# 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 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_2
_database_code_depnum_ccdc_archive 'CCDC 1832173'
loop_
_audit_author_name
_audit_author_address
'Wen-Min Wang'
;Taiyuan Normal University
China
;
_audit_update_record             
;
2019-04-08 deposited with the CCDC.	2019-04-09 downloaded from the CCDC.
;
_audit_creation_date             2019-02-24
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2016/6
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C60 H56 N12 O16 Tb4, 4(C H4 O)'
_chemical_formula_sum            'C64 H72 N12 O20 Tb4'
_chemical_formula_weight         1965.01
_chemical_melting_point          ?
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'

_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.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 1 2/c 1'
_space_group_name_Hall           '-C 2yc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'

_cell_length_a                   28.3380(9)
_cell_length_b                   8.4206(3)
_cell_length_c                   30.5231(11)
_cell_angle_alpha                90
_cell_angle_beta                 110.1814(12)
_cell_angle_gamma                90
_cell_volume                     6836.3(4)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    9135
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      26.39
_cell_measurement_theta_min      2.54
_shelx_estimated_absorpt_T_max   0.657
_shelx_estimated_absorpt_T_min   0.323
_exptl_absorpt_coefficient_mu    4.170
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.4992
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1008 before and 0.0612 after correction.
The Ratio of minimum to maximum transmission is 0.6697.
The λ/2 correction factor is Not present.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.909
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             3840
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.11
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0616
_diffrn_reflns_av_unetI/netI     0.0360
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -34
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            50673
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.020
_diffrn_reflns_theta_min         2.423
_diffrn_ambient_temperature      150.0
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                5479
_reflns_number_total             6726
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    
;
Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_refine_diff_density_max         0.775
_refine_diff_density_min         -1.195
_refine_diff_density_rms         0.135
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     463
_refine_ls_number_reflns         6726
_refine_ls_number_restraints     13
_refine_ls_R_factor_all          0.0457
_refine_ls_R_factor_gt           0.0289
_refine_ls_restrained_S_all      1.055
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0262P)²+28.5118P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0584
_refine_ls_wR_factor_ref         0.0641
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2. Restrained distances
 O1-H1
 0.87 with sigma of 0.01
 O4-H4
 0.87 with sigma of 0.01
 C1-H1
 1.891762 with sigma of 0.02
 Tb1-H1
 3.022987 with sigma of 0.02
 C15-H4
 1.893235 with sigma of 0.02
 Tb2-H4
 3.059012 with sigma of 0.02
3. Rigid bond restraints
 O10, C32
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
4. Uiso/Uaniso restraints and constraints
Uanis(C32) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
5.a Secondary CH2 refined with riding coordinates:
 C15(H15A,H15B), C1(H1A,H1B)
5.b Aromatic/amide H refined with riding coordinates:
 C24(H24), C27(H27), C5(H5), C11(H11), C8(H8), C10(H10), C22(H22), C3(H3),
 C25(H25), C13(H13), C19(H19), C18(H18), C17(H17), C4(H4A), C12(H12), C26(H26)
5.c Idealised Me refined as rotating group:
 C30(H30A,H30B,H30C), C31(H31A,H31B,H31C), C29(H29A,H29B,H29C), C32(H32A,H32B,
 H32C)
5.d Idealised tetrahedral OH refined as rotating group:
 O10(H10A), O9(H9)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   ?
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
Tb2 Tb 0.41103(2) 0.74072(2) 0.17714(2) 0.01715(6) Uani 1 1 d D . . . .
Tb1 Tb 0.44937(2) 0.70799(2) 0.31173(2) 0.01788(6) Uani 1 1 d D . . . .
O8 O 0.51483(10) 0.8712(3) 0.31436(10) 0.0201(7) Uani 1 1 d . . . . .
O7 O 0.43328(11) 0.5784(3) 0.24150(10) 0.0193(6) Uani 1 1 d . . . . .
O3 O 0.67386(11) 0.6954(4) 0.33857(11) 0.0242(7) Uani 1 1 d . . . . .
O4 O 0.38690(12) 0.8694(4) 0.09930(11) 0.0285(7) Uani 1 1 d D . . . .
H4 H 0.4052(13) 0.858(4) 0.0815(10) 0.043 Uiso 1 1 d DR . . . .
O1 O 0.37068(12) 0.5737(4) 0.30620(11) 0.0285(7) Uani 1 1 d D . . . .
H1 H 0.3448(8) 0.578(4) 0.2802(8) 0.043 Uiso 1 1 d DR . . . .
C24 C 0.3471(2) 0.8422(7) 0.41847(17) 0.0398(13) Uani 1 1 d . . . . .
H24 H 0.317528 0.905350 0.407353 0.048 Uiso 1 1 calc R . . . .
O6 O 0.45903(12) 0.7508(3) 0.38921(11) 0.0258(7) Uani 1 1 d . . . . .
N2 N 0.58779(14) 0.4286(4) 0.39768(13) 0.0233(8) Uani 1 1 d . . . . .
O10 O 0.54708(15) 0.8601(6) 0.44132(13) 0.0590(12) Uani 1 1 d . U . . .
H10A H 0.521411 0.810957 0.424560 0.089 Uiso 1 1 calc GR . . . .
C7 C 0.54224(16) 0.4677(5) 0.37192(15) 0.0184(9) Uani 1 1 d . . . . .
O9 O 0.29690(13) 0.5916(5) 0.22887(13) 0.0436(10) Uani 1 1 d . . . . .
H9 H 0.304436 0.620918 0.205814 0.065 Uiso 1 1 calc GR . . . .
N6 N 0.38681(14) 0.9209(4) 0.31896(13) 0.0234(8) Uani 1 1 d . . . . .
C21 C 0.37682(16) 0.9829(5) 0.24592(16) 0.0200(9) Uani 1 1 d . . . . .
C6 C 0.49993(17) 0.3801(5) 0.37947(15) 0.0216(10) Uani 1 1 d . . . . .
C28 C 0.42542(19) 0.7503(5) 0.41031(16) 0.0282(11) Uani 1 1 d . . . . .
C27 C 0.4343(2) 0.6624(6) 0.45174(17) 0.0382(13) Uani 1 1 d . . . . .
H27 H 0.464084 0.600589 0.463751 0.046 Uiso 1 1 calc R . . . .
C5 C 0.50649(19) 0.2548(5) 0.41010(17) 0.0277(11) Uani 1 1 d . . . . .
H5 H 0.539171 0.215736 0.427034 0.033 Uiso 1 1 calc R . . . .
C11 C 0.79419(19) 0.7013(6) 0.46292(18) 0.0368(12) Uani 1 1 d . . . . .
H11 H 0.822011 0.702329 0.491346 0.044 Uiso 1 1 calc R . . . .
C8 C 0.66654(17) 0.5217(5) 0.41834(16) 0.0256(10) Uani 1 1 d . . . . .
H8 H 0.670918 0.452223 0.443975 0.031 Uiso 1 1 calc R . . . .
N3 N 0.62220(13) 0.5280(4) 0.38689(13) 0.0214(8) Uani 1 1 d . . . . .
C10 C 0.75225(17) 0.6109(6) 0.45879(17) 0.0301(11) Uani 1 1 d . . . . .
H10 H 0.752071 0.546986 0.484386 0.036 Uiso 1 1 calc R . . . .
N4 N 0.36473(13) 1.0111(4) 0.16510(13) 0.0217(8) Uani 1 1 d . . . . .
N5 N 0.36320(14) 1.0210(4) 0.28094(13) 0.0244(9) Uani 1 1 d . . . . .
C20 C 0.35289(16) 1.0688(5) 0.20130(16) 0.0212(10) Uani 1 1 d . . . . .
C22 C 0.36534(18) 0.9279(6) 0.35032(17) 0.0293(11) Uani 1 1 d . . . . .
H22 H 0.337700 0.998492 0.344606 0.035 Uiso 1 1 calc R . . . .
C16 C 0.34165(17) 1.0719(5) 0.12277(16) 0.0248(10) Uani 1 1 d . . . . .
C14 C 0.71167(16) 0.6980(5) 0.37868(16) 0.0237(10) Uani 1 1 d . . . . .
C23 C 0.38007(18) 0.8370(6) 0.39326(16) 0.0267(10) Uani 1 1 d . . . . .
C3 C 0.41787(19) 0.2492(5) 0.39137(17) 0.0290(11) Uani 1 1 d . . . . .
H3 H 0.388599 0.208425 0.395820 0.035 Uiso 1 1 calc R . . . .
N1 N 0.45424(13) 0.4378(4) 0.35409(12) 0.0203(8) Uani 1 1 d . . . . .
O2 O 0.52966(11) 0.5806(3) 0.34110(11) 0.0217(7) Uani 1 1 d . . . . .
C15 C 0.35708(19) 1.0072(6) 0.08408(16) 0.0312(11) Uani 1 1 d D . . . .
H15A H 0.326800 0.980705 0.056995 0.037 Uiso 1 1 calc R . . . .
H15B H 0.376466 1.088547 0.074079 0.037 Uiso 1 1 calc R . . . .
C2 C 0.41428(17) 0.3725(5) 0.36030(16) 0.0245(10) Uani 1 1 d . . . . .
C25 C 0.3570(2) 0.7561(8) 0.4595(2) 0.0499(16) Uani 1 1 d . . . . .
H25 H 0.334520 0.759952 0.476445 0.060 Uiso 1 1 calc R . . . .
C13 C 0.75480(18) 0.7871(6) 0.38363(18) 0.0290(11) Uani 1 1 d . . . . .
H13 H 0.756571 0.847245 0.357910 0.035 Uiso 1 1 calc R . . . .
C9 C 0.71011(16) 0.6107(5) 0.41807(16) 0.0242(10) Uani 1 1 d . . . . .
C19 C 0.31851(17) 1.1919(6) 0.19545(17) 0.0295(11) Uani 1 1 d . . . . .
H19 H 0.311512 1.232957 0.221541 0.035 Uiso 1 1 calc R . . . .
C18 C 0.29490(19) 1.2532(6) 0.15195(19) 0.0349(12) Uani 1 1 d . . . . .
H18 H 0.271493 1.337740 0.147454 0.042 Uiso 1 1 calc R . . . .
O5 O 0.40804(11) 0.8703(3) 0.24520(10) 0.0205(6) Uani 1 1 d . . . . .
C17 C 0.30551(18) 1.1908(5) 0.11469(17) 0.0295(11) Uani 1 1 d . . . . .
H17 H 0.288412 1.228260 0.083926 0.035 Uiso 1 1 calc R . . . .
C4 C 0.4643(2) 0.1871(6) 0.41561(18) 0.0341(12) Uani 1 1 d . . . . .
H4A H 0.467478 0.098925 0.435858 0.041 Uiso 1 1 calc R . . . .
C1 C 0.36417(17) 0.4394(6) 0.33141(17) 0.0310(11) Uani 1 1 d D . . . .
H1A H 0.344470 0.357549 0.309363 0.037 Uiso 1 1 calc R . . . .
H1B H 0.345253 0.470184 0.351957 0.037 Uiso 1 1 calc R . . . .
C12 C 0.79522(18) 0.7895(6) 0.42551(19) 0.0344(12) Uani 1 1 d . . . . .
H12 H 0.823824 0.852887 0.428212 0.041 Uiso 1 1 calc R . . . .
C26 C 0.3999(2) 0.6652(7) 0.47531(19) 0.0496(16) Uani 1 1 d . . . . .
H26 H 0.406280 0.603238 0.502755 0.060 Uiso 1 1 calc R . . . .
C30 C 0.51060(19) 1.0383(5) 0.3127(2) 0.0377(13) Uani 1 1 d . . . . .
H30A H 0.532574 1.083318 0.342295 0.057 Uiso 1 1 calc GR . . . .
H30B H 0.475691 1.068535 0.307484 0.057 Uiso 1 1 calc GR . . . .
H30C H 0.520597 1.078988 0.287092 0.057 Uiso 1 1 calc GR . . . .
C31 C 0.2646(2) 0.7066(9) 0.2382(2) 0.066(2) Uani 1 1 d . . . . .
H31A H 0.229687 0.683792 0.219076 0.099 Uiso 1 1 calc GR . . . .
H31B H 0.273769 0.812810 0.230645 0.099 Uiso 1 1 calc GR . . . .
H31C H 0.268334 0.702374 0.271310 0.099 Uiso 1 1 calc GR . . . .
C29 C 0.4324(2) 0.4115(6) 0.23745(18) 0.0405(14) Uani 1 1 d . . . . .
H29A H 0.406341 0.368147 0.248357 0.061 Uiso 1 1 calc GR . . . .
H29B H 0.465227 0.368351 0.256457 0.061 Uiso 1 1 calc GR . . . .
H29C H 0.425122 0.381974 0.204709 0.061 Uiso 1 1 calc GR . . . .
C32 C 0.5633(3) 0.7973(15) 0.4831(3) 0.148(5) Uani 1 1 d . U . . .
H32A H 0.576371 0.690554 0.481507 0.221 Uiso 1 1 calc GR . . . .
H32B H 0.535540 0.790706 0.495253 0.221 Uiso 1 1 calc GR . . . .
H32C H 0.590156 0.863697 0.503896 0.221 Uiso 1 1 calc GR . . . .


_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
Tb2 O8 2.305(3) 2_655 ?
Tb2 O7 2.296(3) . ?
Tb2 O3 2.317(3) 2_655 ?
Tb2 O4 2.483(3) . ?
Tb2 N3 2.578(4) 2_655 ?
Tb2 N4 2.590(3) . ?
Tb2 O2 2.366(3) 2_655 ?
Tb2 O5 2.374(3) . ?
Tb1 O8 2.287(3) . ?
Tb1 O7 2.306(3) . ?
Tb1 O1 2.454(3) . ?
Tb1 O6 2.313(3) . ?
Tb1 N6 2.584(4) . ?
Tb1 N1 2.597(3) . ?
Tb1 O2 2.392(3) . ?
Tb1 O5 2.392(3) . ?
O8 C30 1.412(5) . ?
O7 C29 1.411(5) . ?
O3 C14 1.320(5) . ?
O4 C15 1.417(5) . ?
O1 C1 1.415(5) . ?
C24 C23 1.402(6) . ?
C24 C25 1.390(8) . ?
O6 C28 1.321(5) . ?
N2 C7 1.301(5) . ?
N2 N3 1.408(5) . ?
O10 C32 1.309(9) . ?
C7 C6 1.492(6) . ?
C7 O2 1.297(5) . ?
O9 C31 1.426(7) . ?
N6 N5 1.403(5) . ?
N6 C22 1.301(5) . ?
C21 N5 1.296(5) . ?
C21 C20 1.483(6) . ?
C21 O5 1.303(5) . ?
C6 C5 1.380(6) . ?
C6 N1 1.349(6) . ?
C28 C27 1.410(7) . ?
C28 C23 1.412(7) . ?
C27 C26 1.398(7) . ?
C5 C4 1.386(7) . ?
C11 C10 1.380(7) . ?
C11 C12 1.371(7) . ?
C8 N3 1.293(6) . ?
C8 C9 1.447(6) . ?
C10 C9 1.395(6) . ?
N4 C20 1.351(5) . ?
N4 C16 1.333(6) . ?
C20 C19 1.391(6) . ?
C22 C23 1.450(7) . ?
C16 C15 1.496(6) . ?
C16 C17 1.392(6) . ?
C14 C13 1.397(6) . ?
C14 C9 1.423(6) . ?
C3 C2 1.385(6) . ?
