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

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

data_s
_database_code_depnum_ccdc_archive 'CCDC 1856586'
loop_
_audit_author_name
_audit_author_address
'Xiu-Mei Zhang'
;Huaibei Normal University
China
;
_audit_update_record             
;
2019-10-18 deposited with the CCDC.	2019-11-21 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2016/6
_shelx_SHELXL_version_number     2016/6
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C60 H60 N4 O50 Pr4'
_chemical_formula_weight         2200.76

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'
Pr Pr -0.2180 2.8214 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      trigonal
_space_group_IT_number           147
_space_group_name_H-M_alt        'P -3'
_space_group_name_Hall           '-P 3'

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

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'

_cell_length_a                   23.2883(16)
_cell_length_b                   23.2883(16)
_cell_length_c                   14.1304(11)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     6636.8(10)
_cell_formula_units_Z            3
_cell_measurement_temperature    298(2)
_cell_measurement_reflns_used    9974
_cell_measurement_theta_min      2.27
_cell_measurement_theta_max      25.79

_exptl_crystal_description       block
_exptl_crystal_colour            green
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.652
_exptl_crystal_F_000             3252
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.080
_exptl_absorpt_coefficient_mu    2.262
_shelx_estimated_absorpt_T_min   0.805
_shelx_estimated_absorpt_T_max   0.840
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.5473
_exptl_absorpt_correction_T_max  0.7455
_exptl_absorpt_process_details   SADABS
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      298(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            47456
_diffrn_reflns_av_unetI/netI     0.0432
_diffrn_reflns_av_R_equivalents  0.0642
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         1.441
_diffrn_reflns_theta_max         24.997
_diffrn_reflns_theta_full        24.997
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             7812
_reflns_number_gt                6265
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0424P)²+11.2010P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         7812
_refine_ls_number_parameters     487
_refine_ls_number_restraints     462
_refine_ls_R_factor_all          0.0489
_refine_ls_R_factor_gt           0.0369
_refine_ls_wR_factor_ref         0.0923
_refine_ls_wR_factor_gt          0.0888
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_restrained_S_all      1.006
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Pr1 Pr -0.09671(2) 0.37660(2) 0.47668(2) 0.02885(9) Uani 1 1 d . U . . .
Pr2 Pr -0.15339(2) 0.21548(2) 0.31610(2) 0.03100(9) Uani 1 1 d . U . . .
O1 O -0.0206(2) 0.45285(18) 0.3644(3) 0.0513(11) Uani 1 1 d . U . . .
O2 O 0.0431(2) 0.55858(19) 0.3878(3) 0.0583(12) Uani 1 1 d . U . . .
O3 O 0.1350(2) 0.6961(2) -0.2005(3) 0.0485(10) Uani 1 1 d . U . . .
O4 O 0.15975(17) 0.66192(18) -0.3313(2) 0.0378(9) Uani 1 1 d . U . . .
O5 O 0.1935(2) 0.4648(2) -0.3183(3) 0.0516(11) Uani 1 1 d . U . . .
O6 O 0.1635(2) 0.4048(2) -0.1888(3) 0.0580(12) Uani 1 1 d . U . . .
O7 O 0.0126(3) 0.3545(2) 0.0645(3) 0.0724(15) Uani 1 1 d . U . . .
O8 O -0.0022(2) 0.4096(2) -0.0445(3) 0.0614(12) Uani 1 1 d . U . . .
O9 O 0.01206(18) 0.3766(2) 0.4858(2) 0.0457(10) Uani 1 1 d . U . . .
O10 O -0.04939(16) 0.31522(17) 0.3676(2) 0.0351(8) Uani 1 1 d . U . . .
O11 O 0.24322(17) 0.41560(19) 0.5217(2) 0.0381(9) Uani 1 1 d . U . . .
O12 O 0.29337(19) 0.4097(2) 0.3946(3) 0.0579(12) Uani 1 1 d . U . . .
O13 O 0.1056(3) 0.1834(2) -0.1647(4) 0.095(2) Uani 1 1 d . U . . .
O14 O 0.1860(2) 0.2856(2) -0.2018(3) 0.0524(11) Uani 1 1 d . U . . .
O15 O 0.1902(3) 0.4536(2) 0.1254(4) 0.0783(15) Uani 1 1 d . U . . .
O16 O 0.2704(3) 0.4480(3) 0.0659(5) 0.116(2) Uani 1 1 d . U . . .
