 0.9500 . ?
C7 C8 1.373(9) . ?
C7 H7 0.9500 . ?
C8 C9 1.412(9) . ?
C8 H8 0.9500 . ?
C9 O3 1.391(8) . ?
C9 C10 1.385(9) . ?
C10 O2 1.333(8) . ?
C11 O3 1.437(8) . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C12 N2 1.376(8) . ?
C12 C13 1.470(9) . ?
C13 N5 1.288(8) . ?
C13 O4 1.301(7) . ?
C14 N6 1.278(8) . ?
C14 C15 1.419(9) . ?
C14 H14 0.9500 . ?
C15 C16 1.389(9) . ?
C15 C20 1.396(9) . ?
C16 C17 1.452(9) . ?
C16 H16 0.9500 . ?
C17 C18 1.386(9) . ?
C17 H17 0.9500 . ?
C18 C19 1.385(9) . ?
C18 H18 0.9500 . ?
C19 O6 1.375(7) . ?
C19 C20 1.389(9) . ?
C20 O5 1.314(7) . ?
C21 O6 1.478(7) . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C22 N10 1.488(11) . ?
C22 C23 1.581(14) . ?
C22 H22A 0.9900 . ?
C22 H22B 0.9900 . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 H23C 0.9800 . ?
Dy1 O2 2.328(4) . ?
Dy1 O8 2.332(4) . ?
Dy1 O7 2.366(4) . ?
Dy1 O9 2.386(4) . ?
Dy1 O1 2.426(4) . ?
Dy1 O10 2.486(4) . ?
Dy1 O1W 2.503(5) . ?
Dy1 O12 2.500(4) . ?
Dy1 N4 2.554(5) . ?
Dy1 N7 2.888(6) . ?
Dy1 Dy3 3.4902(5) . ?
Dy1 Dy4 3.5194(5) . ?
Dy2 O9 2.377(4) . ?
Dy2 O2W 2.402(4) . ?
Dy2 O1 2.411(4) . ?
Dy2 O4 2.417(4) . ?
Dy2 O3W 2.411(4) . ?
Dy2 O13 2.448(5) . ?
Dy2 N1 2.509(5) . ?
Dy2 N2 2.542(5) . ?
Dy2 O15 2.556(4) . ?
Dy2 N8 2.937(7) . ?
Dy2 Dy3 3.9986(5) . ?
Dy3 O7 2.306(4) . ?
Dy3 O5 2.315(4) . ?
Dy3 O4 2.365(4) . ?
Dy3 O8 2.376(4) . ?
Dy3 O6W 2.415(4) . ?
Dy3 O9 2.421(4) . ?
Dy3 N6 2.522(5) . ?
Dy3 O5W 2.522(4) . ?
Dy3 O4W 2.555(6) . ?
Dy3 Dy4 3.5476(5) . ?
Dy4 O5 2.297(4) . ?
Dy4 O2 2.350(4) . ?
Dy4 O8 2.370(4) . ?
Dy4 O7 2.387(4) . ?
Dy4 O7W 2.408(4) . ?
Dy4 O8W 2.421(4) . ?
Dy4 O18 2.475(4) . ?
Dy4 O16 2.498(5) . ?
Dy4 O6 2.649(4) . ?
Dy4 N9 2.888(6) . ?
N3 N4 1.399(7) . ?
N3 H3A 0.9202 . ?
N5 N6 1.431(7) . ?
N5 H5A 0.9198 . ?
N7 O12 1.223(6) . ?
N7 O11 1.226(6) . ?
N7 O10 1.289(6) . ?
N8 O13 1.233(7) . ?
N8 O15 1.270(7) . ?
N8 O14 1.254(7) . ?
N9 O17 1.201(7) . ?
N9 O18 1.240(7) . ?
N9 O16 1.262(7) . ?
O1W H1X 0.8496 . ?
O1W H1Y 0.8503 . ?
O2W H2X 0.8498 . ?
O2W H2Y 0.8501 . ?
O3W H3X 0.8500 . ?
O3W H3Y 0.8508 . ?
O4W H4X 0.8447 . ?
O4W H4Y 0.8506 . ?
O5W H5X 0.8505 . ?
O5W H5Y 0.8499 . ?
O6W H6X 0.8498 . ?
O6W H6Y 0.8501 . ?
O7W H7X 0.8497 . ?
O7W H7Y 0.8502 . ?
O8W H8X 0.8499 . ?
O8W H8Y 0.8495 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 C1 N2 115.1(6) . 2_665 ?
N1 C1 H1 122.5 . . ?
N2 C1 H1 122.5 2_665 . ?
C12 C2 N1 108.2(5) 2_665 . ?
C12 C2 C3 136.4(7) 2_665 . ?
N1 C2 C3 115.5(6) . . ?
O1 C3 N3 122.5(6) . . ?
O1 C3 C2 118.7(6) . . ?
N3 C3 C2 118.8(6) . . ?
N4 C4 C5 124.3(6) . . ?
N4 C4 H4 117.9 . . ?
C5 C4 H4 117.9 . . ?
C10 C5 C6 121.6(6) . . ?
C10 C5 C4 122.5(7) . . ?
C6 C5 C4 115.6(6) . . ?
C7 C6 C5 119.8(7) . . ?
C7 C6 H6 120.1 . . ?
C5 C6 H6 120.1 . . ?
C6 C7 C8 119.7(7) . . ?
C6 C7 H7 120.2 . . ?
C8 C7 H7 120.2 . . ?
C7 C8 C9 120.8(6) . . ?
C7 C8 H8 119.6 . . ?
C9 C8 H8 119.6 . . ?
O3 C9 C10 114.5(6) . . ?
O3 C9 C8 123.6(6) . . ?
C10 C9 C8 121.9(7) . . ?
O2 C10 C9 120.4(6) . . ?
O2 C10 C5 123.6(6) . . ?
C9 C10 C5 116.1(7) . . ?
O3 C11 H11A 109.5 . . ?
O3 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
O3 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
C2 C12 N2 107.7(6) 3_565 . ?
C2 C12 C13 133.8(6) 3_565 . ?
N2 C12 C13 118.6(6) . . ?
N5 C13 O4 126.4(6) . . ?
N5 C13 C12 118.7(6) . . ?
O4 C13 C12 115.0(6) . . ?
N6 C14 C15 124.1(7) . . ?
N6 C14 H14 117.9 . . ?
C15 C14 H14 117.9 . . ?
C16 C15 C20 121.4(6) . . ?
C16 C15 C14 116.1(7) . . ?
C20 C15 C14 122.3(6) . . ?
C15 C16 C17 119.4(7) . . ?
C15 C16 H16 120.3 . . ?
C17 C16 H16 120.3 . . ?
C18 C17 C16 118.9(7) . . ?
C18 C17 H17 120.6 . . ?
C16 C17 H17 120.6 . . ?
C17 C18 C19 118.6(7) . . ?
C17 C18 H18 120.7 . . ?
C19 C18 H18 120.7 . . ?
O6 C19 C20 111.7(6) . . ?
O6 C19 C18 124.2(6) . . ?
C20 C19 C18 124.0(7) . . ?
O5 C20 C19 120.2(6) . . ?
O5 C20 C15 122.7(6) . . ?
C19 C20 C15 117.1(6) . . ?
O6 C21 H21A 109.5 . . ?
O6 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
O6 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
N10 C22 C23 128.6(11) . . ?
N10 C22 H22A 105.1 . . ?
C23 C22 H22A 105.1 . . ?
N10 C22 H22B 105.1 . . ?
C23 C22 H22B 105.1 . . ?
H22A C22 H22B 105.9 . . ?
C22 C23 H23A 109.5 . . ?
C22 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
C22 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
O2 Dy1 O8 77.27(14) . . ?
O2 Dy1 O7 71.63(14) . . ?
O8 Dy1 O7 61.06(14) . . ?
O2 Dy1 O9 145.11(14) . . ?
O8 Dy1 O9 76.97(13) . . ?
O7 Dy1 O9 75.45(13) . . ?
O2 Dy1 O1 128.52(14) . . ?
O8 Dy1 O1 73.60(14) . . ?
O7 Dy1 O1 124.62(14) . . ?
O9 Dy1 O1 64.30(13) . . ?
O2 Dy1 O10 121.94(15) . . ?
O8 Dy1 O10 143.77(14) . . ?
O7 Dy1 O10 149.89(15) . . ?
O9 Dy1 O10 92.55(14) . . ?
O1 Dy1 O10 70.64(14) . . ?
O2 Dy1 O1W 108.56(16) . . ?
O8 Dy1 O1W 133.08(15) . . ?
O7 Dy1 O1W 76.40(15) . . ?
O9 Dy1 O1W 73.87(15) . . ?
O1 Dy1 O1W 122.41(16) . . ?
O10 Dy1 O1W 73.73(15) . . ?
O2 Dy1 O12 73.69(15) . . ?
O8 Dy1 O12 147.17(15) . . ?
O7 Dy1 O12 121.48(14) . . ?
O9 Dy1 O12 135.73(14) . . ?
O1 Dy1 O12 113.89(14) . . ?
O10 Dy1 O12 51.25(14) . . ?
O1W Dy1 O12 71.96(15) . . ?
O2 Dy1 N4 71.28(16) . . ?
O8 Dy1 N4 83.16(15) . . ?
O7 Dy1 N4 132.87(16) . . ?
O9 Dy1 N4 127.84(15) . . ?
O1 Dy1 N4 63.92(15) . . ?
O10 Dy1 N4 76.21(16) . . ?
O1W Dy1 N4 143.59(16) . . ?
O12 Dy1 N4 73.34(16) . . ?
O2 Dy1 N7 97.75(16) . . ?
O8 Dy1 N7 157.70(14) . . ?
O7 Dy1 N7 138.51(15) . . ?
O9 Dy1 N7 114.70(15) . . ?
O1 Dy1 N7 93.84(15) . . ?
O10 Dy1 N7 26.41(14) . . ?
O1W Dy1 N7 69.20(15) . . ?
O12 Dy1 N7 24.94(14) . . ?
N4 Dy1 N7 74.71(16) . . ?
O2 Dy1 Dy3 101.74(10) . . ?
O8 Dy1 Dy3 42.63(10) . . ?
O7 Dy1 Dy3 41.01(10) . . ?
O9 Dy1 Dy3 43.83(9) . . ?
O1 Dy1 Dy3 84.14(10) . . ?
O10 Dy1 Dy3 136.29(11) . . ?
O1W Dy1 Dy3 92.15(11) . . ?
O12 Dy1 Dy3 160.37(11) . . ?
N4 Dy1 Dy3 124.00(11) . . ?
N7 Dy1 Dy3 156.56(11) . . ?
O2 Dy1 Dy4 41.44(10) . . ?
O8 Dy1 Dy4 41.96(10) . . ?
O7 Dy1 Dy4 42.47(10) . . ?
O9 Dy1 Dy4 104.64(9) . . ?
O1 Dy1 Dy4 113.82(10) . . ?
O10 Dy1 Dy4 162.52(11) . . ?
O1W Dy1 Dy4 113.74(12) . . ?
O12 Dy1 Dy4 114.42(10) . . ?
N4 Dy1 Dy4 90.45(12) . . ?
N7 Dy1 Dy4 139.04(12) . . ?
Dy3 Dy1 Dy4 60.807(9) . . ?
O9 Dy2 O2W 82.61(13) . . ?
O9 Dy2 O1 64.67(13) . . ?
O2W Dy2 O1 74.77(14) . . ?
O9 Dy2 O4 66.47(13) . . ?
O2W Dy2 O4 147.22(13) . . ?
O1 Dy2 O4 82.08(14) . . ?
O9 Dy2 O3W 144.37(15) . . ?
O2W Dy2 O3W 80.61(16) . . ?
O1 Dy2 O3W 138.17(16) . . ?
O4 Dy2 O3W 131.19(16) . . ?
O9 Dy2 O13 92.62(15) . . ?
O2W Dy2 O13 119.93(16) . . ?
O1 Dy2 O13 152.32(15) . . ?
O4 Dy2 O13 73.99(15) . . ?
O3W Dy2 O13 69.49(16) . . ?
O9 Dy2 N1 130.06(15) . . ?
O2W Dy2 N1 80.09(15) . . ?
O1 Dy2 N1 65.65(15) . . ?
O4 Dy2 N1 111.15(14) . . ?
O3W Dy2 N1 77.27(16) . . ?
O13 Dy2 N1 136.30(16) . . ?
O9 Dy2 N2 131.56(15) . . ?
O2W Dy2 N2 145.63(15) . . ?
O1 Dy2 N2 113.05(14) . . ?
O4 Dy2 N2 65.40(15) . . ?
O3W Dy2 N2 71.98(17) . . ?
O13 Dy2 N2 69.29(15) . . ?
N1 Dy2 N2 74.04(15) . . ?
O9 Dy2 O15 72.83(14) . . ?
O2W Dy2 O15 72.11(16) . . ?
O1 Dy2 O15 128.48(15) . . ?
O4 Dy2 O15 106.76(16) . . ?
O3W Dy2 O15 72.17(15) . . ?
O13 Dy2 O15 49.82(15) . . ?
N1 Dy2 O15 141.31(16) . . ?
N2 Dy2 O15 116.68(16) . . ?
O9 Dy2 N8 83.66(16) . . ?
O2W Dy2 N8 96.23(18) . . ?
O1 Dy2 N8 147.76(16) . . ?
O4 Dy2 N8 91.09(17) . . ?
O3W Dy2 N8 67.29(17) . . ?
O13 Dy2 N8 24.37(15) . . ?
N1 Dy2 N8 144.47(17) . . ?
N2 Dy2 N8 92.02(18) . . ?
O15 Dy2 N8 25.53(15) . . ?
O9 Dy2 Dy3 33.89(9) . . ?
O2W Dy2 Dy3 116.35(10) . . ?
O1 Dy2 Dy3 73.54(10) . . ?
O4 Dy2 Dy3 32.86(9) . . ?
O3W Dy2 Dy3 148.29(12) . . ?
O13 Dy2 Dy3 78.80(11) . . ?
N1 Dy2 Dy3 129.83(11) . . ?
N2 Dy2 Dy3 97.67(12) . . ?
O15 Dy2 Dy3 87.26(12) . . ?
N8 Dy2 Dy3 83.66(13) . . ?
O7 Dy3 O5 74.27(14) . . ?
O7 Dy3 O4 130.19(14) . . ?
O5 Dy3 O4 119.03(14) . . ?
O7 Dy3 O8 61.28(14) . . ?
O5 Dy3 O8 70.07(14) . . ?
O4 Dy3 O8 78.02(14) . . ?
O7 Dy3 O6W 78.58(15) . . ?
O5 Dy3 O6W 72.11(15) . . ?
O4 Dy3 O6W 150.07(15) . . ?
O8 Dy3 O6W 130.47(15) . . ?
O7 Dy3 O9 75.90(14) . . ?
O5 Dy3 O9 142.20(14) . . ?
O4 Dy3 O9 66.59(13) . . ?
O8 Dy3 O9 75.49(13) . . ?
O6W Dy3 O9 123.43(15) . . ?
O7 Dy3 N6 139.87(16) . . ?
O5 Dy3 N6 67.40(15) . . ?
O4 Dy3 N6 64.57(16) . . ?
O8 Dy3 N6 93.91(15) . . ?
O6W Dy3 N6 99.94(17) . . ?
O9 Dy3 N6 131.15(15) . . ?
O7 Dy3 O5W 141.84(16) . . ?
O5 Dy3 O5W 124.71(15) . . ?
O4 Dy3 O5W 73.50(15) . . ?
O8 Dy3 O5W 151.51(14) . . ?
O6W Dy3 O5W 77.65(15) . . ?
O9 Dy3 O5W 93.07(15) . . ?
N6 Dy3 O5W 73.87(17) . . ?
O7 Dy3 O4W 80.4(2) . . ?
O5 Dy3 O4W 137.5(2) . . ?
O4 Dy3 O4W 103.4(2) . . ?
O8 Dy3 O4W 124.9(2) . . ?
O6W Dy3 O4W 69.7(2) . . ?
O9 Dy3 O4W 56.80(19) . . ?
N6 Dy3 O4W 137.3(2) . . ?
O5W Dy3 O4W 63.5(2) . . ?
O7 Dy3 Dy1 42.33(10) . . ?
O5 Dy3 Dy1 99.32(10) . . ?
O4 Dy3 Dy1 88.22(10) . . ?
O8 Dy3 Dy1 41.67(9) . . ?
O6W Dy3 Dy1 118.68(12) . . ?
O9 Dy3 Dy1 43.05(9) . . ?
N6 Dy3 Dy1 133.50(12) . . ?
O5W Dy3 Dy1 135.91(12) . . ?
O4W Dy3 Dy1 83.29(18) . . ?
O7 Dy3 Dy4 41.77(10) . . ?
O5 Dy3 Dy4 39.52(10) . . ?
O4 Dy3 Dy4 117.36(10) . . ?
O8 Dy3 Dy4 41.57(9) . . ?
O6W Dy3 Dy4 89.20(11) . . ?
O9 Dy3 Dy4 103.05(9) . . ?
N6 Dy3 Dy4 98.47(12) . . ?
O5W Dy3 Dy4 163.14(11) . . ?
O4W Dy3 Dy4 121.87(18) . . ?
Dy1 Dy3 Dy4 60.004(9) . . ?
O7 Dy3 Dy2 105.50(10) . . ?
O5 Dy3 Dy2 142.80(10) . . ?
O4 Dy3 Dy2 33.69(10) . . ?
O8 Dy3 Dy2 77.38(9) . . ?
O6W Dy3 Dy2 145.05(11) . . ?
O9 Dy3 Dy2 33.19(9) . . ?
N6 Dy3 Dy2 98.12(12) . . ?
O5W Dy3 Dy2 79.02(11) . . ?
O4W Dy3 Dy2 76.67(17) . . ?
Dy1 Dy3 Dy2 65.041(9) . . ?
Dy4 Dy3 Dy2 117.351(11) . . ?
O5 Dy4 O2 139.56(15) . . ?
O5 Dy4 O8 70.47(13) . . ?
O2 Dy4 O8 76.09(13) . . ?
O5 Dy4 O7 73.07(14) . . ?
O2 Dy4 O7 70.87(14) . . ?
O8 Dy4 O7 60.22(13) . . ?
O5 Dy4 O7W 104.53(15) . . ?
O2 Dy4 O7W 82.72(15) . . ?
O8 Dy4 O7W 133.83(14) . . ?
O7 Dy4 O7W 74.23(14) . . ?
O5 Dy4 O8W 135.14(15) . . ?
O2 Dy4 O8W 85.23(15) . . ?
O8 Dy4 O8W 143.31(15) . . ?
O7 Dy4 O8W 141.21(15) . . ?
O7W Dy4 O8W 72.74(16) . . ?
O5 Dy4 O18 75.57(16) . . ?
O2 Dy4 O18 126.67(17) . . ?
O8 Dy4 O18 89.31(15) . . ?
O7 Dy4 O18 141.96(15) . . ?
O7W Dy4 O18 135.22(16) . . ?
O8W Dy4 O18 76.83(16) . . ?
O5 Dy4 O16 114.45(15) . . ?
O2 Dy4 O16 75.63(15) . . ?
O8 Dy4 O16 73.51(14) . . ?
O7 Dy4 O16 127.62(14) . . ?
O7W Dy4 O16 139.19(16) . . ?
O8W Dy4 O16 71.36(16) . . ?
O18 Dy4 O16 51.09(16) . . ?
O5 Dy4 O6 61.91(14) . . ?
O2 Dy4 O6 149.68(14) . . ?
O8 Dy4 O6 131.77(14) . . ?
O7 Dy4 O6 109.68(15) . . ?
O7W Dy4 O6 68.96(15) . . ?
O8W Dy4 O6 76.42(15) . . ?
O18 Dy4 O6 72.53(17) . . ?
O16 Dy4 O6 119.37(15) . . ?
O5 Dy4 N9 95.09(17) . . ?
O2 Dy4 N9 101.43(18) . . ?
O8 Dy4 N9 80.76(15) . . ?
O7 Dy4 N9 140.98(15) . . ?
O7W Dy4 N9 144.23(16) . . ?
O8W Dy4 N9 72.26(16) . . ?
O18 Dy4 N9 25.26(15) . . ?
O16 Dy4 N9 25.83(16) . . ?
O6 Dy4 N9 95.75(17) . . ?
O5 Dy4 Dy1 98.88(10) . . ?
O2 Dy4 Dy1 40.96(10) . . ?
O8 Dy4 Dy1 41.13(9) . . ?
O7 Dy4 Dy1 42.01(10) . . ?
O7W Dy4 Dy1 98.89(11) . . ?
O8W Dy4 Dy1 125.96(11) . . ?
O18 Dy4 Dy1 125.64(13) . . ?
O16 Dy4 Dy1 86.98(11) . . ?
O6 Dy4 Dy1 151.53(11) . . ?
N9 Dy4 Dy1 107.37(13) . . ?
O5 Dy4 Dy3 39.89(10) . . ?
O2 Dy4 Dy3 99.66(10) . . ?
O8 Dy4 Dy3 41.69(9) . . ?
O7 Dy4 Dy3 40.04(10) . . ?
O7W Dy4 Dy3 104.95(11) . . ?
O8W Dy4 Dy3 174.36(11) . . ?
O18 Dy4 Dy3 102.14(11) . . ?
O16 Dy4 Dy3 112.44(11) . . ?
O6 Dy4 Dy3 97.97(11) . . ?
N9 Dy4 Dy3 109.21(12) . . ?
Dy1 Dy4 Dy3 59.189(9) . . ?
C1 N1 C2 104.7(5) . . ?
C1 N1 Dy2 138.9(4) . . ?
C2 N1 Dy2 116.5(4) . . ?
C1 N2 C12 104.3(5) 3_565 . ?
C1 N2 Dy2 140.0(4) 3_565 . ?
C12 N2 Dy2 115.7(4) . . ?
C3 N3 N4 115.9(5) . . ?
C3 N3 H3A 108.1 . . ?
N4 N3 H3A 107.9 . . ?
C4 N4 N3 114.6(5) . . ?
C4 N4 Dy1 130.4(4) . . ?
N3 N4 Dy1 114.5(4) . . ?
C13 N5 N6 112.1(5) . . ?
C13 N5 H5A 109.4 . . ?
N6 N5 H5A 109.3 . . ?
C14 N6 N5 113.4(5) . . ?
C14 N6 Dy3 130.4(5) . . ?
N5 N6 Dy3 115.4(4) . . ?
O12 N7 O11 120.5(6) . . ?
O12 N7 O10 118.2(5) . . ?
O11 N7 O10 121.0(6) . . ?
O12 N7 Dy1 59.5(3) . . ?
O11 N7 Dy1 178.9(5) . . ?
O10 N7 Dy1 59.1(3) . . ?
O13 N8 O15 114.9(6) . . ?
O13 N8 O14 121.1(7) . . ?
O15 N8 O14 124.0(7) . . ?
O13 N8 Dy2 55.0(4) . . ?
O15 N8 Dy2 60.2(4) . . ?
O14 N8 Dy2 172.7(6) . . ?
O17 N9 O18 120.4(7) . . ?
O17 N9 O16 121.7(7) . . ?
O18 N9 O16 117.9(6) . . ?
O17 N9 Dy4 178.2(5) . . ?
O18 N9 Dy4 58.4(3) . . ?
O16 N9 Dy4 59.5(3) . . ?
C22 N10 C22 115.7(5) 3_565 2_665 ?
C22 N10 C22 115.7(5) 3_565 . ?
C22 N10 C22 115.7(5) 2_665 . ?
C3 O1 Dy2 123.7(4) . . ?
C3 O1 Dy1 121.3(4) . . ?
Dy2 O1 Dy1 113.65(16) . . ?
C10 O2 Dy1 129.0(4) . . ?
C10 O2 Dy4 130.1(4) . . ?
Dy1 O2 Dy4 97.60(16) . . ?
C9 O3 C11 121.0(6) . . ?
C13 O4 Dy3 119.2(4) . . ?
C13 O4 Dy2 124.7(4) . . ?
Dy3 O4 Dy2 113.45(16) . . ?
C20 O5 Dy4 123.9(4) . . ?
C20 O5 Dy3 135.4(4) . . ?
Dy4 O5 Dy3 100.59(15) . . ?
C19 O6 C21 116.7(5) . . ?
C19 O6 Dy4 113.9(4) . . ?
C21 O6 Dy4 128.4(4) . . ?
Dy3 O7 Dy1 96.66(14) . . ?
Dy3 O7 Dy4 98.20(15) . . ?
Dy1 O7 Dy4 95.52(15) . . ?
Dy1 O8 Dy4 96.91(14) . . ?
Dy1 O8 Dy3 95.70(14) . . ?
Dy4 O8 Dy3 96.75(14) . . ?
Dy2 O9 Dy1 116.45(16) . . ?
Dy2 O9 Dy3 112.92(15) . . ?
Dy1 O9 Dy3 93.12(13) . . ?
N7 O10 Dy1 94.5(3) . . ?
N7 O12 Dy1 95.6(4) . . ?
N8 O13 Dy2 100.6(4) . . ?
N8 O15 Dy2 94.3(4) . . ?
N9 O16 Dy4 94.6(4) . . ?
N9 O18 Dy4 96.3(4) . . ?
Dy1 O1W H1X 95.4 . . ?
Dy1 O1W H1Y 97.2 . . ?
H1X O1W H1Y 119.7 . . ?
Dy2 O2W H2X 109.5 . . ?
Dy2 O2W H2Y 109.4 . . ?
H2X O2W H2Y 109.5 . . ?
Dy2 O3W H3X 93.2 . . ?
Dy2 O3W H3Y 100.8 . . ?
H3X O3W H3Y 108.9 . . ?
Dy3 O4W H4X 103.5 . . ?
Dy3 O4W H4Y 95.4 . . ?
H4X O4W H4Y 121.7 . . ?
Dy3 O5W H5X 95.0 . . ?
Dy3 O5W H5Y 106.0 . . ?
H5X O5W H5Y 109.2 . . ?
Dy3 O6W H6X 95.6 . . ?
Dy3 O6W H6Y 98.8 . . ?
H6X O6W H6Y 108.7 . . ?
Dy4 O7W H7X 109.2 . . ?
Dy4 O7W H7Y 109.5 . . ?
H7X O7W H7Y 109.5 . . ?
Dy4 O8W H8X 94.4 . . ?
Dy4 O8W H8Y 96.7 . . ?
H8X O8W H8Y 113.4 . . ?

