# Electronic Supplementary Material (ESI) for New Journal of Chemistry.
# This journal is © The Royal Society of Chemistry and the Centre National de la Recherche Scientifique 2018

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

data_t
_database_code_depnum_ccdc_archive 'CCDC 1428655'
_audit_update_record             
;
2018-12-10 deposited with the CCDC.
2018-12-11 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C90 H100 Gd8 N16 O50'
_chemical_formula_weight         3463.85

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'
Gd Gd -0.1653 3.9035 '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      tetragonal
_space_group_IT_number           82
_space_group_name_H-M_alt        'I -4'
_space_group_name_Hall           'I -4'

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

_cell_length_a                   18.970(3)
_cell_length_b                   18.970(3)
_cell_length_c                   18.214(4)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     6555(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       ?
_exptl_crystal_colour            ?
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.755
_exptl_crystal_F_000             3328
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          ?
_exptl_crystal_size_mid          ?
_exptl_crystal_size_min          ?
_exptl_absorpt_coefficient_mu    4.072
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  ?
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            26736
_diffrn_reflns_av_unetI/netI     0.0360
_diffrn_reflns_av_R_equivalents  0.0449
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         2.147
_diffrn_reflns_theta_max         24.998
_diffrn_reflns_theta_full        24.998
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             5789
_reflns_number_gt                5447
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.932
_reflns_Friedel_fraction_max     1.000
_reflns_Friedel_fraction_full    1.000

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          
;
 Refined as a 2-component inversion twin.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0716P)²+1.5413P] 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     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_extinction_coef       0.00147(13)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_abs_structure_details 
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.50(3)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         5789
_refine_ls_number_parameters     378
_refine_ls_number_restraints     6
_refine_ls_R_factor_all          0.0447
_refine_ls_R_factor_gt           0.0422
_refine_ls_wR_factor_ref         0.1080
_refine_ls_wR_factor_gt          0.1056
_refine_ls_goodness_of_fit_ref   1.078
_refine_ls_restrained_S_all      1.078
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Gd1 Gd 0.40427(3) 0.40246(3) 0.72321(3) 0.0469(2) Uani 1 1 d . . . . .
Gd2 Gd 0.43150(3) 0.56848(3) 0.62747(3) 0.0404(2) Uani 1 1 d . . . . .
O1 O 0.3232(4) 0.6372(4) 0.6493(4) 0.0410(19) Uani 1 1 d . . . . .
O2 O 0.3495(4) 0.5129(4) 0.7074(4) 0.0346(17) Uani 1 1 d . . . . .
O3 O 0.3973(5) 0.3071(5) 0.8063(5) 0.049(2) Uani 1 1 d . . . . .
O4 O 0.3618(5) 0.2629(5) 0.9133(5) 0.058(2) Uani 1 1 d . . . . .
O5 O 0.3826(5) 0.6511(7) 0.8142(7) 0.078(4) Uani 1 1 d . . . . .
O6 O 0.4811(4) 0.6422(4) 0.7138(5) 0.045(2) Uani 1 1 d . . . . .
O7 O 0.6989(4) 0.6278(5) 0.6496(5) 0.046(2) Uani 1 1 d . . . . .
O8 O 0.7545(7) 0.6963(7) 0.5634(6) 0.076(3) Uani 1 1 d . . . . .
O9 O 0.4465(4) 0.4457(4) 0.6072(4) 0.0327(15) Uani 1 1 d . . . . .
O10 O 0.4563(4) 0.6649(4) 0.5481(4) 0.0411(19) Uani 1 1 d . . . . .
O11 O 0.5461(4) 0.6306(4) 0.4797(4) 0.0376(17) Uani 1 1 d . . . . .
O12 O 0.5000 0.5000 0.7223(6) 0.032(2) Uani 1 2 d S T P . .
O13 O 0.4553(4) 0.4601(5) 0.8291(4) 0.0427(19) Uani 1 1 d . . . . .
N1 N 0.3054(5) 0.4079(5) 0.8147(6) 0.039(2) Uani 1 1 d . . . . .
N2 N 0.3059(6) 0.3566(6) 0.8695(6) 0.049(2) Uani 1 1 d . . . . .
H2 H 0.2765 0.3552 0.9054 0.059 Uiso 1 1 calc R U . . .
N3 N 0.5927(7) 0.7158(6) 0.6502(7) 0.055(3) Uani 1 1 d . . . . .
N4 N 0.6500(8) 0.7284(6) 0.6039(7) 0.066(4) Uani 1 1 d . . . . .
H4 H 0.6519 0.7637 0.5743 0.079 Uiso 1 1 calc R U . . .
C1 C 0.3092(7) 0.7067(6) 0.6178(8) 0.051(3) Uani 1 1 d . . . . .
H1A H 0.2703 0.7035 0.5842 0.077 Uiso 1 1 calc R U . . .
H1B H 0.3503 0.7229 0.5921 0.077 Uiso 1 1 calc R U . . .
H1C H 0.2978 0.7392 0.6564 0.077 Uiso 1 1 calc R U . . .
C2 C 0.2699(7) 0.6084(7) 0.6929(7) 0.046(3) Uani 1 1 d . . . . .
C3 C 0.2053(7) 0.6395(8) 0.7044(8) 0.054(3) Uani 1 1 d . . . . .
H3 H 0.1945 0.6816 0.6808 0.065 Uiso 1 1 calc R U . . .
C4 C 0.1564(7) 0.6090(8) 0.7507(10) 0.068(5) Uani 1 1 d . . . . .
H4A H 0.1127 0.6301 0.7583 0.081 Uiso 1 1 calc R U . . .
C5 C 0.1731(7) 0.5473(8) 0.7852(8) 0.059(4) Uani 1 1 d . . . . .
H5 H 0.1402 0.5270 0.8166 0.071 Uiso 1 1 calc R U . . .
C6 C 0.2396(7) 0.5126(7) 0.7748(7) 0.045(3) Uani 1 1 d . . . . .
C7 C 0.2865(6) 0.5424(6) 0.7252(6) 0.034(2) Uani 1 1 d . . . . .
C8 C 0.2521(6) 0.4496(7) 0.8202(6) 0.041(3) Uani 1 1 d . . . . .
H8 H 0.2187 0.4390 0.8559 0.049 Uiso 1 1 calc R U . . .
C9 C 0.3576(7) 0.3102(7) 0.8594(7) 0.052(3) Uani 1 1 d . . . . .
C10 C 0.4157(11) 0.2085(11) 0.9064(12) 0.099(8) Uani 1 1 d . . . . .
H10A H 0.4132 0.1879 0.8584 0.148 Uiso 1 1 calc R U . . .
H10B H 0.4078 0.1727 0.9428 0.148 Uiso 1 1 calc R U . . .
H10C H 0.4614 0.2291 0.9136 0.148 Uiso 1 1 calc R U . . .
C11 C 0.3269(10) 0.6556(16) 0.8648(12) 0.117(9) Uani 1 1 d . . . . .
H11A H 0.3353 0.6941 0.8978 0.176 Uiso 1 1 calc R U . . .
H11B H 0.3239 0.6124 0.8921 0.176 Uiso 1 1 calc R U . . .
H11C H 0.2835 0.6633 0.8389 0.176 Uiso 1 1 calc R U . . .
C12 C 0.4038(9) 0.7119(11) 0.7849(13) 0.087(7) Uani 1 1 d . . . . .
C13 C 0.3748(11) 0.7795(13) 0.8030(16) 0.118(10) Uani 1 1 d . . . . .
H13 H 0.3408 0.7842 0.8394 0.142 Uiso 1 1 calc R U . . .
C14 C 0.3995(13) 0.8386(11) 0.7639(17) 0.115(8) Uani 1 1 d . U . . .
H14 H 0.3778 0.8822 0.7696 0.138 Uiso 1 1 calc R U . . .
C15 C 0.4546(11) 0.8315(9) 0.7183(13) 0.095(6) Uani 1 1 d . U . . .
H15 H 0.4726 0.8722 0.6970 0.114 Uiso 1 1 calc R U . . .
C16 C 0.4867(10) 0.7683(8) 0.7005(10) 0.071(5) Uani 1 1 d . . . . .
C17 C 0.4593(7) 0.7090(7) 0.7306(9) 0.055(4) Uani 1 1 d . . . . .
C18 C 0.5499(10) 0.7671(8) 0.6534(9) 0.067(5) Uani 1 1 d . . . . .
H18 H 0.5590 0.8064 0.6244 0.080 Uiso 1 1 calc R U . . .
C19 C 0.7005(8) 0.6818(8) 0.6096(7) 0.058(4) Uani 1 1 d . . . . .
C20 C 0.8154(12) 0.6529(11) 0.5663(10) 0.083(6) Uani 1 1 d . . . . .
H20A H 0.8167 0.6285 0.6124 0.125 Uiso 1 1 calc R U . . .
H20B H 0.8568 0.6816 0.5613 0.125 Uiso 1 1 calc R U . . .
H20C H 0.8138 0.6192 0.5270 0.125 Uiso 1 1 calc R U . . .
C21 C 0.5042(6) 0.6772(6) 0.5024(6) 0.037(3) Uani 1 1 d . . . . .
C22 C 0.5137(9) 0.7505(6) 0.4723(7) 0.055(4) Uani 1 1 d . . . . .
H22A H 0.4989 0.7516 0.4219 0.082 Uiso 1 1 calc R U . . .
H22B H 0.5624 0.7637 0.4755 0.082 Uiso 1 1 calc R U . . .
H22C H 0.4857 0.7830 0.5003 0.082 Uiso 1 1 calc R U . . .
C23 C 0.5000 0.5000 0.7981(11) 0.057(5) Uani 1 2 d S T P . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Gd1 O6 2.339(8) 3_665 ?
Gd1 O2 2.357(7) . ?
Gd1 O3 2.361(8) . ?
Gd1 O9 2.404(7) . ?
Gd1 O13 2.419(8) . ?
Gd1 O7 2.441(8) 3_665 ?
Gd1 N1 2.510(10) . ?
Gd1 O12 2.5927(8) . ?
Gd1 N3 2.608(11) 3_665 ?
Gd1 C23 2.929(10) . ?
Gd1 Gd2 3.6126(10) 3_665 ?
Gd1 Gd2 3.6368(9) . ?
Gd2 O6 2.306(8) . ?
Gd2 O11 2.319(7) 4_656 ?
Gd2 O9 2.359(7) 3_665 ?
Gd2 O9 2.376(7) . ?
Gd2 O2 2.376(8) . ?
Gd2 O10 2.378(8) . ?
Gd2 O1 2.465(8) . ?
Gd2 O12 2.522(7) . ?
Gd2 Gd1 3.6127(10) 3_665 ?
Gd2 Gd2 3.6749(12) 3_665 ?
O1 C2 1.397(16) . ?
O1 C1 1.463(13) . ?
O2 C7 1.359(13) . ?
O3 C9 1.228(16) . ?
O4 C9 1.333(15) . ?
O4 C10 1.459(19) . ?
O5 C12 1.33(3) . ?
O5 C11 1.40(2) . ?
O6 C17 1.368(15) . ?
O6 Gd1 2.340(8) 3_665 ?
O7 C19 1.259(17) . ?
O7 Gd1 2.441(8) 3_665 ?
O8 C19 1.353(18) . ?
O8 C20 1.42(3) . ?
O9 Gd2 2.359(7) 3_665 ?
O10 C21 1.254(14) . ?
O11 C21 1.259(14) . ?
O11 Gd2 2.319(7) 2_566 ?
O12 C23 1.38(2) . ?
O12 Gd2 2.521(7) 3_665 ?
O12 Gd1 2.5928(8) 3_665 ?
O13 C23 1.269(12) . ?
N1 C8 1.288(15) . ?
N1 N2 1.394(14) . ?
N2 C9 1.329(18) . ?
N2 H2 0.8600 . ?
N3 C18 1.27(2) . ?
N3 N4 1.397(18) . ?
N3 Gd1 2.608(11) 3_665 ?
N4 C19 1.31(2) . ?
N4 H4 0.8600 . ?
C1 H1A 0.9600 . ?
C1 H1B 0.9600 . ?
C1 H1C 0.9600 . ?
C2 C3 1.377(18) . ?
C2 C7 1.420(17) . ?
C3 C4 1.38(2) . ?
C3 H3 0.9300 . ?
C4 C5 1.37(2) . ?
C4 H4A 0.9300 . ?
C5 C6 1.435(18) . ?
C5 H5 0.9300 . ?
C6 C7 1.388(17) . ?
C6 C8 1.473(18) . ?
C8 H8 0.9300 . ?
C10 H10A 0.9600 . ?
C10 H10B 0.9600 . ?
C10 H10C 0.9600 . ?
C11 H11A 0.9600 . ?
C11 H11B 0.9600 . ?
C11 H11C 0.9600 . ?
C12 C13 1.43(2) . ?
C12 C17 1.45(3) . ?
C13 C14 1.41(4) . ?
C13 H13 0.9300 . ?
C14 C15 1.34(3) . ?
C14 H14 0.9300 . ?
C15 C16 1.38(2) . ?
C15 H15 0.9300 . ?
C16 C17 1.35(2) . ?
C16 C18 1.48(3) . ?
C18 H18 0.9300 . ?
C20 H20A 0.9600 . ?
C20 H20B 0.9600 . ?
C20 H20C 0.9600 . ?
C21 C22 1.506(16) . ?
C22 H22A 0.9600 . ?
C22 H22B 0.9600 . ?
C22 H22C 0.9600 . ?
C23 O13 1.269(12) 3_665 ?
C23 Gd1 2.930(9) 3_665 ?