O17 O -0.2227(3) 0.0953(2) 0.3468(4) 0.0812(15) Uani 1 1 d . U . . .
H17A H -0.215712 0.065192 0.312602 0.097 Uiso 1 1 calc R U . . .
H17B H -0.255801 0.080094 0.392626 0.097 Uiso 1 1 calc R U . . .
O18 O -0.0913(3) 0.1767(2) 0.4198(3) 0.0774(15) Uani 1 1 d . U . . .
H18A H -0.064874 0.161622 0.392480 0.093 Uiso 1 1 calc R U . . .
H18C H -0.094741 0.177450 0.485256 0.093 Uiso 1 1 calc R U . . .
O19 O -0.1132(2) 0.4780(2) 0.4740(3) 0.0663(13) Uani 1 1 d . U . . .
H19A H -0.095483 0.509441 0.522044 0.080 Uiso 1 1 calc R U . . .
H19B H -0.136903 0.483185 0.425005 0.080 Uiso 1 1 calc R U . . .
O20 O -0.2060(2) 0.3473(2) 0.5484(4) 0.0822(17) Uani 1 1 d . U . . .
H20A H -0.207717 0.363988 0.607481 0.099 Uiso 1 1 calc R U . . .
H20C H -0.245093 0.319673 0.516018 0.099 Uiso 1 1 calc R U . . .
N1 N 0.0188(2) 0.4054(2) 0.0325(3) 0.0425(11) Uani 1 1 d . U . . .
N2 N 0.2134(3) 0.4240(3) 0.0872(4) 0.0624(15) Uani 1 1 d . U . . .
C1 C 0.0242(3) 0.5076(2) 0.3391(3) 0.0332(12) Uani 1 1 d . U . . .
C2 C 0.0530(2) 0.5141(2) 0.2423(3) 0.0319(11) Uani 1 1 d . U . . .
C3 C 0.1018(3) 0.5742(3) 0.2078(4) 0.0390(13) Uani 1 1 d . U . . .
H3A H 0.119845 0.611262 0.246959 0.047 Uiso 1 1 calc R U . . .
C4 C 0.1245(3) 0.5804(3) 0.1153(3) 0.0399(13) Uani 1 1 d . U . . .
H4A H 0.157376 0.621505 0.093517 0.048 Uiso 1 1 calc R U . . .
C5 C 0.0991(3) 0.5263(3) 0.0550(3) 0.0321(11) Uani 1 1 d . U . . .
C6 C 0.0514(2) 0.4654(2) 0.0936(3) 0.0290(11) Uani 1 1 d . U . . .
C7 C 0.0293(2) 0.4584(2) 0.1845(3) 0.0304(11) Uani 1 1 d . U . . .
H7A H -0.001291 0.416749 0.207736 0.036 Uiso 1 1 calc R U . . .
C8 C 0.1214(3) 0.5361(3) -0.0468(3) 0.0325(11) Uani 1 1 d . U . . .
C9 C 0.1265(3) 0.5904(3) -0.0960(3) 0.0329(12) Uani 1 1 d . U . . .
H9A H 0.117506 0.620345 -0.065194 0.040 Uiso 1 1 calc R U . . .
C10 C 0.1450(2) 0.6001(3) -0.1912(3) 0.0322(11) Uani 1 1 d . U . . .
C11 C 0.1596(3) 0.5562(3) -0.2358(3) 0.0368(12) Uani 1 1 d . U . . .
H11A H 0.171702 0.562204 -0.299315 0.044 Uiso 1 1 calc R U . . .
C12 C 0.1565(3) 0.5029(3) -0.1866(4) 0.0371(12) Uani 1 1 d . U . . .
C13 C 0.1372(3) 0.4929(3) -0.0923(4) 0.0401(13) Uani 1 1 d . U . . .
H13A H 0.134954 0.457207 -0.059457 0.048 Uiso 1 1 calc R U . . .
C14 C 0.1715(3) 0.4543(3) -0.2332(4) 0.0433(14) Uani 1 1 d . U . . .
C15 C 0.1466(2) 0.6563(3) -0.2429(4) 0.0354(12) Uani 1 1 d . U . . .
C16 C 0.0060(2) 0.3451(3) 0.4092(4) 0.0351(12) Uani 1 1 d . U . . .
C17 C 0.0655(2) 0.3470(2) 0.3665(3) 0.0306(11) Uani 1 1 d . U . . .
C18 C 0.0638(3) 0.3262(3) 0.2737(3) 0.0372(12) Uani 1 1 d . U . . .
H18B H 0.024448 0.308065 0.239592 0.045 Uiso 1 1 calc R U . . .
C19 C 0.1213(3) 0.3324(3) 0.2313(3) 0.0375(13) Uani 1 1 d . U . . .
C20 C 0.1778(3) 0.3559(3) 0.2856(4) 0.0426(14) Uani 1 1 d . U . . .
H20B H 0.215479 0.358326 0.258933 0.051 Uiso 1 1 calc R U . . .
C21 C 0.1805(2) 0.3763(3) 0.3797(3) 0.0343(12) Uani 1 1 d . U . . .
C22 C 0.1237(2) 0.3725(3) 0.4192(4) 0.0330(11) Uani 1 1 d . U . . .
H22A H 0.124781 0.386990 0.480822 0.040 Uiso 1 1 calc R U . . .
C23 C 0.2425(3) 0.4014(3) 0.4334(4) 0.0379(13) Uani 1 1 d . U . . .
C24 C 0.1226(3) 0.3120(3) 0.1314(4) 0.0417(13) Uani 1 1 d . U . . .
C25 C 0.0793(3) 0.2478(3) 0.1019(4) 0.0613(18) Uani 1 1 d . U . . .
H25A H 0.046024 0.218909 0.142773 0.074 Uiso 1 1 calc R U . . .
C26 C 0.0844(3) 0.2256(3) 0.0129(4) 0.064(2) Uani 1 1 d . U . . .
H26A H 0.053829 0.182641 -0.005738 0.077 Uiso 1 1 calc R U . . .
C27 C 0.1351(3) 0.2674(3) -0.0492(4) 0.0494(15) Uani 1 1 d . U . . .
C28 C 0.1793(3) 0.3324(3) -0.0214(4) 0.0442(14) Uani 1 1 d . U . . .
H28A H 0.213257 0.361137 -0.061390 0.053 Uiso 1 1 calc R U . . .
C29 C 0.1715(3) 0.3531(3) 0.0672(4) 0.0436(14) Uani 1 1 d . U . . .
C30 C 0.1425(4) 0.2433(3) -0.1448(4) 0.0553(16) Uani 1 1 d . U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Pr1 O2 2.370(4) 4_566 ?
Pr1 O1 2.380(3) . ?
Pr1 O4 2.421(3) 4_565 ?
Pr1 O20 2.498(4) . ?
Pr1 O12 2.528(4) 6_556 ?
Pr1 O9 2.536(4) . ?
Pr1 O19 2.576(4) . ?
Pr1 O10 2.685(3) . ?
Pr1 O11 2.698(3) 6_556 ?
Pr1 C16 2.986(5) . ?
Pr1 C23 2.990(5) 6_556 ?
