# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2020

####################################################################### 
# 
# 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_l71-dy_sq
_database_code_depnum_ccdc_archive 'CCDC 1922332'
loop_
_audit_author_name
_audit_author_address
'Yapei Shang'
;Zhengzhou University
China
;
_audit_update_record             
;
2019-06-11 deposited with the CCDC.	2020-03-09 downloaded from the CCDC.
;
_audit_creation_date             2019-06-11
_audit_creation_method           
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_chemical_formula_moiety         'C24 H16 Dy N3 O8'
_chemical_formula_sum            'C24 H16 Dy N3 O8'
_chemical_formula_weight         636.91
_chemical_oxdiff_formula         'C H N O Dy'
loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source
_atom_type_scat_dispersion_source
H 0.00000 0.00000 0.49300 0.32291 0.14019 0.04081 10.51090 26.12570 3.14236
57.79970 0.0030380000826
'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'
C 0.00347 0.00161 2.31000 1.02000 1.58860 0.86500 20.84390 10.20750 0.56870
51.65120 0.215599998832
'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'
Dy -0.09334 4.42894 26.50700 17.63830 14.55960 2.96577 2.18020 0.20217 12.18990
111.87400 4.29727983475
'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'
O 0.01158 0.00611 3.04850 2.28680 1.54630 0.86700 13.27710 5.70110 0.32390
32.90890 0.250800013542
'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'
N 0.00653 0.00323 12.21260 3.13220 2.01250 1.16630 0.00570 9.89330 28.99750
0.58260 -11.5290002823
'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/c 1'
_space_group_name_Hall           '-P 2ybc'
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 x,y,z
2 -x,y+1/2,-z+1/2
3 -x,-y,-z
4 x,-y-1/2,z-1/2

_symmetry_Int_Tables_number      14
_cell_length_a                   10.6979(5)
_cell_length_b                   12.2441(6)
_cell_length_c                   18.0543(8)
_cell_angle_alpha                90
_cell_angle_beta                 95.091(4)
_cell_angle_gamma                90
_cell_volume                     2355.53(19)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    4145
_cell_measurement_theta_max      27.1010
_cell_measurement_theta_min      3.7760
_exptl_absorpt_coefficient_mu    3.227
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.82329
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.7958
_exptl_crystal_description       needle
_exptl_crystal_F_000             1244.2481
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.1
_diffrn_reflns_av_R_equivalents  0.0440
_diffrn_reflns_av_unetI/netI     0.0808
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            11078
_diffrn_reflns_theta_full        28.4197
_diffrn_reflns_theta_max         28.42
_diffrn_reflns_theta_min         3.28
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0584
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 0.8408
_diffrn_measured_fraction_theta_max 0.8408
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -79.00  -2.00   1.00   22.00    --  -13.80 -57.00-150.00   77
  2  ω    -19.00   6.00   1.00   22.00    --  -13.80 -99.00  60.00   25
  3  ω     36.00  71.00   1.00   22.00    --   14.82 178.00 -60.00   35
  4  ω     -3.00  84.00   1.00   22.00    --   14.82  38.00   0.00   87
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Single source at offset/far, EosS2'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0146726000
_diffrn_orient_matrix_UB_12      0.0162549000
_diffrn_orient_matrix_UB_13      -0.0375033000
_diffrn_orient_matrix_UB_21      -0.0648512000
_diffrn_orient_matrix_UB_22      -0.0062509000
_diffrn_orient_matrix_UB_23      0.0043172000
_diffrn_orient_matrix_UB_31      -0.0030207000
_diffrn_orient_matrix_UB_32      0.0552183000
_diffrn_orient_matrix_UB_33      0.0115226000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              14
_reflns_limit_h_min              -14
_reflns_limit_k_max              16
_reflns_limit_k_min              0
_reflns_limit_l_max              24
_reflns_limit_l_min              0
_reflns_number_gt                3813
_reflns_number_total             4984
_reflns_odcompleteness_completeness 99.69
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     25.30
_reflns_threshold_expression     I>=2u(I)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine (Bourhis et al., 2015)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_refine_diff_density_max         3.6267
_refine_diff_density_min         -2.0117
_refine_diff_density_rms         0.3055
_refine_ls_d_res_high            0.7467
_refine_ls_d_res_low             6.2024
_refine_ls_goodness_of_fit_ref   1.0030
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    32
_refine_ls_number_parameters     330
_refine_ls_number_reflns         4984
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0713
_refine_ls_R_factor_gt           0.0507
_refine_ls_restrained_S_all      1.0028
_refine_ls_shift/su_max          0.3931
_refine_ls_shift/su_mean         0.0113
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0598P)²+14.8264P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1277
_refine_ls_wR_factor_ref         0.1380
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H,H) groups
2. Restrained distances
 O2A-C7 \\sim O2-C7
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(O2A) = Uanis(O2)
4. Others
 Sof(O2)=1-FVAR(1)
 Sof(O2A)=FVAR(1)
5.a Rotating group:
 O7(H7a,H7b), O8(H8a,H8b)
5.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C4(H4), C11(H11), C14(H14), C16(H16), C17(H17), C18(H18), C19(H19),
 C20(H20), C21(H21), C23(H23), C24(H24)
;
_atom_sites_solution_primary     iterative
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_refinement_flags_posn
_atom_site_disorder_group
Dy1 Dy 0.81746(3) 0.46232(3) 0.361484(19) 0.01786(13) Uani 1.000000 . .
O1 O 0.7944(5) 0.3086(5) 0.2978(3) 0.0297(14) Uani 1.000000 . .
O2A O 0.9472(12) 0.215(2) 0.2509(15) 0.050(6) Uani 0.74(6) D 1
O3 O 0.8534(5) 0.1129(6) -0.0144(3) 0.0313(15) Uani 1.000000 . .
O4 O 0.6590(5) 0.0921(6) -0.0590(3) 0.0345(16) Uani 1.000000 . .
O5 O 0.3113(5) 0.1205(5) 0.1262(4) 0.0357(15) Uani 1.000000 . .
O6 O 0.3887(5) -0.0010(5) 0.2062(3) 0.0291(14) Uani 1.000000 . .
O7 O 0.8818(6) 0.5448(6) 0.2544(3) 0.0365(16) Uani 1.000000 . .
H7a H 0.858(7) 0.6164(18) 0.250(2) 0.055(2) Uiso 1.000000 GR .
H7b H 0.842(6) 0.516(4) 0.2123(3) 0.055(2) Uiso 1.000000 GR .
O8 O 0.9398(5) 0.6012(5) 0.4183(4) 0.0349(15) Uani 1.000000 . .
H8a H 1.016(2) 0.578(2) 0.431(4) 0.052(2) Uiso 1.000000 GR .
H8b H 0.913(4) 0.618(4) 0.461(2) 0.052(2) Uiso 1.000000 GR .
N1 N 0.4685(7) 0.1971(6) 0.4253(4) 0.0320(18) Uani 1.000000 . .
N2 N 0.0443(6) 0.3881(6) 0.3696(4) 0.0289(16) Uani 1.000000 . .
N3 N 0.7727(11) 0.0317(8) 0.6233(5) 0.058(3) Uani 1.000000 . .
C1 C 0.7372(7) 0.1878(7) 0.1986(4) 0.0195(17) Uani 1.000000 . .
C2 C 0.7770(7) 0.1722(6) 0.1281(4) 0.0206(17) Uani 1.000000 . .
H2 H 0.8598(7) 0.1871(6) 0.1195(4) 0.025(2) Uiso 1.000000 R .
C3 C 0.6934(7) 0.1343(6) 0.0703(4) 0.0190(17) Uani 1.000000 . .
C4 C 0.5717(7) 0.1092(7) 0.0832(4) 0.0233(18) Uani 1.000000 . .
H4 H 0.5154(7) 0.0853(7) 0.0444(4) 0.028(2) Uiso 1.000000 R .
C5 C 0.5332(7) 0.1200(7) 0.1550(4) 0.0208(17) Uani 1.000000 . .
C6 C 0.6169(7) 0.1615(7) 0.2137(4) 0.0186(16) Uani 1.000000 . .
C7 C 0.8328(8) 0.2379(8) 0.2552(5) 0.033(2) Uani 1.000000 D .
C8 C 0.7368(7) 0.1133(7) -0.0058(4) 0.0225(17) Uani 1.000000 . .
C9 C 0.4040(7) 0.0772(8) 0.1657(5) 0.0258(19) Uani 1.000000 . .
C10 C 0.5678(7) 0.1760(7) 0.2878(4) 0.0222(18) Uani 1.000000 . .
C11 C 0.4601(7) 0.2318(7) 0.2957(5) 0.0271(19) Uani 1.000000 . .
H11 H 0.4189(7) 0.2657(7) 0.2543(5) 0.033(2) Uiso 1.000000 R .
C12 C 0.4107(7) 0.2395(7) 0.3622(5) 0.0260(19) Uani 1.000000 . .
C13 C 0.5793(8) 0.1471(8) 0.4206(5) 0.028(2) Uani 1.000000 . .
C14 C 0.6266(8) 0.1323(7) 0.3518(4) 0.0250(19) Uani 1.000000 . .
H14 H 0.6996(8) 0.0918(7) 0.3491(4) 0.030(2) Uiso 1.000000 R .
C15 C 0.2876(8) 0.2937(8) 0.3690(5) 0.030(2) Uani 1.000000 . .
C16 C 0.2494(8) 0.3812(8) 0.3252(6) 0.042(3) Uani 1.000000 . .
H16 H 0.3047(8) 0.4113(8) 0.2939(6) 0.050(3) Uiso 1.000000 R .
C17 C 0.1316(9) 0.4258(8) 0.3265(6) 0.042(3) Uani 1.000000 . .
H17 H 0.1109(9) 0.4854(8) 0.2960(6) 0.050(3) Uiso 1.000000 R .
C18 C 0.0834(9) 0.3032(10) 0.4121(6) 0.049(3) Uani 1.000000 . .
H18 H 0.0265(9) 0.2734(10) 0.4426(6) 0.058(3) Uiso 1.000000 R .
C19 C 0.2017(10) 0.2556(10) 0.4149(6) 0.051(3) Uani 1.000000 . .
H19 H 0.2225(10) 0.1984(10) 0.4476(6) 0.061(4) Uiso 1.000000 R .
C20 C 0.8321(13) 0.0479(12) 0.5627(7) 0.070(4) Uani 1.000000 . .
H20 H 0.9182(13) 0.0356(12) 0.5652(7) 0.084(5) Uiso 1.000000 R .
C21 C 0.7716(10) 0.0824(11) 0.4959(6) 0.057(3) Uani 1.000000 . .
H21 H 0.8166(10) 0.0886(11) 0.4544(6) 0.069(4) Uiso 1.000000 R .
C22 C 0.6480(9) 0.1071(8) 0.4902(5) 0.031(2) Uani 1.000000 . .
C23 C 0.5872(10) 0.0957(9) 0.5540(5) 0.041(2) Uani 1.000000 . .
H23 H 0.5026(10) 0.1134(9) 0.5540(5) 0.049(3) Uiso 1.000000 R .
C24 C 0.6540(13) 0.0576(9) 0.6183(6) 0.051(3) Uani 1.000000 . .
H24 H 0.6112(13) 0.0500(9) 0.6606(6) 0.061(4) Uiso 1.000000 R .
O2 O 0.928(4) 0.179(5) 0.275(3) 0.050(6) Uani 0.26(6) D 2


loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Dy1 O1 2.208(6) . ?
Dy1 O3 2.422(6) 4_566 ?
Dy1 O4 2.410(5) 4_566 ?
Dy1 O5 2.399(6) 2_655 ?
Dy1 O6 2.466(6) 2_655 ?
Dy1 O7 2.338(6) . ?
Dy1 O8 2.327(6) . ?
Dy1 N2 2.583(7) 1_655 ?
Dy1 C8 2.776(8) 4_566 ?
Dy1 C9 2.761(8) 2_655 ?
O1 C7 1.252(10) . ?
O2A C7 1.265(14) . ?
O3 C8 1.271(9) . ?
O4 C8 1.241(9) . ?
O5 C9 1.284(10) . ?
O6 C9 1.225(10) . ?
O7 H7a 0.9132 . ?
O7 H7b 0.9110 . ?
O8 H8a 0.8723 . ?
O8 H8b 0.8724 . ?
N1 C12 1.352(11) . ?
N1 C13 1.343(11) . ?
N2 C17 1.348(12) . ?
N2 C18 1.337(13) . ?
N3 C20 1.329(15) . ?
N3 C24 1.304(15) . ?
C1 C2 1.391(11) . ?
C1 C6 1.377(10) . ?
C1 C7 1.511(11) . ?
C2 H2 0.9300 . ?
C2 C3 1.393(10) . ?
C3 C4 1.378(10) . ?
C3 C8 1.510(10) . ?
C4 H4 0.9300 . ?
C4 C5 1.401(10) . ?
C5 C6 1.420(10) . ?
C5 C9 1.506(11) . ?
C6 C10 1.490(10) . ?
C7 O2 1.27(3) . ?
C10 C11 1.358(11) . ?
C10 C14 1.374(11) . ?
C11 H11 0.9300 . ?
C11 C12 1.357(11) . ?
C12 C15 1.489(11) . ?
C13 C14 1.394(11) . ?
C13 C22 1.481(12) . ?
C14 H14 0.9300 . ?
C15 C16 1.372(13) . ?
C15 C19 1.372(13) . ?
C16 H16 0.9300 . ?
C16 C17 1.376(13) . ?
C17 H17 0.9300 . ?
C18 H18 0.9300 . ?
C18 C19 1.390(13) . ?
C19 H19 0.9300 . ?
C20 H20 0.9300 . ?
C20 C21 1.382(15) . ?
C21 H21 0.9300 . ?
C21 C22 1.351(13) . ?
C22 C23 1.381(12) . ?
C23 H23 0.9300 . ?
C23 C24 1.389(14) . ?
C24 H24 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
O3 Dy1 O1 99.1(2) 4_566 . ?
O4 Dy1 O1 91.3(2) 4_566 . ?
O4 Dy1 O3 53.57(18) 4_566 4_566 ?
O5 Dy1 O1 134.3(2) 2_655 . ?
O5 Dy1 O3 105.5(2) 2_655 4_566 ?
O5 Dy1 O4 74.2(2) 2_655 4_566 ?
O6 Dy1 O1 81.0(2) 2_655 . ?
O6 Dy1 O3 126.12(18) 2_655 4_566 ?
O6 Dy1 O4 72.55(19) 2_655 4_566 ?
O6 Dy1 O5 53.4(2) 2_655 2_655 ?
O7 Dy1 O1 88.0(2) . . ?
O7 Dy1 O3 153.5(2) . 4_566 ?
O7 Dy1 O4 152.4(2) . 4_566 ?
O7 Dy1 O5 86.6(2) . 2_655 ?
O7 Dy1 O6 80.1(2) . 2_655 ?
O8 Dy1 O1 152.2(2) . . ?
O8 Dy1 O3 80.4(2) . 4_566 ?
O8 Dy1 O4 109.7(2) . 4_566 ?
O8 Dy1 O5 71.0(2) . 2_655 ?
O8 Dy1 O6 121.9(2) . 2_655 ?
O8 Dy1 O7 81.5(2) . . ?
N2 Dy1 O1 77.9(2) 1_655 . ?
N2 Dy1 O3 75.1(2) 1_655 4_566 ?
N2 Dy1 O4 125.2(2) 1_655 4_566 ?
N2 Dy1 O5 145.4(2) 1_655 2_655 ?
N2 Dy1 O6 152.4(2) 1_655 2_655 ?
N2 Dy1 O7 81.7(2) 1_655 . ?
N2 Dy1 O8 75.1(2) 1_655 . ?
C8 Dy1 O1 97.8(2) 4_566 . ?
C8 Dy1 O3 27.2(2) 4_566 4_566 ?
C8 Dy1 O4 26.5(2) 4_566 4_566 ?
C8 Dy1 O5 87.9(2) 4_566 2_655 ?
C8 Dy1 O6 98.9(2) 4_566 2_655 ?
C8 Dy1 O7 173.9(2) 4_566 . ?
C8 Dy1 O8 94.0(2) 4_566 . ?
C8 Dy1 N2 101.3(2) 4_566 1_655 ?
C9 Dy1 O1 106.7(2) 2_655 . ?
C9 Dy1 O3 114.9(2) 2_655 4_566 ?
C9 Dy1 O4 67.0(2) 2_655 4_566 ?
C9 Dy1 O5 27.7(2) 2_655 2_655 ?
C9 Dy1 O6 26.3(2) 2_655 2_655 ?
C9 Dy1 O7 86.8(2) 2_655 . ?
C9 Dy1 O8 98.4(2) 2_655 . ?
C9 Dy1 N2 167.4(2) 2_655 1_655 ?
C9 Dy1 C8 89.7(2) 2_655 4_566 ?
C7 O1 Dy1 151.9(6) . . ?
C8 O3 Dy1 92.1(5) . 4_565 ?
C8 O4 Dy1 93.5(5) . 4_565 ?
C9 O5 Dy1 92.1(5) . 2_645 ?
C9 O6 Dy1 90.4(5) . 2_645 ?
H7a O7 Dy1 112.8 . . ?
H7b O7 Dy1 111.8 . . ?
H7b O7 H7a 101.5 . . ?
H8a O8 Dy1 110.8 . . ?
H8b O8 Dy1 110.2 . . ?
H8b O8 H8a 103.4 . . ?
C13 N1 C12 117.5(7) . . ?
C17 N2 Dy1 122.8(6) . 1_455 ?
C18 N2 Dy1 123.4(6) . 1_455 ?
C18 N2 C17 113.6(8) . . ?
C24 N3 C20 116.1(10) . . ?
C6 C1 C2 121.2(7) . . ?
C7 C1 C2 115.5(7) . . ?
C7 C1 C6 123.3(7) . . ?
H2 C2 C1 119.9(4) . . ?
C3 C2 C1 120.2(7) . . ?
C3 C2 H2 119.9(4) . . ?
C4 C3 C2 120.0(7) . . ?
C8 C3 C2 120.7(7) . . ?
C8 C3 C4 119.2(7) . . ?
H4 C4 C3 120.1(4) . . ?
C5 C4 C3 119.8(7) . . ?
C5 C4 H4 120.1(5) . . ?
C6 C5 C4 120.4(7) . . ?
C9 C5 C4 115.7(7) . . ?
C9 C5 C6 123.7(7) . . ?
C5 C6 C1 118.3(7) . . ?
C10 C6 C1 124.1(7) . . ?
C10 C6 C5 117.5(7) . . ?
C1 C7 O1 117.2(7) . . ?
O3 C8 Dy1 60.6(4) . 4_565 ?
O4 C8 Dy1 60.1(4) . 4_565 ?
O4 C8 O3 120.2(7) . . ?
C3 C8 Dy1 170.2(6) . 4_565 ?
C3 C8 O3 119.7(7) . . ?
C3 C8 O4 120.1(7) . . ?
O5 C9 Dy1 60.2(4) . 2_645 ?
O6 C9 Dy1 63.3(4) . 2_645 ?
O6 C9 O5 121.2(7) . . ?
C5 C9 Dy1 159.5(6) . 2_645 ?
C5 C9 O5 117.3(8) . . ?
C5 C9 O6 121.4(8) . . ?
C11 C10 C6 121.6(7) . . ?
C14 C10 C6 122.5(7) . . ?
C14 C10 C11 115.9(7) . . ?
H11 C11 C10 119.1(5) . . ?
C12 C11 C10 121.9(8) . . ?
C12 C11 H11 119.1(5) . . ?
C11 C12 N1 122.3(8) . . ?
C15 C12 N1 116.3(7) . . ?
C15 C12 C11 121.4(8) . . ?
C14 C13 N1 120.5(8) . . ?
C22 C13 N1 118.1(7) . . ?
C22 C13 C14 121.4(8) . . ?
C13 C14 C10 121.5(8) . . ?
H14 C14 C10 119.2(5) . . ?
H14 C14 C13 119.2(5) . . ?
C16 C15 C12 121.3(8) . . ?
C19 C15 C12 122.9(9) . . ?
C19 C15 C16 115.6(8) . . ?
H16 C16 C15 119.1(5) . . ?
C17 C16 C15 121.8(9) . . ?
C17 C16 H16 119.1(6) . . ?
C16 C17 N2 123.8(10) . . ?
H17 C17 N2 118.1(6) . . ?
H17 C17 C16 118.1(6) . . ?
H18 C18 N2 117.2(5) . . ?
C19 C18 N2 125.7(9) . . ?
C19 C18 H18 117.2(6) . . ?
C18 C19 C15 119.5(10) . . ?
H19 C19 C15 120.2(6) . . ?
H19 C19 C18 120.2(6) . . ?
H20 C20 N3 118.6(7) . . ?
C21 C20 N3 122.8(12) . . ?
C21 C20 H20 118.6(7) . . ?
H21 C21 C20 119.5(7) . . ?
C22 C21 C20 121.0(10) . . ?
C22 C21 H21 119.5(6) . . ?
C21 C22 C13 123.3(8) . . ?
C23 C22 C13 120.4(8) . . ?
C23 C22 C21 116.3(9) . . ?
H23 C23 C22 120.5(6) . . ?
C24 C23 C22 119.0(10) . . ?
C24 C23 H23 120.5(7) . . ?
C23 C24 N3 124.5(10) . . ?
H24 C24 N3 117.7(6) . . ?
H24 C24 C23 117.7(7) . . ?

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
O7 H7b N3 0.9110 1.804(11) 2.711(11) 173.9(5) 4_565

_olex2_date_sample_data_collection 2018-12-17
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.458
_oxdiff_exptl_absorpt_empirical_full_min 0.796
loop_
_restr_equal_distance_atom_site_label_1
_restr_equal_distance_atom_site_label_2
_restr_equal_distance_site_symmetry_2
_restr_equal_distance_class_id
O2A C7 1 1
O2 C7 1 1

loop_
_restr_equal_distance_class_class_id
_restr_equal_distance_class_target_weight_param
_restr_equal_distance_class_average
_restr_equal_distance_class_esd
_restr_equal_distance_class_diff_max
1 0.0200 1.2685 0.0037 0.0037

