# Electronic Supplementary Material (ESI) for CrystEngComm.
# This journal is © The Royal Society of Chemistry 2021

####################################################################### 
# 
# 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. 
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data_mo_1210_2_0m
_database_code_depnum_ccdc_archive 'CCDC 2071646'
loop_
_audit_author_name
_audit_author_address
'Yun-Shan Xue' 'Yancheng Teachers University'
_audit_update_record             
;
2021-03-19 deposited with the CCDC.	2021-04-20 downloaded from the CCDC.
;
_audit_creation_date             2020-07-30
_audit_creation_method           
;
Olex2 1.2-beta
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         '0.25(C176 H184 Ce8 N16 O72), C3 H7 N O, H2 O'
_chemical_formula_sum            'C47 H55 Ce2 N5 O20'
_chemical_formula_weight         1290.20
_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'
Ce Ce -0.2486 2.6331 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 1 2/c 1'
_space_group_name_Hall           '-C 2yc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'

_cell_length_a                   28.6190(12)
_cell_length_b                   14.2049(5)
_cell_length_c                   14.1485(6)
_cell_angle_alpha                90
_cell_angle_beta                 100.1739(14)
_cell_angle_gamma                90
_cell_volume                     5661.4(4)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    9966
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      26.42
_cell_measurement_theta_min      2.26
_shelx_estimated_absorpt_T_max   0.813
_shelx_estimated_absorpt_T_min   0.681
_exptl_absorpt_coefficient_mu    1.662
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.6316
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0874 before and 0.0547 after correction.
The Ratio of minimum to maximum transmission is 0.8473.
The λ/2 correction factor is Not present.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            ?
_exptl_crystal_density_diffrn    1.514
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             2592
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.13
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0378
_diffrn_reflns_av_unetI/netI     0.0231
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       35
_diffrn_reflns_limit_h_min       -35
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            37048
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.019
_diffrn_reflns_theta_min         2.256
_diffrn_ambient_temperature      150.01
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                5124
_reflns_number_total             5585
_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       'SAINT v8.37A (Bruker, 2015)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    
;
Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_refine_diff_density_max         1.598
_refine_diff_density_min         -0.778
_refine_diff_density_rms         0.139
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.233
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     463
_refine_ls_number_reflns         5585
_refine_ls_number_restraints     517
_refine_ls_R_factor_all          0.0464
_refine_ls_R_factor_gt           0.0419
_refine_ls_restrained_S_all      1.220
_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)+(0.0098P)²+98.4410P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1000
_refine_ls_wR_factor_ref         0.1019
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
2. Restrained distances
 Ce1-O9 = Ce1-O11
 2.5 with sigma of 0.01
 O9-C19 = O11-C26
 1.2 with sigma of 0.01
 N2-C19 = N4-C26 = N4-C27 = N2-C20 = N4-C28 = N2-C21
 1.48 with sigma of 0.01
 C19-C20
 2.5 with sigma of 0.02
 C19-C21
 2.5 with sigma of 0.02
 C21-C20
 2.5 with sigma of 0.02
 C28-C27
 2.5 with sigma of 0.02
 C26-C27
 2.5 with sigma of 0.02
 C26-C28
 2.5 with sigma of 0.02
 O11-C26
 1.2 with sigma of 0.005
 N4-C26
 1.48 with sigma of 0.01
 Ce1-C26
 3.4 with sigma of 0.02
 O11-N4
 2.3 with sigma of 0.01
 Ce1-O3A = Ce1-O3
 2.4 with sigma of 0.01
 O3-C18 = O3A-C18A
 1.2 with sigma of 0.01
 N1-C18 = N1A-C18A = N1A-C22A = N1-C22 = N1-C17 = N1A-C17A
 1.48 with sigma of 0.01
 C18A-C22A
 2.5 with sigma of 0.02
 C22A-C17A
 2.5 with sigma of 0.02
 C17A-C18A
 2.5 with sigma of 0.02
 C18-C22
 2.5 with sigma of 0.02
 C22-C17
 2.5 with sigma of 0.02
 C17-C18
 2.5 with sigma of 0.02
3. Restrained planarity
 O9, N2, C19, C20, C21
 with sigma of 0.01
 O11, N4, C26, C27, C28
 with sigma of 0.01
4. Rigid bond restraints
 C25, N3, C24
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
5. Uiso/Uaniso restraints and constraints
C21 \\sim N2 \\sim C20: within 2A with sigma of 0.01 and sigma for terminal
atoms of 0.02
O9 \\sim N2 \\sim C19 \\sim C20 \\sim C21 \\sim O11 \\sim N4 \\sim C26 \\sim
C27 \\sim C28: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
O3 \\sim N1 \\sim C17 \\sim C18 \\sim C22 \\sim O3A \\sim N1A \\sim C17A \\sim
C18A \\sim C22A: within 2A with sigma of 0.01 and sigma for terminal atoms of
0.02
Uanis(C23) \\sim Ueq, Uanis(O10) \\sim Ueq, Uanis(C24) \\sim Ueq, Uanis(C18)
\\sim Ueq, Uanis(C17) \\sim Ueq: with sigma of 0.01 and sigma for terminal
atoms of 0.02
Uanis(C21) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O9) \\sim Ueq, Uanis(N2) \\sim Ueq, Uanis(C19) \\sim Ueq, Uanis(C20)
\\sim Ueq, Uanis(C21) \\sim Ueq, Uanis(O11) \\sim Ueq, Uanis(N4) \\sim Ueq,
Uanis(C26) \\sim Ueq, Uanis(C27) \\sim Ueq, Uanis(C28) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
Uanis(O12) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O3) \\sim Ueq, Uanis(N1) \\sim Ueq, Uanis(C17) \\sim Ueq, Uanis(C18)
\\sim Ueq, Uanis(C22) \\sim Ueq, Uanis(O3A) \\sim Ueq, Uanis(N1A) \\sim Ueq,
Uanis(C17A) \\sim Ueq, Uanis(C18A) \\sim Ueq, Uanis(C22A) \\sim Ueq: with sigma
of 0.01 and sigma for terminal atoms of 0.02
6. Rigid body (RIGU) restrains
 O9, N2, C19, C20, C21, O11, N4, C26, C27, C28
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 O3, N1, C17, C18, C22, O3A, N1A, C17A, C18A, C22A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
7. Others
 Sof(O11)=Sof(N4)=Sof(C26)=Sof(H26)=Sof(C27)=Sof(H27A)=Sof(H27B)=Sof(H27C)=
 Sof(C28)=Sof(H28A)=Sof(H28B)=Sof(H28C)=1-FVAR(1)
 Sof(O9)=Sof(N2)=Sof(C19)=Sof(H19)=Sof(C20)=Sof(H20A)=Sof(H20B)=Sof(H20C)=
 Sof(C21)=Sof(H21A)=Sof(H21B)=Sof(H21C)=FVAR(1)
 Sof(O3A)=Sof(N1A)=Sof(C17A)=Sof(H17D)=Sof(H17E)=Sof(H17F)=Sof(C18A)=Sof(H18A)=
 Sof(C22A)=Sof(H22D)=Sof(H22E)=Sof(H22F)=1-FVAR(2)
 Sof(O3)=Sof(N1)=Sof(C17)=Sof(H17A)=Sof(H17B)=Sof(H17C)=Sof(C18)=Sof(H18)=
 Sof(C22)=Sof(H22A)=Sof(H22B)=Sof(H22C)=FVAR(2)
 Fixed Sof: N3(0.5) O10(0.5) C23(0.5) H23(0.5) C24(0.5) H24A(0.5) H24B(0.5)
 H24C(0.5) C25(0.5) H25A(0.5) H25B(0.5) H25C(0.5) O12(0.5) H12A(0.5) H12B(0.5)
8.a Riding coordinates:
 O12(H12A,H12B)
8.b Secondary CH2 refined with riding coordinates:
 C14(H14A,H14B)
8.c Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C7(H7), C9(H9), C10(H10), C15(H15), C16(H16), C18(H18),
 C19(H19), C23(H23), C26(H26), C18A(H18A)
8.d Idealised Me refined as rotating group:
 C17(H17A,H17B,H17C), C20(H20A,H20B,H20C), C21(H21A,H21B,H21C), C22(H22A,H22B,
 H22C), C24(H24A,H24B,H24C), C25(H25A,H25B,H25C), C27(H27A,H27B,H27C), C28(H28A,
 H28B,H28C), C17A(H17D,H17E,H17F), C22A(H22D,H22E,H22F)
;
_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
Ce1 Ce 0.31969(2) 0.21522(2) 0.54370(2) 0.01101(9) Uani 1 1 d D . . . .
