# Electronic Supplementary Material (ESI) for Journal of Materials Chemistry C.
# This journal is © The Royal Society of Chemistry 2022

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

data_sxc-eu-11262h
_database_code_depnum_ccdc_archive 'CCDC 2128999'
loop_
_audit_author_name
_audit_author_address
'Sun Xuechun'
;The Cambridge Crystallographic Data Centre
China
;
_audit_update_record             
;
2021-12-16 deposited with the CCDC.	2022-09-15 downloaded from the CCDC.
;
_audit_creation_date             2021-12-16
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.02.04 svn.rd84adfe8 for OlexSys, GUI svn.r6032)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C21 H11 Eu N6 O8, H2 O'
_chemical_formula_sum            'C21 H15 Eu N6 O9'
_chemical_formula_weight         647.35
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   5.2645(2)
_cell_length_b                   13.1605(7)
_cell_length_c                   16.6532(9)
_cell_angle_alpha                97.157(4)
_cell_angle_beta                 96.532(4)
_cell_angle_gamma                92.653(4)
_cell_volume                     1135.23(10)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    6861
_cell_measurement_temperature    293.15
_cell_measurement_theta_max      30.1670
_cell_measurement_theta_min      3.0520
_shelx_estimated_absorpt_T_max   0.765
_shelx_estimated_absorpt_T_min   0.601
_exptl_absorpt_coefficient_mu    2.830
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.60478
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.41.43a (Rigaku Oxford Diffraction, 2019)
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    1.894
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       needle
_exptl_crystal_F_000             636
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0377
_diffrn_reflns_av_unetI/netI     0.0538
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.936
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            19462
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.936
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         32.530
_diffrn_reflns_theta_min         2.756
_diffrn_ambient_temperature      293.15
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.936
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -74.00 119.00   1.00   15.50    --   30.00  54.00 -30.00  193
  2  ω    -74.00 119.00   1.00   15.50    --   30.00  54.00  90.00  193
  3  ω    -74.00 119.00   1.00   15.50    --   30.00  54.00-150.00  193
  4  ω    -74.00  28.00   1.00   15.50    --   30.00  54.00 150.00  102
;
_diffrn_measurement_device       'two-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Mini (ROW)'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0071505000
_diffrn_orient_matrix_UB_12      0.0457809000
_diffrn_orient_matrix_UB_13      0.0268456000
_diffrn_orient_matrix_UB_21      -0.0509387000
_diffrn_orient_matrix_UB_22      -0.0289071000
_diffrn_orient_matrix_UB_23      0.0283187000
_diffrn_orient_matrix_UB_31      0.1257571000
_diffrn_orient_matrix_UB_32      -0.0055006000
_diffrn_orient_matrix_UB_33      0.0186305000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                6492
_reflns_number_total             7686
_reflns_odcompleteness_completeness 99.89
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.41.43a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.41.43a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.41.43a (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS  (Sheldrick, 2008)'
_refine_diff_density_max         2.628
_refine_diff_density_min         -0.898
_refine_diff_density_rms         0.145
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     338
_refine_ls_number_reflns         7686
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0488
_refine_ls_R_factor_gt           0.0349
_refine_ls_restrained_S_all      1.058
_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+0.7525P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0714
_refine_ls_wR_factor_ref         0.0766
_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 Free rotating group:
 O1(H1A,H1B)
2.b Rotating group:
 O6(H6A,H6B)
2.c Aromatic/amide H refined with riding coordinates:
 C16(H16), C17(H17), C18(H18), C19(H19), C105(H105), C119(H119), C132(H132),
 C156(H156), C161(H161)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_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 0.70906(3) 0.26725(2) 0.24878(2) 0.01724(5) Uani 1 1 d . . . . .
O6 O 0.5035(4) 0.43033(19) 0.24732(15) 0.0296(5) Uani 1 1 d . . . . .
H6A H 0.356693 0.421965 0.215873 0.044 Uiso 1 1 d R U . . .
H6B H 0.593650 0.473362 0.224027 0.044 Uiso 1 1 d R U . . .
O8 O 0.6889(5) 0.31051(18) 0.10505(14) 0.0307(5) Uani 1 1 d . . . . .
O9 O 0.9992(4) 0.38859(17) 0.19290(13) 0.0247(5) Uani 1 1 d . . . . .
O52 O 0.3955(4) 0.15690(18) 0.16813(14) 0.0276(5) Uani 1 1 d . . . . .
O73 O 0.4056(4) 0.27665(18) 0.34502(13) 0.0261(5) Uani 1 1 d . . . . .
O89 O 0.7565(5) 0.12672(19) 0.33264(14) 0.0338(6) Uani 1 1 d . . . . .
C128 C 0.3760(5) 0.4198(2) 0.44359(17) 0.0191(6) Uani 1 1 d . . . . .
O133 O 1.0225(4) 0.33825(18) 0.35741(13) 0.0262(5) Uani 1 1 d . . . . .
O168 O 0.9947(4) 0.15898(19) 0.19490(13) 0.0286(5) Uani 1 1 d . . . . .
N5 N 0.4160(6) 0.2302(2) 0.5256(2) 0.0400(8) Uani 1 1 d . . . . .
N124 N 0.6099(5) 0.2956(2) 0.51782(15) 0.0219(5) Uani 1 1 d . . . . .
N139 N 0.3853(5) -0.0756(2) 0.10392(15) 0.0224(5) Uani 1 1 d . . . . .
N140 N 0.3902(6) -0.0613(2) 0.18599(17) 0.0309(6) Uani 1 1 d . . . . .
C16 C 0.5780(6) -0.1312(3) 0.0802(2) 0.0314(7) Uani 1 1 d . . . . .
H16 H 0.609550 -0.151012 0.026870 0.038 Uiso 1 1 calc R U . . .
C17 C 0.8379(7) 0.2553(3) 0.5223(2) 0.0312(7) Uani 1 1 d . . . . .
H17 H 0.995189 0.288368 0.518455 0.037 Uiso 1 1 calc R U . . .
C18 C 0.7927(8) 0.1556(3) 0.5336(2) 0.0403(9) Uani 1 1 d . . . . .
H18 H 0.912065 0.106184 0.538884 0.048 Uiso 1 1 calc R U . . .
C19 C 0.5313(9) 0.1437(3) 0.5355(3) 0.0438(10) Uani 1 1 d . . . . .
H19 H 0.445969 0.082683 0.542845 0.053 Uiso 1 1 calc R U . . .
N32 N 0.9788(5) 0.3995(2) -0.15945(15) 0.0231(5) Uani 1 1 d . . . . .
C55 C 0.5576(6) 0.4005(2) 0.50715(17) 0.0199(6) Uani 1 1 d . . . . .
C102 C 0.0792(5) 0.0561(2) 0.07710(17) 0.0180(5) Uani 1 1 d . . . . .
C104 C 0.1917(5) -0.0348(2) 0.05212(17) 0.0190(6) Uani 1 1 d . . . . .
C105 C 0.9215(7) 0.3981(3) -0.01860(19) 0.0261(7) Uani 1 1 d . . . . .
H105 H 0.867389 0.329154 -0.031720 0.031 Uiso 1 1 calc R U . . .
C107 C 0.7838(7) 0.3354(3) -0.1984(2) 0.0288(7) Uani 1 1 d . . . . .
C108 C 0.1653(6) 0.1283(2) 0.15376(17) 0.0177(5) Uani 1 1 d . . . . .
N1 N 1.1776(5) 0.4056(2) -0.20420(16) 0.0277(6) Uani 1 1 d . . . . .
C114 C 0.3198(6) 0.5206(2) 0.43753(18) 0.0226(6) Uani 1 1 d . . . . .
C119 C 0.7178(7) -0.1528(3) 0.1491(2) 0.0382(9) Uani 1 1 d . . . . .
H119 H 0.864095 -0.189713 0.152954 0.046 Uiso 1 1 calc R U . . .
C120 C 0.2591(6) 0.3374(2) 0.37698(17) 0.0191(6) Uani 1 1 d . . . . .
C121 C 0.9900(6) 0.4529(2) -0.07899(18) 0.0231(6) Uani 1 1 d . . . . .
C123 C 0.9320(6) 0.4440(2) 0.06129(18) 0.0239(6) Uani 1 1 d . . . . .
C132 C 1.0983(7) 0.3447(3) -0.2726(2) 0.0325(8) Uani 1 1 d . . . . .
H132 H 1.194307 0.333671 -0.316065 0.039 Uiso 1 1 calc R U . . .
C134 C -0.1159(6) 0.0888(2) 0.02405(18) 0.0211(6) Uani 1 1 d . . . . .
