# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2022

####################################################################### 
# 
# 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_LaL66
_database_code_depnum_ccdc_archive 'CCDC 2096052'
loop_
_audit_author_name
_audit_author_address
'Ai Wang' 'Shanxi University'
_audit_update_record             
;
2022-07-19 deposited with the CCDC.	2022-07-21 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         'C18 H13 La N9 O8, H2 O'
_chemical_formula_sum            'C18 H15 La N9 O9'
_chemical_formula_weight         640.30

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'
La La -0.2871 2.4523 '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                   9.5199(5)
_cell_length_b                   10.4152(6)
_cell_length_c                   12.6533(7)
_cell_angle_alpha                84.4347(15)
_cell_angle_beta                 79.2703(15)
_cell_angle_gamma                67.2952(14)
_cell_volume                     1136.70(11)
_cell_formula_units_Z            2
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    9893
_cell_measurement_theta_min      2.64
_cell_measurement_theta_max      27.25

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.871
_exptl_crystal_F_000             630
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.260
_exptl_crystal_size_mid          0.250
_exptl_crystal_size_min          0.240
_exptl_absorpt_coefficient_mu    1.950
_shelx_estimated_absorpt_T_min   0.631
_shelx_estimated_absorpt_T_max   0.652
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6756
_exptl_absorpt_correction_T_max  0.7455
_exptl_absorpt_process_details   SADABS
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'Incoatec microsource'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            24825
_diffrn_reflns_av_unetI/netI     0.0288
_diffrn_reflns_av_R_equivalents  0.0298
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         2.639
_diffrn_reflns_theta_max         27.248
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             5038
_reflns_number_gt                4579
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT, SADABS and XPREP'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_computing_structure_refinement  'SHELXL-2014 (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)+(0.0197P)²+0.8337P] 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         5038
_refine_ls_number_parameters     390
_refine_ls_number_restraints     189
_refine_ls_R_factor_all          0.0281
_refine_ls_R_factor_gt           0.0228
_refine_ls_wR_factor_ref         0.0482
_refine_ls_wR_factor_gt          0.0466
_refine_ls_goodness_of_fit_ref   1.080
_refine_ls_restrained_S_all      1.127
_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
La1 La -0.04276(2) 0.96489(2) 0.68646(2) 0.01360(5) Uani 1 1 d . . . . .
N1 N -0.2741(2) 0.6499(2) 0.63549(16) 0.0205(4) Uani 1 1 d . . . . .
N2 N -0.3018(3) 0.5955(3) 0.73625(18) 0.0363(6) Uani 1 1 d . . . . .
N3 N -0.5051(2) 0.7867(3) 0.70299(19) 0.0361(6) Uani 1 1 d . . . . .
N4A N 0.5823(12) 0.6608(13) 0.3289(10) 0.0256(10) Uani 0.646(17) 1 d D U P A 1
N5A N 0.6009(9) 0.7810(9) 0.3547(7) 0.0360(13) Uani 0.646(17) 1 d D U P A 1
N6A N 0.6698(10) 0.7381(7) 0.1755(6) 0.0447(13) Uani 0.646(17) 1 d D U P A 1
C5A C 0.6542(9) 0.8196(9) 0.2596(7) 0.0394(12) Uani 0.646(17) 1 d D U P A 1
H5A H 0.6694 0.9026 0.2559 0.047 Uiso 0.646(17) 1 d DR U P A 1
C6A C 0.6250(11) 0.6392(8) 0.2259(6) 0.0418(12) Uani 0.646(17) 1 d D U P A 1
H6A H 0.5854 0.5658 0.1875 0.050 Uiso 0.646(17) 1 d DR U P A 1
N4B N 0.573(2) 0.668(2) 0.3284(18) 0.0282(15) Uani 0.354(17) 1 d D U P A 1
N5B N 0.6319(18) 0.7604(19) 0.3352(14) 0.0406(18) Uani 0.354(17) 1 d D U P A 1
N6B N 0.6194(16) 0.7432(13) 0.1632(10) 0.0450(15) Uani 0.354(17) 1 d D U P A 1
C5B C 0.6581(19) 0.8038(18) 0.2300(13) 0.0436(16) Uani 0.354(17) 1 d D U P A 1
H5B H 0.7111 0.8801 0.2177 0.052 Uiso 0.354(17) 1 d DR U P A 1
C6B C 0.5735(18) 0.6525(14) 0.2223(11) 0.0359(15) Uani 0.354(17) 1 d D U P A 1
H6B H 0.4989 0.6401 0.2118 0.043 Uiso 0.354(17) 1 d DR U P A 1
N7 N 0.1043(2) 0.6949(2) 1.06166(15) 0.0199(4) Uani 1 1 d . . . B 1
N8 N 0.2176(3) 0.7327(3) 1.00163(19) 0.0403(6) Uani 1 1 d . . . B 1
N9 N 0.1322(2) 0.8412(2) 1.15962(16) 0.0224(4) Uani 1 1 d . . . C 1
O1 O 0.17630(19) 0.83496(17) 0.54945(14) 0.0283(4) Uani 1 1 d . . . D 1
O2 O 0.26221(19) 0.82531(17) 0.37369(13) 0.0261(4) Uani 1 1 d . . . E 1
O3 O 0.0396(2) 0.70189(18) 0.74916(13) 0.0318(4) Uani 1 1 d . . . F 1
O4 O -0.0491(2) 0.84837(17) 0.88227(14) 0.0286(4) Uani 1 1 d . . . G 1
O5 O -0.15186(19) 0.87012(17) 0.56484(13) 0.0238(4) Uani 1 1 d . . . H 1
O6 O -0.06415(19) 0.85139(16) 0.38877(13) 0.0234(4) Uani 1 1 d . . . I 1
O7 O 0.18994(19) 0.93021(19) 0.77784(14) 0.0312(4) Uani 1 1 d . . . J 1
H7A H 0.1795 0.8814 0.8313 0.047 Uiso 1 1 d R U . J 1
H7B H 0.2805 0.8976 0.7490 0.047 Uiso 1 1 d R U . J 1
O8 O -0.3091(2) 0.9704(2) 0.77677(16) 0.0419(5) Uani 1 1 d . . . K 1
H8A H -0.3378 0.9311 0.8308 0.063 Uiso 1 1 d R U . K 1
H8B H -0.3803 1.0021 0.7420 0.063 Uiso 1 1 d R U . K 1
O9A O 0.5848(15) 0.8582(8) 0.9635(6) 0.091(3) Uani 0.60(2) 1 d . U P L 1
H9A H 0.5802 0.8696 1.0281 0.136 Uiso 0.60(2) 1 d R U P L 1
H9B H 0.6003 0.9245 0.9293 0.136 Uiso 0.60(2) 1 d R U P L 1
O9B O 0.650(2) 0.8911(13) 0.9822(9) 0.079(5) Uani 0.40(2) 1 d . U P L 2
H9C H 0.7323 0.8798 0.9423 0.119 Uiso 0.40(2) 1 d R U P L 2
H9D H 0.6696 0.8638 1.0428 0.119 Uiso 0.40(2) 1 d R U P L 2
C1 C 0.2690(2) 0.7791(2) 0.46788(19) 0.0180(5) Uani 1 1 d . . . . .
C2 C 0.3941(2) 0.6375(2) 0.48495(18) 0.0161(5) Uani 1 1 d . . . . .
C3 C 0.5336(3) 0.5814(2) 0.41562(18) 0.0192(5) Uani 1 1 d D U . . .
C4 C 0.3628(3) 0.5528(2) 0.57019(18) 0.0197(5) Uani 1 1 d . . . . .
H4 H 0.2711 0.5868 0.6184 0.024 Uiso 1 1 calc R U . . .
C7 C 0.0017(3) 0.7273(2) 0.84684(19) 0.0207(5) Uani 1 1 d . . . . .
C8 C 0.0093(3) 0.6078(2) 0.92643(18) 0.0186(5) Uani 1 1 d . . . . .
C9 C 0.0513(3) 0.5969(2) 1.02755(19) 0.0185(5) Uani 1 1 d . . . . .
C10 C -0.0412(3) 0.5087(2) 0.90031(19) 0.0205(5) Uani 1 1 d . . . . .
H10 H -0.0687 0.5132 0.8329 0.025 Uiso 1 1 calc R U . . .
C11 C 0.0566(3) 0.7604(3) 1.1541(2) 0.0238(5) Uani 1 1 d . . . . .
H11 H -0.0200 0.7505 1.2078 0.029 Uiso 1 1 calc R U . B 1
C12 C 0.2289(3) 0.8202(3) 1.0650(2) 0.0388(7) Uani 1 1 d . . . . .
H12 H 0.2986 0.8643 1.0457 0.047 Uiso 1 1 calc R U . B 1
C13 C -0.1333(3) 0.5788(2) 0.56587(18) 0.0176(5) Uani 1 1 d . . . . .
C14 C -0.3974(3) 0.7627(3) 0.6179(2) 0.0276(6) Uani 1 1 d . . . . .
H14 H -0.4055 0.8162 0.5544 0.033 Uiso 1 1 calc R U . . .
C15 C -0.4412(3) 0.6823(3) 0.7724(2) 0.0418(7) Uani 1 1 d . . . . .
H15 H -0.4926 0.6728 0.8410 0.050 Uiso 1 1 calc R U . . .
C16 C -0.0968(2) 0.8031(2) 0.48008(19) 0.0176(5) Uani 1 1 d . . . . .
C17 C -0.0584(3) 0.6473(2) 0.49001(18) 0.0173(5) Uani 1 1 d . . . . .
C18 C -0.0749(3) 0.4347(2) 0.57545(19) 0.0192(5) Uani 1 1 d . . . . .
H18 H -0.1265 0.3916 0.6272 0.023 Uiso 1 1 calc R U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
La1 O5 2.4702(16) . ?
La1 O1 2.4730(16) . ?
La1 O6 2.5283(16) 2_576 ?
La1 O2 2.5424(16) 2_576 ?
La1 O8 2.5613(18) . ?
La1 O7 2.5749(17) . ?
La1 O3 2.6268(17) . ?
La1 O4 2.6520(17) . ?
La1 N9 2.7230(19) 2_577 ?
N1 C14 1.338(3) . ?
N1 N2 1.366(3) . ?
N1 C13 1.429(3) . ?
N2 C15 1.309(4) . ?
N3 C14 1.310(3) . ?
N3 C15 1.352(4) . ?
N4A C6A 1.305(12) . ?
N4A N5A 1.406(19) . ?
N5A C5A 1.304(8) . ?
N6A C6A 1.327(8) . ?
N6A C5A 1.376(9) . ?
C5A H5A 0.9251 . ?
C5A H5B 1.0312 . ?
C6A H6A 1.1524 . ?
C6A H6B 1.2428 . ?
N4B N5B 1.31(4) . ?
N4B C6B 1.37(2) . ?
N4B C3 1.443(17) . ?
N5B C5B 1.372(16) . ?
N6B C5B 1.284(17) . ?
N6B C6B 1.305(14) . ?
C5B H5A 1.1582 . ?
C5B H5B 1.0806 . ?
C6B H6A 1.0013 . ?
C6B H6B 0.8047 . ?
N7 C11 1.326(3) . ?
N7 N8 1.363(3) . ?
N7 C9 1.431(3) . ?
N8 C12 1.317(3) . ?
N9 C11 1.315(3) . ?
N9 C12 1.347(3) . ?
N9 La1 2.7231(19) 2_577 ?
O1 C1 1.250(3) . ?
O2 C1 1.245(3) . ?
O2 La1 2.5424(16) 2_576 ?
O3 C7 1.246(3) . ?
O4 C7 1.258(3) . ?
O5 C16 1.251(3) . ?
O6 C16 1.248(3) . ?
O6 La1 2.5283(15) 2_576 ?
O7 H7A 0.8200 . ?
O7 H7B 0.8200 . ?
O8 H8A 0.8199 . ?
O8 H8B 0.8199 . ?
O9A H9A 0.8274 . ?
O9A H9B 0.8259 . ?
O9B H9C 0.8199 . ?
O9B H9D 0.8200 . ?
C1 C2 1.523(3) . ?
C2 C4 1.389(3) . ?
C2 C3 1.394(3) . ?
C3 C4 1.382(3) 2_666 ?
C4 C3 1.382(3) 2_666 ?
C4 H4 0.9300 . ?
C7 C8 1.512(3) . ?
C8 C10 1.383(3) . ?
C8 C9 1.392(3) . ?
C9 C10 1.381(3) 2_567 ?
C10 C9 1.381(3) 2_567 ?
C10 H10 0.9300 . ?
C11 H11 0.9300 . ?
C12 H12 0.9300 . ?
C13 C18 1.386(3) . ?
C13 C17 1.394(3) . ?
C14 H14 0.9300 . ?
C15 H15 0.9300 . ?
C16 C17 1.517(3) . ?
C17 C18 1.391(3) 2_566 ?
C18 C17 1.391(3) 2_566 ?
C18 H18 0.9300 . ?

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 La1 O1 73.93(6) . . ?
O5 La1 O6 118.06(5) . 2_576 ?
O1 La1 O6 78.03(5) . 2_576 ?
O5 La1 O2 75.27(6) . 2_576 ?
O1 La1 O2 118.84(6) . 2_576 ?
O6 La1 O2 72.08(6) 2_576 2_576 ?
O5 La1 O8 70.15(6) . . ?
O1 La1 O8 140.30(6) . . ?
O6 La1 O8 134.46(6) 2_576 . ?
O2 La1 O8 67.22(6) 2_576 . ?
O5 La1 O7 147.06(6) . . ?
O1 La1 O7 78.23(6) . . ?
O6 La1 O7 71.82(6) 2_576 . ?
O2 La1 O7 135.01(6) 2_576 . ?
O8 La1 O7 127.58(6) . . ?
O5 La1 O3 77.33(6) . . ?
O1 La1 O3 74.25(5) . . ?
O6 La1 O3 142.72(6) 2_576 . ?
O2 La1 O3 144.05(6) 2_576 . ?
O8 La1 O3 81.86(6) . . ?
O7 La1 O3 78.46(6) . . ?
O5 La1 O4 113.01(5) . . ?
O1 La1 O4 115.89(5) . . ?
O6 La1 O4 128.90(5) 2_576 . ?
O2 La1 O4 124.56(5) 2_576 . ?
O8 La1 O4 65.69(6) . . ?
O7 La1 O4 64.62(6) . . ?
O3 La1 O4 49.32(5) . . ?
O5 La1 N9 140.80(6) . 2_577 ?
O1 La1 N9 143.00(6) . 2_577 ?
O6 La1 N9 73.08(6) 2_576 2_577 ?
O2 La1 N9 73.30(6) 2_576 2_577 ?
O8 La1 N9 76.41(6) . 2_577 ?
O7 La1 N9 71.19(6) . 2_577 ?
O3 La1 N9 117.90(6) . 2_577 ?
O4 La1 N9 68.73(6) . 2_577 ?
C14 N1 N2 109.6(2) . . ?
C14 N1 C13 130.9(2) . . ?
N2 N1 C13 119.35(19) . . ?
C15 N2 N1 101.9(2) . . ?
C14 N3 C15 103.1(2) . . ?
C6A N4A N5A 110.3(8) . . ?
C5A N5A N4A 100.4(7) . . ?
C6A N6A C5A 101.6(6) . . ?
N5A C5A N6A 116.3(7) . . ?
N5A C5A H5A 116.0 . . ?
N6A C5A H5A 127.5 . . ?
N5A C5A H5B 145.4 . . ?
N6A C5A H5B 97.1 . . ?
H5A C5A H5B 33.3 . . ?
N4A C6A N6A 111.4(8) . . ?
N4A C6A H6A 118.9 . . ?
N6A C6A H6A 126.5 . . ?
N4A C6A H6B 94.5 . . ?
N6A C6A H6B 117.2 . . ?
H6A C6A H6B 44.6 . . ?
N5B N4B C6B 108.5(15) . . ?
N5B N4B C3 126(2) . . ?
C6B N4B C3 125(2) . . ?
N4B N5B C5B 102.8(17) . . ?
C5B N6B C6B 104.3(12) . . ?
N6B C5B N5B 114.1(15) . . ?
N6B C5B H5A 149.6 . . ?
N5B C5B H5A 91.6 . . ?
N6B C5B H5B 131.4 . . ?
N5B C5B H5B 114.5 . . ?
H5A C5B H5B 29.2 . . ?
N6B C6B N4B 110.0(14) . . ?
N6B C6B H6A 117.9 . . ?
N4B C6B H6A 127.0 . . ?
N6B C6B H6B 120.2 . . ?
N4B C6B H6B 113.3 . . ?
H6A C6B H6B 59.5 . . ?
C11 N7 N8 109.47(19) . . ?
C11 N7 C9 127.1(2) . . ?
N8 N7 C9 123.45(19) . . ?
C12 N8 N7 101.9(2) . . ?
C11 N9 C12 102.6(2) . . ?
C11 N9 La1 122.63(16) . 2_577 ?
C12 N9 La1 133.42(17) . 2_577 ?
C1 O1 La1 168.98(16) . . ?
C1 O2 La1 125.44(14) . 2_576 ?
C7 O3 La1 94.42(14) . . ?
C7 O4 La1 92.94(14) . . ?
C16 O5 La1 133.78(15) . . ?
C16 O6 La1 135.99(15) . 2_576 ?
La1 O7 H7A 103.8 . . ?
La1 O7 H7B 125.0 . . ?
H7A O7 H7B 107.7 . . ?
La1 O8 H8A 132.6 . . ?
La1 O8 H8B 118.3 . . ?
H8A O8 H8B 107.6 . . ?
H9A O9A H9B 107.6 . . ?
H9C O9B H9D 107.7 . . ?
O2 C1 O1 125.7(2) . . ?
O2 C1 C2 117.4(2) . . ?
O1 C1 C2 116.8(2) . . ?
C4 C2 C3 117.1(2) . . ?
C4 C2 C1 118.17(19) . . ?
C3 C2 C1 124.5(2) . . ?
C4 C3 C2 122.0(2) 2_666 . ?
C4 C3 N4B 119.1(7) 2_666 . ?
C2 C3 N4B 118.8(7) . . ?
C3 C4 C2 120.9(2) 2_666 . ?
C3 C4 H4 119.6 2_666 . ?
C2 C4 H4 119.6 . . ?
O3 C7 O4 123.2(2) . . ?
O3 C7 C8 118.4(2) . . ?
O4 C7 C8 118.3(2) . . ?
C10 C8 C9 117.9(2) . . ?
C10 C8 C7 117.5(2) . . ?
C9 C8 C7 124.4(2) . . ?
C10 C9 C8 120.9(2) 2_567 . ?
C10 C9 N7 117.3(2) 2_567 . ?
C8 C9 N7 121.8(2) . . ?
C9 C10 C8 121.2(2) 2_567 . ?
C9 C10 H10 119.4 2_567 . ?
C8 C10 H10 119.4 . . ?
N9 C11 N7 110.9(2) . . ?
N9 C11 H11 124.6 . . ?
N7 C11 H11 124.6 . . ?
N8 C12 N9 115.2(2) . . ?
N8 C12 H12 122.4 . . ?
N9 C12 H12 122.4 . . ?
C18 C13 C17 120.7(2) . . ?
C18 C13 N1 116.1(2) . . ?
C17 C13 N1 123.1(2) . . ?
N3 C14 N1 110.1(2) . . ?
N3 C14 H14 124.9 . . ?
N1 C14 H14 124.9 . . ?
N2 C15 N3 115.3(3) . . ?
N2 C15 H15 122.4 . . ?
N3 C15 H15 122.4 . . ?
O6 C16 O5 126.1(2) . . ?
O6 C16 C17 116.8(2) . . ?
O5 C16 C17 117.0(2) . . ?
C18 C17 C13 117.3(2) 2_566 . ?
C18 C17 C16 116.0(2) 2_566 . ?
C13 C17 C16 126.3(2) . . ?
C13 C18 C17 122.0(2) . 2_566 ?
C13 C18 H18 119.0 . . ?
C17 C18 H18 119.0 2_566 . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
C5A H5A O7 0.93 2.54 3.420(9) 159.1 2_676
C5B H5B O7 1.08 2.50 3.57(2) 169.9 2_676
C5A H5A O7 0.93 2.54 3.420(9) 159.1 2_676
C5B H5B O7 1.08 2.50 3.57(2) 169.9 2_676
O7 H7A N8 0.82 2.53 3.324(3) 164.3 .
O7 H7A O4 0.82 2.30 2.794(2) 119.4 .
O7 H7B N3 0.82 1.93 2.731(3) 167.3 1_655
O8 H8A O9A 0.82 1.91 2.731(8) 173.9 1_455
O9A H9A N6A 0.83 2.30 2.964(11) 138.0 1_556
O9A H9A N6B 0.83 2.05 2.710(15) 135.9 1_556
O9A H9B O8 0.83 2.05 2.731(8) 138.9 1_655
C4 H4 O3 0.93 2.45 3.378(3) 172.4 .
C10 H10 N2 0.93 2.55 3.333(3) 142.3 .
C11 H11 O6 0.93 2.51 3.077(3) 119.7 1_556
C14 H14 N5A 0.93 2.57 3.320(9) 137.4 1_455