O1 O 0.60200(14) 0.1861(3) 0.0019(3) 0.0304(10) Uani 1 1 d . . . . .
O2 O 0.30171(13) 0.2708(3) 0.3763(3) 0.0196(8) Uani 1 1 d . . . . .
O3 O 0.3557(4) 0.2903(10) 0.6960(6) 0.035(2) Uani 0.704(10) 1 d D U P A 1
O4 O 0.26619(12) 0.6487(2) 0.0405(3) 0.0165(7) Uani 1 1 d . . . . .
O5 O 0.20255(12) 0.5680(3) 0.0600(3) 0.0222(8) Uani 1 1 d . . . . .
O6 O 0.39776(13) 0.4173(3) 0.1467(3) 0.0229(9) Uani 1 1 d . . . . .
O7 O 0.22894(13) 0.3328(3) 0.3350(3) 0.0239(9) Uani 1 1 d . . . . .
O8 O 0.61429(14) 0.3382(3) -0.0130(3) 0.0259(9) Uani 1 1 d . . . . .
C1 C 0.4797(3) 0.2303(5) 0.1159(7) 0.052(2) Uani 1 1 d . . . . .
H1 H 0.463196 0.178326 0.136534 0.062 Uiso 1 1 calc R . . . .
C2 C 0.5194(2) 0.2149(5) 0.0739(6) 0.0437(19) Uani 1 1 d . . . . .
H2 H 0.529204 0.152377 0.063616 0.052 Uiso 1 1 calc R . . . .
C3 C 0.58985(18) 0.2716(4) 0.0084(4) 0.0208(12) Uani 1 1 d . . . . .
C4 C 0.27787(18) 0.5066(4) 0.1325(4) 0.0148(10) Uani 1 1 d . . . . .
C5 C 0.27143(18) 0.3243(4) 0.3265(4) 0.0159(10) Uani 1 1 d . . . . .
O9 O 0.3605(3) 0.0851(5) 0.6502(5) 0.0282(17) Uani 0.657(8) 1 d D U P A 1
C6 C 0.24688(18) 0.5783(4) 0.0750(4) 0.0156(10) Uani 1 1 d . . . . .
C7 C 0.32451(18) 0.4956(4) 0.1177(4) 0.0156(10) Uani 1 1 d . . . . .
H7 H 0.336810 0.534903 0.073567 0.019 Uiso 1 1 calc R . . . .
C8 C 0.28912(17) 0.3841(4) 0.2515(4) 0.0149(10) Uani 1 1 d . . . . .
C9 C 0.25987(17) 0.4493(4) 0.1977(4) 0.0149(10) Uani 1 1 d . . . . .
H9 H 0.227644 0.455005 0.205081 0.018 Uiso 1 1 calc R . . . .
C10 C 0.33567(18) 0.3713(4) 0.2364(4) 0.0162(10) Uani 1 1 d . . . . .
H10 H 0.355498 0.325491 0.272337 0.019 Uiso 1 1 calc R . . . .
C11 C 0.35273(18) 0.4260(4) 0.1686(4) 0.0168(11) Uani 1 1 d . . . . .
C12 C 0.54489(19) 0.2906(4) 0.0471(4) 0.0250(12) Uani 1 1 d . . . . .
C13 C 0.4640(2) 0.3212(5) 0.1277(5) 0.0326(15) Uani 1 1 d . . . . .
C14 C 0.4220(2) 0.3324(5) 0.1782(5) 0.0381(17) Uani 1 1 d . . . . .
H14A H 0.400208 0.278108 0.163185 0.046 Uiso 1 1 calc R . . . .
H14B H 0.432950 0.334408 0.248525 0.046 Uiso 1 1 calc R . . . .
C15 C 0.5294(2) 0.3804(4) 0.0590(5) 0.0286(14) Uani 1 1 d . . . . .
H15 H 0.546080 0.432466 0.039032 0.034 Uiso 1 1 calc R . . . .
N1 N 0.3761(3) 0.3806(7) 0.8294(6) 0.050(2) Uani 0.704(10) 1 d D U P A 1
C16 C 0.4891(2) 0.3961(4) 0.1004(5) 0.0328(15) Uani 1 1 d . . . . .
H16 H 0.479016 0.458612 0.109606 0.039 Uiso 1 1 calc R . . . .