C3 C4 1.371(7) . ?
N1 C2 1.330(5) . ?
C2 C1 1.499(6) . ?
C25 C26 1.375(9) . ?
C13 C12 1.391(7) . ?
C19 C18 1.366(7) . ?
C18 C17 1.377(7) . ?

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
O8 Tb2 O3 160.56(10) 2_655 2_655 ?
O8 Tb2 O4 80.75(11) 2_655 . ?
O8 Tb2 N3 119.80(10) 2_655 2_655 ?
O8 Tb2 N4 89.69(10) 2_655 . ?
O8 Tb2 O2 66.68(9) 2_655 2_655 ?
O8 Tb2 O5 89.36(10) 2_655 . ?
O7 Tb2 O8 102.52(10) . 2_655 ?
O7 Tb2 O3 92.18(10) . 2_655 ?
O7 Tb2 O4 169.19(10) . . ?
O7 Tb2 N3 98.96(11) . 2_655 ?
O7 Tb2 N4 128.38(10) . . ?
O7 Tb2 O2 81.63(10) . 2_655 ?
O7 Tb2 O5 66.84(10) . . ?
O3 Tb2 O4 87.15(11) 2_655 . ?
O3 Tb2 N3 69.33(11) 2_655 2_655 ?
O3 Tb2 N4 71.11(11) 2_655 . ?
O3 Tb2 O2 128.95(10) 2_655 2_655 ?
O3 Tb2 O5 84.76(10) 2_655 . ?
O4 Tb2 N3 70.71(11) . 2_655 ?
O4 Tb2 N4 61.44(11) . . ?
N3 Tb2 N4 117.94(11) 2_655 . ?
O2 Tb2 O4 90.40(10) 2_655 . ?
O2 Tb2 N3 61.90(10) 2_655 2_655 ?
O2 Tb2 N4 146.49(11) 2_655 . ?
O2 Tb2 O5 135.28(10) 2_655 . ?
O5 Tb2 O4 123.77(10) . . ?
O5 Tb2 N3 150.32(10) . 2_655 ?
O5 Tb2 N4 63.31(11) . . ?
O8 Tb1 Tb2 32.90(7) . 2_655 ?
O8 Tb1 O7 102.39(10) . . ?
O8 Tb1 O1 170.39(10) . . ?
O8 Tb1 O6 93.56(10) . . ?
O8 Tb1 N6 98.75(11) . . ?
O8 Tb1 N1 127.28(11) . . ?
O8 Tb1 O2 66.51(10) . . ?
O8 Tb1 O5 80.81(10) . . ?
O7 Tb1 Tb2 89.06(7) . 2_655 ?
O7 Tb1 O1 80.47(10) . . ?
O7 Tb1 O6 160.00(10) . . ?
O7 Tb1 N6 119.09(11) . . ?
O7 Tb1 N1 90.45(10) . . ?
O7 Tb1 O2 89.64(10) . . ?
O7 Tb1 O5 66.37(10) . . ?
O1 Tb1 Tb2 156.65(8) . 2_655 ?
O1 Tb1 N6 72.03(11) . . ?
O1 Tb1 N1 61.41(11) . . ?
O6 Tb1 Tb2 98.20(8) . 2_655 ?
O6 Tb1 O1 85.77(11) . . ?
O6 Tb1 N6 69.34(11) . . ?
O6 Tb1 N1 70.15(11) . . ?
O6 Tb1 O2 85.71(11) . . ?
O6 Tb1 O5 129.01(10) . . ?
N6 Tb1 Tb2 130.93(8) . 2_655 ?
N6 Tb1 N1 119.06(11) . . ?
N1 Tb1 Tb2 98.16(8) . 2_655 ?
O2 Tb1 Tb2 35.53(6) . 2_655 ?
O2 Tb1 O1 122.92(10) . . ?
O2 Tb1 N6 150.58(11) . . ?
O2 Tb1 N1 62.63(10) . . ?
O5 Tb1 Tb2 102.74(7) . 2_655 ?
O5 Tb1 O1 92.15(10) . . ?
O5 Tb1 N6 61.75(10) . . ?
O5 Tb1 N1 148.16(11) . . ?
O5 Tb1 O2 134.27(10) . . ?
Tb1 O8 Tb2 114.48(11) . 2_655 ?
C30 O8 Tb2 122.8(3) . 2_655 ?
C30 O8 Tb1 122.7(3) . . ?
Tb2 O7 Tb1 114.94(11) . . ?
C29 O7 Tb2 121.8(3) . . ?
C29 O7 Tb1 123.0(3) . . ?
C14 O3 Tb2 129.9(3) . 2_655 ?
C15 O4 Tb2 127.4(3) . . ?
C1 O1 Tb1 128.1(3) . . ?
C25 C24 C23 120.8(6) . . ?
C28 O6 Tb1 130.3(3) . . ?
C7 N2 N3 109.3(3) . . ?
N2 C7 C6 117.6(4) . . ?
O2 C7 N2 126.2(4) . . ?
O2 C7 C6 116.1(4) . . ?
N5 N6 Tb1 119.4(2) . . ?
C22 N6 Tb1 127.1(3) . . ?
C22 N6 N5 111.8(4) . . ?
N5 C21 C20 117.7(4) . . ?
N5 C21 O5 126.3(4) . . ?
O5 C21 C20 116.0(4) . . ?
C5 C6 C7 123.8(4) . . ?
N1 C6 C7 113.4(4) . . ?
N1 C6 C5 122.9(4) . . ?
O6 C28 C27 120.2(5) . . ?
O6 C28 C23 122.4(4) . . ?
C27 C28 C23 117.4(4) . . ?
C26 C27 C28 120.8(6) . . ?
C6 C5 C4 118.5(5) . . ?
C12 C11 C10 119.2(5) . . ?
N3 C8 C9 126.0(4) . . ?
N2 N3 Tb2 119.3(3) . 2_655 ?
C8 N3 Tb2 126.8(3) . 2_655 ?
C8 N3 N2 112.1(4) . . ?
C11 C10 C9 121.8(5) . . ?
C20 N4 Tb2 117.2(3) . . ?
C16 N4 Tb2 122.0(3) . . ?
C16 N4 C20 118.5(4) . . ?
C21 N5 N6 109.9(3) . . ?
N4 C20 C21 114.3(4) . . ?
N4 C20 C19 121.6(4) . . ?
C19 C20 C21 124.0(4) . . ?
N6 C22 C23 125.4(4) . . ?
N4 C16 C15 116.5(4) . . ?
N4 C16 C17 122.2(4) . . ?
C17 C16 C15 121.3(4) . . ?
O3 C14 C13 120.6(4) . . ?
O3 C14 C9 121.6(4) . . ?
C13 C14 C9 117.8(4) . . ?
C24 C23 C28 120.6(5) . . ?
C24 C23 C22 116.2(5) . . ?
C28 C23 C22 123.2(4) . . ?
C4 C3 C2 119.1(4) . . ?
C6 N1 Tb1 118.5(3) . . ?
C2 N1 Tb1 122.1(3) . . ?
C2 N1 C6 117.7(4) . . ?
Tb2 O2 Tb1 108.49(11) 2_655 . ?
C7 O2 Tb2 123.2(3) . 2_655 ?
C7 O2 Tb1 126.0(3) . . ?
O4 C15 C16 110.1(4) . . ?
C3 C2 C1 121.0(4) . . ?
N1 C2 C3 122.8(4) . . ?
N1 C2 C1 116.1(4) . . ?
C26 C25 C24 119.1(5) . . ?
C12 C13 C14 121.3(5) . . ?
C10 C9 C8 117.7(4) . . ?
C10 C9 C14 119.0(4) . . ?
C14 C9 C8 123.2(4) . . ?
C18 C19 C20 119.6(4) . . ?
C19 C18 C17 119.0(4) . . ?
Tb2 O5 Tb1 109.01(11) . . ?
C21 O5 Tb2 125.4(3) . . ?
C21 O5 Tb1 122.6(3) . . ?
C18 C17 C16 119.0(5) . . ?
C3 C4 C5 119.0(4) . . ?
O1 C1 C2 110.2(4) . . ?
C11 C12 C13 120.7(5) . . ?
C25 C26 C27 121.2(5) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Tb2 O3 C14 C13 -128.9(4) 2_655 . . . ?
Tb2 O3 C14 C9 51.3(5) 2_655 . . . ?
Tb2 O4 C15 C16 1.1(6) . . . . ?
Tb2 N4 C20 C21 11.1(5) . . . . ?
Tb2 N4 C20 C19 -165.0(3) . . . . ?
Tb2 N4 C16 C15 -19.3(5) . . . . ?
Tb2 N4 C16 C17 161.6(3) . . . . ?
Tb1 O1 C1 C2 -6.3(6) . . . . ?
Tb1 O6 C28 C27 130.8(4) . . . . ?
Tb1 O6 C28 C23 -49.9(6) . . . . ?
Tb1 N6 N5 C21 2.1(5) . . . . ?
Tb1 N6 C22 C23 13.9(7) . . . . ?
Tb1 N1 C2 C3 -165.0(3) . . . . ?
Tb1 N1 C2 C1 15.2(5) . . . . ?
O3 C14 C13 C12 -179.2(4) . . . . ?
O3 C14 C9 C8 -4.0(7) . . . . ?
O3 C14 C9 C10 176.5(4) . . . . ?
C24 C25 C26 C27 2.2(9) . . . . ?
O6 C28 C27 C26 177.7(4) . . . . ?
O6 C28 C23 C24 -175.5(4) . . . . ?
O6 C28 C23 C22 2.8(7) . . . . ?
N2 C7 C6 C5 -3.9(6) . . . . ?
N2 C7 C6 N1 174.7(4) . . . . ?
N2 C7 O2 Tb2 1.8(6) . . . 2_655 ?
N2 C7 O2 Tb1 -159.1(3) . . . . ?
C7 N2 N3 Tb2 -1.2(4) . . . 2_655 ?
C7 N2 N3 C8 164.4(4) . . . . ?
C7 C6 C5 C4 177.3(4) . . . . ?
C7 C6 N1 Tb1 -11.1(5) . . . . ?
C7 C6 N1 C2 -176.6(4) . . . . ?
N6 C22 C23 C24 -169.8(5) . . . . ?
N6 C22 C23 C28 11.8(7) . . . . ?
C21 C20 C19 C18 -173.7(4) . . . . ?
C6 C7 O2 Tb2 179.2(3) . . . 2_655 ?
C6 C7 O2 Tb1 18.2(5) . . . . ?
C6 C5 C4 C3 -1.5(7) . . . . ?
C6 N1 C2 C3 0.0(6) . . . . ?
C6 N1 C2 C1 -179.8(4) . . . . ?
C28 C27 C26 C25 -1.5(8) . . . . ?
C27 C28 C23 C24 3.8(7) . . . . ?
C27 C28 C23 C22 -177.9(4) . . . . ?
C5 C6 N1 Tb1 167.4(3) . . . . ?
C5 C6 N1 C2 2.0(6) . . . . ?
C11 C10 C9 C8 -175.3(4) . . . . ?
C11 C10 C9 C14 4.1(7) . . . . ?
N3 N2 C7 C6 -177.6(3) . . . . ?
N3 N2 C7 O2 -0.3(6) . . . . ?
N3 C8 C9 C10 168.5(4) . . . . ?
N3 C8 C9 C14 -10.9(7) . . . . ?
C10 C11 C12 C13 -0.7(8) . . . . ?
N4 C20 C19 C18 2.0(7) . . . . ?
N4 C16 C15 O4 11.6(6) . . . . ?
N4 C16 C17 C18 3.2(7) . . . . ?
N5 N6 C22 C23 178.8(4) . . . . ?
N5 C21 C20 N4 -173.1(4) . . . . ?
N5 C21 C20 C19 2.9(6) . . . . ?
N5 C21 O5 Tb2 156.7(3) . . . . ?
N5 C21 O5 Tb1 -1.3(6) . . . . ?
C20 C21 N5 N6 175.8(4) . . . . ?
C20 C21 O5 Tb2 -19.8(5) . . . . ?
C20 C21 O5 Tb1 -177.8(3) . . . . ?
C20 N4 C16 C15 178.4(4) . . . . ?
C20 N4 C16 C17 -0.8(6) . . . . ?
C20 C19 C18 C17 0.4(7) . . . . ?
C22 N6 N5 C21 -164.2(4) . . . . ?
C16 N4 C20 C21 174.3(4) . . . . ?
C16 N4 C20 C19 -1.8(6) . . . . ?
C14 C13 C12 C11 1.4(7) . . . . ?
C23 C24 C25 C26 0.1(9) . . . . ?
C23 C28 C27 C26 -1.6(7) . . . . ?
C3 C2 C1 O1 174.0(4) . . . . ?
N1 C6 C5 C4 -1.2(7) . . . . ?
N1 C2 C1 O1 -6.2(6) . . . . ?
O2 C7 C6 C5 178.5(4) . . . . ?
O2 C7 C6 N1 -2.9(5) . . . . ?
C15 C16 C17 C18 -176.0(5) . . . . ?
C2 C3 C4 C5 3.3(7) . . . . ?
C25 C24 C23 C28 -3.2(8) . . . . ?
C25 C24 C23 C22 178.4(5) . . . . ?
C13 C14 C9 C8 176.2(4) . . . . ?
C13 C14 C9 C10 -3.3(6) . . . . ?
C9 C8 N3 Tb2 -14.8(6) . . . 2_655 ?
C9 C8 N3 N2 -179.1(4) . . . . ?
C9 C14 C13 C12 0.6(7) . . . . ?
C19 C18 C17 C16 -2.9(7) . . . . ?
O5 C21 N5 N6 -0.6(6) . . . . ?
O5 C21 C20 N4 3.8(5) . . . . ?
O5 C21 C20 C19 179.8(4) . . . . ?
C17 C16 C15 O4 -169.2(4) . . . . ?
C4 C3 C2 N1 -2.6(7) . . . . ?
C4 C3 C2 C1 177.2(5) . . . . ?
C12 C11 C10 C9 -2.1(8) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_3
_database_code_depnum_ccdc_archive 'CCDC 1832174'
loop_
_audit_author_name
_audit_author_address
'Wen-Min Wang'
;Taiyuan Normal University
China
;
_audit_update_record             
;
2019-04-08 deposited with the CCDC.	2019-04-09 downloaded from the CCDC.
;
_audit_creation_date             2019-02-24
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2016/6
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C60 H56 Dy4 N12 O16, 4(C H4 O)'
_chemical_formula_sum            'C64 H72 Dy4 N12 O20'
_chemical_formula_weight         1979.33
_chemical_melting_point          ?
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'

_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.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 1 2/c 1'
_space_group_name_Hall           '-C 2yc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'

_cell_length_a                   28.2350(16)
_cell_length_b                   8.4751(5)
_cell_length_c                   30.4106(14)
_cell_angle_alpha                90
_cell_angle_beta                 110.4302(15)
_cell_angle_gamma                90
_cell_volume                     6819.3(6)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    9889
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      26.40
_cell_measurement_theta_min      2.52
_shelx_estimated_absorpt_T_max   0.577
_shelx_estimated_absorpt_T_min   0.361
_exptl_absorpt_coefficient_mu    4.415
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.4039
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1378 before and 0.0627 after correction.
The Ratio of minimum to maximum transmission is 0.5419.