C154 C 0.8697(6) 0.3771(2) 0.12395(18) 0.0237(6) Uani 1 1 d . . . . .
C156 C 0.5949(7) -0.1078(3) 0.2122(2) 0.0367(9) Uani 1 1 d . . . . .
H156 H 0.650020 -0.109937 0.267046 0.044 Uiso 1 1 calc R U . . .
C161 C 0.8559(7) 0.2992(3) -0.2722(2) 0.0354(8) Uani 1 1 d . . . . .
H161 H 0.762376 0.253772 -0.313389 0.043 Uiso 1 1 calc R U . . .
O1 O 0.1975(6) 0.0320(3) 0.3341(2) 0.0533(8) Uani 1 1 d G . . . .
H1A H 0.275724 0.090984 0.344745 0.080 Uiso 1 1 d G U . . .
H1B H 0.232482 0.009169 0.286833 0.080 Uiso 1 1 d G U . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Eu1 O6 2.449(2) . ?
Eu1 O8 2.520(2) . ?
Eu1 O9 2.493(2) . ?
Eu1 O52 2.329(2) . ?
Eu1 O73 2.385(2) . ?
Eu1 O89 2.458(2) . ?
Eu1 O133 2.372(2) . ?
Eu1 O168 2.298(2) . ?
Eu1 C154 2.857(3) . ?
O6 H6A 0.8773 . ?
O6 H6B 0.8764 . ?
O8 C154 1.249(4) . ?
O9 C154 1.255(4) . ?
O52 C108 1.240(3) . ?
O73 C120 1.249(4) . ?
C128 C55 1.399(4) . ?
C128 C114 1.387(4) . ?
C128 C120 1.506(4) . ?
O133 C120 1.252(4) 1_655 ?
O168 C108 1.242(4) 1_655 ?
N5 N124 1.333(4) . ?
N5 C19 1.334(5) . ?
N124 C17 1.333(4) . ?
N124 C55 1.448(4) . ?
N139 N140 1.353(4) . ?
N139 C16 1.344(4) . ?
N139 C104 1.427(4) . ?
N140 C156 1.322(4) . ?
C16 H16 0.9300 . ?
C16 C119 1.360(5) . ?
C17 H17 0.9300 . ?
C17 C18 1.363(5) . ?
C18 H18 0.9300 . ?
C18 C19 1.382(6) . ?
C19 H19 0.9300 . ?
N32 C107 1.348(4) . ?
N32 N1 1.357(4) . ?
N32 C121 1.427(4) . ?
C55 C114 1.382(4) 2_666 ?
C102 C104 1.397(4) . ?
C102 C108 1.505(4) . ?
C102 C134 1.397(4) . ?
C104 C134 1.381(4) 2 ?
C105 H105 0.9300 . ?
C105 C121 1.379(4) . ?
C105 C123 1.385(4) . ?
C107 C161 1.363(5) . ?
N1 C132 1.322(4) . ?
C119 H119 0.9300 . ?
C119 C156 1.382(6) . ?
C121 C123 1.385(4) 2_765 ?
C123 C154 1.501(4) . ?
C132 H132 0.9300 . ?
C132 C161 1.386(5) . ?
C156 H156 0.9300 . ?
C161 H161 0.9300 . ?
O1 H1A 0.8504 . ?
O1 H1B 0.8505 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O6 Eu1 O8 73.24(8) . . ?
O6 Eu1 O9 72.18(8) . . ?
O6 Eu1 O89 139.79(8) . . ?
O6 Eu1 C154 68.78(8) . . ?
O8 Eu1 C154 25.89(8) . . ?
O9 Eu1 O8 51.77(7) . . ?
O9 Eu1 C154 26.01(8) . . ?
O52 Eu1 O6 100.32(8) . . ?
O52 Eu1 O8 72.19(8) . . ?
O52 Eu1 O9 123.54(8) . . ?
O52 Eu1 O73 84.06(8) . . ?
O52 Eu1 O89 84.82(8) . . ?
O52 Eu1 O133 161.95(8) . . ?
O52 Eu1 C154 98.05(9) . . ?
O73 Eu1 O6 71.18(8) . . ?
O73 Eu1 O8 132.31(8) . . ?
O73 Eu1 O9 137.40(8) . . ?
O73 Eu1 O89 69.76(8) . . ?
O73 Eu1 C154 139.62(9) . . ?
O89 Eu1 O8 143.88(8) . . ?
O89 Eu1 O9 136.81(8) . . ?
O89 Eu1 C154 150.57(9) . . ?
O133 Eu1 O6 91.92(8) . . ?
O133 Eu1 O8 124.56(8) . . ?
O133 Eu1 O9 72.79(7) . . ?
O133 Eu1 O73 87.45(8) . . ?
O133 Eu1 O89 77.30(8) . . ?
O133 Eu1 C154 98.74(9) . . ?
O168 Eu1 O6 147.63(8) . . ?
O168 Eu1 O8 78.37(8) . . ?
O168 Eu1 O9 78.18(8) . . ?
O168 Eu1 O52 85.23(8) . . ?
O168 Eu1 O73 141.15(8) . . ?
O168 Eu1 O89 72.16(9) . . ?
O168 Eu1 O133 91.53(8) . . ?
O168 Eu1 C154 78.88(9) . . ?
Eu1 O6 H6A 110.6 . . ?
Eu1 O6 H6B 110.5 . . ?
H6A O6 H6B 103.3 . . ?
C154 O8 Eu1 92.29(18) . . ?
C154 O9 Eu1 93.40(18) . . ?
C108 O52 Eu1 147.0(2) . . ?
C120 O73 Eu1 141.0(2) . . ?
C55 C128 C120 122.9(3) . . ?
C114 C128 C55 118.3(3) . . ?
C114 C128 C120 118.5(3) . . ?
C120 O133 Eu1 138.6(2) 1_655 . ?
C108 O168 Eu1 159.2(2) 1_655 . ?
N124 N5 C19 103.0(3) . . ?
N5 N124 C17 114.2(3) . . ?
N5 N124 C55 118.9(3) . . ?
C17 N124 C55 126.8(3) . . ?
N140 N139 C104 121.4(3) . . ?
C16 N139 N140 112.0(3) . . ?
C16 N139 C104 126.6(3) . . ?
C156 N140 N139 103.8(3) . . ?
N139 C16 H16 126.6 . . ?
N139 C16 C119 106.9(3) . . ?
C119 C16 H16 126.6 . . ?
N124 C17 H17 127.1 . . ?
N124 C17 C18 105.8(3) . . ?
C18 C17 H17 127.1 . . ?
C17 C18 H18 127.4 . . ?
C17 C18 C19 105.2(3) . . ?
C19 C18 H18 127.4 . . ?
N5 C19 C18 111.9(4) . . ?
N5 C19 H19 124.0 . . ?
C18 C19 H19 124.0 . . ?
C107 N32 N1 112.4(3) . . ?
C107 N32 C121 125.9(3) . . ?
N1 N32 C121 121.7(3) . . ?
C128 C55 N124 119.6(3) . . ?
C114 C55 C128 121.3(3) 2_666 . ?
C114 C55 N124 119.0(3) 2_666 . ?
C104 C102 C108 125.7(3) . . ?
C134 C102 C104 118.2(3) . . ?
C134 C102 C108 115.9(3) . . ?
C102 C104 N139 121.7(3) . . ?
C134 C104 N139 117.7(3) 2 . ?
C134 C104 C102 120.5(3) 2 . ?
C121 C105 H105 119.4 . . ?
C121 C105 C123 121.1(3) . . ?
C123 C105 H105 119.4 . . ?
N32 C107 C161 106.4(3) . . ?
O52 C108 O168 125.5(3) . 1_455 ?
O52 C108 C102 117.9(3) . . ?
O168 C108 C102 116.4(3) 1_455 . ?
C132 N1 N32 103.7(3) . . ?
C55 C114 C128 120.4(3) 2_666 . ?
C16 C119 H119 127.6 . . ?
C16 C119 C156 104.9(3) . . ?
C156 C119 H119 127.6 . . ?
O73 C120 C128 117.8(3) . . ?
O73 C120 O133 126.1(3) . 1_455 ?
O133 C120 C128 116.2(3) 1_455 . ?
C105 C121 N32 117.7(3) . . ?
C105 C121 C123 120.6(3) . 2_765 ?
C123 C121 N32 121.7(3) 2_765 . ?
C105 C123 C154 117.5(3) . . ?
C121 C123 C105 118.3(3) 2_765 . ?
C121 C123 C154 124.2(3) 2_765 . ?
N1 C132 H132 123.8 . . ?
N1 C132 C161 112.4(3) . . ?