_refine_diff_density_max         0.670
_refine_diff_density_min         -0.354
_refine_diff_density_rms         0.087

####################################################################### 
# 
# 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_CeL66
_database_code_depnum_ccdc_archive 'CCDC 2096053'
loop_
_audit_author_name
_audit_author_address
'Ai Wang' 'Shanxi University'
_audit_update_record             
;
2022-07-19 deposited with the CCDC.	2022-07-21 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         'C18 H13 Ce N9 O8, H2 O'
_chemical_formula_sum            'C18 H15 Ce N9 O9'
_chemical_formula_weight         641.51

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'
Ce Ce -0.2486 2.6331 '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                   9.4853(4)
_cell_length_b                   10.3887(5)
_cell_length_c                   12.6157(6)
_cell_angle_alpha                84.4594(15)
_cell_angle_beta                 79.4366(14)
_cell_angle_gamma                67.3666(14)
_cell_volume                     1127.50(9)
_cell_formula_units_Z            2
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    9768
_cell_measurement_theta_min      2.65
_cell_measurement_theta_max      28.29

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.890
_exptl_crystal_F_000             632
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.260
_exptl_crystal_size_mid          0.250
_exptl_crystal_size_min          0.240
_exptl_absorpt_coefficient_mu    2.091
_shelx_estimated_absorpt_T_min   0.612
_shelx_estimated_absorpt_T_max   0.634
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6759
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_process_details   SADABS
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'Incoatec microsource'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            34355
_diffrn_reflns_av_unetI/netI     0.0180
_diffrn_reflns_av_R_equivalents  0.0238
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         3.232
_diffrn_reflns_theta_max         28.306
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.969
_diffrn_measured_fraction_theta_full 0.963
_diffrn_reflns_Laue_measured_fraction_max 0.969
_diffrn_reflns_Laue_measured_fraction_full 0.963
_diffrn_reflns_point_group_measured_fraction_max 0.969
_diffrn_reflns_point_group_measured_fraction_full 0.963
_reflns_number_total             5437
_reflns_number_gt                5388
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT, SADABS and XPREP'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_computing_structure_refinement  'SHELXL-2014 (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)+(0.0071P)²+0.7180P] 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         5437
_refine_ls_number_parameters     390
_refine_ls_number_restraints     191
_refine_ls_R_factor_all          0.0140
_refine_ls_R_factor_gt           0.0138
_refine_ls_wR_factor_ref         0.0355
_refine_ls_wR_factor_gt          0.0354
_refine_ls_goodness_of_fit_ref   1.087
_refine_ls_restrained_S_all      1.139
_refine_ls_shift/su_max          0.004
_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
Ce1 Ce -0.04273(2) 0.96500(2) 0.68644(2) 0.01392(3) Uani 1 1 d . . . . .
N1 N -0.27497(14) 0.65067(12) 0.63501(10) 0.0210(2) Uani 1 1 d . . . . .
N2 N -0.30353(18) 0.59625(16) 0.73596(11) 0.0348(3) Uani 1 1 d . . . . .
N3 N -0.50638(17) 0.78893(16) 0.70249(13) 0.0354(3) Uani 1 1 d . . . . .
N4A N 0.5813(10) 0.6608(10) 0.3273(8) 0.0244(8) Uani 0.652(15) 1 d D U P A 1
N5A N 0.6012(8) 0.7813(8) 0.3520(6) 0.0358(10) Uani 0.652(15) 1 d D U P A 1
N6A N 0.6682(8) 0.7367(6) 0.1731(5) 0.0487(10) Uani 0.652(15) 1 d D U P A 1
C5A C 0.6536(8) 0.8202(7) 0.2568(5) 0.0410(10) Uani 0.652(15) 1 d D U P A 1
H5A H 0.6688 0.9032 0.2531 0.049 Uiso 0.652(15) 1 d DR U P A 1
C6A C 0.6220(9) 0.6385(6) 0.2241(4) 0.0416(10) Uani 0.652(15) 1 d D U P A 1
H6A H 0.5824 0.5650 0.1856 0.050 Uiso 0.652(15) 1 d DR U P A 1
N4B N 0.572(2) 0.6705(19) 0.3290(16) 0.0274(14) Uani 0.348(15) 1 d D U P A 1
N5B N 0.6302(16) 0.7634(16) 0.3359(12) 0.0403(16) Uani 0.348(15) 1 d D U P A 1
N6B N 0.6199(13) 0.7468(11) 0.1641(8) 0.0475(13) Uani 0.348(15) 1 d D U P A 1
C5B C 0.6570(17) 0.8054(15) 0.2315(10) 0.0450(14) Uani 0.348(15) 1 d D U P A 1
H5B H 0.7101 0.8818 0.2192 0.054 Uiso 0.348(15) 1 d DR U P A 1
C6B C 0.5725(14) 0.6557(11) 0.2217(8) 0.0357(12) Uani 0.348(15) 1 d D U P A 1
H6B H 0.4979 0.6433 0.2112 0.043 Uiso 0.348(15) 1 d DR U P A 1
N7 N 0.10450(15) 0.69596(12) 1.06168(9) 0.0206(2) Uani 1 1 d . . . B 1
N8 N 0.2170(2) 0.73492(18) 1.00113(12) 0.0380(4) Uani 1 1 d . . . B 1
N9 N 0.13275(16) 0.84215(13) 1.16070(10) 0.0234(2) Uani 1 1 d . . . C 1
O1 O 0.17663(13) 0.83565(11) 0.55165(9) 0.0284(2) Uani 1 1 d . . . D 1
O2 O 0.25999(13) 0.82692(11) 0.37491(9) 0.0265(2) Uani 1 1 d . . . E 1
O3 O 0.03860(16) 0.70354(11) 0.74844(9) 0.0323(3) Uani 1 1 d . . . F 1
O4 O -0.05067(15) 0.84975(11) 0.88247(9) 0.0303(2) Uani 1 1 d . . . G 1
O5 O -0.15108(13) 0.87129(11) 0.56511(8) 0.0247(2) Uani 1 1 d . . . H 1
O6 O -0.06317(13) 0.85226(11) 0.38833(8) 0.0247(2) Uani 1 1 d . . . I 1
O7 O 0.18794(13) 0.93110(13) 0.77793(9) 0.0302(2) Uani 1 1 d . . . J 1
H7A H 0.1775 0.8823 0.8314 0.045 Uiso 1 1 d R U . J 1
H7B H 0.2785 0.8985 0.7491 0.045 Uiso 1 1 d R U . J 1
O8 O -0.30812(15) 0.97115(16) 0.77493(11) 0.0412(3) Uani 1 1 d . . . K 1
H8A H -0.3368 0.9318 0.8290 0.062 Uiso 1 1 d R U . K 1
H8B H -0.3793 1.0028 0.7402 0.062 Uiso 1 1 d R U . K 1
O9A O 0.5833(12) 0.8596(6) 0.9619(4) 0.0803(18) Uani 0.56(2) 1 d . U P L 1
H9A H 0.5787 0.8710 1.0264 0.120 Uiso 0.56(2) 1 d R U P L 1
H9B H 0.5988 0.9258 0.9277 0.120 Uiso 0.56(2) 1 d R U P L 1
O9B O 0.6459(16) 0.8879(10) 0.9779(7) 0.084(4) Uani 0.44(2) 1 d . U P L 2
H9C H 0.7279 0.8765 0.9380 0.125 Uiso 0.44(2) 1 d R U P L 2
H9D H 0.6652 0.8605 1.0385 0.125 Uiso 0.44(2) 1 d R U P L 2
C1 C 0.26786(15) 0.78029(13) 0.46952(11) 0.0184(2) Uani 1 1 d . . . . .
C2 C 0.39374(15) 0.63842(13) 0.48558(11) 0.0176(2) Uani 1 1 d . . . . .
C3 C 0.53277(16) 0.58212(14) 0.41495(11) 0.0192(3) Uani 1 1 d D U . . .
C4 C 0.36314(16) 0.55332(14) 0.57150(11) 0.0200(3) Uani 1 1 d . . . . .
H4 H 0.2720 0.5875 0.6204 0.024 Uiso 1 1 calc R U . . .
C7 C 0.00011(17) 0.72874(14) 0.84674(11) 0.0210(3) Uani 1 1 d . . . . .
C8 C 0.00870(17) 0.60862(14) 0.92597(11) 0.0191(3) Uani 1 1 d . . . . .
C9 C 0.05128(17) 0.59775(14) 1.02759(11) 0.0190(3) Uani 1 1 d . . . . .
C10 C -0.04178(18) 0.50862(14) 0.89956(11) 0.0215(3) Uani 1 1 d . . . . .
H10 H -0.0696 0.5130 0.8320 0.026 Uiso 1 1 calc R U . . .
C11 C 0.05692(18) 0.76103(15) 1.15513(11) 0.0233(3) Uani 1 1 d . . . . .
H11 H -0.0194 0.7505 1.2090 0.028 Uiso 1 1 calc R U . B 1
C12 C 0.2286(2) 0.8227(2) 1.06504(14) 0.0364(4) Uani 1 1 d . . . . .
H12 H 0.2976 0.8679 1.0456 0.044 Uiso 1 1 calc R U . B 1
C13 C -0.13395(16) 0.57908(14) 0.56586(11) 0.0181(2) Uani 1 1 d . . . . .
C14 C -0.39785(18) 0.76440(16) 0.61687(14) 0.0277(3) Uani 1 1 d . . . . .
H14 H -0.4054 0.8181 0.5532 0.033 Uiso 1 1 calc R U . . .
C15 C -0.4431(2) 0.6840(2) 0.77243(15) 0.0400(4) Uani 1 1 d . . . . .
H15 H -0.4946 0.6747 0.8412 0.048 Uiso 1 1 calc R U . . .
C16 C -0.09613(16) 0.80388(13) 0.47992(11) 0.0175(2) Uani 1 1 d . . . . .
C17 C -0.05799(16) 0.64776(13) 0.48970(11) 0.0175(2) Uani 1 1 d . . . . .
C18 C -0.07587(17) 0.43463(14) 0.57557(11) 0.0193(3) Uani 1 1 d . . . . .
H18 H -0.1279 0.3915 0.6272 0.023 Uiso 1 1 calc R U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ce1 O5 2.4456(10) . ?
Ce1 O1 2.4533(10) . ?
Ce1 O6 2.5055(10) 2_576 ?
Ce1 O2 2.5202(10) 2_576 ?
Ce1 O8 2.5391(13) . ?
Ce1 O7 2.5491(12) . ?
Ce1 O3 2.6044(11) . ?
Ce1 O4 2.6429(11) . ?
Ce1 N9 2.6996(12) 2_577 ?
N1 C14 1.339(2) . ?
N1 N2 1.3665(18) . ?
N1 C13 1.4266(17) . ?
N2 C15 1.313(2) . ?
N3 C14 1.317(2) . ?
N3 C15 1.354(3) . ?
N4A C6A 1.304(10) . ?
N4A N5A 1.407(15) . ?
N4A C3 1.425(8) . ?
N5A C5A 1.302(7) . ?
N6A C6A 1.327(6) . ?
N6A C5A 1.385(7) . ?
C5A H5A 0.9226 . ?
C5A H5B 1.0162 . ?
C6A H6A 1.1482 . ?
C6A H6B 1.1986 . ?
N4B N5B 1.30(3) . ?
N4B C6B 1.38(2) . ?
N4B C3 1.441(16) . ?
N5B C5B 1.357(13) . ?
N6B C5B 1.263(15) . ?
N6B C6B 1.305(12) . ?
C5B H5A 1.1267 . ?
C5B H5B 1.0772 . ?
C6B H6A 1.0499 . ?
C6B H6B 0.8014 . ?
N7 C11 1.3320(18) . ?
N7 N8 1.3636(18) . ?
N7 C9 1.4287(17) . ?
N8 C12 1.322(2) . ?
N9 C11 1.3149(19) . ?
N9 C12 1.352(2) . ?
N9 Ce1 2.6995(12) 2_577 ?
O1 C1 1.2475(17) . ?
O2 C1 1.2483(17) . ?
O2 Ce1 2.5202(10) 2_576 ?
O3 C7 1.2502(18) . ?
O4 C7 1.2567(18) . ?
O5 C16 1.2555(17) . ?
O6 C16 1.2497(17) . ?
O6 Ce1 2.5054(10) 2_576 ?
O7 H7A 0.8180 . ?
O7 H7B 0.8186 . ?
O8 H8A 0.8182 . ?
O8 H8B 0.8165 . ?
O9A H9A 0.8251 . ?
O9A H9B 0.8239 . ?
O9B H9C 0.8185 . ?
O9B H9D 0.8172 . ?
C1 C2 1.5217(18) . ?
C2 C4 1.3921(18) . ?
C2 C3 1.3969(18) . ?
C3 C4 1.3892(18) 2_666 ?
C4 C3 1.3893(18) 2_666 ?
C4 H4 0.9300 . ?
C7 C8 1.5079(18) . ?
C8 C10 1.3885(19) . ?
C8 C9 1.3952(19) . ?
C9 C10 1.3871(18) 2_567 ?
C10 C9 1.3871(18) 2_567 ?
C10 H10 0.9300 . ?
C11 H11 0.9300 . ?
C12 H12 0.9300 . ?
C13 C18 1.3869(18) . ?
C13 C17 1.4002(18) . ?
C14 H14 0.9300 . ?
C15 H15 0.9300 . ?
C16 C17 1.5176(18) . ?
C17 C18 1.3925(19) 2_566 ?
C18 C17 1.3925(19) 2_566 ?
C18 H18 0.9300 . ?