####################################################################### 
# 
# 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_l71-sm_sq
_database_code_depnum_ccdc_archive 'CCDC 1961834'
loop_
_audit_author_name
_audit_author_address
'yapei shang'
;zhengzhou university
China
;
_audit_update_record             
;
2019-10-29 deposited with the CCDC.	2020-03-09 downloaded from the CCDC.
;
_audit_creation_date             2019-06-11
_audit_creation_method           
;
Olex2 1.2-alpha
(compiled 2018.07.26 svn.r3523 for OlexSys, GUI svn.r5532)
;
_shelx_SHELXL_version_number     2014/7
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C24 H16 N3 O8 Sm'
_chemical_formula_sum            'C24 H16 N3 O8 Sm'
_chemical_formula_weight         624.75
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C  H N O Sm'
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'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/c 1'
_space_group_name_Hall           '-P 2ybc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   10.7541(3)
_cell_length_b                   12.3686(4)
_cell_length_c                   18.2242(4)
_cell_angle_alpha                90
_cell_angle_beta                 95.145(2)
_cell_angle_gamma                90
_cell_volume                     2414.29(12)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    4917
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.5650
_cell_measurement_theta_min      3.7960
_shelx_estimated_absorpt_T_max   0.755
_shelx_estimated_absorpt_T_min   0.564
_exptl_absorpt_coefficient_mu    2.486
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.69874
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear light yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.719
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1228
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.12
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0395
_diffrn_reflns_av_unetI/netI     0.0636
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.839
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            11153
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.839
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.343
_diffrn_reflns_theta_min         3.480
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0584
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.839
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     19.00  52.00   1.00    6.00    --  -13.80  77.00-180.00   33
  2  ω    -24.00  51.00   1.00    6.00    --  -13.80  77.00 -30.00   75
  3  ω    -11.00  82.00   1.00    6.00    --   14.82  77.00  90.00   93
  4  ω     53.00  78.00   1.00    6.00    --   14.82  77.00 -60.00   25
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Single source at offset/far, EosS2'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0301291000
_diffrn_orient_matrix_UB_12      -0.0045428000
_diffrn_orient_matrix_UB_13      -0.0329229000
_diffrn_orient_matrix_UB_21      0.0583973000
_diffrn_orient_matrix_UB_22      -0.0058246000
_diffrn_orient_matrix_UB_23      0.0210089000
_diffrn_orient_matrix_UB_31      -0.0083686000
_diffrn_orient_matrix_UB_32      -0.0568805000
_diffrn_orient_matrix_UB_33      0.0004712000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4168
_reflns_number_total             5063
_reflns_odcompleteness_completeness 99.63
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     25.30
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_refine_diff_density_max         0.785
_refine_diff_density_min         -0.802
_refine_diff_density_rms         0.128
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     327
_refine_ls_number_reflns         5063
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0509
_refine_ls_R_factor_gt           0.0385
_refine_ls_restrained_S_all      1.032
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0274P)²+0.6717P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0743
_refine_ls_wR_factor_ref         0.0804
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H,H) groups
2.a Rotating group:
 O8(H8A,H8B), O7(H7A,H7B)
2.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C6(H6), C11(H11), C14(H14), C15(H15), C16(H16), C17(H17), C18(H18),
 C21(H21), C22(H22), C23(H23), C24(H24)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Sm1 Sm 0.18238(2) 0.53855(2) 0.63868(2) 0.01792(8) Uani 1 1 d . . . . .
O1 O 0.2025(3) 0.6956(3) 0.70146(16) 0.0325(8) Uani 1 1 d . . . . .
O2 O 0.0556(3) 0.7934(4) 0.7454(2) 0.0797(17) Uani 1 1 d . . . . .
O3 O 0.1480(3) 0.8835(3) 1.01319(14) 0.0276(8) Uani 1 1 d . . . . .
O4 O 0.3421(3) 0.9118(3) 1.05573(15) 0.0340(9) Uani 1 1 d . . . . .
O8 O 0.0590(3) 0.3978(3) 0.57994(16) 0.0350(8) Uani 1 1 d . . . . .
H8A H 0.0819 0.3371 0.5991 0.052 Uiso 1 1 d GR . . . .
H8B H -0.0081 0.3877 0.5516 0.052 Uiso 1 1 d GR . . . .
O7 O 0.1165(3) 0.4564(3) 0.74861(16) 0.0383(9) Uani 1 1 d . . . . .
H7A H 0.0565 0.4050 0.7381 0.057 Uiso 1 1 d GR . . . .
H7B H 0.0761 0.5041 0.7763 0.057 Uiso 1 1 d GR . . . .
O5 O 0.6085(3) 1.0009(3) 0.79266(16) 0.0300(8) Uani 1 1 d . . . . .
O6 O 0.6868(3) 0.8758(3) 0.86979(17) 0.0338(8) Uani 1 1 d . . . . .
N1 N 0.5294(3) 0.8030(3) 0.57468(19) 0.0281(9) Uani 1 1 d . . . . .
N2 N 0.2255(5) 0.9665(4) 0.3781(2) 0.0555(14) Uani 1 1 d . . . . .
N3 N 0.9509(3) 0.6132(4) 0.6291(2) 0.0303(9) Uani 1 1 d . . . . .
C1 C 0.3065(4) 0.8676(4) 0.9286(2) 0.0199(10) Uani 1 1 d . . . . .
C2 C 0.4284(4) 0.8915(4) 0.9146(2) 0.0225(10) Uani 1 1 d . . . . .
H2 H 0.4853 0.9150 0.9528 0.027 Uiso 1 1 calc R . . . .
C3 C 0.4659(4) 0.8805(4) 0.8436(2) 0.0197(10) Uani 1 1 d . . . . .
C4 C 0.3836(4) 0.8401(3) 0.7858(2) 0.0181(9) Uani 1 1 d . . . . .
C5 C 0.2609(4) 0.8135(4) 0.8010(2) 0.0213(10) Uani 1 1 d . . . . .
C6 C 0.2243(4) 0.8285(4) 0.8714(2) 0.0237(10) Uani 1 1 d . . . . .
H6 H 0.1428 0.8119 0.8806 0.028 Uiso 1 1 calc R . . . .
C7 C 0.1651(4) 0.7651(4) 0.7437(2) 0.0289(11) Uani 1 1 d . . . . .
C8 C 0.2645(4) 0.8878(4) 1.0034(2) 0.0210(10) Uani 1 1 d . . . . .
C9 C 0.5948(4) 0.9211(4) 0.8325(2) 0.0240(11) Uani 1 1 d . . . . .
C10 C 0.4301(4) 0.8245(4) 0.7116(2) 0.0211(10) Uani 1 1 d . . . . .
C11 C 0.5384(4) 0.7683(4) 0.7051(2) 0.0241(11) Uani 1 1 d . . . . .
H11 H 0.5795 0.7354 0.7463 0.029 Uiso 1 1 calc R . . . .
C12 C 0.5870(4) 0.7605(4) 0.6368(2) 0.0266(11) Uani 1 1 d . . . . .
C13 C 0.4193(4) 0.8541(4) 0.5802(2) 0.0251(11) Uani 1 1 d . . . . .
C14 C 0.3697(4) 0.8694(4) 0.6481(2) 0.0258(11) Uani 1 1 d . . . . .
H14 H 0.2969 0.9094 0.6506 0.031 Uiso 1 1 calc R . . . .
C15 C 0.7478(4) 0.6205(4) 0.6755(3) 0.0376(13) Uani 1 1 d . . . . .
H15 H 0.6944 0.5920 0.7080 0.045 Uiso 1 1 calc R . . . .
C16 C 0.8662(5) 0.5759(5) 0.6718(3) 0.0426(14) Uani 1 1 d . . . . .
H16 H 0.8875 0.5159 0.7011 0.051 Uiso 1 1 calc R . . . .
C17 C 0.9130(5) 0.6972(5) 0.5857(3) 0.0460(15) Uani 1 1 d . . . . .
H17 H 0.9687 0.7256 0.5545 0.055 Uiso 1 1 calc R . . . .
C18 C 0.7951(5) 0.7439(5) 0.5848(3) 0.0468(15) Uani 1 1 d . . . . .
H18 H 0.7733 0.8007 0.5527 0.056 Uiso 1 1 calc R . . . .
C19 C 0.7103(4) 0.7063(4) 0.6314(2) 0.0288(11) Uani 1 1 d . . . . .
C20 C 0.3509(4) 0.8945(4) 0.5105(2) 0.0291(11) Uani 1 1 d . . . . .
C21 C 0.4118(5) 0.9046(5) 0.4476(2) 0.0406(13) Uani 1 1 d . . . . .
H21 H 0.4959 0.8869 0.4481 0.049 Uiso 1 1 calc R . . . .
C22 C 0.3459(6) 0.9418(5) 0.3831(3) 0.0490(16) Uani 1 1 d . . . . .
H22 H 0.3889 0.9496 0.3413 0.059 Uiso 1 1 calc R . . . .
C23 C 0.1662(6) 0.9518(6) 0.4380(3) 0.072(2) Uani 1 1 d . . . . .
H23 H 0.0810 0.9662 0.4350 0.086 Uiso 1 1 calc R . . . .
C24 C 0.2241(5) 0.9160(6) 0.5053(3) 0.0569(18) Uani 1 1 d . . . . .
H24 H 0.1783 0.9068 0.5458 0.068 Uiso 1 1 calc R . . . .


_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 O1 2.255(3) . ?
Sm1 O3 2.479(3) 4_575 ?
Sm1 O4 2.465(3) 4_575 ?
Sm1 O8 2.384(3) . ?
Sm1 O7 2.409(3) . ?
Sm1 O5 2.517(3) 2_646 ?
Sm1 O6 2.469(3) 2_646 ?
Sm1 N3 2.646(4) 1_455 ?
Sm1 C8 2.841(4) 4_575 ?
Sm1 C9 2.810(4) 2_646 ?
O1 C7 1.245(5) . ?
O2 C7 1.232(5) . ?
O3 Sm1 2.479(3) 4_576 ?
O3 C8 1.282(5) . ?
O4 Sm1 2.465(3) 4_576 ?
O4 C8 1.246(5) . ?
O8 H8A 0.8545 . ?
O8 H8B 0.8577 . ?
O7 H7A 0.9145 . ?
O7 H7B 0.9115 . ?
O5 Sm1 2.517(3) 2_656 ?
O5 C9 1.242(5) . ?
O6 Sm1 2.469(3) 2_656 ?
O6 C9 1.278(5) . ?
N1 C12 1.348(5) . ?
N1 C13 1.354(6) . ?
N2 C22 1.326(8) . ?
N2 C23 1.325(8) . ?
N3 Sm1 2.646(4) 1_655 ?
N3 C16 1.333(6) . ?
N3 C17 1.347(6) . ?
C1 C2 1.389(5) . ?
C1 C6 1.392(5) . ?
C1 C8 1.496(5) . ?
C2 H2 0.9300 . ?
C2 C3 1.397(5) . ?
C3 C4 1.406(5) . ?
C3 C9 1.505(6) . ?
C4 C5 1.411(6) . ?
C4 C10 1.496(5) . ?
C5 C6 1.388(5) . ?
C5 C7 1.521(5) . ?
C6 H6 0.9300 . ?
C8 Sm1 2.841(4) 4_576 ?
C9 Sm1 2.810(4) 2_656 ?
C10 C11 1.371(6) . ?
C10 C14 1.391(5) . ?
C11 H11 0.9300 . ?
C11 C12 1.395(6) . ?
C12 C19 1.497(6) . ?
C13 C14 1.403(5) . ?
C13 C20 1.495(6) . ?
C14 H14 0.9300 . ?
C15 H15 0.9300 . ?
C15 C16 1.395(7) . ?
C15 C19 1.370(7) . ?
C16 H16 0.9300 . ?
C17 H17 0.9300 . ?
C17 C18 1.392(7) . ?
C18 H18 0.9300 . ?
C18 C19 1.382(7) . ?
C20 C21 1.375(6) . ?
C20 C24 1.385(7) . ?
C21 H21 0.9300 . ?
C21 C22 1.396(7) . ?
C22 H22 0.9300 . ?
C23 H23 0.9300 . ?
C23 C24 1.398(7) . ?
C24 H24 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
O1 Sm1 O3 97.64(11) . 4_575 ?
O1 Sm1 O4 93.22(12) . 4_575 ?
O1 Sm1 O8 151.79(11) . . ?
O1 Sm1 O7 87.89(12) . . ?
O1 Sm1 O5 82.32(11) . 2_646 ?
O1 Sm1 O6 134.81(10) . 2_646 ?
O1 Sm1 N3 77.27(11) . 1_455 ?
O1 Sm1 C8 98.10(12) . 4_575 ?
O1 Sm1 C9 108.00(13) . 2_646 ?
O3 Sm1 O5 125.70(10) 4_575 2_646 ?
O3 Sm1 N3 75.03(11) 4_575 1_455 ?
O3 Sm1 C8 26.80(10) 4_575 4_575 ?
O3 Sm1 C9 115.30(11) 4_575 2_646 ?
O4 Sm1 O3 52.57(9) 4_575 4_575 ?
O4 Sm1 O5 73.16(10) 4_575 2_646 ?
O4 Sm1 O6 74.48(11) 4_575 2_646 ?
O4 Sm1 N3 125.16(12) 4_575 1_455 ?
O4 Sm1 C8 25.93(10) 4_575 4_575 ?
O4 Sm1 C9 67.29(11) 4_575 2_646 ?
O8 Sm1 O3 80.71(11) . 4_575 ?
O8 Sm1 O4 107.27(11) . 4_575 ?
O8 Sm1 O7 82.66(11) . . ?
O8 Sm1 O5 121.64(11) . 2_646 ?
O8 Sm1 O6 70.96(10) . 2_646 ?
O8 Sm1 N3 75.10(12) . 1_455 ?
O8 Sm1 C8 92.77(11) . 4_575 ?
O8 Sm1 C9 97.89(13) . 2_646 ?
O7 Sm1 O3 154.25(10) . 4_575 ?
O7 Sm1 O4 152.61(11) . 4_575 ?
O7 Sm1 O5 79.90(11) . 2_646 ?
O7 Sm1 O6 85.40(12) . 2_646 ?
O7 Sm1 N3 81.78(12) . 1_455 ?
O7 Sm1 C8 173.75(13) . 4_575 ?
O7 Sm1 C9 86.34(12) . 2_646 ?
O5 Sm1 N3 152.95(10) 2_646 1_455 ?
O5 Sm1 C8 99.05(11) 2_646 4_575 ?
O5 Sm1 C9 26.22(11) 2_646 2_646 ?
O6 Sm1 O3 107.35(10) 2_646 4_575 ?
O6 Sm1 O5 52.51(10) 2_646 2_646 ?
O6 Sm1 N3 144.94(12) 2_646 1_455 ?
O6 Sm1 C8 89.09(12) 2_646 4_575 ?
O6 Sm1 C9 27.03(11) 2_646 2_646 ?
N3 Sm1 C8 101.22(12) 1_455 4_575 ?
N3 Sm1 C9 166.86(13) 1_455 2_646 ?
C9 Sm1 C8 90.09(12) 2_646 4_575 ?
C7 O1 Sm1 152.5(3) . . ?
C8 O3 Sm1 92.6(2) . 4_576 ?
C8 O4 Sm1 94.1(2) . 4_576 ?
Sm1 O8 H8A 109.2 . . ?
Sm1 O8 H8B 141.3 . . ?
H8A O8 H8B 108.3 . . ?
Sm1 O7 H7A 112.0 . . ?
Sm1 O7 H7B 112.2 . . ?
H7A O7 H7B 101.7 . . ?
C9 O5 Sm1 90.2(2) . 2_656 ?
C9 O6 Sm1 91.5(3) . 2_656 ?
C12 N1 C13 117.3(4) . . ?
C23 N2 C22 116.8(5) . . ?
C16 N3 Sm1 121.9(3) . 1_655 ?
C16 N3 C17 115.1(4) . . ?
C17 N3 Sm1 122.8(3) . 1_655 ?
C2 C1 C6 118.9(4) . . ?
C2 C1 C8 119.9(4) . . ?
C6 C1 C8 121.1(4) . . ?
C1 C2 H2 119.9 . . ?
C1 C2 C3 120.3(4) . . ?
C3 C2 H2 119.9 . . ?
C2 C3 C4 120.9(4) . . ?
C2 C3 C9 115.9(3) . . ?
C4 C3 C9 123.0(4) . . ?
C3 C4 C5 118.3(4) . . ?
C3 C4 C10 118.9(4) . . ?
C5 C4 C10 122.8(3) . . ?
C4 C5 C7 123.0(4) . . ?
C6 C5 C4 119.9(4) . . ?
C6 C5 C7 117.1(4) . . ?
C1 C6 H6 119.2 . . ?
C5 C6 C1 121.7(4) . . ?
C5 C6 H6 119.2 . . ?
O1 C7 C5 117.4(4) . . ?
O2 C7 O1 125.1(4) . . ?
O2 C7 C5 117.4(4) . . ?
O3 C8 Sm1 60.6(2) . 4_576 ?
O3 C8 C1 119.9(4) . . ?
O4 C8 Sm1 59.9(2) . 4_576 ?
O4 C8 O3 120.0(4) . . ?
O4 C8 C1 120.1(4) . . ?
C1 C8 Sm1 170.8(3) . 4_576 ?
O5 C9 Sm1 63.6(2) . 2_656 ?
O5 C9 O6 122.2(4) . . ?
O5 C9 C3 120.1(4) . . ?
O6 C9 Sm1 61.4(2) . 2_656 ?
O6 C9 C3 117.4(4) . . ?
C3 C9 Sm1 158.1(3) . 2_656 ?
C11 C10 C4 119.9(4) . . ?
C11 C10 C14 117.9(4) . . ?
C14 C10 C4 122.2(4) . . ?
C10 C11 H11 120.0 . . ?
C10 C11 C12 120.1(4) . . ?
C12 C11 H11 120.0 . . ?
N1 C12 C11 122.8(4) . . ?
N1 C12 C19 117.5(4) . . ?
C11 C12 C19 119.6(4) . . ?
N1 C13 C14 122.2(4) . . ?
N1 C13 C20 117.4(4) . . ?
C14 C13 C20 120.5(4) . . ?
C10 C14 C13 119.6(4) . . ?
C10 C14 H14 120.2 . . ?
C13 C14 H14 120.2 . . ?
C16 C15 H15 120.0 . . ?
C19 C15 H15 120.0 . . ?
C19 C15 C16 120.0(5) . . ?
N3 C16 C15 124.4(5) . . ?
N3 C16 H16 117.8 . . ?
C15 C16 H16 117.8 . . ?
N3 C17 H17 118.2 . . ?
N3 C17 C18 123.7(5) . . ?
C18 C17 H17 118.2 . . ?
C17 C18 H18 119.9 . . ?
C19 C18 C17 120.2(5) . . ?
C19 C18 H18 119.9 . . ?
C15 C19 C12 121.7(4) . . ?
C15 C19 C18 116.5(4) . . ?
C18 C19 C12 121.8(5) . . ?
C21 C20 C13 120.2(4) . . ?
C21 C20 C24 117.7(4) . . ?
C24 C20 C13 121.9(4) . . ?
C20 C21 H21 120.4 . . ?
C20 C21 C22 119.2(5) . . ?
C22 C21 H21 120.4 . . ?
N2 C22 C21 123.6(5) . . ?
N2 C22 H22 118.2 . . ?
C21 C22 H22 118.2 . . ?
N2 C23 H23 118.0 . . ?
N2 C23 C24 123.9(6) . . ?
C24 C23 H23 118.0 . . ?
C20 C24 C23 118.6(5) . . ?
C20 C24 H24 120.7 . . ?
C23 C24 H24 120.7 . . ?