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 Gd1 O2 136.3(3) 3_665 . ?
O6 Gd1 O3 79.7(3) 3_665 . ?
O2 Gd1 O3 137.3(3) . . ?
O6 Gd1 O9 75.5(3) 3_665 . ?
O2 Gd1 O9 74.7(3) . . ?
O3 Gd1 O9 147.4(3) . . ?
O6 Gd1 O13 81.4(3) 3_665 . ?
O2 Gd1 O13 82.6(3) . . ?
O3 Gd1 O13 81.8(3) . . ?
O9 Gd1 O13 114.4(2) . . ?
O6 Gd1 O7 128.3(3) 3_665 3_665 ?
O2 Gd1 O7 77.8(3) . 3_665 ?
O3 Gd1 O7 97.3(3) . 3_665 ?
O9 Gd1 O7 82.2(3) . 3_665 ?
O13 Gd1 O7 149.9(3) . 3_665 ?
O6 Gd1 N1 139.2(3) 3_665 . ?
O2 Gd1 N1 73.5(3) . . ?
O3 Gd1 N1 64.2(3) . . ?
O9 Gd1 N1 144.9(3) . . ?
O13 Gd1 N1 75.6(3) . . ?
O7 Gd1 N1 77.0(3) 3_665 . ?
O6 Gd1 O12 66.9(2) 3_665 . ?
O2 Gd1 O12 70.92(19) . . ?
O3 Gd1 O12 126.2(3) . . ?
O9 Gd1 O12 61.1(3) . . ?
O13 Gd1 O12 53.3(3) . . ?
O7 Gd1 O12 136.5(3) 3_665 . ?
N1 Gd1 O12 119.9(3) . . ?
O6 Gd1 N3 68.3(4) 3_665 3_665 ?
O2 Gd1 N3 135.4(3) . 3_665 ?
O3 Gd1 N3 70.7(4) . 3_665 ?
O9 Gd1 N3 80.7(3) . 3_665 ?
O13 Gd1 N3 141.8(3) . 3_665 ?
O7 Gd1 N3 62.3(3) 3_665 3_665 ?
N1 Gd1 N3 113.0(3) . 3_665 ?
O12 Gd1 N3 126.5(3) . 3_665 ?
O6 Gd1 C23 71.8(2) 3_665 . ?
O2 Gd1 C23 76.6(2) . . ?
O3 Gd1 C23 102.7(4) . . ?
O9 Gd1 C23 89.3(4) . . ?
O13 Gd1 C23 25.2(4) . . ?
O7 Gd1 C23 154.3(2) 3_665 . ?
N1 Gd1 C23 97.4(4) . . ?
O12 Gd1 C23 28.1(4) . . ?
N3 Gd1 C23 140.1(3) 3_665 . ?
O6 Gd1 Gd2 38.6(2) 3_665 3_665 ?
O2 Gd1 Gd2 100.68(19) . 3_665 ?
O3 Gd1 Gd2 118.3(2) . 3_665 ?
O9 Gd1 Gd2 40.20(16) . 3_665 ?
O13 Gd1 Gd2 88.32(18) . 3_665 ?
O7 Gd1 Gd2 117.5(2) 3_665 3_665 ?
N1 Gd1 Gd2 163.4(2) . 3_665 ?
O12 Gd1 Gd2 44.26(15) . 3_665 ?
N3 Gd1 Gd2 82.3(3) 3_665 3_665 ?
C23 Gd1 Gd2 66.0(3) . 3_665 ?
O6 Gd1 Gd2 98.4(2) 3_665 . ?
O2 Gd1 Gd2 39.99(18) . . ?
O3 Gd1 Gd2 168.0(2) . . ?
O9 Gd1 Gd2 40.18(17) . . ?
O13 Gd1 Gd2 86.2(2) . . ?
O7 Gd1 Gd2 93.1(2) 3_665 . ?
N1 Gd1 Gd2 112.9(2) . . ?
O12 Gd1 Gd2 43.89(15) . . ?
N3 Gd1 Gd2 119.8(3) 3_665 . ?
C23 Gd1 Gd2 65.7(3) . . ?
Gd2 Gd1 Gd2 60.917(19) 3_665 . ?
O6 Gd2 O11 153.2(3) . 4_656 ?
O6 Gd2 O9 77.0(3) . 3_665 ?
O11 Gd2 O9 110.2(3) 4_656 3_665 ?
O6 Gd2 O9 130.7(3) . . ?
O11 Gd2 O9 75.5(3) 4_656 . ?
O9 Gd2 O9 75.3(3) 3_665 . ?
O6 Gd2 O2 96.8(3) . . ?
O11 Gd2 O2 95.8(3) 4_656 . ?
O9 Gd2 O2 133.4(2) 3_665 . ?
O9 Gd2 O2 74.9(3) . . ?
O6 Gd2 O10 82.4(3) . . ?
O11 Gd2 O10 74.3(3) 4_656 . ?
O9 Gd2 O10 78.4(3) 3_665 . ?
O9 Gd2 O10 129.5(3) . . ?
O2 Gd2 O10 147.4(3) . . ?
O6 Gd2 O1 84.8(3) . . ?
O11 Gd2 O1 79.0(3) 4_656 . ?
O9 Gd2 O1 154.6(3) 3_665 . ?
O9 Gd2 O1 130.0(3) . . ?
O2 Gd2 O1 65.8(2) . . ?
O10 Gd2 O1 81.7(3) . . ?
O6 Gd2 O12 68.6(2) . . ?
O11 Gd2 O12 138.0(2) 4_656 . ?
O9 Gd2 O12 62.8(2) 3_665 . ?
O9 Gd2 O12 62.6(2) . . ?
O2 Gd2 O12 71.89(19) . . ?
O10 Gd2 O12 135.3(2) . . ?
O1 Gd2 O12 126.2(2) . . ?
O6 Gd2 Gd1 39.3(2) . 3_665 ?
O11 Gd2 Gd1 150.73(19) 4_656 3_665 ?
O9 Gd2 Gd1 41.14(17) 3_665 3_665 ?
O9 Gd2 Gd1 96.97(17) . 3_665 ?
O2 Gd2 Gd1 109.65(18) . 3_665 ?
O10 Gd2 Gd1 90.3(2) . 3_665 ?
O1 Gd2 Gd1 124.1(2) . 3_665 ?
O12 Gd2 Gd1 45.863(15) . 3_665 ?
O6 Gd2 Gd1 104.9(2) . . ?
O11 Gd2 Gd1 99.9(2) 4_656 . ?
O9 Gd2 Gd1 96.66(17) 3_665 . ?
O9 Gd2 Gd1 40.75(17) . . ?
O2 Gd2 Gd1 39.59(17) . . ?
O10 Gd2 Gd1 170.2(2) . . ?
O1 Gd2 Gd1 105.19(18) . . ?
O12 Gd2 Gd1 45.468(14) . . ?
Gd1 Gd2 Gd1 91.33(2) 3_665 . ?
O6 Gd2 Gd2 98.1(2) . 3_665 ?
O11 Gd2 Gd2 103.3(2) 4_656 3_665 ?
O9 Gd2 Gd2 39.26(17) 3_665 3_665 ?
O9 Gd2 Gd2 38.92(16) . 3_665 ?
O2 Gd2 Gd2 98.58(17) . 3_665 ?
O10 Gd2 Gd2 113.82(19) . 3_665 ?
O1 Gd2 Gd2 164.39(18) . 3_665 ?
O12 Gd2 Gd2 43.22(17) . 3_665 ?
Gd1 Gd2 Gd2 59.865(17) 3_665 3_665 ?
Gd1 Gd2 Gd2 59.216(17) . 3_665 ?
C2 O1 C1 116.4(9) . . ?
C2 O1 Gd2 119.3(6) . . ?
C1 O1 Gd2 124.4(7) . . ?
C7 O2 Gd1 136.4(7) . . ?
C7 O2 Gd2 122.7(7) . . ?
Gd1 O2 Gd2 100.4(3) . . ?
C9 O3 Gd1 120.1(9) . . ?
C9 O4 C10 117.1(12) . . ?
C12 O5 C11 115.9(17) . . ?
C17 O6 Gd2 126.2(7) . . ?
C17 O6 Gd1 127.0(7) . 3_665 ?
Gd2 O6 Gd1 102.1(3) . 3_665 ?
C19 O7 Gd1 121.9(9) . 3_665 ?
C19 O8 C20 118.3(14) . . ?
Gd2 O9 Gd2 101.8(3) 3_665 . ?
Gd2 O9 Gd1 98.7(3) 3_665 . ?
Gd2 O9 Gd1 99.1(3) . . ?
C21 O10 Gd2 133.6(7) . . ?
C21 O11 Gd2 138.6(7) . 2_566 ?
C23 O12 Gd2 133.22(17) . 3_665 ?
C23 O12 Gd2 133.22(17) . . ?
Gd2 O12 Gd2 93.6(3) 3_665 . ?
C23 O12 Gd1 89.6(2) . . ?
Gd2 O12 Gd1 89.87(15) 3_665 . ?
Gd2 O12 Gd1 90.64(15) . . ?
C23 O12 Gd1 89.6(2) . 3_665 ?
Gd2 O12 Gd1 90.64(15) 3_665 3_665 ?
Gd2 O12 Gd1 89.87(15) . 3_665 ?
Gd1 O12 Gd1 179.2(4) . 3_665 ?
C23 O13 Gd1 100.5(9) . . ?
C8 N1 N2 112.3(10) . . ?
C8 N1 Gd1 131.5(9) . . ?
N2 N1 Gd1 116.2(7) . . ?
C9 N2 N1 111.6(11) . . ?
C9 N2 H2 124.2 . . ?
N1 N2 H2 124.2 . . ?
C18 N3 N4 113.2(13) . . ?
C18 N3 Gd1 130.6(12) . 3_665 ?
N4 N3 Gd1 116.0(8) . 3_665 ?
C19 N4 N3 114.0(11) . . ?
C19 N4 H4 123.0 . . ?
N3 N4 H4 123.0 . . ?
O1 C1 H1A 109.5 . . ?
O1 C1 H1B 109.5 . . ?
H1A C1 H1B 109.5 . . ?
O1 C1 H1C 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
C3 C2 O1 124.3(12) . . ?
C3 C2 C7 120.9(13) . . ?
O1 C2 C7 114.8(10) . . ?
C2 C3 C4 120.8(13) . . ?
C2 C3 H3 119.6 . . ?
C4 C3 H3 119.6 . . ?
C5 C4 C3 119.0(12) . . ?
C5 C4 H4A 120.5 . . ?
C3 C4 H4A 120.5 . . ?
C4 C5 C6 122.4(13) . . ?
C4 C5 H5 118.8 . . ?
C6 C5 H5 118.8 . . ?
C7 C6 C5 117.6(12) . . ?
C7 C6 C8 126.2(11) . . ?
C5 C6 C8 116.1(11) . . ?
O2 C7 C6 123.6(10) . . ?
O2 C7 C2 117.3(10) . . ?
C6 C7 C2 119.1(11) . . ?
N1 C8 C6 125.6(11) . . ?
N1 C8 H8 117.2 . . ?
C6 C8 H8 117.2 . . ?
O3 C9 O4 120.8(13) . . ?
O3 C9 N2 126.4(12) . . ?
O4 C9 N2 112.8(12) . . ?
O4 C10 H10A 109.5 . . ?
O4 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
O4 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
O5 C11 H11A 109.5 . . ?
O5 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
O5 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
O5 C12 C13 124(2) . . ?
O5 C12 C17 117.5(13) . . ?
C13 C12 C17 118(2) . . ?
C14 C13 C12 118(2) . . ?
C14 C13 H13 121.1 . . ?
C12 C13 H13 121.1 . . ?
C15 C14 C13 119.5(17) . . ?
C15 C14 H14 120.3 . . ?
C13 C14 H14 120.3 . . ?
C14 C15 C16 125(2) . . ?
C14 C15 H15 117.4 . . ?
C16 C15 H15 117.4 . . ?
C17 C16 C15 117(2) . . ?
C17 C16 C18 122.3(13) . . ?
C15 C16 C18 120.5(19) . . ?
C16 C17 O6 124.2(14) . . ?
C16 C17 C12 121.6(14) . . ?
O6 C17 C12 114.2(15) . . ?
N3 C18 C16 123.9(15) . . ?
N3 C18 H18 118.0 . . ?
C16 C18 H18 118.0 . . ?
O7 C19 N4 125.3(14) . . ?
O7 C19 O8 122.9(16) . . ?
N4 C19 O8 111.6(14) . . ?
O8 C20 H20A 109.5 . . ?
O8 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
O8 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
O10 C21 O11 123.0(10) . . ?
O10 C21 C22 120.1(11) . . ?
O11 C21 C22 116.9(11) . . ?
C21 C22 H22A 109.5 . . ?
C21 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
C21 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
O13 C23 O13 127.1(18) . 3_665 ?
O13 C23 O12 116.4(9) . . ?
O13 C23 O12 116.4(9) 3_665 . ?
O13 C23 Gd1 54.3(6) . . ?
O13 C23 Gd1 176.4(6) 3_665 . ?
O12 C23 Gd1 62.3(4) . . ?
O13 C23 Gd1 176.4(6) . 3_665 ?
O13 C23 Gd1 54.3(6) 3_665 3_665 ?
O12 C23 Gd1 62.3(4) . 3_665 ?
Gd1 C23 Gd1 124.5(7) . 3_665 ?