The λ/2 correction factor is Not present.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.928
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             3856
_exptl_crystal_size_max          0.29
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.14
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0459
_diffrn_reflns_av_unetI/netI     0.0288
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       35
_diffrn_reflns_limit_h_min       -35
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            49080
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.428
_diffrn_reflns_theta_min         2.439
_diffrn_ambient_temperature      149.98
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                6095
_reflns_number_total             6995
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    
;
Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_refine_diff_density_max         0.994
_refine_diff_density_min         -1.017
_refine_diff_density_rms         0.127
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     469
_refine_ls_number_reflns         6995
_refine_ls_number_restraints     38
_refine_ls_R_factor_all          0.0368
_refine_ls_R_factor_gt           0.0285
_refine_ls_restrained_S_all      1.063
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0295P)²+43.0549P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0646
_refine_ls_wR_factor_ref         0.0684
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2. Restrained distances
 O4-H4
 0.87 with sigma of 0.01
 H9-O9
 0.84 with sigma of 0.02
 O1-H1
 0.87 with sigma of 0.01
 O10-H10A
 0.84 with sigma of 0.02
 C15-H4
 1.894799 with sigma of 0.02
 Dy2-H4
 3.027688 with sigma of 0.02
 C1-H1
 1.897856 with sigma of 0.02
 Dy1-H1
 3.003858 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
O9 \\sim C31: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O9) \\sim Ueq, Uanis(C31) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C25) \\sim Ueq, Uanis(C26) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
4.a Secondary CH2 refined with riding coordinates:
 C15(H15A,H15B), C1(H1A,H1B)
4.b Aromatic/amide H refined with riding coordinates:
 C5(H5), C24(H24), C3(H3), C19(H19), C8(H8), C17(H17), C27(H27), C25(H25),
 C4(H4A), C22(H22), C12(H12), C10(H10), C13(H13), C18(H18), C26(H26), C11(H11)
4.c Idealised Me refined as rotating group:
 C29(H29A,H29B,H29C), C30(H30A,H30B,H30C), C32(H32A,H32B,H32C), C31(H31A,H31B,
 H31C)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   ?
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
Dy2 Dy 0.58908(2) 0.25780(2) 0.82258(2) 0.01698(6) Uani 1 1 d D . . . .
Dy1 Dy 0.44999(2) 0.29008(2) 0.81147(2) 0.01778(6) Uani 1 1 d D . . . .
O5 O 0.59104(11) 0.1303(3) 0.75425(9) 0.0224(6) Uani 1 1 d . . . . .
O8 O 0.56672(10) 0.4175(3) 0.75855(9) 0.0218(6) Uani 1 1 d . . . . .
O4 O 0.61384(12) 0.1360(4) 0.90073(10) 0.0304(7) Uani 1 1 d D . . . .
H4 H 0.5931(12) 0.142(4) 0.9166(10) 0.046 Uiso 1 1 d DR . . . .
O7 O 0.51534(10) 0.1294(3) 0.81408(9) 0.0211(6) Uani 1 1 d . . . . .
O6 O 0.53927(12) 0.2503(4) 0.61109(10) 0.0283(7) Uani 1 1 d . . . . .
O1 O 0.37078(11) 0.4177(4) 0.80551(11) 0.0297(7) Uani 1 1 d D . . . .
H1 H 0.3450(8) 0.416(4) 0.7789(8) 0.045 Uiso 1 1 d DR . . . .
C20 C 0.64623(16) -0.0684(5) 0.79870(14) 0.0232(9) Uani 1 1 d . . . . .
N2 N 0.58830(14) 0.5691(4) 0.89619(12) 0.0267(8) Uani 1 1 d . . . . .
O3 O 0.67369(11) 0.2993(4) 0.83804(10) 0.0263(7) Uani 1 1 d . . . . .
C21 C 0.62197(15) 0.0172(5) 0.75378(15) 0.0222(9) Uani 1 1 d . . . . .
C5 C 0.50684(19) 0.7428(5) 0.90832(16) 0.0312(10) Uani 1 1 d . . . . .
H5 H 0.539638 0.782384 0.925220 0.037 Uiso 1 1 calc R . . . .
O10 O 0.29653(13) 0.4063(5) 0.72848(13) 0.0491(10) Uani 1 1 d D . . . .
C24 C 0.6512(2) 0.1621(7) 0.58067(17) 0.0452(14) Uani 1 1 d . . . . .
H24 H 0.680941 0.099622 0.591468 0.054 Uiso 1 1 calc R . . . .
N1 N 0.45421(14) 0.5579(4) 0.85285(12) 0.0241(8) Uani 1 1 d . . . . .
C3 C 0.41715(19) 0.7468(5) 0.88931(17) 0.0323(11) Uani 1 1 d . . . . .
H3 H 0.387782 0.788149 0.893582 0.039 Uiso 1 1 calc R . . . .
C6 C 0.50014(16) 0.6164(5) 0.87793(14) 0.0247(9) Uani 1 1 d . . . . .
C19 C 0.68002(17) -0.1922(6) 0.80416(17) 0.0311(10) Uani 1 1 d . . . . .
H19 H 0.686407 -0.234137 0.777798 0.037 Uiso 1 1 calc R . . . .
N6 N 0.61149(13) 0.0794(4) 0.68028(12) 0.0253(8) Uani 1 1 d . . . . .
N5 N 0.63558(14) -0.0213(4) 0.71856(12) 0.0264(8) Uani 1 1 d . . . . .
N3 N 0.62295(13) 0.4693(4) 0.88589(12) 0.0248(8) Uani 1 1 d . . . . .
C28 C 0.57259(19) 0.2521(5) 0.58944(15) 0.0300(10) Uani 1 1 d . . . . .
C8 C 0.66740(16) 0.4763(5) 0.91756(15) 0.0272(9) Uani 1 1 d . . . . .
H8 H 0.671991 0.546177 0.943141 0.033 Uiso 1 1 calc R . . . .
C15 C 0.64309(19) -0.0019(6) 0.91633(16) 0.0339(11) Uani 1 1 d D . . . .
H15A H 0.623323 -0.080555 0.926761 0.041 Uiso 1 1 calc R . . . .
H15B H 0.673823 0.023974 0.943408 0.041 Uiso 1 1 calc R . . . .
C17 C 0.69404(18) -0.1891(5) 0.88566(17) 0.0328(11) Uani 1 1 d . . . . .
H17 H 0.711566 -0.225593 0.916633 0.039 Uiso 1 1 calc R . . . .
O9 O 0.54861(18) 0.1455(9) 0.94164(15) 0.098(2) Uani 1 1 d D U . . .
C9 C 0.71101(16) 0.3860(5) 0.91733(15) 0.0255(9) Uani 1 1 d . . . . .
N4 N 0.63465(13) -0.0097(4) 0.83491(12) 0.0223(7) Uani 1 1 d . . . . .
C23 C 0.61816(18) 0.1646(6) 0.60636(16) 0.0316(11) Uani 1 1 d . . . . .
C2 C 0.41339(17) 0.6217(5) 0.85874(15) 0.0268(9) Uani 1 1 d . . . . .
C27 C 0.5633(2) 0.3424(7) 0.54822(16) 0.0427(13) Uani 1 1 d . . . . .
H27 H 0.533605 0.404896 0.536777 0.051 Uiso 1 1 calc R . . . .
C25 C 0.6408(3) 0.2498(8) 0.53985(19) 0.0548(17) Uani 1 1 d . U . . .
H25 H 0.663219 0.247507 0.522755 0.066 Uiso 1 1 calc R . . . .
C7 C 0.54233(16) 0.5289(5) 0.87066(14) 0.0224(9) Uani 1 1 d . . . . .
C4 C 0.4640(2) 0.8101(6) 0.91336(17) 0.0364(11) Uani 1 1 d . . . . .
H4A H 0.467127 0.898893 0.933230 0.044 Uiso 1 1 calc R . . . .
C22 C 0.63300(17) 0.0734(6) 0.64911(16) 0.0302(10) Uani 1 1 d . . . . .
H22 H 0.660777 0.003403 0.654793 0.036 Uiso 1 1 calc R . . . .
C12 C 0.79608(18) 0.2040(6) 0.92550(18) 0.0371(11) Uani 1 1 d . . . . .
H12 H 0.824486 0.139292 0.928432 0.044 Uiso 1 1 calc R . . . .
C10 C 0.75358(17) 0.3855(6) 0.95894(16) 0.0319(10) Uani 1 1 d . . . . .
H10 H 0.753220 0.448508 0.984648 0.038 Uiso 1 1 calc R . . . .
C16 C 0.65788(16) -0.0700(5) 0.87767(15) 0.0259(9) Uani 1 1 d . . . . .
C14 C 0.71194(16) 0.2971(5) 0.87816(15) 0.0259(9) Uani 1 1 d . . . . .
O2 O 0.52992(10) 0.4156(3) 0.84016(10) 0.0230(6) Uani 1 1 d . . . . .
C13 C 0.75525(17) 0.2059(6) 0.88336(17) 0.0313(10) Uani 1 1 d . . . . .
H13 H 0.756647 0.144679 0.857677 0.038 Uiso 1 1 calc R . . . .
C1 C 0.36365(17) 0.5515(6) 0.83075(17) 0.0347(11) Uani 1 1 d D . . . .
H1A H 0.345514 0.519622 0.851920 0.042 Uiso 1 1 calc R . . . .
H1B H 0.342809 0.631013 0.808493 0.042 Uiso 1 1 calc R . . . .
C18 C 0.7041(2) -0.2531(6) 0.84818(19) 0.0384(12) Uani 1 1 d . . . . .
H18 H 0.727269 -0.338081 0.852734 0.046 Uiso 1 1 calc R . . . .
C26 C 0.5971(3) 0.3411(8) 0.52420(19) 0.0537(16) Uani 1 1 d . U . . .
H26 H 0.590223 0.403310 0.496694 0.064 Uiso 1 1 calc R . . . .
C29 C 0.51139(18) -0.0367(5) 0.81274(19) 0.0367(12) Uani 1 1 d . . . . .
H29A H 0.523368 -0.078034 0.788386 0.055 Uiso 1 1 calc GR . . . .
H29B H 0.476018 -0.067193 0.805643 0.055 Uiso 1 1 calc GR . . . .
H29C H 0.532053 -0.080257 0.843276 0.055 Uiso 1 1 calc GR . . . .
C11 C 0.79580(18) 0.2958(7) 0.96337(17) 0.0388(12) Uani 1 1 d . . . . .
H11 H 0.824136 0.296667 0.991731 0.047 Uiso 1 1 calc R . . . .
C30 C 0.5678(2) 0.5828(5) 0.76251(17) 0.0385(12) Uani 1 1 d . . . . .
H30A H 0.574727 0.612449 0.795314 0.058 Uiso 1 1 calc GR . . . .
H30B H 0.535097 0.626164 0.742900 0.058 Uiso 1 1 calc GR . . . .
H30C H 0.594467 0.625081 0.752094 0.058 Uiso 1 1 calc GR . . . .
C32 C 0.2635(2) 0.2944(10) 0.7379(2) 0.073(2) Uani 1 1 d . . . . .
H32A H 0.265796 0.303932 0.770676 0.109 Uiso 1 1 calc GR . . . .
H32B H 0.273393 0.187535 0.732231 0.109 Uiso 1 1 calc GR . . . .
H32C H 0.228694 0.314730 0.717200 0.109 Uiso 1 1 calc GR . . . .
C31 C 0.5605(3) 0.1725(15) 0.9849(3) 0.124(4) Uani 1 1 d . U . . .
H31A H 0.568553 0.284682 0.990999 0.186 Uiso 1 1 calc GR . . . .
H31B H 0.590105 0.108966 1.002412 0.186 Uiso 1 1 calc GR . . . .
H31C H 0.532173 0.144848 0.994981 0.186 Uiso 1 1 calc GR . . . .
H9 H 0.5215(18) 0.185(9) 0.923(2) 0.10(3) Uiso 1 1 d D . . . .
H10A H 0.304(2) 0.361(7) 0.7072(16) 0.057(19) Uiso 1 1 d 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
Dy2 Dy1 3.8434(3) 2_656 ?
Dy2 Dy1 3.8322(3) . ?
Dy2 O5 2.360(3) . ?
Dy2 O8 2.272(3) . ?
Dy2 O4 2.458(3) . ?
Dy2 O7 2.283(3) . ?
Dy2 O3 2.295(3) . ?
Dy2 N3 2.559(4) . ?
Dy2 N4 2.569(3) . ?
Dy2 O2 2.342(3) . ?
Dy1 O5 2.357(3) 2_656 ?
Dy1 O8 2.285(3) 2_656 ?
Dy1 O7 2.272(3) . ?
Dy1 O6 2.292(3) 2_656 ?
Dy1 O1 2.434(3) . ?
Dy1 N1 2.578(4) . ?
Dy1 N6 2.563(4) 2_656 ?
Dy1 O2 2.369(3) . ?
O5 C21 1.300(5) . ?
O8 C30 1.406(5) . ?
O4 H4 0.881(9) . ?
O4 C15 1.414(5) . ?
O7 C29 1.412(5) . ?
O6 C28 1.323(6) . ?
O1 H1 0.879(9) . ?
O1 C1 1.422(5) . ?
C20 C21 1.486(6) . ?
C20 C19 1.389(6) . ?
C20 N4 1.348(5) . ?
N2 N3 1.409(5) . ?
N2 C7 1.304(5) . ?
O3 C14 1.317(5) . ?
C21 N5 1.299(5) . ?
C5 H5 0.9500 . ?
C5 C6 1.384(6) . ?
C5 C4 1.393(7) . ?
O10 C32 1.427(8) . ?
O10 H10A 0.84(2) . ?
C24 H24 0.9500 . ?
C24 C23 1.410(7) . ?
C24 C25 1.387(8) . ?
N1 C6 1.349(6) . ?
N1 C2 1.340(5) . ?
C3 H3 0.9500 . ?
C3 C2 1.389(6) . ?
C3 C4 1.378(7) . ?
C6 C7 1.484(6) . ?
C19 H19 0.9500 . ?
C19 C18 1.373(7) . ?
N6 N5 1.412(5) . ?
N6 C22 1.293(5) . ?
N3 C8 1.289(5) . ?
C28 C23 1.417(7) . ?
C28 C27 1.413(7) . ?
C8 H8 0.9500 . ?
C8 C9 1.452(6) . ?
C15 H15A 0.9900 . ?
C15 H15B 0.9900 . ?
C15 C16 1.494(6) . ?
C17 H17 0.9500 . ?
C17 C16 1.395(6) . ?
C17 C18 1.379(7) . ?
O9 C31 1.260(9) . ?
O9 H9 0.85(2) . ?
C9 C10 1.409(6) . ?
C9 C14 1.417(6) . ?
N4 C16 1.337(5) . ?
C23 C22 1.443(7) . ?
C2 C1 1.489(7) . ?
C27 H27 0.9500 . ?
C27 C26 1.388(8) . ?
C25 H25 0.9500 . ?
C25 C26 1.392(9) . ?
C7 O2 1.296(5) . ?
C4 H4A 0.9500 . ?
C22 H22 0.9500 . ?
C12 H12 0.9500 . ?
C12 C13 1.393(7) . ?
C12 C11 1.392(8) . ?
C10 H10 0.9500 . ?
C10 C11 1.380(7) . ?
C14 C13 1.408(6) . ?
C13 H13 0.9500 . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C18 H18 0.9500 . ?
C26 H26 0.9500 . ?
C29 H29A 0.9800 . ?
C29 H29B 0.9800 . ?
C29 H29C 0.9800 . ?
C11 H11 0.9500 . ?
C30 H30A 0.9800 . ?
C30 H30B 0.9800 . ?