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 H8B O3 0.86 1.83 2.681(4) 172.7 2_546
O7 H7A O2 0.91 1.87 2.746(5) 158.7 2_546

_smtbx_masks_special_details     ?
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 -0.180 -0.116 0.373 68.4 13.4 ?
2 0.180 0.116 0.627 68.4 13.8 ?
3 0.180 0.384 0.127 68.4 13.1 ?
4 -0.180 0.616 0.873 68.4 14.1 ?

_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_olex2_date_sample_data_collection 2018-12-06
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.503
_oxdiff_exptl_absorpt_empirical_full_min 0.683
####################################################################### 
# 
# 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_l71-gd_sq
_database_code_depnum_ccdc_archive 'CCDC 1961835'
loop_
_audit_author_name
_audit_author_address
'yapei shang'
;zhengzhou university
China
;
_audit_update_record             
;
2019-10-29 deposited with the CCDC.	2020-03-09 downloaded from the CCDC.
;
_audit_creation_date             2019-06-11
_audit_creation_method           
;
Olex2 1.2-alpha
(compiled 2018.07.26 svn.r3523 for OlexSys, GUI svn.r5532)
;
_shelx_SHELXL_version_number     2014/7
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C24 H17 Gd N3 O8'
_chemical_formula_sum            'C24 H17 Gd N3 O8'
_chemical_formula_weight         632.65
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C H N O Gd'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Gd Gd -0.1653 3.9035 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/c 1'
_space_group_name_Hall           '-P 2ybc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   10.7504(4)
_cell_length_b                   12.3081(7)
_cell_length_c                   18.1494(7)
_cell_angle_alpha                90
_cell_angle_beta                 95.071(4)
_cell_angle_gamma                90
_cell_volume                     2392.07(19)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    3518
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      26.9730
_cell_measurement_theta_min      3.8150
_shelx_estimated_absorpt_T_max   0.728
_shelx_estimated_absorpt_T_min   0.575
_exptl_absorpt_coefficient_mu    2.827
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.04416
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear light yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.757
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1240
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.12
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0586
_diffrn_reflns_av_unetI/netI     0.0983
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.836
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            10661
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.836
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.355
_diffrn_reflns_theta_min         3.493
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0584
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.836
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -74.00 -47.00   1.00   10.00    --  -13.80-178.00-180.00   27
  2  ω    -42.00  54.00   1.00   10.00    --  -13.80  19.00-150.00   96
  3  ω    -74.00  16.00   1.00   10.00    --  -13.80 -19.00   0.00   90
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Single source at offset/far, EosS2'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0488167000
_diffrn_orient_matrix_UB_12      0.0129132000
_diffrn_orient_matrix_UB_13      -0.0274433000
_diffrn_orient_matrix_UB_21      -0.0301747000
_diffrn_orient_matrix_UB_22      0.0305461000
_diffrn_orient_matrix_UB_23      0.0263880000
_diffrn_orient_matrix_UB_31      0.0330638000
_diffrn_orient_matrix_UB_32      0.0471347000
_diffrn_orient_matrix_UB_33      -0.0094860000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3737
_reflns_number_total             5001
_reflns_odcompleteness_completeness 99.67
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     25.30
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_refine_diff_density_max         1.261
_refine_diff_density_min         -1.999
_refine_diff_density_rms         0.171
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     327
_refine_ls_number_reflns         5001
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0731
_refine_ls_R_factor_gt           0.0508
_refine_ls_restrained_S_all      1.030
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0283P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0887
_refine_ls_wR_factor_ref         0.0994
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
 At 1.5 times of:
  All O(H,H) groups
2.a Rotating group:
 O7(H7A,H7B), O8(H8A,H8B)
2.b Aromatic/amide H refined with riding coordinates:
 N1(H1), C2(H2), C4(H4), C14(H14), C11(H11), C24(H24), C23(H23), C22(H22),
 C21(H21), C16(H16), C17(H17), C18(H18), C19(H19)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Gd1 Gd 0.81752(2) 0.53820(2) 0.36165(2) 0.01936(11) Uani 1 1 d . . . . .
O1 O 0.7957(4) 0.6950(4) 0.2986(2) 0.0336(11) Uani 1 1 d . . . . .
O2 O 0.9429(4) 0.7944(5) 0.2561(3) 0.075(2) Uani 1 1 d . . . . .
O3 O 0.8521(4) 0.8855(4) -0.0134(2) 0.0308(11) Uani 1 1 d . . . . .
O4 O 0.6584(4) 0.9112(4) -0.0567(2) 0.0369(12) Uani 1 1 d . . . . .
O5 O 0.3892(4) 1.0007(4) 0.2063(2) 0.0319(11) Uani 1 1 d . . . . .
O6 O 0.3115(4) 0.8767(4) 0.1286(2) 0.0349(11) Uani 1 1 d . . . . .
O7 O 0.9424(4) 0.3996(4) 0.4186(2) 0.0373(12) Uani 1 1 d . . . . .
H7A H 0.9084 0.3383 0.4080 0.056 Uiso 1 1 d GR . . . .
H7B H 0.9419 0.4047 0.4654 0.056 Uiso 1 1 d GR . . . .
O8 O 0.8839(4) 0.4573(4) 0.2530(2) 0.0389(12) Uani 1 1 d . . . . .
H8A H 0.8223 0.4540 0.2194 0.058 Uiso 1 1 d GR . . . .
H8B H 0.9030 0.3903 0.2617 0.058 Uiso 1 1 d GR . . . .
N1 N 0.4697(5) 0.8028(4) 0.4245(3) 0.0324(13) Uani 1 1 d . . . . .
H1 H 0.4376 0.7981 0.4661 0.039 Uiso 1 1 calc R . . . .
N2 N 0.0456(5) 0.6136(4) 0.3703(3) 0.0304(13) Uani 1 1 d . . . . .
N3 N 0.7752(7) 0.9676(5) 0.6228(3) 0.0557(19) Uani 1 1 d . . . . .
C8 C 0.7359(5) 0.8872(5) -0.0037(3) 0.0207(13) Uani 1 1 d . . . . .
C7 C 0.8341(6) 0.7648(5) 0.2564(3) 0.0282(15) Uani 1 1 d . . . . .
C1 C 0.7381(5) 0.8141(5) 0.1995(3) 0.0224(14) Uani 1 1 d . . . . .
C2 C 0.7752(5) 0.8294(5) 0.1287(3) 0.0217(14) Uani 1 1 d . . . . .
H2 H 0.8568 0.8132 0.1194 0.026 Uiso 1 1 calc R . . . .
C3 C 0.6929(5) 0.8684(4) 0.0718(3) 0.0180(13) Uani 1 1 d . . . . .
C4 C 0.5705(5) 0.8908(5) 0.0846(3) 0.0243(14) Uani 1 1 d . . . . .
H4 H 0.5139 0.9133 0.0459 0.029 Uiso 1 1 calc R . . . .
C5 C 0.5323(5) 0.8797(5) 0.1555(3) 0.0196(13) Uani 1 1 d . . . . .
C6 C 0.6156(5) 0.8399(5) 0.2141(3) 0.0183(13) Uani 1 1 d . . . . .
C10 C 0.5681(5) 0.8248(5) 0.2884(3) 0.0222(14) Uani 1 1 d . . . . .
C14 C 0.4596(5) 0.7679(5) 0.2952(3) 0.0271(15) Uani 1 1 d . . . . .
H14 H 0.4184 0.7347 0.2540 0.033 Uiso 1 1 calc R . . . .
C13 C 0.4117(5) 0.7602(5) 0.3631(3) 0.0262(15) Uani 1 1 d . . . . .