Pr1 Pr2 4.0021(4) . ?
Pr2 O14 2.346(4) 6 ?
Pr2 O17 2.473(4) . ?
Pr2 O11 2.480(3) 6_556 ?
Pr2 O10 2.483(3) . ?
Pr2 O3 2.492(4) 4_565 ?
Pr2 O18 2.522(4) . ?
Pr2 O5 2.530(4) 6 ?
Pr2 O6 2.533(4) 6 ?
Pr2 C14 2.901(6) 6 ?
Pr2 O4 2.940(4) 4_565 ?
Pr2 C15 3.088(6) 4_565 ?
O1 C1 1.229(6) . ?
O2 C1 1.247(6) . ?
O3 C15 1.240(6) . ?
O4 C15 1.277(6) . ?
O5 C14 1.282(6) . ?
O6 C14 1.243(7) . ?
O7 N1 1.206(6) . ?
O8 N1 1.217(6) . ?
O9 C16 1.276(6) . ?
O10 C16 1.262(6) . ?
O11 C23 1.289(6) . ?
O12 C23 1.230(6) . ?
O13 C30 1.251(8) . ?
O14 C30 1.283(7) . ?
O15 N2 1.197(7) . ?
O16 N2 1.192(8) . ?
N1 C6 1.488(6) . ?
N2 C29 1.465(8) . ?
C1 C2 1.497(7) . ?
C2 C3 1.378(7) . ?
C2 C7 1.393(7) . ?
C3 C4 1.391(7) . ?
C4 C5 1.383(7) . ?
C5 C6 1.403(7) . ?
C5 C8 1.506(6) . ?
C6 C7 1.363(6) . ?
C8 C13 1.390(7) . ?
C8 C9 1.396(7) . ?
C9 C10 1.396(6) . ?
C10 C11 1.382(7) . ?
C10 C15 1.483(7) . ?
C11 C12 1.390(7) . ?
C12 C13 1.388(7) . ?
C12 C14 1.495(7) . ?
C16 C17 1.493(7) . ?
C17 C18 1.391(7) . ?
C17 C22 1.392(7) . ?
C18 C19 1.406(7) . ?
C19 C20 1.380(7) . ?
C19 C24 1.494(7) . ?
C20 C21 1.403(7) . ?
C21 C22 1.396(7) . ?
C21 C23 1.470(7) . ?
C24 C25 1.385(8) . ?
C24 C29 1.395(8) . ?
C25 C26 1.387(8) . ?
C26 C27 1.402(8) . ?
C27 C28 1.394(8) . ?
C27 C30 1.505(8) . ?
C28 C29 1.386(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
O2 Pr1 O1 96.02(14) 4_566 . ?
O2 Pr1 O4 161.78(15) 4_566 4_565 ?
O1 Pr1 O4 78.34(13) . 4_565 ?
O2 Pr1 O20 89.23(16) 4_566 . ?
O1 Pr1 O20 138.71(17) . . ?
O4 Pr1 O20 84.07(16) 4_565 . ?
O2 Pr1 O12 75.09(14) 4_566 6_556 ?
O1 Pr1 O12 146.47(15) . 6_556 ?
O4 Pr1 O12 118.88(12) 4_565 6_556 ?
O20 Pr1 O12 74.32(17) . 6_556 ?
O2 Pr1 O9 75.58(14) 4_566 . ?
O1 Pr1 O9 70.31(14) . . ?
O4 Pr1 O9 117.63(12) 4_565 . ?
O20 Pr1 O9 149.42(16) . . ?
O12 Pr1 O9 76.16(14) 6_556 . ?
O2 Pr1 O19 72.56(16) 4_566 . ?
O1 Pr1 O19 72.72(14) . . ?
O4 Pr1 O19 89.22(14) 4_565 . ?
O20 Pr1 O19 69.96(15) . . ?
O12 Pr1 O19 131.37(15) 6_556 . ?
O9 Pr1 O19 127.42(14) . . ?
O2 Pr1 O10 125.25(14) 4_566 . ?
O1 Pr1 O10 70.35(12) . . ?
O4 Pr1 O10 69.51(11) 4_565 . ?
O20 Pr1 O10 136.15(13) . . ?
O12 Pr1 O10 88.27(13) 6_556 . ?
O9 Pr1 O10 49.72(11) . . ?
O19 Pr1 O10 140.26(13) . . ?
O2 Pr1 O11 124.00(12) 4_566 6_556 ?
O1 Pr1 O11 132.74(12) . 6_556 ?
O4 Pr1 O11 69.81(11) 4_565 6_556 ?
O20 Pr1 O11 72.07(13) . 6_556 ?
O12 Pr1 O11 49.28(12) 6_556 6_556 ?
O9 Pr1 O11 94.41(12) . 6_556 ?
O19 Pr1 O11 138.13(13) . 6_556 ?
O10 Pr1 O11 66.28(11) . 6_556 ?
O2 Pr1 C16 100.56(15) 4_566 . ?
O1 Pr1 C16 65.26(14) . . ?
O4 Pr1 C16 92.84(13) 4_565 . ?
O20 Pr1 C16 153.44(15) . . ?
O12 Pr1 C16 84.35(15) 6_556 . ?
O9 Pr1 C16 25.05(12) . . ?
O19 Pr1 C16 136.50(14) . . ?
O10 Pr1 C16 24.99(11) . . ?
O11 Pr1 C16 82.08(13) 6_556 . ?
O2 Pr1 C23 98.49(14) 4_566 6_556 ?
O1 Pr1 C23 148.63(15) . 6_556 ?
O4 Pr1 C23 94.96(13) 4_565 6_556 ?
O20 Pr1 C23 69.31(16) . 6_556 ?
O12 Pr1 C23 23.92(13) 6_556 6_556 ?
O9 Pr1 C23 86.60(15) . 6_556 ?
O19 Pr1 C23 138.35(15) . 6_556 ?
O10 Pr1 C23 78.56(13) . 6_556 ?
O11 Pr1 C23 25.54(12) 6_556 6_556 ?
C16 Pr1 C23 84.76(15) . 6_556 ?
O2 Pr1 Pr2 151.27(12) 4_566 . ?
O1 Pr1 Pr2 95.45(9) . . ?
O4 Pr1 Pr2 46.92(9) 4_565 . ?
O20 Pr1 Pr2 99.24(11) . . ?
O12 Pr1 Pr2 80.84(9) 6_556 . ?
O9 Pr1 Pr2 83.69(9) . . ?
O19 Pr1 Pr2 136.12(11) . . ?
O10 Pr1 Pr2 37.46(7) . . ?
O11 Pr1 Pr2 37.45(7) 6_556 . ?
C16 Pr1 Pr2 61.17(10) . . ?
C23 Pr1 Pr2 60.10(10) 6_556 . ?
O14 Pr2 O17 86.05(17) 6 . ?
O14 Pr2 O11 154.54(13) 6 6_556 ?
O17 Pr2 O11 91.84(14) . 6_556 ?
O14 Pr2 O10 93.57(13) 6 . ?
O17 Pr2 O10 141.91(15) . . ?
O11 Pr2 O10 72.72(11) 6_556 . ?
O14 Pr2 O3 83.95(14) 6 4_565 ?
O17 Pr2 O3 142.77(15) . 4_565 ?
O11 Pr2 O3 111.69(12) 6_556 4_565 ?
O10 Pr2 O3 74.60(13) . 4_565 ?
O14 Pr2 O18 79.01(16) 6 . ?
O17 Pr2 O18 70.07(17) . . ?
O11 Pr2 O18 76.44(15) 6_556 . ?
O10 Pr2 O18 72.48(14) . . ?
O3 Pr2 O18 141.63(16) 4_565 . ?
O14 Pr2 O5 129.29(13) 6 6 ?
O17 Pr2 O5 74.96(17) . 6 ?
O11 Pr2 O5 74.00(12) 6_556 6 ?
O10 Pr2 O5 129.65(12) . 6 ?
O3 Pr2 O5 84.04(14) 4_565 6 ?
O18 Pr2 O5 132.80(16) . 6 ?
O14 Pr2 O6 78.05(13) 6 6 ?