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
C12 C2 C3 O1 -176.6(6) 2_665 . . . ?
N1 C2 C3 O1 2.8(8) . . . . ?
C12 C2 C3 N3 3.7(11) 2_665 . . . ?
N1 C2 C3 N3 -177.0(5) . . . . ?
N4 C4 C5 C10 12.8(10) . . . . ?
N4 C4 C5 C6 -161.7(7) . . . . ?
C10 C5 C6 C7 0.3(11) . . . . ?
C4 C5 C6 C7 174.9(6) . . . . ?
C5 C6 C7 C8 -2.9(11) . . . . ?
C6 C7 C8 C9 2.8(11) . . . . ?
C7 C8 C9 O3 179.2(6) . . . . ?
C7 C8 C9 C10 0.0(11) . . . . ?
O3 C9 C10 O2 -2.7(9) . . . . ?
C8 C9 C10 O2 176.5(6) . . . . ?
O3 C9 C10 C5 178.3(6) . . . . ?
C8 C9 C10 C5 -2.4(10) . . . . ?
C6 C5 C10 O2 -176.6(6) . . . . ?
C4 C5 C10 O2 9.2(10) . . . . ?
C6 C5 C10 C9 2.3(10) . . . . ?
C4 C5 C10 C9 -171.9(6) . . . . ?
C2 C12 C13 N5 -7.4(10) 3_565 . . . ?
N2 C12 C13 N5 173.7(5) . . . . ?
C2 C12 C13 O4 171.4(6) 3_565 . . . ?
N2 C12 C13 O4 -7.5(8) . . . . ?
N6 C14 C15 C16 173.8(7) . . . . ?
N6 C14 C15 C20 -11.1(11) . . . . ?
C20 C15 C16 C17 -5.0(12) . . . . ?
C14 C15 C16 C17 170.2(7) . . . . ?
C15 C16 C17 C18 4.8(12) . . . . ?
C16 C17 C18 C19 -5.9(12) . . . . ?
C17 C18 C19 O6 -175.5(7) . . . . ?
C17 C18 C19 C20 7.8(12) . . . . ?
O6 C19 C20 O5 -2.2(10) . . . . ?
C18 C19 C20 O5 174.9(7) . . . . ?
O6 C19 C20 C15 175.1(6) . . . . ?
C18 C19 C20 C15 -7.8(11) . . . . ?
C16 C15 C20 O5 -176.5(7) . . . . ?
C14 C15 C20 O5 8.6(11) . . . . ?
C16 C15 C20 C19 6.3(11) . . . . ?
C14 C15 C20 C19 -168.6(7) . . . . ?
N2 C1 N1 C2 3.4(7) 2_665 . . . ?
N2 C1 N1 Dy2 -174.7(4) 2_665 . . . ?
C12 C2 N1 C1 -1.6(6) 2_665 . . . ?
C3 C2 N1 C1 178.9(5) . . . . ?
C12 C2 N1 Dy2 177.0(3) 2_665 . . . ?
C3 C2 N1 Dy2 -2.5(6) . . . . ?
C2 C12 N2 C1 2.5(6) 3_565 . . 3_565 ?
C13 C12 N2 C1 -178.4(5) . . . 3_565 ?
C2 C12 N2 Dy2 -177.2(3) 3_565 . . . ?
C13 C12 N2 Dy2 2.0(7) . . . . ?
O1 C3 N3 N4 -1.1(9) . . . . ?
C2 C3 N3 N4 178.7(5) . . . . ?
C5 C4 N4 N3 175.9(6) . . . . ?
C5 C4 N4 Dy1 4.5(10) . . . . ?
C3 N3 N4 C4 178.0(6) . . . . ?
C3 N3 N4 Dy1 -9.2(6) . . . . ?
O4 C13 N5 N6 -2.3(9) . . . . ?
C12 C13 N5 N6 176.3(5) . . . . ?
C15 C14 N6 N5 168.5(6) . . . . ?
C15 C14 N6 Dy3 -22.5(10) . . . . ?
C13 N5 N6 C14 -176.2(6) . . . . ?
C13 N5 N6 Dy3 13.0(6) . . . . ?
C23 C22 N10 C22 55.6(15) . . . 3_565 ?
C23 C22 N10 C22 -84.3(12) . . . 2_665 ?
N3 C3 O1 Dy2 178.1(4) . . . . ?
C2 C3 O1 Dy2 -1.7(8) . . . . ?
N3 C3 O1 Dy1 12.1(8) . . . . ?
C2 C3 O1 Dy1 -167.7(4) . . . . ?
C9 C10 O2 Dy1 129.6(5) . . . . ?
C5 C10 O2 Dy1 -51.5(8) . . . . ?
C9 C10 O2 Dy4 -75.8(8) . . . . ?
C5 C10 O2 Dy4 103.1(7) . . . . ?
C10 C9 O3 C11 -175.4(6) . . . . ?
C8 C9 O3 C11 5.4(10) . . . . ?
N5 C13 O4 Dy3 -10.7(8) . . . . ?
C12 C13 O4 Dy3 170.6(4) . . . . ?
N5 C13 O4 Dy2 -171.2(5) . . . . ?
C12 C13 O4 Dy2 10.1(7) . . . . ?
C19 C20 O5 Dy4 27.4(9) . . . . ?
C15 C20 O5 Dy4 -149.7(5) . . . . ?
C19 C20 O5 Dy3 -149.2(5) . . . . ?
C15 C20 O5 Dy3 33.7(10) . . . . ?
C20 C19 O6 C21 172.1(6) . . . . ?
C18 C19 O6 C21 -5.0(10) . . . . ?
C20 C19 O6 Dy4 -18.2(7) . . . . ?
C18 C19 O6 Dy4 164.6(6) . . . . ?
O12 N7 O10 Dy1 6.9(6) . . . . ?
O11 N7 O10 Dy1 -178.7(5) . . . . ?
O11 N7 O12 Dy1 178.7(5) . . . . ?
O10 N7 O12 Dy1 -6.8(6) . . . . ?
O15 N8 O13 Dy2 -6.0(7) . . . . ?
O14 N8 O13 Dy2 172.6(6) . . . . ?
O13 N8 O15 Dy2 5.6(6) . . . . ?
O14 N8 O15 Dy2 -172.9(7) . . . . ?
O17 N9 O16 Dy4 -178.5(6) . . . . ?
O18 N9 O16 Dy4 0.5(6) . . . . ?
O17 N9 O18 Dy4 178.5(6) . . . . ?
O16 N9 O18 Dy4 -0.5(6) . . . . ?