C9 C 0.4043(6) 0.9209(5) 0.1668(3) 0.0247(15) Uani 1 1 d . . . . .
C12 C 0.5806(5) 0.8536(5) 0.4196(3) 0.0247(15) Uani 1 1 d . . . . .
C11 C 0.6289(5) 0.8688(5) 0.3519(3) 0.0270(15) Uani 1 1 d . . . . .
H11 H 0.7019 0.9086 0.3492 0.032 Uiso 1 1 calc R . . . .
C20 C 0.2883(6) 0.7058(6) 0.3690(3) 0.0312(16) Uani 1 1 d . . . . .
C24 C 0.2512(6) 0.6210(6) 0.3247(4) 0.0379(17) Uani 1 1 d . . . . .
H24 H 0.3053 0.5926 0.2924 0.046 Uiso 1 1 calc R . . . .
C23 C 0.1325(7) 0.5760(6) 0.3273(4) 0.047(2) Uani 1 1 d . . . . .
H23 H 0.1118 0.5162 0.2973 0.056 Uiso 1 1 calc R . . . .
C22 C 0.0850(6) 0.6977(6) 0.4135(4) 0.046(2) Uani 1 1 d . . . . .
H22 H 0.0294 0.7266 0.4448 0.055 Uiso 1 1 calc R . . . .
C21 C 0.2024(7) 0.7446(6) 0.4148(4) 0.050(2) Uani 1 1 d . . . . .
H21 H 0.2233 0.8023 0.4466 0.060 Uiso 1 1 calc R . . . .
C15 C 0.6466(6) 0.8940(5) 0.4902(3) 0.0315(16) Uani 1 1 d . . . . .
C16 C 0.7734(7) 0.9168(7) 0.4948(4) 0.055(2) Uani 1 1 d . . . . .
H16 H 0.8186 0.9084 0.4538 0.066 Uiso 1 1 calc R . . . .
C17 C 0.8321(8) 0.9524(7) 0.5622(4) 0.065(3) Uani 1 1 d . . . . .
H17 H 0.9174 0.9665 0.5644 0.077 Uiso 1 1 calc R . . . .
C18 C 0.6545(8) 0.9418(6) 0.6179(4) 0.053(2) Uani 1 1 d . . . . .
H18 H 0.6122 0.9489 0.6602 0.063 Uiso 1 1 calc R . . . .
C19 C 0.5873(7) 0.9049(6) 0.5536(3) 0.0394(18) Uani 1 1 d . . . . .
H19 H 0.5031 0.8877 0.5537 0.047 Uiso 1 1 calc R . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Gd1 O1 2.245(4) . ?
Gd1 O3 2.452(4) 4_576 ?
Gd1 O4 2.441(4) 4_576 ?
Gd1 O5 2.488(4) 2_645 ?
Gd1 O6 2.439(4) 2_645 ?
Gd1 O7 2.353(4) . ?
Gd1 O8 2.374(4) . ?
Gd1 N2 2.613(5) 1_655 ?
Gd1 C8 2.822(6) 4_576 ?
Gd1 C9 2.797(6) 2_645 ?
O1 C7 1.246(7) . ?
O2 C7 1.225(7) . ?
O3 Gd1 2.452(4) 4_575 ?
O3 C8 1.276(6) . ?
O4 Gd1 2.441(4) 4_575 ?
O4 C8 1.251(6) . ?
O5 Gd1 2.487(4) 2_655 ?
O5 C9 1.237(7) . ?
O6 Gd1 2.439(4) 2_655 ?
O6 C9 1.284(7) . ?
O7 H7A 0.8523 . ?
O7 H7B 0.8529 . ?
O8 H8A 0.8610 . ?
O8 H8B 0.8617 . ?
N1 H1 0.8600 . ?
N1 C13 1.335(7) . ?
N1 C12 1.357(7) . ?
N2 Gd1 2.613(5) 1_455 ?
N2 C23 1.351(8) . ?
N2 C22 1.345(8) . ?
N3 C17 1.319(10) . ?
N3 C18 1.332(10) . ?
C8 Gd1 2.822(6) 4_575 ?
C8 C3 1.503(7) . ?
C7 C1 1.521(7) . ?
C1 C2 1.391(8) . ?
C1 C6 1.403(8) . ?
C2 H2 0.9300 . ?
C2 C3 1.385(7) . ?
C3 C4 1.384(7) . ?
C4 H4 0.9300 . ?
C4 C5 1.392(7) . ?
C5 C6 1.414(7) . ?
C5 C9 1.497(8) . ?
C6 C10 1.497(7) . ?
C10 C14 1.375(8) . ?
C10 C11 1.384(7) . ?
C14 H14 0.9300 . ?
C14 C13 1.380(8) . ?
C13 C20 1.498(8) . ?
C9 Gd1 2.797(6) 2_655 ?
C12 C11 1.388(8) . ?
C12 C15 1.494(8) . ?
C11 H11 0.9300 . ?
C20 C24 1.355(8) . ?
C20 C21 1.381(9) . ?
C24 H24 0.9300 . ?
C24 C23 1.396(9) . ?
C23 H23 0.9300 . ?
C22 H22 0.9300 . ?
C22 C21 1.386(9) . ?
C21 H21 0.9300 . ?
C15 C16 1.388(9) . ?
C15 C19 1.369(8) . ?
C16 H16 0.9300 . ?
C16 C17 1.396(9) . ?
C17 H17 0.9300 . ?
C18 H18 0.9300 . ?
C18 C19 1.393(9) . ?
C19 H19 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
O1 Gd1 O3 98.21(15) . 4_576 ?
O1 Gd1 O4 92.44(16) . 4_576 ?
O1 Gd1 O5 81.82(15) . 2_645 ?
O1 Gd1 O6 134.66(14) . 2_645 ?
O1 Gd1 O7 151.29(15) . . ?
O1 Gd1 O8 87.86(15) . . ?
O1 Gd1 N2 77.33(15) . 1_655 ?
O1 Gd1 C8 97.76(16) . 4_576 ?
O1 Gd1 C9 107.50(17) . 2_645 ?
O3 Gd1 O5 125.83(14) 4_576 2_645 ?
O3 Gd1 N2 75.17(15) 4_576 1_655 ?
O3 Gd1 C8 26.85(13) 4_576 4_576 ?
O3 Gd1 C9 115.17(15) 4_576 2_645 ?
O4 Gd1 O3 52.97(13) 4_576 4_576 ?
O4 Gd1 O5 72.87(13) 4_576 2_645 ?
O4 Gd1 N2 125.24(16) 4_576 1_655 ?
O4 Gd1 C8 26.24(13) 4_576 4_576 ?
O4 Gd1 C9 67.17(15) 4_576 2_645 ?
O5 Gd1 N2 152.59(15) 2_645 1_655 ?
O5 Gd1 C8 99.07(15) 2_645 4_576 ?
O5 Gd1 C9 26.24(15) 2_645 2_645 ?
O6 Gd1 O3 106.56(14) 2_645 4_576 ?
O6 Gd1 O4 74.35(15) 2_645 4_576 ?
O6 Gd1 O5 52.87(14) 2_645 2_645 ?
O6 Gd1 N2 145.25(15) 2_645 1_655 ?
O6 Gd1 C8 88.84(16) 2_645 4_576 ?
O6 Gd1 C9 27.32(15) 2_645 2_645 ?
O7 Gd1 O3 80.65(15) . 4_576 ?
O7 Gd1 O4 108.77(15) . 4_576 ?
O7 Gd1 O5 122.23(15) . 2_645 ?
O7 Gd1 O6 71.53(14) . 2_645 ?
O7 Gd1 O8 81.89(16) . . ?
O7 Gd1 N2 74.65(15) . 1_655 ?
O7 Gd1 C8 93.71(16) . 4_576 ?
O7 Gd1 C9 98.67(17) . 2_645 ?
O8 Gd1 O3 153.70(14) . 4_576 ?
O8 Gd1 O4 152.81(14) . 4_576 ?
O8 Gd1 O5 80.28(15) . 2_645 ?
O8 Gd1 O6 86.19(15) . 2_645 ?
O8 Gd1 N2 81.33(16) . 1_655 ?
O8 Gd1 C8 174.21(16) . 4_576 ?
O8 Gd1 C9 86.81(16) . 2_645 ?
N2 Gd1 C8 101.20(17) 1_655 4_576 ?
N2 Gd1 C9 167.07(17) 1_655 2_645 ?
C9 Gd1 C8 90.15(16) 2_645 4_576 ?
C7 O1 Gd1 151.7(4) . . ?
C8 O3 Gd1 92.9(3) . 4_575 ?
C8 O4 Gd1 94.1(3) . 4_575 ?
C9 O5 Gd1 91.0(3) . 2_655 ?
C9 O6 Gd1 92.1(4) . 2_655 ?
Gd1 O7 H7A 109.1 . . ?
Gd1 O7 H7B 109.3 . . ?
H7A O7 H7B 104.4 . . ?
Gd1 O8 H8A 109.9 . . ?
Gd1 O8 H8B 109.5 . . ?
H8A O8 H8B 103.9 . . ?
C13 N1 H1 120.8 . . ?
C13 N1 C12 118.3(5) . . ?
C12 N1 H1 120.8 . . ?
C23 N2 Gd1 122.5(4) . 1_455 ?
C22 N2 Gd1 123.6(4) . 1_455 ?
C22 N2 C23 113.7(6) . . ?
C17 N3 C18 115.6(7) . . ?
O3 C8 Gd1 60.2(3) . 4_575 ?
O3 C8 C3 120.5(5) . . ?
O4 C8 Gd1 59.6(3) . 4_575 ?
O4 C8 O3 119.4(5) . . ?
O4 C8 C3 120.0(5) . . ?
C3 C8 Gd1 169.8(4) . 4_575 ?
O1 C7 C1 116.8(5) . . ?
O2 C7 O1 125.2(6) . . ?
O2 C7 C1 118.0(6) . . ?
C2 C1 C7 116.7(5) . . ?
C2 C1 C6 119.6(5) . . ?
C6 C1 C7 123.7(5) . . ?
C1 C2 H2 119.3 . . ?
C3 C2 C1 121.3(5) . . ?
C3 C2 H2 119.3 . . ?
C2 C3 C8 120.4(5) . . ?
C4 C3 C8 119.8(5) . . ?
C4 C3 C2 119.8(5) . . ?
C3 C4 H4 120.0 . . ?
C3 C4 C5 119.9(5) . . ?
C5 C4 H4 120.0 . . ?
C4 C5 C6 120.6(5) . . ?
C4 C5 C9 116.3(5) . . ?
C6 C5 C9 122.9(5) . . ?
C1 C6 C5 118.6(5) . . ?
C1 C6 C10 122.9(5) . . ?
C5 C6 C10 118.5(5) . . ?
C14 C10 C6 120.3(5) . . ?
C14 C10 C11 117.9(5) . . ?
C11 C10 C6 121.9(5) . . ?
C10 C14 H14 119.9 . . ?
C10 C14 C13 120.1(6) . . ?
C13 C14 H14 119.9 . . ?
N1 C13 C14 122.3(5) . . ?
N1 C13 C20 117.8(5) . . ?
C14 C13 C20 119.9(5) . . ?
O5 C9 Gd1 62.8(3) . 2_655 ?
O5 C9 O6 120.9(6) . . ?
O5 C9 C5 121.2(5) . . ?
O6 C9 Gd1 60.6(3) . 2_655 ?
O6 C9 C5 117.6(6) . . ?
C5 C9 Gd1 158.2(4) . 2_655 ?
N1 C12 C11 121.3(5) . . ?
N1 C12 C15 116.7(5) . . ?
C11 C12 C15 121.9(5) . . ?
C10 C11 C12 119.8(6) . . ?
C10 C11 H11 120.1 . . ?
C12 C11 H11 120.1 . . ?
C24 C20 C13 121.2(6) . . ?
C24 C20 C21 116.4(6) . . ?
C21 C20 C13 122.2(6) . . ?
C20 C24 H24 119.7 . . ?
C20 C24 C23 120.5(7) . . ?
C23 C24 H24 119.7 . . ?
N2 C23 C24 124.4(7) . . ?
N2 C23 H23 117.8 . . ?
C24 C23 H23 117.8 . . ?
N2 C22 H22 117.6 . . ?
N2 C22 C21 124.8(7) . . ?
C21 C22 H22 117.6 . . ?
C20 C21 C22 120.2(7) . . ?
C20 C21 H21 119.9 . . ?
C22 C21 H21 119.9 . . ?
C16 C15 C12 120.5(6) . . ?
C19 C15 C12 122.2(6) . . ?
C19 C15 C16 117.2(6) . . ?
C15 C16 H16 120.6 . . ?
C15 C16 C17 118.8(7) . . ?
C17 C16 H16 120.6 . . ?
N3 C17 C16 124.7(8) . . ?
N3 C17 H17 117.7 . . ?
C16 C17 H17 117.7 . . ?
N3 C18 H18 117.9 . . ?
N3 C18 C19 124.3(7) . . ?
C19 C18 H18 117.9 . . ?
C15 C19 C18 119.4(7) . . ?
C15 C19 H19 120.3 . . ?
C18 C19 H19 120.3 . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O7 H7B O3 0.85 2.32 2.683(5) 106.1 2_745
O8 H8B O2 0.86 2.08 2.752(7) 134.0 2_745