O17 Pr2 O6 70.69(17) . 6 ?
O11 Pr2 O6 125.04(13) 6_556 6 ?
O10 Pr2 O6 146.38(14) . 6 ?
O3 Pr2 O6 72.17(15) 4_565 6 ?
O18 Pr2 O6 135.44(16) . 6 ?
O5 Pr2 O6 51.39(12) 6 6 ?
O14 Pr2 C14 103.33(15) 6 6 ?
O17 Pr2 C14 72.33(18) . 6 ?
O11 Pr2 C14 100.14(14) 6_556 6 ?
O10 Pr2 C14 143.48(14) . 6 ?
O3 Pr2 C14 75.29(15) 4_565 6 ?
O18 Pr2 C14 142.08(17) . 6 ?
O5 Pr2 C14 26.18(14) 6 6 ?
O6 Pr2 C14 25.28(14) 6 6 ?
O14 Pr2 O4 128.89(13) 6 4_565 ?
O17 Pr2 O4 139.95(15) . 4_565 ?
O11 Pr2 O4 65.01(10) 6_556 4_565 ?
O10 Pr2 O4 64.49(10) . 4_565 ?
O3 Pr2 O4 46.88(11) 4_565 4_565 ?
O18 Pr2 O4 128.46(13) . 4_565 ?
O5 Pr2 O4 67.59(12) 6 4_565 ?
O6 Pr2 O4 95.46(13) 6 4_565 ?
C14 Pr2 O4 79.88(14) 6 4_565 ?
O14 Pr2 C15 105.99(15) 6 4_565 ?
O17 Pr2 C15 147.41(16) . 4_565 ?
O11 Pr2 C15 89.28(13) 6_556 4_565 ?
O10 Pr2 C15 68.85(12) . 4_565 ?
O3 Pr2 C15 22.61(12) 4_565 4_565 ?
O18 Pr2 C15 141.21(15) . 4_565 ?
O5 Pr2 C15 74.08(14) 6 4_565 ?
O6 Pr2 C15 82.12(15) 6 4_565 ?
C14 Pr2 C15 75.41(15) 6 4_565 ?
O4 Pr2 C15 24.31(11) 4_565 4_565 ?
O14 Pr2 Pr1 133.68(10) 6 . ?
O17 Pr2 Pr1 133.20(12) . . ?
O11 Pr2 Pr1 41.42(8) 6_556 . ?
O10 Pr2 Pr1 41.11(8) . . ?
O3 Pr2 Pr1 75.92(9) 4_565 . ?
O18 Pr2 Pr1 91.56(11) . . ?
O5 Pr2 Pr1 89.91(9) 6 . ?
O6 Pr2 Pr1 131.29(11) 6 . ?
C14 Pr2 Pr1 110.93(12) 6 . ?
O4 Pr2 Pr1 36.99(7) 4_565 . ?
C15 Pr2 Pr1 56.64(10) 4_565 . ?
C1 O1 Pr1 153.7(4) . . ?
C1 O2 Pr1 151.1(4) . 4_566 ?
C15 O3 Pr2 106.8(3) . 4_565 ?
C15 O4 Pr1 136.2(3) . 4_565 ?
C15 O4 Pr2 84.4(3) . 4_565 ?
Pr1 O4 Pr2 96.09(11) 4_565 4_565 ?
C14 O5 Pr2 93.3(3) . 5 ?
C14 O6 Pr2 94.2(3) . 5 ?
C16 O9 Pr1 97.6(3) . . ?
C16 O10 Pr2 154.4(3) . . ?
C16 O10 Pr1 91.0(3) . . ?
Pr2 O10 Pr1 101.44(11) . . ?
C23 O11 Pr2 144.6(4) . 5_556 ?
C23 O11 Pr1 90.0(3) . 5_556 ?
Pr2 O11 Pr1 101.13(11) 5_556 5_556 ?
C23 O12 Pr1 99.6(3) . 5_556 ?
C30 O14 Pr2 149.2(4) . 5 ?
O7 N1 O8 124.0(5) . . ?
O7 N1 C6 117.3(5) . . ?
O8 N1 C6 118.6(5) . . ?
O16 N2 O15 124.2(7) . . ?
O16 N2 C29 116.0(6) . . ?
O15 N2 C29 119.8(6) . . ?
O1 C1 O2 122.7(5) . . ?
O1 C1 C2 118.4(4) . . ?
O2 C1 C2 118.7(4) . . ?
C3 C2 C7 118.7(5) . . ?
C3 C2 C1 121.8(4) . . ?
C7 C2 C1 119.5(4) . . ?
C2 C3 C4 121.0(5) . . ?
C5 C4 C3 121.2(5) . . ?
C4 C5 C6 116.3(4) . . ?
C4 C5 C8 119.5(5) . . ?
C6 C5 C8 124.2(4) . . ?
C7 C6 C5 123.2(4) . . ?
C7 C6 N1 116.7(4) . . ?
C5 C6 N1 120.0(4) . . ?
C6 C7 C2 119.4(5) . . ?
C13 C8 C9 119.5(4) . . ?
C13 C8 C5 121.9(5) . . ?
C9 C8 C5 118.6(4) . . ?
C8 C9 C10 120.4(5) . . ?
C11 C10 C9 119.3(5) . . ?
C11 C10 C15 121.6(4) . . ?
C9 C10 C15 119.1(5) . . ?
C10 C11 C12 120.7(5) . . ?
C13 C12 C11 119.9(5) . . ?
C13 C12 C14 118.2(5) . . ?
C11 C12 C14 121.8(5) . . ?
C12 C13 C8 120.2(5) . . ?
O6 C14 O5 120.7(5) . . ?
O6 C14 C12 119.8(5) . . ?
O5 C14 C12 119.4(5) . . ?
O6 C14 Pr2 60.5(3) . 5 ?
O5 C14 Pr2 60.5(3) . 5 ?
C12 C14 Pr2 173.7(4) . 5 ?
O3 C15 O4 121.8(5) . . ?
O3 C15 C10 120.2(4) . . ?
O4 C15 C10 118.0(5) . . ?
O3 C15 Pr2 50.6(3) . 4_565 ?
O4 C15 Pr2 71.3(3) . 4_565 ?
C10 C15 Pr2 170.0(4) . 4_565 ?
O10 C16 O9 120.1(5) . . ?
O10 C16 C17 120.4(5) . . ?
O9 C16 C17 119.4(4) . . ?
O10 C16 Pr1 64.0(3) . . ?
O9 C16 Pr1 57.3(3) . . ?
C17 C16 Pr1 165.4(4) . . ?
C18 C17 C22 120.3(5) . . ?
C18 C17 C16 120.4(4) . . ?
C22 C17 C16 119.3(4) . . ?
C17 C18 C19 120.4(5) . . ?
C20 C19 C18 118.3(5) . . ?
C20 C19 C24 119.0(5) . . ?
C18 C19 C24 122.7(5) . . ?
C19 C20 C21 122.3(5) . . ?
C22 C21 C20 118.5(5) . . ?
C22 C21 C23 122.0(5) . . ?
C20 C21 C23 119.5(5) . . ?
C17 C22 C21 120.1(5) . . ?
O12 C23 O11 120.2(5) . . ?
O12 C23 C21 120.7(5) . . ?
O11 C23 C21 119.1(5) . . ?
O12 C23 Pr1 56.5(3) . 5_556 ?
O11 C23 Pr1 64.5(3) . 5_556 ?
C21 C23 Pr1 170.4(4) . 5_556 ?
C25 C24 C29 116.7(5) . . ?
C25 C24 C19 120.4(5) . . ?
C29 C24 C19 122.4(5) . . ?
C24 C25 C26 121.5(6) . . ?
C25 C26 C27 120.5(6) . . ?
C28 C27 C26 119.0(5) . . ?
C28 C27 C30 119.9(5) . . ?
C26 C27 C30 121.1(6) . . ?
C29 C28 C27 118.6(5) . . ?
C28 C29 C24 123.5(5) . . ?
C28 C29 N2 115.9(5) . . ?
C24 C29 N2 120.2(5) . . ?
O13 C30 O14 123.6(6) . . ?
O13 C30 C27 118.3(6) . . ?
O14 C30 C27 118.0(6) . . ?