_refine_diff_density_max         1.432
_refine_diff_density_min         -1.046
_refine_diff_density_rms         0.149



####################################################################### 
# 
# 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_shelxs-sr
_database_code_depnum_ccdc_archive 'CCDC 1428656'
_audit_update_record             
;
2018-12-10 deposited with the CCDC.
2018-12-11 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C90 H100 N16 O50 Tb8'
_chemical_formula_weight         3477.21

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      tetragonal
_space_group_IT_number           82
_space_group_name_H-M_alt        'I -4'
_space_group_name_Hall           'I -4'

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

_cell_length_a                   19.107(3)
_cell_length_b                   19.107(3)
_cell_length_c                   18.188(4)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     6640(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       ?
_exptl_crystal_colour            ?
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.739
_exptl_crystal_F_000             3344
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          ?
_exptl_crystal_size_mid          ?
_exptl_crystal_size_min          ?
_exptl_absorpt_coefficient_mu    4.284
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  ?
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            26062
_diffrn_reflns_av_unetI/netI     0.0355
_diffrn_reflns_av_R_equivalents  0.0411
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         2.634
_diffrn_reflns_theta_max         24.990
_diffrn_reflns_theta_full        24.990
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measured_fraction_theta_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_point_group_measured_fraction_full 0.997
_reflns_number_total             5856
_reflns_number_gt                5743
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.932
_reflns_Friedel_fraction_max     0.998
_reflns_Friedel_fraction_full    0.998

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          
;
 Refined as a 2-component inversion twin.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0700P)²+6.0000P] 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     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_extinction_coef       0.00134(12)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_abs_structure_details 
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.11(2)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         5856
_refine_ls_number_parameters     365
_refine_ls_number_restraints     49
_refine_ls_R_factor_all          0.0348
_refine_ls_R_factor_gt           0.0342
_refine_ls_wR_factor_ref         0.0943
_refine_ls_wR_factor_gt          0.0936
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_restrained_S_all      1.026
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Tb1 Tb 0.40236(2) 0.40621(2) 0.72367(2) 0.03324(18) Uani 1 1 d . . . . .
Tb2 Tb 0.56693(2) 0.43154(2) 0.62804(2) 0.02948(17) Uani 1 1 d . . . . .
O1 O 0.6350(4) 0.3238(4) 0.6498(4) 0.0359(16) Uani 1 1 d . . . . .
O2 O 0.5116(4) 0.3496(3) 0.7059(4) 0.0306(14) Uani 1 1 d . . . . .
O3 O 0.3085(4) 0.4007(4) 0.8073(5) 0.0452(19) Uani 1 1 d . . . . .
O4 O 0.2593(5) 0.3605(5) 0.9095(5) 0.059(2) Uani 1 1 d . . . . .
O5 O 0.6447(6) 0.3817(5) 0.8173(6) 0.066(3) Uani 1 1 d . U . . .
O6 O 0.6406(4) 0.4800(4) 0.7145(4) 0.0416(17) Uani 1 1 d . . . . .
O7 O 0.6294(4) 0.6947(4) 0.6481(4) 0.0455(19) Uani 1 1 d . . . . .
O8 O 0.7034(6) 0.7469(6) 0.5662(6) 0.070(3) Uani 1 1 d . . . . .
O9 O 0.5541(3) 0.5530(3) 0.6093(4) 0.0290(13) Uani 1 1 d . . . . .
O10 O 0.5438(4) 0.3706(4) 0.5206(4) 0.0348(15) Uani 1 1 d . . . . .
O11 O 0.6633(4) 0.4553(4) 0.5500(4) 0.0388(17) Uani 1 1 d . . . . .
O12 O 0.5000 0.5000 0.7235(5) 0.0304(19) Uani 1 2 d S T P . .
O13 O 0.4600(4) 0.4557(4) 0.8289(4) 0.0404(17) Uani 1 1 d . . . . .
N1 N 0.4054(5) 0.3056(5) 0.8134(5) 0.0358(19) Uani 1 1 d . . . . .
N2 N 0.3541(5) 0.3067(5) 0.8670(6) 0.046(2) Uani 1 1 d . . . . .
H2 H 0.3520 0.2772 0.9027 0.055 Uiso 1 1 calc R U . . .
N3 N 0.7169(5) 0.5872(6) 0.6529(6) 0.048(2) Uani 1 1 d . . . . .
N4 N 0.7293(5) 0.6414(6) 0.6049(6) 0.054(3) Uani 1 1 d . . . . .
H4 H 0.7637 0.6413 0.5743 0.065 Uiso 1 1 calc R U . . .
C1 C 0.7041(5) 0.3105(7) 0.6186(8) 0.051(3) Uani 1 1 d . . . . .
H1A H 0.7211 0.3523 0.5952 0.076 Uiso 1 1 calc R U . . .
H1B H 0.7010 0.2736 0.5829 0.076 Uiso 1 1 calc R U . . .
H1C H 0.7358 0.2970 0.6570 0.076 Uiso 1 1 calc R U . . .
C2 C 0.6065(6) 0.2707(6) 0.6936(6) 0.038(2) Uani 1 1 d . . . . .
C3 C 0.6371(6) 0.2064(6) 0.7064(6) 0.042(2) Uani 1 1 d . . . . .
H3 H 0.6804 0.1964 0.6855 0.050 Uiso 1 1 calc R U . . .
C4 C 0.6059(8) 0.1585(6) 0.7478(8) 0.058(3) Uani 1 1 d . . . . .
H4A H 0.6238 0.1134 0.7511 0.069 Uiso 1 1 calc R U . . .
C5 C 0.5454(6) 0.1772(6) 0.7865(7) 0.049(3) Uani 1 1 d . . . . .
H5 H 0.5283 0.1469 0.8223 0.058 Uiso 1 1 calc R U . . .
C6 C 0.5094(6) 0.2403(6) 0.7733(6) 0.040(2) Uani 1 1 d . . . . .
C7 C 0.5403(5) 0.2880(5) 0.7232(6) 0.034(2) Uani 1 1 d . . . . .
C8 C 0.4468(7) 0.2531(6) 0.8185(6) 0.044(3) Uani 1 1 d . . . . .
H8 H 0.4363 0.2199 0.8543 0.053 Uiso 1 1 calc R U . . .
C9 C 0.3083(6) 0.3582(6) 0.8573(7) 0.045(3) Uani 1 1 d . . . . .
C10 C 0.2046(11) 0.4124(11) 0.8935(15) 0.127(12) Uani 1 1 d . . . . .
H10A H 0.2247 0.4511 0.8673 0.191 Uiso 1 1 calc R U . . .
H10B H 0.1847 0.4288 0.9388 0.191 Uiso 1 1 calc R U . . .
H10C H 0.1687 0.3912 0.8641 0.191 Uiso 1 1 calc R U . . .
C11 C 0.6468(12) 0.3271(8) 0.8649(9) 0.088(6) Uani 1 1 d . U . . .
H11A H 0.6003 0.3169 0.8818 0.132 Uiso 1 1 calc R U . . .
H11B H 0.6657 0.2868 0.8404 0.132 Uiso 1 1 calc R U . . .
H11C H 0.6759 0.3389 0.9061 0.132 Uiso 1 1 calc R U . . .
C12 C 0.7046(4) 0.4017(5) 0.7895(5) 0.068(4) Uani 1 1 d G U . . .
C13 C 0.7683(5) 0.3720(5) 0.8091(6) 0.088(5) Uani 1 1 d G U . . .
H13 H 0.7698 0.3364 0.8440 0.106 Uiso 1 1 calc R U . . .
C14 C 0.8298(4) 0.3955(6) 0.7766(7) 0.087(5) Uani 1 1 d G U . . .
H14 H 0.8725 0.3756 0.7897 0.104 Uiso 1 1 calc R U . . .
C15 C 0.8276(4) 0.4486(6) 0.7245(7) 0.079(4) Uani 1 1 d G U . . .
H15 H 0.8688 0.4644 0.7028 0.095 Uiso 1 1 calc R U . . .
C16 C 0.7639(4) 0.4783(5) 0.7049(5) 0.064(4) Uani 1 1 d G U . . .
C17 C 0.7024(3) 0.4549(5) 0.7374(5) 0.051(3) Uani 1 1 d G U . . .
C18 C 0.7660(7) 0.5415(9) 0.6581(9) 0.066(4) Uani 1 1 d . U . . .
H18 H 0.8061 0.5488 0.6301 0.079 Uiso 1 1 calc R U . . .
C19 C 0.6835(7) 0.6944(7) 0.6095(6) 0.050(3) Uani 1 1 d . . . . .
C20 C 0.6587(8) 0.8061(9) 0.5637(9) 0.073(5) Uani 1 1 d . . . . .
H20A H 0.6147 0.7930 0.5422 0.110 Uiso 1 1 calc R U . . .
H20B H 0.6800 0.8421 0.5344 0.110 Uiso 1 1 calc R U . . .
H20C H 0.6510 0.8232 0.6126 0.110 Uiso 1 1 calc R U . . .
C21 C 0.6766(5) 0.5025(5) 0.5022(5) 0.031(2) Uani 1 1 d . . . . .
C22 C 0.7493(5) 0.5122(8) 0.4700(7) 0.049(3) Uani 1 1 d . . . . .
H22A H 0.7514 0.4906 0.4224 0.074 Uiso 1 1 calc R U . . .
H22B H 0.7833 0.4909 0.5018 0.074 Uiso 1 1 calc R U . . .
H22C H 0.7593 0.5613 0.4653 0.074 Uiso 1 1 calc R U . . .
C23 C 0.5000 0.5000 0.7969(8) 0.041(4) Uani 1 2 d S T P . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Tb1 O6 2.331(7) 3_665 ?
Tb1 O3 2.354(8) . ?
Tb1 O9 2.371(6) 3_665 ?
Tb1 O2 2.373(7) . ?
Tb1 O13 2.401(7) . ?
Tb1 O7 2.445(8) 3_665 ?
Tb1 N1 2.522(9) . ?
Tb1 O12 2.5868(6) . ?
Tb1 N3 2.620(9) 3_665 ?
Tb1 C23 2.910(7) . ?
Tb1 Tb2 3.6028(8) 3_665 ?
Tb1 Tb2 3.6258(8) . ?
Tb2 O6 2.305(8) . ?
Tb2 O10 2.317(7) . ?
Tb2 O9 2.357(6) 3_665 ?
Tb2 O9 2.358(7) . ?
Tb2 O2 2.361(7) . ?
Tb2 O11 2.369(7) . ?
Tb2 O1 2.468(7) . ?
Tb2 O12 2.522(7) . ?
Tb2 Tb1 3.6028(8) 3_665 ?
Tb2 Tb2 3.6587(10) 3_665 ?
O1 C2 1.399(13) . ?
O1 C1 1.461(11) . ?
O2 C7 1.336(11) . ?
O3 C9 1.218(14) . ?
O4 C9 1.333(14) . ?
O4 C10 1.470(18) . ?
O5 C12 1.309(14) . ?
O5 C11 1.356(18) . ?
O6 C17 1.341(9) . ?
O6 Tb1 2.331(7) 3_665 ?
O7 C19 1.250(15) . ?
O7 Tb1 2.445(8) 3_665 ?
O8 C19 1.330(16) . ?
O8 C20 1.42(2) . ?
O9 Tb2 2.357(6) 3_665 ?
O9 Tb1 2.371(6) 3_665 ?
O10 C21 1.268(13) 2_566 ?
O11 C21 1.279(13) . ?
O12 C23 1.336(18) . ?
O12 Tb2 2.522(7) 3_665 ?
O12 Tb1 2.5868(6) 3_665 ?
O13 C23 1.281(10) . ?
N1 C8 1.281(15) . ?
N1 N2 1.383(13) . ?
N2 C9 1.330(16) . ?
N2 H2 0.8600 . ?
N3 C18 1.284(19) . ?
N3 N4 1.375(16) . ?
N3 Tb1 2.620(9) 3_665 ?
N4 C19 1.342(19) . ?
N4 H4 0.8600 . ?
C1 H1A 0.9600 . ?
C1 H1B 0.9600 . ?
C1 H1C 0.9600 . ?
C2 C3 1.382(15) . ?
C2 C7 1.413(15) . ?
C3 C4 1.326(18) . ?
C3 H3 0.9300 . ?
C4 C5 1.400(19) . ?
C4 H4A 0.9300 . ?
C5 C6 1.407(15) . ?
C5 H5 0.9300 . ?
C6 C7 1.418(15) . ?
C6 C8 1.472(15) . ?
C8 H8 0.9300 . ?
C10 H10A 0.9600 . ?
C10 H10B 0.9600 . ?
C10 H10C 0.9600 . ?
C11 H11A 0.9600 . ?
C11 H11B 0.9600 . ?
C11 H11C 0.9600 . ?
C12 C13 1.3900 . ?
C12 C17 1.3900 . ?
C13 C14 1.3900 . ?
C13 H13 0.9300 . ?
C14 C15 1.3900 . ?
C14 H14 0.9300 . ?
C15 C16 1.3900 . ?
C15 H15 0.9300 . ?
C16 C17 1.3900 . ?
C16 C18 1.48(2) . ?
C18 H18 0.9300 . ?
C20 H20A 0.9600 . ?
C20 H20B 0.9600 . ?
C20 H20C 0.9600 . ?
C21 O10 1.267(13) 4_656 ?
C21 C22 1.520(14) . ?
C22 H22A 0.9600 . ?
C22 H22B 0.9600 . ?
C22 H22C 0.9600 . ?
C23 O13 1.281(10) 3_665 ?
C23 Tb1 2.910(7) 3_665 ?