_refine_diff_density_max         1.021
_refine_diff_density_min         -0.811
_refine_diff_density_rms         0.107



####################################################################### 
# 
# 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_Compound-2
_database_code_depnum_ccdc_archive 'CCDC 1902976'
_audit_update_record             
;
2019-03-13 deposited with the CCDC.	2019-10-31 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C63 H99 N27 O78 Tb12, C6 H15 N [+ solvent]'
_chemical_formula_sum            'C69 H114 N28 O78 Tb12 [+ solvent]'
_chemical_formula_weight         4490.92

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      trigonal
_space_group_IT_number           167
_space_group_name_H-M_alt        'R -3 c :H'
_space_group_name_Hall           '-R 3 2"c'

_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'
'-y, x-y, z'
'-x+y, -x, z'
'y, x, -z+1/2'
'x-y, -y, -z+1/2'
'-x, -x+y, -z+1/2'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'y+2/3, x+1/3, -z+5/6'
'x-y+2/3, -y+1/3, -z+5/6'
'-x+2/3, -x+y+1/3, -z+5/6'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'y+1/3, x+2/3, -z+7/6'
'x-y+1/3, -y+2/3, -z+7/6'
'-x+1/3, -x+y+2/3, -z+7/6'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-y, -x, z-1/2'
'-x+y, y, z-1/2'
'x, x-y, z-1/2'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-y+2/3, -x+1/3, z-1/6'
'-x+y+2/3, y+1/3, z-1/6'
'x+2/3, x-y+1/3, z-1/6'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'
'-y+1/3, -x+2/3, z+1/6'
'-x+y+1/3, y+2/3, z+1/6'
'x+1/3, x-y+2/3, z+1/6'

_cell_length_a                   31.0269(10)
_cell_length_b                   31.0269(10)
_cell_length_c                   60.690(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     50597(4)
_cell_formula_units_Z            12
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    9124
_cell_measurement_theta_min      2.40
_cell_measurement_theta_max      25.32

_exptl_crystal_description       block
_exptl_crystal_colour            orange-yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.769
_exptl_crystal_F_000             25536
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.240
_exptl_crystal_size_mid          0.220
_exptl_crystal_size_min          0.200
_exptl_absorpt_coefficient_mu    5.046
_shelx_estimated_absorpt_T_min   0.377
_shelx_estimated_absorpt_T_max   0.432
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.38
_exptl_absorpt_correction_T_max  0.43
_exptl_absorpt_process_details   'SADABS; Bruker, 2008'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            120577
_diffrn_reflns_av_unetI/netI     0.0173
_diffrn_reflns_av_R_equivalents  0.0241
_diffrn_reflns_limit_h_min       -37
_diffrn_reflns_limit_h_max       37
_diffrn_reflns_limit_k_min       -37
_diffrn_reflns_limit_k_max       37
_diffrn_reflns_limit_l_min       -73
_diffrn_reflns_limit_l_max       72
_diffrn_reflns_theta_min         2.274
_diffrn_reflns_theta_max         25.442
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             10355
_reflns_number_gt                8505
_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.
 
 Structure factors included contributions from the .fab file.
 
 _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       'SMART (Bruker, 2008)'
_computing_cell_refinement       SMART
_computing_data_reduction        'SAINT (Bruker, 2008)'
_computing_structure_solution    'SHELXTL (Bruker, 2008)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    'SHELXTL (Bruker, 2008)'
_computing_publication_material  'SHELXTL (Bruker, 2008)'
_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)+(0.06P)²+1.88P] 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         10355
_refine_ls_number_parameters     565
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0356
_refine_ls_R_factor_gt           0.0285
_refine_ls_wR_factor_ref         0.0868
_refine_ls_wR_factor_gt          0.0845
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_restrained_S_all      1.059
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.35698(14) 0.73991(14) 0.08559(7) 0.0351(9) Uani 1 1 d . . . . .
H1 H 0.350889 0.720018 0.098378 0.042 Uiso 1 1 calc R U . . .
C2 C 0.39495(15) 0.78984(15) 0.05891(7) 0.0417(10) Uani 1 1 d . . . . .
C3 C 0.43839(15) 0.82098(14) 0.04556(7) 0.0399(10) Uani 1 1 d . . . . .
C4 C 0.47803(18) 0.90467(18) 0.00297(8) 0.0560(12) Uani 1 1 d . . . . .
H4 H 0.446079 0.900474 0.000029 0.067 Uiso 1 1 calc R U . . .
C5 C 0.51997(18) 0.94086(16) -0.01095(8) 0.0513(11) Uani 1 1 d . . . . .
C6 C 0.5119(2) 0.97383(19) -0.02288(8) 0.0611(13) Uani 1 1 d . . . . .
H6 H 0.479405 0.969730 -0.022803 0.073 Uiso 1 1 calc R U . . .
C7 C 0.5482(2) 1.01230(19) -0.03489(9) 0.0665(14) Uani 1 1 d . . . . .
H7 H 0.541317 1.034242 -0.043117 0.080 Uiso 1 1 calc R U . . .
C8 C 0.5951(2) 1.01771(19) -0.03450(9) 0.0670(15) Uani 1 1 d . . . . .
H8 H 0.621305 1.044712 -0.042230 0.080 Uiso 1 1 calc R U . . .
C9 C 0.6054(2) 0.98351(17) -0.02269(9) 0.0592(13) Uani 1 1 d . . . . .
C10 C 0.56678(18) 0.94433(16) -0.01113(8) 0.0506(11) Uani 1 1 d . . . . .
C11 C 0.6946(2) 1.0235(3) -0.03377(15) 0.125(3) Uani 1 1 d . . . . .
H11A H 0.684391 1.037929 -0.045624 0.188 Uiso 1 1 calc R U . . .
H11B H 0.712247 1.007575 -0.040081 0.188 Uiso 1 1 calc R U . . .
H11C H 0.716745 1.049885 -0.023591 0.188 Uiso 1 1 calc R U . . .
C12 C 0.43239(15) 0.65396(15) 0.05875(7) 0.0405(9) Uani 1 1 d . . . . .
C13 C 0.47767(15) 0.68324(16) 0.04547(8) 0.0449(10) Uani 1 1 d . . . . .
C14 C 0.54132(19) 0.67143(17) 0.00324(9) 0.0588(13) Uani 1 1 d . . . . .
H14 H 0.525036 0.636130 0.003791 0.071 Uiso 1 1 calc R U . . .
C15 C 0.57577(19) 0.69602(18) -0.01482(9) 0.0607(13) Uani 1 1 d . . . . .
C16 C 0.5852(2) 0.6671(2) -0.02925(10) 0.0736(17) Uani 1 1 d . . . . .
H16 H 0.571242 0.632437 -0.026686 0.088 Uiso 1 1 calc R U . . .
C17 C 0.6161(3) 0.6898(2) -0.04795(10) 0.0855(19) Uani 1 1 d . . . . .
H17 H 0.625829 0.671205 -0.057056 0.103 Uiso 1 1 calc R U . . .
C18 C 0.6318(2) 0.7390(2) -0.05278(10) 0.0793(18) Uani 1 1 d . . . . .
H18 H 0.649862 0.753483 -0.065947 0.095 Uiso 1 1 calc R U . . .
C19 C 0.6214(2) 0.76693(18) -0.03852(9) 0.0631(14) Uani 1 1 d . . . . .
C20 C 0.59553(19) 0.74716(18) -0.01903(8) 0.0559(12) Uani 1 1 d . . . . .
C21 C 0.6687(2) 0.8415(2) -0.05951(10) 0.0829(19) Uani 1 1 d . . . . .
H21A H 0.683890 0.877493 -0.057422 0.124 Uiso 1 1 calc R U . . .
H21B H 0.650171 0.831841 -0.073416 0.124 Uiso 1 1 calc R U . . .
H21C H 0.694814 0.832489 -0.059930 0.124 Uiso 1 1 calc R U . . .
C22 C 0.3220(3) 0.6205(3) 0.02331(18) 0.138(3) Uani 1 1 d . U . . .
H22A H 0.317025 0.599888 0.036556 0.166 Uiso 1 1 calc R U . . .
H22B H 0.357168 0.632607 0.019367 0.166 Uiso 1 1 calc R U . . .
C23 C 0.2999(3) 0.5733(2) 0.00626(14) 0.131(4) Uani 1 1 d . . . . .
H23A H 0.286516 0.542233 0.014653 0.197 Uiso 1 1 calc R U . . .
H23B H 0.326681 0.576529 -0.003411 0.197 Uiso 1 1 calc R U . . .
H23C H 0.273401 0.572892 -0.002656 0.197 Uiso 1 1 calc R U . . .
N1 N 0.40176(13) 0.76395(12) 0.07621(5) 0.0404(8) Uani 1 1 d . . . . .
N2 N 0.42359(12) 0.67843(12) 0.07621(6) 0.0426(8) Uani 1 1 d . . . . .
N3 N 0.43698(13) 0.84940(14) 0.02994(6) 0.0491(9) Uani 1 1 d . . . . .
H3A H 0.427093 0.870231 0.036196 0.059 Uiso 1 1 d R U . . .
N4 N 0.48119(13) 0.87870(13) 0.01855(6) 0.0468(9) Uani 1 1 d . . . . .
N5 N 0.48829(14) 0.65966(13) 0.03092(6) 0.0483(9) Uani 1 1 d . . . . .
H5A H 0.461390 0.641630 0.021708 0.058 Uiso 1 1 d R U . . .
N6 N 0.53120(14) 0.69337(14) 0.01838(7) 0.0531(10) Uani 1 1 d . . . . .
N7 N 0.55338(15) 0.96565(14) 0.05404(7) 0.0531(9) Uani 1 1 d . . . . .
N8 N 0.55554(16) 0.75549(17) 0.10748(8) 0.0656(12) Uani 1 1 d . . . . .
N9 N 0.49225(19) 0.79037(19) -0.03999(8) 0.0704(12) Uani 1 1 d . . . . .
N10 N 0.333333 0.666667 0.03630(13) 0.072(2) Uani 1 3 d S TU P . .
O1 O 0.47883(10) 0.82072(10) 0.05043(5) 0.0425(6) Uani 1 1 d . . . . .
O2 O 0.57593(11) 0.91144(10) -0.00111(5) 0.0478(7) Uani 1 1 d . . . . .
O3 O 0.65075(14) 0.98657(13) -0.02189(7) 0.0737(11) Uani 1 1 d . . . . .
O4 O 0.50175(10) 0.73080(10) 0.04946(5) 0.0438(7) Uani 1 1 d . . . . .
O5 O 0.58895(11) 0.77664(10) -0.00495(5) 0.0481(7) Uani 1 1 d . . . . .
O6 O 0.63490(14) 0.81563(12) -0.04133(6) 0.0651(10) Uani 1 1 d . . . . .
O7 O 0.61878(11) 0.86299(11) 0.01992(5) 0.0487(7) Uani 1 1 d . . . . .
O8 O 0.53109(10) 0.80876(10) 0.01417(5) 0.0430(7) Uani 1 1 d . . . . .
O9 O 0.56023(10) 0.82395(10) 0.06073(5) 0.0437(7) Uani 1 1 d . . . . .
O10 O 0.53258(13) 0.92249(12) 0.06331(5) 0.0580(8) Uani 1 1 d . . . . .
O11 O 0.55211(13) 1.00024(12) 0.06244(6) 0.0621(9) Uani 1 1 d . . . . .
O12 O 0.57087(12) 0.96770(11) 0.03570(6) 0.0571(8) Uani 1 1 d . . . . .
O13 O 0.52204(12) 0.72342(12) 0.09593(6) 0.0578(8) Uani 1 1 d . . . . .
O14 O 0.58176(15) 0.74548(15) 0.11901(8) 0.0879(13) Uani 1 1 d . . . . .
O15 O 0.55963(13) 0.79834(13) 0.10677(6) 0.0661(9) Uani 1 1 d . . . . .
O16 O 0.50013(13) 0.82809(13) -0.02928(6) 0.0602(8) Uani 1 1 d . . . . .
O17 O 0.45402(17) 0.76618(17) -0.04988(8) 0.0934(13) Uani 1 1 d . . . . .
O18 O 0.52582(15) 0.77944(13) -0.04013(6) 0.0662(9) Uani 1 1 d . . . . .
O1W O 0.63339(14) 0.93362(15) 0.05683(8) 0.0926(14) Uani 1 1 d . . . . .
H1XX H 0.653723 0.928001 0.049593 0.111 Uiso 1 1 d R U . . .
H1YY H 0.634598 0.961496 0.055179 0.111 Uiso 1 1 d R U . . .
O2W O 0.50162(13) 0.84852(11) 0.09695(5) 0.0574(8) Uani 1 1 d . . . . .
H2X H 0.530284 0.862405 0.102995 0.069 Uiso 1 1 d R U . . .
H2Y H 0.500835 0.867765 0.087056 0.069 Uiso 1 1 d R U . . .
O3W O 0.45019(12) 0.74822(12) 0.11602(5) 0.0572(8) Uani 1 1 d . . . . .
H3Y H 0.476720 0.767047 0.123254 0.069 Uiso 1 1 d R U . . .
H3X H 0.447741 0.719597 0.116202 0.069 Uiso 1 1 d R U . . .
O6W O 0.66269(12) 0.79387(14) 0.02486(6) 0.0656(9) Uani 1 1 d . . . . .
H6X H 0.667180 0.805821 0.009638 0.079 Uiso 1 1 d R U . . .
H6Y H 0.680415 0.822493 0.034750 0.079 Uiso 1 1 d R U . . .
O4W O 0.64185(14) 0.8226(3) 0.06269(7) 0.159(3) Uani 1 1 d . . . . .
H4X H 0.636983 0.793955 0.071476 0.191 Uiso 1 1 d DR U . . .
H4Y H 0.627119 0.842038 0.068114 0.191 Uiso 1 1 d R U . . .
O5W O 0.59412(14) 0.72660(16) 0.05843(7) 0.0815(12) Uani 1 1 d . . . . .
H5X H 0.575524 0.692701 0.052519 0.098 Uiso 1 1 d R U . . .
H5Y H 0.581071 0.725710 0.073231 0.098 Uiso 1 1 d R U . . .
O7W O 0.67130(12) 0.91040(12) -0.01971(6) 0.0666(9) Uani 1 1 d . . . . .
H7X H 0.689565 0.897141 -0.020640 0.080 Uiso 1 1 d R U . . .
H7Y H 0.674689 0.927273 -0.031400 0.080 Uiso 1 1 d R U . . .
O8W O 0.59585(14) 0.88909(13) -0.05114(6) 0.0694(10) Uani 1 1 d . . . . .
H8X H 0.584708 0.863536 -0.059455 0.083 Uiso 1 1 d R U . . .
H8Y H 0.574354 0.897899 -0.048540 0.083 Uiso 1 1 d R U . . .
Tb1 Tb 0.55846(2) 0.88168(2) 0.03487(2) 0.04701(8) Uani 1 1 d . . . . .
Tb2 Tb 0.48536(2) 0.77126(2) 0.07984(2) 0.04313(7) Uani 1 1 d . . . . .
Tb3 Tb 0.58102(2) 0.78120(2) 0.03281(2) 0.04916(8) Uani 1 1 d . . . . .
Tb4 Tb 0.58522(2) 0.84604(2) -0.01652(2) 0.04992(8) Uani 1 1 d . . . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 N2 1.318(5) 2_665 ?
C1 N1 1.332(5) . ?
C1 H1 0.9500 . ?
C2 C12 1.375(6) 2_665 ?
C2 N1 1.401(5) . ?
C2 C3 1.451(6) . ?
C3 O1 1.293(5) . ?
C3 N3 1.310(5) . ?
C4 N4 1.277(6) . ?
C4 C5 1.485(7) . ?
C4 H4 0.9500 . ?
C5 C6 1.375(7) . ?
C5 C10 1.401(6) . ?
C6 C7 1.371(7) . ?
C6 H6 0.9500 . ?
C7 C8 1.379(7) . ?
C7 H7 0.9500 . ?
C8 C9 1.444(7) . ?
C8 H8 0.9500 . ?
C9 O3 1.362(6) . ?
C9 C10 1.396(6) . ?
C10 O2 1.335(5) . ?
C11 O3 1.458(6) . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C12 N2 1.408(5) . ?
C12 C13 1.474(6) . ?
C13 N5 1.290(6) . ?
C13 O4 1.301(5) . ?
C14 N6 1.273(6) . ?
C14 C15 1.453(6) . ?
C14 H14 0.9500 . ?
C15 C16 1.387(7) . ?
C15 C20 1.409(7) . ?
C16 C17 1.423(8) . ?
C16 H16 0.9500 . ?
C17 C18 1.382(8) . ?
C17 H17 0.9500 . ?
C18 C19 1.373(7) . ?
C18 H18 0.9500 . ?
C19 O6 1.362(6) . ?
C19 C20 1.388(7) . ?
C20 O5 1.340(5) . ?
C21 O6 1.456(6) . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C22 N10 1.515(9) . ?
C22 C23 1.637(10) . ?
C22 H22A 0.9900 . ?
C22 H22B 0.9900 . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 H23C 0.9800 . ?
N1 Tb2 2.498(3) . ?
N2 Tb2 2.549(3) . ?
N3 N4 1.393(5) . ?
N3 H3A 0.9241 . ?
N4 Tb1 2.553(4) . ?
N5 N6 1.433(5) . ?
N5 H5A 0.9248 . ?
N6 Tb3 2.524(4) . ?
N7 O11 1.207(5) . ?
N7 O12 1.225(5) . ?
N7 O10 1.289(5) . ?
N7 Tb1 2.928(4) . ?
N8 O14 1.225(5) . ?
N8 O13 1.236(5) . ?
N8 O15 1.272(5) . ?
N9 O17 1.200(6) . ?
N9 O18 1.246(6) . ?
N9 O16 1.251(6) . ?
N9 Tb4 2.890(5) . ?
O1 Tb1 2.429(3) . ?
O1 Tb2 2.428(3) . ?
O2 Tb1 2.327(3) . ?
O2 Tb4 2.379(3) . ?
O4 Tb3 2.381(3) . ?
O4 Tb2 2.424(3) . ?
O5 Tb4 2.322(3) . ?
O5 Tb3 2.317(3) . ?
O6 Tb4 2.644(3) . ?
O7 Tb3 2.335(3) . ?
O7 Tb4 2.389(3) . ?
O7 Tb1 2.398(3) . ?
O8 Tb1 2.345(3) . ?
O8 Tb4 2.384(3) . ?
O8 Tb3 2.395(3) . ?
O9 Tb2 2.370(3) . ?
O9 Tb1 2.402(3) . ?
O9 Tb3 2.430(3) . ?
O10 Tb1 2.499(3) . ?
O12 Tb1 2.499(3) . ?
O13 Tb2 2.478(3) . ?
O15 Tb2 2.598(3) . ?
O16 Tb4 2.532(3) . ?
O18 Tb4 2.431(4) . ?
O1W Tb1 2.456(4) . ?
O1W H1XX 0.8550 . ?
O1W H1YY 0.8527 . ?
O2W Tb2 2.423(3) . ?
O2W H2X 0.8535 . ?
O2W H2Y 0.8554 . ?
O3W Tb2 2.396(3) . ?
O3W H3Y 0.8548 . ?
O3W H3X 0.8526 . ?
O6W Tb3 2.411(3) . ?
O6W H6X 0.9793 . ?
O6W H6Y 0.9811 . ?
O4W Tb3 2.4651(11) . ?
O4W H4X 0.9805 . ?
O4W H4Y 0.9787 . ?
O5W Tb3 2.478(3) . ?
O5W H5X 0.9805 . ?
O5W H5Y 0.9798 . ?
O7W Tb4 2.413(3) . ?
O7W H7X 0.8525 . ?
O7W H7Y 0.8565 . ?
O8W Tb4 2.422(4) . ?
O8W H8X 0.8537 . ?
O8W H8Y 0.8525 . ?
Tb1 Tb3 3.5225(3) . ?
Tb1 Tb4 3.5441(3) . ?
Tb2 Tb3 4.0173(3) . ?
Tb3 Tb4 3.5729(3) . ?