C161 C132 H132 123.8 . . ?
C104 C134 C102 121.2(3) 2 . ?
O8 C154 Eu1 61.82(16) . . ?
O8 C154 O9 121.9(3) . . ?
O8 C154 C123 118.2(3) . . ?
O9 C154 Eu1 60.59(15) . . ?
O9 C154 C123 119.9(3) . . ?
C123 C154 Eu1 173.2(2) . . ?
N140 C156 C119 112.4(3) . . ?
N140 C156 H156 123.8 . . ?
C119 C156 H156 123.8 . . ?
C107 C161 C132 105.2(3) . . ?
C107 C161 H161 127.4 . . ?
C132 C161 H161 127.4 . . ?
H1A O1 H1B 104.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Eu1 O8 C154 O9 8.2(3) . . . . ?
Eu1 O8 C154 C123 -172.3(3) . . . . ?
Eu1 O9 C154 O8 -8.3(3) . . . . ?
Eu1 O9 C154 C123 172.2(3) . . . . ?
Eu1 O52 C108 O168 -5.0(6) . . . 1_455 ?
Eu1 O52 C108 C102 170.4(3) . . . . ?
Eu1 O73 C120 C128 -77.3(4) . . . . ?
Eu1 O73 C120 O133 100.7(4) . . . 1_455 ?
N5 N124 C17 C18 0.2(4) . . . . ?
N5 N124 C55 C128 -55.0(4) . . . . ?
N5 N124 C55 C114 122.0(3) . . . 2_666 ?
N124 N5 C19 C18 -0.2(4) . . . . ?
N124 C17 C18 C19 -0.3(4) . . . . ?
N139 N140 C156 C119 -1.1(4) . . . . ?
N139 C16 C119 C156 0.4(4) . . . . ?
N140 N139 C16 C119 -1.1(4) . . . . ?
N140 N139 C104 C102 30.9(4) . . . . ?
N140 N139 C104 C134 -148.5(3) . . . 2 ?
C16 N139 N140 C156 1.3(4) . . . . ?
C16 N139 C104 C102 -149.5(3) . . . . ?
C16 N139 C104 C134 31.2(5) . . . 2 ?
C16 C119 C156 N140 0.4(5) . . . . ?
C17 N124 C55 C128 126.1(3) . . . . ?
C17 N124 C55 C114 -56.8(4) . . . 2_666 ?
C17 C18 C19 N5 0.3(5) . . . . ?
C19 N5 N124 C17 0.0(4) . . . . ?
C19 N5 N124 C55 -179.0(3) . . . . ?
N32 C107 C161 C132 0.5(4) . . . . ?
N32 N1 C132 C161 -0.7(4) . . . . ?
C55 C128 C114 C55 0.5(5) . . . 2_666 ?
C55 C128 C120 O73 -45.1(4) . . . . ?
C55 C128 C120 O133 136.7(3) . . . 1_455 ?
C55 N124 C17 C18 179.1(3) . . . . ?
C104 N139 N140 C156 -179.0(3) . . . . ?
C104 N139 C16 C119 179.2(3) . . . . ?
C104 C102 C108 O52 50.3(4) . . . . ?
C104 C102 C108 O168 -133.9(3) . . . 1_455 ?
C104 C102 C134 C104 -1.8(5) . . . 2 ?
C105 C123 C154 O8 -40.1(5) . . . . ?
C105 C123 C154 O9 139.4(3) . . . . ?
C107 N32 N1 C132 1.0(4) . . . . ?
C107 N32 C121 C105 46.3(5) . . . . ?
C107 N32 C121 C123 -134.1(4) . . . 2_765 ?
C108 C102 C104 N139 8.4(5) . . . . ?
C108 C102 C104 C134 -172.3(3) . . . 2 ?
C108 C102 C134 C104 172.8(3) . . . 2 ?
N1 N32 C107 C161 -1.0(4) . . . . ?
N1 N32 C121 C105 -130.7(3) . . . . ?
N1 N32 C121 C123 48.9(4) . . . 2_765 ?
N1 C132 C161 C107 0.1(4) . . . . ?
C114 C128 C55 N124 176.5(3) . . . . ?
C114 C128 C55 C114 -0.5(5) . . . 2_666 ?
C114 C128 C120 O73 128.6(3) . . . . ?
C114 C128 C120 O133 -49.6(4) . . . 1_455 ?
C120 C128 C55 N124 -9.7(4) . . . . ?
C120 C128 C55 C114 173.3(3) . . . 2_666 ?
C120 C128 C114 C55 -173.5(3) . . . 2_666 ?
C121 N32 C107 C161 -178.2(3) . . . . ?
C121 N32 N1 C132 178.3(3) . . . . ?
C121 C105 C123 C121 0.8(6) . . . 2_765 ?
C121 C105 C123 C154 -176.3(3) . . . . ?
C121 C123 C154 O8 142.9(3) 2_765 . . . ?
C121 C123 C154 O9 -37.5(5) 2_765 . . . ?
C123 C105 C121 N32 178.8(3) . . . . ?
C123 C105 C121 C123 -0.9(6) . . . 2_765 ?
C134 C102 C104 N139 -177.6(3) . . . . ?
C134 C102 C104 C134 1.8(5) . . . 2 ?
C134 C102 C108 O52 -123.9(3) . . . . ?
C134 C102 C108 O168 51.9(4) . . . 1_455 ?

_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 1.767
_oxdiff_exptl_absorpt_empirical_full_min 0.700
####################################################################### 
# 
# 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_exp_357_tw
_database_code_depnum_ccdc_archive 'CCDC 2184518'
loop_
_audit_author_name
_audit_author_address
'Sun Xuechun'
;Shenyang University of Chemical Technology
China
;
_audit_update_record             
;
2022-07-06 deposited with the CCDC.	2022-09-15 downloaded from the CCDC.
;
_audit_creation_date             2022-05-08
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.02.04 svn.rd84adfe8 for OlexSys, GUI svn.r6032)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C21 H15 Dy N6 O8, H2 O'
_chemical_formula_sum            'C21 H17 Dy N6 O9'
_chemical_formula_weight         659.91
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Dy Dy -0.1892 4.4098 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

_cell_length_a                   5.2345(3)
_cell_length_b                   13.1182(12)
_cell_length_c                   16.6342(12)
_cell_angle_alpha                97.377(7)
_cell_angle_beta                 96.786(5)
_cell_angle_gamma                92.674(6)
_cell_volume                     1122.61(14)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    6000
_cell_measurement_temperature    298
_cell_measurement_theta_max      25
_cell_measurement_theta_min      3
_shelx_estimated_absorpt_T_max   0.741
_shelx_estimated_absorpt_T_min   0.741
_exptl_absorpt_coefficient_mu    3.396
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   ?
_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    1.952
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       needle
_exptl_crystal_F_000             646
_exptl_crystal_preparation       ?
_exptl_crystal_recrystallization_method ?
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_exptl_transmission_factor_max   0.864
_exptl_transmission_factor_min   0.864
_diffrn_reflns_av_R_equivalents  ?
_diffrn_reflns_av_unetI/netI     0.0677
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            5550
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.279
_diffrn_reflns_theta_min         2.757
_diffrn_ambient_temperature      298
_diffrn_detector                 'Bruker APEX2 area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker SMART APEX2 area detector'
_diffrn_measurement_method       'ω and φ scans'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_target            Mo
_diffrn_source_type              'Incoatec I\ms'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4991
_reflns_number_total             5550
_reflns_special_details          
;
 _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. Completness statistics refer to single and
 composite reflections containing twin component 1 only.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       ?
_computing_data_collection       ?
_computing_data_reduction        ?
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve 1.3 (Bourhis et al., 2015)'
_refine_diff_density_max         6.183
_refine_diff_density_min         -4.891
_refine_diff_density_rms         0.329
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.160
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     347
_refine_ls_number_reflns         5550
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0880
_refine_ls_R_factor_gt           0.0799
_refine_ls_restrained_S_all      1.160
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+47.7888P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2081
_refine_ls_wR_factor_ref         0.2129
_refine_special_details          
;
 Refined as a 2-component twin.
;
_olex2_refinement_description    
;
1. Twinned data refinement
 Scales: 0.769(4)
 0.231(4)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H) groups, All O(H,H) groups
3.a Free rotating group:
 O2(H2a,H2b)
3.b Rotating group:
 O8(H8)
3.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C7(H7), C10(H10), C15(H15), C25(H25), C30(H30), C31(H31), C38(H38),
 C40(H40), C43(H43), C46(H46), C49(H49)
;
_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
Dy1 Dy 0.21010(11) 0.76799(5) 0.24788(4) 0.01846(17) Uani 1 1 d . . . . .