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 Tb1 O3 79.6(3) 3_665 . ?
O6 Tb1 O9 75.8(2) 3_665 3_665 ?
O3 Tb1 O9 148.1(3) . 3_665 ?
O6 Tb1 O2 136.5(2) 3_665 . ?
O3 Tb1 O2 137.5(3) . . ?
O9 Tb1 O2 73.9(2) 3_665 . ?
O6 Tb1 O13 81.4(3) 3_665 . ?
O3 Tb1 O13 81.5(3) . . ?
O9 Tb1 O13 114.1(2) 3_665 . ?
O2 Tb1 O13 83.4(3) . . ?
O6 Tb1 O7 127.5(3) 3_665 3_665 ?
O3 Tb1 O7 98.0(3) . 3_665 ?
O9 Tb1 O7 81.5(3) 3_665 3_665 ?
O2 Tb1 O7 77.4(3) . 3_665 ?
O13 Tb1 O7 150.7(3) . 3_665 ?
O6 Tb1 N1 139.9(3) 3_665 . ?
O3 Tb1 N1 64.2(3) . . ?
O9 Tb1 N1 144.1(3) 3_665 . ?
O2 Tb1 N1 73.8(3) . . ?
O13 Tb1 N1 76.9(3) . . ?
O7 Tb1 N1 76.6(3) 3_665 . ?
O6 Tb1 O12 66.9(2) 3_665 . ?
O3 Tb1 O12 125.5(3) . . ?
O9 Tb1 O12 61.2(3) 3_665 . ?
O2 Tb1 O12 71.42(16) . . ?
O13 Tb1 O12 53.0(3) . . ?
O7 Tb1 O12 136.4(3) 3_665 . ?
N1 Tb1 O12 120.8(3) . . ?
O6 Tb1 N3 67.3(3) 3_665 3_665 ?
O3 Tb1 N3 70.0(3) . 3_665 ?
O9 Tb1 N3 81.9(3) 3_665 3_665 ?
O2 Tb1 N3 136.1(3) . 3_665 ?
O13 Tb1 N3 140.5(3) . 3_665 ?
O7 Tb1 N3 63.0(3) 3_665 3_665 ?
N1 Tb1 N3 112.0(3) . 3_665 ?
O12 Tb1 N3 126.4(3) . 3_665 ?
O6 Tb1 C23 71.6(2) 3_665 . ?
O3 Tb1 C23 102.7(3) . . ?
O9 Tb1 C23 88.5(3) 3_665 . ?
O2 Tb1 C23 77.24(18) . . ?
O13 Tb1 C23 25.7(3) . . ?
O7 Tb1 C23 154.5(2) 3_665 . ?
N1 Tb1 C23 99.1(3) . . ?
O12 Tb1 C23 27.3(4) . . ?
N3 Tb1 C23 138.8(2) 3_665 . ?
O6 Tb1 Tb2 38.73(18) 3_665 3_665 ?
O3 Tb1 Tb2 118.33(19) . 3_665 ?
O9 Tb1 Tb2 40.24(16) 3_665 3_665 ?
O2 Tb1 Tb2 100.57(16) . 3_665 ?
O13 Tb1 Tb2 88.36(18) . 3_665 ?
O7 Tb1 Tb2 116.6(2) 3_665 3_665 ?
N1 Tb1 Tb2 164.7(2) . 3_665 ?
O12 Tb1 Tb2 44.43(15) . 3_665 ?
N3 Tb1 Tb2 82.1(2) 3_665 3_665 ?
C23 Tb1 Tb2 65.6(2) . 3_665 ?
O6 Tb1 Tb2 98.43(18) 3_665 . ?
O3 Tb1 Tb2 167.6(2) . . ?
O9 Tb1 Tb2 39.77(15) 3_665 . ?
O2 Tb1 Tb2 39.90(16) . . ?
O13 Tb1 Tb2 86.11(18) . . ?
O7 Tb1 Tb2 92.9(2) 3_665 . ?
N1 Tb1 Tb2 113.1(2) . . ?
O12 Tb1 Tb2 44.07(15) . . ?
N3 Tb1 Tb2 120.8(2) 3_665 . ?
C23 Tb1 Tb2 65.3(2) . . ?
Tb2 Tb1 Tb2 60.814(14) 3_665 . ?
O6 Tb2 O10 153.4(3) . . ?
O6 Tb2 O9 130.4(2) . 3_665 ?
O10 Tb2 O9 75.8(2) . 3_665 ?
O6 Tb2 O9 76.5(2) . . ?
O10 Tb2 O9 110.7(2) . . ?
O9 Tb2 O9 75.8(2) 3_665 . ?
O6 Tb2 O2 97.5(3) . . ?
O10 Tb2 O2 95.0(2) . . ?
O9 Tb2 O2 74.4(2) 3_665 . ?
O9 Tb2 O2 133.8(2) . . ?
O6 Tb2 O11 81.8(3) . . ?
O10 Tb2 O11 74.9(3) . . ?
O9 Tb2 O11 130.7(2) 3_665 . ?
O9 Tb2 O11 78.8(2) . . ?
O2 Tb2 O11 146.6(2) . . ?
O6 Tb2 O1 84.5(2) . . ?
O10 Tb2 O1 79.4(3) . . ?
O9 Tb2 O1 130.2(2) 3_665 . ?
O9 Tb2 O1 154.0(2) . . ?
O2 Tb2 O1 65.5(2) . . ?
O11 Tb2 O1 81.2(2) . . ?
O6 Tb2 O12 68.4(2) . . ?
O10 Tb2 O12 138.1(2) . . ?
O9 Tb2 O12 62.40(19) 3_665 . ?
O9 Tb2 O12 62.37(19) . . ?
O2 Tb2 O12 72.79(18) . . ?
O11 Tb2 O12 135.0(2) . . ?
O1 Tb2 O12 126.1(2) . . ?
O6 Tb2 Tb1 39.25(17) . 3_665 ?
O10 Tb2 Tb1 150.53(18) . 3_665 ?
O9 Tb2 Tb1 96.99(16) 3_665 3_665 ?
O9 Tb2 Tb1 40.51(16) . 3_665 ?
O2 Tb2 Tb1 110.73(16) . 3_665 ?
O11 Tb2 Tb1 89.84(19) . 3_665 ?
O1 Tb2 Tb1 123.69(18) . 3_665 ?
O12 Tb2 Tb1 45.889(11) . 3_665 ?
O6 Tb2 Tb1 104.8(2) . . ?
O10 Tb2 Tb1 99.90(19) . . ?
O9 Tb2 Tb1 40.07(16) 3_665 . ?
O9 Tb2 Tb1 96.35(16) . . ?
O2 Tb2 Tb1 40.15(16) . . ?
O11 Tb2 Tb1 170.82(18) . . ?
O1 Tb2 Tb1 105.58(16) . . ?
O12 Tb2 Tb1 45.515(11) . . ?
Tb1 Tb2 Tb1 91.403(17) 3_665 . ?
O6 Tb2 Tb2 98.04(18) . 3_665 ?
O10 Tb2 Tb2 103.06(18) . 3_665 ?
O9 Tb2 Tb2 39.12(16) 3_665 3_665 ?
O9 Tb2 Tb2 39.09(15) . 3_665 ?
O2 Tb2 Tb2 99.29(16) . 3_665 ?
O11 Tb2 Tb2 113.97(18) . 3_665 ?
O1 Tb2 Tb2 164.83(16) . 3_665 ?
O12 Tb2 Tb2 43.51(16) . 3_665 ?
Tb1 Tb2 Tb2 59.905(13) 3_665 3_665 ?
Tb1 Tb2 Tb2 59.283(13) . 3_665 ?
C2 O1 C1 116.6(8) . . ?
C2 O1 Tb2 119.4(6) . . ?
C1 O1 Tb2 124.0(6) . . ?
C7 O2 Tb2 122.8(6) . . ?
C7 O2 Tb1 137.0(6) . . ?
Tb2 O2 Tb1 100.0(2) . . ?
C9 O3 Tb1 121.0(7) . . ?
C9 O4 C10 112.4(11) . . ?
C12 O5 C11 116.4(13) . . ?
C17 O6 Tb2 127.3(6) . . ?
C17 O6 Tb1 128.4(6) . 3_665 ?
Tb2 O6 Tb1 102.0(3) . 3_665 ?
C19 O7 Tb1 121.2(8) . 3_665 ?
C19 O8 C20 116.6(13) . . ?
Tb2 O9 Tb2 101.8(2) 3_665 . ?
Tb2 O9 Tb1 100.2(2) 3_665 3_665 ?
Tb2 O9 Tb1 99.2(2) . 3_665 ?
C21 O10 Tb2 138.8(6) 2_566 . ?
C21 O11 Tb2 134.2(7) . . ?
C23 O12 Tb2 133.50(16) . . ?
C23 O12 Tb2 133.51(16) . 3_665 ?
Tb2 O12 Tb2 93.0(3) . 3_665 ?
C23 O12 Tb1 89.9(2) . 3_665 ?
Tb2 O12 Tb1 89.68(15) . 3_665 ?
Tb2 O12 Tb1 90.41(15) 3_665 3_665 ?
C23 O12 Tb1 89.9(2) . . ?
Tb2 O12 Tb1 90.41(15) . . ?
Tb2 O12 Tb1 89.68(15) 3_665 . ?
Tb1 O12 Tb1 179.9(4) 3_665 . ?
C23 O13 Tb1 99.9(7) . . ?
C8 N1 N2 113.4(9) . . ?
C8 N1 Tb1 131.2(8) . . ?
N2 N1 Tb1 115.4(6) . . ?
C9 N2 N1 112.6(9) . . ?
C9 N2 H2 123.7 . . ?
N1 N2 H2 123.7 . . ?
C18 N3 N4 115.6(11) . . ?
C18 N3 Tb1 129.2(10) . 3_665 ?
N4 N3 Tb1 115.2(7) . 3_665 ?
C19 N4 N3 114.6(10) . . ?
C19 N4 H4 122.7 . . ?
N3 N4 H4 122.7 . . ?
O1 C1 H1A 109.5 . . ?
O1 C1 H1B 109.5 . . ?
H1A C1 H1B 109.5 . . ?
O1 C1 H1C 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
C3 C2 O1 125.2(10) . . ?
C3 C2 C7 121.5(11) . . ?
O1 C2 C7 113.3(8) . . ?
C4 C3 C2 121.2(11) . . ?
C4 C3 H3 119.4 . . ?
C2 C3 H3 119.4 . . ?
C3 C4 C5 118.8(10) . . ?
C3 C4 H4A 120.6 . . ?
C5 C4 H4A 120.6 . . ?
C4 C5 C6 122.4(11) . . ?
C4 C5 H5 118.8 . . ?
C6 C5 H5 118.8 . . ?
C5 C6 C7 117.2(10) . . ?
C5 C6 C8 116.4(10) . . ?
C7 C6 C8 126.2(10) . . ?
O2 C7 C2 118.9(9) . . ?
O2 C7 C6 123.1(9) . . ?
C2 C7 C6 117.9(9) . . ?
N1 C8 C6 126.3(10) . . ?
N1 C8 H8 116.9 . . ?
C6 C8 H8 116.9 . . ?
O3 C9 N2 126.2(10) . . ?
O3 C9 O4 120.8(11) . . ?
N2 C9 O4 113.1(10) . . ?
O4 C10 H10A 109.5 . . ?
O4 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
O4 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
O5 C11 H11A 109.5 . . ?
O5 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
O5 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
O5 C12 C13 123.2(7) . . ?
O5 C12 C17 116.8(7) . . ?
C13 C12 C17 120.0 . . ?
C12 C13 C14 120.0 . . ?
C12 C13 H13 120.0 . . ?
C14 C13 H13 120.0 . . ?
C15 C14 C13 120.0 . . ?
C15 C14 H14 120.0 . . ?
C13 C14 H14 120.0 . . ?
C14 C15 C16 120.0 . . ?
C14 C15 H15 120.0 . . ?
C16 C15 H15 120.0 . . ?
C17 C16 C15 120.0 . . ?
C17 C16 C18 122.1(8) . . ?
C15 C16 C18 117.2(8) . . ?
O6 C17 C16 119.8(7) . . ?
O6 C17 C12 120.0(7) . . ?
C16 C17 C12 120.0 . . ?
N3 C18 C16 125.2(12) . . ?
N3 C18 H18 117.4 . . ?
C16 C18 H18 117.4 . . ?
O7 C19 O8 124.4(14) . . ?
O7 C19 N4 125.3(12) . . ?
O8 C19 N4 110.3(12) . . ?
O8 C20 H20A 109.5 . . ?
O8 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
O8 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
O10 C21 O11 121.4(9) 4_656 . ?
O10 C21 C22 116.6(9) 4_656 . ?
O11 C21 C22 122.0(10) . . ?
C21 C22 H22A 109.5 . . ?
C21 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
C21 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
O13 C23 O13 126.1(13) . 3_665 ?
O13 C23 O12 117.0(7) . . ?
O13 C23 O12 117.0(7) 3_665 . ?
O13 C23 Tb1 176.4(4) . 3_665 ?
O13 C23 Tb1 54.4(5) 3_665 3_665 ?
O12 C23 Tb1 62.7(3) . 3_665 ?
O13 C23 Tb1 54.4(5) . . ?
O13 C23 Tb1 176.4(4) 3_665 . ?
O12 C23 Tb1 62.7(3) . . ?
Tb1 C23 Tb1 125.5(5) 3_665 . ?