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
N2 C1 N1 116.5(4) 2_665 . ?
N2 C1 H1 121.7 2_665 . ?
N1 C1 H1 121.7 . . ?
C12 C2 N1 108.7(4) 2_665 . ?
C12 C2 C3 134.9(4) 2_665 . ?
N1 C2 C3 116.4(4) . . ?
O1 C3 N3 121.9(4) . . ?
O1 C3 C2 116.7(4) . . ?
N3 C3 C2 121.3(4) . . ?
N4 C4 C5 125.7(4) . . ?
N4 C4 H4 117.2 . . ?
C5 C4 H4 117.2 . . ?
C6 C5 C10 120.4(4) . . ?
C6 C5 C4 116.4(4) . . ?
C10 C5 C4 123.0(4) . . ?
C7 C6 C5 123.5(5) . . ?
C7 C6 H6 118.3 . . ?
C5 C6 H6 118.3 . . ?
C8 C7 C6 117.0(5) . . ?
C8 C7 H7 121.5 . . ?
C6 C7 H7 121.5 . . ?
C7 C8 C9 121.9(5) . . ?
C7 C8 H8 119.1 . . ?
C9 C8 H8 119.1 . . ?
O3 C9 C10 116.8(4) . . ?
O3 C9 C8 124.6(4) . . ?
C10 C9 C8 118.6(5) . . ?
O2 C10 C9 118.4(4) . . ?
O2 C10 C5 123.1(4) . . ?
C9 C10 C5 118.5(4) . . ?
O3 C11 H11A 109.5 . . ?
O3 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
O3 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
C2 C12 N2 107.7(4) 3_565 . ?
C2 C12 C13 134.8(4) 3_565 . ?
N2 C12 C13 117.5(4) . . ?
N5 C13 O4 127.3(4) . . ?
N5 C13 C12 117.4(4) . . ?
O4 C13 C12 115.3(4) . . ?
N6 C14 C15 125.3(4) . . ?
N6 C14 H14 117.4 . . ?
C15 C14 H14 117.4 . . ?
C16 C15 C20 120.0(4) . . ?
C16 C15 C14 118.4(4) . . ?
C20 C15 C14 121.3(4) . . ?
C15 C16 C17 119.4(5) . . ?
C15 C16 H16 120.3 . . ?
C17 C16 H16 120.3 . . ?
C18 C17 C16 119.6(5) . . ?
C18 C17 H17 120.2 . . ?
C16 C17 H17 120.2 . . ?
C19 C18 C17 120.0(5) . . ?
C19 C18 H18 120.0 . . ?
C17 C18 H18 120.0 . . ?
C18 C19 O6 125.7(5) . . ?
C18 C19 C20 121.6(5) . . ?
O6 C19 C20 112.7(4) . . ?
O5 C20 C19 119.6(4) . . ?
O5 C20 C15 121.6(4) . . ?
C19 C20 C15 118.8(4) . . ?
O6 C21 H21A 109.5 . . ?
O6 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
O6 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
N10 C22 C23 166.0(9) . . ?
N10 C22 H22A 94.3 . . ?
C23 C22 H22A 94.3 . . ?
N10 C22 H22B 94.3 . . ?
C23 C22 H22B 94.3 . . ?
H22A C22 H22B 103.1 . . ?
C22 C23 H23A 109.5 . . ?
C22 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
C22 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C1 N1 C2 103.1(3) . . ?
C1 N1 Tb2 139.3(3) . . ?
C2 N1 Tb2 117.5(3) . . ?
C1 N2 C12 103.8(3) 3_565 . ?
C1 N2 Tb2 140.4(3) 3_565 . ?
C12 N2 Tb2 115.8(3) . . ?
C3 N3 N4 116.4(4) . . ?
C3 N3 H3A 107.9 . . ?
N4 N3 H3A 108.1 . . ?
C4 N4 N3 114.7(4) . . ?
C4 N4 Tb1 129.1(3) . . ?
N3 N4 Tb1 115.6(3) . . ?
C13 N5 N6 110.9(4) . . ?
C13 N5 H5A 110.3 . . ?
N6 N5 H5A 110.4 . . ?
C14 N6 N5 112.4(4) . . ?
C14 N6 Tb3 130.2(3) . . ?
N5 N6 Tb3 116.6(3) . . ?
O11 N7 O12 123.2(4) . . ?
O11 N7 O10 121.1(4) . . ?
O12 N7 O10 115.4(4) . . ?
O11 N7 Tb1 178.1(3) . . ?
O12 N7 Tb1 57.7(2) . . ?
O10 N7 Tb1 58.1(2) . . ?
O14 N8 O13 121.2(5) . . ?
O14 N8 O15 123.5(5) . . ?
O13 N8 O15 115.3(4) . . ?
O17 N9 O18 121.7(5) . . ?
O17 N9 O16 121.0(5) . . ?
O18 N9 O16 117.3(5) . . ?
O17 N9 Tb4 178.0(4) . . ?
O18 N9 Tb4 56.3(3) . . ?
O16 N9 Tb4 61.0(3) . . ?
C22 N10 C22 95.4(7) . 3_565 ?
C22 N10 C22 95.4(7) . 2_665 ?
C22 N10 C22 95.4(7) 3_565 2_665 ?
C3 O1 Tb1 121.2(3) . . ?
C3 O1 Tb2 124.1(3) . . ?
Tb1 O1 Tb2 113.84(11) . . ?
C10 O2 Tb1 129.4(3) . . ?
C10 O2 Tb4 129.5(3) . . ?
Tb1 O2 Tb4 97.72(10) . . ?
C9 O3 C11 124.2(5) . . ?
C13 O4 Tb3 119.0(3) . . ?
C13 O4 Tb2 125.4(3) . . ?
Tb3 O4 Tb2 113.46(11) . . ?
C20 O5 Tb4 122.4(3) . . ?
C20 O5 Tb3 136.9(3) . . ?
Tb4 O5 Tb3 100.74(11) . . ?
C19 O6 C21 116.3(4) . . ?
C19 O6 Tb4 114.5(3) . . ?
C21 O6 Tb4 128.5(3) . . ?
Tb3 O7 Tb4 98.30(11) . . ?
Tb3 O7 Tb1 96.20(10) . . ?
Tb4 O7 Tb1 95.54(11) . . ?
Tb1 O8 Tb4 97.08(10) . . ?
Tb1 O8 Tb3 96.01(10) . . ?
Tb4 O8 Tb3 96.76(9) . . ?
Tb2 O9 Tb1 117.01(11) . . ?
Tb2 O9 Tb3 113.64(11) . . ?
Tb1 O9 Tb3 93.60(10) . . ?
N7 O10 Tb1 96.0(3) . . ?
N7 O12 Tb1 97.8(3) . . ?
N8 O13 Tb2 101.2(3) . . ?
N8 O15 Tb2 94.3(3) . . ?
N9 O16 Tb4 93.4(3) . . ?
N9 O18 Tb4 98.4(3) . . ?
Tb1 O1W H1XX 98.1 . . ?
Tb1 O1W H1YY 98.6 . . ?
H1XX O1W H1YY 118.9 . . ?
Tb2 O2W H2X 109.4 . . ?
Tb2 O2W H2Y 109.0 . . ?
H2X O2W H2Y 109.6 . . ?
Tb2 O3W H3Y 97.3 . . ?
Tb2 O3W H3X 96.5 . . ?
H3Y O3W H3X 105.0 . . ?
Tb3 O6W H6X 100.9 . . ?
Tb3 O6W H6Y 95.3 . . ?
H6X O6W H6Y 109.0 . . ?
Tb3 O4W H4X 101.4 . . ?
Tb3 O4W H4Y 95.5 . . ?
H4X O4W H4Y 117.9 . . ?
Tb3 O5W H5X 107.1 . . ?
Tb3 O5W H5Y 112.8 . . ?
H5X O5W H5Y 107.0 . . ?
Tb4 O7W H7X 109.5 . . ?
Tb4 O7W H7Y 108.6 . . ?
H7X O7W H7Y 109.4 . . ?
Tb4 O8W H8X 96.9 . . ?
Tb4 O8W H8Y 96.0 . . ?
H8X O8W H8Y 112.9 . . ?
O2 Tb1 O8 77.29(10) . . ?
O2 Tb1 O7 71.67(10) . . ?
O8 Tb1 O7 60.89(10) . . ?
O2 Tb1 O9 145.19(10) . . ?
O8 Tb1 O9 76.28(10) . . ?
O7 Tb1 O9 75.83(10) . . ?
O2 Tb1 O1 128.19(10) . . ?
O8 Tb1 O1 73.76(9) . . ?
O7 Tb1 O1 124.88(10) . . ?
O9 Tb1 O1 63.83(9) . . ?
O2 Tb1 O1W 107.00(14) . . ?
O8 Tb1 O1W 133.72(11) . . ?
O7 Tb1 O1W 76.51(12) . . ?
O9 Tb1 O1W 76.58(13) . . ?
O1 Tb1 O1W 124.11(14) . . ?
O2 Tb1 O10 121.16(10) . . ?
O8 Tb1 O10 143.71(10) . . ?
O7 Tb1 O10 150.64(11) . . ?
O9 Tb1 O10 93.42(10) . . ?
O1 Tb1 O10 70.53(10) . . ?
O1W Tb1 O10 74.42(13) . . ?
O2 Tb1 O12 73.40(11) . . ?
O8 Tb1 O12 146.03(11) . . ?
O7 Tb1 O12 122.95(10) . . ?
O9 Tb1 O12 137.25(11) . . ?
O1 Tb1 O12 112.17(10) . . ?
O1W Tb1 O12 72.45(12) . . ?
O10 Tb1 O12 50.35(10) . . ?
O2 Tb1 N4 71.24(11) . . ?
O8 Tb1 N4 82.91(10) . . ?
O7 Tb1 N4 132.60(11) . . ?
O9 Tb1 N4 126.70(10) . . ?
O1 Tb1 N4 63.36(10) . . ?
O1W Tb1 N4 142.96(12) . . ?
O10 Tb1 N4 75.67(11) . . ?
O12 Tb1 N4 71.75(11) . . ?
O2 Tb1 N7 97.19(11) . . ?
O8 Tb1 N7 156.45(10) . . ?
O7 Tb1 N7 139.58(11) . . ?
O9 Tb1 N7 115.81(10) . . ?
O1 Tb1 N7 92.99(11) . . ?
O1W Tb1 N7 69.83(12) . . ?
O10 Tb1 N7 25.97(11) . . ?
O12 Tb1 N7 24.50(10) . . ?
N4 Tb1 N7 73.68(11) . . ?
O2 Tb1 Tb3 101.99(7) . . ?
O8 Tb1 Tb3 42.54(7) . . ?
O7 Tb1 Tb3 41.22(7) . . ?
O9 Tb1 Tb3 43.50(7) . . ?
O1 Tb1 Tb3 84.23(7) . . ?
O1W Tb1 Tb3 93.34(9) . . ?
O10 Tb1 Tb3 136.85(7) . . ?
O12 Tb1 Tb3 162.40(8) . . ?
N4 Tb1 Tb3 123.56(8) . . ?
N7 Tb1 Tb3 157.59(8) . . ?
O2 Tb1 Tb4 41.70(7) . . ?
O8 Tb1 Tb4 41.89(7) . . ?
O7 Tb1 Tb4 42.13(8) . . ?
O9 Tb1 Tb4 104.24(7) . . ?
O1 Tb1 Tb4 113.88(7) . . ?
O1W Tb1 Tb4 112.93(11) . . ?
O10 Tb1 Tb4 161.96(8) . . ?
O12 Tb1 Tb4 114.57(8) . . ?
N4 Tb1 Tb4 90.54(8) . . ?
N7 Tb1 Tb4 138.79(8) . . ?
Tb3 Tb1 Tb4 60.742(7) . . ?
O9 Tb2 O3W 142.88(11) . . ?
O9 Tb2 O4 66.28(9) . . ?
O3W Tb2 O4 136.46(11) . . ?
O9 Tb2 O2W 83.09(10) . . ?
O3W Tb2 O2W 75.00(11) . . ?
O4 Tb2 O2W 147.64(10) . . ?
O9 Tb2 O1 64.33(9) . . ?
O3W Tb2 O1 133.85(10) . . ?
O4 Tb2 O1 82.72(10) . . ?
O2W Tb2 O1 74.42(10) . . ?
O9 Tb2 O13 91.19(10) . . ?
O3W Tb2 O13 74.78(11) . . ?
O4 Tb2 O13 73.22(11) . . ?
O2W Tb2 O13 119.55(11) . . ?
O1 Tb2 O13 151.26(10) . . ?
O9 Tb2 N1 129.38(10) . . ?
O3W Tb2 N1 75.91(11) . . ?
O4 Tb2 N1 111.29(10) . . ?
O2W Tb2 N1 79.67(11) . . ?
O1 Tb2 N1 65.26(10) . . ?
O13 Tb2 N1 138.37(11) . . ?
O9 Tb2 N2 131.38(10) . . ?
O3W Tb2 N2 76.66(11) . . ?
O4 Tb2 N2 65.35(10) . . ?
O2W Tb2 N2 145.29(11) . . ?
O1 Tb2 N2 113.41(10) . . ?
O13 Tb2 N2 70.63(11) . . ?
N1 Tb2 N2 74.32(10) . . ?
O9 Tb2 O15 71.32(10) . . ?
O3W Tb2 O15 73.64(11) . . ?
O4 Tb2 O15 105.32(11) . . ?
O2W Tb2 O15 72.45(12) . . ?
O1 Tb2 O15 126.79(10) . . ?
O13 Tb2 O15 49.25(11) . . ?
N1 Tb2 O15 142.92(11) . . ?
N2 Tb2 O15 117.66(11) . . ?
O9 Tb2 Tb3 33.64(7) . . ?
O3W Tb2 Tb3 151.98(8) . . ?
O4 Tb2 Tb3 32.94(7) . . ?
O2W Tb2 Tb3 116.62(8) . . ?
O1 Tb2 Tb3 73.79(6) . . ?
O13 Tb2 Tb3 77.46(8) . . ?
N1 Tb2 Tb3 129.64(8) . . ?
N2 Tb2 Tb3 97.73(8) . . ?
O15 Tb2 Tb3 85.43(9) . . ?
O5 Tb3 O7 73.99(10) . . ?
O5 Tb3 O4 119.08(10) . . ?
O7 Tb3 O4 130.41(10) . . ?
O5 Tb3 O8 70.24(10) . . ?
O7 Tb3 O8 61.08(10) . . ?
O4 Tb3 O8 78.16(10) . . ?
O5 Tb3 O6W 71.16(12) . . ?
O7 Tb3 O6W 80.82(11) . . ?
O4 Tb3 O6W 148.03(11) . . ?
O8 Tb3 O6W 131.47(11) . . ?
O5 Tb3 O9 142.05(10) . . ?
O7 Tb3 O9 76.48(10) . . ?
O4 Tb3 O9 66.01(9) . . ?
O8 Tb3 O9 74.85(9) . . ?
O6W Tb3 O9 126.50(11) . . ?
O5 Tb3 O4W 133.05(15) . . ?
O7 Tb3 O4W 81.0(2) . . ?
O4 Tb3 O4W 107.47(16) . . ?
O8 Tb3 O4W 128.69(17) . . ?
O6W Tb3 O4W 66.02(14) . . ?
O9 Tb3 O4W 62.98(13) . . ?
O5 Tb3 O5W 121.35(12) . . ?
O7 Tb3 O5W 142.05(13) . . ?
O4 Tb3 O5W 75.72(11) . . ?
O8 Tb3 O5W 153.75(11) . . ?
O6W Tb3 O5W 73.67(12) . . ?
O9 Tb3 O5W 96.58(12) . . ?
O4W Tb3 O5W 63.2(2) . . ?
O5 Tb3 N6 67.50(11) . . ?
O7 Tb3 N6 139.55(12) . . ?
O4 Tb3 N6 64.16(11) . . ?
O8 Tb3 N6 93.75(11) . . ?
O6W Tb3 N6 97.65(12) . . ?
O9 Tb3 N6 130.16(10) . . ?
O4W Tb3 N6 135.5(2) . . ?
O5W Tb3 N6 72.59(14) . . ?
O5 Tb3 Tb1 99.41(7) . . ?
O7 Tb3 Tb1 42.59(7) . . ?
O4 Tb3 Tb1 88.22(7) . . ?
O8 Tb3 Tb1 41.45(7) . . ?
O6W Tb3 Tb1 121.38(9) . . ?
O9 Tb3 Tb1 42.90(7) . . ?
O4W Tb3 Tb1 87.26(16) . . ?
O5W Tb3 Tb1 139.08(10) . . ?
N6 Tb3 Tb1 133.04(9) . . ?
O5 Tb3 Tb4 39.68(7) . . ?
O7 Tb3 Tb4 41.42(8) . . ?
O4 Tb3 Tb4 117.40(7) . . ?
O8 Tb3 Tb4 41.51(7) . . ?
O6W Tb3 Tb4 90.07(9) . . ?
O9 Tb3 Tb4 102.82(7) . . ?
O4W Tb3 Tb4 121.37(18) . . ?
O5W Tb3 Tb4 159.80(9) . . ?
N6 Tb3 Tb4 98.49(9) . . ?
Tb1 Tb3 Tb4 59.928(6) . . ?
O5 Tb3 Tb2 142.67(7) . . ?
O7 Tb3 Tb2 105.75(7) . . ?
O4 Tb3 Tb2 33.60(7) . . ?
O8 Tb3 Tb2 77.17(7) . . ?
O6W Tb3 Tb2 146.16(9) . . ?
O9 Tb3 Tb2 32.71(6) . . ?
O4W Tb3 Tb2 82.01(12) . . ?
O5W Tb3 Tb2 82.47(9) . . ?
N6 Tb3 Tb2 97.66(8) . . ?
Tb1 Tb3 Tb2 64.943(6) . . ?
Tb4 Tb3 Tb2 117.142(8) . . ?
O5 Tb4 O7 72.89(10) . . ?
O5 Tb4 O2 139.06(10) . . ?
O7 Tb4 O2 70.94(10) . . ?
O5 Tb4 O8 70.34(10) . . ?
O7 Tb4 O8 60.47(10) . . ?
O2 Tb4 O8 75.54(9) . . ?
O5 Tb4 O8W 135.85(11) . . ?
O7 Tb4 O8W 139.26(11) . . ?
O2 Tb4 O8W 84.95(11) . . ?
O8 Tb4 O8W 144.48(11) . . ?
O5 Tb4 O7W 104.11(11) . . ?
O7 Tb4 O7W 73.25(11) . . ?
O2 Tb4 O7W 83.21(11) . . ?
O8 Tb4 O7W 133.12(11) . . ?
O8W Tb4 O7W 71.64(13) . . ?
O5 Tb4 O18 76.00(12) . . ?
O7 Tb4 O18 142.61(11) . . ?
O2 Tb4 O18 126.38(12) . . ?
O8 Tb4 O18 89.85(11) . . ?
O8W Tb4 O18 78.10(12) . . ?
O7W Tb4 O18 135.31(12) . . ?
O5 Tb4 O16 114.74(11) . . ?
O7 Tb4 O16 128.58(10) . . ?
O2 Tb4 O16 75.54(11) . . ?
O8 Tb4 O16 74.23(10) . . ?
O8W Tb4 O16 72.28(12) . . ?
O7W Tb4 O16 139.33(12) . . ?
O18 Tb4 O16 50.86(12) . . ?
O5 Tb4 O6 62.15(10) . . ?
O7 Tb4 O6 109.76(11) . . ?
O2 Tb4 O6 150.38(10) . . ?
O8 Tb4 O6 131.81(9) . . ?
O8W Tb4 O6 76.11(11) . . ?
O7W Tb4 O6 69.40(12) . . ?
O18 Tb4 O6 71.97(13) . . ?
O16 Tb4 O6 118.51(12) . . ?
O5 Tb4 N9 95.30(13) . . ?
O7 Tb4 N9 141.54(12) . . ?
O2 Tb4 N9 101.14(13) . . ?
O8 Tb4 N9 81.06(12) . . ?
O8W Tb4 N9 73.87(13) . . ?
O7W Tb4 N9 144.69(13) . . ?
O18 Tb4 N9 25.26(12) . . ?
O16 Tb4 N9 25.61(12) . . ?
O6 Tb4 N9 95.27(14) . . ?
O5 Tb4 Tb1 98.70(7) . . ?
O7 Tb4 Tb1 42.33(7) . . ?
O2 Tb4 Tb1 40.59(7) . . ?
O8 Tb4 Tb1 41.04(7) . . ?
O8W Tb4 Tb1 125.45(8) . . ?
O7W Tb4 Tb1 98.47(9) . . ?
O18 Tb4 Tb1 125.99(9) . . ?
O16 Tb4 Tb1 87.51(8) . . ?
O6 Tb4 Tb1 151.89(9) . . ?
N9 Tb4 Tb1 107.50(10) . . ?
O5 Tb4 Tb3 39.57(7) . . ?
O7 Tb4 Tb3 40.28(7) . . ?
O2 Tb4 Tb3 99.49(7) . . ?
O8 Tb4 Tb3 41.73(7) . . ?
O8W Tb4 Tb3 173.69(9) . . ?
O7W Tb4 Tb3 104.28(9) . . ?
O18 Tb4 Tb3 102.51(9) . . ?
O16 Tb4 Tb3 113.08(8) . . ?
O6 Tb4 Tb3 98.03(8) . . ?
N9 Tb4 Tb3 109.39(10) . . ?
Tb1 Tb4 Tb3 59.330(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
C12 C2 C3 O1 -177.3(4) 2_665 . . . ?
N1 C2 C3 O1 2.1(6) . . . . ?
C12 C2 C3 N3 5.4(8) 2_665 . . . ?
N1 C2 C3 N3 -175.3(4) . . . . ?
N4 C4 C5 C6 -164.1(5) . . . . ?
N4 C4 C5 C10 11.7(8) . . . . ?
C10 C5 C6 C7 -2.1(8) . . . . ?
C4 C5 C6 C7 173.8(5) . . . . ?
C5 C6 C7 C8 -0.7(9) . . . . ?
C6 C7 C8 C9 2.2(9) . . . . ?
C7 C8 C9 O3 179.2(5) . . . . ?
C7 C8 C9 C10 -0.9(8) . . . . ?
O3 C9 C10 O2 -3.3(7) . . . . ?
C8 C9 C10 O2 176.8(4) . . . . ?
O3 C9 C10 C5 177.9(4) . . . . ?
C8 C9 C10 C5 -2.0(7) . . . . ?
C6 C5 C10 O2 -175.3(4) . . . . ?
C4 C5 C10 O2 9.0(7) . . . . ?
C6 C5 C10 C9 3.4(7) . . . . ?
C4 C5 C10 C9 -172.2(5) . . . . ?
C2 C12 C13 N5 -3.8(7) 3_565 . . . ?
N2 C12 C13 N5 173.2(4) . . . . ?
C2 C12 C13 O4 174.3(5) 3_565 . . . ?
N2 C12 C13 O4 -8.7(6) . . . . ?
N6 C14 C15 C16 175.9(6) . . . . ?
N6 C14 C15 C20 -10.2(9) . . . . ?
C20 C15 C16 C17 1.7(10) . . . . ?
C14 C15 C16 C17 175.6(6) . . . . ?
C15 C16 C17 C18 -6.9(11) . . . . ?
C16 C17 C18 C19 5.8(11) . . . . ?
C17 C18 C19 O6 179.8(6) . . . . ?
C17 C18 C19 C20 0.6(10) . . . . ?
C18 C19 C20 O5 175.8(6) . . . . ?
O6 C19 C20 O5 -3.5(8) . . . . ?
C18 C19 C20 C15 -5.7(9) . . . . ?
O6 C19 C20 C15 175.0(5) . . . . ?
C16 C15 C20 O5 -177.1(5) . . . . ?
C14 C15 C20 O5 9.2(8) . . . . ?
C16 C15 C20 C19 4.5(9) . . . . ?
C14 C15 C20 C19 -169.2(5) . . . . ?
N2 C1 N1 C2 2.6(5) 2_665 . . . ?
N2 C1 N1 Tb2 -174.0(3) 2_665 . . . ?
C12 C2 N1 C1 -1.6(4) 2_665 . . . ?
C3 C2 N1 C1 178.9(4) . . . . ?
C12 C2 N1 Tb2 175.8(3) 2_665 . . . ?
C3 C2 N1 Tb2 -3.7(5) . . . . ?
C2 C12 N2 C1 1.1(4) 3_565 . . 3_565 ?
C13 C12 N2 C1 -176.7(4) . . . 3_565 ?
C2 C12 N2 Tb2 -178.1(3) 3_565 . . . ?
C13 C12 N2 Tb2 4.1(5) . . . . ?
O1 C3 N3 N4 1.2(6) . . . . ?
C2 C3 N3 N4 178.4(4) . . . . ?
C5 C4 N4 N3 176.7(4) . . . . ?
C5 C4 N4 Tb1 5.8(7) . . . . ?
C3 N3 N4 C4 177.8(4) . . . . ?
C3 N3 N4 Tb1 -10.0(5) . . . . ?
O4 C13 N5 N6 -1.7(6) . . . . ?
C12 C13 N5 N6 176.1(4) . . . . ?
C15 C14 N6 N5 166.9(5) . . . . ?
C15 C14 N6 Tb3 -23.6(8) . . . . ?
C13 N5 N6 C14 -177.1(4) . . . . ?
C13 N5 N6 Tb3 11.8(5) . . . . ?
C23 C22 N10 C22 -4(4) . . . 3_565 ?
C23 C22 N10 C22 -100(3) . . . 2_665 ?
N3 C3 O1 Tb1 9.3(5) . . . . ?
C2 C3 O1 Tb1 -168.0(3) . . . . ?
N3 C3 O1 Tb2 178.0(3) . . . . ?
C2 C3 O1 Tb2 0.7(5) . . . . ?
C9 C10 O2 Tb1 130.7(4) . . . . ?
C5 C10 O2 Tb1 -50.6(6) . . . . ?
C9 C10 O2 Tb4 -75.0(5) . . . . ?
C5 C10 O2 Tb4 103.7(5) . . . . ?
C10 C9 O3 C11 177.0(6) . . . . ?
C8 C9 O3 C11 -3.1(9) . . . . ?
N5 C13 O4 Tb3 -10.2(6) . . . . ?
C12 C13 O4 Tb3 172.0(3) . . . . ?
N5 C13 O4 Tb2 -172.4(4) . . . . ?
C12 C13 O4 Tb2 9.8(5) . . . . ?
C19 C20 O5 Tb4 28.5(6) . . . . ?
C15 C20 O5 Tb4 -150.0(4) . . . . ?
C19 C20 O5 Tb3 -149.3(4) . . . . ?
C15 C20 O5 Tb3 32.3(7) . . . . ?
C18 C19 O6 C21 -8.5(9) . . . . ?
C20 C19 O6 C21 170.7(5) . . . . ?
C18 C19 O6 Tb4 162.8(5) . . . . ?
C20 C19 O6 Tb4 -18.0(6) . . . . ?
O11 N7 O10 Tb1 -178.0(4) . . . . ?
O12 N7 O10 Tb1 7.1(4) . . . . ?
O11 N7 O12 Tb1 178.1(4) . . . . ?
O10 N7 O12 Tb1 -7.1(4) . . . . ?
O14 N8 O13 Tb2 177.3(4) . . . . ?
O15 N8 O13 Tb2 -1.2(5) . . . . ?
O14 N8 O15 Tb2 -177.4(5) . . . . ?
O13 N8 O15 Tb2 1.1(5) . . . . ?
O17 N9 O16 Tb4 179.7(5) . . . . ?
O18 N9 O16 Tb4 -1.1(5) . . . . ?
O17 N9 O18 Tb4 -179.7(5) . . . . ?
O16 N9 O18 Tb4 1.1(5) . . . . ?