_refine_diff_density_max         0.985
_refine_diff_density_min         -0.709
_refine_diff_density_rms         0.103



####################################################################### 
# 
# 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 1856587'
loop_
_audit_author_name
_audit_author_address
'Xiu-Mei Zhang'
;Huaibei Normal University
China
;
_audit_update_record             
;
2019-10-18 deposited with the CCDC.	2019-11-21 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C16 H9 Gd N O9.50'
_chemical_formula_weight         524.49

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Gd Gd -0.1653 3.9035 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/c'
_space_group_name_Hall           '-P 2ybc'

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

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

_cell_length_a                   13.649(6)
_cell_length_b                   14.334(6)
_cell_length_c                   7.994(3)
_cell_angle_alpha                90
_cell_angle_beta                 92.233(16)
_cell_angle_gamma                90
_cell_volume                     1562.8(11)
_cell_formula_units_Z            4
_cell_measurement_temperature    298(2)
_cell_measurement_reflns_used    8115
_cell_measurement_theta_min      2.92
_cell_measurement_theta_max      27.47

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    2.229
_exptl_crystal_F_000             1008
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.080
_exptl_absorpt_coefficient_mu    4.305
_shelx_estimated_absorpt_T_min   0.673
_shelx_estimated_absorpt_T_max   0.725
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.5717
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   SADABS
_diffrn_ambient_temperature      298(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            32707
_diffrn_reflns_av_unetI/netI     0.0170
_diffrn_reflns_av_R_equivalents  0.0404
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_theta_min         2.919
_diffrn_reflns_theta_max         25.010
_diffrn_reflns_theta_full        25.010
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             2754
_reflns_number_gt                2562
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0131P)²+3.0806P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         2754
_refine_ls_number_parameters     263
_refine_ls_number_restraints     37
_refine_ls_R_factor_all          0.0238
_refine_ls_R_factor_gt           0.0206
_refine_ls_wR_factor_ref         0.0445
_refine_ls_wR_factor_gt          0.0435
_refine_ls_goodness_of_fit_ref   1.205
_refine_ls_restrained_S_all      1.206
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Gd1 Gd 0.59871(2) 0.70720(2) 0.62238(2) 0.01472(6) Uani 1 1 d . . . . .
N1 N 0.9535(2) 0.3758(3) 0.4399(4) 0.0342(8) Uani 1 1 d . . . . .
O1 O 0.60025(19) 0.65681(17) 0.2923(3) 0.0291(6) Uani 1 1 d . . . . .
O2 O 0.7153(2) 0.6092(2) 0.4689(4) 0.0424(8) Uani 1 1 d . . . . .
O3 O 0.52176(17) 0.82142(18) 0.4109(3) 0.0236(6) Uani 1 1 d . . . . .
O4 O 0.4261(2) 0.7597(3) 0.5946(5) 0.0571(11) Uani 1 1 d . . . . .
O5 O 0.71396(19) 0.8534(2) 0.3089(3) 0.0429(8) Uani 1 1 d . . . . .
O6 O 0.74348(19) 0.79408(19) 0.5628(4) 0.0328(6) Uani 1 1 d . . . . .
O7 O 1.0112(3) 0.4002(3) 0.5518(4) 0.0690(12) Uani 1 1 d . . . . .
O8 O 0.8698(2) 0.3490(3) 0.4678(4) 0.0499(9) Uani 1 1 d . . . . .
O9 O 0.5191(2) 0.5639(2) 0.5691(3) 0.0375(7) Uani 1 1 d . U . . .
H9 H 0.5619 0.5253 0.5919 0.045 Uiso 0.5 1 calc R U P E .
O10 O 0.3479(9) 0.5870(11) 0.3810(15) 0.050(3) Uani 0.5 1 d . U P A -2
H10D H 0.3335 0.5381 0.4351 0.059 Uiso 0.5 1 d R U P A -2
H10E H 0.3681 0.6284 0.4501 0.059 Uiso 0.5 1 d R U P A -2
C1 C 0.6697(3) 0.6011(2) 0.3319(5) 0.0227(8) Uani 1 1 d . . . B -2
C2 C 0.6930(2) 0.5185(2) 0.2275(4) 0.0177(7) Uani 1 1 d . . . B -2
C3 C 0.6186(2) 0.4651(3) 0.1515(4) 0.0212(8) Uani 1 1 d . . . B -2
H3A H 0.5541 0.4861 0.1498 0.025 Uiso 1 1 calc R U . B -2
C4 C 0.6414(2) 0.3803(3) 0.0782(4) 0.0195(7) Uani 1 1 d . . . B -2
C5 C 0.7393(3) 0.3524(3) 0.0675(5) 0.0242(8) Uani 1 1 d . . . B -2
H5A H 0.7544 0.2979 0.0109 0.029 Uiso 1 1 calc R U . B -2
C6 C 0.8144(2) 0.4066(2) 0.1417(4) 0.0205(7) Uani 1 1 d . . . B -2
C7 C 0.7899(3) 0.4875(3) 0.2263(4) 0.0215(7) Uani 1 1 d . . . B -2
H7A H 0.8388 0.5216 0.2829 0.026 Uiso 1 1 calc R U . B -2
C8 C 0.4396(2) 0.8169(2) 0.4800(5) 0.0212(8) Uani 1 1 d . . . C -2
C9 C 0.9197(2) 0.3802(3) 0.1298(5) 0.0225(8) Uani 1 1 d . . . B -2
C10 C 0.9579(3) 0.3673(3) -0.0284(5) 0.0265(8) Uani 1 1 d . . . B -2
H10A H 0.9158 0.3704 -0.1226 0.032 Uiso 1 1 calc R U . B -2
C11 C 1.0572(3) 0.3499(3) -0.0489(5) 0.0259(8) Uani 1 1 d . . . B -2
H11A H 1.0800 0.3387 -0.1551 0.031 Uiso 1 1 calc R U . B -2
C12 C 1.1218(3) 0.3493(3) 0.0893(5) 0.0238(8) Uani 1 1 d . . . B -2
C13 C 1.0865(3) 0.3628(3) 0.2481(5) 0.0275(9) Uani 1 1 d . . . B -2
H13A H 1.1294 0.3641 0.3414 0.033 Uiso 1 1 calc R U . B -2
C14 C 0.9864(3) 0.3744(3) 0.2661(5) 0.0243(8) Uani 1 1 d . . . B -2
C15 C 0.7698(3) 0.8312(3) 0.4303(5) 0.0258(8) Uani 1 1 d . . . D -2
C16 C 0.4542(6) 0.5276(5) 0.4583(9) 0.0261(15) Uani 0.5 1 d D U P E -1
C17 C 0.3699(13) 0.5713(17) 0.358(2) 0.056(4) Uani 0.5 1 d D U P E -1
H17A H 0.3940 0.6216 0.2922 0.084 Uiso 0.5 1 calc R U P E -1
H17B H 0.3225 0.5949 0.4334 0.084 Uiso 0.5 1 calc R U P E -1
H17C H 0.3397 0.5253 0.2861 0.084 Uiso 0.5 1 calc R U P E -1