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 Ce1 O1 74.34(4) . . ?
O5 Ce1 O6 117.82(4) . 2_576 ?
O1 Ce1 O6 77.97(4) . 2_576 ?
O5 Ce1 O2 75.03(4) . 2_576 ?
O1 Ce1 O2 118.89(4) . 2_576 ?
O6 Ce1 O2 71.83(4) 2_576 2_576 ?
O5 Ce1 O8 70.08(4) . . ?
O1 Ce1 O8 140.60(4) . . ?
O6 Ce1 O8 134.20(4) 2_576 . ?
O2 Ce1 O8 67.19(4) 2_576 . ?
O5 Ce1 O7 147.21(4) . . ?
O1 Ce1 O7 77.86(4) . . ?
O6 Ce1 O7 71.93(4) 2_576 . ?
O2 Ce1 O7 135.01(4) 2_576 . ?
O8 Ce1 O7 127.75(4) . . ?
O5 Ce1 O3 77.27(4) . . ?
O1 Ce1 O3 74.07(4) . . ?
O6 Ce1 O3 142.90(4) 2_576 . ?
O2 Ce1 O3 143.99(4) 2_576 . ?
O8 Ce1 O3 82.03(5) . . ?
O7 Ce1 O3 78.68(4) . . ?
O5 Ce1 O4 113.15(4) . . ?
O1 Ce1 O4 115.88(4) . . ?
O6 Ce1 O4 129.01(4) 2_576 . ?
O2 Ce1 O4 124.56(4) 2_576 . ?
O8 Ce1 O4 65.70(4) . . ?
O7 Ce1 O4 64.77(4) . . ?
O3 Ce1 O4 49.70(3) . . ?
O5 Ce1 N9 140.55(4) . 2_577 ?
O1 Ce1 N9 142.86(4) . 2_577 ?
O6 Ce1 N9 73.23(4) 2_576 2_577 ?
O2 Ce1 N9 73.40(4) 2_576 2_577 ?
O8 Ce1 N9 76.23(4) . 2_577 ?
O7 Ce1 N9 71.31(4) . 2_577 ?
O3 Ce1 N9 118.07(4) . 2_577 ?
O4 Ce1 N9 68.52(4) . 2_577 ?
C14 N1 N2 109.68(12) . . ?
C14 N1 C13 130.84(13) . . ?
N2 N1 C13 119.32(12) . . ?
C15 N2 N1 102.14(14) . . ?
C14 N3 C15 103.24(14) . . ?
C6A N4A N5A 110.5(7) . . ?
C6A N4A C3 131.9(10) . . ?
N5A N4A C3 117.5(9) . . ?
C5A N5A N4A 101.0(6) . . ?
C6A N6A C5A 102.2(5) . . ?
N5A C5A N6A 115.4(6) . . ?
N5A C5A H5A 116.0 . . ?
N6A C5A H5A 128.4 . . ?
N5A C5A H5B 142.3 . . ?
N6A C5A H5B 100.9 . . ?
H5A C5A H5B 30.9 . . ?
N4A C6A N6A 110.9(6) . . ?
N4A C6A H6A 119.9 . . ?
N6A C6A H6A 126.3 . . ?
N4A C6A H6B 94.6 . . ?
N6A C6A H6B 116.4 . . ?
H6A C6A H6B 46.5 . . ?
N5B N4B C6B 108.1(13) . . ?
N5B N4B C3 127.2(19) . . ?
C6B N4B C3 124.2(19) . . ?
N4B N5B C5B 102.7(15) . . ?
C5B N6B C6B 104.3(10) . . ?
N6B C5B N5B 115.3(13) . . ?
N6B C5B H5A 146.6 . . ?
N5B C5B H5A 93.7 . . ?
N6B C5B H5B 130.2 . . ?
N5B C5B H5B 114.5 . . ?
H5A C5B H5B 27.4 . . ?
N6B C6B N4B 109.3(12) . . ?
N6B C6B H6A 119.5 . . ?
N4B C6B H6A 126.5 . . ?
N6B C6B H6B 121.3 . . ?
N4B C6B H6B 112.9 . . ?
H6A C6B H6B 58.4 . . ?
C11 N7 N8 109.66(12) . . ?
C11 N7 C9 126.82(12) . . ?
N8 N7 C9 123.50(12) . . ?
C12 N8 N7 101.81(13) . . ?
C11 N9 C12 102.71(12) . . ?
C11 N9 Ce1 122.38(10) . 2_577 ?
C12 N9 Ce1 133.27(10) . 2_577 ?
C1 O1 Ce1 167.77(11) . . ?
C1 O2 Ce1 126.12(9) . 2_576 ?
C7 O3 Ce1 94.48(8) . . ?
C7 O4 Ce1 92.50(8) . . ?
C16 O5 Ce1 134.02(9) . . ?
C16 O6 Ce1 136.10(9) . 2_576 ?
Ce1 O7 H7A 103.8 . . ?
Ce1 O7 H7B 124.7 . . ?
H7A O7 H7B 107.8 . . ?
Ce1 O8 H8A 132.3 . . ?
Ce1 O8 H8B 118.6 . . ?
H8A O8 H8B 107.6 . . ?
H9A O9A H9B 107.7 . . ?
H9C O9B H9D 107.8 . . ?
O1 C1 O2 125.94(13) . . ?
O1 C1 C2 116.85(12) . . ?
O2 C1 C2 117.08(12) . . ?
C4 C2 C3 117.25(12) . . ?
C4 C2 C1 117.84(12) . . ?
C3 C2 C1 124.66(12) . . ?
C4 C3 C2 121.98(12) 2_666 . ?
C4 C3 N4A 115.3(3) 2_666 . ?
C2 C3 N4A 122.7(3) . . ?
C4 C3 N4B 119.5(6) 2_666 . ?
C2 C3 N4B 118.4(6) . . ?
N4A C3 N4B 4.3(9) . . ?
C3 C4 C2 120.76(12) 2_666 . ?
C3 C4 H4 119.6 2_666 . ?
C2 C4 H4 119.6 . . ?
O3 C7 O4 123.23(13) . . ?
O3 C7 C8 118.31(12) . . ?
O4 C7 C8 118.40(12) . . ?
C10 C8 C9 117.89(12) . . ?
C10 C8 C7 117.57(12) . . ?
C9 C8 C7 124.30(12) . . ?
C10 C9 C8 121.07(12) 2_567 . ?
C10 C9 N7 117.18(12) 2_567 . ?
C8 C9 N7 121.75(12) . . ?
C9 C10 C8 121.03(12) 2_567 . ?
C9 C10 H10 119.5 2_567 . ?
C8 C10 H10 119.5 . . ?
N9 C11 N7 110.69(13) . . ?
N9 C11 H11 124.7 . . ?
N7 C11 H11 124.7 . . ?
N8 C12 N9 115.12(14) . . ?
N8 C12 H12 122.4 . . ?
N9 C12 H12 122.4 . . ?
C18 C13 C17 120.64(12) . . ?
C18 C13 N1 116.26(12) . . ?
C17 C13 N1 123.09(12) . . ?
N3 C14 N1 109.94(15) . . ?
N3 C14 H14 125.0 . . ?
N1 C14 H14 125.0 . . ?
N2 C15 N3 114.98(15) . . ?
N2 C15 H15 122.5 . . ?
N3 C15 H15 122.5 . . ?
O6 C16 O5 126.06(12) . . ?
O6 C16 C17 116.71(12) . . ?
O5 C16 C17 117.15(12) . . ?
C18 C17 C13 117.39(12) 2_566 . ?
C18 C17 C16 116.02(12) 2_566 . ?
C13 C17 C16 126.16(12) . . ?
C13 C18 C17 121.98(12) . 2_566 ?
C13 C18 H18 119.0 . . ?
C17 C18 H18 119.0 2_566 . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
C14 H14 N5A 0.93 2.59 3.331(7) 137.0 1_455
C11 H11 O6 0.93 2.49 3.0545(17) 119.5 1_556
C10 H10 N2 0.93 2.54 3.321(2) 142.0 .
C4 H4 O3 0.93 2.44 3.3690(18) 173.0 .
O9A H9B O8 0.82 2.06 2.732(6) 138.8 1_655
O9A H9A N6B 0.83 2.06 2.727(11) 137.0 1_556
O9A H9A N6A 0.83 2.29 2.953(9) 137.3 1_556
O8 H8A O9A 0.82 1.92 2.732(6) 173.7 1_455
O7 H7B N3 0.82 1.93 2.7310(18) 167.8 1_655
O7 H7A O4 0.82 2.29 2.7818(17) 119.5 .
O7 H7A N8 0.82 2.51 3.302(2) 163.9 .
C5B H5B O7 1.08 2.49 3.555(16) 170.5 2_676
C5A H5A O7 0.92 2.54 3.414(7) 158.8 2_676
C5B H5B O7 1.08 2.49 3.555(16) 170.5 2_676
C5A H5A O7 0.92 2.54 3.414(7) 158.8 2_676
C14 H14 N5A 0.93 2.59 3.331(7) 137.0 1_455
C11 H11 O6 0.93 2.49 3.0545(17) 119.5 1_556
C10 H10 N2 0.93 2.54 3.321(2) 142.0 .
C4 H4 O3 0.93 2.44 3.3690(18) 173.0 .
O9A H9B O8 0.82 2.06 2.732(6) 138.8 1_655
O9A H9A N6B 0.83 2.06 2.727(11) 137.0 1_556
O9A H9A N6A 0.83 2.29 2.953(9) 137.3 1_556
O8 H8A O9A 0.82 1.92 2.732(6) 173.7 1_455
O7 H7B N3 0.82 1.93 2.7310(18) 167.8 1_655
O7 H7A O4 0.82 2.29 2.7818(17) 119.5 .
O7 H7A N8 0.82 2.51 3.302(2) 163.9 .
C5B H5B O7 1.08 2.49 3.555(16) 170.5 2_676
C5A H5A O7 0.92 2.54 3.414(7) 158.8 2_676
C5B H5B O7 1.08 2.49 3.555(16) 170.5 2_676
C5A H5A O7 0.92 2.54 3.414(7) 158.8 2_676
C5A H5A O7 0.92 2.54 3.414(7) 158.8 2_676
C5B H5B O7 1.08 2.49 3.555(16) 170.5 2_676
C5A H5A O7 0.92 2.54 3.414(7) 158.8 2_676
C5B H5B O7 1.08 2.49 3.555(16) 170.5 2_676
O7 H7A N8 0.82 2.51 3.302(2) 163.9 .
O7 H7A O4 0.82 2.29 2.7818(17) 119.5 .
O7 H7B N3 0.82 1.93 2.7310(18) 167.8 1_655
O8 H8A O9A 0.82 1.92 2.732(6) 173.7 1_455
O9A H9A N6A 0.83 2.29 2.953(9) 137.3 1_556
O9A H9A N6B 0.83 2.06 2.727(11) 137.0 1_556
O9A H9B O8 0.82 2.06 2.732(6) 138.8 1_655
C4 H4 O3 0.93 2.44 3.3690(18) 173.0 .
C10 H10 N2 0.93 2.54 3.321(2) 142.0 .
C11 H11 O6 0.93 2.49 3.0545(17) 119.5 1_556
C14 H14 N5A 0.93 2.59 3.331(7) 137.0 1_455

_refine_diff_density_max         0.406
_refine_diff_density_min         -0.345
_refine_diff_density_rms         0.053

####################################################################### 
# 
# 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_NdL66
_database_code_depnum_ccdc_archive 'CCDC 2096054'
loop_
_audit_author_name
_audit_author_address
'Ai Wang' 'Shanxi University'
_audit_update_record             
;
2022-07-19 deposited with the CCDC.	2022-07-21 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         'C18 H13 N9 Nd O8, H2 O'
_chemical_formula_sum            'C18 H15 N9 Nd O9'
_chemical_formula_weight         645.63

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'
Nd Nd -0.1943 3.0179 '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                   9.4901(4)
_cell_length_b                   10.3535(5)
_cell_length_c                   12.5438(5)
_cell_angle_alpha                84.3246(13)
_cell_angle_beta                 79.5509(13)
_cell_angle_gamma                67.1626(13)
_cell_volume                     1116.50(9)
_cell_formula_units_Z            2
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    9935
_cell_measurement_theta_min      3.08
_cell_measurement_theta_max      28.28

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.920
_exptl_crystal_F_000             636
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.260
_exptl_crystal_size_mid          0.250
_exptl_crystal_size_min          0.230
_exptl_absorpt_coefficient_mu    2.398
_shelx_estimated_absorpt_T_min   0.574
_shelx_estimated_absorpt_T_max   0.609
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6375
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_process_details   SADABS
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'Incoatec microsource'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            39858
_diffrn_reflns_av_unetI/netI     0.0172
_diffrn_reflns_av_R_equivalents  0.0267
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         2.741
_diffrn_reflns_theta_max         28.295
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measured_fraction_theta_full 0.980
_diffrn_reflns_Laue_measured_fraction_max 0.983
_diffrn_reflns_Laue_measured_fraction_full 0.980
_diffrn_reflns_point_group_measured_fraction_max 0.983
_diffrn_reflns_point_group_measured_fraction_full 0.980
_reflns_number_total             5459
_reflns_number_gt                5394
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT, SADABS and XPREP'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_computing_structure_refinement  'SHELXL-2014 (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)+(0.0109P)²+0.8593P] 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         5459
_refine_ls_number_parameters     390
_refine_ls_number_restraints     189
_refine_ls_R_factor_all          0.0154
_refine_ls_R_factor_gt           0.0152
_refine_ls_wR_factor_ref         0.0384
_refine_ls_wR_factor_gt          0.0383
_refine_ls_goodness_of_fit_ref   1.118
_refine_ls_restrained_S_all      1.169
_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
Nd1 Nd -0.04135(2) 0.96511(2) 0.68656(2) 0.01446(3) Uani 1 1 d . . . . .
N1 N -0.27552(16) 0.65181(15) 0.63486(12) 0.0216(3) Uani 1 1 d . . . . .
N2 N -0.3053(2) 0.59635(19) 0.73564(14) 0.0371(4) Uani 1 1 d . . . . .
N3 N -0.50709(19) 0.79147(19) 0.70163(15) 0.0366(4) Uani 1 1 d . . . . .
N4A N 0.5785(11) 0.6624(9) 0.3259(8) 0.0262(8) Uani 0.672(15) 1 d D U P A 1
N5A N 0.5970(8) 0.7835(7) 0.3508(5) 0.0373(10) Uani 0.672(15) 1 d D U P A 1
N6A N 0.6657(8) 0.7383(6) 0.1712(5) 0.0505(11) Uani 0.672(15) 1 d D U P A 1
C5A C 0.6494(8) 0.8223(7) 0.2545(6) 0.0436(10) Uani 0.672(15) 1 d D U P A 1
H5A H 0.6647 0.9052 0.2508 0.052 Uiso 0.672(15) 1 d DR U P A 1
C6A C 0.6206(9) 0.6390(6) 0.2225(5) 0.0441(10) Uani 0.672(15) 1 d D U P A 1
H6A H 0.5810 0.5655 0.1840 0.053 Uiso 0.672(15) 1 d DR U P A 1
N4B N 0.570(2) 0.672(2) 0.3282(17) 0.0289(15) Uani 0.328(15) 1 d D U P A 1
N5B N 0.6288(16) 0.7656(17) 0.3315(12) 0.0427(16) Uani 0.328(15) 1 d D U P A 1
N6B N 0.6158(14) 0.7462(12) 0.1605(9) 0.0491(14) Uani 0.328(15) 1 d D U P A 1
C5B C 0.6550(18) 0.8065(16) 0.2268(12) 0.0466(15) Uani 0.328(15) 1 d D U P A 1
H5B H 0.7080 0.8828 0.2145 0.056 Uiso 0.328(15) 1 d DR U P A 1
C6B C 0.5701(15) 0.6554(12) 0.2204(9) 0.0374(13) Uani 0.328(15) 1 d D U P A 1
H6B H 0.4955 0.6430 0.2099 0.045 Uiso 0.328(15) 1 d DR U P A 1
N7 N 0.10312(17) 0.69680(15) 1.06319(11) 0.0219(3) Uani 1 1 d . . . B 1
N8 N 0.2164(2) 0.7355(2) 1.00323(15) 0.0418(5) Uani 1 1 d . . . B 1
N9 N 0.12980(17) 0.84381(15) 1.16301(12) 0.0235(3) Uani 1 1 d . . . C 1
O1 O 0.17584(15) 0.83688(13) 0.55366(11) 0.0283(3) Uani 1 1 d . . . D 1
O2 O 0.25623(14) 0.82911(12) 0.37562(10) 0.0258(2) Uani 1 1 d . . . E 1
O3 O 0.03822(18) 0.70562(13) 0.74770(10) 0.0328(3) Uani 1 1 d . . . F 1
O4 O -0.05004(18) 0.85137(13) 0.88238(11) 0.0337(3) Uani 1 1 d . . . G 1
O5 O -0.14864(15) 0.87200(12) 0.56689(10) 0.0247(2) Uani 1 1 d . . . H 1
O6 O -0.06273(15) 0.85438(12) 0.38898(10) 0.0253(2) Uani 1 1 d . . . I 1
O7 O 0.18653(14) 0.93091(15) 0.77670(11) 0.0301(3) Uani 1 1 d . . . J 1
H7A H 0.1761 0.8821 0.8301 0.045 Uiso 1 1 d R U . J 1
H7B H 0.2771 0.8983 0.7479 0.045 Uiso 1 1 d R U . J 1
O8 O -0.30382(18) 0.97215(19) 0.77433(13) 0.0431(4) Uani 1 1 d . . . K 1
H8A H -0.3325 0.9328 0.8284 0.065 Uiso 1 1 d R U . K 1
H8B H -0.3750 1.0038 0.7395 0.065 Uiso 1 1 d R U . K 1
O9A O 0.5849(11) 0.8604(7) 0.9587(4) 0.092(2) Uani 0.65(2) 1 d . U P L 1
H9A H 0.5802 0.8719 1.0233 0.138 Uiso 0.65(2) 1 d R U P L 1
H9B H 0.6003 0.9267 0.9245 0.138 Uiso 0.65(2) 1 d R U P L 1
O9B O 0.648(2) 0.8925(12) 0.9781(9) 0.082(5) Uani 0.35(2) 1 d . U P L 2
H9C H 0.7302 0.8811 0.9382 0.123 Uiso 0.35(2) 1 d R U P L 2
H9D H 0.6675 0.8651 1.0387 0.123 Uiso 0.35(2) 1 d R U P L 2
C1 C 0.26607(17) 0.78193(15) 0.47030(13) 0.0183(3) Uani 1 1 d . . . . .
C2 C 0.39297(17) 0.63922(16) 0.48607(13) 0.0178(3) Uani 1 1 d . . . . .
C3 C 0.53142(18) 0.58314(16) 0.41456(13) 0.0197(3) Uani 1 1 d D U . . .
C4 C 0.36388(18) 0.55331(16) 0.57227(13) 0.0207(3) Uani 1 1 d . . . . .
H4 H 0.2732 0.5875 0.6218 0.025 Uiso 1 1 calc R U . . .
C7 C -0.0002(2) 0.73029(17) 0.84626(14) 0.0219(3) Uani 1 1 d . . . . .
C8 C 0.0086(2) 0.60926(16) 0.92591(13) 0.0203(3) Uani 1 1 d . . . . .
C9 C 0.05048(19) 0.59814(16) 1.02831(13) 0.0197(3) Uani 1 1 d . . . . .
C10 C -0.0413(2) 0.50895(17) 0.89875(13) 0.0222(3) Uani 1 1 d . . . . .
H10 H -0.0688 0.5137 0.8306 0.027 Uiso 1 1 calc R U . . .
C11 C 0.0543(2) 0.76255(18) 1.15650(14) 0.0237(3) Uani 1 1 d . . . . .
H11 H -0.0229 0.7525 1.2100 0.028 Uiso 1 1 calc R U . B 1
C12 C 0.2269(3) 0.8238(2) 1.06749(18) 0.0395(5) Uani 1 1 d . . . . .
H12 H 0.2961 0.8690 1.0485 0.047 Uiso 1 1 calc R U . B 1
C13 C -0.13422(18) 0.57978(16) 0.56582(13) 0.0183(3) Uani 1 1 d . . . . .
C14 C -0.3978(2) 0.76692(19) 0.61608(16) 0.0287(4) Uani 1 1 d . . . . .
H14 H -0.4046 0.8214 0.5522 0.034 Uiso 1 1 calc R U . . .
C15 C -0.4452(3) 0.6850(3) 0.77186(18) 0.0423(5) Uani 1 1 d . . . . .
H15 H -0.4975 0.6752 0.8405 0.051 Uiso 1 1 calc R U . . .
C16 C -0.09493(17) 0.80533(16) 0.48087(13) 0.0176(3) Uani 1 1 d . . . . .
C17 C -0.05769(18) 0.64849(15) 0.49015(13) 0.0175(3) Uani 1 1 d . . . . .
C18 C -0.07651(19) 0.43426(16) 0.57522(13) 0.0196(3) Uani 1 1 d . . . . .
H18 H -0.1290 0.3909 0.6266 0.024 Uiso 1 1 calc R U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Nd1 O5 2.4129(12) . ?
Nd1 O1 2.4202(12) . ?
Nd1 O6 2.4717(12) 2_576 ?
Nd1 O2 2.4864(12) 2_576 ?
Nd1 O7 2.5087(13) . ?
Nd1 O8 2.5104(15) . ?
Nd1 O3 2.5698(13) . ?
Nd1 O4 2.6185(13) . ?
Nd1 N9 2.6559(14) 2_577 ?
N1 C14 1.339(2) . ?
N1 N2 1.364(2) . ?
N1 C13 1.426(2) . ?
N2 C15 1.315(3) . ?
N3 C14 1.318(3) . ?
N3 C15 1.353(3) . ?
N4A C6A 1.304(10) . ?
N4A N5A 1.403(14) . ?
N5A C5A 1.307(6) . ?
N6A C6A 1.328(6) . ?
N6A C5A 1.374(7) . ?
C5A H5A 0.9201 . ?
C5A H5B 1.0298 . ?
C6A H6A 1.1459 . ?
C6A H6B 1.2104 . ?
N4B N5B 1.30(3) . ?
N4B C6B 1.38(2) . ?
N4B C3 1.441(17) . ?
N5B C5B 1.349(14) . ?
N6B C5B 1.270(16) . ?
N6B C6B 1.302(13) . ?
C5B H5A 1.1352 . ?
C5B H5B 1.0761 . ?
C6B H6A 1.0373 . ?
C6B H6B 0.8015 . ?
N7 C11 1.328(2) . ?
N7 N8 1.365(2) . ?
N7 C9 1.4312(19) . ?
N8 C12 1.320(3) . ?
N9 C11 1.315(2) . ?
N9 C12 1.352(2) . ?
N9 Nd1 2.6559(14) 2_577 ?
O1 C1 1.251(2) . ?
O2 C1 1.244(2) . ?
O2 Nd1 2.4864(12) 2_576 ?
O3 C7 1.246(2) . ?
O4 C7 1.255(2) . ?
O5 C16 1.255(2) . ?
O6 C16 1.248(2) . ?
O6 Nd1 2.4717(12) 2_576 ?
O7 H7A 0.8136 . ?
O7 H7B 0.8182 . ?
O8 H8A 0.8147 . ?
O8 H8B 0.8131 . ?
O9A H9A 0.8207 . ?
O9A H9B 0.8207 . ?
O9B H9C 0.8183 . ?
O9B H9D 0.8118 . ?
C1 C2 1.523(2) . ?
C2 C4 1.389(2) . ?
C2 C3 1.397(2) . ?
C3 C4 1.391(2) 2_666 ?
C4 C3 1.391(2) 2_666 ?
C4 H4 0.9300 . ?
C7 C8 1.509(2) . ?
C8 C10 1.388(2) . ?
C8 C9 1.394(2) . ?
C9 C10 1.386(2) 2_567 ?
C10 C9 1.386(2) 2_567 ?
C10 H10 0.9300 . ?
C11 H11 0.9300 . ?
C12 H12 0.9300 . ?
C13 C18 1.390(2) . ?
C13 C17 1.397(2) . ?
C14 H14 0.9300 . ?
C15 H15 0.9300 . ?
C16 C17 1.519(2) . ?
C17 C18 1.393(2) 2_566 ?
C18 C17 1.393(2) 2_566 ?
C18 H18 0.9300 . ?