_refine_diff_density_max         1.526
_refine_diff_density_min         -1.133
_refine_diff_density_rms         0.129



####################################################################### 
# 
# 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_shelxs
_database_code_depnum_ccdc_archive 'CCDC 1428657'
_audit_update_record             
;
2018-12-10 deposited with the CCDC.
2018-12-11 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C90 H100 Dy8 N16 O50'
_chemical_formula_weight         3505.85

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

_space_group_crystal_system      tetragonal
_space_group_IT_number           82
_space_group_name_H-M_alt        'I -4'
_space_group_name_Hall           'I -4'

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

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

_cell_length_a                   19.037(3)
_cell_length_b                   19.037(3)
_cell_length_c                   18.195(4)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     6594(2)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       ?
_exptl_crystal_colour            ?
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.766
_exptl_crystal_F_000             3360
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          ?
_exptl_crystal_size_mid          ?
_exptl_crystal_size_min          ?
_exptl_absorpt_coefficient_mu    4.557
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  ?
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            26386
_diffrn_reflns_av_unetI/netI     0.0305
_diffrn_reflns_av_R_equivalents  0.0336
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         2.641
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_full        25.000
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measured_fraction_theta_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_point_group_measured_fraction_full 0.997
_reflns_number_total             5819
_reflns_number_gt                5647
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.933
_reflns_Friedel_fraction_max     0.998
_reflns_Friedel_fraction_full    0.998