C30 H30C 0.9800 . ?
C32 H32A 0.9800 . ?
C32 H32B 0.9800 . ?
C32 H32C 0.9800 . ?
C31 H31A 0.9800 . ?
C31 H31B 0.9800 . ?
C31 H31C 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
Dy1 Dy2 Dy1 89.742(6) . 2_656 ?
O5 Dy2 Dy1 107.06(7) . . ?
O5 Dy2 Dy1 35.40(7) . 2_656 ?
O5 Dy2 O4 124.95(10) . . ?
O5 Dy2 N3 149.96(11) . . ?
O5 Dy2 N4 63.89(10) . . ?
O8 Dy2 Dy1 32.60(7) . 2_656 ?
O8 Dy2 Dy1 84.97(7) . . ?
O8 Dy2 O5 66.61(10) . . ?
O8 Dy2 O4 168.17(10) . . ?
O8 Dy2 O7 102.55(10) . . ?
O8 Dy2 O3 92.42(10) . . ?
O8 Dy2 N3 98.43(11) . . ?
O8 Dy2 N4 128.74(10) . . ?
O8 Dy2 O2 81.30(10) . . ?
O4 Dy2 Dy1 159.21(8) . 2_656 ?
O4 Dy2 Dy1 92.99(7) . . ?
O4 Dy2 N3 70.20(11) . . ?
O4 Dy2 N4 61.93(10) . . ?
O7 Dy2 Dy1 90.05(7) . 2_656 ?
O7 Dy2 Dy1 32.64(7) . . ?
O7 Dy2 O5 89.00(10) . . ?
O7 Dy2 O4 81.36(10) . . ?
O7 Dy2 O3 159.93(10) . . ?
O7 Dy2 N3 120.39(10) . . ?
O7 Dy2 N4 89.21(10) . . ?
O7 Dy2 O2 66.62(10) . . ?
O3 Dy2 Dy1 165.59(8) . . ?
O3 Dy2 Dy1 95.69(7) . 2_656 ?
O3 Dy2 O5 84.71(10) . . ?
O3 Dy2 O4 86.67(11) . . ?
O3 Dy2 N3 69.50(11) . . ?
O3 Dy2 N4 70.90(11) . . ?
O3 Dy2 O2 129.80(10) . . ?
N3 Dy2 Dy1 129.91(8) . 2_656 ?
N3 Dy2 Dy1 96.82(8) . . ?
N3 Dy2 N4 118.15(11) . . ?
N4 Dy2 Dy1 121.43(8) . . ?
N4 Dy2 Dy1 99.28(8) . 2_656 ?
O2 Dy2 Dy1 103.76(7) . 2_656 ?
O2 Dy2 Dy1 35.80(7) . . ?
O2 Dy2 O5 134.43(10) . . ?
O2 Dy2 O4 90.22(10) . . ?
O2 Dy2 N3 62.45(10) . . ?
O2 Dy2 N4 146.22(11) . . ?
Dy2 Dy1 Dy2 89.677(5) . 2_656 ?
O5 Dy1 Dy2 102.65(7) 2_656 . ?
O5 Dy1 Dy2 35.46(7) 2_656 2_656 ?
O5 Dy1 O1 91.45(10) 2_656 . ?
O5 Dy1 N1 147.69(10) 2_656 . ?
O5 Dy1 N6 62.18(10) 2_656 2_656 ?
O5 Dy1 O2 133.90(10) 2_656 . ?
O8 Dy1 Dy2 89.30(7) 2_656 . ?
O8 Dy1 Dy2 32.41(7) 2_656 2_656 ?
O8 Dy1 O5 66.47(10) 2_656 2_656 ?
O8 Dy1 O6 159.60(11) 2_656 2_656 ?
O8 Dy1 O1 80.51(10) 2_656 . ?
O8 Dy1 N1 89.89(10) 2_656 . ?
O8 Dy1 N6 119.59(11) 2_656 2_656 ?
O8 Dy1 O2 89.50(10) 2_656 . ?
O7 Dy1 Dy2 32.80(7) . . ?
O7 Dy1 Dy2 85.60(7) . 2_656 ?
O7 Dy1 O5 80.68(10) . 2_656 ?
O7 Dy1 O8 102.52(10) . 2_656 ?
O7 Dy1 O6 93.52(10) . 2_656 ?
O7 Dy1 O1 169.42(11) . . ?
O7 Dy1 N1 127.75(11) . . ?
O7 Dy1 N6 98.54(11) . 2_656 ?
O7 Dy1 O2 66.33(10) . . ?
O6 Dy1 Dy2 164.89(8) 2_656 2_656 ?
O6 Dy1 Dy2 97.75(8) 2_656 . ?
O6 Dy1 O5 129.52(11) 2_656 2_656 ?
O6 Dy1 O1 86.02(11) 2_656 . ?
O6 Dy1 N1 70.19(11) 2_656 . ?
O6 Dy1 N6 69.40(11) 2_656 2_656 ?
O6 Dy1 O2 85.43(11) 2_656 . ?
O1 Dy1 Dy2 92.10(7) . 2_656 ?
O1 Dy1 Dy2 157.70(8) . . ?
O1 Dy1 N1 61.94(11) . . ?
O1 Dy1 N6 71.39(12) . 2_656 ?
N1 Dy1 Dy2 121.85(7) . 2_656 ?
N1 Dy1 Dy2 98.54(8) . . ?
N6 Dy1 Dy2 95.78(8) 2_656 2_656 ?
N6 Dy1 Dy2 130.53(8) 2_656 . ?
N6 Dy1 N1 118.90(11) 2_656 . ?
O2 Dy1 Dy2 35.34(7) . . ?
O2 Dy1 Dy2 107.84(7) . 2_656 ?
O2 Dy1 O1 124.09(10) . . ?
O2 Dy1 N1 63.20(10) . . ?
O2 Dy1 N6 150.18(11) . 2_656 ?
Dy1 O5 Dy2 109.14(11) 2_656 . ?
C21 O5 Dy2 124.7(2) . . ?
C21 O5 Dy1 123.2(3) . 2_656 ?
Dy2 O8 Dy1 114.99(12) . 2_656 ?
C30 O8 Dy2 121.9(3) . . ?
C30 O8 Dy1 122.8(3) . 2_656 ?
Dy2 O4 H4 119.0(15) . . ?
C15 O4 Dy2 127.4(3) . . ?
C15 O4 H4 106.8(15) . . ?
Dy1 O7 Dy2 114.56(12) . . ?
C29 O7 Dy2 122.6(3) . . ?
C29 O7 Dy1 122.8(3) . . ?
C28 O6 Dy1 130.3(3) . 2_656 ?
Dy1 O1 H1 120.3(15) . . ?
C1 O1 Dy1 127.9(3) . . ?
C1 O1 H1 106.5(15) . . ?
C19 C20 C21 123.7(4) . . ?
N4 C20 C21 113.9(4) . . ?
N4 C20 C19 122.2(4) . . ?
C7 N2 N3 109.6(3) . . ?
C14 O3 Dy2 130.2(3) . . ?
O5 C21 C20 116.4(4) . . ?
N5 C21 O5 125.9(4) . . ?
N5 C21 C20 117.5(4) . . ?
C6 C5 H5 121.0 . . ?
C6 C5 C4 118.0(5) . . ?
C4 C5 H5 121.0 . . ?
C32 O10 H10A 103(4) . . ?
C23 C24 H24 119.6 . . ?
C25 C24 H24 119.6 . . ?
C25 C24 C23 120.9(6) . . ?
C6 N1 Dy1 118.1(3) . . ?
C2 N1 Dy1 121.7(3) . . ?
C2 N1 C6 118.6(4) . . ?
C2 C3 H3 120.4 . . ?
C4 C3 H3 120.4 . . ?
C4 C3 C2 119.1(4) . . ?
C5 C6 C7 123.8(4) . . ?
N1 C6 C5 122.8(4) . . ?
N1 C6 C7 113.3(4) . . ?
C20 C19 H19 120.4 . . ?
C18 C19 C20 119.1(5) . . ?
C18 C19 H19 120.4 . . ?
N5 N6 Dy1 119.2(2) . 2_656 ?
C22 N6 Dy1 127.3(3) . 2_656 ?
C22 N6 N5 111.5(4) . . ?
C21 N5 N6 109.4(3) . . ?
N2 N3 Dy2 118.8(2) . . ?
C8 N3 Dy2 127.2(3) . . ?
C8 N3 N2 112.1(3) . . ?
O6 C28 C23 121.7(4) . . ?
O6 C28 C27 120.3(5) . . ?
C27 C28 C23 117.9(5) . . ?
N3 C8 H8 117.3 . . ?
N3 C8 C9 125.3(4) . . ?
C9 C8 H8 117.3 . . ?
O4 C15 H15A 109.6 . . ?
O4 C15 H15B 109.6 . . ?
O4 C15 C16 110.3(4) . . ?
H15A C15 H15B 108.1 . . ?
C16 C15 H15A 109.6 . . ?
C16 C15 H15B 109.6 . . ?
C16 C17 H17 120.3 . . ?
C18 C17 H17 120.3 . . ?
C18 C17 C16 119.4(4) . . ?
C31 O9 H9 119(6) . . ?
C10 C9 C8 117.2(4) . . ?
C10 C9 C14 119.5(4) . . ?
C14 C9 C8 123.3(4) . . ?
C20 N4 Dy2 117.3(3) . . ?
C16 N4 Dy2 122.0(3) . . ?
C16 N4 C20 118.5(4) . . ?
C24 C23 C28 119.9(5) . . ?
C24 C23 C22 116.8(5) . . ?
C28 C23 C22 123.3(4) . . ?
N1 C2 C3 121.9(4) . . ?
N1 C2 C1 116.5(4) . . ?
C3 C2 C1 121.6(4) . . ?
C28 C27 H27 119.5 . . ?
C26 C27 C28 121.0(6) . . ?
C26 C27 H27 119.5 . . ?
C24 C25 H25 120.4 . . ?
C24 C25 C26 119.3(5) . . ?
C26 C25 H25 120.4 . . ?
N2 C7 C6 117.7(4) . . ?
O2 C7 N2 125.7(4) . . ?
O2 C7 C6 116.5(4) . . ?
C5 C4 H4A 120.3 . . ?
C3 C4 C5 119.5(4) . . ?
C3 C4 H4A 120.3 . . ?
N6 C22 C23 125.2(5) . . ?
N6 C22 H22 117.4 . . ?
C23 C22 H22 117.4 . . ?
C13 C12 H12 119.6 . . ?
C13 C12 C11 120.9(5) . . ?
C11 C12 H12 119.6 . . ?
C9 C10 H10 119.1 . . ?
C11 C10 C9 121.8(5) . . ?
C11 C10 H10 119.1 . . ?
C17 C16 C15 122.1(4) . . ?
N4 C16 C15 116.1(4) . . ?
N4 C16 C17 121.8(4) . . ?
O3 C14 C9 121.4(4) . . ?
O3 C14 C13 120.7(4) . . ?
C13 C14 C9 117.9(4) . . ?
Dy2 O2 Dy1 108.86(11) . . ?
C7 O2 Dy2 123.4(3) . . ?
C7 O2 Dy1 125.5(3) . . ?
C12 C13 C14 121.1(5) . . ?
C12 C13 H13 119.4 . . ?
C14 C13 H13 119.4 . . ?
O1 C1 C2 110.1(4) . . ?
O1 C1 H1A 109.6 . . ?
O1 C1 H1B 109.6 . . ?
C2 C1 H1A 109.6 . . ?
C2 C1 H1B 109.6 . . ?
H1A C1 H1B 108.1 . . ?
C19 C18 C17 118.9(4) . . ?
C19 C18 H18 120.6 . . ?
C17 C18 H18 120.6 . . ?
C27 C26 C25 120.9(5) . . ?
C27 C26 H26 119.5 . . ?
C25 C26 H26 119.5 . . ?
O7 C29 H29A 109.5 . . ?
O7 C29 H29B 109.5 . . ?
O7 C29 H29C 109.5 . . ?
H29A C29 H29B 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
C12 C11 H11 120.6 . . ?
C10 C11 C12 118.8(4) . . ?
C10 C11 H11 120.6 . . ?
O8 C30 H30A 109.5 . . ?
O8 C30 H30B 109.5 . . ?
O8 C30 H30C 109.5 . . ?
H30A C30 H30B 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
O10 C32 H32A 109.5 . . ?
O10 C32 H32B 109.5 . . ?
O10 C32 H32C 109.5 . . ?
H32A C32 H32B 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
O9 C31 H31A 109.5 . . ?
O9 C31 H31B 109.5 . . ?
O9 C31 H31C 109.5 . . ?
H31A C31 H31B 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Dy2 O5 C21 C20 19.2(5) . . . . ?
Dy2 O5 C21 N5 -156.6(3) . . . . ?
Dy2 O4 C15 C16 -0.4(6) . . . . ?
Dy2 O3 C14 C9 -51.4(6) . . . . ?
Dy2 O3 C14 C13 128.7(4) . . . . ?
Dy2 N3 C8 C9 15.0(6) . . . . ?
Dy2 N4 C16 C15 18.2(5) . . . . ?
Dy2 N4 C16 C17 -161.4(3) . . . . ?
Dy1 O5 C21 C20 177.7(3) 2_656 . . . ?
Dy1 O5 C21 N5 1.8(6) 2_656 . . . ?
Dy1 O6 C28 C23 50.3(6) 2_656 . . . ?
Dy1 O6 C28 C27 -129.9(4) 2_656 . . . ?
Dy1 O1 C1 C2 7.4(6) . . . . ?
Dy1 N1 C6 C5 -167.8(3) . . . . ?
Dy1 N1 C6 C7 10.5(4) . . . . ?
Dy1 N1 C2 C3 165.9(3) . . . . ?
Dy1 N1 C2 C1 -14.2(5) . . . . ?
Dy1 N6 N5 C21 -1.6(4) 2_656 . . . ?
Dy1 N6 C22 C23 -14.8(6) 2_656 . . . ?
O5 C21 N5 N6 0.0(6) . . . . ?
O4 C15 C16 C17 168.3(4) . . . . ?
O4 C15 C16 N4 -11.3(6) . . . . ?
O6 C28 C23 C24 176.1(4) . . . . ?
O6 C28 C23 C22 -2.9(7) . . . . ?
O6 C28 C27 C26 -177.7(5) . . . . ?
C20 C21 N5 N6 -175.8(3) . . . . ?
C20 C19 C18 C17 -0.2(7) . . . . ?
C20 N4 C16 C15 -179.3(4) . . . . ?
C20 N4 C16 C17 1.1(6) . . . . ?
N2 N3 C8 C9 179.1(4) . . . . ?
N2 C7 O2 Dy2 -1.5(6) . . . . ?
N2 C7 O2 Dy1 159.7(3) . . . . ?
O3 C14 C13 C12 179.4(4) . . . . ?
C21 C20 C19 C18 173.7(4) . . . . ?
C21 C20 N4 Dy2 -11.1(4) . . . . ?
C21 C20 N4 C16 -174.5(4) . . . . ?
C5 C6 C7 N2 3.5(6) . . . . ?
C5 C6 C7 O2 -178.4(4) . . . . ?
C24 C23 C22 N6 169.6(4) . . . . ?
C24 C25 C26 C27 -1.6(9) . . . . ?
N1 C6 C7 N2 -174.8(4) . . . . ?
N1 C6 C7 O2 3.3(5) . . . . ?
N1 C2 C1 O1 4.9(6) . . . . ?