_refine_diff_density_max         1.276
_refine_diff_density_min         -1.051
_refine_diff_density_rms         0.092



####################################################################### 
# 
# 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_Compound-1
_database_code_depnum_ccdc_archive 'CCDC 1902975'
_audit_update_record             
;
2019-03-13 deposited with the CCDC.	2019-10-31 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C63 H99 Gd12 N27 O78, C6 H15 N [+ solvent]'
_chemical_formula_sum            'C69 H114 Gd12 N28 O78 [+ solvent]'
_chemical_formula_weight         4470.88

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'
Gd Gd -0.1653 3.9035 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      trigonal
_space_group_IT_number           167
_space_group_name_H-M_alt        'R -3 c :H'
_space_group_name_Hall           '-R 3 2"c'

_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'
'-y, x-y, z'
'-x+y, -x, z'
'y, x, -z+1/2'
'x-y, -y, -z+1/2'
'-x, -x+y, -z+1/2'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'y+2/3, x+1/3, -z+5/6'
'x-y+2/3, -y+1/3, -z+5/6'
'-x+2/3, -x+y+1/3, -z+5/6'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'y+1/3, x+2/3, -z+7/6'
'x-y+1/3, -y+2/3, -z+7/6'
'-x+1/3, -x+y+2/3, -z+7/6'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-y, -x, z-1/2'
'-x+y, y, z-1/2'
'x, x-y, z-1/2'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-y+2/3, -x+1/3, z-1/6'
'-x+y+2/3, y+1/3, z-1/6'
'x+2/3, x-y+1/3, z-1/6'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'
'-y+1/3, -x+2/3, z+1/6'
'-x+y+1/3, y+2/3, z+1/6'
'x+1/3, x-y+2/3, z+1/6'

_cell_length_a                   31.0997(3)
_cell_length_b                   31.0997(3)
_cell_length_c                   61.3340(12)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     51374.1(14)
_cell_formula_units_Z            12
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    3993
_cell_measurement_theta_min      2.11
_cell_measurement_theta_max      27.12

_exptl_crystal_description       block
_exptl_crystal_colour            orange
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.734
_exptl_crystal_F_000             25392
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.220
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.180
_exptl_absorpt_coefficient_mu    4.661
_shelx_estimated_absorpt_T_min   0.427
_shelx_estimated_absorpt_T_max   0.488
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.43
_exptl_absorpt_correction_T_max  0.49
_exptl_absorpt_process_details   'SADABS, Bruker, 2008'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'multiwire proportional'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            256286
_diffrn_reflns_av_unetI/netI     0.0117
_diffrn_reflns_av_R_equivalents  0.0281
_diffrn_reflns_limit_h_min       -39
_diffrn_reflns_limit_h_max       39
_diffrn_reflns_limit_k_min       -39
_diffrn_reflns_limit_k_max       39
_diffrn_reflns_limit_l_min       -78
_diffrn_reflns_limit_l_max       78
_diffrn_reflns_theta_min         1.310
_diffrn_reflns_theta_max         26.998
_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             12448
_reflns_number_gt                10911
_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.
 