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 Nd1 O1 74.71(5) . . ?
O5 Nd1 O6 117.72(4) . 2_576 ?
O1 Nd1 O6 77.61(4) . 2_576 ?
O5 Nd1 O2 74.81(4) . 2_576 ?
O1 Nd1 O2 118.81(4) . 2_576 ?
O6 Nd1 O2 71.88(4) 2_576 2_576 ?
O5 Nd1 O7 147.06(4) . . ?
O1 Nd1 O7 77.41(5) . . ?
O6 Nd1 O7 72.07(4) 2_576 . ?
O2 Nd1 O7 135.33(4) 2_576 . ?
O5 Nd1 O8 69.96(5) . . ?
O1 Nd1 O8 140.92(5) . . ?
O6 Nd1 O8 134.18(5) 2_576 . ?
O2 Nd1 O8 67.08(5) 2_576 . ?
O7 Nd1 O8 127.96(5) . . ?
O5 Nd1 O3 76.69(4) . . ?
O1 Nd1 O3 74.07(4) . . ?
O6 Nd1 O3 143.15(5) 2_576 . ?
O2 Nd1 O3 143.45(5) 2_576 . ?
O7 Nd1 O3 79.08(5) . . ?
O8 Nd1 O3 81.95(5) . . ?
O5 Nd1 O4 112.94(4) . . ?
O1 Nd1 O4 116.08(4) . . ?
O6 Nd1 O4 129.34(4) 2_576 . ?
O2 Nd1 O4 124.43(4) 2_576 . ?
O7 Nd1 O4 65.09(5) . . ?
O8 Nd1 O4 65.53(5) . . ?
O3 Nd1 O4 50.18(4) . . ?
O5 Nd1 N9 140.52(4) . 2_577 ?
O1 Nd1 N9 142.54(5) . 2_577 ?
O6 Nd1 N9 73.40(4) 2_576 2_577 ?
O2 Nd1 N9 73.63(4) 2_576 2_577 ?
O7 Nd1 N9 71.48(5) . 2_577 ?
O8 Nd1 N9 76.25(5) . 2_577 ?
O3 Nd1 N9 118.50(4) . 2_577 ?
O4 Nd1 N9 68.46(4) . 2_577 ?
C14 N1 N2 109.79(15) . . ?
C14 N1 C13 130.66(15) . . ?
N2 N1 C13 119.38(14) . . ?
C15 N2 N1 102.19(17) . . ?
C14 N3 C15 103.33(16) . . ?
C6A N4A N5A 110.7(7) . . ?
C5A N5A N4A 100.5(6) . . ?
C6A N6A C5A 102.3(5) . . ?
N5A C5A N6A 115.7(6) . . ?
N5A C5A H5A 115.7 . . ?
N6A C5A H5A 128.5 . . ?
N5A C5A H5B 143.4 . . ?
N6A C5A H5B 99.2 . . ?
H5A C5A H5B 32.5 . . ?
N4A C6A N6A 110.7(6) . . ?
N4A C6A H6A 119.7 . . ?
N6A C6A H6A 126.4 . . ?
N4A C6A H6B 93.8 . . ?
N6A C6A H6B 116.7 . . ?
H6A C6A H6B 46.2 . . ?
N5B N4B C6B 107.1(14) . . ?
N5B N4B C3 129(2) . . ?
C6B N4B C3 123(2) . . ?
N4B N5B C5B 104.1(15) . . ?
C5B N6B C6B 104.4(11) . . ?
N6B C5B N5B 114.5(14) . . ?
N6B C5B H5A 148.5 . . ?
N5B C5B H5A 91.7 . . ?
N6B C5B H5B 131.7 . . ?
N5B C5B H5B 113.8 . . ?
H5A C5B H5B 29.0 . . ?
N6B C6B N4B 109.7(13) . . ?
N6B C6B H6A 117.7 . . ?
N4B C6B H6A 127.9 . . ?
N6B C6B H6B 120.2 . . ?
N4B C6B H6B 113.3 . . ?
H6A C6B H6B 58.8 . . ?
C11 N7 N8 109.54(14) . . ?
C11 N7 C9 126.90(14) . . ?
N8 N7 C9 123.55(14) . . ?
C12 N8 N7 101.93(15) . . ?
C11 N9 C12 102.63(14) . . ?
C11 N9 Nd1 122.92(11) . 2_577 ?
C12 N9 Nd1 132.88(12) . 2_577 ?
C1 O1 Nd1 166.86(12) . . ?
C1 O2 Nd1 126.92(10) . 2_576 ?
C7 O3 Nd1 94.50(10) . . ?
C7 O4 Nd1 91.99(10) . . ?
C16 O5 Nd1 134.27(11) . . ?
C16 O6 Nd1 136.57(11) . 2_576 ?
Nd1 O7 H7A 103.5 . . ?
Nd1 O7 H7B 125.0 . . ?
H7A O7 H7B 108.0 . . ?
Nd1 O8 H8A 132.4 . . ?
Nd1 O8 H8B 118.9 . . ?
H8A O8 H8B 107.1 . . ?
H9A O9A H9B 107.5 . . ?
H9C O9B H9D 107.7 . . ?
O2 C1 O1 126.08(15) . . ?
O2 C1 C2 117.22(14) . . ?
O1 C1 C2 116.56(14) . . ?
C4 C2 C3 117.25(14) . . ?
C4 C2 C1 117.88(13) . . ?
C3 C2 C1 124.62(14) . . ?
C4 C3 C2 121.91(14) 2_666 . ?
C4 C3 N4B 119.4(7) 2_666 . ?
C2 C3 N4B 118.6(7) . . ?
C2 C4 C3 120.84(14) . 2_666 ?
C2 C4 H4 119.6 . . ?
C3 C4 H4 119.6 2_666 . ?
O3 C7 O4 123.23(15) . . ?
O3 C7 C8 118.42(15) . . ?
O4 C7 C8 118.32(15) . . ?
C10 C8 C9 118.00(14) . . ?
C10 C8 C7 117.49(14) . . ?
C9 C8 C7 124.28(14) . . ?
C10 C9 C8 121.02(14) 2_567 . ?
C10 C9 N7 117.16(14) 2_567 . ?
C8 C9 N7 121.81(14) . . ?
C9 C10 C8 120.98(15) 2_567 . ?
C9 C10 H10 119.5 2_567 . ?
C8 C10 H10 119.5 . . ?
N9 C11 N7 110.87(15) . . ?
N9 C11 H11 124.6 . . ?
N7 C11 H11 124.6 . . ?
N8 C12 N9 115.04(17) . . ?
N8 C12 H12 122.5 . . ?
N9 C12 H12 122.5 . . ?
C18 C13 C17 120.60(14) . . ?
C18 C13 N1 116.23(14) . . ?
C17 C13 N1 123.15(14) . . ?
N3 C14 N1 109.82(17) . . ?
N3 C14 H14 125.1 . . ?
N1 C14 H14 125.1 . . ?
N2 C15 N3 114.85(19) . . ?
N2 C15 H15 122.6 . . ?
N3 C15 H15 122.6 . . ?
O6 C16 O5 126.24(14) . . ?
O6 C16 C17 116.65(14) . . ?
O5 C16 C17 117.03(14) . . ?
C18 C17 C13 117.52(14) 2_566 . ?
C18 C17 C16 115.82(13) 2_566 . ?
C13 C17 C16 126.22(14) . . ?
C13 C18 C17 121.88(14) . 2_566 ?
C13 C18 H18 119.1 . . ?
C17 C18 H18 119.1 2_566 . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
C5A H5A O7 0.92 2.56 3.431(7) 158.0 2_676
C5B H5B O7 1.08 2.51 3.575(18) 169.2 2_676
C5A H5A O7 0.92 2.56 3.431(7) 158.0 2_676
C5B H5B O7 1.08 2.51 3.575(18) 169.2 2_676
O7 H7A N8 0.81 2.52 3.310(3) 163.3 .
O7 H7A O4 0.81 2.26 2.7596(19) 119.9 .
O7 H7B N3 0.82 1.92 2.728(2) 168.4 1_655
O8 H8A O9A 0.81 1.90 2.709(6) 173.8 1_455
O9A H9A N6A 0.82 2.28 2.935(9) 137.6 1_556
O9A H9A N6B 0.82 2.05 2.702(13) 136.2 1_556
O9A H9B O8 0.82 2.03 2.709(6) 139.3 1_655
C4 H4 O3 0.93 2.44 3.364(2) 172.8 .
C10 H10 N2 0.93 2.54 3.319(3) 141.3 .
C11 H11 O6 0.93 2.48 3.032(2) 118.3 1_556
C14 H14 N5A 0.93 2.59 3.324(7) 135.9 1_455

_refine_diff_density_max         0.718
_refine_diff_density_min         -0.511
_refine_diff_density_rms         0.060

####################################################################### 
# 
# 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_SmL66
_database_code_depnum_ccdc_archive 'CCDC 2096055'
loop_
_audit_author_name
_audit_author_address
'Ai Wang' 'Shanxi University'
_audit_update_record             
;
2022-07-19 deposited with the CCDC.	2022-07-21 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         'C18 H13 Sm N9 O8, H2 O'
_chemical_formula_sum            'C18 H15 N9 O9 Sm'
_chemical_formula_weight         651.74

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'
Sm Sm -0.1638 3.4418 '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                   9.4774(4)
_cell_length_b                   10.3232(4)
_cell_length_c                   12.4655(5)
_cell_angle_alpha                84.0976(13)
_cell_angle_beta                 80.0670(13)
_cell_angle_gamma                66.9366(12)
_cell_volume                     1104.45(8)
_cell_formula_units_Z            2
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    9710
_cell_measurement_theta_min      3.32
_cell_measurement_theta_max      28.29

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.960
_exptl_crystal_F_000             640
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.230
_exptl_crystal_size_mid          0.220
_exptl_crystal_size_min          0.200
_exptl_absorpt_coefficient_mu    2.732
_shelx_estimated_absorpt_T_min   0.572
_shelx_estimated_absorpt_T_max   0.611
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6217
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_process_details   SADABS
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'Incoatec microsource'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            39636
_diffrn_reflns_av_unetI/netI     0.0176
_diffrn_reflns_av_R_equivalents  0.0257
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         2.764
_diffrn_reflns_theta_max         28.296
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measured_fraction_theta_full 0.989
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_Laue_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_point_group_measured_fraction_full 0.989
_reflns_number_total             5452
_reflns_number_gt                5313
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT, SADABS and XPREP'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_computing_structure_refinement  'SHELXL-2014 (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)+(0.0182P)²+1.0844P] 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         5452
_refine_ls_number_parameters     400
_refine_ls_number_restraints     195
_refine_ls_R_factor_all          0.0176
_refine_ls_R_factor_gt           0.0171
_refine_ls_wR_factor_ref         0.0451
_refine_ls_wR_factor_gt          0.0448
_refine_ls_goodness_of_fit_ref   1.103
_refine_ls_restrained_S_all      1.151
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Sm1 Sm -0.03752(2) 0.96448(2) 0.68545(2) 0.01693(4) Uani 1 1 d . . . . .
N1 N -0.2752(2) 0.65098(17) 0.63456(14) 0.0231(3) Uani 1 1 d . . . . .
N2 N -0.3051(3) 0.5934(2) 0.73507(16) 0.0392(5) Uani 1 1 d . . . . .
N3 N -0.5064(2) 0.7915(2) 0.70095(18) 0.0377(4) Uani 1 1 d . . . . .
N4A N 0.5761(10) 0.6651(9) 0.3256(8) 0.0275(8) Uani 0.691(16) 1 d D U P A 1
N5A N 0.5904(8) 0.7888(7) 0.3493(5) 0.0403(10) Uani 0.691(16) 1 d D U P A 1
N6A N 0.6623(9) 0.7412(6) 0.1699(5) 0.0529(11) Uani 0.691(16) 1 d D U P A 1
C5A C 0.6417(8) 0.8274(7) 0.2526(6) 0.0476(11) Uani 0.691(16) 1 d D U P A 1
H5A H 0.6570 0.9104 0.2489 0.057 Uiso 0.691(16) 1 d DR U P A 1
C6A C 0.6211(10) 0.6405(6) 0.2220(5) 0.0461(11) Uani 0.691(16) 1 d D U P A 1
H6A H 0.5815 0.5671 0.1836 0.055 Uiso 0.691(16) 1 d DR U P A 1
N4B N 0.567(2) 0.675(2) 0.3271(18) 0.0313(16) Uani 0.309(16) 1 d D U P A 1
N5B N 0.6241(18) 0.7689(18) 0.3300(13) 0.0468(16) Uani 0.309(16) 1 d D U P A 1
N6B N 0.6103(17) 0.7490(13) 0.1576(11) 0.0498(14) Uani 0.309(16) 1 d D U P A 1
C5B C 0.649(2) 0.8112(19) 0.2244(13) 0.0496(15) Uani 0.309(16) 1 d D U P A 1
H5B H 0.7024 0.8875 0.2121 0.060 Uiso 0.309(16) 1 d DR U P A 1
C6B C 0.5694(18) 0.6551(14) 0.2189(11) 0.0389(14) Uani 0.309(16) 1 d D U P A 1
H6B H 0.4948 0.6427 0.2084 0.047 Uiso 0.309(16) 1 d DR U P A 1
N7 N 0.0984(2) 0.70010(18) 1.06428(14) 0.0263(4) Uani 1 1 d . . . B 1
N8 N 0.2112(3) 0.7396(3) 1.00486(19) 0.0534(7) Uani 1 1 d . . . B 1
N9 N 0.1231(2) 0.84831(18) 1.16455(14) 0.0252(3) Uani 1 1 d . . . C 1
O1 O 0.17535(18) 0.83812(15) 0.55346(13) 0.0307(3) Uani 1 1 d . . . D 1
O2 O 0.25253(17) 0.83136(15) 0.37415(12) 0.0275(3) Uani 1 1 d . . . E 1
O3 O 0.0433(2) 0.70565(16) 0.74656(12) 0.0366(4) Uani 1 1 d . . . F 1
O4 O -0.0462(6) 0.8509(2) 0.8820(3) 0.0313(11) Uani 0.803(14) 1 d . . P D 1
O4A O -0.1170(18) 0.8602(8) 0.8515(10) 0.026(4) Uani 0.197(14) 1 d . . P D 2
O5 O -0.14707(18) 0.87196(15) 0.56929(12) 0.0264(3) Uani 1 1 d . . . . .
O6 O -0.06465(19) 0.85736(15) 0.39028(12) 0.0275(3) Uani 1 1 d . . . . .
O7 O 0.18765(18) 0.92815(18) 0.77615(13) 0.0315(3) Uani 1 1 d . . . . .
H7A H 0.1772 0.8794 0.8296 0.047 Uiso 1 1 d R U . . .
H7B H 0.2782 0.8955 0.7474 0.047 Uiso 1 1 d R U . . .
O8 O -0.2983(3) 0.9708(3) 0.77357(18) 0.0575(5) Uani 1 1 d . . . . .
H8A H -0.3269 0.9315 0.8276 0.086 Uiso 1 1 d R U . . .
H8B H -0.3695 1.0025 0.7388 0.086 Uiso 1 1 d R U . . .
O9A O 0.5825(8) 0.8660(6) 0.9552(4) 0.093(2) Uani 0.784(17) 1 d . U P . .
H9A H 0.5779 0.8775 1.0197 0.139 Uiso 0.784(17) 1 d R U P G .
H9B H 0.5979 0.9323 0.9210 0.139 Uiso 0.784(17) 1 d R U P . .
O9B O 0.654(3) 0.8970(19) 0.9802(14) 0.082(7) Uani 0.216(17) 1 d . U P G 2
H9C H 0.7358 0.8857 0.9403 0.123 Uiso 0.216(17) 1 d R U P G 2
H9D H 0.6732 0.8697 1.0408 0.123 Uiso 0.216(17) 1 d R U P G 2
C1 C 0.2645(2) 0.78348(19) 0.46973(16) 0.0207(3) Uani 1 1 d . . . . .
C2 C 0.3926(2) 0.64031(19) 0.48577(15) 0.0197(3) Uani 1 1 d . . . . .
C3 C 0.5306(2) 0.5843(2) 0.41441(15) 0.0214(3) Uani 1 1 d D U . . .
C4 C 0.3641(2) 0.5532(2) 0.57242(16) 0.0222(4) Uani 1 1 d . . . . .
H4 H 0.2738 0.5872 0.6220 0.027 Uiso 1 1 calc R U . . .
C7 C -0.0009(3) 0.7306(2) 0.84387(16) 0.0252(4) Uani 1 1 d . . . . .
C8 C 0.0080(3) 0.6096(2) 0.92507(15) 0.0234(4) Uani 1 1 d . . . . .
C9 C 0.0479(3) 0.5998(2) 1.02888(15) 0.0238(4) Uani 1 1 d . . . . .
C10 C -0.0393(3) 0.5075(2) 0.89753(16) 0.0258(4) Uani 1 1 d . . . . .
H10 H -0.0656 0.5113 0.8284 0.031 Uiso 1 1 calc R U . . .
C11 C 0.0486(3) 0.7661(2) 1.15773(16) 0.0247(4) Uani 1 1 d . . . . .
H11 H -0.0283 0.7555 1.2110 0.030 Uiso 1 1 calc R U . B 1
C12 C 0.2207(4) 0.8288(3) 1.0694(2) 0.0464(7) Uani 1 1 d . . . . .
H12 H 0.2892 0.8746 1.0508 0.056 Uiso 1 1 calc R U . B 1
C13 C -0.1341(2) 0.57924(19) 0.56591(15) 0.0196(3) Uani 1 1 d . . . . .
C14 C -0.3974(2) 0.7681(2) 0.61617(19) 0.0296(4) Uani 1 1 d . . . . .
H14 H -0.4040 0.8247 0.5527 0.036 Uiso 1 1 calc R U . . .
C15 C -0.4447(3) 0.6823(3) 0.7712(2) 0.0449(6) Uani 1 1 d . . . . .
H15 H -0.4971 0.6712 0.8395 0.054 Uiso 1 1 calc R U . . .
C16 C -0.0953(2) 0.80649(19) 0.48258(15) 0.0193(3) Uani 1 1 d . . . . .
C17 C -0.0580(2) 0.64919(18) 0.49064(15) 0.0185(3) Uani 1 1 d . . . . .
C18 C -0.0761(2) 0.43310(19) 0.57463(15) 0.0207(3) Uani 1 1 d . . . . .
H18 H -0.1283 0.3889 0.6255 0.025 Uiso 1 1 calc R U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Sm1 O4A 2.377(8) . ?
Sm1 O5 2.3805(14) . ?
Sm1 O1 2.3902(14) . ?
Sm1 O6 2.4360(14) 2_576 ?
Sm1 O2 2.4458(14) 2_576 ?
Sm1 O7 2.4680(15) . ?
Sm1 O8 2.504(2) . ?
Sm1 O3 2.5466(15) . ?
Sm1 O4 2.607(3) . ?
Sm1 N9 2.6231(17) 2_577 ?
N1 C14 1.339(3) . ?
N1 N2 1.364(2) . ?
N1 C13 1.425(2) . ?
N2 C15 1.312(3) . ?
N3 C14 1.313(3) . ?
N3 C15 1.355(4) . ?
N4A C6A 1.306(10) . ?
N4A N5A 1.401(14) . ?
N5A C5A 1.304(6) . ?
N6A C6A 1.322(7) . ?
N6A C5A 1.369(8) . ?
C5A H5A 0.9179 . ?
C5A H5B 1.0419 . ?
C6A H6A 1.1428 . ?
C6A H6B 1.2294 . ?
N4B N5B 1.29(3) . ?
N4B C6B 1.38(2) . ?
N4B C3 1.445(18) . ?
N5B C5B 1.355(15) . ?
N6B C5B 1.283(18) . ?
N6B C6B 1.308(14) . ?
C5B H5A 1.1294 . ?
C5B H5B 1.0751 . ?
C6B H6A 1.0076 . ?
C6B H6B 0.7996 . ?
N7 C11 1.329(2) . ?
N7 N8 1.366(3) . ?
N7 C9 1.432(2) . ?
N8 C12 1.321(3) . ?
N9 C11 1.316(3) . ?
N9 C12 1.352(3) . ?
N9 Sm1 2.6232(17) 2_577 ?
O1 C1 1.251(2) . ?
O2 C1 1.248(2) . ?
O2 Sm1 2.4458(14) 2_576 ?
O3 C7 1.232(3) . ?
O4 C7 1.259(3) . ?
O4A C7 1.359(10) . ?
O5 C16 1.254(2) . ?
O6 C16 1.250(2) . ?
O6 Sm1 2.4360(14) 2_576 ?
O7 H7A 0.8089 . ?
O7 H7B 0.8192 . ?
O8 H8A 0.8121 . ?
O8 H8B 0.8057 . ?
O9A O9B 0.96(3) . ?
O9A H9A 0.8164 . ?
O9A H9B 0.8175 . ?
O9B H9A 0.8791 . ?
O9B H9B 0.9415 . ?
O9B H9C 0.8202 . ?
O9B H9D 0.8043 . ?
C1 C2 1.522(2) . ?
C2 C4 1.392(3) . ?
C2 C3 1.395(3) . ?
C3 C4 1.391(3) 2_666 ?
C4 C3 1.391(3) 2_666 ?
C4 H4 0.9300 . ?
C7 C8 1.510(3) . ?
C8 C10 1.388(3) . ?
C8 C9 1.393(3) . ?
C9 C10 1.382(3) 2_567 ?
C10 C9 1.382(3) 2_567 ?
C10 H10 0.9300 . ?
C11 H11 0.9300 . ?
C12 H12 0.9300 . ?
C13 C18 1.388(2) . ?
C13 C17 1.399(3) . ?
C14 H14 0.9300 . ?
C15 H15 0.9300 . ?
C16 C17 1.517(2) . ?
C17 C18 1.392(3) 2_566 ?
C18 C17 1.392(3) 2_566 ?
C18 H18 0.9300 . ?