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          
;
 Refined as a 2-component inversion twin.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0650P)²+10.0000P] 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     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_extinction_coef       0.00120(11)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_abs_structure_details 
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.19(2)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         5819
_refine_ls_number_parameters     366
_refine_ls_number_restraints     48
_refine_ls_R_factor_all          0.0348
_refine_ls_R_factor_gt           0.0338
_refine_ls_wR_factor_ref         0.0900
_refine_ls_wR_factor_gt          0.0886
_refine_ls_goodness_of_fit_ref   1.020
_refine_ls_restrained_S_all      1.018
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Dy1 Dy 0.59351(2) 0.40307(2) 0.72333(2) 0.03633(18) Uani 1 1 d . . . . .
Dy2 Dy 0.43188(2) 0.43291(2) 0.62799(2) 0.03279(17) Uani 1 1 d . . . . .
O1 O 0.3819(5) 0.3545(6) 0.8179(6) 0.072(3) Uani 1 1 d . U . . .
O2 O 0.4796(4) 0.3600(4) 0.7145(5) 0.0430(17) Uani 1 1 d . . . . .
O3 O 0.6955(4) 0.3719(4) 0.6500(4) 0.0478(19) Uani 1 1 d . . . . .
O4 O 0.7484(6) 0.2989(7) 0.5661(6) 0.078(3) Uani 1 1 d . . . . .
O5 O 0.3251(4) 0.3640(4) 0.6495(4) 0.0382(16) Uani 1 1 d . . . . .
O6 O 0.3509(3) 0.4878(4) 0.7063(4) 0.0338(15) Uani 1 1 d . . . . .
O7 O 0.4007(4) 0.6913(4) 0.8056(5) 0.050(2) Uani 1 1 d . . . . .
O8 O 0.3621(5) 0.7402(5) 0.9097(5) 0.060(2) Uani 1 1 d . . . . .
O9 O 0.5527(4) 0.4461(3) 0.6090(4) 0.0345(14) Uani 1 1 d . . . . .
O10 O 0.4563(4) 0.3364(4) 0.5497(4) 0.0413(17) Uani 1 1 d . . . . .
O11 O 0.5445(4) 0.3711(4) 0.4796(4) 0.0376(15) Uani 1 1 d . . . . .
O12 O 0.5000 0.5000 0.7229(5) 0.0299(19) Uani 1 2 d S T P . .
O13 O 0.5443(4) 0.4596(4) 0.8287(3) 0.0399(16) Uani 1 1 d . . . . .
N1 N 0.5888(6) 0.2854(5) 0.6518(6) 0.054(3) Uani 1 1 d . . . . .
N2 N 0.6440(7) 0.2720(6) 0.6045(7) 0.062(3) Uani 1 1 d . . . . .
H2 H 0.6448 0.2372 0.5743 0.075 Uiso 1 1 calc R U . . .
N3 N 0.3068(5) 0.5939(5) 0.8125(5) 0.040(2) Uani 1 1 d . . . . .
N4 N 0.3079(5) 0.6451(5) 0.8663(6) 0.046(2) Uani 1 1 d . . . . .
H4 H 0.2788 0.6467 0.9024 0.055 Uiso 1 1 calc R U . . .
C1 C 0.3271(9) 0.3509(13) 0.8654(9) 0.099(7) Uani 1 1 d . U . . .
H1A H 0.2853 0.3381 0.8391 0.148 Uiso 1 1 calc R U . . .
H1B H 0.3205 0.3958 0.8885 0.148 Uiso 1 1 calc R U . . .
H1C H 0.3368 0.3161 0.9023 0.148 Uiso 1 1 calc R U . . .
C2 C 0.4022(5) 0.2937(4) 0.7888(6) 0.075(4) Uani 1 1 d G U . . .
C3 C 0.3733(5) 0.2294(5) 0.8088(6) 0.093(5) Uani 1 1 d G U . . .
H3 H 0.3379 0.2276 0.8439 0.112 Uiso 1 1 calc R U . . .
C4 C 0.3975(6) 0.1679(4) 0.7764(7) 0.096(5) Uani 1 1 d G U . . .
H4A H 0.3782 0.1249 0.7898 0.115 Uiso 1 1 calc R U . . .
C5 C 0.4505(6) 0.1706(4) 0.7240(6) 0.079(4) Uani 1 1 d G U . . .
H5 H 0.4667 0.1294 0.7023 0.095 Uiso 1 1 calc R U . . .
C6 C 0.4794(5) 0.2349(4) 0.7039(5) 0.066(4) Uani 1 1 d G U . . .
C7 C 0.4552(5) 0.2965(4) 0.7363(5) 0.054(3) Uani 1 1 d G U . . .
C8 C 0.5426(9) 0.2354(7) 0.6566(9) 0.071(5) Uani 1 1 d . . . . .
H8 H 0.5499 0.1960 0.6273 0.085 Uiso 1 1 calc R U . . .
C9 C 0.6955(8) 0.3184(8) 0.6106(7) 0.059(3) Uani 1 1 d . . . . .
C10 C 0.8102(11) 0.3428(9) 0.5658(10) 0.087(6) Uani 1 1 d . . . . .
H10A H 0.8475 0.3193 0.5401 0.130 Uiso 1 1 calc R U . . .
H10B H 0.8245 0.3520 0.6155 0.130 Uiso 1 1 calc R U . . .
H10C H 0.7997 0.3864 0.5416 0.130 Uiso 1 1 calc R U . . .
C11 C 0.3109(7) 0.2953(5) 0.6186(8) 0.052(3) Uani 1 1 d . . . . .
H11A H 0.2743 0.2990 0.5825 0.078 Uiso 1 1 calc R U . . .
H11B H 0.2962 0.2639 0.6570 0.078 Uiso 1 1 calc R U . . .
H11C H 0.3527 0.2773 0.5959 0.078 Uiso 1 1 calc R U . . .
C12 C 0.2720(6) 0.3933(6) 0.6930(6) 0.040(2) Uani 1 1 d . . . . .
C13 C 0.2070(6) 0.3620(6) 0.7058(7) 0.049(3) Uani 1 1 d . . . . .
H13 H 0.1966 0.3192 0.6838 0.059 Uiso 1 1 calc R U . . .
C14 C 0.1594(6) 0.3928(8) 0.7494(8) 0.062(4) Uani 1 1 d . . . . .
H14 H 0.1149 0.3733 0.7551 0.074 Uiso 1 1 calc R U . . .
C15 C 0.1775(6) 0.4546(6) 0.7861(8) 0.054(3) Uani 1 1 d . . . . .
H15 H 0.1465 0.4732 0.8205 0.064 Uiso 1 1 calc R U . . .
C16 C 0.2406(6) 0.4890(6) 0.7726(7) 0.043(2) Uani 1 1 d . . . . .
C17 C 0.2887(5) 0.4589(5) 0.7238(6) 0.038(2) Uani 1 1 d . . . . .
C18 C 0.2528(6) 0.5520(7) 0.8184(6) 0.044(2) Uani 1 1 d . . . . .
H18 H 0.2195 0.5626 0.8541 0.053 Uiso 1 1 calc R U . . .
C19 C 0.3592(6) 0.6917(6) 0.8561(7) 0.047(3) Uani 1 1 d . . . . .
C20 C 0.4166(10) 0.7947(11) 0.8972(13) 0.111(9) Uani 1 1 d . . . . .
H20A H 0.4248 0.7997 0.8454 0.166 Uiso 1 1 calc R U . . .
H20B H 0.4595 0.7808 0.9211 0.166 Uiso 1 1 calc R U . . .
H20C H 0.4009 0.8386 0.9171 0.166 Uiso 1 1 calc R U . . .
C21 C 0.5024(6) 0.3248(5) 0.5020(5) 0.035(2) Uani 1 1 d . . . . .
C22 C 0.5134(9) 0.2510(6) 0.4714(7) 0.061(4) Uani 1 1 d . . . . .
H22A H 0.4896 0.2175 0.5020 0.092 Uiso 1 1 calc R U . . .
H22B H 0.5628 0.2404 0.4705 0.092 Uiso 1 1 calc R U . . .
H22C H 0.4950 0.2485 0.4223 0.092 Uiso 1 1 calc R U . . .
C23 C 0.5000 0.5000 0.7970(9) 0.046(4) Uani 1 2 d S T P . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Dy1 O2 2.324(7) . ?
Dy1 O7 2.341(8) 2_665 ?
Dy1 O6 2.352(7) 2_665 ?
Dy1 O9 2.367(7) . ?
Dy1 O13 2.390(7) . ?
Dy1 O3 2.429(8) . ?
Dy1 N3 2.497(9) 2_665 ?
Dy1 O12 2.5640(6) . ?
Dy1 N1 2.592(10) . ?
Dy1 C23 2.893(7) . ?
Dy1 Dy2 3.5777(8) . ?
Dy1 Dy2 3.6046(8) 2_665 ?
Dy2 O2 2.287(7) . ?
Dy2 O11 2.315(7) 3_566 ?
Dy2 O9 2.340(7) . ?
Dy2 O6 2.346(7) . ?
Dy2 O9 2.348(7) 2_665 ?
Dy2 O10 2.371(7) . ?
Dy2 O5 2.450(7) . ?
Dy2 O12 2.509(7) . ?
Dy2 Dy1 3.6046(8) 2_665 ?
Dy2 Dy2 3.6402(10) 2_665 ?
O1 C2 1.330(14) . ?
O1 C1 1.357(18) . ?
O2 C7 1.355(9) . ?
O3 C9 1.245(16) . ?
O4 C9 1.345(17) . ?
O4 C10 1.44(2) . ?
O5 C12 1.400(13) . ?
O5 C11 1.450(12) . ?
O6 C17 1.345(11) . ?
O6 Dy1 2.352(7) 2_665 ?
O7 C19 1.211(14) . ?
O7 Dy1 2.341(8) 2_665 ?
O8 C19 1.344(14) . ?
O8 C20 1.485(18) . ?
O9 Dy2 2.348(7) 2_665 ?
O10 C21 1.255(13) . ?
O11 C21 1.259(13) . ?
O11 Dy2 2.315(7) 4_656 ?
O12 C23 1.348(19) . ?
O12 Dy2 2.509(7) 2_665 ?
O12 Dy1 2.5640(6) 2_665 ?
O13 C23 1.279(10) . ?
N1 C8 1.300(19) . ?
N1 N2 1.382(16) . ?
N2 C9 1.33(2) . ?
N2 H2 0.8600 . ?
N3 C18 1.304(15) . ?
N3 N4 1.383(13) . ?
N3 Dy1 2.497(9) 2_665 ?
N4 C19 1.332(16) . ?
N4 H4 0.8600 . ?
C1 H1A 0.9600 . ?
C1 H1B 0.9600 . ?
C1 H1C 0.9600 . ?
C2 C3 1.3900 . ?
C2 C7 1.3900 . ?
C3 C4 1.3900 . ?
C3 H3 0.9300 . ?
C4 C5 1.3900 . ?
C4 H4A 0.9300 . ?
C5 C6 1.3900 . ?
C5 H5 0.9300 . ?
C6 C7 1.3900 . ?
C6 C8 1.48(2) . ?
C8 H8 0.9300 . ?
C10 H10A 0.9600 . ?
C10 H10B 0.9600 . ?
C10 H10C 0.9600 . ?
C11 H11A 0.9600 . ?
C11 H11B 0.9600 . ?
C11 H11C 0.9600 . ?
C12 C13 1.391(15) . ?
C12 C17 1.405(15) . ?
C13 C14 1.341(18) . ?
C13 H13 0.9300 . ?
C14 C15 1.396(18) . ?
C14 H14 0.9300 . ?
C15 C16 1.391(15) . ?
C15 H15 0.9300 . ?
C16 C17 1.398(16) . ?
C16 C18 1.479(16) . ?
C18 H18 0.9300 . ?
C20 H20A 0.9600 . ?
C20 H20B 0.9600 . ?
C20 H20C 0.9600 . ?
C21 C22 1.526(15) . ?
C22 H22A 0.9600 . ?
C22 H22B 0.9600 . ?
C22 H22C 0.9600 . ?
C23 O13 1.279(10) 2_665 ?
C23 Dy1 2.893(7) 2_665 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O2 Dy1 O7 79.5(3) . 2_665 ?
O2 Dy1 O6 136.3(2) . 2_665 ?
O7 Dy1 O6 137.8(3) 2_665 2_665 ?
O2 Dy1 O9 75.8(3) . . ?
O7 Dy1 O9 147.5(3) 2_665 . ?
O6 Dy1 O9 74.1(2) 2_665 . ?
O2 Dy1 O13 81.3(3) . . ?
O7 Dy1 O13 81.4(3) 2_665 . ?
O6 Dy1 O13 83.4(3) 2_665 . ?
O9 Dy1 O13 114.9(2) . . ?
O2 Dy1 O3 128.4(3) . . ?
O7 Dy1 O3 97.2(3) 2_665 . ?
O6 Dy1 O3 77.5(3) 2_665 . ?
O9 Dy1 O3 82.1(3) . . ?
O13 Dy1 O3 149.8(3) . . ?
O2 Dy1 N3 139.7(3) . 2_665 ?
O7 Dy1 N3 64.3(3) 2_665 2_665 ?
O6 Dy1 N3 73.9(3) 2_665 2_665 ?
O9 Dy1 N3 144.3(3) . 2_665 ?
O13 Dy1 N3 76.5(3) . 2_665 ?
O3 Dy1 N3 75.8(3) . 2_665 ?
O2 Dy1 O12 66.81(18) . . ?
O7 Dy1 O12 125.9(3) 2_665 . ?
O6 Dy1 O12 71.14(17) 2_665 . ?
O9 Dy1 O12 61.4(3) . . ?
O13 Dy1 O12 53.6(3) . . ?
O3 Dy1 O12 136.8(3) . . ?
N3 Dy1 O12 120.9(3) 2_665 . ?
O2 Dy1 N1 68.1(3) . . ?
O7 Dy1 N1 70.1(3) 2_665 . ?
O6 Dy1 N1 135.5(3) 2_665 . ?
O9 Dy1 N1 81.2(3) . . ?
O13 Dy1 N1 141.1(3) . . ?
O3 Dy1 N1 62.7(3) . . ?
N3 Dy1 N1 111.9(3) 2_665 . ?
O12 Dy1 N1 126.6(3) . . ?
O2 Dy1 C23 71.5(2) . . ?
O7 Dy1 C23 102.8(3) 2_665 . ?
O6 Dy1 C23 76.99(19) 2_665 . ?
O9 Dy1 C23 89.1(3) . . ?
O13 Dy1 C23 25.8(3) . . ?
O3 Dy1 C23 154.4(2) . . ?
N3 Dy1 C23 98.7(3) 2_665 . ?
O12 Dy1 C23 27.8(4) . . ?
N1 Dy1 C23 139.7(3) . . ?
O2 Dy1 Dy2 38.75(17) . . ?
O7 Dy1 Dy2 118.2(2) 2_665 . ?
O6 Dy1 Dy2 100.55(16) 2_665 . ?
O9 Dy1 Dy2 40.25(17) . . ?
O13 Dy1 Dy2 88.88(17) . . ?
O3 Dy1 Dy2 117.4(2) . . ?
N3 Dy1 Dy2 164.8(2) 2_665 . ?
O12 Dy1 Dy2 44.54(15) . . ?
N1 Dy1 Dy2 82.2(3) . . ?
C23 Dy1 Dy2 66.1(2) . . ?
O2 Dy1 Dy2 98.48(17) . 2_665 ?
O7 Dy1 Dy2 168.2(2) 2_665 2_665 ?
O6 Dy1 Dy2 39.83(16) 2_665 2_665 ?
O9 Dy1 Dy2 39.94(16) . 2_665 ?
O13 Dy1 Dy2 86.77(17) . 2_665 ?
O3 Dy1 Dy2 93.1(2) . 2_665 ?
N3 Dy1 Dy2 113.2(2) 2_665 2_665 ?
O12 Dy1 Dy2 44.12(15) . 2_665 ?
N1 Dy1 Dy2 120.2(3) . 2_665 ?
C23 Dy1 Dy2 65.7(2) . 2_665 ?
Dy2 Dy1 Dy2 60.905(15) . 2_665 ?
O2 Dy2 O11 153.3(3) . 3_566 ?
O2 Dy2 O9 77.1(3) . . ?
O11 Dy2 O9 110.3(2) 3_566 . ?
O2 Dy2 O6 96.5(3) . . ?
O11 Dy2 O6 95.9(3) 3_566 . ?
O9 Dy2 O6 133.5(2) . . ?
O2 Dy2 O9 130.4(3) . 2_665 ?
O11 Dy2 O9 75.8(2) 3_566 2_665 ?
O9 Dy2 O9 75.6(3) . 2_665 ?
O6 Dy2 O9 74.6(2) . 2_665 ?
O2 Dy2 O10 82.3(3) . . ?
O11 Dy2 O10 74.5(3) 3_566 . ?
O9 Dy2 O10 78.6(2) . . ?
O6 Dy2 O10 147.1(2) . . ?
O9 Dy2 O10 130.3(2) 2_665 . ?
O2 Dy2 O5 84.0(3) . . ?
O11 Dy2 O5 79.6(3) 3_566 . ?
O9 Dy2 O5 153.7(2) . . ?
O6 Dy2 O5 66.2(2) . . ?
O9 Dy2 O5 130.7(2) 2_665 . ?
O10 Dy2 O5 81.0(2) . . ?
O2 Dy2 O12 68.3(2) . . ?
O11 Dy2 O12 138.3(2) 3_566 . ?
O9 Dy2 O12 62.57(19) . . ?
O6 Dy2 O12 72.23(18) . . ?
O9 Dy2 O12 62.47(19) 2_665 . ?
O10 Dy2 O12 135.0(2) . . ?
O5 Dy2 O12 126.2(2) . . ?
O2 Dy2 Dy1 39.49(18) . . ?
O11 Dy2 Dy1 150.41(18) 3_566 . ?
O9 Dy2 Dy1 40.82(16) . . ?
O6 Dy2 Dy1 109.98(17) . . ?
O9 Dy2 Dy1 96.90(17) 2_665 . ?
O10 Dy2 Dy1 90.0(2) . . ?
O5 Dy2 Dy1 123.43(18) . . ?
O12 Dy2 Dy1 45.779(11) . . ?
O2 Dy2 Dy1 104.4(2) . 2_665 ?
O11 Dy2 Dy1 100.32(19) 3_566 2_665 ?
O9 Dy2 Dy1 96.33(16) . 2_665 ?
O6 Dy2 Dy1 39.95(16) . 2_665 ?
O9 Dy2 Dy1 40.34(17) 2_665 2_665 ?
O10 Dy2 Dy1 170.66(18) . 2_665 ?
O5 Dy2 Dy1 106.00(16) . 2_665 ?
O12 Dy2 Dy1 45.340(11) . 2_665 ?
Dy1 Dy2 Dy1 91.119(17) . 2_665 ?
O2 Dy2 Dy2 98.22(18) . 2_665 ?
O11 Dy2 Dy2 103.05(18) 3_566 2_665 ?
O9 Dy2 Dy2 39.14(16) . 2_665 ?
O6 Dy2 Dy2 98.96(16) . 2_665 ?
O9 Dy2 Dy2 38.98(17) 2_665 2_665 ?
O10 Dy2 Dy2 113.85(17) . 2_665 ?
O5 Dy2 Dy2 165.14(16) . 2_665 ?
O12 Dy2 Dy2 43.51(16) . 2_665 ?
Dy1 Dy2 Dy2 59.913(13) . 2_665 ?
Dy1 Dy2 Dy2 59.183(13) 2_665 2_665 ?
C2 O1 C1 115.6(14) . . ?
C7 O2 Dy2 127.4(6) . . ?
C7 O2 Dy1 128.0(6) . . ?
Dy2 O2 Dy1 101.8(3) . . ?
C9 O3 Dy1 121.1(9) . . ?
C9 O4 C10 116.9(14) . . ?
C12 O5 C11 116.3(8) . . ?
C12 O5 Dy2 118.5(6) . . ?
C11 O5 Dy2 125.2(6) . . ?
C17 O6 Dy2 122.7(6) . . ?
C17 O6 Dy1 136.7(6) . 2_665 ?
Dy2 O6 Dy1 100.2(2) . 2_665 ?
C19 O7 Dy1 121.4(8) . 2_665 ?
C19 O8 C20 113.4(10) . . ?
Dy2 O9 Dy2 101.9(2) . 2_665 ?
Dy2 O9 Dy1 98.9(2) . . ?
Dy2 O9 Dy1 99.7(3) 2_665 . ?
C21 O10 Dy2 133.6(7) . . ?
C21 O11 Dy2 137.8(7) . 4_656 ?
C23 O12 Dy2 133.51(16) . . ?
C23 O12 Dy2 133.51(16) . 2_665 ?
Dy2 O12 Dy2 93.0(3) . 2_665 ?
C23 O12 Dy1 89.8(2) . . ?
Dy2 O12 Dy1 89.68(14) . . ?
Dy2 O12 Dy1 90.54(15) 2_665 . ?
C23 O12 Dy1 89.8(2) . 2_665 ?
Dy2 O12 Dy1 90.54(15) . 2_665 ?
Dy2 O12 Dy1 89.68(14) 2_665 2_665 ?
Dy1 O12 Dy1 179.7(4) . 2_665 ?
C23 O13 Dy1 99.7(7) . . ?
C8 N1 N2 114.8(12) . . ?
C8 N1 Dy1 128.6(10) . . ?
N2 N1 Dy1 116.5(8) . . ?
C9 N2 N1 112.8(11) . . ?
C9 N2 H2 123.6 . . ?
N1 N2 H2 123.6 . . ?
C18 N3 N4 112.6(9) . . ?
C18 N3 Dy1 131.8(8) . 2_665 ?
N4 N3 Dy1 115.6(7) . 2_665 ?
C19 N4 N3 112.5(9) . . ?
C19 N4 H4 123.8 . . ?
N3 N4 H4 123.8 . . ?
O1 C1 H1A 109.5 . . ?
O1 C1 H1B 109.5 . . ?
H1A C1 H1B 109.5 . . ?
O1 C1 H1C 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
O1 C2 C3 123.2(7) . . ?
O1 C2 C7 116.8(7) . . ?
C3 C2 C7 120.0 . . ?
C4 C3 C2 120.0 . . ?
C4 C3 H3 120.0 . . ?
C2 C3 H3 120.0 . . ?
C3 C4 C5 120.0 . . ?
C3 C4 H4A 120.0 . . ?
C5 C4 H4A 120.0 . . ?
C4 C5 C6 120.0 . . ?
C4 C5 H5 120.0 . . ?
C6 C5 H5 120.0 . . ?
C7 C6 C5 120.0 . . ?
C7 C6 C8 120.8(8) . . ?
C5 C6 C8 118.6(8) . . ?
O2 C7 C6 120.9(7) . . ?
O2 C7 C2 119.0(7) . . ?
C6 C7 C2 120.0 . . ?
N1 C8 C6 126.4(13) . . ?
N1 C8 H8 116.8 . . ?
C6 C8 H8 116.8 . . ?
O3 C9 N2 126.3(13) . . ?
O3 C9 O4 125.0(15) . . ?
N2 C9 O4 108.6(13) . . ?
O4 C10 H10A 109.5 . . ?
O4 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
O4 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
O5 C11 H11A 109.5 . . ?
O5 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
O5 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
C13 C12 O5 124.5(10) . . ?
C13 C12 C17 120.9(11) . . ?
O5 C12 C17 114.6(9) . . ?
C14 C13 C12 120.9(11) . . ?
C14 C13 H13 119.6 . . ?
C12 C13 H13 119.6 . . ?
C13 C14 C15 119.0(11) . . ?
C13 C14 H14 120.5 . . ?
C15 C14 H14 120.5 . . ?
C16 C15 C14 121.7(11) . . ?
C16 C15 H15 119.1 . . ?
C14 C15 H15 119.1 . . ?
C15 C16 C17 118.9(10) . . ?
C15 C16 C18 114.7(10) . . ?
C17 C16 C18 126.1(10) . . ?
O6 C17 C16 123.9(9) . . ?
O6 C17 C12 118.0(9) . . ?
C16 C17 C12 118.1(9) . . ?
N3 C18 C16 124.9(10) . . ?
N3 C18 H18 117.6 . . ?
C16 C18 H18 117.6 . . ?
O7 C19 N4 125.4(11) . . ?
O7 C19 O8 121.9(11) . . ?
N4 C19 O8 112.7(10) . . ?
O8 C20 H20A 109.5 . . ?
O8 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
O8 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
O10 C21 O11 123.0(10) . . ?
O10 C21 C22 120.8(10) . . ?
O11 C21 C22 116.1(10) . . ?
C21 C22 H22A 109.5 . . ?
C21 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
C21 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
O13 C23 O13 126.4(14) 2_665 . ?
O13 C23 O12 116.8(7) 2_665 . ?
O13 C23 O12 116.8(7) . . ?
O13 C23 Dy1 176.7(4) 2_665 . ?
O13 C23 Dy1 54.5(5) . . ?
O12 C23 Dy1 62.4(3) . . ?
O13 C23 Dy1 54.5(5) 2_665 2_665 ?
O13 C23 Dy1 176.7(4) . 2_665 ?
O12 C23 Dy1 62.4(3) . 2_665 ?
Dy1 C23 Dy1 124.8(6) . 2_665 ?