N2 N 0.3861(2) 0.0096(5) 0.7972(6) 0.0425(19) Uani 0.657(8) 1 d D U P A 1
C17 C 0.4222(4) 0.4038(12) 0.8065(9) 0.058(3) Uani 0.704(10) 1 d D U P A 1
H17A H 0.447239 0.376934 0.855319 0.087 Uiso 0.704(10) 1 calc GR . P A 1
H17B H 0.425869 0.472415 0.805325 0.087 Uiso 0.704(10) 1 calc GR . P A 1
H17C H 0.424758 0.377897 0.743414 0.087 Uiso 0.704(10) 1 calc GR . P A 1
C18 C 0.3439(4) 0.3251(8) 0.7641(6) 0.044(2) Uani 0.704(10) 1 d D U P A 1
H18 H 0.312494 0.315793 0.775408 0.053 Uiso 0.704(10) 1 calc R . P A 1
C19 C 0.3730(2) 0.0875(7) 0.7353(6) 0.038(2) Uani 0.657(8) 1 d D U P A 1
H19 H 0.374325 0.147859 0.764661 0.046 Uiso 0.657(8) 1 calc R . P A 1
N3 N 0.2808(4) -0.1673(8) 0.5442(8) 0.036(3) Uani 0.5 1 d . U P B -1
C20 C 0.4009(4) 0.0253(8) 0.8998(6) 0.049(3) Uani 0.657(8) 1 d D U P A 1
H20A H 0.435382 0.034669 0.914253 0.074 Uiso 0.657(8) 1 calc GR . P A 1
H20B H 0.392391 -0.029485 0.935212 0.074 Uiso 0.657(8) 1 calc GR . P A 1
H20C H 0.384966 0.081390 0.918998 0.074 Uiso 0.657(8) 1 calc GR . P A 1
O10 O 0.3371(4) -0.2048(8) 0.4498(9) 0.060(3) Uani 0.5 1 d . U P B -1
C21 C 0.3855(5) -0.0858(7) 0.7606(9) 0.061(3) Uani 0.657(8) 1 d D U P A 1
H21A H 0.361419 -0.122541 0.785655 0.092 Uiso 0.657(8) 1 calc GR . P A 1
H21B H 0.416765 -0.114749 0.781124 0.092 Uiso 0.657(8) 1 calc GR . P A 1
H21C H 0.378001 -0.084670 0.690297 0.092 Uiso 0.657(8) 1 calc GR . P A 1
C22 C 0.3587(5) 0.4268(10) 0.9089(7) 0.065(3) Uani 0.704(10) 1 d D U P A 1
H22A H 0.376998 0.404810 0.970057 0.097 Uiso 0.704(10) 1 calc GR . P A 1
H22B H 0.325075 0.411363 0.906074 0.097 Uiso 0.704(10) 1 calc GR . P A 1
H22C H 0.362264 0.495122 0.903868 0.097 Uiso 0.704(10) 1 calc GR . P A 1
C23 C 0.3215(5) -0.1509(10) 0.5043(10) 0.037(3) Uani 0.5 1 d . U P B -1
H23 H 0.338219 -0.093815 0.520661 0.044 Uiso 0.5 1 calc R . P B -1
C24 C 0.2649(6) -0.1001(12) 0.6091(12) 0.049(4) Uani 0.5 1 d . U P B -1
H24A H 0.286364 -0.045827 0.617536 0.073 Uiso 0.5 1 calc GR . P B -1
H24B H 0.264777 -0.130094 0.671378 0.073 Uiso 0.5 1 calc GR . P B -1
H24C H 0.232685 -0.078924 0.581987 0.073 Uiso 0.5 1 calc GR . P B -1
C25 C 0.253(2) -0.262(3) 0.508(5) 0.066(9) Uani 0.5 1 d . U P B -1
H25A H 0.225680 -0.246185 0.458566 0.099 Uiso 0.5 1 calc GR . P B -1
H25B H 0.242754 -0.293127 0.561708 0.099 Uiso 0.5 1 calc GR . P B -1
H25C H 0.274579 -0.303406 0.479952 0.099 Uiso 0.5 1 calc GR . P B -1
O11 O 0.3515(6) 0.0682(9) 0.6221(10) 0.041(3) Uani 0.343(8) 1 d D U P A 2
N4 N 0.3578(5) -0.0581(8) 0.7217(9) 0.044(3) Uani 0.343(8) 1 d D U P A 2
C26 C 0.3705(5) 0.0380(9) 0.6980(10) 0.043(3) Uani 0.343(8) 1 d D U P A 2
H26 H 0.392719 0.074413 0.740776 0.051 Uiso 0.343(8) 1 calc R . P A 2
C27 C 0.3802(8) -0.0984(16) 0.8139(12) 0.060(5) Uani 0.343(8) 1 d D U P A 2
H27A H 0.414059 -0.082123 0.826404 0.091 Uiso 0.343(8) 1 calc GR . P A 2
H27B H 0.376703 -0.166991 0.811641 0.091 Uiso 0.343(8) 1 calc GR . P A 2
H27C H 0.365018 -0.072944 0.865232 0.091 Uiso 0.343(8) 1 calc GR . P A 2
C28 C 0.3237(9) -0.1123(17) 0.6552(18) 0.092(8) Uani 0.343(8) 1 d D U P A 2
H28A H 0.301478 -0.069500 0.615796 0.138 Uiso 0.343(8) 1 calc GR . P A 2
H28B H 0.306097 -0.154285 0.691362 0.138 Uiso 0.343(8) 1 calc GR . P A 2
H28C H 0.340459 -0.149884 0.613672 0.138 Uiso 0.343(8) 1 calc GR . P A 2
O12 O 0.4253(7) 0.0186(15) 0.9953(12) 0.129(7) Uani 0.5 1 d . U P C 3
H12A H 0.443510 0.036620 0.955605 0.194 Uiso 0.5 1 d R . P C 3
H12B H 0.415460 0.067709 1.022985 0.194 Uiso 0.5 1 d R . P C 3
O3A O 0.3615(12) 0.278(3) 0.6940(12) 0.043(3) Uani 0.296(10) 1 d D U P A 2
N1A N 0.3794(8) 0.3326(17) 0.8520(13) 0.055(3) Uani 0.296(10) 1 d D U P A 2
C17A C 0.4188(13) 0.393(3) 0.838(2) 0.064(6) Uani 0.296(10) 1 d D U P A 2
H17D H 0.446414 0.354676 0.831909 0.096 Uiso 0.296(10) 1 calc GR . P A 2
H17E H 0.426930 0.435452 0.893593 0.096 Uiso 0.296(10) 1 calc GR . P A 2
H17F H 0.409470 0.430992 0.779813 0.096 Uiso 0.296(10) 1 calc GR . P A 2
C18A C 0.3575(9) 0.2693(18) 0.7763(13) 0.045(3) Uani 0.296(10) 1 d D U P A 2
H18A H 0.339066 0.218311 0.792915 0.054 Uiso 0.296(10) 1 calc R . P A 2
C22A C 0.3734(12) 0.310(2) 0.9505(13) 0.075(6) Uani 0.296(10) 1 d D U P A 2
H22D H 0.387457 0.359800 0.994092 0.113 Uiso 0.296(10) 1 calc GR . P A 2
H22E H 0.389332 0.249930 0.970023 0.113 Uiso 0.296(10) 1 calc GR . P A 2
H22F H 0.339547 0.304199 0.952910 0.113 Uiso 0.296(10) 1 calc GR . P A 2


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ce1 O1 2.475(4) 2_655 ?
Ce1 O2 2.463(3) . ?
Ce1 O3 2.461(6) . ?
Ce1 O4 2.705(4) 4_545 ?
Ce1 O4 2.462(4) 6_566 ?
Ce1 O5 2.569(4) 4_545 ?
Ce1 O7 2.488(3) 7_556 ?
Ce1 O8 2.665(4) 2_655 ?
Ce1 C3 2.926(5) 2_655 ?
Ce1 O9 2.537(6) . ?
Ce1 O11 2.462(8) . ?
Ce1 O3A 2.421(10) . ?
O1 C3 1.271(7) . ?
O2 C5 1.268(6) . ?
O3 C18 1.185(8) . ?
O4 C6 1.279(6) . ?
O5 C6 1.258(6) . ?
O6 C11 1.383(6) . ?
O6 C14 1.423(7) . ?
O7 C5 1.249(6) . ?
O8 C3 1.245(7) . ?
C1 H1 0.9500 . ?
C1 C2 1.390(8) . ?
C1 C13 1.387(9) . ?
C2 H2 0.9500 . ?
C2 C12 1.389(9) . ?
C3 C12 1.509(7) . ?
C4 C6 1.494(7) . ?
C4 C7 1.396(7) . ?
C4 C9 1.395(7) . ?
C5 C8 1.516(7) . ?
O9 C19 1.195(8) . ?
C7 H7 0.9500 . ?
C7 C11 1.394(7) . ?
C8 C9 1.382(7) . ?
C8 C10 1.398(7) . ?
C9 H9 0.9500 . ?
C10 H10 0.9500 . ?
C10 C11 1.388(7) . ?
C12 C15 1.372(8) . ?
C13 C14 1.512(7) . ?
C13 C16 1.376(9) . ?