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Gd1 O5 2.295(3) 4_576 ?
Gd1 O9 2.355(3) . ?
Gd1 O1 2.376(3) 4_576 ?
Gd1 O6 2.399(3) . ?
Gd1 O4 2.475(3) . ?
Gd1 O2 2.483(3) . ?
Gd1 O3 2.550(3) . ?
Gd1 O3 2.604(3) 4_576 ?
Gd1 O1 2.737(3) . ?
N1 O7 1.220(5) . ?
N1 O8 1.233(4) . ?
N1 C14 1.477(5) . ?
O1 C1 1.269(4) . ?
O1 Gd1 2.375(3) 4_575 ?
O2 C1 1.244(5) . ?
O3 C8 1.271(4) . ?
O3 Gd1 2.604(3) 4_575 ?
O4 C8 1.248(5) . ?
O5 C15 1.252(5) . ?
O5 Gd1 2.295(3) 4_575 ?
O6 C15 1.251(5) . ?
O9 C16 1.334(7) . ?
C1 C2 1.490(5) . ?
C2 C3 1.392(5) . ?
C2 C7 1.395(5) . ?
C3 C4 1.390(5) . ?
C4 C5 1.401(5) . ?
C5 C6 1.400(5) . ?
C6 C7 1.391(5) . ?
C6 C9 1.492(5) . ?
C9 C14 1.395(5) . ?
C9 C10 1.399(5) . ?
C10 C11 1.394(5) . ?
C11 C12 1.387(5) . ?
C12 C13 1.389(5) . ?
C13 C14 1.389(5) . ?
C16 C17 1.511(10) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O5 Gd1 O9 95.00(12) 4_576 . ?
O5 Gd1 O1 87.05(11) 4_576 4_576 ?
O9 Gd1 O1 144.37(9) . 4_576 ?
O5 Gd1 O6 77.08(11) 4_576 . ?
O9 Gd1 O6 142.64(10) . . ?
O1 Gd1 O6 72.46(9) 4_576 . ?
O5 Gd1 O4 143.05(11) 4_576 . ?
O9 Gd1 O4 79.51(12) . . ?
O1 Gd1 O4 77.82(12) 4_576 . ?
O6 Gd1 O4 127.80(10) . . ?
O5 Gd1 O2 70.78(11) 4_576 . ?
O9 Gd1 O2 73.59(11) . . ?
O1 Gd1 O2 139.05(10) 4_576 . ?
O6 Gd1 O2 69.31(11) . . ?
O4 Gd1 O2 138.94(12) . . ?
O5 Gd1 O3 158.06(10) 4_576 . ?
O9 Gd1 O3 105.37(10) . . ?
O1 Gd1 O3 81.17(9) 4_576 . ?
O6 Gd1 O3 81.73(9) . . ?
O4 Gd1 O3 51.63(9) . . ?
O2 Gd1 O3 106.92(10) . . ?
O5 Gd1 O3 69.81(9) 4_576 4_576 ?
O9 Gd1 O3 79.83(8) . 4_576 ?
O1 Gd1 O3 67.52(9) 4_576 4_576 ?
O6 Gd1 O3 128.42(9) . 4_576 ?
O4 Gd1 O3 73.27(10) . 4_576 ?
O2 Gd1 O3 129.58(10) . 4_576 ?
O3 Gd1 O3 121.23(9) . 4_576 ?
O5 Gd1 O1 119.71(9) 4_576 . ?
O9 Gd1 O1 67.44(8) . . ?
O1 Gd1 O1 140.15(7) 4_576 . ?
O6 Gd1 O1 84.73(9) . . ?
O4 Gd1 O1 92.11(11) . . ?
O2 Gd1 O1 49.07(9) . . ?
O3 Gd1 O1 63.17(8) . . ?
O3 Gd1 O1 146.21(8) 4_576 . ?
O7 N1 O8 122.2(4) . . ?
O7 N1 C14 118.8(3) . . ?
O8 N1 C14 118.9(3) . . ?
C1 O1 Gd1 130.4(2) . 4_575 ?
C1 O1 Gd1 87.7(2) . . ?
Gd1 O1 Gd1 109.55(10) 4_575 . ?
C1 O2 Gd1 100.3(2) . . ?
C8 O3 Gd1 91.5(2) . . ?
C8 O3 Gd1 140.3(2) . 4_575 ?
Gd1 O3 Gd1 108.43(9) . 4_575 ?
C8 O4 Gd1 95.6(2) . . ?
C15 O5 Gd1 142.0(3) . 4_575 ?
C15 O6 Gd1 130.9(2) . . ?
C16 O9 Gd1 138.6(4) . . ?
O2 C1 O1 120.3(3) . . ?
O2 C1 C2 117.1(3) . . ?
O1 C1 C2 122.3(3) . . ?
C3 C2 C7 119.9(3) . . ?
C3 C2 C1 120.8(3) . . ?
C7 C2 C1 118.7(3) . . ?
C4 C3 C2 119.5(3) . . ?
C3 C4 C5 120.3(3) . . ?
C6 C5 C4 120.0(3) . . ?
C7 C6 C5 118.9(3) . . ?
C7 C6 C9 119.5(3) . . ?
C5 C6 C9 121.6(3) . . ?
C6 C7 C2 121.0(3) . . ?
O4 C8 O3 120.7(3) . . ?
C14 C9 C10 116.3(3) . . ?
C14 C9 C6 124.5(3) . . ?
C10 C9 C6 119.0(3) . . ?
C11 C10 C9 121.9(3) . . ?
C12 C11 C10 119.9(4) . . ?
C11 C12 C13 119.6(3) . . ?
C14 C13 C12 119.3(3) . . ?
C13 C14 C9 122.8(3) . . ?
C13 C14 N1 115.8(3) . . ?
C9 C14 N1 121.4(3) . . ?
O6 C15 O5 125.3(3) . . ?
O9 C16 C17 131.4(11) . . ?

_refine_diff_density_max         0.476
_refine_diff_density_min         -0.539
_refine_diff_density_rms         0.084

####################################################################### 
# 
# 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 1856588'
loop_
_audit_author_name
_audit_author_address
'Xiu-Mei Zhang'
;Huaibei Normal University
China
;
_audit_update_record             
;
2019-10-18 deposited with the CCDC.	2019-11-21 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C15 H12 Dy N O11'
_chemical_formula_weight         544.76

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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Dy Dy -0.1892 4.4098 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

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

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   9.4885(11)
_cell_length_b                   9.5857(10)
_cell_length_c                   12.4176(14)
_cell_angle_alpha                93.605(4)
_cell_angle_beta                 108.083(4)
_cell_angle_gamma                112.343(3)
_cell_volume                     971.80(19)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    9978
_cell_measurement_theta_min      3.21
_cell_measurement_theta_max      27.50