_refine_diff_density_max         1.612
_refine_diff_density_min         -1.108
_refine_diff_density_rms         0.125



####################################################################### 
# 
# 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_141107f_0m
_database_code_depnum_ccdc_archive 'CCDC 1428658'
_audit_update_record             
;
2018-12-10 deposited with the CCDC.
2018-12-11 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C90 H100 Ho8 N16 O50'
_chemical_formula_weight         3525.29

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'
Ho Ho -0.2175 4.6783 '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      tetragonal
_space_group_IT_number           82
_space_group_name_H-M_alt        'I -4'
_space_group_name_Hall           'I -4'

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

_cell_length_a                   18.7121(5)
_cell_length_b                   18.7121(5)
_cell_length_c                   18.3396(11)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     6421.5(5)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       ?
_exptl_crystal_colour            ?
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.823
_exptl_crystal_F_000             3376
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          ?
_exptl_crystal_size_mid          ?
_exptl_crystal_size_min          ?
_exptl_absorpt_coefficient_mu    4.953
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  ?
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            44033
_diffrn_reflns_av_unetI/netI     0.0162
_diffrn_reflns_av_R_equivalents  0.0222
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         3.079
_diffrn_reflns_theta_max         25.019
_diffrn_reflns_theta_full        25.019
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measured_fraction_theta_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_point_group_measured_fraction_full 0.994
_reflns_number_total             5625
_reflns_number_gt                5488
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.932
_reflns_Friedel_fraction_max     0.995
_reflns_Friedel_fraction_full    0.995