_smtbx_masks_special_details     ?
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 -0.175 0.117 0.373 67.8 14.7 ?
2 0.175 -0.117 0.627 67.8 13.5 ?
3 -0.175 0.383 0.873 67.8 13.8 ?
4 0.175 0.617 0.127 67.8 14.4 ?

_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_olex2_date_sample_data_collection 2018-12-16
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 9.405
_oxdiff_exptl_absorpt_empirical_full_min 0.400
####################################################################### 
# 
# 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_l71-tb_sq
_database_code_depnum_ccdc_archive 'CCDC 1961833'
loop_
_audit_author_name
_audit_author_address
'yapei shang'
;zhengzhou university
China
;
_audit_update_record             
;
2019-10-29 deposited with the CCDC.	2020-03-09 downloaded from the CCDC.
;
_audit_creation_date             2019-06-17
_audit_creation_method           
;
Olex2 1.2-alpha
(compiled 2018.07.26 svn.r3523 for OlexSys, GUI svn.r5532)
;
_shelx_SHELXL_version_number     2014/7
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C24 H16 N3 O8 Tb'
_chemical_formula_sum            'C24 H16 N3 O8 Tb'
_chemical_formula_weight         633.32
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C H N O Tb'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Tb Tb -0.1723 4.1537 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/c 1'
_space_group_name_Hall           '-P 2ybc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   10.6848(5)
_cell_length_b                   12.2007(8)
_cell_length_c                   18.0868(9)
_cell_angle_alpha                90
_cell_angle_beta                 95.351(4)
_cell_angle_gamma                90
_cell_volume                     2347.6(2)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    3174
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.0260
_cell_measurement_theta_min      3.8390
_shelx_estimated_absorpt_T_max   0.608
_shelx_estimated_absorpt_T_min   0.526
_exptl_absorpt_coefficient_mu    3.068
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.55044
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear light yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.792
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1240
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.18
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0558
_diffrn_reflns_av_unetI/netI     0.1030
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.841
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            11014
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.841
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.339
_diffrn_reflns_theta_min         3.281
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0584
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.841
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -77.00  12.00   1.00   30.00    --  -13.80 -77.00 -60.00   89
  2  ω     -8.00  24.00   1.00   30.00    --  -13.80 -99.00-150.00   32
  3  ω    -49.00  29.00   1.00   30.00    --   14.74 -57.00  60.00   78
  4  ω     11.00  36.00   1.00   30.00    --   14.74  19.00-150.00   25
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Single source at offset/far, EosS2'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0235621000
_diffrn_orient_matrix_UB_12      -0.0544513000
_diffrn_orient_matrix_UB_13      -0.0016654000
_diffrn_orient_matrix_UB_21      -0.0547531000
_diffrn_orient_matrix_UB_22      0.0181621000
_diffrn_orient_matrix_UB_23      -0.0217074000
_diffrn_orient_matrix_UB_31      0.0299510000
_diffrn_orient_matrix_UB_32      -0.0094246000
_diffrn_orient_matrix_UB_33      -0.0327753000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3570
_reflns_number_total             4931
_reflns_odcompleteness_completeness 99.65
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     25.30
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_refine_diff_density_max         1.383
_refine_diff_density_min         -1.146
_refine_diff_density_rms         0.170
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.018
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     327
_refine_ls_number_reflns         4931
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0893
_refine_ls_R_factor_gt           0.0568
_refine_ls_restrained_S_all      1.018
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0306P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0886
_refine_ls_wR_factor_ref         0.0974
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H,H) groups
2.a Rotating group:
 O7(H7A,H7B), O8(H8A,H8B)
2.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C4(H4), C11(H11), C14(H14), C16(H16), C17(H17), C18(H18), C19(H19),
 C21(H21), C22(H22), C23(H23), C24(H24)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Tb1 Tb 0.18267(3) 0.53642(3) 0.63849(2) 0.01814(11) Uani 1 1 d . . . . .
O1 O 0.2043(4) 0.6924(4) 0.7018(3) 0.0304(13) Uani 1 1 d . . . . .
O2 O 0.0534(5) 0.7900(6) 0.7446(4) 0.078(2) Uani 1 1 d . . . . .
O3 O 0.1457(4) 0.8862(5) 1.0139(2) 0.0312(13) Uani 1 1 d . . . . .
O4 O 0.3410(4) 0.9110(5) 1.0577(3) 0.0364(14) Uani 1 1 d . . . . .
O5 O 0.6888(4) 0.8749(4) 0.8726(3) 0.0320(13) Uani 1 1 d . . . . .
O6 O 0.6105(4) 0.9987(4) 0.7942(2) 0.0283(12) Uani 1 1 d . . . . .
O7 O 0.1186(5) 0.4509(5) 0.7455(2) 0.0373(14) Uani 1 1 d . . . . .
H7A H 0.0972 0.4834 0.7841 0.056 Uiso 1 1 d GR . . . .
H7B H 0.1843 0.4303 0.7742 0.056 Uiso 1 1 d GR . . . .
O8 O 0.0590(4) 0.3981(4) 0.5801(3) 0.0367(13) Uani 1 1 d . . . . .
H8A H 0.0777 0.3373 0.6015 0.055 Uiso 1 1 d GR . . . .
H8B H 0.0790 0.3895 0.5360 0.055 Uiso 1 1 d GR . . . .
N1 N 0.5295(5) 0.8007(5) 0.5758(3) 0.0305(16) Uani 1 1 d . . . . .
N2 N 0.9560(5) 0.6101(5) 0.6308(3) 0.0297(15) Uani 1 1 d . . . . .
N3 N 0.2279(8) 0.9692(7) 0.3761(4) 0.059(2) Uani 1 1 d . . . . .
C1 C 0.2608(6) 0.8131(6) 0.8008(4) 0.0207(16) Uani 1 1 d . . . . .
C2 C 0.2231(6) 0.8277(5) 0.8714(4) 0.0206(16) Uani 1 1 d . . . . .
H2 H 0.1408 0.8109 0.8801 0.025 Uiso 1 1 calc R . . . .
C3 C 0.3047(6) 0.8667(5) 0.9291(3) 0.0171(15) Uani 1 1 d . . . . .
C4 C 0.4272(6) 0.8892(6) 0.9157(3) 0.0216(16) Uani 1 1 d . . . . .
H4 H 0.4842 0.9126 0.9545 0.026 Uiso 1 1 calc R . . . .
C5 C 0.4659(6) 0.8774(6) 0.8456(4) 0.0188(15) Uani 1 1 d . . . . .
C6 C 0.3832(6) 0.8386(5) 0.7864(3) 0.0184(15) Uani 1 1 d . . . . .
C7 C 0.1645(7) 0.7623(7) 0.7439(4) 0.0321(19) Uani 1 1 d . . . . .
C8 C 0.2630(6) 0.8883(6) 1.0042(4) 0.0212(16) Uani 1 1 d . . . . .
C9 C 0.5964(6) 0.9182(6) 0.8353(4) 0.0222(17) Uani 1 1 d . . . . .
C10 C 0.4296(6) 0.8237(6) 0.7121(3) 0.0235(17) Uani 1 1 d . . . . .
C11 C 0.5386(6) 0.7661(6) 0.7049(4) 0.0251(17) Uani 1 1 d . . . . .
H11 H 0.5801 0.7327 0.7465 0.030 Uiso 1 1 calc R . . . .
C12 C 0.5872(6) 0.7569(6) 0.6371(4) 0.0226(17) Uani 1 1 d . . . . .
C13 C 0.4181(6) 0.8539(6) 0.5796(4) 0.0253(18) Uani 1 1 d . . . . .
C14 C 0.3697(6) 0.8690(6) 0.6479(3) 0.0243(18) Uani 1 1 d . . . . .
H14 H 0.2967 0.9098 0.6504 0.029 Uiso 1 1 calc R . . . .
C15 C 0.7108(7) 0.7026(7) 0.6322(4) 0.0301(19) Uani 1 1 d . . . . .
C16 C 0.7501(7) 0.6204(7) 0.6781(4) 0.036(2) Uani 1 1 d . . . . .
H16 H 0.6977 0.5937 0.7122 0.043 Uiso 1 1 calc R . . . .
C17 C 0.8704(7) 0.5746(7) 0.6746(5) 0.041(2) Uani 1 1 d . . . . .
H17 H 0.8919 0.5150 0.7052 0.050 Uiso 1 1 calc R . . . .
C18 C 0.9136(8) 0.6938(8) 0.5870(5) 0.053(3) Uani 1 1 d . . . . .
H18 H 0.9690 0.7234 0.5557 0.063 Uiso 1 1 calc R . . . .
C19 C 0.7947(8) 0.7399(8) 0.5844(4) 0.052(3) Uani 1 1 d . . . . .
H19 H 0.7716 0.7955 0.5507 0.062 Uiso 1 1 calc R . . . .
C20 C 0.3539(7) 0.8943(7) 0.5108(4) 0.0319(19) Uani 1 1 d . . . . .
C21 C 0.4137(7) 0.9037(6) 0.4466(4) 0.0336(19) Uani 1 1 d . . . . .
H21 H 0.4979 0.8840 0.4469 0.040 Uiso 1 1 calc R . . . .
C22 C 0.3494(9) 0.9423(7) 0.3817(4) 0.045(2) Uani 1 1 d . . . . .
H22 H 0.3932 0.9499 0.3399 0.054 Uiso 1 1 calc R . . . .
C23 C 0.1698(9) 0.9578(9) 0.4366(5) 0.070(3) Uani 1 1 d . . . . .
H23 H 0.0848 0.9751 0.4340 0.084 Uiso 1 1 calc R . . . .
C24 C 0.2276(8) 0.9213(8) 0.5043(5) 0.058(3) Uani 1 1 d . . . . .
H24 H 0.1813 0.9152 0.5451 0.069 Uiso 1 1 calc R . . . .


_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 O1 2.222(5) . ?
Tb1 O3 2.441(4) 4_575 ?
Tb1 O4 2.423(4) 4_575 ?
Tb1 O5 2.422(5) 2_646 ?
Tb1 O6 2.465(5) 2_646 ?
Tb1 O7 2.356(4) . ?
Tb1 O8 2.334(5) . ?
Tb1 N2 2.575(6) 1_455 ?
Tb1 C8 2.805(6) 4_575 ?
Tb1 C9 2.769(7) 2_646 ?
O1 C7 1.244(8) . ?
O2 C7 1.235(8) . ?
O3 Tb1 2.441(4) 4_576 ?
O3 C8 1.282(7) . ?
O4 Tb1 2.423(4) 4_576 ?
O4 C8 1.248(8) . ?
O5 Tb1 2.422(5) 2_656 ?
O5 C9 1.258(8) . ?
O6 Tb1 2.465(5) 2_656 ?
O6 C9 1.250(8) . ?
O7 H7A 0.8521 . ?
O7 H7B 0.8706 . ?
O8 H8A 0.8518 . ?
O8 H8B 0.8517 . ?
N1 C12 1.330(8) . ?
N1 C13 1.363(8) . ?
N2 Tb1 2.575(6) 1_655 ?
N2 C17 1.337(9) . ?
N2 C18 1.345(10) . ?
N3 C22 1.334(10) . ?
N3 C23 1.315(10) . ?
C1 C2 1.386(8) . ?
C1 C6 1.392(8) . ?
C1 C7 1.518(9) . ?
C2 H2 0.9300 . ?
C2 C3 1.380(9) . ?
C3 C4 1.381(8) . ?
C3 C8 1.492(8) . ?
C4 H4 0.9300 . ?
C4 C5 1.377(8) . ?
C5 C6 1.406(9) . ?
C5 C9 1.509(8) . ?
C6 C10 1.486(8) . ?
C8 Tb1 2.805(6) 4_576 ?
C9 Tb1 2.769(7) 2_656 ?
C10 C11 1.377(9) . ?
C10 C14 1.387(9) . ?
C11 H11 0.9300 . ?
C11 C12 1.381(8) . ?
C12 C15 1.488(9) . ?
C13 C14 1.395(8) . ?
C13 C20 1.451(9) . ?
C14 H14 0.9300 . ?
C15 C16 1.344(10) . ?
C15 C19 1.379(9) . ?
C16 H16 0.9300 . ?
C16 C17 1.408(10) . ?
C17 H17 0.9300 . ?
C18 H18 0.9300 . ?
C18 C19 1.386(10) . ?
C19 H19 0.9300 . ?
C20 C21 1.382(9) . ?
C20 C24 1.383(10) . ?
C21 H21 0.9300 . ?
C21 C22 1.386(10) . ?
C22 H22 0.9300 . ?
C23 H23 0.9300 . ?
C23 C24 1.391(11) . ?
C24 H24 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
O1 Tb1 O3 98.34(18) . 4_575 ?
O1 Tb1 O4 92.22(18) . 4_575 ?
O1 Tb1 O5 135.00(17) . 2_646 ?
O1 Tb1 O6 81.93(17) . 2_646 ?
O1 Tb1 O7 88.87(18) . . ?
O1 Tb1 O8 151.62(17) . . ?
O1 Tb1 N2 77.36(18) . 1_455 ?
O1 Tb1 C8 98.08(19) . 4_575 ?
O1 Tb1 C9 108.2(2) . 2_646 ?
O3 Tb1 O6 126.05(14) 4_575 2_646 ?
O3 Tb1 N2 75.22(17) 4_575 1_455 ?
O3 Tb1 C8 27.16(16) 4_575 4_575 ?
O3 Tb1 C9 114.90(17) 4_575 2_646 ?
O4 Tb1 O3 53.33(15) 4_575 4_575 ?
O4 Tb1 O6 72.72(15) 4_575 2_646 ?
O4 Tb1 N2 125.53(18) 4_575 1_455 ?
O4 Tb1 C8 26.34(16) 4_575 4_575 ?
O4 Tb1 C9 66.99(18) 4_575 2_646 ?
O5 Tb1 O3 106.40(17) 2_646 4_575 ?
O5 Tb1 O4 74.48(17) 2_646 4_575 ?
O5 Tb1 O6 53.11(16) 2_646 2_646 ?
O5 Tb1 N2 144.85(18) 2_646 1_455 ?
O5 Tb1 C8 88.45(18) 2_646 4_575 ?
O5 Tb1 C9 27.01(18) 2_646 2_646 ?
O6 Tb1 N2 152.52(17) 2_646 1_455 ?
O6 Tb1 C8 98.98(18) 2_646 4_575 ?
O6 Tb1 C9 26.84(17) 2_646 2_646 ?
O7 Tb1 O3 153.53(16) . 4_575 ?
O7 Tb1 O4 152.31(17) . 4_575 ?
O7 Tb1 O5 85.29(18) . 2_646 ?
O7 Tb1 O6 80.06(16) . 2_646 ?
O7 Tb1 N2 81.66(19) . 1_455 ?
O7 Tb1 C8 172.8(2) . 4_575 ?
O7 Tb1 C9 86.40(18) . 2_646 ?
O8 Tb1 O3 79.97(18) . 4_575 ?
O8 Tb1 O4 108.44(18) . 4_575 ?
O8 Tb1 O5 71.06(16) . 2_646 ?
O8 Tb1 O6 122.15(17) . 2_646 ?
O8 Tb1 O7 81.71(18) . . ?
O8 Tb1 N2 74.83(19) . 1_455 ?
O8 Tb1 C8 92.91(19) . 4_575 ?
O8 Tb1 C9 97.9(2) . 2_646 ?
N2 Tb1 C8 101.6(2) 1_455 4_575 ?
N2 Tb1 C9 166.8(2) 1_455 2_646 ?
C9 Tb1 C8 89.64(19) 2_646 4_575 ?
C7 O1 Tb1 151.3(5) . . ?
C8 O3 Tb1 92.5(4) . 4_576 ?
C8 O4 Tb1 94.2(4) . 4_576 ?
C9 O5 Tb1 92.1(4) . 2_656 ?
C9 O6 Tb1 90.3(4) . 2_656 ?
Tb1 O7 H7A 126.0 . . ?
Tb1 O7 H7B 109.7 . . ?
H7A O7 H7B 84.7 . . ?
Tb1 O8 H8A 109.0 . . ?
Tb1 O8 H8B 109.4 . . ?
H8A O8 H8B 104.4 . . ?
C12 N1 C13 119.1(6) . . ?
C17 N2 Tb1 123.2(5) . 1_655 ?
C17 N2 C18 112.5(7) . . ?
C18 N2 Tb1 124.1(5) . 1_655 ?
C23 N3 C22 116.2(8) . . ?
C2 C1 C6 120.2(6) . . ?
C2 C1 C7 116.1(6) . . ?
C6 C1 C7 123.6(6) . . ?
C1 C2 H2 119.2 . . ?
C3 C2 C1 121.5(6) . . ?
C3 C2 H2 119.2 . . ?
C2 C3 C4 118.6(6) . . ?
C2 C3 C8 121.9(6) . . ?
C4 C3 C8 119.5(6) . . ?
C3 C4 H4 119.6 . . ?
C5 C4 C3 120.7(6) . . ?
C5 C4 H4 119.6 . . ?
C4 C5 C6 121.0(6) . . ?
C4 C5 C9 116.1(6) . . ?
C6 C5 C9 122.6(6) . . ?
C1 C6 C5 117.8(6) . . ?
C1 C6 C10 122.7(6) . . ?
C5 C6 C10 119.4(6) . . ?
O1 C7 C1 116.5(6) . . ?
O2 C7 O1 125.3(7) . . ?
O2 C7 C1 118.2(7) . . ?
O3 C8 Tb1 60.4(3) . 4_576 ?
O3 C8 C3 120.0(6) . . ?
O4 C8 Tb1 59.5(3) . 4_576 ?
O4 C8 O3 119.2(6) . . ?
O4 C8 C3 120.8(6) . . ?
C3 C8 Tb1 171.0(5) . 4_576 ?
O5 C9 Tb1 60.9(4) . 2_656 ?
O5 C9 C5 118.9(6) . . ?
O6 C9 Tb1 62.9(4) . 2_656 ?
O6 C9 O5 121.1(6) . . ?
O6 C9 C5 119.8(6) . . ?
C5 C9 Tb1 159.0(5) . 2_656 ?
C11 C10 C6 120.3(6) . . ?
C11 C10 C14 116.9(6) . . ?
C14 C10 C6 122.8(6) . . ?
C10 C11 H11 119.4 . . ?
C10 C11 C12 121.1(7) . . ?
C12 C11 H11 119.4 . . ?
N1 C12 C11 121.7(6) . . ?
N1 C12 C15 118.3(6) . . ?
C11 C12 C15 119.9(6) . . ?
N1 C13 C14 120.4(6) . . ?
N1 C13 C20 117.6(6) . . ?
C14 C13 C20 122.0(6) . . ?
C10 C14 C13 120.6(6) . . ?
C10 C14 H14 119.7 . . ?
C13 C14 H14 119.7 . . ?
C16 C15 C12 121.6(6) . . ?
C16 C15 C19 116.7(7) . . ?
C19 C15 C12 121.5(7) . . ?
C15 C16 H16 119.9 . . ?
C15 C16 C17 120.1(7) . . ?
C17 C16 H16 119.9 . . ?
N2 C17 C16 125.2(8) . . ?
N2 C17 H17 117.4 . . ?
C16 C17 H17 117.4 . . ?
N2 C18 H18 117.1 . . ?
N2 C18 C19 125.8(8) . . ?
C19 C18 H18 117.1 . . ?
C15 C19 C18 119.5(8) . . ?
C15 C19 H19 120.3 . . ?
C18 C19 H19 120.3 . . ?
C21 C20 C13 122.1(7) . . ?
C21 C20 C24 115.6(7) . . ?
C24 C20 C13 122.3(7) . . ?
C20 C21 H21 119.7 . . ?
C20 C21 C22 120.5(8) . . ?
C22 C21 H21 119.7 . . ?
N3 C22 C21 123.4(7) . . ?
N3 C22 H22 118.3 . . ?
C21 C22 H22 118.3 . . ?
N3 C23 H23 117.9 . . ?
N3 C23 C24 124.1(9) . . ?
C24 C23 H23 117.9 . . ?
C20 C24 C23 120.0(8) . . ?
C20 C24 H24 120.0 . . ?
C23 C24 H24 120.0 . . ?