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
O4A Sm1 O5 97.0(4) . . ?
O5 Sm1 O1 75.18(6) . . ?
O4A Sm1 O6 143.4(4) . 2_576 ?
O5 Sm1 O6 118.41(5) . 2_576 ?
O1 Sm1 O6 77.31(5) . 2_576 ?
O5 Sm1 O2 75.22(5) . 2_576 ?
O1 Sm1 O2 119.38(5) . 2_576 ?
O6 Sm1 O2 72.43(5) 2_576 2_576 ?
O4A Sm1 O7 82.6(5) . . ?
O5 Sm1 O7 147.07(5) . . ?
O1 Sm1 O7 77.80(6) . . ?
O6 Sm1 O7 72.62(5) 2_576 . ?
O2 Sm1 O7 135.63(5) 2_576 . ?
O4A Sm1 O8 48.4(5) . . ?
O5 Sm1 O8 69.23(7) . . ?
O1 Sm1 O8 140.81(7) . . ?
O6 Sm1 O8 134.53(7) 2_576 . ?
O2 Sm1 O8 66.63(7) 2_576 . ?
O7 Sm1 O8 127.37(6) . . ?
O5 Sm1 O3 76.17(5) . . ?
O1 Sm1 O3 74.06(5) . . ?
O6 Sm1 O3 142.89(6) 2_576 . ?
O2 Sm1 O3 143.23(6) 2_576 . ?
O7 Sm1 O3 78.61(6) . . ?
O8 Sm1 O3 81.89(7) . . ?
O5 Sm1 O4 111.93(11) . . ?
O1 Sm1 O4 116.75(8) . . ?
O6 Sm1 O4 129.66(11) 2_576 . ?
O2 Sm1 O4 123.14(9) 2_576 . ?
O7 Sm1 O4 64.99(12) . . ?
O8 Sm1 O4 64.86(13) . . ?
O3 Sm1 O4 50.55(6) . . ?
O5 Sm1 N9 140.20(6) . 2_577 ?
O1 Sm1 N9 142.72(6) . 2_577 ?
O6 Sm1 N9 73.99(5) 2_576 2_577 ?
O2 Sm1 N9 73.44(5) 2_576 2_577 ?
O7 Sm1 N9 71.30(6) . 2_577 ?
O8 Sm1 N9 76.14(7) . 2_577 ?
O3 Sm1 N9 118.17(5) . 2_577 ?
O4 Sm1 N9 67.82(6) . 2_577 ?
C14 N1 N2 109.58(18) . . ?
C14 N1 C13 130.93(18) . . ?
N2 N1 C13 119.35(17) . . ?
C15 N2 N1 102.3(2) . . ?
C14 N3 C15 103.3(2) . . ?
C6A N4A N5A 110.3(7) . . ?
C5A N5A N4A 100.5(6) . . ?
C6A N6A C5A 102.0(5) . . ?
N5A C5A N6A 116.1(6) . . ?
N5A C5A H5A 115.3 . . ?
N6A C5A H5A 128.6 . . ?
N5A C5A H5B 142.9 . . ?
N6A C5A H5B 98.5 . . ?
H5A C5A H5B 33.1 . . ?
N4A C6A N6A 111.1(6) . . ?
N4A C6A H6A 119.0 . . ?
N6A C6A H6A 125.8 . . ?
N4A C6A H6B 92.9 . . ?
N6A C6A H6B 116.1 . . ?
H6A C6A H6B 45.3 . . ?
N5B N4B C6B 107.3(15) . . ?
N5B N4B C3 129(2) . . ?
C6B N4B C3 123(2) . . ?
N4B N5B C5B 104.5(17) . . ?
C5B N6B C6B 104.1(12) . . ?
N6B C5B N5B 113.8(15) . . ?
N6B C5B H5A 149.0 . . ?
N5B C5B H5A 91.6 . . ?
N6B C5B H5B 132.2 . . ?
N5B C5B H5B 114.0 . . ?
H5A C5B H5B 29.9 . . ?
N6B C6B N4B 109.7(14) . . ?
N6B C6B H6A 117.6 . . ?
N4B C6B H6A 128.7 . . ?
N6B C6B H6B 118.8 . . ?
N4B C6B H6B 112.7 . . ?
H6A C6B H6B 59.6 . . ?
C11 N7 N8 109.55(17) . . ?
C11 N7 C9 127.01(17) . . ?
N8 N7 C9 123.42(17) . . ?
C12 N8 N7 102.04(19) . . ?
C11 N9 C12 102.88(17) . . ?
C11 N9 Sm1 123.16(14) . 2_577 ?
C12 N9 Sm1 132.67(14) . 2_577 ?
C1 O1 Sm1 166.93(15) . . ?
C1 O2 Sm1 126.30(13) . 2_576 ?
C7 O3 Sm1 94.09(12) . . ?
C7 O4 Sm1 90.59(18) . . ?
C7 O4A Sm1 98.5(4) . . ?
C16 O5 Sm1 133.88(13) . . ?
C16 O6 Sm1 137.15(13) . 2_576 ?
Sm1 O7 H7A 103.5 . . ?
Sm1 O7 H7B 124.8 . . ?
H7A O7 H7B 108.5 . . ?
Sm1 O8 H8A 133.1 . . ?
Sm1 O8 H8B 118.7 . . ?
H8A O8 H8B 106.5 . . ?
O9B O9A H9A 58.7 . . ?
O9B O9A H9B 63.4 . . ?
H9A O9A H9B 107.3 . . ?
O9A O9B H9A 52.5 . . ?
O9A O9B H9B 50.9 . . ?
H9A O9B H9B 92.5 . . ?
O9A O9B H9C 117.5 . . ?
H9A O9B H9C 159.9 . . ?
H9B O9B H9C 91.2 . . ?
O9A O9B H9D 115.4 . . ?
H9A O9B H9D 68.9 . . ?
H9B O9B H9D 160.8 . . ?
H9C O9B H9D 108.0 . . ?
O2 C1 O1 126.10(18) . . ?
O2 C1 C2 117.19(17) . . ?
O1 C1 C2 116.56(17) . . ?
C4 C2 C3 117.28(16) . . ?
C4 C2 C1 117.55(17) . . ?
C3 C2 C1 124.88(17) . . ?
C4 C3 C2 122.05(17) 2_666 . ?
C4 C3 N4B 119.4(7) 2_666 . ?
C2 C3 N4B 118.5(7) . . ?
C3 C4 C2 120.67(17) 2_666 . ?
C3 C4 H4 119.7 2_666 . ?
C2 C4 H4 119.7 . . ?
O3 C7 O4 124.2(2) . . ?
O3 C7 C8 118.95(18) . . ?
O4 C7 C8 116.8(2) . . ?
O4A C7 C8 124.1(4) . . ?
C10 C8 C9 117.92(17) . . ?
C10 C8 C7 117.48(18) . . ?
C9 C8 C7 124.38(17) . . ?
C10 C9 C8 121.00(17) 2_567 . ?
C10 C9 N7 117.20(17) 2_567 . ?
C8 C9 N7 121.80(17) . . ?
C9 C10 C8 121.08(18) 2_567 . ?
C9 C10 H10 119.5 2_567 . ?
C8 C10 H10 119.5 . . ?
N9 C11 N7 110.72(18) . . ?
N9 C11 H11 124.6 . . ?
N7 C11 H11 124.6 . . ?
N8 C12 N9 114.8(2) . . ?
N8 C12 H12 122.6 . . ?
N9 C12 H12 122.6 . . ?
C18 C13 C17 120.57(17) . . ?
C18 C13 N1 116.36(17) . . ?
C17 C13 N1 123.05(16) . . ?
N3 C14 N1 110.0(2) . . ?
N3 C14 H14 125.0 . . ?
N1 C14 H14 125.0 . . ?
N2 C15 N3 114.7(2) . . ?
N2 C15 H15 122.6 . . ?
N3 C15 H15 122.6 . . ?
O6 C16 O5 126.15(17) . . ?
O6 C16 C17 116.47(16) . . ?
O5 C16 C17 117.29(16) . . ?
C18 C17 C13 117.54(16) 2_566 . ?
C18 C17 C16 115.81(16) 2_566 . ?
C13 C17 C16 126.16(17) . . ?
C13 C18 C17 121.89(17) . 2_566 ?
C13 C18 H18 119.1 . . ?
C17 C18 H18 119.1 2_566 . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
C14 H14 N5A 0.93 2.61 3.330(7) 134.6 1_455
C11 H11 O6 0.93 2.48 3.023(2) 117.4 1_556
C10 H10 N2 0.93 2.54 3.298(3) 139.4 .
C4 H4 O3 0.93 2.41 3.333(3) 172.3 .
O9B H9B O8 0.94 2.01 2.624(14) 121.3 1_655
O9B H9C O4A 0.82 1.57 2.39(2) 172.4 1_655
O9B H9B O8 0.94 2.01 2.624(14) 121.3 1_655
O9A H9B O8 0.82 2.01 2.673(5) 138.0 1_655
O9A H9A N6B 0.82 2.05 2.693(14) 135.3 1_556
O9A H9A N6A 0.82 2.28 2.937(8) 137.3 1_556
O8 H8B N5A 0.81 2.65 3.387(7) 153.4 2_576
O8 H8A O9B 0.81 1.89 2.624(14) 149.9 1_455
O8 H8A O9A 0.81 1.87 2.673(5) 171.6 1_455
O7 H7B N3 0.82 1.91 2.721(3) 169.1 1_655
O7 H7A O4 0.81 2.23 2.729(4) 120.4 .
O7 H7A N8 0.81 2.49 3.272(3) 163.6 .
C5B H5B O7 1.08 2.53 3.59(2) 168.6 2_676
C5A H5A O7 0.92 2.59 3.453(7) 157.0 2_676
C5B H5B O7 1.08 2.53 3.59(2) 168.6 2_676
C5A H5A O7 0.92 2.59 3.453(7) 157.0 2_676

_refine_diff_density_max         0.681
_refine_diff_density_min         -0.833
_refine_diff_density_rms         0.074

####################################################################### 
# 
# 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_EuL66
_database_code_depnum_ccdc_archive 'CCDC 2096056'
loop_
_audit_author_name
_audit_author_address
'Ai Wang' 'Shanxi University'
_audit_update_record             
;
2022-07-19 deposited with the CCDC.	2022-07-21 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         'C18 H13 Eu N9 O8, H2 O'
_chemical_formula_sum            'C18 H15 Eu N9 O9'
_chemical_formula_weight         653.35

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'
Eu Eu -0.1578 3.6682 '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                   9.4618(4)
_cell_length_b                   10.3098(5)
_cell_length_c                   12.4302(6)
_cell_angle_alpha                83.9876(17)
_cell_angle_beta                 80.5410(18)
_cell_angle_gamma                66.8943(16)
_cell_volume                     1099.04(9)
_cell_formula_units_Z            2
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    9254
_cell_measurement_theta_min      2.66
_cell_measurement_theta_max      28.30