C3 C2 C1 O1 -175.1(4) . . . . ?
C6 C5 C4 C3 1.8(7) . . . . ?
C6 N1 C2 C3 0.9(6) . . . . ?
C6 N1 C2 C1 -179.2(4) . . . . ?
C6 C7 O2 Dy2 -179.4(3) . . . . ?
C6 C7 O2 Dy1 -18.2(5) . . . . ?
C19 C20 C21 O5 179.8(4) . . . . ?
C19 C20 C21 N5 -4.0(6) . . . . ?
C19 C20 N4 Dy2 165.6(3) . . . . ?
C19 C20 N4 C16 2.2(6) . . . . ?
N5 N6 C22 C23 -178.6(4) . . . . ?
N3 N2 C7 C6 177.5(3) . . . . ?
N3 N2 C7 O2 -0.4(6) . . . . ?
N3 C8 C9 C10 -167.9(4) . . . . ?
N3 C8 C9 C14 10.4(7) . . . . ?
C28 C23 C22 N6 -11.3(7) . . . . ?
C28 C27 C26 C25 0.5(8) . . . . ?
C8 C9 C10 C11 176.0(4) . . . . ?
C8 C9 C14 O3 4.3(7) . . . . ?
C8 C9 C14 C13 -175.8(4) . . . . ?
C9 C10 C11 C12 0.2(8) . . . . ?
C9 C14 C13 C12 -0.5(7) . . . . ?
N4 C20 C21 O5 -3.5(5) . . . . ?
N4 C20 C21 N5 172.7(4) . . . . ?
N4 C20 C19 C18 -2.7(7) . . . . ?
C23 C24 C25 C26 0.0(8) . . . . ?
C23 C28 C27 C26 2.1(7) . . . . ?
C2 N1 C6 C5 -2.2(6) . . . . ?
C2 N1 C6 C7 176.1(4) . . . . ?
C2 C3 C4 C5 -3.1(7) . . . . ?
C27 C28 C23 C24 -3.7(7) . . . . ?
C27 C28 C23 C22 177.3(4) . . . . ?
C25 C24 C23 C28 2.7(7) . . . . ?
C25 C24 C23 C22 -178.2(5) . . . . ?
C7 N2 N3 Dy2 1.9(4) . . . . ?
C7 N2 N3 C8 -163.7(4) . . . . ?
C4 C5 C6 N1 0.9(7) . . . . ?
C4 C5 C6 C7 -177.2(4) . . . . ?
C4 C3 C2 N1 1.8(7) . . . . ?
C4 C3 C2 C1 -178.2(4) . . . . ?
C22 N6 N5 C21 163.7(4) . . . . ?
C10 C9 C14 O3 -177.4(4) . . . . ?
C10 C9 C14 C13 2.5(6) . . . . ?
C16 C17 C18 C19 3.3(7) . . . . ?
C14 C9 C10 C11 -2.4(7) . . . . ?
C13 C12 C11 C10 1.9(8) . . . . ?
C18 C17 C16 C15 176.5(5) . . . . ?
C18 C17 C16 N4 -3.9(7) . . . . ?
C11 C12 C13 C14 -1.8(8) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_1
_database_code_depnum_ccdc_archive 'CCDC 1832176'
loop_
_audit_author_name
_audit_author_address
'Wen-Min Wang'
;Taiyuan Normal University
China
;
_audit_update_record             
;
2019-04-08 deposited with the CCDC.	2019-04-09 downloaded from the CCDC.
;
_audit_creation_date             2019-02-24
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2016/6
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C60 H56 Gd4 N12 O16, 4(C H4 O)'
_chemical_formula_sum            'C64 H72 Gd4 N12 O20'
_chemical_formula_weight         1958.33
_chemical_melting_point          ?
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'

_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.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 1 2/c 1'
_space_group_name_Hall           '-C 2yc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'

_cell_length_a                   28.4296(10)
_cell_length_b                   8.4017(3)
_cell_length_c                   30.5551(10)
_cell_angle_alpha                90
_cell_angle_beta                 110.0660(10)
_cell_angle_gamma                90
_cell_volume                     6855.3(4)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    9991
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      26.32
_cell_measurement_theta_min      2.54
_shelx_estimated_absorpt_T_max   0.631
_shelx_estimated_absorpt_T_min   0.368
_exptl_absorpt_coefficient_mu    3.902
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.5161
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0851 before and 0.0609 after correction.
The Ratio of minimum to maximum transmission is 0.6924.
The λ/2 correction factor is Not present.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.897
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             3824
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.13
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0605
_diffrn_reflns_av_unetI/netI     0.0401
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       34
_diffrn_reflns_limit_h_min       -34
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            40689
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.021
_diffrn_reflns_theta_min         2.414
_diffrn_ambient_temperature      150.0
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                5300
_reflns_number_total             6748
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    
;
Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_refine_diff_density_max         1.154
_refine_diff_density_min         -1.199
_refine_diff_density_rms         0.155
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     464
_refine_ls_number_reflns         6748
_refine_ls_number_restraints     16
_refine_ls_R_factor_all          0.0543
_refine_ls_R_factor_gt           0.0330
_refine_ls_restrained_S_all      1.054
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0319P)²+51.5849P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0701
_refine_ls_wR_factor_ref         0.0796
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2. Restrained distances
 O4-H4
 0.87 with sigma of 0.01
 O1-H1
 0.85 with sigma of 0.02
 C15-H4
 1.895697 with sigma of 0.02
 Gd1-H4
 3.07824 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
O10 \\sim C32: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C32) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
4.a Secondary CH2 refined with riding coordinates:
 C15(H15A,H15B), C1(H1A,H1B)
4.b Aromatic/amide H refined with riding coordinates:
 C24(H24), C25(H25), C10(H10), C12(H12), C13(H13), C26(H26), C22(H22), C5(H5),
 C19(H19), C8(H8), C27(H27), C4(H4A), C17(H17), C3(H3), C11(H11), C18(H18)
4.c Idealised Me refined as rotating group:
 C30(H30A,H30B,H30C), C31(H31A,H31B,H31C), C29(H29A,H29B,H29C), C32(H32A,H32B,
 H32C)
4.d Idealised tetrahedral OH refined as rotating group:
 O9(H9), O10(H10A)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   ?
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 0.58925(2) 0.23965(3) 0.82292(2) 0.01796(8) Uani 1 1 d D . . . .
Gd2 Gd 0.55069(2) 0.20799(3) 0.68783(2) 0.01859(8) Uani 1 1 d . . . . .
O4 O 0.61335(15) 0.3705(5) 0.90096(13) 0.0295(9) Uani 1 1 d D . . . .
H4 H 0.5938(14) 0.365(5) 0.9178(12) 0.044 Uiso 1 1 d DR . . . .
O7 O 0.51503(12) 0.3720(4) 0.81443(12) 0.0196(8) Uani 1 1 d . . . . .
O3 O 0.67443(13) 0.1921(4) 0.83901(12) 0.0254(8) Uani 1 1 d . . . . .
O6 O 0.54151(14) 0.2528(4) 0.61011(12) 0.0270(9) Uani 1 1 d . . . . .
O1 O 0.37077(14) 0.0707(5) 0.80675(14) 0.0273(9) Uani 1 1 d D . . . .
O5 O 0.59221(13) 0.3709(4) 0.75435(11) 0.0204(8) Uani 1 1 d . . . . .
O8 O 0.56663(13) 0.0769(4) 0.75835(11) 0.0208(8) Uani 1 1 d . . . . .
O9 O 0.70255(15) 0.0907(6) 0.77063(14) 0.0426(11) Uani 1 1 d . . . . .
H9 H 0.694219 0.120405 0.793189 0.064 Uiso 1 1 calc GR . . . .
O2 O 0.52968(13) 0.0789(4) 0.84131(12) 0.0206(8) Uani 1 1 d . . . . .
C24 C 0.6542(2) 0.3459(8) 0.5819(2) 0.0371(15) Uani 1 1 d . . . . .
H24 H 0.683609 0.409063 0.593093 0.044 Uiso 1 1 calc R . . . .
N6 N 0.61366(17) 0.4212(5) 0.68089(15) 0.0241(10) Uani 1 1 d . . . . .
C6 C 0.49997(19) -0.1202(6) 0.88015(17) 0.0206(11) Uani 1 1 d . . . . .
O10 O 0.54738(17) 0.3601(7) 0.94125(15) 0.0515(13) Uani 1 1 d . U . . .
H10A H 0.520039 0.319666 0.924674 0.077 Uiso 1 1 calc GR . . . .
N2 N 0.58771(17) -0.0721(5) 0.89827(15) 0.0249(10) Uani 1 1 d . . . . .
N5 N 0.63771(17) 0.5213(5) 0.71920(15) 0.0256(10) Uani 1 1 d . . . . .
C9 C 0.70998(19) 0.1083(6) 0.91837(18) 0.0235(12) Uani 1 1 d . . . . .
C25 C 0.6443(3) 0.2586(9) 0.5405(2) 0.0473(18) Uani 1 1 d . . . . .
H25 H 0.667066 0.261317 0.523871 0.057 Uiso 1 1 calc R . . . .
C21 C 0.62348(19) 0.4833(6) 0.75410(18) 0.0214(11) Uani 1 1 d . . . . .
C28 C 0.5756(2) 0.2513(7) 0.58948(18) 0.0273(13) Uani 1 1 d . . . . .
N1 N 0.45441(16) -0.0655(5) 0.85485(14) 0.0214(10) Uani 1 1 d . . . . .
C20 C 0.64776(19) 0.5688(6) 0.79865(18) 0.0206(11) Uani 1 1 d . . . . .
C10 C 0.7518(2) 0.1084(7) 0.95954(19) 0.0295(13) Uani 1 1 d . . . . .
H10 H 0.751082 0.045766 0.985192 0.035 Uiso 1 1 calc R . . . .
C12 C 0.7950(2) 0.2865(7) 0.9260(2) 0.0332(14) Uani 1 1 d . . . . .
H12 H 0.823403 0.350655 0.928920 0.040 Uiso 1 1 calc R . . . .
C13 C 0.7552(2) 0.2837(7) 0.8841(2) 0.0297(13) Uani 1 1 d . . . . .
H13 H 0.757358 0.342712 0.858303 0.036 Uiso 1 1 calc R . . . .
C26 C 0.6009(3) 0.1688(9) 0.5241(2) 0.0462(18) Uani 1 1 d . . . . .
H26 H 0.594332 0.108714 0.496311 0.055 Uiso 1 1 calc R . . . .
N3 N 0.62228(16) 0.0268(5) 0.88758(15) 0.0223(10) Uani 1 1 d . . . . .
C22 C 0.6351(2) 0.4277(7) 0.64977(19) 0.0284(13) Uani 1 1 d . . . . .
H22 H 0.663017 0.497203 0.655957 0.034 Uiso 1 1 calc R . . . .
N4 N 0.63580(15) 0.5116(5) 0.83469(14) 0.0205(9) Uani 1 1 d . . . . .
C15 C 0.6432(2) 0.5092(7) 0.91577(19) 0.0324(14) Uani 1 1 d D . . . .
H15A H 0.673298 0.483112 0.942871 0.039 Uiso 1 1 calc R . . . .
H15B H 0.623880 0.591277 0.925600 0.039 Uiso 1 1 calc R . . . .
C5 C 0.5067(2) -0.2467(6) 0.91110(19) 0.0273(12) Uani 1 1 d . . . . .
H5 H 0.539228 -0.286020 0.927955 0.033 Uiso 1 1 calc R . . . .
C19 C 0.6816(2) 0.6916(7) 0.8040(2) 0.0297(13) Uani 1 1 d . . . . .
H19 H 0.688182 0.732835 0.777731 0.036 Uiso 1 1 calc R . . . .
C14 C 0.71215(19) 0.1952(6) 0.87923(18) 0.0237(12) Uani 1 1 d . . . . .
C8 C 0.6664(2) 0.0194(6) 0.91855(18) 0.0247(12) Uani 1 1 d . . . . .
H8 H 0.670730 -0.051099 0.943957 0.030 Uiso 1 1 calc R . . . .
C27 C 0.5668(2) 0.1647(8) 0.5477(2) 0.0363(15) Uani 1 1 d . . . . .
H27 H 0.537171 0.102841 0.535624 0.044 Uiso 1 1 calc R . . . .
C4 C 0.4644(2) -0.3139(7) 0.9166(2) 0.0338(14) Uani 1 1 d . . . . .
H4A H 0.467522 -0.401746 0.936976 0.041 Uiso 1 1 calc R . . . .
C7 C 0.5422(2) -0.0337(6) 0.87251(17) 0.0207(11) Uani 1 1 d . . . . .
C23 C 0.6208(2) 0.3403(7) 0.60689(18) 0.0272(13) Uani 1 1 d . . . . .
C17 C 0.6951(2) 0.6908(7) 0.8848(2) 0.0299(13) Uani 1 1 d . . . . .
H17 H 0.712310 0.727600 0.915534 0.036 Uiso 1 1 calc R . . . .
C3 C 0.4179(2) -0.2519(6) 0.8923(2) 0.0285(13) Uani 1 1 d . . . . .
H3 H 0.388775 -0.292657 0.896936 0.034 Uiso 1 1 calc R . . . .
C16 C 0.6588(2) 0.5733(6) 0.87700(18) 0.0232(12) Uani 1 1 d . . . . .
C2 C 0.4141(2) -0.1293(6) 0.86097(18) 0.0248(12) Uani 1 1 d . . . . .
C11 C 0.7938(2) 0.1974(8) 0.9636(2) 0.0354(14) Uani 1 1 d . . . . .
H11 H 0.821584 0.197394 0.991869 0.042 Uiso 1 1 calc R . . . .
C18 C 0.7059(2) 0.7539(7) 0.8478(2) 0.0352(14) Uani 1 1 d . . . . .
H18 H 0.729425 0.838037 0.852205 0.042 Uiso 1 1 calc R . . . .
C1 C 0.3645(2) -0.0636(7) 0.8324(2) 0.0305(13) Uani 1 1 d . . . . .
H1A H 0.344877 -0.146230 0.810664 0.037 Uiso 1 1 calc R . . . .
H1B H 0.345720 -0.032103 0.852980 0.037 Uiso 1 1 calc R . . . .
C30 C 0.5679(3) -0.0911(7) 0.7626(2) 0.0417(16) Uani 1 1 d . . . . .
H30A H 0.593800 -0.133901 0.751374 0.063 Uiso 1 1 calc GR . . . .
H30B H 0.535268 -0.135098 0.743926 0.063 Uiso 1 1 calc GR . . . .
H30C H 0.575602 -0.120409 0.795328 0.063 Uiso 1 1 calc GR . . . .
C31 C 0.7350(3) 0.2075(11) 0.7617(2) 0.061(2) Uani 1 1 d . . . . .
H31A H 0.729952 0.209180 0.728318 0.092 Uiso 1 1 calc GR . . . .
H31B H 0.769947 0.180317 0.779275 0.092 Uiso 1 1 calc GR . . . .
H31C H 0.727322 0.312572 0.771407 0.092 Uiso 1 1 calc GR . . . .
C29 C 0.5108(2) 0.5407(7) 0.8128(2) 0.0414(16) Uani 1 1 d . . . . .
H29A H 0.532612 0.585646 0.842439 0.062 Uiso 1 1 calc GR . . . .
H29B H 0.476041 0.571094 0.807563 0.062 Uiso 1 1 calc GR . . . .
H29C H 0.520962 0.581631 0.787356 0.062 Uiso 1 1 calc GR . . . .