C14 H14A 0.9900 . ?
C14 H14B 0.9900 . ?
C15 H15 0.9500 . ?
C15 C16 1.400(8) . ?
N1 C17 1.451(8) . ?
N1 C18 1.422(8) . ?
N1 C22 1.465(8) . ?
C16 H16 0.9500 . ?
N2 C19 1.419(8) . ?
N2 C20 1.456(8) . ?
N2 C21 1.450(8) . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C18 H18 0.9500 . ?
C19 H19 0.9500 . ?
N3 C23 1.399(18) . ?
N3 C24 1.453(19) . ?
N3 C25 1.59(5) . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
O10 C23 1.225(17) . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C23 H23 0.9500 . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?
C25 H25A 0.9800 . ?
C25 H25B 0.9800 . ?
C25 H25C 0.9800 . ?
O11 C26 1.195(5) . ?
N4 C26 1.467(7) . ?
N4 C27 1.465(9) . ?
N4 C28 1.451(9) . ?
C26 H26 0.9500 . ?
C27 H27A 0.9800 . ?
C27 H27B 0.9800 . ?
C27 H27C 0.9800 . ?
C28 H28A 0.9800 . ?
C28 H28B 0.9800 . ?
C28 H28C 0.9800 . ?
O12 H12A 0.8699 . ?
O12 H12B 0.8700 . ?
O3A C18A 1.197(10) . ?
N1A C17A 1.460(10) . ?
N1A C18A 1.453(10) . ?
N1A C22A 1.470(10) . ?
C17A H17D 0.9800 . ?
C17A H17E 0.9800 . ?
C17A H17F 0.9800 . ?
C18A H18A 0.9500 . ?
C22A H22D 0.9800 . ?
C22A H22E 0.9800 . ?
C22A H22F 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Ce1 O4 128.38(13) 2_655 4_545 ?
O1 Ce1 O5 81.91(13) 2_655 4_545 ?
O1 Ce1 O7 140.99(14) 2_655 7_556 ?
O1 Ce1 O8 50.65(12) 2_655 2_655 ?
O1 Ce1 C3 25.50(15) 2_655 2_655 ?
O1 Ce1 O9 71.9(2) 2_655 . ?
O2 Ce1 O1 81.23(14) . 2_655 ?
O2 Ce1 O4 70.68(11) . 4_545 ?
O2 Ce1 O5 73.91(13) . 4_545 ?
O2 Ce1 O7 134.73(12) . 7_556 ?
O2 Ce1 O8 70.55(13) . 2_655 ?
O2 Ce1 C3 73.37(14) . 2_655 ?
O2 Ce1 O9 143.21(19) . . ?
O3 Ce1 O1 92.4(3) . 2_655 ?
O3 Ce1 O2 133.4(3) . . ?
O3 Ce1 O4 80.7(4) . 6_566 ?
O3 Ce1 O4 138.1(3) . 4_545 ?
O3 Ce1 O5 151.1(4) . 4_545 ?
O3 Ce1 O7 73.4(3) . 7_556 ?
O3 Ce1 O8 70.1(3) . 2_655 ?
O3 Ce1 C3 81.4(3) . 2_655 ?
O3 Ce1 O9 73.6(4) . . ?
O4 Ce1 O1 135.69(12) 6_566 2_655 ?
O4 Ce1 O2 72.97(12) 6_566 . ?
O4 Ce1 O4 75.69(12) 6_566 4_545 ?
O4 Ce1 O5 122.56(12) 6_566 4_545 ?
O4 Ce1 O7 78.81(12) 6_566 7_556 ?
O4 Ce1 O8 86.50(12) 6_566 2_655 ?
O4 Ce1 C3 139.46(13) 4_545 2_655 ?
O4 Ce1 C3 110.83(14) 6_566 2_655 ?
O4 Ce1 O9 143.45(19) 6_566 . ?
O4 Ce1 O11 148.6(4) 6_566 . ?
O5 Ce1 O4 49.45(11) 4_545 4_545 ?
O5 Ce1 O8 123.48(12) 4_545 2_655 ?
O5 Ce1 C3 102.69(14) 4_545 2_655 ?
O7 Ce1 O4 68.46(12) 7_556 4_545 ?
O7 Ce1 O5 93.37(13) 7_556 4_545 ?
O7 Ce1 O8 142.29(13) 7_556 2_655 ?
O7 Ce1 C3 151.21(14) 7_556 2_655 ?
O7 Ce1 O9 69.26(19) 7_556 . ?
O8 Ce1 O4 140.58(12) 2_655 4_545 ?
O8 Ce1 C3 25.19(14) 2_655 2_655 ?
O9 Ce1 O4 107.1(2) . 4_545 ?
O9 Ce1 O5 77.7(2) . 4_545 ?
O9 Ce1 O8 108.0(2) . 2_655 ?
O9 Ce1 C3 90.8(2) . 2_655 ?
O11 Ce1 O2 134.6(4) . . ?
O3A Ce1 O2 135.5(9) . . ?
O3A Ce1 O11 80.4(11) . . ?
C3 O1 Ce1 97.5(3) . 2_655 ?
C5 O2 Ce1 137.1(3) . . ?
C18 O3 Ce1 139.3(9) . . ?
Ce1 O4 Ce1 104.31(12) 6_565 4 ?
C6 O4 Ce1 156.3(3) . 6_565 ?
C6 O4 Ce1 91.2(3) . 4 ?
C6 O5 Ce1 98.2(3) . 4 ?
C11 O6 C14 115.2(4) . . ?
C5 O7 Ce1 135.5(3) . 7_556 ?
C3 O8 Ce1 89.2(3) . 2_655 ?
C2 C1 H1 119.8 . . ?
C13 C1 H1 119.8 . . ?
C13 C1 C2 120.3(6) . . ?
C1 C2 H2 119.9 . . ?
C12 C2 C1 120.2(6) . . ?
C12 C2 H2 119.9 . . ?
O1 C3 Ce1 57.0(3) . 2_655 ?
O1 C3 C12 117.3(5) . . ?
O8 C3 Ce1 65.6(3) . 2_655 ?
O8 C3 O1 122.4(5) . . ?
O8 C3 C12 120.3(5) . . ?
C12 C3 Ce1 171.7(4) . 2_655 ?
C7 C4 C6 119.1(4) . . ?
C9 C4 C6 120.3(4) . . ?
C9 C4 C7 120.6(5) . . ?
O2 C5 C8 116.4(4) . . ?
O7 C5 O2 125.9(5) . . ?
O7 C5 C8 117.7(5) . . ?
C19 O9 Ce1 127.0(6) . . ?
O4 C6 Ce1 63.7(3) . 4 ?
O4 C6 C4 119.1(4) . . ?
O5 C6 Ce1 57.5(3) . 4 ?
O5 C6 O4 121.2(5) . . ?
O5 C6 C4 119.8(5) . . ?
C4 C6 Ce1 176.9(4) . 4 ?
C4 C7 H7 120.5 . . ?
C11 C7 C4 118.9(5) . . ?
C11 C7 H7 120.5 . . ?
C9 C8 C5 121.1(4) . . ?
C9 C8 C10 120.3(5) . . ?
C10 C8 C5 118.6(4) . . ?
C4 C9 H9 120.1 . . ?
C8 C9 C4 119.7(4) . . ?
C8 C9 H9 120.1 . . ?
C8 C10 H10 120.2 . . ?