O4 O 0.5186(18) 0.8383(7) 0.3562(5) 0.026(2) Uani 1 1 d . . . . .
O5 O 0.8994(18) 0.6570(7) 0.1681(6) 0.027(2) Uani 1 1 d . . . . .
O8 O 0.252(2) 0.6292(8) 0.3295(7) 0.034(2) Uani 1 1 d . . . . .
H8 H 0.408350 0.612234 0.334732 0.052 Uiso 1 1 d R U . . .
O14 O 0.183(2) 0.8103(7) 0.1053(6) 0.030(2) Uani 1 1 d . . . . .
O16 O 0.007(2) 0.9279(9) 0.2466(7) 0.032(2) Uani 1 1 d . . . . .
O18 O 0.4894(19) 0.6621(7) 0.1942(6) 0.029(2) Uani 1 1 d . . . . .
O19 O 0.9098(19) 0.7775(7) 0.3423(6) 0.028(2) Uani 1 1 d . . . . .
C22 C 0.666(2) 0.6299(9) 0.1534(7) 0.016(2) Uani 1 1 d . . . . .
O26 O 0.5000(18) 0.8886(7) 0.1930(6) 0.026(2) Uani 1 1 d . . . . .
N2 N 0.889(2) 0.4251(8) 0.1053(7) 0.024(2) Uani 1 1 d . . . . .
N5 N 0.891(3) 0.4398(10) 0.1874(7) 0.032(3) Uani 1 1 d . . . . .
N8 N 0.525(2) 1.1001(8) 0.1602(7) 0.025(2) Uani 1 1 d . . . . .
N10 N 1.114(2) 0.7957(9) 0.5167(7) 0.025(2) Uani 1 1 d . . . . .
N12 N 0.322(2) 1.0935(9) 0.2048(7) 0.031(3) Uani 1 1 d . . . . .
C2 C 0.817(2) 1.0212(10) 0.4375(8) 0.023(3) Uani 1 1 d . . . . .
H2 H 0.693528 1.035965 0.396309 0.028 Uiso 1 1 calc R U . . .
N19 N 1.342(3) 0.7560(13) 0.5209(9) 0.050(4) Uani 1 1 d . . . . .
O2 O 0.696(3) 0.5335(12) 0.3338(8) 0.054(3) Uani 1 1 d G . . . .
H2A H 0.827289 0.575677 0.345817 0.080 Uiso 1 1 d G U . . .
H2B H 0.689575 0.515104 0.282676 0.080 Uiso 1 1 d G U . . .
C4 C 0.510(3) 1.0471(10) 0.0795(8) 0.023(3) Uani 1 1 d . . . . .
C5 C 0.695(2) 0.4656(9) 0.0526(8) 0.019(2) Uani 1 1 d . . . . .
C7 C 0.385(2) 0.5875(9) 0.0233(8) 0.022(3) Uani 1 1 d . . . . .
H7 H 0.304205 0.646965 0.039456 0.026 Uiso 1 1 calc R U . . .
C10 C 0.921(3) 0.7285(11) 0.5241(10) 0.033(3) Uani 1 1 d . . . . .
H10 H 0.746866 0.739791 0.523379 0.040 Uiso 1 1 calc R U . . .
C14 C 0.758(3) 0.8375(9) 0.3757(7) 0.020(2) Uani 1 1 d . . . . .
C15 C 1.098(3) 0.3928(13) 0.2128(10) 0.039(4) Uani 1 1 d . . . . .
H15 H 1.153588 0.390396 0.267699 0.047 Uiso 1 1 calc R U . . .
C17 C 0.581(2) 0.5574(9) 0.0775(7) 0.019(2) Uani 1 1 d . . . . .
C20 C 1.058(3) 0.8998(10) 0.5062(8) 0.024(3) Uani 1 1 d . . . . .
C21 C 0.877(2) 0.9198(10) 0.4427(8) 0.022(2) Uani 1 1 d . . . . .
C25 C 1.035(4) 0.6427(12) 0.5327(12) 0.050(5) Uani 1 1 d . . . . .
H25 H 0.948391 0.581118 0.538845 0.060 Uiso 1 1 calc R U . . .
C28 C 0.366(3) 0.8755(10) 0.1236(8) 0.024(3) Uani 1 1 d . . . . .
C30 C 0.401(3) 1.1559(12) 0.2741(9) 0.034(3) Uani 1 1 d . . . . .
H30 H 0.303923 1.167567 0.317406 0.041 Uiso 1 1 calc R U . . .
C31 C 1.082(3) 0.3693(11) 0.0814(9) 0.030(3) Uani 1 1 d . . . . .
H31 H 1.113673 0.349414 0.027952 0.036 Uiso 1 1 calc R U . . .
C34 C 0.431(3) 0.9434(10) 0.0611(8) 0.024(3) Uani 1 1 d . . . . .
C38 C 1.223(3) 0.3478(12) 0.1504(11) 0.039(4) Uani 1 1 d . . . . .
H38 H 1.370335 0.310995 0.154546 0.047 Uiso 1 1 calc R U . . .
C40 C 1.295(4) 0.6544(13) 0.5316(10) 0.043(4) Uani 1 1 d . . . . .
H40 H 1.414399 0.604667 0.536951 0.052 Uiso 1 1 calc R U . . .
C43 C 0.421(3) 0.8987(11) -0.0194(9) 0.029(3) Uani 1 1 d . . . . .
H43 H 0.366098 0.829530 -0.033045 0.035 Uiso 1 1 calc R U . . .
C46 C 0.719(3) 1.1645(12) 0.2003(9) 0.033(3) Uani 1 1 d . . . . .
H46 H 0.874046 1.180766 0.181359 0.040 Uiso 1 1 calc R U . . .
C49 C 0.646(3) 1.2013(12) 0.2735(9) 0.035(3) Uani 1 1 d . . . . .
H49 H 0.740160 1.247401 0.314759 0.042 Uiso 1 1 calc R U . . .
H16A H -0.16(3) 0.923(10) 0.225(8) 0.01(3) Uiso 1 1 d . . . . .
H16B H 0.09(3) 0.963(11) 0.236(9) 0.01(4) Uiso 1 1 d . . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Dy1 O4 2.334(9) . ?
Dy1 O5 2.302(9) 1_455 ?
Dy1 O8 2.410(10) . ?
Dy1 O14 2.494(9) . ?
Dy1 O16 2.397(10) . ?
Dy1 O18 2.246(9) . ?
Dy1 O19 2.346(9) 1_455 ?
Dy1 O26 2.472(9) . ?
Dy1 C28 2.824(13) . ?
O4 C14 1.255(15) . ?
O5 C22 1.245(15) . ?
O8 H8 0.8573 . ?
O14 C28 1.238(16) . ?
O16 H16A 0.90(14) . ?
O16 H16B 0.66(15) . ?
O18 C22 1.266(14) . ?
O19 C14 1.270(15) . ?
C22 C17 1.488(15) . ?
O26 C28 1.265(16) . ?
N2 N5 1.353(16) . ?
N2 C5 1.428(16) . ?
N2 C31 1.345(17) . ?
N5 C15 1.324(19) . ?
N8 N12 1.368(15) . ?
N8 C4 1.422(16) . ?
N8 C46 1.345(18) . ?
N10 N19 1.326(18) . ?
N10 C10 1.335(17) . ?
N10 C20 1.436(17) . ?
N12 C30 1.335(19) . ?
C2 H2 0.9300 . ?
C2 C20 1.386(18) 2_776 ?
C2 C21 1.393(18) . ?
N19 C40 1.38(2) . ?
O2 H2A 0.8505 . ?
O2 H2B 0.8500 . ?
C4 C34 1.387(18) . ?
C4 C43 1.371(19) 2_675 ?
C5 C7 1.370(17) 2_665 ?
C5 C17 1.406(16) . ?
C7 H7 0.9300 . ?
C7 C17 1.387(17) . ?
C10 H10 0.9300 . ?
C10 C25 1.31(2) . ?
C14 C21 1.503(17) . ?
C15 H15 0.9300 . ?
C15 C38 1.38(2) . ?
C20 C21 1.394(18) . ?
C25 H25 0.9300 . ?
C25 C40 1.36(3) . ?
C28 C34 1.511(18) . ?
C30 H30 0.9300 . ?
C30 C49 1.39(2) . ?
C31 H31 0.9300 . ?
C31 C38 1.36(2) . ?
C34 C43 1.385(18) . ?
C38 H38 0.9300 . ?
C40 H40 0.9300 . ?
C43 H43 0.9300 . ?