C32 C 0.5643(4) 0.2843(16) 0.9824(3) 0.118(4) Uani 1 1 d . U . . .
H32A H 0.576264 0.178158 0.978095 0.176 Uiso 1 1 calc GR . . . .
H32B H 0.537076 0.274296 0.995103 0.176 Uiso 1 1 calc GR . . . .
H32C H 0.591848 0.345290 1.004182 0.176 Uiso 1 1 calc GR . . . .
H1 H 0.348(2) 0.080(9) 0.7808(14) 0.07(3) Uiso 1 1 d 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
Gd1 Gd2 3.8873(4) 2_656 ?
Gd1 O4 2.499(4) . ?
Gd1 O7 2.320(3) . ?
Gd1 O3 2.334(4) . ?
Gd1 O5 2.394(3) . ?
Gd1 O8 2.303(3) . ?
Gd1 O2 2.379(3) . ?
Gd1 N3 2.590(4) . ?
Gd1 N4 2.603(4) . ?
Gd2 O7 2.303(3) 2_656 ?
Gd2 O6 2.329(3) . ?
Gd2 O1 2.468(4) 2_656 ?
Gd2 O5 2.398(3) . ?
Gd2 O8 2.322(3) . ?
Gd2 O2 2.407(3) 2_656 ?
Gd2 N6 2.592(4) . ?
Gd2 N1 2.621(4) 2_656 ?
O4 C15 1.421(7) . ?
O7 C29 1.422(7) . ?
O3 C14 1.325(6) . ?
O6 C28 1.326(6) . ?
O1 C1 1.420(6) . ?
O5 C21 1.299(6) . ?
O8 C30 1.416(7) . ?
O9 C31 1.436(8) . ?
O2 C7 1.303(6) . ?
C24 C25 1.405(9) . ?
C24 C23 1.408(8) . ?
N6 N5 1.413(6) . ?
N6 C22 1.295(7) . ?
C6 N1 1.341(7) . ?
C6 C5 1.392(7) . ?
C6 C7 1.488(7) . ?
O10 C32 1.343(10) . ?
N2 N3 1.409(6) . ?
N2 C7 1.304(7) . ?
N5 C21 1.303(6) . ?
C9 C10 1.403(7) . ?
C9 C14 1.420(8) . ?
C9 C8 1.450(7) . ?
C25 C26 1.384(10) . ?
C21 C20 1.483(7) . ?
C28 C27 1.414(8) . ?
C28 C23 1.423(8) . ?
N1 C2 1.335(7) . ?
C20 N4 1.348(6) . ?
C20 C19 1.382(7) . ?
C10 C11 1.378(8) . ?
C12 C13 1.388(8) . ?
C12 C11 1.380(9) . ?
C13 C14 1.396(8) . ?
C26 C27 1.395(9) . ?
N3 C8 1.287(7) . ?
C22 C23 1.434(8) . ?
N4 C16 1.337(6) . ?
C15 C16 1.501(7) . ?
C5 C4 1.390(8) . ?
C19 C18 1.380(8) . ?
C4 C3 1.378(8) . ?
C17 C16 1.387(8) . ?
C17 C18 1.377(8) . ?
C3 C2 1.385(8) . ?
C2 C1 1.488(8) . ?

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
O4 Gd1 Gd2 92.76(9) . 2_656 ?
O4 Gd1 N3 70.54(13) . . ?
O4 Gd1 N4 61.44(13) . . ?
O7 Gd1 Gd2 32.63(8) . 2_656 ?
O7 Gd1 O4 80.61(13) . . ?
O7 Gd1 O3 160.71(13) . . ?
O7 Gd1 O5 89.15(12) . . ?
O7 Gd1 O2 66.69(11) . . ?
O7 Gd1 N3 119.60(13) . . ?
O7 Gd1 N4 89.69(12) . . ?
O3 Gd1 Gd2 164.55(9) . 2_656 ?
O3 Gd1 O4 87.10(13) . . ?
O3 Gd1 O5 85.28(12) . . ?
O3 Gd1 O2 128.63(12) . . ?
O3 Gd1 N3 69.08(13) . . ?
O3 Gd1 N4 71.32(13) . . ?
O5 Gd1 Gd2 107.44(8) . 2_656 ?
O5 Gd1 O4 123.50(12) . . ?
O5 Gd1 N3 150.81(13) . . ?
O5 Gd1 N4 63.12(12) . . ?
O8 Gd1 Gd2 84.84(9) . 2_656 ?
O8 Gd1 O4 169.49(12) . . ?
O8 Gd1 O7 102.29(12) . . ?
O8 Gd1 O3 92.49(12) . . ?
O8 Gd1 O5 66.88(12) . . ?
O8 Gd1 O2 81.55(12) . . ?
O8 Gd1 N3 99.50(13) . . ?
O8 Gd1 N4 128.24(13) . . ?
O2 Gd1 Gd2 35.93(8) . 2_656 ?
O2 Gd1 O4 90.49(12) . . ?
O2 Gd1 O5 135.20(12) . . ?
O2 Gd1 N3 61.91(12) . . ?
O2 Gd1 N4 146.60(13) . . ?
N3 Gd1 Gd2 96.31(10) . 2_656 ?
N3 Gd1 N4 117.81(13) . . ?
N4 Gd1 Gd2 121.92(9) . 2_656 ?
O7 Gd2 O6 93.82(12) 2_656 . ?
O7 Gd2 O1 170.95(13) 2_656 2_656 ?
O7 Gd2 O5 80.93(12) 2_656 . ?
O7 Gd2 O8 102.10(12) 2_656 . ?
O7 Gd2 O2 66.48(11) 2_656 2_656 ?
O7 Gd2 N6 99.22(13) 2_656 . ?
O7 Gd2 N1 127.12(13) 2_656 2_656 ?
O6 Gd2 O1 85.78(13) . 2_656 ?
O6 Gd2 O5 128.48(12) . . ?
O6 Gd2 O2 86.30(13) . 2_656 ?
O6 Gd2 N6 69.13(13) . . ?
O6 Gd2 N1 70.54(13) . 2_656 ?
O1 Gd2 N6 72.18(14) 2_656 . ?
O1 Gd2 N1 61.20(13) 2_656 2_656 ?
O5 Gd2 O1 92.23(12) . 2_656 ?
O5 Gd2 O2 134.37(11) . 2_656 ?
O5 Gd2 N6 61.45(12) . . ?
O5 Gd2 N1 148.11(12) . 2_656 ?
O8 Gd2 O6 160.19(12) . . ?
O8 Gd2 O1 80.33(13) . 2_656 ?
O8 Gd2 O5 66.53(12) . . ?
O8 Gd2 O2 89.30(12) . 2_656 ?
O8 Gd2 N6 118.91(13) . . ?
O8 Gd2 N1 90.33(12) . 2_656 ?
O2 Gd2 O1 122.45(12) 2_656 2_656 ?
O2 Gd2 N6 151.12(13) 2_656 . ?
O2 Gd2 N1 62.46(12) 2_656 2_656 ?
N6 Gd2 N1 119.13(13) . 2_656 ?
C15 O4 Gd1 127.1(3) . . ?
Gd2 O7 Gd1 114.47(14) 2_656 . ?
C29 O7 Gd1 122.9(3) . . ?
C29 O7 Gd2 122.5(3) . 2_656 ?
C14 O3 Gd1 130.0(3) . . ?
C28 O6 Gd2 129.7(3) . . ?
C1 O1 Gd2 128.1(3) . 2_656 ?
Gd1 O5 Gd2 108.90(13) . . ?
C21 O5 Gd1 124.7(3) . . ?
C21 O5 Gd2 123.3(3) . . ?
Gd1 O8 Gd2 114.92(14) . . ?
C30 O8 Gd1 121.5(3) . . ?
C30 O8 Gd2 123.2(3) . . ?
Gd1 O2 Gd2 108.62(13) . 2_656 ?
C7 O2 Gd1 123.2(3) . . ?
C7 O2 Gd2 125.7(3) . 2_656 ?
C25 C24 C23 120.5(6) . . ?
N5 N6 Gd2 119.7(3) . . ?
C22 N6 Gd2 127.0(4) . . ?
C22 N6 N5 111.5(4) . . ?
N1 C6 C5 122.3(5) . . ?
N1 C6 C7 114.4(4) . . ?
C5 C6 C7 123.3(5) . . ?
C7 N2 N3 109.9(4) . . ?
C21 N5 N6 109.5(4) . . ?
C10 C9 C14 119.1(5) . . ?
C10 C9 C8 117.3(5) . . ?
C14 C9 C8 123.5(5) . . ?
C26 C25 C24 119.2(6) . . ?
O5 C21 N5 126.0(5) . . ?
O5 C21 C20 116.8(4) . . ?
N5 C21 C20 117.1(5) . . ?
O6 C28 C27 120.1(5) . . ?
O6 C28 C23 122.1(5) . . ?
C27 C28 C23 117.8(5) . . ?
C6 N1 Gd2 117.7(3) . 2_656 ?
C2 N1 Gd2 121.2(4) . 2_656 ?
C2 N1 C6 119.1(5) . . ?
N4 C20 C21 114.1(4) . . ?
N4 C20 C19 122.0(5) . . ?
C19 C20 C21 123.8(5) . . ?
C11 C10 C9 121.5(5) . . ?
C11 C12 C13 120.9(6) . . ?
C12 C13 C14 120.9(5) . . ?
C25 C26 C27 121.2(6) . . ?
N2 N3 Gd1 119.0(3) . . ?
C8 N3 Gd1 127.0(4) . . ?
C8 N3 N2 112.4(4) . . ?
N6 C22 C23 126.3(5) . . ?
C20 N4 Gd1 117.3(3) . . ?
C16 N4 Gd1 122.1(3) . . ?
C16 N4 C20 118.3(4) . . ?
O4 C15 C16 110.4(4) . . ?
C4 C5 C6 118.0(5) . . ?
C18 C19 C20 119.7(5) . . ?
O3 C14 C9 121.0(5) . . ?
O3 C14 C13 120.7(5) . . ?
C13 C14 C9 118.3(5) . . ?
N3 C8 C9 126.2(5) . . ?
C26 C27 C28 120.9(6) . . ?
C3 C4 C5 119.5(5) . . ?
O2 C7 C6 115.9(4) . . ?
O2 C7 N2 125.9(5) . . ?
N2 C7 C6 118.1(5) . . ?
C24 C23 C28 120.3(5) . . ?
C24 C23 C22 116.5(5) . . ?
C28 C23 C22 123.2(5) . . ?
C18 C17 C16 119.7(5) . . ?
C4 C3 C2 119.1(5) . . ?
N4 C16 C15 116.4(5) . . ?
N4 C16 C17 122.0(5) . . ?
C17 C16 C15 121.6(5) . . ?
N1 C2 C3 122.0(5) . . ?
N1 C2 C1 117.1(5) . . ?
C3 C2 C1 120.9(5) . . ?
C10 C11 C12 119.1(5) . . ?
C17 C18 C19 118.1(5) . . ?
O1 C1 C2 110.2(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
Gd1 O4 C15 C16 0.9(7) . . . . ?
Gd1 O3 C14 C9 51.6(7) . . . . ?
Gd1 O3 C14 C13 -128.7(5) . . . . ?
Gd1 O5 C21 N5 156.1(4) . . . . ?
Gd1 O5 C21 C20 -19.5(6) . . . . ?
Gd1 O2 C7 C6 178.8(3) . . . . ?
Gd1 O2 C7 N2 1.5(7) . . . . ?
Gd1 N3 C8 C9 -13.5(8) . . . . ?
Gd1 N4 C16 C15 -19.3(6) . . . . ?
Gd1 N4 C16 C17 161.0(4) . . . . ?
Gd2 O6 C28 C27 131.3(5) . . . . ?
Gd2 O6 C28 C23 -51.4(7) . . . . ?
Gd2 O1 C1 C2 -7.0(7) 2_656 . . . ?
Gd2 O5 C21 N5 -1.8(7) . . . . ?
Gd2 O5 C21 C20 -177.4(3) . . . . ?
Gd2 O2 C7 C6 18.7(6) 2_656 . . . ?
Gd2 O2 C7 N2 -158.6(4) 2_656 . . . ?
Gd2 N6 N5 C21 1.3(5) . . . . ?
Gd2 N6 C22 C23 14.6(8) . . . . ?
Gd2 N1 C2 C3 -164.5(4) 2_656 . . . ?
Gd2 N1 C2 C1 15.8(6) 2_656 . . . ?
O4 C15 C16 N4 11.7(7) . . . . ?
O4 C15 C16 C17 -168.6(5) . . . . ?
O6 C28 C27 C26 176.4(5) . . . . ?
O6 C28 C23 C24 -174.8(5) . . . . ?
O6 C28 C23 C22 5.2(8) . . . . ?
O5 C21 C20 N4 3.3(7) . . . . ?
O5 C21 C20 C19 -179.7(5) . . . . ?
C24 C25 C26 C27 0.7(10) . . . . ?
N6 N5 C21 O5 0.2(7) . . . . ?
N6 N5 C21 C20 175.8(4) . . . . ?
N6 C22 C23 C24 -169.9(6) . . . . ?
N6 C22 C23 C28 10.0(9) . . . . ?
C6 N1 C2 C3 -0.8(8) . . . . ?
C6 N1 C2 C1 179.5(5) . . . . ?
C6 C5 C4 C3 -1.2(8) . . . . ?
N2 N3 C8 C9 -178.8(5) . . . . ?
N5 N6 C22 C23 179.2(5) . . . . ?
N5 C21 C20 N4 -172.7(5) . . . . ?
N5 C21 C20 C19 4.4(8) . . . . ?
C9 C10 C11 C12 -0.9(9) . . . . ?
C25 C24 C23 C28 -2.6(9) . . . . ?
C25 C24 C23 C22 177.4(6) . . . . ?
C25 C26 C27 C28 -0.6(10) . . . . ?
C21 C20 N4 Gd1 11.8(6) . . . . ?
C21 C20 N4 C16 175.0(4) . . . . ?
C21 C20 C19 C18 -173.9(5) . . . . ?
N1 C6 C5 C4 -2.1(8) . . . . ?
N1 C6 C7 O2 -2.4(6) . . . . ?
N1 C6 C7 N2 175.1(5) . . . . ?
N1 C2 C1 O1 -6.2(7) . . . . ?
C20 N4 C16 C15 178.3(5) . . . . ?
C20 N4 C16 C17 -1.4(8) . . . . ?
C20 C19 C18 C17 -0.3(9) . . . . ?
C10 C9 C14 O3 176.8(5) . . . . ?
C10 C9 C14 C13 -2.9(8) . . . . ?
C10 C9 C8 N3 167.4(5) . . . . ?
C12 C13 C14 O3 -179.6(5) . . . . ?
C12 C13 C14 C9 0.1(8) . . . . ?
C13 C12 C11 C10 -2.0(9) . . . . ?
N3 N2 C7 O2 0.0(7) . . . . ?
N3 N2 C7 C6 -177.3(4) . . . . ?
C22 N6 N5 C21 -164.6(5) . . . . ?
N4 C20 C19 C18 3.0(9) . . . . ?
C5 C6 N1 Gd2 167.4(4) . . . 2_656 ?
C5 C6 N1 C2 3.1(7) . . . . ?
C5 C6 C7 O2 178.0(5) . . . . ?
C5 C6 C7 N2 -4.5(8) . . . . ?
C5 C4 C3 C2 3.4(9) . . . . ?