C11 C10 C8 119.6(5) . . ?
C11 C10 H10 120.2 . . ?
O6 C11 C7 115.1(4) . . ?
O6 C11 C10 124.1(5) . . ?
C10 C11 C7 120.8(5) . . ?
C2 C12 C3 118.9(5) . . ?
C15 C12 C2 119.3(5) . . ?
C15 C12 C3 121.8(5) . . ?
C1 C13 C14 117.1(5) . . ?
C16 C13 C1 119.3(5) . . ?
C16 C13 C14 123.3(6) . . ?
O6 C14 C13 109.0(5) . . ?
O6 C14 H14A 109.9 . . ?
O6 C14 H14B 109.9 . . ?
C13 C14 H14A 109.9 . . ?
C13 C14 H14B 109.9 . . ?
H14A C14 H14B 108.3 . . ?
C12 C15 H15 119.7 . . ?
C12 C15 C16 120.5(5) . . ?
C16 C15 H15 119.7 . . ?
C17 N1 C22 121.1(9) . . ?
C18 N1 C17 119.5(8) . . ?
C18 N1 C22 118.5(8) . . ?
C13 C16 C15 120.3(6) . . ?
C13 C16 H16 119.9 . . ?
C15 C16 H16 119.9 . . ?
C19 N2 C20 119.6(8) . . ?
C19 N2 C21 121.6(8) . . ?
C21 N2 C20 118.8(8) . . ?
N1 C17 H17A 109.5 . . ?
N1 C17 H17B 109.5 . . ?
N1 C17 H17C 109.5 . . ?
H17A C17 H17B 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
O3 C18 N1 121.0(9) . . ?
O3 C18 H18 119.5 . . ?
N1 C18 H18 119.5 . . ?
O9 C19 N2 126.7(9) . . ?
O9 C19 H19 116.6 . . ?
N2 C19 H19 116.6 . . ?
C23 N3 C24 121.5(12) . . ?
C23 N3 C25 114(3) . . ?
C24 N3 C25 124(3) . . ?
N2 C20 H20A 109.5 . . ?
N2 C20 H20B 109.5 . . ?
N2 C20 H20C 109.5 . . ?
H20A C20 H20B 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
N2 C21 H21A 109.5 . . ?
N2 C21 H21B 109.5 . . ?
N2 C21 H21C 109.5 . . ?
H21A C21 H21B 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
N1 C22 H22A 109.5 . . ?
N1 C22 H22B 109.5 . . ?
N1 C22 H22C 109.5 . . ?
H22A C22 H22B 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
N3 C23 H23 117.6 . . ?
O10 C23 N3 124.9(13) . . ?
O10 C23 H23 117.6 . . ?
N3 C24 H24A 109.5 . . ?
N3 C24 H24B 109.5 . . ?
N3 C24 H24C 109.5 . . ?
H24A C24 H24B 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
N3 C25 H25A 109.5 . . ?
N3 C25 H25B 109.5 . . ?
N3 C25 H25C 109.5 . . ?
H25A C25 H25B 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
C26 O11 Ce1 141.5(10) . . ?
C27 N4 C26 118.7(11) . . ?
C28 N4 C26 120.8(11) . . ?
C28 N4 C27 120.6(12) . . ?
O11 C26 N4 116.6(9) . . ?
O11 C26 H26 121.7 . . ?
N4 C26 H26 121.7 . . ?
N4 C27 H27A 109.5 . . ?
N4 C27 H27B 109.5 . . ?
N4 C27 H27C 109.5 . . ?
H27A C27 H27B 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
N4 C28 H28A 109.5 . . ?
N4 C28 H28B 109.5 . . ?
N4 C28 H28C 109.5 . . ?
H28A C28 H28B 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
H12A O12 H12B 109.5 . . ?
C18A O3A Ce1 134.2(18) . . ?
C17A N1A C22A 118.7(13) . . ?
C18A N1A C17A 120.7(14) . . ?
C18A N1A C22A 117.0(13) . . ?
N1A C17A H17D 109.5 . . ?
N1A C17A H17E 109.5 . . ?
N1A C17A H17F 109.5 . . ?
H17D C17A H17E 109.5 . . ?
H17D C17A H17F 109.5 . . ?
H17E C17A H17F 109.5 . . ?
O3A C18A N1A 123.2(18) . . ?
O3A C18A H18A 118.4 . . ?
N1A C18A H18A 118.4 . . ?
N1A C22A H22D 109.5 . . ?
N1A C22A H22E 109.5 . . ?
N1A C22A H22F 109.5 . . ?
H22D C22A H22E 109.5 . . ?
H22D C22A H22F 109.5 . . ?
H22E C22A H22F 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Ce1 O1 C3 O8 4.8(6) 2_655 . . . ?
Ce1 O1 C3 C12 -173.0(4) 2_655 . . . ?
Ce1 O2 C5 O7 -35.6(9) . . . . ?
Ce1 O2 C5 C8 143.2(4) . . . . ?
Ce1 O3 C18 N1 -165.5(11) . . . . ?
Ce1 O4 C6 Ce1 131.5(8) 6_565 . . 4 ?
Ce1 O4 C6 O5 -0.4(5) 4 . . . ?
Ce1 O4 C6 O5 131.1(7) 6_565 . . . ?
Ce1 O4 C6 C4 178.5(4) 4 . . . ?
Ce1 O4 C6 C4 -50.0(10) 6_565 . . . ?
Ce1 O5 C6 O4 0.4(5) 4 . . . ?
Ce1 O5 C6 C4 -178.5(4) 4 . . . ?
Ce1 O7 C5 O2 12.8(9) 7_556 . . . ?
Ce1 O7 C5 C8 -166.0(4) 7_556 . . . ?
Ce1 O8 C3 O1 -4.4(6) 2_655 . . . ?
Ce1 O8 C3 C12 173.3(5) 2_655 . . . ?
Ce1 O9 C19 N2 165.1(5) . . . . ?
Ce1 O11 C26 N4 144.9(16) . . . . ?
Ce1 O3A C18A N1A -164(3) . . . . ?
O1 C3 C12 C2 0.4(9) . . . . ?
O1 C3 C12 C15 178.4(6) . . . . ?
O2 C5 C8 C9 -175.7(5) . . . . ?
O2 C5 C8 C10 5.2(7) . . . . ?
O7 C5 C8 C9 3.2(8) . . . . ?
O7 C5 C8 C10 -175.9(5) . . . . ?
O8 C3 C12 C2 -177.5(6) . . . . ?
O8 C3 C12 C15 0.6(9) . . . . ?
C1 C2 C12 C3 175.6(7) . . . . ?
C1 C2 C12 C15 -2.5(12) . . . . ?
C1 C13 C14 O6 -153.6(7) . . . . ?
C1 C13 C16 C15 1.5(11) . . . . ?
C2 C1 C13 C14 -177.2(8) . . . . ?
C2 C1 C13 C16 -2.1(13) . . . . ?
C2 C12 C15 C16 1.9(10) . . . . ?
C3 C12 C15 C16 -176.2(6) . . . . ?
C4 C7 C11 O6 177.4(5) . . . . ?
C4 C7 C11 C10 -3.0(8) . . . . ?
C5 C8 C9 C4 176.9(5) . . . . ?
C5 C8 C10 C11 -179.4(5) . . . . ?
C6 C4 C7 C11 -177.5(5) . . . . ?