 Structure factors included contributions from the .fab file.
 
 _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       'SMART (Bruker, 2008)'
_computing_cell_refinement       SMART
_computing_data_reduction        'SAINT (Bruker, 2008)'
_computing_structure_solution    'SHELXTL (Bruker, 2008)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    'SHELXTL (Bruker, 2008)'
_computing_publication_material  'SHELXTL (Bruker, 2008)'
_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)+(0.07P)²+1.99P] 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         12448
_refine_ls_number_parameters     565
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0356
_refine_ls_R_factor_gt           0.0291
_refine_ls_wR_factor_ref         0.0955
_refine_ls_wR_factor_gt          0.0922
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_restrained_S_all      1.048
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.35738(14) 0.74019(14) 0.08511(6) 0.0432(8) Uani 1 1 d . . . . .
H1 H 0.351760 0.720908 0.097923 0.052 Uiso 1 1 calc R U . . .
C2 C 0.39471(14) 0.78998(14) 0.05860(6) 0.0422(8) Uani 1 1 d . . . . .
C3 C 0.43898(14) 0.82180(14) 0.04533(6) 0.0437(8) Uani 1 1 d . . . . .
C4 C 0.47849(16) 0.90379(16) 0.00352(7) 0.0542(10) Uani 1 1 d . . . . .
H4 H 0.446349 0.898878 0.000565 0.065 Uiso 1 1 calc R U . . .
C5 C 0.51969(18) 0.94079(18) -0.01051(8) 0.0612(11) Uani 1 1 d . . . . .
C6 C 0.51189(17) 0.97584(16) -0.02304(7) 0.0568(10) Uani 1 1 d . . . . .
H6 H 0.479727 0.972287 -0.023181 0.068 Uiso 1 1 calc R U . . .
C7 C 0.54819(17) 1.01304(17) -0.03445(8) 0.0577(10) Uani 1 1 d . . . . .
H7 H 0.542193 1.035758 -0.042381 0.069 Uiso 1 1 calc R U . . .
C8 C 0.5947(2) 1.01734(18) -0.03430(8) 0.0675(13) Uani 1 1 d . . . . .
H8 H 0.620944 1.043580 -0.042215 0.081 Uiso 1 1 calc R U . . .
C9 C 0.60399(19) 0.98347(17) -0.02261(9) 0.0653(13) Uani 1 1 d . . . . .
C10 C 0.56727(19) 0.94434(16) -0.01092(7) 0.0577(11) Uani 1 1 d . . . . .
C11 C 0.69614(19) 1.02752(18) -0.02956(9) 0.0707(13) Uani 1 1 d . . . . .
H11A H 0.709243 1.016299 -0.041429 0.106 Uiso 1 1 calc R U . . .
H11B H 0.720565 1.041159 -0.017737 0.106 Uiso 1 1 calc R U . . .
H11C H 0.689465 1.053247 -0.034997 0.106 Uiso 1 1 calc R U . . .
C12 C 0.43297(14) 0.65313(15) 0.05884(6) 0.0455(8) Uani 1 1 d . . . . .
C13 C 0.47657(15) 0.68191(15) 0.04515(7) 0.0474(9) Uani 1 1 d . . . . .
C14 C 0.54090(16) 0.67110(15) 0.00298(7) 0.0497(9) Uani 1 1 d . . . . .
H14 H 0.525014 0.635911 0.003639 0.060 Uiso 1 1 calc R U . . .
C15 C 0.57471(16) 0.69524(15) -0.01486(7) 0.0496(9) Uani 1 1 d . . . . .
C16 C 0.58448(18) 0.66778(18) -0.02943(7) 0.0572(10) Uani 1 1 d . . . . .
H16 H 0.573419 0.633981 -0.026138 0.069 Uiso 1 1 calc R U . . .
C17 C 0.6097(2) 0.6873(2) -0.04865(9) 0.0721(13) Uani 1 1 d . . . . .
H17 H 0.613260 0.666067 -0.058739 0.087 Uiso 1 1 calc R U . . .
C18 C 0.62968(18) 0.73653(18) -0.05349(8) 0.0589(11) Uani 1 1 d . . . . .
H18 H 0.648462 0.750707 -0.066369 0.071 Uiso 1 1 calc R U . . .
C19 C 0.62065(16) 0.76533(16) -0.03805(7) 0.0514(9) Uani 1 1 d . . . . .
C20 C 0.59407(17) 0.74634(17) -0.01871(8) 0.0585(11) Uani 1 1 d . . . . .
C21 C 0.66578(18) 0.83848(18) -0.06004(8) 0.0638(12) Uani 1 1 d . . . . .
H21A H 0.675877 0.873800 -0.060076 0.096 Uiso 1 1 calc R U . . .
H21B H 0.647946 0.823034 -0.073573 0.096 Uiso 1 1 calc R U . . .
H21C H 0.695291 0.834921 -0.058983 0.096 Uiso 1 1 calc R U . . .
C22 C 0.3277(2) 0.6202(2) 0.02922(10) 0.0806(15) Uani 1 1 d . . . . .
H22A H 0.305900 0.598115 0.040905 0.097 Uiso 1 1 calc R U . . .
H22B H 0.360941 0.625057 0.032659 0.097 Uiso 1 1 calc R U . . .
C23 C 0.3116(2) 0.58272(19) 0.00899(10) 0.0744(14) Uani 1 1 d . . . . .
H23A H 0.283646 0.582219 0.001368 0.112 Uiso 1 1 calc R U . . .
H23B H 0.301585 0.549283 0.014299 0.112 Uiso 1 1 calc R U . . .
H23C H 0.339647 0.593697 -0.001056 0.112 Uiso 1 1 calc R U . . .
Gd1 Gd 0.55850(2) 0.88181(2) 0.03471(2) 0.04792(7) Uani 1 1 d . . . . .
Gd2 Gd 0.48533(2) 0.77095(2) 0.07931(2) 0.04674(7) Uani 1 1 d . . . . .
Gd3 Gd 0.58135(2) 0.78098(2) 0.03246(2) 0.05006(7) Uani 1 1 d . . . . .
Gd4 Gd 0.58501(2) 0.84594(2) -0.01676(2) 0.04793(7) Uani 1 1 d . . . . .
N1 N 0.40106(13) 0.76380(13) 0.07526(5) 0.0494(8) Uani 1 1 d . . . . .
N2 N 0.42485(12) 0.67899(13) 0.07532(5) 0.0473(7) Uani 1 1 d . . . . .
N3 N 0.43702(13) 0.84946(13) 0.02976(5) 0.0507(8) Uani 1 1 d . . . . .
H3A H 0.427135 0.870286 0.036009 0.061 Uiso 1 1 d R U . . .
N4 N 0.48140(13) 0.87891(12) 0.01846(6) 0.0496(8) Uani 1 1 d . . . . .
N5 N 0.48889(13) 0.65999(14) 0.03082(6) 0.0532(8) Uani 1 1 d . . . . .
H5A H 0.461987 0.641965 0.021608 0.064 Uiso 1 1 d R U . . .
N6 N 0.53042(13) 0.69285(14) 0.01799(6) 0.0525(8) Uani 1 1 d . . . . .
N7 N 0.55457(15) 0.96586(15) 0.05409(7) 0.0637(10) Uani 1 1 d . U . . .
N8 N 0.55237(15) 0.75370(16) 0.10745(7) 0.0639(10) Uani 1 1 d . . . . .
N9 N 0.49135(16) 0.78942(16) -0.03966(7) 0.0647(10) Uani 1 1 d . U . . .
N10 N 0.333333 0.666667 0.03567(11) 0.0605(16) Uani 1 3 d S T P . .
O1 O 0.47861(10) 0.82079(10) 0.04989(4) 0.0485(6) Uani 1 1 d . . . . .
O2 O 0.57591(11) 0.91131(11) -0.00127(5) 0.0550(7) Uani 1 1 d . . . . .
O3 O 0.65023(13) 0.98566(12) -0.02139(7) 0.0760(10) Uani 1 1 d . . . . .
O4 O 0.50207(10) 0.73075(10) 0.04896(5) 0.0504(6) Uani 1 1 d . . . . .
O5 O 0.58873(12) 0.77630(11) -0.00562(5) 0.0573(7) Uani 1 1 d . . . . .
O6 O 0.63402(12) 0.81468(11) -0.04182(5) 0.0606(8) Uani 1 1 d . . . . .
O7 O 0.61859(10) 0.86273(11) 0.01959(5) 0.0548(7) Uani 1 1 d . . . . .
O8 O 0.53208(10) 0.80834(10) 0.01395(4) 0.0462(6) Uani 1 1 d . . . . .
O9 O 0.56130(10) 0.82399(10) 0.06029(4) 0.0507(6) Uani 1 1 d . . . . .
O10 O 0.53375(13) 0.92352(12) 0.06312(5) 0.0634(8) Uani 1 1 d . . . . .
O11 O 0.55416(13) 1.00189(12) 0.06263(6) 0.0659(8) Uani 1 1 d . . . . .
O12 O 0.57142(12) 0.96835(11) 0.03522(5) 0.0581(8) Uani 1 1 d . U . . .
O13 O 0.52170(13) 0.72309(13) 0.09533(5) 0.0709(9) Uani 1 1 d . . . . .
O14 O 0.57775(14) 0.74437(15) 0.12153(7) 0.0810(10) Uani 1 1 d . . . . .
O15 O 0.56052(12) 0.79862(13) 0.10578(5) 0.0644(8) Uani 1 1 d . . . . .
O16 O 0.49885(14) 0.82617(16) -0.02954(6) 0.0784(10) Uani 1 1 d . U . . .
O17 O 0.45365(13) 0.76509(13) -0.04982(6) 0.0727(9) Uani 1 1 d . . . . .
O18 O 0.52355(13) 0.77853(12) -0.03995(5) 0.0638(8) Uani 1 1 d . . . . .
O1W O 0.63655(12) 0.93669(13) 0.05535(6) 0.0681(9) Uani 1 1 d . . . . .
H1X H 0.655793 0.930226 0.047753 0.082 Uiso 1 1 d R U . . .
H1Y H 0.637755 0.964575 0.053707 0.082 Uiso 1 1 d R U . . .
O2W O 0.50105(12) 0.84768(11) 0.09700(5) 0.0570(7) Uani 1 1 d . . . . .
H2X H 0.529720 0.861561 0.103053 0.068 Uiso 1 1 d R U . . .
H2Y H 0.500270 0.866921 0.087113 0.068 Uiso 1 1 d R U . . .
O3W O 0.45054(11) 0.74564(11) 0.11557(5) 0.0556(7) Uani 1 1 d . . . . .
H3 H 0.455140 0.720857 0.116639 0.067 Uiso 1 1 d R U . . .
H3Y H 0.474009 0.768261 0.123227 0.067 Uiso 1 1 d R U . . .
O4W O 0.64064(15) 0.82466(17) 0.06532(6) 0.0866(12) Uani 1 1 d . . . . .
H4X H 0.664354 0.820319 0.061289 0.104 Uiso 1 1 d R U . . .
H4Y H 0.621225 0.808401 0.075979 0.104 Uiso 1 1 d R U . . .
O5W O 0.59316(13) 0.72584(14) 0.05871(6) 0.0761(10) Uani 1 1 d . . . . .
H5X H 0.575700 0.726396 0.068279 0.091 Uiso 1 1 d R U . . .
H5Y H 0.623283 0.742398 0.063062 0.091 Uiso 1 1 d R U . . .
O6W O 0.66178(11) 0.79564(12) 0.02427(5) 0.0627(8) Uani 1 1 d . . . . .
H6Y H 0.656908 0.788403 0.010591 0.075 Uiso 1 1 d R U . . .
H6X H 0.676101 0.827240 0.025526 0.075 Uiso 1 1 d R U . . .
O7W O 0.67155(11) 0.91016(11) -0.02020(5) 0.0583(7) Uani 1 1 d . . . . .
H7Y H 0.672867 0.934921 -0.027174 0.070 Uiso 1 1 d R U . . .
H7X H 0.681920 0.893671 -0.027435 0.070 Uiso 1 1 d R U . . .
O8W O 0.59360(13) 0.88714(12) -0.05123(5) 0.0659(8) Uani 1 1 d . . . . .
H8X H 0.582317 0.861081 -0.059234 0.079 Uiso 1 1 d R U . . .
H8Y H 0.572109 0.895956 -0.048639 0.079 Uiso 1 1 d 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
C1 N1 1.324(5) . ?
C1 N2 1.368(5) 2_665 ?
C1 H1 0.9500 . ?
C2 C12 1.358(5) 2_665 ?
C2 N1 1.381(5) . ?
C2 C3 1.475(5) . ?
C3 O1 1.280(5) . ?
C3 N3 1.307(5) . ?
C4 N4 1.232(5) . ?
C4 C5 1.494(6) . ?
C4 H4 0.9500 . ?
C5 C10 1.428(7) . ?
C5 C6 1.450(7) . ?
C6 C7 1.340(6) . ?
C6 H6 0.9500 . ?
C7 C8 1.383(7) . ?
C7 H7 0.9500 . ?
C8 C9 1.419(7) . ?
C8 H8 0.9500 . ?
C9 C10 1.382(6) . ?
C9 O3 1.407(6) . ?
C10 O2 1.324(5) . ?
C11 O3 1.458(6) . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C12 N2 1.391(5) . ?
C12 C13 1.460(6) . ?
C13 N5 1.283(5) . ?
C13 O4 1.336(5) . ?
C14 N6 1.277(5) . ?
C14 C15 1.441(6) . ?
C14 H14 0.9500 . ?
C15 C16 1.371(6) . ?
C15 C20 1.409(6) . ?
C16 C17 1.377(7) . ?
C16 H16 0.9500 . ?
C17 C18 1.368(7) . ?
C17 H17 0.9500 . ?
C18 C19 1.424(6) . ?
C18 H18 0.9500 . ?
C19 O6 1.394(5) . ?
C19 C20 1.397(6) . ?
C20 O5 1.302(5) . ?
C21 O6 1.429(5) . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C22 N10 1.421(6) . ?
C22 C23 1.602(8) . ?
C22 H22A 0.9900 . ?
C22 H22B 0.9900 . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 H23C 0.9800 . ?
Gd1 O2 2.347(3) . ?
Gd1 O8 2.375(3) . ?
Gd1 O7 2.411(3) . ?
Gd1 O9 2.421(3) . ?
Gd1 O1 2.435(3) . ?
Gd1 O10 2.512(3) . ?
Gd1 O1W 2.503(3) . ?
Gd1 O12 2.515(3) . ?
Gd1 N4 2.556(4) . ?
Gd1 N7 2.929(4) . ?
Gd1 Gd3 3.5476(3) . ?
Gd1 Gd4 3.5789(3) . ?
Gd2 O9 2.401(3) . ?
Gd2 O3W 2.426(3) . ?
Gd2 O2W 2.438(3) . ?
Gd2 O4 2.439(3) . ?
Gd2 O1 2.455(3) . ?
Gd2 O13 2.478(4) . ?
Gd2 N2 2.529(3) . ?
Gd2 N1 2.529(3) . ?
Gd2 O15 2.614(3) . ?
Gd2 N8 2.955(4) . ?
Gd2 Gd3 4.0420(3) . ?
Gd3 O7 2.342(3) . ?
Gd3 O6W 2.362(3) . ?
Gd3 O5 2.359(3) . ?
Gd3 O8 2.380(3) . ?
Gd3 O4 2.386(3) . ?
Gd3 O9 2.434(3) . ?
Gd3 O5W 2.510(3) . ?
Gd3 N6 2.543(4) . ?
Gd3 O4W 2.608(4) . ?
Gd3 Gd4 3.6027(3) . ?
Gd3 H6Y 2.6139 . ?
Gd3 H6X 2.5875 . ?
Gd4 O5 2.328(3) . ?
Gd4 O8 2.388(3) . ?
Gd4 O2 2.385(3) . ?
Gd4 O7 2.406(3) . ?
Gd4 O8W 2.417(3) . ?
Gd4 O7W 2.429(3) . ?
Gd4 O18 2.463(3) . ?
Gd4 O16 2.554(4) . ?
Gd4 O6 2.667(3) . ?
Gd4 N9 2.903(4) . ?
N3 N4 1.400(5) . ?
N3 H3A 0.9276 . ?
N5 N6 1.418(5) . ?
N5 H5A 0.9298 . ?
N7 O11 1.243(5) . ?
N7 O10 1.268(5) . ?
N7 O12 1.257(5) . ?
N8 O13 1.209(5) . ?
N8 O15 1.293(5) . ?
N8 O14 1.297(5) . ?
N9 O17 1.203(5) . ?
N9 O18 1.207(5) . ?
N9 O16 1.216(5) . ?
O1W H1X 0.8579 . ?
O1W H1Y 0.8552 . ?
O2W H2X 0.8568 . ?
O2W H2Y 0.8608 . ?
O3W H3 0.8538 . ?
O3W H3Y 0.8598 . ?
O4W H4X 0.8501 . ?
O4W H4Y 0.8618 . ?
O5W H5X 0.8054 . ?
O5W H5Y 0.8554 . ?
O6W H6Y 0.8623 . ?
O6W H6X 0.8557 . ?
O7W H7Y 0.8639 . ?
O7W H7X 0.8541 . ?
O8W H8X 0.8582 . ?
O8W H8Y 0.8547 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 C1 N2 114.4(3) . 2_665 ?
N1 C1 H1 122.8 . . ?
N2 C1 H1 122.8 2_665 . ?
C12 C2 N1 108.5(3) 2_665 . ?
C12 C2 C3 135.1(4) 2_665 . ?
N1 C2 C3 116.3(3) . . ?
O1 C3 N3 122.6(4) . . ?
O1 C3 C2 116.8(3) . . ?
N3 C3 C2 120.7(4) . . ?
N4 C4 C5 127.5(4) . . ?
N4 C4 H4 116.3 . . ?
C5 C4 H4 116.3 . . ?
C10 C5 C6 119.3(4) . . ?
C10 C5 C4 121.8(4) . . ?
C6 C5 C4 118.9(4) . . ?
C7 C6 C5 122.7(4) . . ?
C7 C6 H6 118.6 . . ?
C5 C6 H6 118.6 . . ?
C6 C7 C8 117.9(5) . . ?
C6 C7 H7 121.0 . . ?
C8 C7 H7 121.0 . . ?
C7 C8 C9 121.5(4) . . ?
C7 C8 H8 119.2 . . ?
C9 C8 H8 119.2 . . ?
C10 C9 O3 112.9(4) . . ?
C10 C9 C8 122.0(5) . . ?
O3 C9 C8 125.0(4) . . ?