C19 C20 N4 Gd1 -165.3(4) . . . . ?
C19 C20 N4 C16 -2.1(8) . . . . ?
C14 C9 C10 C11 3.4(8) . . . . ?
C14 C9 C8 N3 -12.0(9) . . . . ?
C8 C9 C10 C11 -176.0(5) . . . . ?
C8 C9 C14 O3 -3.9(8) . . . . ?
C8 C9 C14 C13 176.4(5) . . . . ?
C27 C28 C23 C24 2.6(8) . . . . ?
C27 C28 C23 C22 -177.4(5) . . . . ?
C4 C3 C2 N1 -2.4(8) . . . . ?
C4 C3 C2 C1 177.2(5) . . . . ?
C7 C6 N1 Gd2 -12.2(5) . . . 2_656 ?
C7 C6 N1 C2 -176.4(4) . . . . ?
C7 C6 C5 C4 177.5(5) . . . . ?
C7 N2 N3 Gd1 -1.3(5) . . . . ?
C7 N2 N3 C8 165.3(5) . . . . ?
C23 C24 C25 C26 0.9(10) . . . . ?
C23 C28 C27 C26 -1.0(9) . . . . ?
C3 C2 C1 O1 174.1(5) . . . . ?
C16 C17 C18 C19 -3.1(9) . . . . ?
C11 C12 C13 C14 2.4(9) . . . . ?
C18 C17 C16 N4 4.0(9) . . . . ?
C18 C17 C16 C15 -175.6(6) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_4
_database_code_depnum_ccdc_archive 'CCDC 1832175'
loop_
_audit_author_name
_audit_author_address
'Wen-Min Wang'
;Taiyuan Normal University
China
;
_audit_update_record             
;
2019-04-08 deposited with the CCDC.	2019-04-09 downloaded from the CCDC.
;
_audit_creation_date             2019-02-24
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2016/6
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C60 H56 Ho4 N12 O16, 4(C H4 O)'
_chemical_formula_sum            'C64 H72 Ho4 N12 O20'
_chemical_formula_weight         1989.05
_chemical_melting_point          ?
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'

_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.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 1 2/c 1'
_space_group_name_Hall           '-C 2yc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'

_cell_length_a                   28.1973(10)
_cell_length_b                   8.4679(3)
_cell_length_c                   30.3722(10)
_cell_angle_alpha                90
_cell_angle_beta                 110.3464(11)
_cell_angle_gamma                90
_cell_volume                     6799.6(4)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    9932
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      26.31
_cell_measurement_theta_min      2.44
_shelx_estimated_absorpt_T_max   0.627
_shelx_estimated_absorpt_T_min   0.343
_exptl_absorpt_coefficient_mu    4.687
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.5766
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0835 before and 0.0595 after correction.
The Ratio of minimum to maximum transmission is 0.7735.
The λ/2 correction factor is Not present.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.943
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             3872
_exptl_crystal_size_max          0.29
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.11
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0561
_diffrn_reflns_av_unetI/netI     0.0363
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_h_min       -33
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            36555
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.010
_diffrn_reflns_theta_max         25.010
_diffrn_reflns_theta_min         2.440
_diffrn_ambient_temperature      149.99
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4849
_reflns_number_total             5985
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    
;
Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_refine_diff_density_max         0.947
_refine_diff_density_min         -1.143
_refine_diff_density_rms         0.155
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     464
_refine_ls_number_reflns         5985
_refine_ls_number_restraints     18
_refine_ls_R_factor_all          0.0484
_refine_ls_R_factor_gt           0.0307
_refine_ls_restrained_S_all      1.059
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0338P)²+36.8485P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0663
_refine_ls_wR_factor_ref         0.0740
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2. Restrained distances
 O4-H4
 0.87 with sigma of 0.01
 H10A-O6_$1
 2 with sigma of 0.02
 H1-O1
 0.85 with sigma of 0.02
 H10A-H4
 2.2 with sigma of 0.02
 C15-H4
 1.896893 with sigma of 0.02
 Ho1-H4
 3.031973 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C32) \\sim Ueq, Uanis(O10) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
4.a Secondary CH2 refined with riding coordinates:
 C15(H15A,H15B), C1(H1A,H1B)
4.b Aromatic/amide H refined with riding coordinates:
 C27(H27), C3(H3), C24(H24), C17(H17), C25(H25), C8(H8), C13(H13), C5(H5),
 C22(H22), C4(H4A), C10(H10), C11(H11), C18(H18), C12(H12), C19(H19), C26(H26)
4.c Idealised Me refined as rotating group:
 C31(H31A,H31B,H31C), C29(H29A,H29B,H29C), C32(H32A,H32B,H32C), C30(H30A,H30B,
 H30C)
4.d Idealised tetrahedral OH refined as rotating group:
 O9(H9), O10(H10A)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   ?
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 0.58921(2) 0.24171(3) 0.32254(2) 0.01924(8) Uani 1 1 d D . . . .
Ho2 Ho 0.54995(2) 0.20966(3) 0.18843(2) 0.02020(8) Uani 1 1 d . . . . .
O6 O 0.53893(15) 0.2498(5) 0.11087(13) 0.0285(9) Uani 1 1 d D . . . .
O8 O 0.51533(13) 0.3709(4) 0.31414(13) 0.0231(9) Uani 1 1 d . . . . .
O1 O 0.37079(16) 0.0823(5) 0.30579(14) 0.0304(10) Uani 1 1 d D . . . .
O7 O 0.56677(14) 0.0819(4) 0.25849(12) 0.0231(9) Uani 1 1 d . . . . .
O3 O 0.67379(14) 0.2001(5) 0.33770(13) 0.0287(9) Uani 1 1 d . . . . .
O5 O 0.59093(14) 0.3692(4) 0.25440(12) 0.0220(8) Uani 1 1 d . . . . .
C21 C 0.6222(2) 0.4820(7) 0.2539(2) 0.0236(13) Uani 1 1 d . . . . .
N2 N 0.58839(18) -0.0690(6) 0.39619(16) 0.0274(11) Uani 1 1 d . . . . .
C20 C 0.6464(2) 0.5673(7) 0.2984(2) 0.0241(13) Uani 1 1 d . . . . .
C27 C 0.5634(3) 0.1568(9) 0.0481(2) 0.0432(18) Uani 1 1 d . . . . .
H27 H 0.533709 0.094103 0.036805 0.052 Uiso 1 1 calc R . . . .
O2 O 0.52991(14) 0.0841(4) 0.34020(13) 0.0230(9) Uani 1 1 d . . . . .
N1 N 0.45422(17) -0.0573(5) 0.35281(15) 0.0220(10) Uani 1 1 d . . . . .
C3 C 0.4172(3) -0.2476(7) 0.3895(2) 0.0351(15) Uani 1 1 d . . . . .
H3 H 0.387775 -0.287593 0.394184 0.042 Uiso 1 1 calc R . . . .
N3 N 0.62304(17) 0.0297(5) 0.38595(16) 0.0240(11) Uani 1 1 d . . . . .
O4 O 0.61378(15) 0.3640(5) 0.40060(13) 0.0298(9) Uani 1 1 d D . . . .
H4 H 0.6084(12) 0.320(3) 0.4243(6) 0.045 Uiso 1 1 d DR . . . .
O9 O 0.70379(17) 0.0954(7) 0.27118(16) 0.0542(14) Uani 1 1 d . . . . .
H9 H 0.694757 0.127525 0.293216 0.081 Uiso 1 1 calc GR . . . .
C28 C 0.5727(2) 0.2462(7) 0.0892(2) 0.0322(15) Uani 1 1 d . . . . .
N5 N 0.63549(18) 0.5215(6) 0.21856(16) 0.0275(11) Uani 1 1 d . . . . .
N6 N 0.61126(17) 0.4203(6) 0.17983(16) 0.0260(11) Uani 1 1 d . . . . .
C23 C 0.6177(2) 0.3346(8) 0.1059(2) 0.0326(15) Uani 1 1 d . . . . .
C15 C 0.6433(2) 0.5020(8) 0.4162(2) 0.0345(15) Uani 1 1 d D . . . .
H15A H 0.673964 0.475810 0.443344 0.041 Uiso 1 1 calc R . . . .
H15B H 0.623565 0.581107 0.426634 0.041 Uiso 1 1 calc R . . . .
C24 C 0.6513(3) 0.3399(9) 0.0808(2) 0.0459(19) Uani 1 1 d . . . . .
H24 H 0.680845 0.403650 0.091471 0.055 Uiso 1 1 calc R . . . .
C17 C 0.6941(2) 0.6878(7) 0.3855(2) 0.0357(15) Uani 1 1 d . . . . .
H17 H 0.711404 0.724929 0.416466 0.043 Uiso 1 1 calc R . . . .
N4 N 0.63492(16) 0.5088(5) 0.33500(16) 0.0233(11) Uani 1 1 d . . . . .
C25 C 0.6403(3) 0.2491(10) 0.0394(3) 0.056(2) Uani 1 1 d . . . . .
H25 H 0.662841 0.250270 0.022335 0.067 Uiso 1 1 calc R . . . .
C7 C 0.5422(2) -0.0296(6) 0.37065(19) 0.0220(12) Uani 1 1 d . . . . .
C8 C 0.6675(2) 0.0242(7) 0.4173(2) 0.0272(13) Uani 1 1 d . . . . .
H8 H 0.672147 -0.045352 0.442997 0.033 Uiso 1 1 calc R . . . .
C14 C 0.7119(2) 0.2023(7) 0.3780(2) 0.0245(13) Uani 1 1 d . . . . .
C6 C 0.5000(2) -0.1167(6) 0.37790(19) 0.0247(13) Uani 1 1 d . . . . .
C13 C 0.7554(2) 0.2924(8) 0.3834(2) 0.0333(15) Uani 1 1 d . . . . .
H13 H 0.757023 0.352962 0.357656 0.040 Uiso 1 1 calc R . . . .
C9 C 0.7110(2) 0.1136(7) 0.4172(2) 0.0262(13) Uani 1 1 d . . . . .
O10 O 0.5486(2) 0.3552(10) 0.44151(18) 0.098(3) Uani 1 1 d . U . . .
H10A H 0.533296 0.275568 0.426802 0.147 Uiso 1 1 calc DGR . . . .
C5 C 0.5064(2) -0.2437(7) 0.4081(2) 0.0319(15) Uani 1 1 d . . . . .
H5 H 0.539251 -0.283129 0.425150 0.038 Uiso 1 1 calc R . . . .
C22 C 0.6326(2) 0.4259(7) 0.1486(2) 0.0335(15) Uani 1 1 d . . . . .
H22 H 0.660404 0.495872 0.154253 0.040 Uiso 1 1 calc R . . . .
C4 C 0.4640(3) -0.3118(8) 0.4129(2) 0.0385(16) Uani 1 1 d . . . . .
H4A H 0.467096 -0.402307 0.432210 0.046 Uiso 1 1 calc R . . . .
C16 C 0.6582(2) 0.5692(7) 0.3776(2) 0.0270(13) Uani 1 1 d . . . . .
C10 C 0.7536(2) 0.1149(8) 0.4585(2) 0.0343(15) Uani 1 1 d . . . . .
H10 H 0.753398 0.051635 0.484280 0.041 Uiso 1 1 calc R . . . .
C11 C 0.7955(2) 0.2044(8) 0.4630(2) 0.0409(17) Uani 1 1 d . . . . .
H11 H 0.823666 0.204076 0.491506 0.049 Uiso 1 1 calc R . . . .
C18 C 0.7043(2) 0.7511(7) 0.3482(2) 0.0399(17) Uani 1 1 d . . . . .
H18 H 0.727731 0.835576 0.352871 0.048 Uiso 1 1 calc R . . . .
C1 C 0.3635(2) -0.0512(8) 0.3307(2) 0.0356(16) Uani 1 1 d . . . . .
H1A H 0.342649 -0.130422 0.308326 0.043 Uiso 1 1 calc R . . . .
H1B H 0.345346 -0.019608 0.351941 0.043 Uiso 1 1 calc R . . . .
C12 C 0.7962(2) 0.2954(8) 0.4254(2) 0.0391(16) Uani 1 1 d . . . . .
H12 H 0.824616 0.360125 0.428260 0.047 Uiso 1 1 calc R . . . .
C19 C 0.6803(2) 0.6905(7) 0.3040(2) 0.0350(15) Uani 1 1 d . . . . .
H19 H 0.686895 0.732570 0.277694 0.042 Uiso 1 1 calc R . . . .
C26 C 0.5969(3) 0.1583(10) 0.0238(2) 0.058(2) Uani 1 1 d . . . . .
H26 H 0.589942 0.096457 -0.003780 0.070 Uiso 1 1 calc R . . . .
C2 C 0.4139(2) -0.1228(7) 0.35899(19) 0.0275(14) Uani 1 1 d . . . . .
C31 C 0.7366(3) 0.2084(14) 0.2622(3) 0.091(4) Uani 1 1 d . . . . .
H31A H 0.730589 0.211729 0.228412 0.136 Uiso 1 1 calc GR . . . .
H31B H 0.771827 0.178499 0.279166 0.136 Uiso 1 1 calc GR . . . .
H31C H 0.730002 0.312732 0.272755 0.136 Uiso 1 1 calc GR . . . .
C29 C 0.5680(3) -0.0834(7) 0.2625(2) 0.0420(18) Uani 1 1 d . . . . .
H29A H 0.595276 -0.125247 0.252782 0.063 Uiso 1 1 calc GR . . . .
H29B H 0.535584 -0.127183 0.242239 0.063 Uiso 1 1 calc GR . . . .
H29C H 0.574041 -0.113109 0.295153 0.063 Uiso 1 1 calc GR . . . .
C32 C 0.5611(4) 0.3312(17) 0.4854(3) 0.121(5) Uani 1 1 d . U . . .
H32A H 0.571883 0.221162 0.492402 0.182 Uiso 1 1 calc GR . . . .
H32B H 0.532079 0.352033 0.495190 0.182 Uiso 1 1 calc GR . . . .
H32C H 0.589031 0.401727 0.502315 0.182 Uiso 1 1 calc GR . . . .
C30 C 0.5114(2) 0.5362(7) 0.3127(2) 0.0371(16) Uani 1 1 d . . . . .
H30A H 0.533559 0.580317 0.342601 0.056 Uiso 1 1 calc GR . . . .
H30B H 0.476362 0.566933 0.307298 0.056 Uiso 1 1 calc GR . . . .
H30C H 0.521685 0.576763 0.287110 0.056 Uiso 1 1 calc GR . . . .
H1 H 0.344(2) 0.096(11) 0.283(2) 0.11(4) Uiso 1 1 d 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
Ho1 Ho2 3.8306(4) 2_655 ?
Ho1 O8 2.287(4) . ?
Ho1 O7 2.271(4) . ?
Ho1 O3 2.293(4) . ?
Ho1 O5 2.350(3) . ?
Ho1 O2 2.343(3) . ?
Ho1 N3 2.562(4) . ?
Ho1 O4 2.456(4) . ?
Ho1 N4 2.566(5) . ?
Ho2 O6 2.292(4) . ?
Ho2 O8 2.271(3) 2_655 ?
Ho2 O1 2.432(4) 2_655 ?
Ho2 O7 2.285(3) . ?
Ho2 O5 2.359(3) . ?
Ho2 O2 2.365(4) 2_655 ?
Ho2 N1 2.567(4) 2_655 ?
Ho2 N6 2.560(5) . ?
O6 C28 1.333(7) . ?
O8 C30 1.404(7) . ?