C46 H46 0.9300 . ?
C46 C49 1.36(2) . ?
C49 H49 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
O4 Dy1 O8 77.7(4) . . ?
O4 Dy1 O14 125.6(3) . . ?
O4 Dy1 O16 91.9(4) . . ?
O4 Dy1 O19 87.0(3) . 1_455 ?
O4 Dy1 O26 73.1(3) . . ?
O4 Dy1 C28 99.6(4) . . ?
O5 Dy1 O4 161.2(3) 1_455 . ?
O5 Dy1 O8 83.7(4) 1_455 . ?
O5 Dy1 O14 72.0(3) 1_455 . ?
O5 Dy1 O16 100.7(4) 1_455 . ?
O5 Dy1 O19 84.0(3) 1_455 1_455 ?
O5 Dy1 O26 123.9(3) 1_455 . ?
O5 Dy1 C28 97.9(4) 1_455 . ?
O8 Dy1 O14 143.8(3) . . ?
O8 Dy1 O26 137.4(3) . . ?
O8 Dy1 C28 151.0(4) . . ?
O14 Dy1 C28 26.0(3) . . ?
O16 Dy1 O8 139.5(4) . . ?
O16 Dy1 O14 73.0(4) . . ?
O16 Dy1 O26 72.4(4) . . ?
O16 Dy1 C28 69.0(4) . . ?
O18 Dy1 O4 92.2(3) . . ?
O18 Dy1 O5 84.7(3) . 1_455 ?
O18 Dy1 O8 72.9(4) . . ?
O18 Dy1 O14 78.4(4) . . ?
O18 Dy1 O16 147.4(4) . . ?
O18 Dy1 O19 141.6(4) . 1_455 ?
O18 Dy1 O26 77.9(3) . . ?
O18 Dy1 C28 78.4(4) . . ?
O19 Dy1 O8 69.4(4) 1_455 . ?
O19 Dy1 O14 131.6(4) 1_455 . ?
O19 Dy1 O16 71.0(4) 1_455 . ?
O19 Dy1 O26 137.4(3) 1_455 . ?
O19 Dy1 C28 139.6(4) 1_455 . ?
O26 Dy1 O14 52.5(3) . . ?
O26 Dy1 C28 26.6(3) . . ?
C14 O4 Dy1 138.0(8) . . ?
C22 O5 Dy1 146.0(8) . 1_655 ?
Dy1 O8 H8 109.8 . . ?
C28 O14 Dy1 92.0(8) . . ?
Dy1 O16 H16A 116(8) . . ?
Dy1 O16 H16B 110(10) . . ?
H16A O16 H16B 119(10) . . ?
C22 O18 Dy1 160.3(9) . . ?
C14 O19 Dy1 142.7(9) . 1_655 ?
O5 C22 O18 126.5(11) . . ?
O5 C22 C17 117.2(10) . . ?
O18 C22 C17 116.2(11) . . ?
C28 O26 Dy1 92.4(8) . . ?
N5 N2 C5 121.4(11) . . ?
C31 N2 N5 112.7(12) . . ?
C31 N2 C5 125.9(11) . . ?
C15 N5 N2 102.5(12) . . ?
N12 N8 C4 121.0(11) . . ?
C46 N8 N12 111.9(11) . . ?
C46 N8 C4 127.0(12) . . ?
N19 N10 C10 113.5(13) . . ?
N19 N10 C20 127.2(13) . . ?
C10 N10 C20 119.3(12) . . ?
C30 N12 N8 103.8(12) . . ?
C20 C2 H2 120.1 2_776 . ?
C20 C2 C21 119.8(12) 2_776 . ?
C21 C2 H2 120.1 . . ?
N10 N19 C40 105.2(15) . . ?
H2A O2 H2B 104.5 . . ?
C34 C4 N8 121.8(12) . . ?
C43 C4 N8 118.1(12) 2_675 . ?
C43 C4 C34 120.1(12) 2_675 . ?
C7 C5 N2 119.1(11) 2_665 . ?
C7 C5 C17 119.3(11) 2_665 . ?
C17 C5 N2 121.5(11) . . ?
C5 C7 H7 118.2 2_665 . ?
C5 C7 C17 123.6(11) 2_665 . ?
C17 C7 H7 118.2 . . ?
N10 C10 H10 128.0 . . ?
C25 C10 N10 104.0(14) . . ?
C25 C10 H10 128.0 . . ?
O4 C14 O19 126.8(12) . . ?
O4 C14 C21 116.4(11) . . ?
O19 C14 C21 116.8(12) . . ?
N5 C15 H15 123.2 . . ?
N5 C15 C38 113.7(14) . . ?
C38 C15 H15 123.2 . . ?
C5 C17 C22 125.8(11) . . ?
C7 C17 C22 116.9(10) . . ?
C7 C17 C5 117.0(11) . . ?
C2 C20 N10 118.1(12) 2_776 . ?
C2 C20 C21 121.3(12) 2_776 . ?
C21 C20 N10 120.5(11) . . ?
C2 C21 C14 118.2(11) . . ?
C2 C21 C20 118.8(12) . . ?
C20 C21 C14 122.8(12) . . ?
C10 C25 H25 124.0 . . ?
C10 C25 C40 112.1(16) . . ?
C40 C25 H25 124.0 . . ?
O14 C28 Dy1 62.0(7) . . ?
O14 C28 O26 122.7(12) . . ?
O14 C28 C34 118.8(12) . . ?
O26 C28 Dy1 61.0(7) . . ?
O26 C28 C34 118.5(12) . . ?
C34 C28 Dy1 173.1(9) . . ?
N12 C30 H30 124.2 . . ?
N12 C30 C49 111.5(13) . . ?
C49 C30 H30 124.2 . . ?
N2 C31 H31 126.6 . . ?
N2 C31 C38 106.7(14) . . ?
C38 C31 H31 126.6 . . ?
C4 C34 C28 124.3(12) . . ?
C43 C34 C4 117.7(12) . . ?
C43 C34 C28 118.0(12) . . ?
C15 C38 H38 127.8 . . ?
C31 C38 C15 104.4(13) . . ?
C31 C38 H38 127.8 . . ?
N19 C40 H40 127.4 . . ?
C25 C40 N19 105.2(14) . . ?
C25 C40 H40 127.4 . . ?
C4 C43 C34 122.2(12) 2_675 . ?
C4 C43 H43 118.9 2_675 . ?
C34 C43 H43 118.9 . . ?
N8 C46 H46 126.5 . . ?
N8 C46 C49 107.0(14) . . ?
C49 C46 H46 126.5 . . ?
C30 C49 H49 127.1 . . ?
C46 C49 C30 105.7(13) . . ?
C46 C49 H49 127.1 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Dy1 O4 C14 O19 -13(2) . . . . ?
Dy1 O4 C14 C21 163.6(9) . . . . ?
Dy1 O5 C22 O18 -7(2) 1_655 . . . ?
Dy1 O5 C22 C17 169.1(11) 1_655 . . . ?
Dy1 O14 C28 O26 6.8(14) . . . . ?
Dy1 O14 C28 C34 -172.2(11) . . . . ?
Dy1 O18 C22 O5 70(3) . . . . ?
Dy1 O18 C22 C17 -106(3) . . . . ?
Dy1 O19 C14 O4 99.6(17) 1_655 . . . ?
Dy1 O19 C14 C21 -76.9(17) 1_655 . . . ?
Dy1 O26 C28 O14 -6.9(14) . . . . ?
Dy1 O26 C28 C34 172.1(11) . . . . ?
O4 C14 C21 C2 -48.8(16) . . . . ?
O4 C14 C21 C20 135.9(13) . . . . ?
O5 C22 C17 C5 49.0(18) . . . . ?
O5 C22 C17 C7 -125.3(13) . . . . ?
O14 C28 C34 C4 141.4(14) . . . . ?
O14 C28 C34 C43 -41.1(19) . . . . ?
O18 C22 C17 C5 -134.7(13) . . . . ?
O18 C22 C17 C7 51.0(16) . . . . ?
O19 C14 C21 C2 128.1(13) . . . . ?
O19 C14 C21 C20 -47.2(18) . . . . ?
O26 C28 C34 C4 -38(2) . . . . ?
O26 C28 C34 C43 139.8(14) . . . . ?
N2 N5 C15 C38 -1.0(18) . . . . ?
N2 C5 C17 C22 9(2) . . . . ?
N2 C5 C17 C7 -176.8(11) . . . . ?
N2 C31 C38 C15 0.6(17) . . . . ?
N5 N2 C5 C7 -147.7(13) . . . 2_665 ?
N5 N2 C5 C17 30.9(18) . . . . ?