O2 C10 C9 121.1(5) . . ?
O2 C10 C5 122.4(4) . . ?
C9 C10 C5 116.5(4) . . ?
O3 C11 H11A 109.5 . . ?
O3 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
O3 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
C2 C12 N2 109.6(4) 3_565 . ?
C2 C12 C13 133.9(4) 3_565 . ?
N2 C12 C13 116.4(3) . . ?
N5 C13 O4 124.0(4) . . ?
N5 C13 C12 120.1(4) . . ?
O4 C13 C12 116.0(3) . . ?
N6 C14 C15 125.7(4) . . ?
N6 C14 H14 117.1 . . ?
C15 C14 H14 117.1 . . ?
C16 C15 C20 119.4(4) . . ?
C16 C15 C14 120.1(4) . . ?
C20 C15 C14 120.2(4) . . ?
C17 C16 C15 122.6(4) . . ?
C17 C16 H16 118.7 . . ?
C15 C16 H16 118.7 . . ?
C16 C17 C18 121.2(5) . . ?
C16 C17 H17 119.4 . . ?
C18 C17 H17 119.4 . . ?
C17 C18 C19 116.0(4) . . ?
C17 C18 H18 122.0 . . ?
C19 C18 H18 122.0 . . ?
O6 C19 C20 113.2(3) . . ?
O6 C19 C18 122.5(4) . . ?
C20 C19 C18 124.0(4) . . ?
O5 C20 C19 118.8(4) . . ?
O5 C20 C15 124.6(4) . . ?
C19 C20 C15 116.6(4) . . ?
O6 C21 H21A 109.5 . . ?
O6 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
O6 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
N10 C22 C23 142.2(6) . . ?
N10 C22 H22A 101.4 . . ?
C23 C22 H22A 101.4 . . ?
N10 C22 H22B 101.4 . . ?
C23 C22 H22B 101.4 . . ?
H22A C22 H22B 104.6 . . ?
C22 C23 H23A 109.5 . . ?
C22 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
C22 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
O2 Gd1 O8 76.89(10) . . ?
O2 Gd1 O7 71.26(11) . . ?
O8 Gd1 O7 59.66(9) . . ?
O2 Gd1 O9 144.39(10) . . ?
O8 Gd1 O9 75.91(9) . . ?
O7 Gd1 O9 75.31(10) . . ?
O2 Gd1 O1 127.64(10) . . ?
O8 Gd1 O1 74.21(9) . . ?
O7 Gd1 O1 124.74(10) . . ?
O9 Gd1 O1 64.83(9) . . ?
O2 Gd1 O10 121.39(11) . . ?
O8 Gd1 O10 145.17(10) . . ?
O7 Gd1 O10 150.36(11) . . ?
O9 Gd1 O10 93.89(10) . . ?
O1 Gd1 O10 71.36(10) . . ?
O2 Gd1 O1W 104.69(11) . . ?
O8 Gd1 O1W 132.71(10) . . ?
O7 Gd1 O1W 75.85(11) . . ?
O9 Gd1 O1W 78.21(10) . . ?
O1 Gd1 O1W 126.99(10) . . ?
O10 Gd1 O1W 74.93(11) . . ?
O2 Gd1 O12 73.21(10) . . ?
O8 Gd1 O12 146.06(10) . . ?
O7 Gd1 O12 122.64(10) . . ?
O9 Gd1 O12 137.82(10) . . ?
O1 Gd1 O12 112.59(10) . . ?
O10 Gd1 O12 50.58(10) . . ?
O1W Gd1 O12 71.49(11) . . ?
O2 Gd1 N4 71.12(11) . . ?
O8 Gd1 N4 83.68(10) . . ?
O7 Gd1 N4 132.09(11) . . ?
O9 Gd1 N4 127.44(10) . . ?
O1 Gd1 N4 63.12(10) . . ?
O10 Gd1 N4 76.37(11) . . ?
O1W Gd1 N4 142.56(11) . . ?
O12 Gd1 N4 71.80(11) . . ?
O2 Gd1 N7 97.89(11) . . ?
O8 Gd1 N7 158.04(11) . . ?
O7 Gd1 N7 139.37(11) . . ?
O9 Gd1 N7 115.64(11) . . ?
O1 Gd1 N7 93.36(11) . . ?
O10 Gd1 N7 25.50(11) . . ?
O1W Gd1 N7 69.22(11) . . ?
O12 Gd1 N7 25.25(10) . . ?
N4 Gd1 N7 74.50(11) . . ?
O2 Gd1 Gd3 101.54(7) . . ?
O8 Gd1 Gd3 41.81(7) . . ?
O7 Gd1 Gd3 40.98(7) . . ?
O9 Gd1 Gd3 43.21(7) . . ?
O1 Gd1 Gd3 84.45(7) . . ?
O10 Gd1 Gd3 137.04(8) . . ?
O1W Gd1 Gd3 93.88(8) . . ?
O12 Gd1 Gd3 161.99(7) . . ?
N4 Gd1 Gd3 123.55(8) . . ?
N7 Gd1 Gd3 157.03(8) . . ?
O2 Gd1 Gd4 41.27(7) . . ?
O8 Gd1 Gd4 41.41(6) . . ?
O7 Gd1 Gd4 41.96(7) . . ?
O9 Gd1 Gd4 103.94(7) . . ?
O1 Gd1 Gd4 113.51(6) . . ?
O10 Gd1 Gd4 161.93(8) . . ?
O1W Gd1 Gd4 111.27(8) . . ?
O12 Gd1 Gd4 113.96(7) . . ?
N4 Gd1 Gd4 90.20(8) . . ?
N7 Gd1 Gd4 139.03(9) . . ?
Gd3 Gd1 Gd4 60.732(6) . . ?
O9 Gd2 O3W 142.58(10) . . ?
O9 Gd2 O2W 84.08(10) . . ?
O3W Gd2 O2W 75.41(10) . . ?
O9 Gd2 O4 65.96(9) . . ?
O3W Gd2 O4 135.09(10) . . ?
O2W Gd2 O4 148.38(10) . . ?
O9 Gd2 O1 64.81(9) . . ?
O3W Gd2 O1 135.54(10) . . ?
O2W Gd2 O1 75.39(9) . . ?
O4 Gd2 O1 82.54(10) . . ?
O9 Gd2 O13 91.00(11) . . ?
O3W Gd2 O13 72.86(12) . . ?
O2W Gd2 O13 118.88(11) . . ?
O4 Gd2 O13 73.51(11) . . ?
O1 Gd2 O13 151.53(11) . . ?
O9 Gd2 N2 130.53(10) . . ?
O3W Gd2 N2 76.29(10) . . ?
O2W Gd2 N2 145.24(11) . . ?
O4 Gd2 N2 64.86(10) . . ?
O1 Gd2 N2 113.13(10) . . ?
O13 Gd2 N2 70.37(11) . . ?
O9 Gd2 N1 129.27(11) . . ?
O3W Gd2 N1 77.70(11) . . ?
O2W Gd2 N1 79.72(11) . . ?
O4 Gd2 N1 110.94(10) . . ?
O1 Gd2 N1 64.64(10) . . ?
O13 Gd2 N1 138.59(12) . . ?
N2 Gd2 N1 74.87(11) . . ?
O9 Gd2 O15 70.40(10) . . ?
O3W Gd2 O15 73.61(10) . . ?
O2W Gd2 O15 72.11(11) . . ?
O4 Gd2 O15 104.93(10) . . ?
O1 Gd2 O15 126.39(10) . . ?
O13 Gd2 O15 49.45(11) . . ?
N2 Gd2 O15 118.01(11) . . ?
N1 Gd2 O15 143.81(10) . . ?
O9 Gd2 N8 82.38(10) . . ?
O3W Gd2 N8 69.29(11) . . ?
O2W Gd2 N8 95.93(11) . . ?
O4 Gd2 N8 90.11(11) . . ?
O1 Gd2 N8 146.57(10) . . ?
O13 Gd2 N8 23.69(11) . . ?
N2 Gd2 N8 92.56(11) . . ?
N1 Gd2 N8 146.67(11) . . ?
O15 Gd2 N8 25.93(11) . . ?
O9 Gd2 Gd3 33.55(7) . . ?
O3W Gd2 Gd3 150.37(8) . . ?
O2W Gd2 Gd3 117.51(7) . . ?
O4 Gd2 Gd3 32.68(6) . . ?
O1 Gd2 Gd3 73.84(6) . . ?
O13 Gd2 Gd3 77.69(9) . . ?
N2 Gd2 Gd3 96.98(7) . . ?
N1 Gd2 Gd3 129.05(7) . . ?
O15 Gd2 Gd3 84.91(7) . . ?
N8 Gd2 Gd3 82.43(8) . . ?
O7 Gd3 O6W 79.49(11) . . ?
O7 Gd3 O5 73.89(10) . . ?
O6W Gd3 O5 71.03(11) . . ?
O7 Gd3 O8 60.55(10) . . ?
O6W Gd3 O8 129.68(10) . . ?
O5 Gd3 O8 69.48(10) . . ?
O7 Gd3 O4 129.95(10) . . ?
O6W Gd3 O4 149.85(11) . . ?
O5 Gd3 O4 118.70(10) . . ?
O8 Gd3 O4 78.31(10) . . ?
O7 Gd3 O9 76.31(10) . . ?
O6W Gd3 O9 125.50(10) . . ?
O5 Gd3 O9 141.99(10) . . ?
O8 Gd3 O9 75.55(9) . . ?
O4 Gd3 O9 66.27(9) . . ?
O7 Gd3 O5W 142.78(12) . . ?
O6W Gd3 O5W 76.45(11) . . ?
O5 Gd3 O5W 122.76(12) . . ?
O8 Gd3 O5W 152.96(10) . . ?
O4 Gd3 O5W 74.74(11) . . ?
O9 Gd3 O5W 95.21(11) . . ?
O7 Gd3 N6 139.10(11) . . ?
O6W Gd3 N6 99.35(11) . . ?
O5 Gd3 N6 67.37(10) . . ?
O8 Gd3 N6 93.07(10) . . ?
O4 Gd3 N6 63.86(10) . . ?
O9 Gd3 N6 130.12(10) . . ?
O5W Gd3 N6 73.29(12) . . ?
O7 Gd3 O4W 81.83(13) . . ?
O6W Gd3 O4W 70.06(12) . . ?
O5 Gd3 O4W 137.06(12) . . ?
O8 Gd3 O4W 126.61(11) . . ?
O4 Gd3 O4W 104.09(12) . . ?
O9 Gd3 O4W 58.71(11) . . ?
O5W Gd3 O4W 63.47(14) . . ?
N6 Gd3 O4W 136.73(13) . . ?
O7 Gd3 Gd1 42.47(7) . . ?
O6W Gd3 Gd1 119.90(8) . . ?
O5 Gd3 Gd1 99.30(7) . . ?
O8 Gd3 Gd1 41.69(6) . . ?
O4 Gd3 Gd1 87.95(7) . . ?
O9 Gd3 Gd1 42.91(7) . . ?
O5W Gd3 Gd1 137.87(9) . . ?
N6 Gd3 Gd1 132.39(8) . . ?
O4W Gd3 Gd1 84.93(10) . . ?
O7 Gd3 Gd4 41.31(8) . . ?
O6W Gd3 Gd4 88.85(8) . . ?
O5 Gd3 Gd4 39.46(7) . . ?
O8 Gd3 Gd4 40.99(6) . . ?
O4 Gd3 Gd4 117.08(7) . . ?
O9 Gd3 Gd4 102.97(7) . . ?
O5W Gd3 Gd4 161.16(9) . . ?
N6 Gd3 Gd4 98.05(8) . . ?
O4W Gd3 Gd4 122.65(10) . . ?
Gd1 Gd3 Gd4 60.064(6) . . ?
O7 Gd3 Gd2 105.59(7) . . ?
O6W Gd3 Gd2 146.77(8) . . ?
O5 Gd3 Gd2 142.20(8) . . ?
O8 Gd3 Gd2 77.53(6) . . ?
O4 Gd3 Gd2 33.51(6) . . ?
O9 Gd3 Gd2 33.03(6) . . ?
O5W Gd3 Gd2 81.14(8) . . ?
N6 Gd3 Gd2 97.29(7) . . ?
O4W Gd3 Gd2 78.09(9) . . ?
Gd1 Gd3 Gd2 64.783(5) . . ?
Gd4 Gd3 Gd2 117.003(7) . . ?
O7 Gd3 H6Y 78.2 . . ?
O6W Gd3 H6Y 19.1 . . ?
O5 Gd3 H6Y 52.1 . . ?
O8 Gd3 H6Y 115.8 . . ?
O4 Gd3 H6Y 149.8 . . ?
O9 Gd3 H6Y 141.0 . . ?
O5W Gd3 H6Y 87.6 . . ?
N6 Gd3 H6Y 87.9 . . ?
O4W Gd3 H6Y 88.9 . . ?
Gd1 Gd3 H6Y 120.7 . . ?
Gd4 Gd3 H6Y 75.3 . . ?
Gd2 Gd3 H6Y 165.6 . . ?
O7 Gd3 H6X 62.2 . . ?
O6W Gd3 H6X 19.2 . . ?
O5 Gd3 H6X 75.7 . . ?
O8 Gd3 H6X 118.7 . . ?
O4 Gd3 H6X 161.9 . . ?
O9 Gd3 H6X 110.1 . . ?
O5W Gd3 H6X 88.3 . . ?
N6 Gd3 H6X 117.7 . . ?
O4W Gd3 H6X 61.7 . . ?
Gd1 Gd3 H6X 101.0 . . ?
Gd4 Gd3 H6X 80.9 . . ?
Gd2 Gd3 H6X 138.7 . . ?
H6Y Gd3 H6X 31.0 . . ?
O5 Gd4 O8 69.86(10) . . ?
O5 Gd4 O2 139.29(10) . . ?
O8 Gd4 O2 75.91(9) . . ?
O5 Gd4 O7 73.26(10) . . ?
O8 Gd4 O7 59.56(9) . . ?
O2 Gd4 O7 70.70(10) . . ?
O5 Gd4 O8W 134.92(11) . . ?
O8 Gd4 O8W 144.71(11) . . ?
O2 Gd4 O8W 85.72(11) . . ?
O7 Gd4 O8W 140.77(11) . . ?
O5 Gd4 O7W 103.90(11) . . ?
O8 Gd4 O7W 132.86(10) . . ?
O2 Gd4 O7W 83.61(10) . . ?
O7 Gd4 O7W 73.72(10) . . ?
O8W Gd4 O7W 72.84(11) . . ?
O5 Gd4 O18 75.88(11) . . ?
O8 Gd4 O18 89.26(10) . . ?
O2 Gd4 O18 125.68(11) . . ?
O7 Gd4 O18 141.99(10) . . ?
O8W Gd4 O18 77.24(11) . . ?
O7W Gd4 O18 135.98(11) . . ?
O5 Gd4 O16 113.58(12) . . ?
O8 Gd4 O16 74.97(11) . . ?
O2 Gd4 O16 76.72(12) . . ?
O7 Gd4 O16 128.74(11) . . ?
O8W Gd4 O16 71.57(12) . . ?
O7W Gd4 O16 140.27(12) . . ?
O18 Gd4 O16 48.97(12) . . ?
O5 Gd4 O6 61.75(10) . . ?
O8 Gd4 O6 130.98(9) . . ?
O2 Gd4 O6 150.83(9) . . ?
O7 Gd4 O6 110.36(10) . . ?
O8W Gd4 O6 75.96(11) . . ?
O7W Gd4 O6 69.48(10) . . ?
O18 Gd4 O6 72.46(11) . . ?
O16 Gd4 O6 117.22(12) . . ?
O5 Gd4 N9 94.59(12) . . ?
O8 Gd4 N9 81.24(11) . . ?
O2 Gd4 N9 101.43(12) . . ?
O7 Gd4 N9 140.80(11) . . ?
O8W Gd4 N9 73.10(12) . . ?
O7W Gd4 N9 145.05(11) . . ?
O18 Gd4 N9 24.26(11) . . ?
O16 Gd4 N9 24.71(12) . . ?
O6 Gd4 N9 94.81(12) . . ?
O5 Gd4 Gd1 99.06(7) . . ?
O8 Gd4 Gd1 41.14(6) . . ?
O2 Gd4 Gd1 40.46(7) . . ?
O7 Gd4 Gd1 42.07(7) . . ?
O8W Gd4 Gd1 126.01(8) . . ?
O7W Gd4 Gd1 98.83(7) . . ?
O18 Gd4 Gd1 124.96(8) . . ?
O16 Gd4 Gd1 88.18(9) . . ?
O6 Gd4 Gd1 152.21(8) . . ?
N9 Gd4 Gd1 107.32(9) . . ?
O5 Gd4 Gd3 40.08(7) . . ?
O8 Gd4 Gd3 40.84(7) . . ?
O2 Gd4 Gd3 99.21(7) . . ?
O7 Gd4 Gd3 39.98(7) . . ?
O8W Gd4 Gd3 174.01(8) . . ?
O7W Gd4 Gd3 104.19(7) . . ?
O18 Gd4 Gd3 102.31(8) . . ?
O16 Gd4 Gd3 112.75(9) . . ?
O6 Gd4 Gd3 98.17(7) . . ?
N9 Gd4 Gd3 108.97(9) . . ?
Gd1 Gd4 Gd3 59.203(6) . . ?
C1 N1 C2 104.8(3) . . ?
C1 N1 Gd2 137.3(3) . . ?
C2 N1 Gd2 117.9(3) . . ?
C1 N2 C12 102.5(3) 3_565 . ?
C1 N2 Gd2 139.1(3) 3_565 . ?
C12 N2 Gd2 118.5(2) . . ?
C3 N3 N4 115.9(3) . . ?
C3 N3 H3A 107.3 . . ?
N4 N3 H3A 108.1 . . ?
C4 N4 N3 114.9(4) . . ?
C4 N4 Gd1 129.1(3) . . ?
N3 N4 Gd1 115.5(2) . . ?
C13 N5 N6 113.8(4) . . ?
C13 N5 H5A 108.6 . . ?
N6 N5 H5A 108.5 . . ?
C14 N6 N5 113.6(4) . . ?
C14 N6 Gd3 129.5(3) . . ?
N5 N6 Gd3 115.8(2) . . ?
O11 N7 O10 121.5(4) . . ?
O11 N7 O12 121.6(4) . . ?
O10 N7 O12 116.6(4) . . ?
O11 N7 Gd1 178.2(3) . . ?
O10 N7 Gd1 58.5(2) . . ?
O12 N7 Gd1 58.6(2) . . ?
O13 N8 O15 117.0(4) . . ?
O13 N8 O14 124.2(4) . . ?
O15 N8 O14 118.8(4) . . ?
O13 N8 Gd2 55.5(2) . . ?
O15 N8 Gd2 62.1(2) . . ?
O14 N8 Gd2 173.3(3) . . ?
O17 N9 O18 120.0(4) . . ?
O17 N9 O16 121.6(5) . . ?
O18 N9 O16 118.4(4) . . ?
O17 N9 Gd4 176.8(4) . . ?
O18 N9 Gd4 57.0(2) . . ?
O16 N9 Gd4 61.4(2) . . ?
C22 N10 C22 112.6(3) . 3_565 ?
C22 N10 C22 112.6(3) . 2_665 ?
C22 N10 C22 112.6(3) 3_565 2_665 ?
C3 O1 Gd1 121.1(2) . . ?
C3 O1 Gd2 124.3(2) . . ?
Gd1 O1 Gd2 113.42(11) . . ?
C10 O2 Gd1 128.8(3) . . ?
C10 O2 Gd4 129.8(3) . . ?
Gd1 O2 Gd4 98.27(11) . . ?
C9 O3 C11 123.1(4) . . ?
C13 O4 Gd3 120.1(2) . . ?
C13 O4 Gd2 124.0(2) . . ?
Gd3 O4 Gd2 113.80(11) . . ?
C20 O5 Gd4 124.6(3) . . ?
C20 O5 Gd3 134.9(3) . . ?
Gd4 O5 Gd3 100.46(10) . . ?
C19 O6 C21 116.7(3) . . ?
C19 O6 Gd4 113.3(2) . . ?
C21 O6 Gd4 129.4(3) . . ?
Gd3 O7 Gd4 98.71(10) . . ?
Gd3 O7 Gd1 96.55(10) . . ?
Gd4 O7 Gd1 95.97(11) . . ?
Gd3 O8 Gd4 98.16(9) . . ?
Gd3 O8 Gd1 96.50(10) . . ?
Gd4 O8 Gd1 97.44(10) . . ?
Gd2 O9 Gd1 115.90(12) . . ?
Gd2 O9 Gd3 113.42(11) . . ?
Gd1 O9 Gd3 93.89(9) . . ?
N7 O10 Gd1 96.0(3) . . ?
N7 O12 Gd1 96.1(2) . . ?
N8 O13 Gd2 100.8(3) . . ?
N8 O15 Gd2 91.9(2) . . ?
N9 O16 Gd4 93.9(3) . . ?
N9 O18 Gd4 98.8(3) . . ?
Gd1 O1W H1X 96.8 . . ?
Gd1 O1W H1Y 99.6 . . ?
H1X O1W H1Y 119.4 . . ?
Gd2 O2W H2X 109.6 . . ?
Gd2 O2W H2Y 107.8 . . ?
H2X O2W H2Y 109.8 . . ?
Gd2 O3W H3 96.6 . . ?
Gd2 O3W H3Y 100.6 . . ?
H3 O3W H3Y 104.5 . . ?
Gd3 O4W H4X 97.8 . . ?
Gd3 O4W H4Y 100.1 . . ?
H4X O4W H4Y 122.4 . . ?
Gd3 O5W H5X 97.0 . . ?
Gd3 O5W H5Y 106.2 . . ?
H5X O5W H5Y 107.9 . . ?
Gd3 O6W H6Y 97.2 . . ?
Gd3 O6W H6X 95.5 . . ?
H6Y O6W H6X 108.1 . . ?
Gd4 O7W H7Y 108.4 . . ?
Gd4 O7W H7X 98.5 . . ?
H7Y O7W H7X 114.4 . . ?
Gd4 O8W H8X 96.6 . . ?
Gd4 O8W H8Y 96.3 . . ?
H8X O8W H8Y 113.2 . . ?