O1 C1 1.415(7) . ?
O7 C29 1.405(7) . ?
O3 C14 1.318(7) . ?
O5 C21 1.303(6) . ?
C21 C20 1.475(8) . ?
C21 N5 1.297(7) . ?
N2 N3 1.400(6) . ?
N2 C7 1.307(7) . ?
C20 N4 1.354(7) . ?
C20 C19 1.386(8) . ?
C27 C28 1.405(8) . ?
C27 C26 1.385(10) . ?
O2 C7 1.296(6) . ?
N1 C6 1.347(7) . ?
N1 C2 1.336(7) . ?
C3 C4 1.375(9) . ?
C3 C2 1.387(8) . ?
N3 C8 1.284(7) . ?
O4 C15 1.417(7) . ?
O9 C31 1.422(10) . ?
C28 C23 1.407(9) . ?
N5 N6 1.423(6) . ?
N6 C22 1.287(7) . ?
C23 C24 1.407(8) . ?
C23 C22 1.443(9) . ?
C15 C16 1.490(8) . ?
C24 C25 1.412(10) . ?
C17 C16 1.386(8) . ?
C17 C18 1.371(9) . ?
N4 C16 1.333(7) . ?
C25 C26 1.383(12) . ?
C7 C6 1.480(8) . ?
C8 C9 1.444(8) . ?
C14 C13 1.406(8) . ?
C14 C9 1.415(8) . ?
C6 C5 1.384(8) . ?
C13 C12 1.387(9) . ?
C9 C10 1.404(8) . ?
O10 C32 1.270(10) . ?
C5 C4 1.381(9) . ?
C10 C11 1.369(9) . ?
C11 C12 1.384(10) . ?
C18 C19 1.376(9) . ?
C1 C2 1.508(8) . ?

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
O8 Ho1 Ho2 32.70(9) . 2_655 ?
O8 Ho1 O3 159.89(13) . . ?
O8 Ho1 O5 88.79(13) . . ?
O8 Ho1 O2 66.61(13) . . ?
O8 Ho1 N3 120.37(14) . . ?
O8 Ho1 O4 81.16(13) . . ?
O8 Ho1 N4 89.21(13) . . ?
O7 Ho1 Ho2 84.92(9) . 2_655 ?
O7 Ho1 O8 102.57(13) . . ?
O7 Ho1 O3 92.34(13) . . ?
O7 Ho1 O5 66.69(13) . . ?
O7 Ho1 O2 81.27(13) . . ?
O7 Ho1 N3 98.42(14) . . ?
O7 Ho1 O4 168.26(13) . . ?
O7 Ho1 N4 128.86(14) . . ?
O3 Ho1 Ho2 165.65(10) . 2_655 ?
O3 Ho1 O5 84.78(13) . . ?
O3 Ho1 O2 129.92(13) . . ?
O3 Ho1 N3 69.63(14) . . ?
O3 Ho1 O4 86.93(14) . . ?
O3 Ho1 N4 70.85(14) . . ?
O5 Ho1 Ho2 106.87(9) . 2_655 ?
O5 Ho1 N3 150.20(14) . . ?
O5 Ho1 O4 124.83(13) . . ?
O5 Ho1 N4 63.99(13) . . ?
O2 Ho1 Ho2 35.75(9) . 2_655 ?
O2 Ho1 O5 134.29(12) . . ?
O2 Ho1 N3 62.47(13) . . ?
O2 Ho1 O4 90.20(13) . . ?
O2 Ho1 N4 146.15(14) . . ?
N3 Ho1 Ho2 96.79(10) . 2_655 ?
N3 Ho1 N4 118.05(14) . . ?
O4 Ho1 Ho2 92.89(9) . 2_655 ?
O4 Ho1 N3 70.33(14) . . ?
O4 Ho1 N4 61.79(13) . . ?
N4 Ho1 Ho2 121.48(10) . 2_655 ?
O6 Ho2 O1 86.15(14) . 2_655 ?
O6 Ho2 O5 129.75(13) . . ?
O6 Ho2 O2 85.26(14) . 2_655 ?
O6 Ho2 N1 70.26(14) . 2_655 ?
O6 Ho2 N6 69.32(15) . . ?
O8 Ho2 O6 93.26(13) 2_655 . ?
O8 Ho2 O1 169.23(14) 2_655 2_655 ?
O8 Ho2 O7 102.69(13) 2_655 . ?
O8 Ho2 O5 80.59(13) 2_655 . ?
O8 Ho2 O2 66.48(13) 2_655 2_655 ?
O8 Ho2 N1 127.84(14) 2_655 2_655 ?
O8 Ho2 N6 98.38(14) 2_655 . ?
O1 Ho2 N1 61.96(15) 2_655 2_655 ?
O1 Ho2 N6 71.34(15) 2_655 . ?
O7 Ho2 O6 159.64(13) . . ?
O7 Ho2 O1 80.50(13) . 2_655 ?
O7 Ho2 O5 66.32(13) . . ?
O7 Ho2 O2 89.56(13) . 2_655 ?
O7 Ho2 N1 89.83(13) . 2_655 ?
O7 Ho2 N6 119.74(14) . . ?
O5 Ho2 O1 91.51(13) . 2_655 ?
O5 Ho2 O2 133.79(12) . 2_655 ?
O5 Ho2 N1 147.62(13) . 2_655 ?
O5 Ho2 N6 62.54(13) . . ?
O2 Ho2 O1 124.11(14) 2_655 2_655 ?
O2 Ho2 N1 63.17(13) 2_655 2_655 ?
O2 Ho2 N6 150.00(14) 2_655 . ?
N6 Ho2 N1 118.81(14) . 2_655 ?
C28 O6 Ho2 129.7(4) . . ?
Ho2 O8 Ho1 114.34(15) 2_655 . ?
C30 O8 Ho1 122.6(3) . . ?
C30 O8 Ho2 123.0(3) . 2_655 ?
C1 O1 Ho2 128.0(4) . 2_655 ?
Ho1 O7 Ho2 114.93(16) . . ?
C29 O7 Ho1 121.9(3) . . ?
C29 O7 Ho2 122.9(3) . . ?
C14 O3 Ho1 129.7(3) . . ?
Ho1 O5 Ho2 109.32(14) . . ?
C21 O5 Ho1 124.6(3) . . ?
C21 O5 Ho2 122.9(3) . . ?
O5 C21 C20 116.5(5) . . ?
N5 C21 O5 126.1(5) . . ?
N5 C21 C20 117.2(5) . . ?
C7 N2 N3 110.2(4) . . ?
N4 C20 C21 114.0(5) . . ?
N4 C20 C19 121.8(5) . . ?
C19 C20 C21 124.1(5) . . ?
C26 C27 C28 121.1(7) . . ?
Ho1 O2 Ho2 108.90(14) . 2_655 ?
C7 O2 Ho1 123.5(3) . . ?
C7 O2 Ho2 125.4(3) . 2_655 ?
C6 N1 Ho2 118.5(3) . 2_655 ?
C2 N1 Ho2 122.5(4) . 2_655 ?
C2 N1 C6 117.4(5) . . ?
C4 C3 C2 118.4(6) . . ?
N2 N3 Ho1 118.6(3) . . ?
C8 N3 Ho1 126.5(4) . . ?
C8 N3 N2 113.0(5) . . ?
C15 O4 Ho1 127.4(3) . . ?
O6 C28 C27 120.4(6) . . ?
O6 C28 C23 121.4(5) . . ?
C27 C28 C23 118.2(6) . . ?
C21 N5 N6 109.6(4) . . ?
N5 N6 Ho2 118.8(3) . . ?
C22 N6 Ho2 127.3(4) . . ?
C22 N6 N5 111.9(5) . . ?
C28 C23 C22 123.5(5) . . ?
C24 C23 C28 121.0(6) . . ?
C24 C23 C22 115.5(6) . . ?
O4 C15 C16 110.2(5) . . ?
C23 C24 C25 118.9(7) . . ?
C18 C17 C16 119.4(6) . . ?
C20 N4 Ho1 116.9(4) . . ?
C16 N4 Ho1 122.3(4) . . ?
C16 N4 C20 118.6(5) . . ?
C26 C25 C24 120.1(7) . . ?
N2 C7 C6 118.2(5) . . ?
O2 C7 N2 125.2(5) . . ?
O2 C7 C6 116.6(5) . . ?
N3 C8 C9 126.2(5) . . ?
O3 C14 C13 120.9(5) . . ?
O3 C14 C9 121.8(5) . . ?
C13 C14 C9 117.3(5) . . ?
N1 C6 C7 113.0(5) . . ?
N1 C6 C5 123.0(5) . . ?
C5 C6 C7 124.0(5) . . ?
C12 C13 C14 121.9(6) . . ?
C14 C9 C8 122.9(5) . . ?
C10 C9 C8 117.7(5) . . ?
C10 C9 C14 119.3(5) . . ?
C4 C5 C6 118.4(6) . . ?
N6 C22 C23 125.4(6) . . ?
C3 C4 C5 119.5(6) . . ?
C17 C16 C15 122.0(5) . . ?
N4 C16 C15 116.1(5) . . ?
N4 C16 C17 122.0(6) . . ?
C11 C10 C9 122.2(6) . . ?
C10 C11 C12 119.0(6) . . ?
C17 C18 C19 119.1(6) . . ?
O1 C1 C2 110.1(5) . . ?
C11 C12 C13 120.2(6) . . ?
C18 C19 C20 119.0(6) . . ?
C27 C26 C25 120.6(7) . . ?
N1 C2 C3 123.2(6) . . ?
N1 C2 C1 115.6(5) . . ?
C3 C2 C1 121.2(5) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Ho1 O3 C14 C13 -129.1(5) . . . . ?
Ho1 O3 C14 C9 51.5(7) . . . . ?
Ho1 O5 C21 C20 -19.9(6) . . . . ?
Ho1 O5 C21 N5 157.1(4) . . . . ?
Ho1 O2 C7 N2 1.9(7) . . . . ?
Ho1 O2 C7 C6 179.5(3) . . . . ?
Ho1 N3 C8 C9 -15.1(8) . . . . ?
Ho1 O4 C15 C16 0.5(7) . . . . ?
Ho1 N4 C16 C15 -18.5(7) . . . . ?
Ho1 N4 C16 C17 161.6(4) . . . . ?
Ho2 O6 C28 C27 130.0(5) . . . . ?
Ho2 O6 C28 C23 -51.8(7) . . . . ?
Ho2 O1 C1 C2 -7.1(7) 2_655 . . . ?
Ho2 O5 C21 C20 -177.6(3) . . . . ?
Ho2 O5 C21 N5 -0.7(8) . . . . ?
Ho2 O2 C7 N2 -159.6(4) 2_655 . . . ?
Ho2 O2 C7 C6 18.0(6) 2_655 . . . ?
Ho2 N1 C6 C7 -10.5(6) 2_655 . . . ?
Ho2 N1 C6 C5 168.0(4) 2_655 . . . ?
Ho2 N1 C2 C3 -165.6(4) 2_655 . . . ?
Ho2 N1 C2 C1 13.8(6) 2_655 . . . ?
Ho2 N6 C22 C23 14.9(9) . . . . ?
O6 C28 C23 C24 -175.0(5) . . . . ?
O6 C28 C23 C22 4.4(9) . . . . ?
O1 C1 C2 N1 -4.8(7) . . . . ?
O1 C1 C2 C3 174.6(5) . . . . ?
O3 C14 C13 C12 -179.4(6) . . . . ?
O3 C14 C9 C8 -4.7(8) . . . . ?
O3 C14 C9 C10 177.2(5) . . . . ?
O5 C21 C20 N4 4.0(7) . . . . ?
O5 C21 C20 C19 -179.7(5) . . . . ?
O5 C21 N5 N6 -1.0(8) . . . . ?
C21 C20 N4 Ho1 11.0(6) . . . . ?
C21 C20 N4 C16 174.5(5) . . . . ?
C21 C20 C19 C18 -173.6(6) . . . . ?
C21 N5 N6 Ho2 2.1(6) . . . . ?
C21 N5 N6 C22 -163.1(5) . . . . ?
N2 N3 C8 C9 -179.0(5) . . . . ?
N2 C7 C6 N1 174.5(5) . . . . ?
N2 C7 C6 C5 -4.0(8) . . . . ?
C20 C21 N5 N6 175.9(4) . . . . ?
C20 N4 C16 C15 178.9(5) . . . . ?
C20 N4 C16 C17 -0.9(8) . . . . ?
C27 C28 C23 C24 3.3(9) . . . . ?
C27 C28 C23 C22 -177.3(6) . . . . ?
O2 C7 C6 N1 -3.3(7) . . . . ?
O2 C7 C6 C5 178.2(5) . . . . ?
N1 C6 C5 C4 -0.4(9) . . . . ?
N3 N2 C7 O2 0.0(8) . . . . ?
N3 N2 C7 C6 -177.6(4) . . . . ?
N3 C8 C9 C14 -10.1(9) . . . . ?
N3 C8 C9 C10 168.0(6) . . . . ?
O4 C15 C16 C17 -168.8(5) . . . . ?
O4 C15 C16 N4 11.4(8) . . . . ?
C28 C27 C26 C25 -0.3(11) . . . . ?
C28 C23 C24 C25 -2.9(10) . . . . ?
C28 C23 C22 N6 10.7(10) . . . . ?
N5 C21 C20 N4 -173.2(5) . . . . ?
N5 C21 C20 C19 3.1(8) . . . . ?
N5 N6 C22 C23 178.5(5) . . . . ?
C23 C24 C25 C26 0.8(11) . . . . ?
C24 C23 C22 N6 -169.9(6) . . . . ?
C24 C25 C26 C27 0.7(11) . . . . ?
C17 C18 C19 C20 0.0(10) . . . . ?
N4 C20 C19 C18 2.4(9) . . . . ?
C7 N2 N3 Ho1 -1.6(6) . . . . ?
C7 N2 N3 C8 163.7(5) . . . . ?
C7 C6 C5 C4 177.9(5) . . . . ?
C8 C9 C10 C11 -175.6(6) . . . . ?
C14 C13 C12 C11 2.0(10) . . . . ?
C14 C9 C10 C11 2.6(9) . . . . ?
C6 N1 C2 C3 -0.2(8) . . . . ?
C6 N1 C2 C1 179.2(5) . . . . ?
C6 C5 C4 C3 -3.1(9) . . . . ?
C13 C14 C9 C8 175.9(5) . . . . ?
C13 C14 C9 C10 -2.2(8) . . . . ?
C9 C14 C13 C12 -0.1(9) . . . . ?
C9 C10 C11 C12 -0.7(10) . . . . ?
C22 C23 C24 C25 177.7(6) . . . . ?
C4 C3 C2 N1 -3.2(9) . . . . ?
C4 C3 C2 C1 177.4(6) . . . . ?
C16 C17 C18 C19 -2.8(10) . . . . ?
C10 C11 C12 C13 -1.6(10) . . . . ?
C18 C17 C16 C15 -176.5(6) . . . . ?
C18 C17 C16 N4 3.3(9) . . . . ?
C19 C20 N4 Ho1 -165.5(4) . . . . ?
C19 C20 N4 C16 -2.0(8) . . . . ?
C26 C27 C28 O6 176.6(6) . . . . ?
C26 C27 C28 C23 -1.7(9) . . . . ?
C2 N1 C6 C7 -176.5(4) . . . . ?
C2 N1 C6 C5 2.0(8) . . . . ?
C2 C3 C4 C5 4.8(9) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