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.974
_exptl_crystal_F_000             642
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.260
_exptl_crystal_size_mid          0.250
_exptl_crystal_size_min          0.230
_exptl_absorpt_coefficient_mu    2.927
_shelx_estimated_absorpt_T_min   0.517
_shelx_estimated_absorpt_T_max   0.552
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6689
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_process_details   SADABS
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'Incoatec microsource'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            22567
_diffrn_reflns_av_unetI/netI     0.0224
_diffrn_reflns_av_R_equivalents  0.0250
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         2.776
_diffrn_reflns_theta_max         28.299
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measured_fraction_theta_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_point_group_measured_fraction_full 0.992
_reflns_number_total             5431
_reflns_number_gt                5118
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT, SADABS and XPREP'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_computing_structure_refinement  'SHELXL-2014 (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)+(0.0215P)²+1.3001P] 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         5431
_refine_ls_number_parameters     400
_refine_ls_number_restraints     195
_refine_ls_R_factor_all          0.0227
_refine_ls_R_factor_gt           0.0207
_refine_ls_wR_factor_ref         0.0526
_refine_ls_wR_factor_gt          0.0514
_refine_ls_goodness_of_fit_ref   1.099
_refine_ls_restrained_S_all      1.141
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Eu1 Eu -0.03503(2) 0.96373(2) 0.68456(2) 0.01875(4) Uani 1 1 d . . . . .
N1 N -0.2748(2) 0.6502(2) 0.63453(17) 0.0231(4) Uani 1 1 d . . . . .
N2 N -0.3046(3) 0.5914(3) 0.7349(2) 0.0394(6) Uani 1 1 d . . . . .
N3 N -0.5062(3) 0.7913(3) 0.7007(2) 0.0374(6) Uani 1 1 d . . . . .
N4A N 0.5744(11) 0.6667(10) 0.3254(8) 0.0281(9) Uani 0.707(17) 1 d D U P A 1
N5A N 0.5868(9) 0.7918(7) 0.3483(5) 0.0408(11) Uani 0.707(17) 1 d D U P A 1
N6A N 0.6597(10) 0.7429(6) 0.1689(5) 0.0513(12) Uani 0.707(17) 1 d D U P A 1
C5A C 0.6371(9) 0.8308(8) 0.2515(6) 0.0475(12) Uani 0.707(17) 1 d D U P A 1
H5A H 0.6524 0.9138 0.2478 0.057 Uiso 0.707(17) 1 d DR U P A 1
C6A C 0.6211(11) 0.6418(7) 0.2219(5) 0.0455(12) Uani 0.707(17) 1 d D U P A 1
H6A H 0.5815 0.5683 0.1834 0.055 Uiso 0.707(17) 1 d DR U P A 1
N4B N 0.567(3) 0.676(2) 0.327(2) 0.0315(16) Uani 0.293(17) 1 d D U P A 1
N5B N 0.623(2) 0.769(2) 0.3293(15) 0.0461(17) Uani 0.293(17) 1 d D U P A 1
N6B N 0.606(2) 0.7505(15) 0.1555(12) 0.0481(15) Uani 0.293(17) 1 d D U P A 1
C5B C 0.647(2) 0.812(2) 0.2231(15) 0.0487(16) Uani 0.293(17) 1 d D U P A 1
H5B H 0.7005 0.8885 0.2108 0.058 Uiso 0.293(17) 1 d DR U P A 1
C6B C 0.569(2) 0.6560(17) 0.2187(13) 0.0382(15) Uani 0.293(17) 1 d D U P A 1
H6B H 0.4941 0.6437 0.2083 0.046 Uiso 0.293(17) 1 d DR U P A 1
N7 N 0.0947(3) 0.7032(2) 1.06433(17) 0.0284(5) Uani 1 1 d . . . B 1
N8 N 0.2068(4) 0.7436(4) 1.0050(2) 0.0595(10) Uani 1 1 d . . . B 1
N9 N 0.1191(3) 0.8517(2) 1.16473(17) 0.0253(4) Uani 1 1 d . . . C 1
O1 O 0.1751(2) 0.83872(18) 0.55290(16) 0.0317(4) Uani 1 1 d . . . D 1
O2 O 0.2509(2) 0.83279(18) 0.37327(15) 0.0284(4) Uani 1 1 d . . . E 1
O3 O 0.0472(3) 0.7046(2) 0.74570(15) 0.0389(5) Uani 1 1 d . . . F 1
O4 O -0.0449(7) 0.8502(3) 0.8815(4) 0.0313(15) Uani 0.715(17) 1 d . . P D 1
O4A O -0.1151(17) 0.8598(7) 0.8487(9) 0.027(3) Uani 0.285(17) 1 d . . P D 2
O5 O -0.1462(2) 0.87163(18) 0.57004(15) 0.0267(4) Uani 1 1 d . . . . .
O6 O -0.0658(2) 0.85874(18) 0.39070(15) 0.0285(4) Uani 1 1 d . . . . .
O7 O 0.1887(2) 0.9259(2) 0.77631(16) 0.0315(4) Uani 1 1 d . . . . .
H7A H 0.1783 0.8771 0.8298 0.047 Uiso 1 1 d R U . . .
H7B H 0.2793 0.8933 0.7475 0.047 Uiso 1 1 d R U . . .
O8 O -0.2957(4) 0.9692(4) 0.7728(2) 0.0690(8) Uani 1 1 d . . . . .
H8A H -0.3243 0.9299 0.8269 0.103 Uiso 1 1 d R U . . .
H8B H -0.3669 1.0009 0.7381 0.103 Uiso 1 1 d R U . . .
O9A O 0.5820(8) 0.8681(6) 0.9544(4) 0.089(2) Uani 0.853(18) 1 d . U P . .
H9A H 0.5774 0.8796 1.0189 0.133 Uiso 0.853(18) 1 d R U P G .
H9B H 0.5975 0.9344 0.9202 0.133 Uiso 0.853(18) 1 d R U P . .
O9B O 0.653(4) 0.894(3) 0.982(2) 0.078(10) Uani 0.147(18) 1 d . U P G 2
H9C H 0.7354 0.8828 0.9418 0.116 Uiso 0.147(18) 1 d R U P G 2
H9D H 0.6728 0.8668 1.0423 0.116 Uiso 0.147(18) 1 d R U P G 2
C1 C 0.2637(3) 0.7847(2) 0.4694(2) 0.0218(5) Uani 1 1 d . . . . .
C2 C 0.3924(3) 0.6407(2) 0.48562(19) 0.0207(4) Uani 1 1 d . . . . .
C3 C 0.5300(3) 0.5851(2) 0.41432(19) 0.0221(4) Uani 1 1 d D U . . .
C4 C 0.3647(3) 0.5528(2) 0.5721(2) 0.0228(5) Uani 1 1 d . . . . .
H4 H 0.2746 0.5867 0.6215 0.027 Uiso 1 1 calc R U . . .
C7 C -0.0019(3) 0.7300(3) 0.8421(2) 0.0272(5) Uani 1 1 d . . . . .
C8 C 0.0072(3) 0.6097(2) 0.92442(19) 0.0250(5) Uani 1 1 d . . . . .
C9 C 0.0457(3) 0.6014(3) 1.0290(2) 0.0261(5) Uani 1 1 d . . . . .
C10 C -0.0377(3) 0.5057(3) 0.8968(2) 0.0269(5) Uani 1 1 d . . . . .
H10 H -0.0628 0.5083 0.8271 0.032 Uiso 1 1 calc R U . . .
C11 C 0.0453(3) 0.7685(3) 1.1580(2) 0.0252(5) Uani 1 1 d . . . . .
H11 H -0.0307 0.7571 1.2113 0.030 Uiso 1 1 calc R U . B 1
C12 C 0.2155(5) 0.8332(4) 1.0696(3) 0.0502(9) Uani 1 1 d . . . . .
H12 H 0.2831 0.8800 1.0511 0.060 Uiso 1 1 calc R U . B 1
C13 C -0.1340(3) 0.5790(2) 0.56570(19) 0.0197(4) Uani 1 1 d . . . . .
C14 C -0.3972(3) 0.7682(3) 0.6160(2) 0.0303(5) Uani 1 1 d . . . . .
H14 H -0.4041 0.8254 0.5525 0.036 Uiso 1 1 calc R U . . .
C15 C -0.4433(4) 0.6804(4) 0.7704(3) 0.0450(8) Uani 1 1 d . . . . .
H15 H -0.4953 0.6686 0.8387 0.054 Uiso 1 1 calc R U . . .
C16 C -0.0959(3) 0.8074(2) 0.48295(19) 0.0202(4) Uani 1 1 d . . . . .
C17 C -0.0582(3) 0.6494(2) 0.49089(19) 0.0195(4) Uani 1 1 d . . . . .
C18 C -0.0754(3) 0.4325(2) 0.57444(19) 0.0211(4) Uani 1 1 d . . . . .
H18 H -0.1269 0.3878 0.6254 0.025 Uiso 1 1 calc R U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Eu1 O4A 2.357(7) . ?
Eu1 O5 2.3651(18) . ?
Eu1 O1 2.3779(18) . ?
Eu1 O6 2.4194(18) 2_576 ?
Eu1 O2 2.4274(17) 2_576 ?
Eu1 O7 2.4472(19) . ?
Eu1 O8 2.511(3) . ?
Eu1 O3 2.5415(19) . ?
Eu1 O4 2.604(4) . ?
Eu1 N9 2.614(2) 2_577 ?
Eu1 H7A 2.7525 . ?
N1 C14 1.341(3) . ?
N1 N2 1.365(3) . ?
N1 C13 1.427(3) . ?
N2 C15 1.308(4) . ?
N3 C14 1.315(4) . ?
N3 C15 1.357(4) . ?
N4A C6A 1.307(10) . ?
N4A N5A 1.402(14) . ?
N5A C5A 1.303(7) . ?
N6A C6A 1.315(7) . ?
N6A C5A 1.376(8) . ?
C5A H5A 0.9168 . ?
C5A H5B 1.0420 . ?
C6A H6A 1.1403 . ?
C6A H6B 1.2333 . ?
N4B N5B 1.27(4) . ?
N4B C6B 1.38(3) . ?
N4B C3 1.446(18) . ?
N5B C5B 1.362(17) . ?
N6B C5B 1.30(2) . ?
N6B C6B 1.305(17) . ?
C5B H5A 1.1418 . ?
C5B H5B 1.0742 . ?
C6B H6A 1.0025 . ?
C6B H6B 0.7974 . ?
N7 C11 1.329(3) . ?
N7 N8 1.366(3) . ?
N7 C9 1.433(3) . ?
N8 C12 1.320(4) . ?
N9 C11 1.316(3) . ?
N9 C12 1.350(4) . ?
N9 Eu1 2.614(2) 2_577 ?
O1 C1 1.248(3) . ?
O2 C1 1.251(3) . ?
O2 Eu1 2.4274(17) 2_576 ?
O3 C7 1.227(3) . ?
O4 C7 1.268(4) . ?
O4A C7 1.347(9) . ?
O5 C16 1.253(3) . ?
O6 C16 1.249(3) . ?
O6 Eu1 2.4195(17) 2_576 ?
O7 H7A 0.8070 . ?
O7 H7B 0.8208 . ?
O8 H8A 0.8115 . ?
O8 H8B 0.8006 . ?
O9A O9B 0.94(4) . ?
O9A H9A 0.8147 . ?
O9A H9B 0.8162 . ?
O9B H9A 0.8453 . ?
O9B H9B 0.9649 . ?
O9B H9C 0.8225 . ?
O9B H9D 0.8002 . ?
C1 C2 1.526(3) . ?
C2 C4 1.391(3) . ?
C2 C3 1.396(3) . ?
C3 C4 1.391(3) 2_666 ?
C4 C3 1.391(3) 2_666 ?
C4 H4 0.9300 . ?
C7 C8 1.507(3) . ?
C8 C10 1.390(3) . ?
C8 C9 1.392(3) . ?
C9 C10 1.380(3) 2_567 ?
C10 C9 1.380(3) 2_567 ?
C10 H10 0.9300 . ?
C11 H11 0.9300 . ?
C12 H12 0.9300 . ?
C13 C18 1.389(3) . ?
C13 C17 1.398(3) . ?
C14 H14 0.9300 . ?
C15 H15 0.9300 . ?
C16 C17 1.521(3) . ?
C17 C18 1.392(3) 2_566 ?
C18 C17 1.393(3) 2_566 ?
C18 H18 0.9300 . ?

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
O4A Eu1 O5 96.0(4) . . ?
O5 Eu1 O1 75.33(7) . . ?
O4A Eu1 O6 143.9(3) . 2_576 ?
O5 Eu1 O6 118.87(6) . 2_576 ?
O1 Eu1 O6 77.30(6) . 2_576 ?
O5 Eu1 O2 75.52(6) . 2_576 ?
O1 Eu1 O2 119.78(7) . 2_576 ?
O6 Eu1 O2 72.76(7) 2_576 2_576 ?
O4A Eu1 O7 82.8(4) . . ?
O5 Eu1 O7 147.05(6) . . ?
O1 Eu1 O7 78.22(7) . . ?
O6 Eu1 O7 73.07(7) 2_576 . ?
O2 Eu1 O7 135.81(7) 2_576 . ?
O4A Eu1 O8 47.6(4) . . ?
O5 Eu1 O8 68.84(9) . . ?
O1 Eu1 O8 140.67(9) . . ?
O6 Eu1 O8 134.66(9) 2_576 . ?
O2 Eu1 O8 66.29(9) 2_576 . ?
O7 Eu1 O8 126.87(8) . . ?
O5 Eu1 O3 75.95(7) . . ?
O1 Eu1 O3 74.03(6) . . ?
O6 Eu1 O3 142.73(7) 2_576 . ?
O2 Eu1 O3 143.16(8) 2_576 . ?
O7 Eu1 O3 78.15(7) . . ?
O8 Eu1 O3 81.92(9) . . ?
O5 Eu1 O4 111.20(15) . . ?
O1 Eu1 O4 117.45(10) . . ?
O6 Eu1 O4 129.93(15) 2_576 . ?
O2 Eu1 O4 121.97(12) 2_576 . ?
O7 Eu1 O4 65.06(17) . . ?
O8 Eu1 O4 64.13(17) . . ?
O3 Eu1 O4 50.85(8) . . ?
O5 Eu1 N9 139.98(7) . 2_577 ?
O1 Eu1 N9 143.02(7) . 2_577 ?
O6 Eu1 N9 74.39(6) 2_576 2_577 ?
O2 Eu1 N9 73.31(7) 2_576 2_577 ?
O7 Eu1 N9 71.14(7) . 2_577 ?
O8 Eu1 N9 75.96(9) . 2_577 ?
O3 Eu1 N9 117.78(6) . 2_577 ?
O4 Eu1 N9 67.19(8) . 2_577 ?
O4A Eu1 H7A 66.5 . . ?
O5 Eu1 H7A 141.0 . . ?
O1 Eu1 H7A 86.1 . . ?
O6 Eu1 H7A 88.9 2_576 . ?
O2 Eu1 H7A 142.4 2_576 . ?
O7 Eu1 H7A 16.5 . . ?
O8 Eu1 H7A 112.1 . . ?
O3 Eu1 H7A 66.0 . . ?
O4 Eu1 H7A 48.9 . . ?
N9 Eu1 H7A 70.2 2_577 . ?
C14 N1 N2 109.5(2) . . ?
C14 N1 C13 130.8(2) . . ?
N2 N1 C13 119.6(2) . . ?
C15 N2 N1 102.2(2) . . ?
C14 N3 C15 102.8(2) . . ?
C6A N4A N5A 109.8(7) . . ?
C5A N5A N4A 100.7(6) . . ?
C6A N6A C5A 101.7(5) . . ?
N5A C5A N6A 115.9(6) . . ?
N5A C5A H5A 115.2 . . ?
N6A C5A H5A 128.8 . . ?
N5A C5A H5B 143.1 . . ?
N6A C5A H5B 97.6 . . ?
H5A C5A H5B 34.4 . . ?
N4A C6A N6A 111.7(7) . . ?
N4A C6A H6A 118.5 . . ?
N6A C6A H6A 125.0 . . ?
N4A C6A H6B 91.8 . . ?
N6A C6A H6B 115.4 . . ?
H6A C6A H6B 45.4 . . ?
N5B N4B C6B 107.0(16) . . ?
N5B N4B C3 130(2) . . ?
C6B N4B C3 122(2) . . ?
N4B N5B C5B 105.0(19) . . ?
C5B N6B C6B 102.5(15) . . ?
N6B C5B N5B 113.6(17) . . ?
N6B C5B H5A 148.0 . . ?
N5B C5B H5A 91.8 . . ?
N6B C5B H5B 132.2 . . ?
N5B C5B H5B 114.1 . . ?
H5A C5B H5B 30.8 . . ?
N6B C6B N4B 111.1(16) . . ?
N6B C6B H6A 116.4 . . ?
N4B C6B H6A 129.0 . . ?
N6B C6B H6B 117.1 . . ?
N4B C6B H6B 112.4 . . ?
H6A C6B H6B 60.1 . . ?
C11 N7 N8 109.7(2) . . ?
C11 N7 C9 126.9(2) . . ?
N8 N7 C9 123.3(2) . . ?
C12 N8 N7 101.9(2) . . ?
C11 N9 C12 102.9(2) . . ?
C11 N9 Eu1 123.05(17) . 2_577 ?
C12 N9 Eu1 132.86(17) . 2_577 ?
C1 O1 Eu1 167.25(18) . . ?
C1 O2 Eu1 125.55(15) . 2_576 ?
C7 O3 Eu1 93.61(15) . . ?
C7 O4 Eu1 89.7(3) . . ?
C7 O4A Eu1 99.0(4) . . ?
C16 O5 Eu1 133.66(16) . . ?
C16 O6 Eu1 137.28(16) . 2_576 ?
Eu1 O7 H7A 103.7 . . ?
Eu1 O7 H7B 124.5 . . ?
H7A O7 H7B 108.9 . . ?
Eu1 O8 H8A 133.6 . . ?
Eu1 O8 H8B 118.6 . . ?
H8A O8 H8B 106.2 . . ?
O9B O9A H9A 57.2 . . ?
O9B O9A H9B 66.3 . . ?
H9A O9A H9B 107.2 . . ?
O9A O9B H9A 54.1 . . ?
O9A O9B H9B 50.8 . . ?
H9A O9B H9B 92.8 . . ?
O9A O9B H9C 116.6 . . ?
H9A O9B H9C 162.5 . . ?
H9B O9B H9C 89.7 . . ?
O9A O9B H9D 118.1 . . ?
H9A O9B H9D 70.4 . . ?
H9B O9B H9D 162.0 . . ?
H9C O9B H9D 108.2 . . ?
O1 C1 O2 126.3(2) . . ?
O1 C1 C2 116.6(2) . . ?
O2 C1 C2 116.9(2) . . ?
C4 C2 C3 117.3(2) . . ?
C4 C2 C1 117.6(2) . . ?
C3 C2 C1 124.8(2) . . ?
C4 C3 C2 121.8(2) 2_666 . ?
C4 C3 N4B 119.3(8) 2_666 . ?
C2 C3 N4B 118.8(8) . . ?
C2 C4 C3 120.9(2) . 2_666 ?
C2 C4 H4 119.6 . . ?
C3 C4 H4 119.6 2_666 . ?
O3 C7 O4 124.6(3) . . ?
O3 C7 C8 119.4(2) . . ?
O4 C7 C8 115.5(3) . . ?
O4A C7 C8 124.4(4) . . ?
C10 C8 C9 117.8(2) . . ?
C10 C8 C7 117.4(2) . . ?
C9 C8 C7 124.6(2) . . ?
C10 C9 C8 121.1(2) 2_567 . ?
C10 C9 N7 117.2(2) 2_567 . ?
C8 C9 N7 121.7(2) . . ?
C9 C10 C8 121.1(2) 2_567 . ?
C9 C10 H10 119.4 2_567 . ?
C8 C10 H10 119.4 . . ?
N9 C11 N7 110.5(2) . . ?
N9 C11 H11 124.7 . . ?
N7 C11 H11 124.7 . . ?
N8 C12 N9 115.0(3) . . ?
N8 C12 H12 122.5 . . ?
N9 C12 H12 122.5 . . ?
C18 C13 C17 120.4(2) . . ?
C18 C13 N1 116.3(2) . . ?
C17 C13 N1 123.2(2) . . ?
N3 C14 N1 110.2(3) . . ?
N3 C14 H14 124.9 . . ?
N1 C14 H14 124.9 . . ?
N2 C15 N3 115.3(3) . . ?
N2 C15 H15 122.4 . . ?
N3 C15 H15 122.4 . . ?
O6 C16 O5 126.5(2) . . ?
O6 C16 C17 116.4(2) . . ?
O5 C16 C17 117.1(2) . . ?
C18 C17 C13 117.6(2) 2_566 . ?
C18 C17 C16 115.8(2) 2_566 . ?
C13 C17 C16 126.1(2) . . ?
C13 C18 C17 121.9(2) . 2_566 ?
C13 C18 H18 119.0 . . ?
C17 C18 H18 119.0 2_566 . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
C14 H14 N5A 0.93 2.62 3.336(7) 134.5 1_455
C11 H11 O6 0.93 2.48 3.022(3) 117.3 1_556
C10 H10 N2 0.93 2.53 3.279(4) 137.8 .
C4 H4 O3 0.93 2.40 3.319(3) 172.0 .
O9B H9B O8 0.96 2.01 2.65(3) 122.0 1_655
O9B H9C O4A 0.82 1.63 2.45(3) 171.8 1_655
O9B H9B O8 0.96 2.01 2.65(3) 122.0 1_655
O9A H9B O8 0.82 2.01 2.667(5) 137.1 1_655
O9A H9A N6B 0.81 2.03 2.666(16) 134.5 1_556
O9A H9A N6A 0.81 2.27 2.915(9) 137.0 1_556
O8 H8B N5A 0.80 2.61 3.344(8) 153.2 2_576
O8 H8A O9B 0.81 1.91 2.65(3) 150.7 1_455
O8 H8A O9A 0.81 1.86 2.667(5) 170.4 1_455
O7 H7B N3 0.82 1.91 2.717(3) 169.7 1_655
C5B H5B O7 1.07 2.55 3.60(2) 168.3 2_676
C5A H5A O7 0.92 2.60 3.464(8) 156.5 2_676
C5B H5B O7 1.07 2.55 3.60(2) 168.3 2_676
C5A H5A O7 0.92 2.60 3.464(8) 156.5 2_676