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.862
_exptl_crystal_F_000             526
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.080
_exptl_absorpt_coefficient_mu    3.901
_shelx_estimated_absorpt_T_min   0.696
_shelx_estimated_absorpt_T_max   0.745
_exptl_absorpt_correction_type   none
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            19762
_diffrn_reflns_av_unetI/netI     0.0200
_diffrn_reflns_av_R_equivalents  0.0307
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         3.213
_diffrn_reflns_theta_max         25.006
_diffrn_reflns_theta_full        25.006
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measured_fraction_theta_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_point_group_measured_fraction_full 0.997
_reflns_number_total             3425
_reflns_number_gt                3239
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0510P)²+8.8381P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         3425
_refine_ls_number_parameters     293
_refine_ls_number_restraints     781
_refine_ls_R_factor_all          0.0368
_refine_ls_R_factor_gt           0.0342
_refine_ls_wR_factor_ref         0.0974
_refine_ls_wR_factor_gt          0.0954
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_restrained_S_all      1.026
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Dy1 Dy 0.55111(3) -0.72636(3) 0.02324(2) 0.02048(12) Uani 1 1 d . U . . .
N1' N 0.716(3) 0.0176(15) 0.4631(16) 0.109(6) Uani 0.5 1 d D U P . .
N1 N 0.758(3) -0.434(2) 0.6193(14) 0.089(6) Uani 0.5 1 d . U P . .
O1 O 0.5798(7) -0.5822(6) 0.1916(5) 0.0441(12) Uani 1 1 d . U . . .
O2 O 0.5069(7) -0.4039(6) 0.1209(4) 0.0417(12) Uani 1 1 d . U . . .
O3 O 0.6693(6) 0.1807(6) 0.9123(5) 0.0375(11) Uani 1 1 d . U . . .
O4 O 0.5328(6) -0.0695(6) 0.8900(5) 0.0336(10) Uani 1 1 d . U . . .
O5 O 1.2960(5) 0.0751(5) 0.8740(4) 0.0309(10) Uani 1 1 d . U . . .
O6 O 1.2699(5) 0.2414(5) 0.9877(4) 0.0282(9) Uani 1 1 d . U . . .
O7 O 0.712(2) -0.5835(19) 0.5929(14) 0.093(4) Uani 0.5 1 d . U P A 1
O8 O 0.7757(19) -0.3956(16) 0.7142(11) 0.066(3) Uani 0.5 1 d . U P A 1
O9 O 0.7859(6) -0.7510(6) 0.1607(5) 0.0427(13) Uani 1 1 d D U . . .
H9D H 0.779(11) -0.737(11) 0.235(4) 0.051 Uiso 1 1 d D U . . .
H9C H 0.769(11) -0.855(4) 0.164(8) 0.051 Uiso 1 1 d D U . . .
O10 O 0.7899(7) -0.4990(6) 0.0513(6) 0.0483(14) Uani 1 1 d . U . . .
H10C H 0.7724 -0.4195 0.0396 0.058 Uiso 1 1 d R U . . .
H10D H 0.8922 -0.4703 0.0845 0.058 Uiso 1 1 d R U . . .
O11 O 1.1051(11) -0.4213(13) 0.1515(11) 0.108(3) Uani 1 1 d D U . . .
H1O H 1.12(2) -0.510(10) 0.175(13) 0.162 Uiso 1 1 d D U . . .
H2O H 1.179(19) -0.338(11) 0.215(9) 0.162 Uiso 1 1 d D U . . .
C1 C 0.5631(9) -0.4591(9) 0.2030(6) 0.0343(13) Uani 1 1 d . U . . .
C2 C 0.6125(10) -0.3745(9) 0.3243(6) 0.0384(14) Uani 1 1 d . U . . .
C3 C 0.6615(12) -0.4353(11) 0.4169(7) 0.0525(16) Uani 1 1 d . U . . .
H3 H 0.6586 -0.5333 0.4050 0.063 Uiso 1 1 calc R U . . .
C4 C 0.7163(12) -0.3536(10) 0.5298(7) 0.0506(15) Uani 1 1 d . U . . .
C5 C 0.7242(10) -0.2068(10) 0.5511(7) 0.0406(13) Uani 1 1 d . U . . .
C6 C 0.6688(12) -0.1514(10) 0.4557(7) 0.0528(16) Uani 1 1 d D U . . .
C7 C 0.6129(12) -0.2310(10) 0.3434(7) 0.0504(16) Uani 1 1 d . U . . .
H7 H 0.5759 -0.1884 0.2814 0.061 Uiso 1 1 calc R U . . .
O7' O 0.737(3) 0.103(2) 0.3879(15) 0.117(5) Uani 0.5 1 d D U P . .
C8 C 0.7919(9) -0.1114(9) 0.6705(6) 0.0355(13) Uani 1 1 d . U . . .
O8' O 0.641(2) 0.071(2) 0.5139(15) 0.097(4) Uani 0.5 1 d D U P . .
C9 C 0.9602(9) -0.0417(8) 0.7305(6) 0.0328(12) Uani 1 1 d . U . . .
H9 H 1.0288 -0.0616 0.6985 0.039 Uiso 1 1 calc R U . . .
C10 C 1.0276(8) 0.0581(8) 0.8384(6) 0.0270(11) Uani 1 1 d . U . . .
C11 C 0.9223(8) 0.0898(8) 0.8841(6) 0.0272(11) Uani 1 1 d . U . . .
H11 H 0.9652 0.1609 0.9532 0.033 Uiso 1 1 calc R U . . .
C12 C 0.7553(8) 0.0155(8) 0.8267(6) 0.0272(11) Uani 1 1 d . U . . .
C13 C 0.6897(9) -0.0866(9) 0.7213(6) 0.0345(12) Uani 1 1 d . U . . .
H13 H 0.5769 -0.1387 0.6846 0.041 Uiso 1 1 calc R U . . .
C14 C 1.2072(8) 0.1291(7) 0.9032(6) 0.0251(12) Uani 1 1 d . U . . .
C15 C 0.6427(8) 0.0433(8) 0.8784(6) 0.0253(11) Uani 1 1 d . U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Dy1 O4 2.288(5) 2_646 ?
Dy1 O2 2.293(5) 2_645 ?
Dy1 O1 2.313(5) . ?
Dy1 O3 2.348(5) 1_544 ?
Dy1 O10 2.380(5) . ?
Dy1 O9 2.454(5) . ?
Dy1 O6 2.456(4) 1_444 ?
Dy1 O5 2.487(4) 1_444 ?
Dy1 C14 2.841(6) 1_444 ?
N1' O7' 1.289(10) . ?
N1' O8' 1.292(10) . ?
N1' C6 1.496(9) . ?
N1 O8 1.15(2) . ?
N1 O7 1.32(2) . ?
N1 C4 1.431(19) . ?
O1 C1 1.254(9) . ?
O2 C1 1.245(9) . ?
O2 Dy1 2.293(5) 2_645 ?
O3 C15 1.259(8) . ?
O3 Dy1 2.349(5) 1_566 ?
O4 C15 1.238(8) . ?
O4 Dy1 2.289(5) 2_646 ?
O5 C14 1.268(8) . ?
O5 Dy1 2.487(4) 1_666 ?
O6 C14 1.264(8) . ?
O6 Dy1 2.456(4) 1_666 ?
O9 H9D 0.949(10) . ?
O9 H9C 0.949(10) . ?
O10 H10C 0.8507 . ?
O10 H10D 0.8501 . ?
O11 H1O 0.953(10) . ?
O11 H2O 0.952(10) . ?
C1 C2 1.505(10) . ?
C2 C3 1.356(12) . ?
C2 C7 1.380(11) . ?
C3 C4 1.396(11) . ?
C3 H3 0.9300 . ?
C4 C5 1.385(12) . ?
C5 C6 1.367(12) . ?
C5 C8 1.496(10) . ?
C6 C7 1.380(12) . ?
C7 H7 0.9300 . ?
C8 C13 1.390(10) . ?
C8 C9 1.392(10) . ?
C9 C10 1.400(9) . ?
C9 H9 0.9300 . ?
C10 C11 1.405(9) . ?
C10 C14 1.488(9) . ?
C11 C12 1.380(10) . ?
C11 H11 0.9300 . ?
C12 C13 1.389(10) . ?
C12 C15 1.499(9) . ?
C13 H13 0.9300 . ?
C14 Dy1 2.841(6) 1_666 ?