N5 N2 C31 C38 -1.3(17) . . . . ?
N5 C15 C38 C31 0(2) . . . . ?
N8 N12 C30 C49 0.2(17) . . . . ?
N8 C4 C34 C28 -3(2) . . . . ?
N8 C4 C34 C43 179.5(13) . . . . ?
N8 C46 C49 C30 -0.2(17) . . . . ?
N10 N19 C40 C25 0.2(18) . . . . ?
N10 C10 C25 C40 1(2) . . . . ?
N10 C20 C21 C2 176.2(12) . . . . ?
N10 C20 C21 C14 -9(2) . . . . ?
N12 N8 C4 C34 -49.6(19) . . . . ?
N12 N8 C4 C43 130.9(14) . . . 2_675 ?
N12 N8 C46 C49 0.4(17) . . . . ?
N12 C30 C49 C46 0.0(19) . . . . ?
C2 C20 C21 C2 -2(2) 2_776 . . . ?
C2 C20 C21 C14 173.6(12) 2_776 . . . ?
N19 N10 C10 C25 -0.4(18) . . . . ?
N19 N10 C20 C2 -57.0(19) . . . 2_776 ?
N19 N10 C20 C21 125.1(15) . . . . ?
C4 N8 N12 C30 -177.2(12) . . . . ?
C4 N8 C46 C49 176.9(13) . . . . ?
C4 C34 C43 C4 1(2) . . . 2_675 ?
C5 N2 N5 C15 -179.0(12) . . . . ?
C5 N2 C31 C38 179.1(13) . . . . ?
C5 C7 C17 C22 173.0(12) 2_665 . . . ?
C5 C7 C17 C5 -2(2) 2_665 . . . ?
C7 C5 C17 C22 -172.5(12) 2_665 . . . ?
C7 C5 C17 C7 2(2) 2_665 . . . ?
C10 N10 N19 C40 0.2(17) . . . . ?
C10 N10 C20 C2 122.5(15) . . . 2_776 ?
C10 N10 C20 C21 -55.5(18) . . . . ?
C10 C25 C40 N19 0(2) . . . . ?
C20 N10 N19 C40 179.6(13) . . . . ?
C20 N10 C10 C25 -179.9(13) . . . . ?
C20 C2 C21 C14 -173.9(12) 2_776 . . . ?
C20 C2 C21 C20 2(2) 2_776 . . . ?
C28 C34 C43 C4 -176.5(13) . . . 2_675 ?
C31 N2 N5 C15 1.3(16) . . . . ?
C31 N2 C5 C7 31.9(19) . . . 2_665 ?
C31 N2 C5 C17 -149.5(13) . . . . ?
C43 C4 C34 C28 176.4(13) 2_675 . . . ?
C43 C4 C34 C43 -1(2) 2_675 . . . ?
C46 N8 N12 C30 -0.4(16) . . . . ?
C46 N8 C4 C34 134.1(15) . . . . ?
C46 N8 C4 C43 -45(2) . . . 2_675 ?

_olex2_submission_special_instructions 'No special instructions were received'
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.769(4)
2 0.231(4)

####################################################################### 
# 
# 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_sxcsm
_database_code_depnum_ccdc_archive 'CCDC 2184517'
loop_
_audit_author_name
_audit_author_address
'Sun Xuechun'
;Shenyang University of Chemical Technology
China
;
_audit_update_record             
;
2022-07-06 deposited with the CCDC.	2022-09-15 downloaded from the CCDC.
;
_audit_creation_date             2022-05-07
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.02.04 svn.rd84adfe8 for OlexSys, GUI svn.r6032)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        sxc
_chemical_formula_moiety         'C21 H14 N6 O8 Sm, H2 O'
_chemical_formula_sum            'C21 H18 N6 O9 Sm'
_chemical_formula_weight         648.76
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   5.2631(3)
_cell_length_b                   13.1534(7)
_cell_length_c                   16.6741(10)
_cell_angle_alpha                97.062(5)
_cell_angle_beta                 96.554(5)
_cell_angle_gamma                92.507(5)
_cell_volume                     1136.11(11)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    6000
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      25
_cell_measurement_theta_min      2
_shelx_estimated_absorpt_T_max   0.777
_shelx_estimated_absorpt_T_min   0.777
_exptl_absorpt_coefficient_mu    2.652
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_type   ?
_exptl_absorpt_process_details   ?
_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    1.896
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       needle
_exptl_crystal_F_000             640
_exptl_crystal_preparation       1
_exptl_crystal_recrystallization_method 1
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0274
_diffrn_reflns_av_unetI/netI     0.0276
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            12484
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.028
_diffrn_reflns_theta_max         25.028
_diffrn_reflns_theta_min         2.756
_diffrn_ambient_temperature      298.0
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       ?
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3747
_reflns_number_total             4022
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       ?
_computing_data_collection       ?
_computing_data_reduction        ?
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve 1.3 (Bourhis et al., 2015)'
_refine_diff_density_max         1.388
_refine_diff_density_min         -0.502
_refine_diff_density_rms         0.097
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.131
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     342
_refine_ls_number_reflns         4022
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0292
_refine_ls_R_factor_gt           0.0255
_refine_ls_restrained_S_all      1.131
_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)+(0.0295P)²+1.8730P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0631
_refine_ls_wR_factor_ref         0.0653
_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) groups, All O(H,H) groups
2.a Riding coordinates:
 C63(H63), C25(H25), C29(H29), C37(H37)
2.b Free rotating group:
 O65(H65A,H65B)
2.c Rotating group:
 O15(H15A)
2.d Aromatic/amide H refined with riding coordinates:
 C47(H47), C48(H48), C51(H51), C56(H56), C60(H60), C64(H64), C67(H67), C75(H75)
;
_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 0.20839(3) 0.76717(2) 0.24900(2) 0.01797(8) Uani 1 1 d . . . . .
O1 O -0.0955(5) 0.7767(2) 0.34555(16) 0.0287(6) Uani 1 1 d . . . . .
O2 O 0.4996(5) 0.8891(2) 0.19298(16) 0.0263(6) Uani 1 1 d . . . . .
O4 O -0.4785(5) 0.8391(2) 0.35811(16) 0.0275(6) Uani 1 1 d . . . . .
O7 O -0.1048(5) 0.6564(2) 0.16739(17) 0.0299(6) Uani 1 1 d . . . . .
O11 O 0.1900(6) 0.8111(2) 0.10522(17) 0.0324(7) Uani 1 1 d . . . . .
O15 O 0.0027(7) 0.9311(2) 0.2469(2) 0.0327(7) Uani 1 1 d . . . . .
H15A H 0.105866 0.976580 0.232741 0.049 Uiso 1 1 d R U . . .
O16 O 0.2568(6) 0.6259(2) 0.33342(18) 0.0364(7) Uani 1 1 d . . . . .
O17 O 0.4952(5) 0.6580(2) 0.19520(16) 0.0299(6) Uani 1 1 d . . . . .
N8 N 0.1087(6) 0.7958(2) 0.51834(19) 0.0243(7) Uani 1 1 d . . . . .
N14 N -0.1159(6) 0.4241(2) 0.10375(19) 0.0229(7) Uani 1 1 d . . . . .
N18 N 0.5208(6) 1.1004(2) 0.15926(19) 0.0235(7) Uani 1 1 d . . . . .
N26 N 0.3226(7) 1.0942(3) 0.2040(2) 0.0288(7) Uani 1 1 d . . . . .
N43 N -0.1111(7) 0.4379(3) 0.1854(2) 0.0335(8) Uani 1 1 d . . . . .
N59 N -0.0857(8) 0.7303(3) 0.5260(3) 0.0427(10) Uani 1 1 d . . . . .
C63 C 0.3352(9) 0.7552(3) 0.5225(3) 0.0333(10) Uani 1 1 d . . . . .
H63 H 0.512576 0.802814 0.521300 0.040 Uiso 1 1 d R U . . .
C9 C -0.3088(7) 0.4650(3) 0.0522(2) 0.0195(7) Uani 1 1 d . . . . .
C23 C -0.4211(7) 0.5561(3) 0.0769(2) 0.0189(7) Uani 1 1 d . . . . .
C25 C -0.1784(7) 1.0208(3) 0.4382(2) 0.0246(8) Uani 1 1 d . . . . .
H25 H -0.316072 1.034771 0.401865 0.029 Uiso 1 1 d R U . . .
C27 C -0.1247(7) 0.9199(3) 0.4441(2) 0.0219(8) Uani 1 1 d . . . . .
C28 C -0.3350(7) 0.6281(3) 0.1537(2) 0.0198(8) Uani 1 1 d . . . . .