_refine_diff_density_max         0.731
_refine_diff_density_min         -1.112
_refine_diff_density_rms         0.090

####################################################################### 
# 
# 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_TbL66
_database_code_depnum_ccdc_archive 'CCDC 2096057'
loop_
_audit_author_name
_audit_author_address
'Ai Wang' 'Shanxi University'
_audit_update_record             
;
2022-07-19 deposited with the CCDC.	2022-07-21 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         'C36 H25 N18 O15.5 Tb2'
_chemical_formula_sum            'C36 H25 N18 O15.5 Tb2'
_chemical_formula_weight         1275.60

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Tb Tb -0.1723 4.1537 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      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                   9.3859(5)
_cell_length_b                   10.4122(5)
_cell_length_c                   12.1355(6)
_cell_angle_alpha                97.9575(15)
_cell_angle_beta                 92.8219(15)
_cell_angle_gamma                114.2386(15)
_cell_volume                     1063.60(9)
_cell_formula_units_Z            1
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    9920
_cell_measurement_theta_min      2.47
_cell_measurement_theta_max      28.31

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.973
_exptl_crystal_F_000             614
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.260
_exptl_crystal_size_mid          0.240
_exptl_crystal_size_min          0.220
_exptl_absorpt_coefficient_mu    3.391
_shelx_estimated_absorpt_T_min   0.473
_shelx_estimated_absorpt_T_max   0.523
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.5486
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_process_details   SADABS
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'Incoatec microsource'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            37043
_diffrn_reflns_av_unetI/netI     0.0164
_diffrn_reflns_av_R_equivalents  0.0238
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         2.993
_diffrn_reflns_theta_max         28.307
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.979
_diffrn_measured_fraction_theta_full 0.977
_diffrn_reflns_Laue_measured_fraction_max 0.979
_diffrn_reflns_Laue_measured_fraction_full 0.977
_diffrn_reflns_point_group_measured_fraction_max 0.979
_diffrn_reflns_point_group_measured_fraction_full 0.977
_reflns_number_total             5185
_reflns_number_gt                5139
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT, SADABS and XPREP'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_computing_structure_refinement  'SHELXL-2014 (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)+(0.0129P)²+1.1800P] 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         5185
_refine_ls_number_parameters     334
_refine_ls_number_restraints     21
_refine_ls_R_factor_all          0.0139
_refine_ls_R_factor_gt           0.0137
_refine_ls_wR_factor_ref         0.0372
_refine_ls_wR_factor_gt          0.0367
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_restrained_S_all      1.052
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Tb1 Tb 0.53320(2) 0.05842(2) 0.68161(2) 0.01408(3) Uani 1 1 d . . . . .
O1 O 0.38322(17) 0.14553(14) 0.58011(11) 0.0251(3) Uani 1 1 d . . . . .
O2 O 0.39459(17) 0.12473(13) 0.39562(11) 0.0245(3) Uani 1 1 d . . . . .
O3 O 0.69518(17) 0.16412(14) 0.55361(12) 0.0283(3) Uani 1 1 d . . . . .
O4 O 0.71141(16) 0.14230(14) 0.37039(11) 0.0257(3) Uani 1 1 d . . . . .
O5 O 0.44227(19) 0.16017(14) 0.83343(12) 0.0305(3) Uani 1 1 d . . . . .
O6 O 0.63382(19) 0.32465(15) 0.76602(13) 0.0335(3) Uani 1 1 d . . . . .
O7 O 0.77515(16) 0.12251(17) 0.79359(13) 0.0335(3) Uani 1 1 d D . . . .
H7A H 0.7903 0.1061 0.8565 0.050 Uiso 1 1 d DR U . . .
H7B H 0.8600 0.1551 0.7699 0.050 Uiso 1 1 d DR U . . .
N1 N 0.73639(18) 0.61930(16) 0.36105(13) 0.0220(3) Uani 1 1 d . . . . .
N2 N 0.7549(2) 0.5230(2) 0.28044(17) 0.0387(4) Uani 1 1 d . . . . .
N3 N 0.9404(2) 0.7441(2) 0.28280(18) 0.0381(4) Uani 1 1 d . . . . .
N4 N 0.96381(19) 0.70146(16) 0.66059(14) 0.0245(3) Uani 1 1 d . . . . .
N5 N 0.9676(3) 0.8257(2) 0.63457(19) 0.0410(5) Uani 1 1 d . . . . .
N6 N 0.9234(4) 0.8107(3) 0.8136(2) 0.0613(7) Uani 1 1 d . . . . .
N7 N 0.4687(2) 0.73099(16) 0.92472(12) 0.0217(3) Uani 1 1 d . . . . .
N8 N 0.3451(2) 0.76193(19) 0.95076(15) 0.0297(4) Uani 1 1 d . . . . .
N9 N 0.48237(19) 0.89759(16) 0.83015(13) 0.0217(3) Uani 1 1 d . . . . .
C1 C 0.39773(19) 0.19246(17) 0.48994(15) 0.0183(3) Uani 1 1 d . . . . .
C2 C 0.4354(2) 0.34980(17) 0.49522(14) 0.0174(3) Uani 1 1 d . . . . .
C3 C 0.5490(2) 0.41813(18) 0.42796(15) 0.0193(3) Uani 1 1 d . . . . .
H3 H 0.5823 0.3627 0.3782 0.023 Uiso 1 1 calc R U . . .
C4 C 0.6153(2) 0.56529(18) 0.43146(14) 0.0180(3) Uani 1 1 d . . . . .
C5 C 0.8499(3) 0.7496(2) 0.3608(2) 0.0344(5) Uani 1 1 d . . . . .
H5 H 0.8629 0.8323 0.4090 0.041 Uiso 1 1 calc R U . . .
C6 C 0.8776(3) 0.6041(3) 0.2368(2) 0.0416(5) Uani 1 1 d . . . . .
H6 H 0.9187 0.5680 0.1783 0.050 Uiso 1 1 calc R U . . .
C7 C 0.75849(19) 0.20666(17) 0.46899(15) 0.0179(3) Uani 1 1 d . . . . .
C8 C 0.89220(19) 0.35499(17) 0.48767(14) 0.0166(3) Uani 1 1 d . . . . .
C9 C 0.88087(19) 0.45775(18) 0.56843(14) 0.0188(3) Uani 1 1 d . . . . .
H9 H 0.8018 0.4307 0.6151 0.023 Uiso 1 1 calc R U . . .
C10 C 0.9865(2) 0.60060(17) 0.58012(14) 0.0184(3) Uani 1 1 d . . . . .
C11 C 0.9358(4) 0.6942(3) 0.7665(2) 0.0504(7) Uani 1 1 d . . . . .
H11 H 0.9262 0.6180 0.8021 0.060 Uiso 1 1 calc R U . . .
C12 C 0.9438(3) 0.8861(3) 0.7291(3) 0.0509(7) Uani 1 1 d . . . . .
H12 H 0.9410 0.9752 0.7376 0.061 Uiso 1 1 calc R U . . .
C13 C 0.5377(2) 0.28788(19) 0.83570(15) 0.0233(4) Uani 1 1 d . . . . .
C14 C 0.5288(2) 0.40090(19) 0.92393(15) 0.0230(3) Uani 1 1 d . . . . .
C15 C 0.5211(3) 0.5205(2) 0.89027(15) 0.0248(4) Uani 1 1 d . . . . .
H15 H 0.5363 0.5358 0.8172 0.030 Uiso 1 1 calc R U . . .
C16 C 0.4907(2) 0.61741(19) 0.96519(15) 0.0225(3) Uani 1 1 d . . . . .
C17 C 0.5474(2) 0.81199(19) 0.85250(15) 0.0230(3) Uani 1 1 d . . . . .
H17 H 0.6352 0.8085 0.8224 0.028 Uiso 1 1 calc R U . . .
C18 C 0.3600(2) 0.8631(2) 0.89265(17) 0.0276(4) Uani 1 1 d . . . . .
H18 H 0.2921 0.9078 0.8941 0.033 Uiso 1 1 calc R U . . .
O8 O 0.8972(7) 0.0432(7) 0.9682(4) 0.0854(17) Uani 0.5 1 d D U P . .
H8A H 0.8997 -0.0342 0.9803 0.128 Uiso 0.5 1 d DR U P . .
H8B H 0.9869 0.1140 0.9656 0.128 Uiso 0.5 1 d DR U P . .
O9 O 0.0638(18) 0.545(2) 0.0270(14) 0.142(6) Uani 0.25 1 d D U P . .
H9A H 0.0192 0.4726 0.0384 0.213 Uiso 0.25 1 d DR U P . .
H9B H 0.0392 0.6196 0.0684 0.213 Uiso 0.25 1 d DR U P . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Tb1 O3 2.2951(13) . ?
Tb1 O1 2.3470(13) . ?
Tb1 O4 2.3642(13) 2_656 ?
Tb1 O5 2.3669(13) . ?
Tb1 O2 2.3672(12) 2_656 ?
Tb1 O7 2.3770(15) . ?
Tb1 N9 2.5585(15) 1_545 ?
Tb1 O6 2.5679(14) . ?
O1 C1 1.250(2) . ?
O2 C1 1.251(2) . ?
O2 Tb1 2.3672(12) 2_656 ?
O3 C7 1.255(2) . ?
O4 C7 1.249(2) . ?
O4 Tb1 2.3642(13) 2_656 ?
O5 C13 1.257(2) . ?
O6 C13 1.248(2) . ?
O7 H7A 0.8235 . ?
O7 H7B 0.8124 . ?
N1 C5 1.338(3) . ?
N1 N2 1.372(2) . ?
N1 C4 1.429(2) . ?
N2 C6 1.305(3) . ?
N3 C5 1.313(3) . ?
N3 C6 1.350(3) . ?
N4 C11 1.331(3) . ?
N4 N5 1.360(2) . ?
N4 C10 1.422(2) . ?
N5 C12 1.305(3) . ?
N6 C11 1.320(3) . ?
N6 C12 1.351(4) . ?
N7 C17 1.335(2) . ?
N7 N8 1.365(2) . ?
N7 C16 1.426(2) . ?
N8 C18 1.312(2) . ?
N9 C17 1.318(2) . ?
N9 C18 1.358(2) . ?
N9 Tb1 2.5585(15) 1_565 ?
C1 C2 1.519(2) . ?
C2 C3 1.390(2) . ?
C2 C4 1.403(2) 2_666 ?
C3 C4 1.390(2) . ?
C3 H3 0.9300 . ?
C4 C2 1.403(2) 2_666 ?
C5 H5 0.9300 . ?
C6 H6 0.9300 . ?
C7 C8 1.515(2) . ?
C8 C9 1.389(2) . ?
C8 C10 1.397(2) 2_766 ?
C9 C10 1.390(2) . ?
C9 H9 0.9300 . ?
C10 C8 1.397(2) 2_766 ?
C11 H11 0.9300 . ?
C12 H12 0.9300 . ?
C13 C14 1.509(2) . ?
C14 C15 1.392(2) . ?
C14 C16 1.395(2) 2_667 ?
C15 C16 1.390(2) . ?
C15 H15 0.9300 . ?
C16 C14 1.395(2) 2_667 ?
C17 H17 0.9300 . ?
C18 H18 0.9300 . ?
O8 H8A 0.8489 . ?
O8 H8B 0.8676 . ?
O9 O9 1.25(3) 2_565 ?
O9 H9A 0.7305 . ?
O9 H9B 0.9834 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O3 Tb1 O1 77.03(5) . . ?
O3 Tb1 O4 122.93(5) . 2_656 ?
O1 Tb1 O4 76.45(5) . 2_656 ?
O3 Tb1 O5 130.46(5) . . ?
O1 Tb1 O5 81.22(5) . . ?
O4 Tb1 O5 93.52(5) 2_656 . ?
O3 Tb1 O2 78.04(5) . 2_656 ?
O1 Tb1 O2 124.11(5) . 2_656 ?
O4 Tb1 O2 76.75(5) 2_656 2_656 ?
O5 Tb1 O2 148.27(5) . 2_656 ?
O3 Tb1 O7 83.24(6) . . ?
O1 Tb1 O7 144.65(5) . . ?
O4 Tb1 O7 138.56(5) 2_656 . ?
O5 Tb1 O7 90.00(6) . . ?
O2 Tb1 O7 78.83(5) 2_656 . ?
O3 Tb1 N9 146.80(5) . 1_545 ?
O1 Tb1 N9 135.38(5) . 1_545 ?
O4 Tb1 N9 70.35(5) 2_656 1_545 ?
O5 Tb1 N9 72.14(5) . 1_545 ?
O2 Tb1 N9 76.15(5) 2_656 1_545 ?
O7 Tb1 N9 71.60(5) . 1_545 ?
O3 Tb1 O6 78.51(5) . . ?
O1 Tb1 O6 74.16(5) . . ?
O4 Tb1 O6 137.86(5) 2_656 . ?
O5 Tb1 O6 52.75(5) . . ?
O2 Tb1 O6 145.32(5) 2_656 . ?
O7 Tb1 O6 73.34(5) . . ?
N9 Tb1 O6 113.01(5) 1_545 . ?
C1 O1 Tb1 132.55(12) . . ?
C1 O2 Tb1 138.39(12) . 2_656 ?
C7 O3 Tb1 167.89(13) . . ?
C7 O4 Tb1 122.95(11) . 2_656 ?
C13 O5 Tb1 96.71(11) . . ?
C13 O6 Tb1 87.57(11) . . ?
Tb1 O7 H7A 129.1 . . ?
Tb1 O7 H7B 123.0 . . ?
H7A O7 H7B 107.3 . . ?
C5 N1 N2 108.94(17) . . ?
C5 N1 C4 132.96(17) . . ?
N2 N1 C4 117.90(15) . . ?
C6 N2 N1 102.47(18) . . ?
C5 N3 C6 103.26(18) . . ?
C11 N4 N5 109.78(18) . . ?
C11 N4 C10 128.87(19) . . ?
N5 N4 C10 121.35(17) . . ?
C12 N5 N4 102.1(2) . . ?
C11 N6 C12 102.5(2) . . ?
C17 N7 N8 109.80(15) . . ?
C17 N7 C16 129.01(16) . . ?
N8 N7 C16 120.94(15) . . ?
C18 N8 N7 102.28(15) . . ?
C17 N9 C18 103.10(15) . . ?
C17 N9 Tb1 130.11(12) . 1_565 ?
C18 N9 Tb1 125.97(12) . 1_565 ?
O1 C1 O2 126.31(16) . . ?
O1 C1 C2 117.57(15) . . ?
O2 C1 C2 115.94(15) . . ?
C3 C2 C4 117.67(15) . 2_666 ?
C3 C2 C1 114.04(14) . . ?
C4 C2 C1 127.77(15) 2_666 . ?
C2 C3 C4 123.18(15) . . ?
C2 C3 H3 118.4 . . ?
C4 C3 H3 118.4 . . ?
C3 C4 C2 119.13(15) . 2_666 ?
C3 C4 N1 116.14(15) . . ?
C2 C4 N1 124.68(15) 2_666 . ?
N3 C5 N1 110.3(2) . . ?
N3 C5 H5 124.9 . . ?
N1 C5 H5 124.9 . . ?
N2 C6 N3 115.0(2) . . ?
N2 C6 H6 122.5 . . ?
N3 C6 H6 122.5 . . ?
O4 C7 O3 125.25(16) . . ?
O4 C7 C8 117.71(15) . . ?
O3 C7 C8 116.72(15) . . ?
C9 C8 C10 118.04(14) . 2_766 ?
C9 C8 C7 116.98(14) . . ?
C10 C8 C7 124.40(15) 2_766 . ?
C8 C9 C10 120.65(15) . . ?
C8 C9 H9 119.7 . . ?
C10 C9 H9 119.7 . . ?
C9 C10 C8 121.30(15) . 2_766 ?
C9 C10 N4 117.87(15) . . ?
C8 C10 N4 120.79(15) 2_766 . ?
N6 C11 N4 110.2(2) . . ?
N6 C11 H11 124.9 . . ?
N4 C11 H11 124.9 . . ?
N5 C12 N6 115.5(2) . . ?
N5 C12 H12 122.3 . . ?
N6 C12 H12 122.3 . . ?
O6 C13 O5 122.85(16) . . ?
O6 C13 C14 119.34(17) . . ?
O5 C13 C14 117.75(17) . . ?
C15 C14 C16 118.53(15) . 2_667 ?
C15 C14 C13 118.32(16) . . ?
C16 C14 C13 122.70(16) 2_667 . ?
C16 C15 C14 120.42(16) . . ?
C16 C15 H15 119.8 . . ?
C14 C15 H15 119.8 . . ?
C15 C16 C14 121.03(16) . 2_667 ?
C15 C16 N7 118.66(16) . . ?
C14 C16 N7 120.16(15) 2_667 . ?
N9 C17 N7 110.04(16) . . ?
N9 C17 H17 125.0 . . ?
N7 C17 H17 125.0 . . ?
N8 C18 N9 114.77(17) . . ?
N8 C18 H18 122.6 . . ?
N9 C18 H18 122.6 . . ?
H8A O8 H8B 116.8 . . ?
O9 O9 H9A 55.1 2_565 . ?
O9 O9 H9B 105.3 2_565 . ?
H9A O9 H9B 115.2 . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O8 H8A O8 0.85 2.02 2.570(10) 121.7 2_757
O8 H8A N6 0.85 2.49 2.953(5) 115.4 1_545
C18 H18 O8 0.93 2.65 3.392(6) 137.6 2_667
C12 H12 O7 0.93 2.65 3.458(3) 146.0 1_565
C9 H9 O6 0.93 2.54 3.446(2) 163.5 .
C6 H6 O9 0.93 2.65 3.528(15) 158.6 2_665
C6 H6 O9 0.93 2.38 3.288(15) 164.0 1_655
C5 H5 O1 0.93 2.42 2.897(3) 111.6 2_666
O7 H7B N3 0.81 1.93 2.734(2) 172.5 2_766
O7 H7A O8 0.82 1.98 2.739(5) 153.0 .