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 Dy1 O2 149.66(19) 2_646 2_645 ?
O4 Dy1 O1 84.1(2) 2_646 . ?
O2 Dy1 O1 106.5(2) 2_645 . ?
O4 Dy1 O3 99.58(18) 2_646 1_544 ?
O2 Dy1 O3 85.6(2) 2_645 1_544 ?
O1 Dy1 O3 149.43(19) . 1_544 ?
O4 Dy1 O10 139.22(19) 2_646 . ?
O2 Dy1 O10 71.1(2) 2_645 . ?
O1 Dy1 O10 78.2(2) . . ?
O3 Dy1 O10 79.55(19) 1_544 . ?
O4 Dy1 O9 68.95(18) 2_646 . ?
O2 Dy1 O9 140.1(2) 2_645 . ?
O1 Dy1 O9 79.9(2) . . ?
O3 Dy1 O9 73.4(2) 1_544 . ?
O10 Dy1 O9 71.90(19) . . ?
O4 Dy1 O6 80.54(16) 2_646 1_444 ?
O2 Dy1 O6 74.38(19) 2_645 1_444 ?
O1 Dy1 O6 77.76(18) . 1_444 ?
O3 Dy1 O6 132.81(17) 1_544 1_444 ?
O10 Dy1 O6 129.62(17) . 1_444 ?
O9 Dy1 O6 143.67(18) . 1_444 ?
O4 Dy1 O5 74.40(18) 2_646 1_444 ?
O2 Dy1 O5 76.89(18) 2_645 1_444 ?
O1 Dy1 O5 128.18(18) . 1_444 ?
O3 Dy1 O5 81.46(16) 1_544 1_444 ?
O10 Dy1 O5 143.7(2) . 1_444 ?
O9 Dy1 O5 130.59(17) . 1_444 ?
O6 Dy1 O5 52.80(14) 1_444 1_444 ?
O4 Dy1 C14 76.77(18) 2_646 1_444 ?
O2 Dy1 C14 73.2(2) 2_645 1_444 ?
O1 Dy1 C14 103.26(19) . 1_444 ?
O3 Dy1 C14 107.14(18) 1_544 1_444 ?
O10 Dy1 C14 142.97(19) . 1_444 ?
O9 Dy1 C14 145.12(19) . 1_444 ?
O6 Dy1 C14 26.34(17) 1_444 1_444 ?
O5 Dy1 C14 26.47(17) 1_444 1_444 ?
O7' N1' O8' 103.1(13) . . ?
O7' N1' C6 131.4(16) . . ?
O8' N1' C6 114.0(16) . . ?
O8 N1 O7 110.8(19) . . ?
O8 N1 C4 123.7(15) . . ?
O7 N1 C4 119.5(14) . . ?
C1 O1 Dy1 127.6(5) . . ?
C1 O2 Dy1 170.2(5) . 2_645 ?
C15 O3 Dy1 128.6(4) . 1_566 ?
C15 O4 Dy1 150.8(5) . 2_646 ?
C14 O5 Dy1 92.5(4) . 1_666 ?
C14 O6 Dy1 94.1(4) . 1_666 ?
Dy1 O9 H9D 107(6) . . ?
Dy1 O9 H9C 114(6) . . ?
H9D O9 H9C 90(8) . . ?
Dy1 O10 H10C 114.5 . . ?
Dy1 O10 H10D 135.5 . . ?
H10C O10 H10D 108.3 . . ?
H1O O11 H2O 105(2) . . ?
O2 C1 O1 124.3(6) . . ?
O2 C1 C2 118.2(6) . . ?
O1 C1 C2 117.4(7) . . ?
C3 C2 C7 118.6(7) . . ?
C3 C2 C1 121.0(7) . . ?
C7 C2 C1 120.4(7) . . ?
C2 C3 C4 121.2(8) . . ?
C2 C3 H3 119.4 . . ?
C4 C3 H3 119.4 . . ?
C5 C4 C3 121.2(8) . . ?
C5 C4 N1 123.4(9) . . ?
C3 C4 N1 115.4(9) . . ?
C6 C5 C4 115.9(7) . . ?
C6 C5 C8 121.2(7) . . ?
C4 C5 C8 122.9(7) . . ?
C5 C6 C7 123.7(8) . . ?
C5 C6 N1' 120.8(10) . . ?
C7 C6 N1' 112.5(10) . . ?
C2 C7 C6 119.3(8) . . ?
C2 C7 H7 120.3 . . ?
C6 C7 H7 120.3 . . ?
C13 C8 C9 119.1(7) . . ?
C13 C8 C5 121.0(7) . . ?
C9 C8 C5 119.9(7) . . ?
C8 C9 C10 121.0(6) . . ?
C8 C9 H9 119.5 . . ?
C10 C9 H9 119.5 . . ?
C9 C10 C11 118.7(6) . . ?
C9 C10 C14 120.6(6) . . ?
C11 C10 C14 120.7(6) . . ?
C12 C11 C10 120.1(6) . . ?
C12 C11 H11 120.0 . . ?
C10 C11 H11 120.0 . . ?
C11 C12 C13 120.6(6) . . ?
C11 C12 C15 120.1(6) . . ?
C13 C12 C15 119.3(6) . . ?
C12 C13 C8 120.3(7) . . ?
C12 C13 H13 119.8 . . ?
C8 C13 H13 119.8 . . ?
O6 C14 O5 120.5(6) . . ?
O6 C14 C10 119.9(6) . . ?
O5 C14 C10 119.6(6) . . ?
O6 C14 Dy1 59.6(3) . 1_666 ?
O5 C14 Dy1 61.0(3) . 1_666 ?
C10 C14 Dy1 178.0(5) . 1_666 ?
O4 C15 O3 123.5(6) . . ?
O4 C15 C12 118.3(6) . . ?
O3 C15 C12 118.1(6) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Dy1 O1 C1 O2 9.7(12) . . . . ?
Dy1 O1 C1 C2 -171.1(5) . . . . ?
O2 C1 C2 C3 174.4(8) . . . . ?
O1 C1 C2 C3 -4.8(12) . . . . ?
O2 C1 C2 C7 -7.3(12) . . . . ?
O1 C1 C2 C7 173.5(8) . . . . ?
C7 C2 C3 C4 -2.0(15) . . . . ?
C1 C2 C3 C4 176.3(9) . . . . ?
C2 C3 C4 C5 -0.7(16) . . . . ?
C2 C3 C4 N1 177.7(15) . . . . ?
O8 N1 C4 C5 14(3) . . . . ?
O7 N1 C4 C5 163.9(18) . . . . ?
O8 N1 C4 C3 -165(2) . . . . ?
O7 N1 C4 C3 -14(3) . . . . ?
C3 C4 C5 C6 2.7(14) . . . . ?
N1 C4 C5 C6 -175.5(16) . . . . ?
C3 C4 C5 C8 -176.0(9) . . . . ?
N1 C4 C5 C8 5.7(19) . . . . ?
C4 C5 C6 C7 -2.2(15) . . . . ?
C8 C5 C6 C7 176.5(9) . . . . ?
C4 C5 C6 N1' -161.2(13) . . . . ?
C8 C5 C6 N1' 17.5(16) . . . . ?
O7' N1' C6 C5 149(2) . . . . ?
O8' N1' C6 C5 -75(2) . . . . ?
O7' N1' C6 C7 -12(3) . . . . ?
O8' N1' C6 C7 124.1(16) . . . . ?
C3 C2 C7 C6 2.5(14) . . . . ?
C1 C2 C7 C6 -175.8(9) . . . . ?
C5 C6 C7 C2 -0.4(16) . . . . ?
N1' C6 C7 C2 160.2(13) . . . . ?
C6 C5 C8 C13 74.2(12) . . . . ?
C4 C5 C8 C13 -107.2(10) . . . . ?
C6 C5 C8 C9 -103.6(10) . . . . ?
C4 C5 C8 C9 75.1(12) . . . . ?
C13 C8 C9 C10 -2.9(12) . . . . ?
C5 C8 C9 C10 174.8(7) . . . . ?
C8 C9 C10 C11 -1.5(11) . . . . ?
C8 C9 C10 C14 178.5(7) . . . . ?
C9 C10 C11 C12 4.2(10) . . . . ?
C14 C10 C11 C12 -175.8(6) . . . . ?
C10 C11 C12 C13 -2.5(11) . . . . ?
C10 C11 C12 C15 176.9(6) . . . . ?
C11 C12 C13 C8 -2.1(11) . . . . ?
C15 C12 C13 C8 178.5(7) . . . . ?
C9 C8 C13 C12 4.8(12) . . . . ?
C5 C8 C13 C12 -173.0(7) . . . . ?
Dy1 O6 C14 O5 3.1(7) 1_666 . . . ?
Dy1 O6 C14 C10 -177.8(5) 1_666 . . . ?
Dy1 O5 C14 O6 -3.1(7) 1_666 . . . ?
Dy1 O5 C14 C10 177.8(5) 1_666 . . . ?
C9 C10 C14 O6 165.7(7) . . . . ?
C11 C10 C14 O6 -14.3(10) . . . . ?
C9 C10 C14 O5 -15.3(10) . . . . ?
C11 C10 C14 O5 164.8(6) . . . . ?
Dy1 O4 C15 O3 -108.3(9) 2_646 . . . ?
Dy1 O4 C15 C12 68.6(11) 2_646 . . . ?
Dy1 O3 C15 O4 7.7(10) 1_566 . . . ?
Dy1 O3 C15 C12 -169.2(4) 1_566 . . . ?
C11 C12 C15 O4 -126.7(7) . . . . ?
C13 C12 C15 O4 52.7(9) . . . . ?
C11 C12 C15 O3 50.3(9) . . . . ?
C13 C12 C15 O3 -130.3(7) . . . . ?

_refine_diff_density_max         1.803
_refine_diff_density_min         -1.371
_refine_diff_density_rms         0.168