C29 C -0.6136(7) 0.5883(3) 0.0240(2) 0.0207(8) Uani 1 1 d . . . . .
H29 H -0.696096 0.646903 0.040799 0.025 Uiso 1 1 d R U . . .
C35 C 0.5097(8) 1.0474(3) 0.0790(2) 0.0249(8) Uani 1 1 d . . . . .
C37 C 0.4213(8) 0.8982(3) -0.0189(2) 0.0273(9) Uani 1 1 d . . . . .
H37 H 0.381140 0.827993 -0.030275 0.033 Uiso 1 1 d R U . . .
C38 C -0.2426(7) 0.8378(3) 0.3778(2) 0.0210(8) Uani 1 1 d . . . . .
C39 C 0.0571(7) 0.9007(3) 0.5071(2) 0.0226(8) Uani 1 1 d . . . . .
C47 C 0.0281(11) 0.6439(4) 0.5360(3) 0.0471(12) Uani 1 1 d . . . . .
H47 H -0.057740 0.583060 0.543490 0.057 Uiso 1 1 calc R U . . .
C48 C 0.4004(9) 1.1554(3) 0.2722(3) 0.0335(10) Uani 1 1 d . . . . .
H48 H 0.303708 1.166631 0.315469 0.040 Uiso 1 1 calc R U . . .
C50 C 0.4325(8) 0.9440(3) 0.0613(2) 0.0255(8) Uani 1 1 d . . . . .
C51 C 0.7117(8) 1.1642(3) 0.1985(3) 0.0313(9) Uani 1 1 d . . . . .
H51 H 0.864961 1.180724 0.179004 0.038 Uiso 1 1 calc R U . . .
C54 C 0.3693(8) 0.8773(3) 0.1237(2) 0.0243(8) Uani 1 1 d . . . . .
C56 C 0.0777(8) 0.3690(3) 0.0801(3) 0.0328(10) Uani 1 1 d . . . . .
H56 H 0.110149 0.349749 0.026801 0.039 Uiso 1 1 calc R U . . .
C60 C 0.0921(9) 0.3919(3) 0.2113(3) 0.0390(11) Uani 1 1 d . . . . .
H60 H 0.147079 0.389632 0.266050 0.047 Uiso 1 1 calc R U . . .
C64 C 0.6415(9) 1.2004(3) 0.2717(3) 0.0372(10) Uani 1 1 d . . . . .
H64 H 0.735317 1.245784 0.312765 0.045 Uiso 1 1 calc R U . . .
C67 C 0.2892(10) 0.6551(4) 0.5339(3) 0.0436(12) Uani 1 1 d . . . . .
H67 H 0.408160 0.605380 0.539173 0.052 Uiso 1 1 calc R U . . .
C75 C 0.2164(9) 0.3470(4) 0.1485(3) 0.0398(11) Uani 1 1 d . . . . .
H75 H 0.362744 0.309851 0.152406 0.048 Uiso 1 1 calc R U . . .
O65 O 0.6974(8) 0.5315(3) 0.3340(2) 0.0558(10) Uani 1 1 d G . . . .
H65A H 0.792362 0.585897 0.335722 0.084 Uiso 1 1 d G U . . .
H65B H 0.694931 0.501940 0.285658 0.084 Uiso 1 1 d G U . . .
H15B H -0.119(9) 0.928(4) 0.234(3) 0.021(14) Uiso 1 1 d . . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Sm1 O1 2.392(3) . ?
Sm1 O2 2.505(3) . ?
Sm1 O4 2.383(3) 1_655 ?
Sm1 O7 2.341(3) . ?
Sm1 O11 2.527(3) . ?
Sm1 O15 2.457(3) . ?
Sm1 O16 2.470(3) . ?
Sm1 O17 2.308(3) . ?
Sm1 C54 2.868(4) . ?
O1 C38 1.256(5) . ?
O2 C54 1.263(5) . ?
O4 C38 1.249(5) . ?
O7 C28 1.239(5) . ?
O11 C54 1.241(5) . ?
O15 H15A 0.8624 . ?
O15 H15B 0.65(5) . ?
O17 C28 1.240(5) 1_655 ?
N8 N59 1.336(5) . ?
N8 C63 1.326(5) . ?
N8 C39 1.447(5) . ?
N14 N43 1.349(5) . ?
N14 C9 1.422(5) . ?
N14 C56 1.344(5) . ?
N18 N26 1.355(5) . ?
N18 C35 1.425(5) . ?
N18 C51 1.335(5) . ?
N26 C48 1.323(5) . ?
N43 C60 1.308(6) . ?
N59 C47 1.328(6) . ?
C63 H63 1.1048 . ?
C63 C67 1.368(7) . ?
C9 C23 1.397(5) . ?
C9 C29 1.382(5) 2_465 ?
C23 C28 1.508(5) . ?
C23 C29 1.381(5) . ?
C25 H25 0.9303 . ?
C25 C27 1.382(5) . ?
C25 C39 1.372(5) 2_576 ?
C27 C38 1.504(5) . ?
C27 C39 1.394(5) . ?
C29 H29 0.9300 . ?
C35 C37 1.373(5) 2_675 ?
C35 C50 1.388(5) . ?
C37 H37 0.9300 . ?
C37 C50 1.391(5) . ?
C47 H47 0.9300 . ?
C47 C67 1.381(7) . ?
C48 H48 0.9300 . ?
C48 C64 1.378(7) . ?
C50 C54 1.496(5) . ?
C51 H51 0.9300 . ?
C51 C64 1.353(6) . ?
C56 H56 0.9300 . ?
C56 C75 1.352(6) . ?
C60 H60 0.9300 . ?
C60 C75 1.383(7) . ?
C64 H64 0.9300 . ?
C67 H67 0.9300 . ?
C75 H75 0.9300 . ?
O65 H65A 0.8504 . ?
O65 H65B 0.8496 . ?

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 O2 137.33(9) . . ?
O1 Sm1 O11 132.57(10) . . ?
O1 Sm1 O15 71.45(10) . . ?
O1 Sm1 O16 69.70(10) . . ?
O1 Sm1 C54 139.70(10) . . ?
O2 Sm1 O11 51.56(9) . . ?
O2 Sm1 C54 26.08(10) . . ?
O4 Sm1 O1 87.15(9) 1_655 . ?
O4 Sm1 O2 72.72(9) 1_655 . ?
O4 Sm1 O11 124.28(9) 1_655 . ?
O4 Sm1 O15 91.59(11) 1_655 . ?
O4 Sm1 O16 77.44(10) 1_655 . ?
O4 Sm1 C54 98.74(11) 1_655 . ?
O7 Sm1 O1 84.54(10) . . ?
O7 Sm1 O2 123.25(9) . . ?
O7 Sm1 O4 162.32(10) . 1_655 ?
O7 Sm1 O11 72.13(9) . . ?
O7 Sm1 O15 100.48(11) . . ?
O7 Sm1 O16 85.04(10) . . ?
O7 Sm1 C54 97.70(11) . . ?
O11 Sm1 C54 25.61(10) . . ?
O15 Sm1 O2 71.94(10) . . ?
O15 Sm1 O11 73.03(10) . . ?
O15 Sm1 O16 140.00(10) . . ?
O15 Sm1 C54 68.58(11) . . ?
O16 Sm1 O2 136.76(10) . . ?
O16 Sm1 O11 144.02(10) . . ?
O16 Sm1 C54 150.55(11) . . ?
O17 Sm1 O1 141.00(10) . . ?
O17 Sm1 O2 78.34(10) . . ?
O17 Sm1 O4 91.91(10) . 1_655 ?
O17 Sm1 O7 84.87(10) . . ?
O17 Sm1 O11 78.39(10) . . ?
O17 Sm1 O15 147.51(11) . . ?
O17 Sm1 O16 72.06(10) . . ?
O17 Sm1 C54 78.96(11) . . ?
C38 O1 Sm1 141.1(2) . . ?
C54 O2 Sm1 93.2(2) . . ?
C38 O4 Sm1 138.3(2) . 1_455 ?
C28 O7 Sm1 146.2(3) . . ?
C54 O11 Sm1 92.8(2) . . ?
Sm1 O15 H15A 110.0 . . ?
Sm1 O15 H15B 116(4) . . ?
H15A O15 H15B 122.2 . . ?
C28 O17 Sm1 158.5(3) 1_655 . ?
N59 N8 C39 119.1(3) . . ?
C63 N8 N59 114.1(4) . . ?
C63 N8 C39 126.8(4) . . ?
N43 N14 C9 121.5(3) . . ?
C56 N14 N43 112.0(3) . . ?