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
O7 H7A N3 0.85 2.15 2.717(8) 123.7 4_576

_smtbx_masks_special_details     ?
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 -0.174 -0.115 0.375 64.0 10.8 ?
2 0.174 0.115 0.625 64.0 11.4 ?
3 0.174 0.385 0.125 64.0 10.6 ?
4 -0.174 0.615 0.875 64.0 11.6 ?

_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_olex2_date_sample_data_collection 2018-12-28
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.786
_oxdiff_exptl_absorpt_empirical_full_min 0.781
####################################################################### 
# 
# 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_l71-eu_sq
_database_code_depnum_ccdc_archive 'CCDC 1961836'
loop_
_audit_author_name
_audit_author_address
'yapei shang'
;zhengzhou university
China
;
_audit_update_record             
;
2019-10-29 deposited with the CCDC.	2020-03-09 downloaded from the CCDC.
;
_audit_creation_date             2019-06-17
_audit_creation_method           
;
Olex2 1.2-alpha
(compiled 2018.07.26 svn.r3523 for OlexSys, GUI svn.r5532)
;
_shelx_SHELXL_version_number     2014/7
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C24 H16 Eu N3 O8'
_chemical_formula_sum            'C24 H16 Eu N3 O8'
_chemical_formula_weight         626.36
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C H N O Eu'
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'
Eu Eu -0.1578 3.6682 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/c 1'
_space_group_name_Hall           '-P 2ybc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   10.7464(4)
_cell_length_b                   12.2838(5)
_cell_length_c                   18.1760(6)
_cell_angle_alpha                90
_cell_angle_beta                 95.143(3)
_cell_angle_gamma                90
_cell_volume                     2389.69(15)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    5125
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.3400
_cell_measurement_theta_min      3.9300
_shelx_estimated_absorpt_T_max   0.674
_shelx_estimated_absorpt_T_min   0.543
_exptl_absorpt_coefficient_mu    2.679
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.70203
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.741
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1232
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.16
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0370
_diffrn_reflns_av_unetI/netI     0.0599
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.849
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            12164
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.849
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.359
_diffrn_reflns_theta_min         3.317
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0584
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.849
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -20.00  25.00   1.00   11.00    --  -13.80 -99.00 150.00   45
  2  ω    -63.00 -35.00   1.00   11.00    --  -13.80-178.00  90.00   28
  3  ω      9.00  53.00   1.00   11.00    --  -13.80  57.00-150.00   44
  4  ω    -82.00  43.00   1.00   11.00    --  -13.80   0.00  30.00  125
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Single source at offset/far, EosS2'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0161911000
_diffrn_orient_matrix_UB_12      -0.0120606000
_diffrn_orient_matrix_UB_13      0.0361014000
_diffrn_orient_matrix_UB_21      0.0593886000
_diffrn_orient_matrix_UB_22      0.0186265000
_diffrn_orient_matrix_UB_23      0.0149762000
_diffrn_orient_matrix_UB_31      -0.0245185000
_diffrn_orient_matrix_UB_32      0.0532962000
_diffrn_orient_matrix_UB_33      0.0029477000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4176
_reflns_number_total             5080
_reflns_odcompleteness_completeness 99.70
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     25.30
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_refine_diff_density_max         0.881
_refine_diff_density_min         -0.622
_refine_diff_density_rms         0.122
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     327
_refine_ls_number_reflns         5080
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0495
_refine_ls_R_factor_gt           0.0377
_refine_ls_restrained_S_all      1.042
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0251P)²+1.0616P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0708
_refine_ls_wR_factor_ref         0.0752
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H,H) groups
2.a Rotating group:
 O8(H8A,H8B), O7(H7A,H7B)
2.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C4(H4), C14(H14), C11(H11), C16(H16), C17(H17), C18(H18), C19(H19),
 C24(H24), C23(H23), C22(H22), C21(H21)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Eu1 Eu 0.18244(2) 0.53762(2) 0.63839(2) 0.01863(8) Uani 1 1 d . . . . .
O1 O 0.2040(3) 0.6946(3) 0.70124(17) 0.0338(8) Uani 1 1 d . . . . .
O2 O 0.0559(3) 0.7935(4) 0.7445(2) 0.0793(16) Uani 1 1 d . . . . .
O3 O 0.1473(3) 0.8853(3) 1.01277(16) 0.0302(8) Uani 1 1 d . . . . .
O4 O 0.3412(3) 0.9106(3) 1.05614(16) 0.0352(8) Uani 1 1 d . . . . .
O6 O 0.6093(3) 1.0006(3) 0.79320(16) 0.0302(8) Uani 1 1 d . . . . .
O5 O 0.6875(3) 0.8751(2) 0.87111(18) 0.0343(8) Uani 1 1 d . . . . .
O8 O 0.0574(3) 0.3980(3) 0.58077(19) 0.0374(8) Uani 1 1 d . . . . .
H8A H 0.0834 0.3364 0.5972 0.056 Uiso 1 1 d GR . . . .
H8B H 0.0682 0.3960 0.5349 0.056 Uiso 1 1 d GR . . . .
O7 O 0.1195(3) 0.4538(3) 0.74792(17) 0.0387(9) Uani 1 1 d . . . . .
H7A H 0.0542 0.4159 0.7372 0.058 Uiso 1 1 d GR . . . .
H7B H 0.0966 0.5033 0.7766 0.058 Uiso 1 1 d GR . . . .
N1 N 0.2281(5) 0.9674(4) 0.3774(2) 0.0571(14) Uani 1 1 d . . . . .
N2 N 0.5294(4) 0.8021(3) 0.5750(2) 0.0296(9) Uani 1 1 d . . . . .
N3 N 0.9534(4) 0.6128(3) 0.6298(2) 0.0304(9) Uani 1 1 d . . . . .
C1 C 0.2614(4) 0.8142(3) 0.8004(2) 0.0209(9) Uani 1 1 d . . . . .
C2 C 0.2236(4) 0.8290(3) 0.8708(2) 0.0213(10) Uani 1 1 d . . . . .
H2 H 0.1417 0.8128 0.8797 0.026 Uiso 1 1 calc R . . . .
C3 C 0.3054(4) 0.8675(3) 0.9278(2) 0.0215(10) Uani 1 1 d . . . . .
C4 C 0.4276(4) 0.8908(3) 0.9147(2) 0.0229(10) Uani 1 1 d . . . . .
H4 H 0.4840 0.9143 0.9532 0.028 Uiso 1 1 calc R . . . .
C5 C 0.4662(4) 0.8793(3) 0.8442(2) 0.0213(9) Uani 1 1 d . . . . .
C6 C 0.3841(4) 0.8397(3) 0.7857(2) 0.0186(9) Uani 1 1 d . . . . .
C7 C 0.1661(4) 0.7646(4) 0.7436(3) 0.0310(11) Uani 1 1 d . . . . .
C8 C 0.2633(4) 0.8886(3) 1.0033(2) 0.0204(9) Uani 1 1 d . . . . .
C9 C 0.5963(4) 0.9201(4) 0.8336(2) 0.0236(10) Uani 1 1 d . . . . .
C10 C 0.4304(4) 0.8244(3) 0.7116(2) 0.0199(9) Uani 1 1 d . . . . .
C14 C 0.5390(4) 0.7673(4) 0.7050(2) 0.0251(10) Uani 1 1 d . . . . .
H14 H 0.5799 0.7337 0.7463 0.030 Uiso 1 1 calc R . . . .
C13 C 0.5877(4) 0.7596(4) 0.6370(2) 0.0285(11) Uani 1 1 d . . . . .
C12 C 0.4198(4) 0.8540(3) 0.5800(2) 0.0245(10) Uani 1 1 d . . . . .
C11 C 0.3703(4) 0.8695(3) 0.6479(2) 0.0234(10) Uani 1 1 d . . . . .
H11 H 0.2975 0.9097 0.6503 0.028 Uiso 1 1 calc R . . . .
C15 C 0.3533(5) 0.8943(4) 0.5098(3) 0.0312(11) Uani 1 1 d . . . . .
C16 C 0.2276(5) 0.9177(5) 0.5042(3) 0.0586(17) Uani 1 1 d . . . . .
H16 H 0.1823 0.9090 0.5451 0.070 Uiso 1 1 calc R . . . .
C17 C 0.1684(6) 0.9540(6) 0.4381(4) 0.075(2) Uani 1 1 d . . . . .
H17 H 0.0836 0.9698 0.4358 0.091 Uiso 1 1 calc R . . . .
C18 C 0.3480(6) 0.9427(4) 0.3818(3) 0.0474(15) Uani 1 1 d . . . . .
H18 H 0.3913 0.9513 0.3401 0.057 Uiso 1 1 calc R . . . .
C19 C 0.4122(5) 0.9043(4) 0.4464(3) 0.0405(13) Uani 1 1 d . . . . .
H19 H 0.4960 0.8853 0.4466 0.049 Uiso 1 1 calc R . . . .
C20 C 0.7104(4) 0.7057(4) 0.6314(2) 0.0309(11) Uani 1 1 d . . . . .
C24 C 0.7484(4) 0.6206(4) 0.6755(3) 0.0394(13) Uani 1 1 d . . . . .
H24 H 0.6943 0.5914 0.7075 0.047 Uiso 1 1 calc R . . . .
C23 C 0.8681(5) 0.5764(4) 0.6734(3) 0.0432(14) Uani 1 1 d . . . . .
H23 H 0.8899 0.5178 0.7043 0.052 Uiso 1 1 calc R . . . .
C22 C 0.9138(5) 0.6968(5) 0.5865(3) 0.0534(16) Uani 1 1 d . . . . .
H22 H 0.9698 0.7267 0.5560 0.064 Uiso 1 1 calc R . . . .
C21 C 0.7946(5) 0.7423(5) 0.5840(3) 0.0550(16) Uani 1 1 d . . . . .
H21 H 0.7718 0.7974 0.5504 0.066 Uiso 1 1 calc R . . . .