C6 C4 C9 C8 -179.0(5) . . . . ?
C7 C4 C6 O4 -24.6(7) . . . . ?
C7 C4 C6 O5 154.3(5) . . . . ?
C7 C4 C9 C8 3.1(8) . . . . ?
C8 C10 C11 O6 -178.4(5) . . . . ?
C8 C10 C11 C7 2.1(8) . . . . ?
C9 C4 C6 O4 157.5(5) . . . . ?
C9 C4 C6 O5 -23.6(7) . . . . ?
C9 C4 C7 C11 0.4(8) . . . . ?
C9 C8 C10 C11 1.5(8) . . . . ?
C10 C8 C9 C4 -4.1(8) . . . . ?
C11 O6 C14 C13 165.3(6) . . . . ?
C12 C15 C16 C13 -1.4(11) . . . . ?
C13 C1 C2 C12 2.6(14) . . . . ?
C14 O6 C11 C7 -164.1(5) . . . . ?
C14 O6 C11 C10 16.4(8) . . . . ?
C14 C13 C16 C15 176.2(7) . . . . ?
C16 C13 C14 O6 31.6(10) . . . . ?
C17 N1 C18 O3 7(2) . . . . ?
C20 N2 C19 O9 179.5(3) . . . . ?
C21 N2 C19 O9 0.0(4) . . . . ?
C22 N1 C18 O3 176.1(14) . . . . ?
C24 N3 C23 O10 179.5(14) . . . . ?
C25 N3 C23 O10 -4(3) . . . . ?
C27 N4 C26 O11 179.8(3) . . . . ?
C28 N4 C26 O11 -0.1(3) . . . . ?
C17A N1A C18A O3A -19(5) . . . . ?
C22A N1A C18A O3A -177(4) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
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# 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_222_sq
_database_code_depnum_ccdc_archive 'CCDC 2071650'
loop_
_audit_author_name
_audit_author_address
'Yun-Shan Xue' 'Yancheng Teachers University'
_audit_update_record             
;
2021-03-19 deposited with the CCDC.	2021-04-20 downloaded from the CCDC.
;
_audit_creation_date             2020-07-30
_audit_creation_method           
;
Olex2 1.2-beta
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         '0.25(C176 H184 Gd8 N16 O72), C3 H7 N O'
_chemical_formula_sum            'C47 H53 Gd2 N5 O19'
_chemical_formula_weight         1306.44
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Gd Gd -0.1653 3.9035 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 1 2/c 1'
_space_group_name_Hall           '-C 2yc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'

_cell_length_a                   28.4297(13)
_cell_length_b                   14.2555(6)
_cell_length_c                   13.8161(5)
_cell_angle_alpha                90
_cell_angle_beta                 100.144(2)
_cell_angle_gamma                90
_cell_volume                     5511.9(4)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    9865
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      26.445
_cell_measurement_theta_min      2.280
_shelx_estimated_absorpt_T_max   0.774
_shelx_estimated_absorpt_T_min   0.526
_exptl_absorpt_coefficient_mu    2.459
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.5650
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0919 before and 0.0562 after correction.
The Ratio of minimum to maximum transmission is 0.7580.
The λ/2 correction factor is Not present.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.574
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             2600
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.11
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0374
_diffrn_reflns_av_unetI/netI     0.0292
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_h_min       -33
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            25032
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.049
_diffrn_reflns_theta_max         25.049
_diffrn_reflns_theta_min         2.609
_diffrn_ambient_temperature      150.02
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_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                4428
_reflns_number_total             4868
_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       'SAINT v8.37A (Bruker, 2015)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    ?
_refine_diff_density_max         2.384
_refine_diff_density_min         -0.869
_refine_diff_density_rms         0.153
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.087
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     435
_refine_ls_number_reflns         4868
_refine_ls_number_restraints     280
_refine_ls_R_factor_all          0.0492
_refine_ls_R_factor_gt           0.0441
_refine_ls_restrained_S_all      1.071
_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)+(0.0500P)²+144.2334P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1195
_refine_ls_wR_factor_ref         0.1218
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 O8-C17 = O8-C20 = O9-C23 = O9-C27
 1.2 with sigma of 0.02
 N1-C17 = N2-C20 = N4-C27 = N3-C23
 1.3 with sigma of 0.01
 N2-C21 = N4-C26
 1.49 with sigma of 0.01
 N3-C24 = N3-C25 = N4-C28 = N1-C18 = N1-C19 = N2-C22
 1.49 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
C25 \\sim C26 \\sim C24 \\sim C28 \\sim N4 \\sim C27 \\sim C23 \\sim N3: within
2A with sigma of 0.01 and sigma for terminal atoms of 0.01
C20 \\sim N2 \\sim C21 \\sim C22 \\sim C17 \\sim N1 \\sim C19 \\sim C18: within
2A with sigma of 0.01 and sigma for terminal atoms of 0.01
Uanis(C4) \\sim Ueq, Uanis(C5) \\sim Ueq, Uanis(C6) \\sim Ueq, Uanis(C29) \\sim
Ueq, Uanis(C30) \\sim Ueq, Uanis(C28) \\sim Ueq, Uanis(N4) \\sim Ueq,
Uanis(C27) \\sim Ueq, Uanis(C26) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C17) \\sim Ueq, Uanis(C25) \\sim Ueq, Uanis(C23) \\sim Ueq, Uanis(C18)
\\sim Ueq, Uanis(C20) \\sim Ueq, Uanis(N2) \\sim Ueq, Uanis(C22) \\sim Ueq,
Uanis(C21) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
4. Others
 Sof(N2)=Sof(C22)=Sof(H22A)=Sof(H22B)=Sof(H22C)=Sof(C20)=Sof(H20)=Sof(C21)=
 Sof(H21A)=Sof(H21B)=Sof(H21C)=1-FVAR(1)
 Sof(N1)=Sof(C18)=Sof(H18A)=Sof(H18B)=Sof(H18C)=Sof(C17)=Sof(H17)=Sof(C19)=
 Sof(H19A)=Sof(H19B)=Sof(H19C)=FVAR(1)
 Sof(N4)=Sof(C26)=Sof(H26A)=Sof(H26B)=Sof(H26C)=Sof(C27)=Sof(H27)=Sof(C28)=
 Sof(H28A)=Sof(H28B)=Sof(H28C)=1-FVAR(2)
 Sof(N3)=Sof(C23)=Sof(H23)=Sof(C24)=Sof(H24A)=Sof(H24B)=Sof(H24C)=Sof(C25)=
 Sof(H25A)=Sof(H25B)=Sof(H25C)=FVAR(2)
 Fixed Sof: O10(0.5) N5(0.5) C29(0.5) H29(0.5) C30(0.5) H30A(0.5) H30B(0.5)
 H30C(0.5) C31(0.5) H31A(0.5) H31B(0.5) H31C(0.5)
5.a Riding coordinates:
 C22(H22A,H22B,H22C)
5.b Secondary CH2 refined with riding coordinates:
 C8(H8A,H8B)
5.c Aromatic/amide H refined with riding coordinates:
 C4(H4), C3(H3), C12(H12), C14(H14), C10(H10), C6(H6), C7(H7), C23(H23),
 C17(H17), C29(H29), C20(H20), C27(H27)
5.d Idealised Me refined as rotating group:
 C18(H18A,H18B,H18C), C19(H19A,H19B,H19C), C24(H24A,H24B,H24C), C25(H25A,H25B,
 H25C), C30(H30A,H30B,H30C), C31(H31A,H31B,H31C), C21(H21A,H21B,H21C), C26(H26A,
 H26B,H26C), C28(H28A,H28B,H28C)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     ?