C56 N14 C9 126.5(3) . . ?
N26 N18 C35 121.8(3) . . ?
C51 N18 N26 111.6(3) . . ?
C51 N18 C35 126.6(3) . . ?
C48 N26 N18 104.0(3) . . ?
C60 N43 N14 103.8(4) . . ?
C47 N59 N8 103.2(4) . . ?
N8 C63 H63 121.0 . . ?
N8 C63 C67 105.7(4) . . ?
C67 C63 H63 133.1 . . ?
C23 C9 N14 121.8(3) . . ?
C29 C9 N14 118.3(3) 2_465 . ?
C29 C9 C23 119.9(3) 2_465 . ?
C9 C23 C28 125.5(3) . . ?
C29 C23 C9 118.0(3) . . ?
C29 C23 C28 116.3(3) . . ?
C27 C25 H25 119.1 . . ?
C39 C25 H25 119.1 2_576 . ?
C39 C25 C27 121.1(4) 2_576 . ?
C25 C27 C38 118.8(3) . . ?
C25 C27 C39 117.7(3) . . ?
C39 C27 C38 123.1(3) . . ?
O7 C28 O17 125.8(3) . 1_455 ?
O7 C28 C23 117.5(3) . . ?
O17 C28 C23 116.5(3) 1_455 . ?
C9 C29 H29 119.0 2_465 . ?
C23 C29 C9 122.1(3) . 2_465 ?
C23 C29 H29 118.9 . . ?
C37 C35 N18 117.9(3) 2_675 . ?
C37 C35 C50 120.5(4) 2_675 . ?
C50 C35 N18 121.6(3) . . ?
C35 C37 H37 120.0 2_675 . ?
C35 C37 C50 121.3(4) 2_675 . ?
C50 C37 H37 118.5 . . ?
O1 C38 C27 117.6(3) . . ?
O4 C38 O1 126.0(3) . . ?
O4 C38 C27 116.4(3) . . ?
C25 C39 N8 119.1(3) 2_576 . ?
C25 C39 C27 121.2(4) 2_576 . ?
C27 C39 N8 119.6(3) . . ?
N59 C47 H47 124.1 . . ?
N59 C47 C67 111.8(4) . . ?
C67 C47 H47 124.1 . . ?
N26 C48 H48 124.0 . . ?
N26 C48 C64 112.1(4) . . ?
C64 C48 H48 124.0 . . ?
C35 C50 C37 118.2(4) . . ?
C35 C50 C54 124.1(4) . . ?
C37 C50 C54 117.6(3) . . ?
N18 C51 H51 126.3 . . ?
N18 C51 C64 107.5(4) . . ?
C64 C51 H51 126.3 . . ?
O2 C54 Sm1 60.67(19) . . ?
O2 C54 C50 119.6(3) . . ?
O11 C54 Sm1 61.6(2) . . ?
O11 C54 O2 121.8(3) . . ?
O11 C54 C50 118.6(4) . . ?
C50 C54 Sm1 173.3(3) . . ?
N14 C56 H56 126.6 . . ?
N14 C56 C75 106.9(4) . . ?
C75 C56 H56 126.6 . . ?
N43 C60 H60 123.6 . . ?
N43 C60 C75 112.7(4) . . ?
C75 C60 H60 123.6 . . ?
C48 C64 H64 127.6 . . ?
C51 C64 C48 104.9(4) . . ?
C51 C64 H64 127.6 . . ?
C63 C67 C47 105.1(4) . . ?
C63 C67 H67 127.4 . . ?
C47 C67 H67 127.4 . . ?
C56 C75 C60 104.6(4) . . ?
C56 C75 H75 127.7 . . ?
C60 C75 H75 127.7 . . ?
H65A O65 H65B 104.4 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Sm1 O1 C38 O4 100.3(5) . . . . ?
Sm1 O1 C38 C27 -77.1(5) . . . . ?
Sm1 O2 C54 O11 -8.1(4) . . . . ?
Sm1 O2 C54 C50 172.4(3) . . . . ?
Sm1 O4 C38 O1 -13.3(6) 1_455 . . . ?
Sm1 O4 C38 C27 164.2(3) 1_455 . . . ?
Sm1 O7 C28 O17 -5.0(7) . . . 1_455 ?
Sm1 O7 C28 C23 170.8(3) . . . . ?
Sm1 O11 C54 O2 8.1(4) . . . . ?
Sm1 O11 C54 C50 -172.4(3) . . . . ?
N8 N59 C47 C67 -0.5(5) . . . . ?
N8 C63 C67 C47 -0.2(5) . . . . ?
N14 N43 C60 C75 -1.1(5) . . . . ?
N14 C9 C23 C28 8.0(6) . . . . ?
N14 C9 C23 C29 -177.7(3) . . . . ?
N14 C56 C75 C60 0.1(5) . . . . ?
N18 N26 C48 C64 0.3(5) . . . . ?
N18 C35 C50 C37 178.6(4) . . . . ?
N18 C35 C50 C54 -3.7(6) . . . . ?
N18 C51 C64 C48 -0.7(5) . . . . ?
N26 N18 C35 C37 131.1(4) . . . 2_675 ?
N26 N18 C35 C50 -49.1(5) . . . . ?
N26 N18 C51 C64 0.9(5) . . . . ?
N26 C48 C64 C51 0.2(5) . . . . ?
N43 N14 C9 C23 31.3(5) . . . . ?
N43 N14 C9 C29 -148.3(4) . . . 2_465 ?
N43 N14 C56 C75 -0.8(5) . . . . ?
N43 C60 C75 C56 0.7(6) . . . . ?
N59 N8 C63 C67 -0.1(5) . . . . ?
N59 N8 C39 C25 122.2(4) . . . 2_576 ?
N59 N8 C39 C27 -54.2(5) . . . . ?
N59 C47 C67 C63 0.5(6) . . . . ?
C63 N8 N59 C47 0.4(5) . . . . ?
C63 N8 C39 C25 -57.4(5) . . . 2_576 ?
C63 N8 C39 C27 126.1(4) . . . . ?
C9 N14 N43 C60 -178.9(3) . . . . ?
C9 N14 C56 C75 179.3(4) . . . . ?
C9 C23 C28 O7 50.9(5) . . . . ?
C9 C23 C28 O17 -132.9(4) . . . 1_455 ?
C9 C23 C29 C9 -1.9(6) . . . 2_465 ?
C25 C27 C38 O1 128.1(4) . . . . ?
C25 C27 C38 O4 -49.6(5) . . . . ?
C25 C27 C39 N8 176.5(3) . . . . ?
C25 C27 C39 C25 0.1(6) . . . 2_576 ?
C28 C23 C29 C9 173.0(3) . . . 2_465 ?
C29 C9 C23 C28 -172.5(3) 2_465 . . . ?
C29 C9 C23 C29 1.8(6) 2_465 . . . ?
C29 C23 C28 O7 -123.5(4) . . . . ?
C29 C23 C28 O17 52.7(5) . . . 1_455 ?
C35 N18 N26 C48 -177.9(3) . . . . ?
C35 N18 C51 C64 177.9(4) . . . . ?
C35 C37 C50 C35 1.6(7) 2_675 . . . ?
C35 C37 C50 C54 -176.3(4) 2_675 . . . ?
C35 C50 C54 O2 -37.8(6) . . . . ?
C35 C50 C54 O11 142.7(4) . . . . ?
C37 C35 C50 C37 -1.5(7) 2_675 . . . ?
C37 C35 C50 C54 176.1(4) 2_675 . . . ?
C37 C50 C54 O2 139.9(4) . . . . ?
C37 C50 C54 O11 -39.6(6) . . . . ?
C38 C27 C39 N8 -10.2(6) . . . . ?
C38 C27 C39 C25 173.5(4) . . . 2_576 ?
C39 N8 N59 C47 -179.3(4) . . . . ?
C39 N8 C63 C67 179.5(4) . . . . ?
C39 C25 C27 C38 -173.8(4) 2_576 . . . ?
C39 C25 C27 C39 -0.1(6) 2_576 . . . ?
C39 C27 C38 O1 -45.2(5) . . . . ?
C39 C27 C38 O4 137.1(4) . . . . ?
C51 N18 N26 C48 -0.8(4) . . . . ?
C51 N18 C35 C37 -45.6(6) . . . 2_675 ?
C51 N18 C35 C50 134.3(4) . . . . ?
C56 N14 N43 C60 1.2(5) . . . . ?
C56 N14 C9 C23 -148.8(4) . . . . ?
C56 N14 C9 C29 31.7(6) . . . 2_465 ?

_olex2_submission_special_instructions 'No special instructions were received'