_refine_diff_density_max         0.396
_refine_diff_density_min         -0.575
_refine_diff_density_rms         0.067

####################################################################### 
# 
# 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_ErL66
_database_code_depnum_ccdc_archive 'CCDC 2096058'
loop_
_audit_author_name
_audit_author_address
'Ai Wang' 'Shanxi University'
_audit_update_record             
;
2022-07-19 deposited with the CCDC.	2022-07-21 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         'C36 H25 Er2 N18 O15.5'
_chemical_formula_sum            'C36 H25 Er2 N18 O15.5'
_chemical_formula_weight         1292.26

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Er Er -0.2586 4.9576 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      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                   9.3751(5)
_cell_length_b                   10.3758(5)
_cell_length_c                   12.0667(5)
_cell_angle_alpha                98.0007(14)
_cell_angle_beta                 93.1898(14)
_cell_angle_gamma                114.3485(13)
_cell_volume                     1050.62(9)
_cell_formula_units_Z            1
_cell_measurement_temperature    298(2)
_cell_measurement_reflns_used    9990
_cell_measurement_theta_min      2.47
_cell_measurement_theta_max      28.91

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.027
_exptl_crystal_F_000             621
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.260
_exptl_crystal_size_mid          0.240
_exptl_crystal_size_min          0.230
_exptl_absorpt_coefficient_mu    4.068
_shelx_estimated_absorpt_T_min   0.418
_shelx_estimated_absorpt_T_max   0.455
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.5420
_exptl_absorpt_correction_T_max  0.7457
_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                   'Incoatec microsource'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            36807
_diffrn_reflns_av_unetI/netI     0.0168
_diffrn_reflns_av_R_equivalents  0.0240
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         2.958
_diffrn_reflns_theta_max         28.310
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measured_fraction_theta_full 0.989
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_Laue_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_point_group_measured_fraction_full 0.989
_reflns_number_total             5169
_reflns_number_gt                5126
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT, SADABS and XPREP'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_computing_structure_refinement  'SHELXL-2014 (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)+(0.0122P)²+1.1531P] 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         5169
_refine_ls_number_parameters     334
_refine_ls_number_restraints     21
_refine_ls_R_factor_all          0.0143
_refine_ls_R_factor_gt           0.0141
_refine_ls_wR_factor_ref         0.0358
_refine_ls_wR_factor_gt          0.0357
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_restrained_S_all      1.073
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Er1 Er 0.53464(2) 0.05855(2) 0.68201(2) 0.01398(3) Uani 1 1 d . . . . .
O1 O 0.38786(17) 0.14550(14) 0.58096(12) 0.0249(3) Uani 1 1 d . . . . .
O2 O 0.39571(17) 0.12326(14) 0.39493(12) 0.0243(3) Uani 1 1 d . . . . .
O3 O 0.69712(17) 0.16435(14) 0.55748(13) 0.0271(3) Uani 1 1 d . . . . .
O4 O 0.70719(16) 0.13948(14) 0.37263(12) 0.0249(3) Uani 1 1 d . . . . .
O5 O 0.4441(2) 0.15919(15) 0.83112(12) 0.0305(3) Uani 1 1 d . . . . .
O6 O 0.6372(2) 0.32574(17) 0.76648(14) 0.0343(3) Uani 1 1 d . . . . .
O7 O 0.77384(17) 0.12294(17) 0.79329(14) 0.0322(3) Uani 1 1 d D . . . .
H7A H 0.7890 0.1065 0.8562 0.048 Uiso 1 1 d DR U . . .
H7B H 0.8587 0.1555 0.7696 0.048 Uiso 1 1 d DR U . . .
N1 N 0.73584(19) 0.62055(17) 0.36066(14) 0.0223(3) Uani 1 1 d . . . . .
N2 N 0.7553(2) 0.5232(2) 0.28084(18) 0.0383(5) Uani 1 1 d . . . . .
N3 N 0.9395(2) 0.7463(2) 0.2821(2) 0.0381(5) Uani 1 1 d . . . . .
N4 N 0.9659(2) 0.70389(17) 0.66086(15) 0.0249(3) Uani 1 1 d . . . . .
N5 N 0.9712(3) 0.8289(2) 0.6347(2) 0.0411(5) Uani 1 1 d . . . . .
N6 N 0.9246(4) 0.8131(3) 0.8142(2) 0.0596(7) Uani 1 1 d . . . . .
N7 N 0.4697(2) 0.73215(16) 0.92419(13) 0.0213(3) Uani 1 1 d . . . . .
N8 N 0.3457(2) 0.76262(19) 0.94980(16) 0.0291(4) Uani 1 1 d . . . . .
N9 N 0.48334(19) 0.89907(16) 0.82862(14) 0.0210(3) Uani 1 1 d . . . . .
C1 C 0.3998(2) 0.19164(18) 0.48973(16) 0.0182(3) Uani 1 1 d . . . . .
C2 C 0.4363(2) 0.34929(18) 0.49512(15) 0.0174(3) Uani 1 1 d . . . . .
C3 C 0.5495(2) 0.41825(19) 0.42793(16) 0.0196(3) Uani 1 1 d . . . . .
H3 H 0.5831 0.3629 0.3782 0.024 Uiso 1 1 calc R U . . .
C4 C 0.6151(2) 0.56621(18) 0.43132(15) 0.0180(3) Uani 1 1 d . . . . .
C5 C 0.8488(3) 0.7519(2) 0.3599(2) 0.0342(5) Uani 1 1 d . . . . .
H5 H 0.8613 0.8352 0.4078 0.041 Uiso 1 1 calc R U . . .
C6 C 0.8781(3) 0.6052(3) 0.2366(2) 0.0409(5) Uani 1 1 d . . . . .
H6 H 0.9196 0.5690 0.1783 0.049 Uiso 1 1 calc R U . . .
C7 C 0.7574(2) 0.20530(17) 0.47147(16) 0.0177(3) Uani 1 1 d . . . . .
C8 C 0.8920(2) 0.35424(17) 0.48851(15) 0.0167(3) Uani 1 1 d . . . . .
C9 C 0.8823(2) 0.45857(18) 0.56951(16) 0.0190(3) Uani 1 1 d . . . . .
H9 H 0.8042 0.4321 0.6170 0.023 Uiso 1 1 calc R U . . .
C10 C 0.9880(2) 0.60211(18) 0.58017(15) 0.0187(3) Uani 1 1 d . . . . .
C11 C 0.9363(4) 0.6960(3) 0.7667(2) 0.0488(7) Uani 1 1 d . . . . .
H11 H 0.9255 0.6191 0.8023 0.059 Uiso 1 1 calc R U . . .
C12 C 0.9464(4) 0.8893(3) 0.7295(3) 0.0506(7) Uani 1 1 d . . . . .
H12 H 0.9439 0.9788 0.7381 0.061 Uiso 1 1 calc R U . . .
C13 C 0.5397(3) 0.2882(2) 0.83513(16) 0.0237(4) Uani 1 1 d . . . . .
C14 C 0.5294(2) 0.4009(2) 0.92382(16) 0.0227(4) Uani 1 1 d . . . . .
C15 C 0.5225(3) 0.5215(2) 0.89041(16) 0.0246(4) Uani 1 1 d . . . . .
H15 H 0.5390 0.5375 0.8173 0.029 Uiso 1 1 calc R U . . .
C16 C 0.4911(2) 0.61784(19) 0.96521(16) 0.0223(4) Uani 1 1 d . . . . .
C17 C 0.5487(2) 0.8133(2) 0.85199(16) 0.0228(4) Uani 1 1 d . . . . .
H17 H 0.6370 0.8100 0.8224 0.027 Uiso 1 1 calc R U . . .
C18 C 0.3607(2) 0.8644(2) 0.89075(18) 0.0264(4) Uani 1 1 d . . . . .
H18 H 0.2926 0.9089 0.8916 0.032 Uiso 1 1 calc R U . . .
O8 O 0.8948(7) 0.0418(7) 0.9684(4) 0.0814(16) Uani 0.5 1 d D U P . .
H8A H 0.8973 -0.0357 0.9806 0.122 Uiso 0.5 1 d DR U P . .
H8B H 0.9845 0.1126 0.9659 0.122 Uiso 0.5 1 d DR U P . .
O9 O 0.0626(17) 0.545(2) 0.0259(15) 0.138(6) Uani 0.25 1 d D U P . .
H9A H 0.0180 0.4728 0.0374 0.208 Uiso 0.25 1 d DR U P . .
H9B H 0.0380 0.6198 0.0674 0.208 Uiso 0.25 1 d DR U P . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Er1 O3 2.2625(13) . ?
Er1 O1 2.3103(13) . ?
Er1 O4 2.3264(13) 2_656 ?
Er1 O5 2.3293(14) . ?
Er1 O2 2.3329(13) 2_656 ?
Er1 O7 2.3363(15) . ?
Er1 N9 2.5204(15) 1_545 ?
Er1 O6 2.5603(15) . ?
O1 C1 1.253(2) . ?
O2 C1 1.249(2) . ?
O2 Er1 2.3330(13) 2_656 ?
O3 C7 1.252(2) . ?
O4 C7 1.247(2) . ?
O4 Er1 2.3264(13) 2_656 ?
O5 C13 1.259(2) . ?
O6 C13 1.246(3) . ?
O7 H7A 0.8185 . ?
O7 H7B 0.8121 . ?
N1 C5 1.339(3) . ?
N1 N2 1.372(2) . ?
N1 C4 1.429(2) . ?
N2 C6 1.312(3) . ?
N3 C5 1.312(3) . ?
N3 C6 1.349(3) . ?
N4 C11 1.329(3) . ?
N4 N5 1.359(3) . ?
N4 C10 1.422(2) . ?
N5 C12 1.306(4) . ?
N6 C11 1.319(3) . ?
N6 C12 1.351(4) . ?
N7 C17 1.334(2) . ?
N7 N8 1.365(2) . ?
N7 C16 1.428(2) . ?
N8 C18 1.319(2) . ?
N9 C17 1.322(2) . ?
N9 C18 1.357(3) . ?
N9 Er1 2.5204(15) 1_565 ?
C1 C2 1.518(2) . ?
C2 C3 1.388(2) . ?
C2 C4 1.403(2) 2_666 ?
C3 C4 1.392(2) . ?
C3 H3 0.9300 . ?
C4 C2 1.403(2) 2_666 ?
C5 H5 0.9300 . ?
C6 H6 0.9300 . ?
C7 C8 1.516(2) . ?
C8 C9 1.390(2) . ?
C8 C10 1.395(2) 2_766 ?
C9 C10 1.390(2) . ?
C9 H9 0.9300 . ?
C10 C8 1.395(2) 2_766 ?
C11 H11 0.9300 . ?
C12 H12 0.9300 . ?
C13 C14 1.510(2) . ?
C14 C15 1.392(2) . ?
C14 C16 1.392(3) 2_667 ?
C15 C16 1.386(2) . ?
C15 H15 0.9300 . ?
C16 C14 1.392(3) 2_667 ?
C17 H17 0.9300 . ?
C18 H18 0.9300 . ?
O8 H8A 0.8460 . ?
O8 H8B 0.8648 . ?
O9 O9 1.22(3) 2_565 ?
O9 H9A 0.7279 . ?
O9 H9B 0.9806 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O3 Er1 O1 77.33(5) . . ?
O3 Er1 O4 122.97(5) . 2_656 ?
O1 Er1 O4 76.25(5) . 2_656 ?
O3 Er1 O5 130.21(5) . . ?
O1 Er1 O5 80.85(5) . . ?
O4 Er1 O5 93.64(5) 2_656 . ?
O3 Er1 O2 78.09(5) . 2_656 ?
O1 Er1 O2 123.97(5) . 2_656 ?
O4 Er1 O2 76.51(5) 2_656 2_656 ?
O5 Er1 O2 148.59(5) . 2_656 ?
O3 Er1 O7 82.33(6) . . ?
O1 Er1 O7 144.17(5) . . ?
O4 Er1 O7 139.31(5) 2_656 . ?
O5 Er1 O7 90.47(6) . . ?
O2 Er1 O7 79.13(5) 2_656 . ?
O3 Er1 N9 146.54(5) . 1_545 ?
O1 Er1 N9 135.43(5) . 1_545 ?
O4 Er1 N9 70.79(5) 2_656 1_545 ?
O5 Er1 N9 72.35(5) . 1_545 ?
O2 Er1 N9 76.24(5) 2_656 1_545 ?
O7 Er1 N9 72.06(5) . 1_545 ?
O3 Er1 O6 77.86(5) . . ?
O1 Er1 O6 73.94(5) . . ?
O4 Er1 O6 138.09(5) 2_656 . ?
O5 Er1 O6 53.13(5) . . ?
O2 Er1 O6 145.26(5) 2_656 . ?
O7 Er1 O6 73.12(6) . . ?
N9 Er1 O6 113.34(5) 1_545 . ?
C1 O1 Er1 133.53(12) . . ?
C1 O2 Er1 138.56(12) . 2_656 ?
C7 O3 Er1 165.91(14) . . ?
C7 O4 Er1 124.61(12) . 2_656 ?
C13 O5 Er1 97.37(12) . . ?
C13 O6 Er1 86.89(12) . . ?
Er1 O7 H7A 128.8 . . ?
Er1 O7 H7B 123.0 . . ?
H7A O7 H7B 107.4 . . ?
C5 N1 N2 108.98(17) . . ?
C5 N1 C4 133.06(18) . . ?
N2 N1 C4 117.73(15) . . ?
C6 N2 N1 102.37(19) . . ?
C5 N3 C6 103.42(19) . . ?
C11 N4 N5 109.93(19) . . ?
C11 N4 C10 128.72(19) . . ?
N5 N4 C10 121.34(18) . . ?
C12 N5 N4 101.9(2) . . ?
C11 N6 C12 102.4(2) . . ?
C17 N7 N8 110.07(15) . . ?
C17 N7 C16 129.08(17) . . ?
N8 N7 C16 120.58(16) . . ?
C18 N8 N7 102.00(16) . . ?
C17 N9 C18 103.01(15) . . ?
C17 N9 Er1 130.18(13) . 1_565 ?
C18 N9 Er1 126.06(12) . 1_565 ?
O2 C1 O1 126.35(16) . . ?
O2 C1 C2 116.08(16) . . ?
O1 C1 C2 117.36(16) . . ?
C3 C2 C4 117.82(15) . 2_666 ?
C3 C2 C1 113.92(15) . . ?
C4 C2 C1 127.73(16) 2_666 . ?
C2 C3 C4 123.25(16) . . ?
C2 C3 H3 118.4 . . ?
C4 C3 H3 118.4 . . ?
C3 C4 C2 118.92(16) . 2_666 ?
C3 C4 N1 116.05(16) . . ?
C2 C4 N1 124.99(16) 2_666 . ?
N3 C5 N1 110.4(2) . . ?
N3 C5 H5 124.8 . . ?
N1 C5 H5 124.8 . . ?
N2 C6 N3 114.8(2) . . ?
N2 C6 H6 122.6 . . ?
N3 C6 H6 122.6 . . ?
O4 C7 O3 125.43(16) . . ?
O4 C7 C8 117.54(16) . . ?
O3 C7 C8 116.70(16) . . ?
C9 C8 C10 117.98(15) . 2_766 ?
C9 C8 C7 116.64(15) . . ?
C10 C8 C7 124.82(16) 2_766 . ?
C10 C9 C8 120.68(16) . . ?
C10 C9 H9 119.7 . . ?
C8 C9 H9 119.7 . . ?
C9 C10 C8 121.33(16) . 2_766 ?
C9 C10 N4 117.60(16) . . ?
C8 C10 N4 121.02(16) 2_766 . ?
N6 C11 N4 110.2(3) . . ?
N6 C11 H11 124.9 . . ?
N4 C11 H11 124.9 . . ?
N5 C12 N6 115.5(2) . . ?
N5 C12 H12 122.2 . . ?
N6 C12 H12 122.2 . . ?
O6 C13 O5 122.50(17) . . ?
O6 C13 C14 119.48(18) . . ?
O5 C13 C14 117.96(18) . . ?
C15 C14 C16 118.36(16) . 2_667 ?
C15 C14 C13 118.44(17) . . ?
C16 C14 C13 122.80(16) 2_667 . ?
C16 C15 C14 120.54(17) . . ?
C16 C15 H15 119.7 . . ?
C14 C15 H15 119.7 . . ?
C15 C16 C14 121.07(16) . 2_667 ?
C15 C16 N7 118.55(17) . . ?
C14 C16 N7 120.25(16) 2_667 . ?
N9 C17 N7 110.04(17) . . ?
N9 C17 H17 125.0 . . ?
N7 C17 H17 125.0 . . ?
N8 C18 N9 114.87(17) . . ?
N8 C18 H18 122.6 . . ?
N9 C18 H18 122.6 . . ?
H8A O8 H8B 116.7 . . ?
O9 O9 H9A 53.9 2_565 . ?
O9 O9 H9B 105.6 2_565 . ?
H9A O9 H9B 115.0 . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O8 H8A O8 0.85 2.04 2.578(10) 120.9 2_757
O8 H8A N6 0.85 2.46 2.923(5) 115.0 1_545
C18 H18 O8 0.93 2.65 3.390(6) 136.8 2_667
C17 H17 N6 0.93 2.69 3.579(3) 159.9 .
C12 H12 N3 0.93 2.65 3.506(3) 152.5 2_776
C12 H12 O7 0.93 2.65 3.455(3) 145.1 1_565
C9 H9 O6 0.93 2.52 3.426(2) 163.9 .
C6 H6 O9 0.93 2.63 3.508(16) 158.5 2_665
C6 H6 O9 0.93 2.38 3.284(15) 164.1 1_655
C5 H5 O1 0.93 2.44 2.912(3) 111.9 2_666
O7 H7B N3 0.81 1.93 2.739(2) 173.6 2_766
O7 H7A O8 0.82 1.98 2.735(5) 152.9 .

_refine_diff_density_max         0.744
_refine_diff_density_min         -0.683
_refine_diff_density_rms         0.071