_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
Gd4 Gd 0.68196(2) 0.78570(2) 0.45830(2) 0.01049(12) Uani 1 1 d . . . . .
O8 O 0.6444(2) 0.7168(4) 0.3081(4) 0.0370(14) Uani 1 1 d D . . . .
O2 O 0.60670(18) 0.8131(3) 0.5072(4) 0.0242(12) Uani 1 1 d . . . . .
O7 O 0.30103(17) 0.7311(3) 0.8765(3) 0.0170(10) Uani 1 1 d . . . . .
O6 O 0.22894(16) 0.6626(4) 0.8401(4) 0.0212(11) Uani 1 1 d . . . . .
O5 O 0.20356(16) 0.4274(3) 0.5569(4) 0.0194(10) Uani 1 1 d . . . . .
O3 O 0.39873(16) 0.5832(3) 0.6451(4) 0.0208(11) Uani 1 1 d . . . . .
O4 O 0.26770(16) 0.3458(3) 0.5437(3) 0.0156(10) Uani 1 1 d . . . . .
O1 O 0.61845(19) 0.6625(4) 0.4888(4) 0.0284(13) Uani 1 1 d . . . . .
C4 C 0.4814(3) 0.7700(6) 0.6147(8) 0.041(2) Uani 1 1 d . U . . .
H4 H 0.464256 0.821899 0.634164 0.049 Uiso 1 1 calc R . . . .
O9 O 0.6424(2) 0.9172(4) 0.3600(4) 0.0372(14) Uani 1 1 d D . . . .
C3 C 0.5219(3) 0.7849(6) 0.5749(7) 0.037(2) Uani 1 1 d . . . . .
H3 H 0.532237 0.847213 0.566149 0.045 Uiso 1 1 calc R . . . .
C9 C 0.3531(2) 0.5732(5) 0.6670(5) 0.0159(14) Uani 1 1 d . . . . .
C11 C 0.2894(2) 0.6151(5) 0.7521(5) 0.0144(13) Uani 1 1 d . . . . .
C1 C 0.5939(2) 0.7288(5) 0.5110(5) 0.0194(15) Uani 1 1 d . . . . .
C15 C 0.2480(2) 0.4177(5) 0.5748(5) 0.0147(13) Uani 1 1 d . . . . .
C16 C 0.2719(2) 0.6745(4) 0.8293(5) 0.0141(13) Uani 1 1 d . . . . .
C2 C 0.5480(3) 0.7097(5) 0.5472(6) 0.0223(16) Uani 1 1 d . . . . .
C12 C 0.2605(2) 0.5472(4) 0.6986(5) 0.0134(13) Uani 1 1 d . . . . .
H12 H 0.228288 0.540028 0.707147 0.016 Uiso 1 1 calc R . . . .
C8 C 0.4222(3) 0.6689(7) 0.6758(7) 0.042(2) Uani 1 1 d . . . . .
H8A H 0.432252 0.669103 0.748094 0.050 Uiso 1 1 calc R . . . .
H8B H 0.400072 0.722183 0.657407 0.050 Uiso 1 1 calc R . . . .
C14 C 0.3256(2) 0.5031(5) 0.6173(5) 0.0151(13) Uani 1 1 d . . . . .
H14 H 0.338316 0.463689 0.572781 0.018 Uiso 1 1 calc R . . . .
C13 C 0.2788(2) 0.4902(4) 0.6326(5) 0.0143(13) Uani 1 1 d . . . . .
C10 C 0.3358(2) 0.6290(5) 0.7362(5) 0.0171(14) Uani 1 1 d . . . . .
H10 H 0.355486 0.675756 0.771894 0.020 Uiso 1 1 calc R . . . .
C5 C 0.4654(3) 0.6792(6) 0.6265(7) 0.034(2) Uani 1 1 d . U . . .
N3 N 0.6162(4) 0.9911(7) 0.2084(7) 0.050(2) Uani 0.722(9) 1 d D U P A 1
C6 C 0.4907(3) 0.6047(6) 0.5995(7) 0.041(2) Uani 1 1 d . U . . .
H6 H 0.480477 0.542398 0.608935 0.050 Uiso 1 1 calc R . . . .
C7 C 0.5318(3) 0.6203(6) 0.5577(7) 0.035(2) Uani 1 1 d . . . . .
H7 H 0.548515 0.568521 0.536678 0.042 Uiso 1 1 calc R . . . .
N1 N 0.6252(4) 0.6291(8) 0.1758(7) 0.050(2) Uani 0.749(10) 1 d D U P B 1
C23 C 0.6300(5) 0.9231(9) 0.2703(9) 0.045(3) Uani 0.722(9) 1 d D U P A 1
H23 H 0.630461 0.864082 0.238464 0.054 Uiso 0.722(9) 1 calc R . P A 1
C18 C 0.5771(4) 0.6034(11) 0.1940(12) 0.057(3) Uani 0.749(10) 1 d D U P B 1
H18A H 0.575565 0.613222 0.263518 0.086 Uiso 0.749(10) 1 calc GR . P B 1
H18B H 0.570855 0.537218 0.177100 0.086 Uiso 0.749(10) 1 calc GR . P B 1
H18C H 0.553062 0.642569 0.153273 0.086 Uiso 0.749(10) 1 calc GR . P B 1
C17 C 0.6545(5) 0.6787(10) 0.2389(9) 0.051(3) Uani 0.749(10) 1 d D U P B 1
H17 H 0.686457 0.684664 0.228334 0.061 Uiso 0.749(10) 1 calc R . P B 1
C19 C 0.6423(6) 0.5783(11) 0.0950(10) 0.061(3) Uani 0.749(10) 1 d D U P B 1
H19A H 0.634466 0.511581 0.098252 0.091 Uiso 0.749(10) 1 calc GR . P B 1
H19B H 0.676944 0.585849 0.101755 0.091 Uiso 0.749(10) 1 calc GR . P B 1
H19C H 0.626660 0.604040 0.031660 0.091 Uiso 0.749(10) 1 calc GR . P B 1
C24 C 0.5989(5) 0.9767(10) 0.1021(8) 0.052(3) Uani 0.722(9) 1 d D U P A 1
H24A H 0.608136 0.914074 0.083097 0.078 Uiso 0.722(9) 1 calc GR . P A 1
H24B H 0.613007 1.024191 0.064610 0.078 Uiso 0.722(9) 1 calc GR . P A 1
H24C H 0.563984 0.982452 0.088100 0.078 Uiso 0.722(9) 1 calc GR . P A 1
C25 C 0.6204(7) 1.0901(8) 0.2390(14) 0.066(3) Uani 0.722(9) 1 d D U P A 1
H25A H 0.631528 1.093664 0.310192 0.099 Uiso 0.722(9) 1 calc GR . P A 1
H25B H 0.589173 1.120634 0.222165 0.099 Uiso 0.722(9) 1 calc GR . P A 1
H25C H 0.643387 1.121922 0.204992 0.099 Uiso 0.722(9) 1 calc GR . P A 1
O10 O 0.6654(6) 0.7976(10) 0.0556(11) 0.055(4) Uani 0.5 1 d . . P C -1
N5 N 0.7187(6) 0.8327(10) -0.0430(10) 0.037(3) Uani 0.5 1 d . . P C -1
C29 C 0.6812(6) 0.8496(12) -0.0008(12) 0.032(4) Uani 0.5 1 d . U P C -1