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          
;
 Refined as a 2-component inversion twin.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1000P)²+58.0000P] 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_abs_structure_details 
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.16(3)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         5625
_refine_ls_number_parameters     365
_refine_ls_number_restraints     48
_refine_ls_R_factor_all          0.0359
_refine_ls_R_factor_gt           0.0348
_refine_ls_wR_factor_ref         0.1237
_refine_ls_wR_factor_gt          0.1206
_refine_ls_goodness_of_fit_ref   1.006
_refine_ls_restrained_S_all      1.006
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ho1 Ho 0.90187(3) 0.90270(3) 0.22067(3) 0.03058(19) Uani 1 1 d . . . . .
Ho2 Ho 0.93077(3) 1.06849(3) 0.12637(3) 0.02633(19) Uani 1 1 d . . . . .
O1 O 0.8448(10) 1.1169(7) 0.3098(9) 0.076(5) Uani 1 1 d . U . . .
O2 O 0.8552(5) 1.0169(5) 0.2101(6) 0.039(2) Uani 1 1 d . . . . .
O3 O 0.8741(5) 0.7972(5) 0.1496(5) 0.033(2) Uani 1 1 d . . . . .
O4 O 0.8064(9) 0.7382(8) 0.0624(7) 0.063(4) Uani 1 1 d . . . . .
O5 O 1.1389(6) 0.8221(5) 0.1472(6) 0.038(2) Uani 1 1 d . . . . .
O6 O 1.0146(5) 0.8489(4) 0.2046(5) 0.0280(19) Uani 1 1 d . . . . .
O7 O 0.8060(6) 0.8984(5) 0.3044(6) 0.038(2) Uani 1 1 d . . . . .
O8 O 0.7657(7) 0.8684(7) 0.4150(7) 0.052(3) Uani 1 1 d . . . . .
O9 O 0.9457(5) 0.9449(5) 0.1071(5) 0.033(2) Uani 1 1 d . . . . .
O10 O 0.8330(5) 1.0440(6) 0.0479(5) 0.036(2) Uani 1 1 d . . . . .
O11 O 0.8692(5) 0.9526(5) -0.0204(5) 0.0310(19) Uani 1 1 d . . . . .
O12 O 0.9583(6) 0.9550(5) 0.3251(5) 0.041(2) Uani 1 1 d . . . . .
O13 O 1.0000 1.0000 0.2195(6) 0.021(2) Uani 1 2 d S T P . .
N1 N 0.7815(6) 0.9048(6) 0.1468(7) 0.035(3) Uani 1 1 d . . . . .
N2 N 0.7732(8) 0.8446(9) 0.1013(8) 0.051(4) Uani 1 1 d . . . . .
H2 H 0.7389 0.8415 0.0703 0.062 Uiso 1 1 calc R U . . .
N3 N 0.9085(6) 0.8057(6) 0.3141(6) 0.029(2) Uani 1 1 d . . . . .
N4 N 0.8581(7) 0.8100(8) 0.3699(9) 0.047(3) Uani 1 1 d . . . . .
H4 H 0.8582 0.7827 0.4077 0.057 Uiso 1 1 calc R U . . .
C1 C 0.8315(19) 1.1719(12) 0.3569(12) 0.090(9) Uani 1 1 d . U . . .
H1A H 0.8088 1.2104 0.3312 0.135 Uiso 1 1 calc R U . . .
H1B H 0.8758 1.1885 0.3774 0.135 Uiso 1 1 calc R U . . .
H1C H 0.8008 1.1556 0.3954 0.135 Uiso 1 1 calc R U . . .
C2 C 0.7814(6) 1.0968(6) 0.2765(7) 0.065(5) Uani 1 1 d G U . . .
C3 C 0.7146(7) 1.1260(6) 0.2910(9) 0.092(7) Uani 1 1 d G U . . .
H3 H 0.7104 1.1641 0.3233 0.110 Uiso 1 1 calc R U . . .
C4 C 0.6541(5) 1.0984(7) 0.2572(10) 0.088(7) Uani 1 1 d G U . . .
H4A H 0.6094 1.1179 0.2670 0.105 Uiso 1 1 calc R U . . .
C5 C 0.6604(5) 1.0415(7) 0.2089(8) 0.067(5) Uani 1 1 d G U . . .
H5 H 0.6199 1.0230 0.1863 0.081 Uiso 1 1 calc R U . . .
C6 C 0.7272(6) 1.0122(6) 0.1944(6) 0.053(4) Uani 1 1 d G U . . .
C7 C 0.7877(5) 1.0399(5) 0.2282(7) 0.049(4) Uani 1 1 d G U . . .
C8 C 0.7298(9) 0.9486(11) 0.1485(10) 0.052(4) Uani 1 1 d . . . . .
H8 H 0.6908 0.9395 0.1184 0.062 Uiso 1 1 calc R U . . .
C9 C 0.8212(8) 0.7933(8) 0.1091(9) 0.040(3) Uani 1 1 d . . . . .
C10 C 0.8475(13) 0.6767(13) 0.0656(12) 0.070(6) Uani 1 1 d . . . . .
H10A H 0.8867 0.6807 0.0321 0.105 Uiso 1 1 calc R U . . .
H10B H 0.8186 0.6362 0.0528 0.105 Uiso 1 1 calc R U . . .
H10C H 0.8656 0.6707 0.1142 0.105 Uiso 1 1 calc R U . . .
C11 C 1.2085(8) 0.8063(9) 0.1148(9) 0.044(3) Uani 1 1 d . . . . .
H11A H 1.2029 0.7706 0.0776 0.066 Uiso 1 1 calc R U . . .
H11B H 1.2403 0.7887 0.1518 0.066 Uiso 1 1 calc R U . . .
H11C H 1.2280 0.8490 0.0937 0.066 Uiso 1 1 calc R U . . .
C12 C 1.1091(8) 0.7670(9) 0.1903(8) 0.041(3) Uani 1 1 d . . . . .
C13 C 1.1412(8) 0.7041(9) 0.2025(8) 0.043(4) Uani 1 1 d . . . . .
H13 H 1.1846 0.6938 0.1803 0.052 Uiso 1 1 calc R U . . .
C14 C 1.1093(9) 0.6539(9) 0.2489(11) 0.050(4) Uani 1 1 d . . . . .
H14 H 1.1292 0.6087 0.2550 0.060 Uiso 1 1 calc R U . . .
C15 C 1.0466(8) 0.6732(9) 0.2861(10) 0.046(4) Uani 1 1 d . . . . .
H15 H 1.0270 0.6419 0.3201 0.056 Uiso 1 1 calc R U . . .
C16 C 1.0144(9) 0.7362(8) 0.2733(8) 0.039(3) Uani 1 1 d . . . . .
C17 C 1.0423(6) 0.7852(7) 0.2230(7) 0.029(3) Uani 1 1 d . . . . .
C18 C 0.9527(8) 0.7533(7) 0.3199(7) 0.034(3) Uani 1 1 d . . . . .
H18 H 0.9446 0.7222 0.3586 0.041 Uiso 1 1 calc R U . . .
C19 C 0.8101(9) 0.8605(7) 0.3583(11) 0.048(4) Uani 1 1 d . . . . .
C20 C 0.7103(12) 0.9227(13) 0.4049(15) 0.087(9) Uani 1 1 d . . . . .
H20A H 0.6758 0.9059 0.3702 0.130 Uiso 1 1 calc R U . . .
H20B H 0.7317 0.9660 0.3872 0.130 Uiso 1 1 calc R U . . .
H20C H 0.6871 0.9318 0.4506 0.130 Uiso 1 1 calc R U . . .
C21 C 0.8208(7) 0.9960(7) 0.0017(7) 0.029(3) Uani 1 1 d . . . . .
C22 C 0.7464(7) 0.9836(10) -0.0286(7) 0.040(4) Uani 1 1 d . . . . .
H22A H 0.7130 1.0140 -0.0037 0.060 Uiso 1 1 calc R U . . .
H22B H 0.7332 0.9346 -0.0215 0.060 Uiso 1 1 calc R U . . .
H22C H 0.7460 0.9945 -0.0798 0.060 Uiso 1 1 calc R U . . .
C23 C 1.0000 1.0000 0.2946(10) 0.029(4) Uani 1 2 d S T P . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ho1 O2 2.317(10) . ?
Ho1 O6 2.355(9) . ?
Ho1 O7 2.363(10) . ?
Ho1 O9 2.374(9) . ?
Ho1 O12 2.397(10) . ?
Ho1 O3 2.422(9) . ?
Ho1 N3 2.500(11) . ?
Ho1 O13 2.5860(6) . ?
Ho1 N1 2.629(11) . ?
Ho1 C23 2.920(9) . ?
Ho1 Ho2 3.5926(8) . ?
Ho1 Ho2 3.6179(8) 3_775 ?
Ho2 O2 2.300(10) . ?
Ho2 O11 2.303(9) 2_575 ?
Ho2 O6 2.344(9) 3_775 ?
Ho2 O9 2.353(9) 3_775 ?
Ho2 O9 2.356(10) . ?
Ho2 O10 2.373(10) . ?
Ho2 O5 2.457(10) 3_775 ?
Ho2 O13 2.497(7) . ?
Ho2 Ho1 3.6179(8) 3_775 ?
Ho2 Ho2 3.6445(11) 3_775 ?
O1 C1 1.37(2) . ?
O1 C2 1.39(2) . ?
O2 C7 1.375(12) . ?
O3 C9 1.240(19) . ?
O4 C9 1.37(2) . ?
O4 C10 1.38(3) . ?
O5 C12 1.413(19) . ?
O5 C11 1.462(18) . ?
O5 Ho2 2.457(10) 3_775 ?
O6 C17 1.343(16) . ?
O6 Ho2 2.344(9) 3_775 ?
O7 C19 1.22(2) . ?
O8 C19 1.339(19) . ?
O8 C20 1.46(2) . ?
O9 Ho2 2.353(9) 3_775 ?
O10 C21 1.254(17) . ?
O11 C21 1.282(18) . ?
O11 Ho2 2.303(9) 4_755 ?
O12 C23 1.276(14) . ?
O13 C23 1.38(2) . ?
O13 Ho2 2.497(7) 3_775 ?
O13 Ho1 2.5860(6) 3_775 ?
N1 C8 1.27(2) . ?
N1 N2 1.41(2) . ?
N2 C9 1.32(2) . ?
N2 H2 0.8600 . ?
N3 C18 1.287(19) . ?
N3 N4 1.393(18) . ?
N4 C19 1.32(2) . ?
N4 H4 0.8600 . ?
C1 H1A 0.9600 . ?
C1 H1B 0.9600 . ?
C1 H1C 0.9600 . ?
C2 C3 1.3900 . ?
C2 C7 1.3900 . ?
C3 C4 1.3900 . ?
C3 H3 0.9300 . ?
C4 C5 1.3900 . ?
C4 H4A 0.9300 . ?
C5 C6 1.3900 . ?
C5 H5 0.9300 . ?
C6 C7 1.3900 . ?
C6 C8 1.46(2) . ?
C8 H8 0.9300 . ?
C10 H10A 0.9600 . ?
C10 H10B 0.9600 . ?
C10 H10C 0.9600 . ?
C11 H11A 0.9600 . ?
C11 H11B 0.9600 . ?
C11 H11C 0.9600 . ?
C12 C13 1.34(2) . ?
C12 C17 1.43(2) . ?
C13 C14 1.40(2) . ?
C13 H13 0.9300 . ?
C14 C15 1.40(2) . ?
C14 H14 0.9300 . ?
C15 C16 1.34(2) . ?
C15 H15 0.9300 . ?
C16 C17 1.40(2) . ?
C16 C18 1.47(2) . ?
C18 H18 0.9300 . ?
C20 H20A 0.9600 . ?
C20 H20B 0.9600 . ?
C20 H20C 0.9600 . ?
C21 C22 1.517(17) . ?
C22 H22A 0.9600 . ?
C22 H22B 0.9600 . ?
C22 H22C 0.9600 . ?
C23 O12 1.277(14) 3_775 ?
C23 Ho1 2.920(9) 3_775 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O2 Ho1 O6 136.2(3) . . ?
O2 Ho1 O7 78.4(3) . . ?
O6 Ho1 O7 138.3(3) . . ?
O2 Ho1 O9 75.5(4) . . ?
O6 Ho1 O9 73.9(3) . . ?
O7 Ho1 O9 147.6(4) . . ?
O2 Ho1 O12 81.7(4) . . ?
O6 Ho1 O12 83.1(4) . . ?
O7 Ho1 O12 80.2(4) . . ?
O9 Ho1 O12 114.4(3) . . ?
O2 Ho1 O3 128.8(4) . . ?
O6 Ho1 O3 77.1(3) . . ?
O7 Ho1 O3 99.1(4) . . ?
O9 Ho1 O3 82.7(3) . . ?
O12 Ho1 O3 149.1(4) . . ?
O2 Ho1 N3 138.2(4) . . ?
O6 Ho1 N3 74.4(3) . . ?
O7 Ho1 N3 64.4(4) . . ?
O9 Ho1 N3 145.7(4) . . ?
O12 Ho1 N3 74.1(4) . . ?
O3 Ho1 N3 77.8(4) . . ?
O2 Ho1 O13 67.5(2) . . ?
O6 Ho1 O13 70.4(2) . . ?
O7 Ho1 O13 124.7(3) . . ?
O9 Ho1 O13 60.9(3) . . ?
O12 Ho1 O13 53.6(3) . . ?
O3 Ho1 O13 136.2(3) . . ?
N3 Ho1 O13 118.8(3) . . ?
O2 Ho1 N1 67.7(4) . . ?
O6 Ho1 N1 135.2(4) . . ?
O7 Ho1 N1 71.6(4) . . ?
O9 Ho1 N1 80.7(4) . . ?
O12 Ho1 N1 141.6(4) . . ?
O3 Ho1 N1 63.3(4) . . ?
N3 Ho1 N1 114.0(4) . . ?
O13 Ho1 N1 126.4(3) . . ?
O2 Ho1 C23 72.6(3) . . ?
O6 Ho1 C23 76.2(2) . . ?
O7 Ho1 C23 101.4(4) . . ?
O9 Ho1 C23 89.0(4) . . ?
O12 Ho1 C23 25.4(4) . . ?
O3 Ho1 C23 153.3(3) . . ?
N3 Ho1 C23 95.9(4) . . ?
O13 Ho1 C23 28.2(4) . . ?
N1 Ho1 C23 140.3(3) . . ?
O2 Ho1 Ho2 38.7(2) . . ?
O6 Ho1 Ho2 100.0(2) . . ?
O7 Ho1 Ho2 117.2(2) . . ?
O9 Ho1 Ho2 40.4(2) . . ?
O12 Ho1 Ho2 88.0(2) . . ?
O3 Ho1 Ho2 118.5(2) . . ?
N3 Ho1 Ho2 161.7(3) . . ?
O13 Ho1 Ho2 44.03(16) . . ?
N1 Ho1 Ho2 82.4(3) . . ?
C23 Ho1 Ho2 65.8(3) . . ?
O2 Ho1 Ho2 98.6(2) . 3_775 ?
O6 Ho1 Ho2 39.5(2) . 3_775 ?
O7 Ho1 Ho2 166.6(3) . 3_775 ?
O9 Ho1 Ho2 39.8(2) . 3_775 ?
O12 Ho1 Ho2 86.6(3) . 3_775 ?
O3 Ho1 Ho2 92.9(2) . 3_775 ?
N3 Ho1 Ho2 113.1(3) . 3_775 ?
O13 Ho1 Ho2 43.64(16) . 3_775 ?
N1 Ho1 Ho2 119.6(3) . 3_775 ?
C23 Ho1 Ho2 65.5(3) . 3_775 ?
Ho2 Ho1 Ho2 60.719(17) . 3_775 ?
O2 Ho2 O11 152.3(4) . 2_575 ?
O2 Ho2 O6 97.8(4) . 3_775 ?
O11 Ho2 O6 96.0(3) 2_575 3_775 ?
O2 Ho2 O9 131.3(4) . 3_775 ?
O11 Ho2 O9 75.7(3) 2_575 3_775 ?
O6 Ho2 O9 74.5(3) 3_775 3_775 ?
O2 Ho2 O9 76.2(3) . . ?
O11 Ho2 O9 110.5(3) 2_575 . ?
O6 Ho2 O9 133.4(3) 3_775 . ?
O9 Ho2 O9 75.9(4) 3_775 . ?
O2 Ho2 O10 81.4(4) . . ?
O11 Ho2 O10 73.9(4) 2_575 . ?
O6 Ho2 O10 146.6(3) 3_775 . ?
O9 Ho2 O10 130.2(3) 3_775 . ?
O9 Ho2 O10 79.1(3) . . ?
O2 Ho2 O5 85.4(4) . 3_775 ?
O11 Ho2 O5 78.7(4) 2_575 3_775 ?
O6 Ho2 O5 65.6(3) 3_775 3_775 ?
O9 Ho2 O5 129.3(3) 3_775 3_775 ?
O9 Ho2 O5 154.7(3) . 3_775 ?
O10 Ho2 O5 81.1(3) . 3_775 ?
O2 Ho2 O13 69.3(3) . . ?
O11 Ho2 O13 138.1(3) 2_575 . ?
O6 Ho2 O13 72.2(2) 3_775 . ?
O9 Ho2 O13 62.5(3) 3_775 . ?
O9 Ho2 O13 62.5(3) . . ?
O10 Ho2 O13 135.7(3) . . ?
O5 Ho2 O13 126.6(3) 3_775 . ?
O2 Ho2 Ho1 39.1(2) . . ?
O11 Ho2 Ho1 150.5(2) 2_575 . ?
O6 Ho2 Ho1 109.9(2) 3_775 . ?
O9 Ho2 Ho1 97.4(2) 3_775 . ?
O9 Ho2 Ho1 40.8(2) . . ?
O10 Ho2 Ho1 90.5(3) . . ?
O5 Ho2 Ho1 124.4(3) 3_775 . ?
O13 Ho2 Ho1 46.038(13) . . ?
O2 Ho2 Ho1 106.0(3) . 3_775 ?
O11 Ho2 Ho1 100.0(2) 2_575 3_775 ?
O6 Ho2 Ho1 39.8(2) 3_775 3_775 ?
O9 Ho2 Ho1 40.3(2) 3_775 3_775 ?
O9 Ho2 Ho1 96.6(2) . 3_775 ?
O10 Ho2 Ho1 170.5(2) . 3_775 ?
O5 Ho2 Ho1 105.1(2) 3_775 3_775 ?
O13 Ho2 Ho1 45.619(13) . 3_775 ?
Ho1 Ho2 Ho1 91.66(2) . 3_775 ?
O2 Ho2 Ho2 98.2(3) . 3_775 ?
O11 Ho2 Ho2 103.3(2) 2_575 3_775 ?
O6 Ho2 Ho2 98.8(2) 3_775 3_775 ?
O9 Ho2 Ho2 39.3(2) 3_775 3_775 ?
O9 Ho2 Ho2 39.3(2) . 3_775 ?
O10 Ho2 Ho2 114.4(2) . 3_775 ?
O5 Ho2 Ho2 164.4(2) 3_775 3_775 ?
O13 Ho2 Ho2 43.14(18) . 3_775 ?
Ho1 Ho2 Ho2 59.982(16) . 3_775 ?
Ho1 Ho2 Ho2 59.297(16) 3_775 3_775 ?
C1 O1 C2 109(2) . . ?
C7 O2 Ho2 126.5(8) . . ?
C7 O2 Ho1 127.9(7) . . ?
Ho2 O2 Ho1 102.2(4) . . ?
C9 O3 Ho1 122.8(9) . . ?
C9 O4 C10 119.2(16) . . ?
C12 O5 C11 115.5(11) . . ?
C12 O5 Ho2 119.0(9) . 3_775 ?
C11 O5 Ho2 125.4(8) . 3_775 ?
C17 O6 Ho2 124.8(8) . 3_775 ?
C17 O6 Ho1 134.0(8) . . ?
Ho2 O6 Ho1 100.7(3) 3_775 . ?
C19 O7 Ho1 119.9(10) . . ?
C19 O8 C20 114.7(14) . . ?
Ho2 O9 Ho2 101.4(3) 3_775 . ?
Ho2 O9 Ho1 99.9(3) 3_775 . ?
Ho2 O9 Ho1 98.9(4) . . ?
C21 O10 Ho2 133.4(9) . . ?
C21 O11 Ho2 137.5(8) . 4_755 ?
C23 O12 Ho1 100.9(9) . . ?
C23 O13 Ho2 133.14(18) . 3_775 ?
C23 O13 Ho2 133.14(18) . . ?
Ho2 O13 Ho2 93.7(4) 3_775 . ?
C23 O13 Ho1 89.5(2) . 3_775 ?
Ho2 O13 Ho1 89.93(16) 3_775 3_775 ?
Ho2 O13 Ho1 90.74(16) . 3_775 ?
C23 O13 Ho1 89.5(2) . . ?
Ho2 O13 Ho1 90.73(16) 3_775 . ?
Ho2 O13 Ho1 89.93(16) . . ?
Ho1 O13 Ho1 179.0(5) 3_775 . ?
C8 N1 N2 116.5(14) . . ?
C8 N1 Ho1 130.6(12) . . ?
N2 N1 Ho1 112.8(9) . . ?
C9 N2 N1 116.2(12) . . ?
C9 N2 H2 121.9 . . ?
N1 N2 H2 121.9 . . ?
C18 N3 N4 114.8(12) . . ?
C18 N3 Ho1 129.9(9) . . ?
N4 N3 Ho1 115.3(9) . . ?
C19 N4 N3 112.6(15) . . ?
C19 N4 H4 123.7 . . ?
N3 N4 H4 123.7 . . ?
O1 C1 H1A 109.5 . . ?
O1 C1 H1B 109.5 . . ?
H1A C1 H1B 109.5 . . ?
O1 C1 H1C 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
O1 C2 C3 125.3(9) . . ?
O1 C2 C7 114.6(9) . . ?
C3 C2 C7 120.0 . . ?
C2 C3 C4 120.0 . . ?
C2 C3 H3 120.0 . . ?
C4 C3 H3 120.0 . . ?
C5 C4 C3 120.0 . . ?
C5 C4 H4A 120.0 . . ?
C3 C4 H4A 120.0 . . ?
C6 C5 C4 120.0 . . ?
C6 C5 H5 120.0 . . ?
C4 C5 H5 120.0 . . ?
C5 C6 C7 120.0 . . ?
C5 C6 C8 117.5(9) . . ?
C7 C6 C8 122.3(10) . . ?
O2 C7 C6 121.7(8) . . ?
O2 C7 C2 118.1(8) . . ?
C6 C7 C2 120.0 . . ?
N1 C8 C6 124.5(16) . . ?
N1 C8 H8 117.7 . . ?
C6 C8 H8 117.7 . . ?
O3 C9 N2 124.4(14) . . ?
O3 C9 O4 125.4(16) . . ?
N2 C9 O4 110.0(14) . . ?
O4 C10 H10A 109.5 . . ?
O4 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
O4 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
O5 C11 H11A 109.5 . . ?
O5 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
O5 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
C13 C12 O5 123.9(14) . . ?
C13 C12 C17 122.1(15) . . ?
O5 C12 C17 114.0(14) . . ?
C12 C13 C14 120.0(14) . . ?
C12 C13 H13 120.0 . . ?
C14 C13 H13 120.0 . . ?
C13 C14 C15 118.6(13) . . ?
C13 C14 H14 120.7 . . ?
C15 C14 H14 120.7 . . ?
C16 C15 C14 120.9(15) . . ?
C16 C15 H15 119.5 . . ?
C14 C15 H15 119.5 . . ?
C15 C16 C17 121.6(15) . . ?
C15 C16 C18 116.1(13) . . ?
C17 C16 C18 122.1(13) . . ?
O6 C17 C16 127.0(13) . . ?
O6 C17 C12 116.4(13) . . ?
C16 C17 C12 116.5(13) . . ?
N3 C18 C16 128.5(12) . . ?
N3 C18 H18 115.8 . . ?
C16 C18 H18 115.8 . . ?
O7 C19 N4 126.1(15) . . ?
O7 C19 O8 121.7(14) . . ?
N4 C19 O8 112.1(17) . . ?
O8 C20 H20A 109.5 . . ?
O8 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
O8 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
O10 C21 O11 122.6(12) . . ?
O10 C21 C22 121.6(14) . . ?
O11 C21 C22 115.7(12) . . ?
C21 C22 H22A 109.5 . . ?
C21 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
C21 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
O12 C23 O12 128.0(17) . 3_775 ?
O12 C23 O13 116.0(9) . . ?
O12 C23 O13 116.0(9) 3_775 . ?
O12 C23 Ho1 177.3(9) . 3_775 ?
O12 C23 Ho1 53.7(6) 3_775 3_775 ?
O13 C23 Ho1 62.3(3) . 3_775 ?
O12 C23 Ho1 53.7(6) . . ?
O12 C23 Ho1 177.3(9) 3_775 . ?
O13 C23 Ho1 62.3(3) . . ?
Ho1 C23 Ho1 124.6(7) 3_775 . ?

_refine_diff_density_max         1.018
_refine_diff_density_min         -0.688
_refine_diff_density_rms         0.142