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
C12 C2 C3 O1 -178.6(4) 2_665 . . . ?
N1 C2 C3 O1 2.6(5) . . . . ?
C12 C2 C3 N3 1.5(7) 2_665 . . . ?
N1 C2 C3 N3 -177.3(3) . . . . ?
N4 C4 C5 C10 13.2(8) . . . . ?
N4 C4 C5 C6 -163.2(5) . . . . ?
C10 C5 C6 C7 -2.7(7) . . . . ?
C4 C5 C6 C7 173.8(4) . . . . ?
C5 C6 C7 C8 0.8(7) . . . . ?
C6 C7 C8 C9 0.4(8) . . . . ?
C7 C8 C9 C10 0.5(8) . . . . ?
C7 C8 C9 O3 -179.1(5) . . . . ?
O3 C9 C10 O2 -4.8(7) . . . . ?
C8 C9 C10 O2 175.6(4) . . . . ?
O3 C9 C10 C5 177.3(4) . . . . ?
C8 C9 C10 C5 -2.3(7) . . . . ?
C6 C5 C10 O2 -174.6(4) . . . . ?
C4 C5 C10 O2 9.0(7) . . . . ?
C6 C5 C10 C9 3.4(7) . . . . ?
C4 C5 C10 C9 -173.0(4) . . . . ?
C2 C12 C13 N5 -10.0(7) 3_565 . . . ?
N2 C12 C13 N5 174.2(4) . . . . ?
C2 C12 C13 O4 171.4(4) 3_565 . . . ?
N2 C12 C13 O4 -4.5(5) . . . . ?
N6 C14 C15 C16 177.1(4) . . . . ?
N6 C14 C15 C20 -9.2(7) . . . . ?
C20 C15 C16 C17 -4.8(7) . . . . ?
C14 C15 C16 C17 169.0(5) . . . . ?
C15 C16 C17 C18 4.9(9) . . . . ?
C16 C17 C18 C19 -3.0(8) . . . . ?
C17 C18 C19 O6 -173.0(5) . . . . ?
C17 C18 C19 C20 1.2(7) . . . . ?
O6 C19 C20 O5 -6.3(6) . . . . ?
C18 C19 C20 O5 179.0(4) . . . . ?
O6 C19 C20 C15 173.6(4) . . . . ?
C18 C19 C20 C15 -1.2(7) . . . . ?
C16 C15 C20 O5 -177.4(5) . . . . ?
C14 C15 C20 O5 8.9(7) . . . . ?
C16 C15 C20 C19 2.8(7) . . . . ?
C14 C15 C20 C19 -171.0(4) . . . . ?
N2 C1 N1 C2 4.4(4) 2_665 . . . ?
N2 C1 N1 Gd2 -175.1(3) 2_665 . . . ?
C12 C2 N1 C1 -1.6(4) 2_665 . . . ?
C3 C2 N1 C1 177.5(3) . . . . ?
C12 C2 N1 Gd2 178.0(2) 2_665 . . . ?
C3 C2 N1 Gd2 -2.9(4) . . . . ?
C2 C12 N2 C1 3.9(4) 3_565 . . 3_565 ?
C13 C12 N2 C1 -179.3(3) . . . 3_565 ?
C2 C12 N2 Gd2 -176.6(2) 3_565 . . . ?
C13 C12 N2 Gd2 0.2(4) . . . . ?
O1 C3 N3 N4 -1.1(6) . . . . ?
C2 C3 N3 N4 178.8(3) . . . . ?
C5 C4 N4 N3 176.0(4) . . . . ?
C5 C4 N4 Gd1 4.6(7) . . . . ?
C3 N3 N4 C4 178.3(4) . . . . ?
C3 N3 N4 Gd1 -9.1(4) . . . . ?
O4 C13 N5 N6 -4.5(6) . . . . ?
C12 C13 N5 N6 176.9(3) . . . . ?
C15 C14 N6 N5 167.8(4) . . . . ?
C15 C14 N6 Gd3 -25.2(7) . . . . ?
C13 N5 N6 C14 -176.4(4) . . . . ?
C13 N5 N6 Gd3 14.7(4) . . . . ?
C23 C22 N10 C22 44.6(10) . . . 3_565 ?
C23 C22 N10 C22 -83.9(7) . . . 2_665 ?
N3 C3 O1 Gd1 11.8(5) . . . . ?
C2 C3 O1 Gd1 -168.1(2) . . . . ?
N3 C3 O1 Gd2 178.8(3) . . . . ?
C2 C3 O1 Gd2 -1.1(5) . . . . ?
C9 C10 O2 Gd1 130.8(4) . . . . ?
C5 C10 O2 Gd1 -51.3(6) . . . . ?
C9 C10 O2 Gd4 -73.8(6) . . . . ?
C5 C10 O2 Gd4 104.1(5) . . . . ?
C10 C9 O3 C11 -170.5(4) . . . . ?
C8 C9 O3 C11 9.1(8) . . . . ?
N5 C13 O4 Gd3 -9.1(5) . . . . ?
C12 C13 O4 Gd3 169.6(2) . . . . ?
N5 C13 O4 Gd2 -171.5(3) . . . . ?
C12 C13 O4 Gd2 7.2(5) . . . . ?
C19 C20 O5 Gd4 30.4(6) . . . . ?
C15 C20 O5 Gd4 -149.4(4) . . . . ?
C19 C20 O5 Gd3 -148.7(3) . . . . ?
C15 C20 O5 Gd3 31.5(7) . . . . ?
C20 C19 O6 C21 173.6(4) . . . . ?
C18 C19 O6 C21 -11.6(6) . . . . ?
C20 C19 O6 Gd4 -14.8(5) . . . . ?
C18 C19 O6 Gd4 160.1(4) . . . . ?
O11 N7 O10 Gd1 -177.8(4) . . . . ?
O12 N7 O10 Gd1 8.7(4) . . . . ?
O11 N7 O12 Gd1 177.9(4) . . . . ?
O10 N7 O12 Gd1 -8.7(4) . . . . ?
O15 N8 O13 Gd2 -9.4(4) . . . . ?
O14 N8 O13 Gd2 171.9(4) . . . . ?
O13 N8 O15 Gd2 8.8(4) . . . . ?
O14 N8 O15 Gd2 -172.4(4) . . . . ?
O17 N9 O16 Gd4 -178.5(4) . . . . ?
O18 N9 O16 Gd4 -1.0(5) . . . . ?
O17 N9 O18 Gd4 178.6(4) . . . . ?
O16 N9 O18 Gd4 1.0(5) . . . . ?

_refine_diff_density_max         0.851
_refine_diff_density_min         -0.750
_refine_diff_density_rms         0.078