_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 O1 2.243(3) . ?
Eu1 O3 2.469(3) 4_575 ?
Eu1 O4 2.451(3) 4_575 ?
Eu1 O6 2.502(3) 2_646 ?
Eu1 O5 2.452(3) 2_646 ?
Eu1 O8 2.365(3) . ?
Eu1 H8A 2.7679 . ?
Eu1 H8B 2.7670 . ?
Eu1 O7 2.392(3) . ?
Eu1 H7A 2.7938 . ?
Eu1 H7B 2.7842 . ?
Eu1 N3 2.621(4) 1_455 ?
Eu1 C8 2.826(4) 4_575 ?
Eu1 C9 2.789(4) 2_646 ?
O1 C7 1.247(5) . ?
O2 C7 1.238(5) . ?
O3 Eu1 2.469(3) 4_576 ?
O3 C8 1.275(5) . ?
O4 Eu1 2.451(3) 4_576 ?
O4 C8 1.246(5) . ?
O6 Eu1 2.502(3) 2_656 ?
O6 C9 1.247(5) . ?
O5 Eu1 2.452(3) 2_656 ?
O5 C9 1.269(5) . ?
O8 H8A 0.8512 . ?
O8 H8B 0.8521 . ?
O7 H7A 0.8504 . ?
O7 H7B 0.8506 . ?
N1 C17 1.336(8) . ?
N1 C18 1.319(7) . ?
N2 C13 1.345(5) . ?
N2 C12 1.350(5) . ?
N3 Eu1 2.621(4) 1_655 ?
N3 C23 1.342(6) . ?
N3 C22 1.343(6) . ?
C1 C2 1.388(6) . ?
C1 C6 1.405(5) . ?
C1 C7 1.515(6) . ?
C2 H2 0.9300 . ?
C2 C3 1.381(6) . ?
C3 C4 1.386(6) . ?
C3 C8 1.505(5) . ?
C4 H4 0.9300 . ?
C4 C5 1.390(5) . ?
C5 C6 1.406(5) . ?
C5 C9 1.514(6) . ?
C6 C10 1.488(5) . ?
C8 Eu1 2.826(4) 4_576 ?
C9 Eu1 2.789(4) 2_656 ?
C10 C14 1.377(6) . ?
C10 C11 1.390(5) . ?
C14 H14 0.9300 . ?
C14 C13 1.389(6) . ?
C13 C20 1.488(6) . ?
C12 C11 1.399(6) . ?
C12 C15 1.490(6) . ?
C11 H11 0.9300 . ?
C15 C16 1.376(7) . ?
C15 C19 1.368(6) . ?
C16 H16 0.9300 . ?
C16 C17 1.382(7) . ?
C17 H17 0.9300 . ?
C18 H18 0.9300 . ?
C18 C19 1.389(7) . ?
C19 H19 0.9300 . ?
C20 C24 1.358(6) . ?
C20 C21 1.379(7) . ?
C24 H24 0.9300 . ?
C24 C23 1.400(7) . ?
C23 H23 0.9300 . ?
C22 H22 0.9300 . ?
C22 C21 1.395(7) . ?
C21 H21 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
O1 Eu1 O3 98.14(11) . 4_575 ?
O1 Eu1 O4 92.39(11) . 4_575 ?
O1 Eu1 O6 81.72(11) . 2_646 ?
O1 Eu1 O5 134.60(11) . 2_646 ?
O1 Eu1 O8 151.40(11) . . ?
O1 Eu1 H8A 157.7 . . ?
O1 Eu1 H8B 155.0 . . ?
O1 Eu1 O7 88.29(12) . . ?
O1 Eu1 H7A 99.6 . . ?
O1 Eu1 H7B 72.5 . . ?
O1 Eu1 N3 77.36(11) . 1_455 ?
O1 Eu1 C8 98.09(12) . 4_575 ?
O1 Eu1 C9 107.72(12) . 2_646 ?
O3 Eu1 O6 125.82(10) 4_575 2_646 ?
O3 Eu1 H8A 93.9 4_575 . ?
O3 Eu1 H8B 65.8 4_575 . ?
O3 Eu1 H7A 139.1 4_575 . ?
O3 Eu1 H7B 148.9 4_575 . ?
O3 Eu1 N3 75.19(11) 4_575 1_455 ?
O3 Eu1 C8 26.79(10) 4_575 4_575 ?
O3 Eu1 C9 115.11(11) 4_575 2_646 ?
O4 Eu1 O3 52.69(9) 4_575 4_575 ?
O4 Eu1 O6 73.13(10) 4_575 2_646 ?
O4 Eu1 O5 74.68(11) 4_575 2_646 ?
O4 Eu1 H8A 109.8 4_575 . ?
O4 Eu1 H8B 92.2 4_575 . ?
O4 Eu1 H7A 160.3 4_575 . ?
O4 Eu1 H7B 153.5 4_575 . ?
O4 Eu1 N3 125.00(11) 4_575 1_455 ?
O4 Eu1 C8 26.08(10) 4_575 4_575 ?
O4 Eu1 C9 67.46(11) 4_575 2_646 ?
O6 Eu1 H8A 106.1 2_646 . ?
O6 Eu1 H8B 123.1 2_646 . ?
O6 Eu1 H7A 93.1 2_646 . ?
O6 Eu1 H7B 83.0 2_646 . ?
O6 Eu1 N3 152.51(11) 2_646 1_455 ?
O6 Eu1 C8 99.15(11) 2_646 4_575 ?
O6 Eu1 C9 26.56(11) 2_646 2_646 ?
O5 Eu1 O3 106.74(10) 2_646 4_575 ?
O5 Eu1 O6 52.91(10) 2_646 2_646 ?
O5 Eu1 H8A 57.4 2_646 . ?
O5 Eu1 H8B 70.2 2_646 . ?
O5 Eu1 H7A 85.8 2_646 . ?
O5 Eu1 H7B 100.2 2_646 . ?
O5 Eu1 N3 145.20(11) 2_646 1_455 ?
O5 Eu1 C8 88.76(11) 2_646 4_575 ?
O5 Eu1 C9 27.05(11) 2_646 2_646 ?
O8 Eu1 O3 80.49(11) . 4_575 ?
O8 Eu1 O4 108.48(11) . 4_575 ?
O8 Eu1 O6 122.38(11) . 2_646 ?
O8 Eu1 O5 71.53(10) . 2_646 ?
O8 Eu1 H8A 16.8 . . ?
O8 Eu1 H8B 16.9 . . ?
O8 Eu1 O7 82.22(12) . . ?
O8 Eu1 H7A 66.6 . . ?
O8 Eu1 H7B 93.9 . . ?
O8 Eu1 N3 74.68(11) . 1_455 ?
O8 Eu1 C8 93.14(12) . 4_575 ?
O8 Eu1 C9 98.44(12) . 2_646 ?
H8A Eu1 H8B 28.1 . . ?
H8A Eu1 H7A 59.7 . . ?
H8A Eu1 H7B 87.6 . . ?
H8B Eu1 H7A 83.5 . . ?
H8B Eu1 H7B 110.8 . . ?
O7 Eu1 O3 154.59(10) . 4_575 ?
O7 Eu1 O4 152.06(11) . 4_575 ?
O7 Eu1 O6 79.34(10) . 2_646 ?
O7 Eu1 O5 85.05(11) . 2_646 ?
O7 Eu1 H8A 73.2 . . ?
O7 Eu1 H8B 98.9 . . ?
O7 Eu1 H7A 16.7 . . ?
O7 Eu1 H7B 16.8 . . ?
O7 Eu1 N3 82.38(12) . 1_455 ?
O7 Eu1 C8 173.19(11) . 4_575 ?
O7 Eu1 C9 85.73(12) . 2_646 ?
H7A Eu1 H7B 27.9 . . ?
N3 Eu1 H8A 87.8 1_455 . ?
N3 Eu1 H8B 79.8 1_455 . ?
N3 Eu1 H7A 73.3 1_455 . ?
N3 Eu1 H7B 73.8 1_455 . ?
N3 Eu1 C8 101.27(12) 1_455 4_575 ?
N3 Eu1 C9 166.95(13) 1_455 2_646 ?
C8 Eu1 H8A 101.1 4_575 . ?
C8 Eu1 H8B 76.3 4_575 . ?
C8 Eu1 H7A 159.7 4_575 . ?
C8 Eu1 H7B 170.0 4_575 . ?
C9 Eu1 H8A 83.6 2_646 . ?
C9 Eu1 H8B 96.8 2_646 . ?
C9 Eu1 H7A 93.9 2_646 . ?
C9 Eu1 H7B 95.9 2_646 . ?
C9 Eu1 C8 90.04(12) 2_646 4_575 ?
C7 O1 Eu1 152.0(3) . . ?
C8 O3 Eu1 92.4(2) . 4_576 ?
C8 O4 Eu1 94.0(2) . 4_576 ?
C9 O6 Eu1 89.7(3) . 2_656 ?
C9 O5 Eu1 91.4(3) . 2_656 ?
Eu1 O8 H8A 109.5 . . ?
Eu1 O8 H8B 109.4 . . ?
H8A O8 H8B 104.4 . . ?
Eu1 O7 H7A 109.5 . . ?
Eu1 O7 H7B 108.7 . . ?
H7A O7 H7B 104.6 . . ?
C18 N1 C17 117.3(5) . . ?
C13 N2 C12 118.0(4) . . ?
C23 N3 Eu1 122.3(3) . 1_655 ?
C23 N3 C22 113.9(4) . . ?
C22 N3 Eu1 123.5(3) . 1_655 ?
C2 C1 C6 120.3(4) . . ?
C2 C1 C7 116.4(4) . . ?
C6 C1 C7 123.2(4) . . ?
C1 C2 H2 119.4 . . ?
C3 C2 C1 121.2(4) . . ?
C3 C2 H2 119.4 . . ?
C2 C3 C4 119.4(4) . . ?
C2 C3 C8 121.4(4) . . ?
C4 C3 C8 119.2(4) . . ?
C3 C4 H4 119.9 . . ?
C3 C4 C5 120.2(4) . . ?
C5 C4 H4 119.9 . . ?
C4 C5 C6 120.9(4) . . ?
C4 C5 C9 116.0(4) . . ?
C6 C5 C9 122.9(4) . . ?
C1 C6 C5 117.9(4) . . ?
C1 C6 C10 122.7(4) . . ?
C5 C6 C10 119.3(4) . . ?
O1 C7 C1 117.4(4) . . ?
O2 C7 O1 124.9(4) . . ?
O2 C7 C1 117.7(4) . . ?
O3 C8 Eu1 60.8(2) . 4_576 ?
O3 C8 C3 119.7(4) . . ?
O4 C8 Eu1 59.9(2) . 4_576 ?
O4 C8 O3 120.1(4) . . ?
O4 C8 C3 120.3(4) . . ?
C3 C8 Eu1 171.1(3) . 4_576 ?
O6 C9 Eu1 63.8(2) . 2_656 ?
O6 C9 O5 122.6(4) . . ?
O6 C9 C5 119.4(4) . . ?
O5 C9 Eu1 61.5(2) . 2_656 ?
O5 C9 C5 117.7(4) . . ?
C5 C9 Eu1 158.5(3) . 2_656 ?
C14 C10 C6 119.9(4) . . ?
C14 C10 C11 117.7(4) . . ?
C11 C10 C6 122.4(4) . . ?
C10 C14 H14 119.9 . . ?
C10 C14 C13 120.1(4) . . ?
C13 C14 H14 119.9 . . ?
N2 C13 C14 122.4(4) . . ?
N2 C13 C20 117.7(4) . . ?
C14 C13 C20 119.9(4) . . ?
N2 C12 C11 121.8(4) . . ?
N2 C12 C15 116.9(4) . . ?
C11 C12 C15 121.3(4) . . ?
C10 C11 C12 119.7(4) . . ?
C10 C11 H11 120.1 . . ?
C12 C11 H11 120.1 . . ?
C16 C15 C12 121.6(4) . . ?
C19 C15 C12 121.9(4) . . ?
C19 C15 C16 116.4(5) . . ?
C15 C16 H16 119.9 . . ?
C15 C16 C17 120.2(5) . . ?
C17 C16 H16 119.9 . . ?
N1 C17 C16 122.8(6) . . ?
N1 C17 H17 118.6 . . ?
C16 C17 H17 118.6 . . ?
N1 C18 H18 118.7 . . ?
N1 C18 C19 122.6(5) . . ?
C19 C18 H18 118.7 . . ?
C15 C19 C18 120.6(5) . . ?
C15 C19 H19 119.7 . . ?
C18 C19 H19 119.7 . . ?
C24 C20 C13 121.6(4) . . ?
C24 C20 C21 116.2(4) . . ?
C21 C20 C13 122.2(5) . . ?
C20 C24 H24 119.6 . . ?
C20 C24 C23 120.7(5) . . ?
C23 C24 H24 119.6 . . ?
N3 C23 C24 124.4(5) . . ?
N3 C23 H23 117.8 . . ?
C24 C23 H23 117.8 . . ?
N3 C22 H22 117.7 . . ?
N3 C22 C21 124.6(5) . . ?
C21 C22 H22 117.7 . . ?
C20 C21 C22 120.1(5) . . ?
C20 C21 H21 120.0 . . ?
C22 C21 H21 120.0 . . ?

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 H8B O3 0.85 2.40 2.661(4) 98.2 2_546
O7 H7A O2 0.85 1.96 2.738(5) 151.6 2_546
O7 H7B N1 0.85 2.24 2.709(6) 114.8 4_576

_smtbx_masks_special_details     ?
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 -0.174 -0.117 0.374 66.2 13.7 ?
2 0.174 0.117 0.626 66.2 14.3 ?
3 0.174 0.383 0.126 66.2 13.6 ?
4 -0.174 0.617 0.874 66.2 14.4 ?

_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_olex2_date_sample_data_collection 2018-12-06
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.953
_oxdiff_exptl_absorpt_empirical_full_min 0.710