H29 H 0.665209 0.907600 -0.015974 0.038 Uiso 0.5 1 calc R . P C -1
C30 C 0.7468(14) 0.746(3) -0.0209(17) 0.049(7) Uani 0.5 1 d . U P C -1
H30A H 0.779197 0.762392 0.012285 0.074 Uiso 0.5 1 calc GR . P C -1
H30B H 0.748516 0.713058 -0.082281 0.074 Uiso 0.5 1 calc GR . P C -1
H30C H 0.731554 0.706061 0.021954 0.074 Uiso 0.5 1 calc GR . P C -1
C31 C 0.7357(7) 0.8992(14) -0.1101(14) 0.045(5) Uani 0.5 1 d . . P C -1
H31A H 0.717970 0.958225 -0.110594 0.068 Uiso 0.5 1 calc GR . P C -1
H31B H 0.730587 0.872748 -0.176629 0.068 Uiso 0.5 1 calc GR . P C -1
H31C H 0.769837 0.911088 -0.088033 0.068 Uiso 0.5 1 calc GR . P C -1
N2 N 0.6284(13) 0.700(2) 0.1395(19) 0.058(3) Uani 0.251(10) 1 d D U P B 2
C22 C 0.6253(18) 0.748(3) 0.043(2) 0.062(6) Uani 0.251(10) 1 d D U P B 2
H22A H 0.592845 0.742043 0.005210 0.093 Uiso 0.251(10) 1 d R . P B 2
H22B H 0.648025 0.718913 0.006470 0.093 Uiso 0.251(10) 1 d R . P B 2
H22C H 0.633145 0.814663 0.053520 0.093 Uiso 0.251(10) 1 d R . P B 2
C20 C 0.6454(16) 0.740(3) 0.2233(14) 0.053(4) Uani 0.251(10) 1 d D U P B 2
H20 H 0.661403 0.798013 0.217462 0.064 Uiso 0.251(10) 1 calc R . P B 2
C21 C 0.5966(18) 0.620(3) 0.155(4) 0.059(4) Uani 0.251(10) 1 d D U P B 2
H21A H 0.563178 0.639146 0.134108 0.088 Uiso 0.251(10) 1 calc GR . P B 2
H21B H 0.602189 0.603184 0.224379 0.088 Uiso 0.251(10) 1 calc GR . P B 2
H21C H 0.603618 0.566656 0.115407 0.088 Uiso 0.251(10) 1 calc GR . P B 2
N4 N 0.6485(9) 1.0496(19) 0.289(2) 0.052(3) Uani 0.278(9) 1 d D U P A 2
C26 C 0.5981(10) 1.069(3) 0.245(3) 0.057(4) Uani 0.278(9) 1 d D U P A 2
H26A H 0.594257 1.063841 0.173092 0.086 Uiso 0.278(9) 1 calc GR . P A 2
H26B H 0.589367 1.131953 0.262860 0.086 Uiso 0.278(9) 1 calc GR . P A 2
H26C H 0.577318 1.022696 0.269116 0.086 Uiso 0.278(9) 1 calc GR . P A 2
C27 C 0.6640(11) 0.9891(16) 0.357(2) 0.052(4) Uani 0.278(9) 1 d D U P A 2
H27 H 0.692041 1.001347 0.403790 0.062 Uiso 0.278(9) 1 calc R . P A 2
C28 C 0.6816(14) 1.132(2) 0.297(3) 0.065(5) Uani 0.278(9) 1 d D U P A 2
H28A H 0.665990 1.183471 0.257012 0.098 Uiso 0.278(9) 1 calc GR . P A 2
H28B H 0.710796 1.113719 0.272863 0.098 Uiso 0.278(9) 1 calc GR . P A 2
H28C H 0.689763 1.151465 0.365664 0.098 Uiso 0.278(9) 1 calc GR . P A 2


_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
Gd4 Gd4 3.9698(6) 7_666 ?
Gd4 O8 2.373(5) . ?
Gd4 O2 2.387(5) . ?
Gd4 O7 2.380(5) 2_656 ?
Gd4 O6 2.400(4) 8_565 ?
Gd4 O5 2.454(5) 3 ?
Gd4 O4 2.362(4) 5_666 ?
Gd4 O4 2.656(5) 3 ?
Gd4 O1 2.605(5) . ?
Gd4 O9 2.467(6) . ?
Gd4 C1 2.847(7) . ?
Gd4 C15 2.932(7) 3 ?
O8 C17 1.178(12) . ?
O8 C20 1.225(19) . ?
O2 C1 1.261(9) . ?
O7 C16 1.253(8) . ?
O6 C16 1.267(8) . ?
O5 C15 1.253(8) . ?
O3 C9 1.390(8) . ?
O3 C8 1.420(9) . ?
O4 C15 1.277(8) . ?
O1 C1 1.245(9) . ?
C4 H4 0.9500 . ?
C4 C3 1.379(11) . ?
C4 C5 1.390(12) . ?
O9 C23 1.231(12) . ?
O9 C27 1.199(19) . ?
C3 H3 0.9500 . ?
C3 C2 1.394(11) . ?
C9 C14 1.378(9) . ?
C9 C10 1.398(9) . ?
C11 C16 1.513(9) . ?
C11 C12 1.393(9) . ?
C11 C10 1.390(9) . ?
C1 C2 1.502(9) . ?
C15 C13 1.492(9) . ?
C2 C7 1.370(11) . ?
C12 H12 0.9500 . ?
C12 C13 1.389(9) . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C8 C5 1.514(10) . ?
C14 H14 0.9500 . ?
C14 C13 1.394(9) . ?
C10 H10 0.9500 . ?
C5 C6 1.370(12) . ?
N3 C23 1.306(9) . ?
N3 C24 1.479(9) . ?
N3 C25 1.473(9) . ?
C6 H6 0.9500 . ?
C6 C7 1.411(11) . ?
C7 H7 0.9500 . ?
N1 C18 1.478(9) . ?
N1 C17 1.304(9) . ?
N1 C19 1.482(9) . ?
C23 H23 0.9500 . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
C17 H17 0.9500 . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?
C25 H25A 0.9800 . ?
C25 H25B 0.9800 . ?
C25 H25C 0.9800 . ?
O10 C29 1.22(2) . ?
N5 C29 1.32(2) . ?
N5 C30 1.47(4) . ?
N5 C31 1.47(2) . ?
C29 H29 0.9500 . ?
C30 H30A 0.9800 . ?
C30 H30B 0.9800 . ?
C30 H30C 0.9800 . ?
C31 H31A 0.9800 . ?
C31 H31B 0.9800 . ?
C31 H31C 0.9800 . ?
N2 C22 1.486(10) . ?
N2 C20 1.304(10) . ?
N2 C21 1.492(10) . ?
C22 H22A 0.9796 . ?
C22 H22B 0.9803 . ?
C22 H22C 0.9798 . ?
C20 H20 0.9500 . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
N4 C26 1.481(10) . ?
N4 C27 1.293(10) . ?
N4 C28 1.493(10) . ?
C26 H26A 0.9800 . ?
C26 H26B 0.9800 . ?
C26 H26C 0.9800 . ?
C27 H27 0.9500 . ?
C28 H28A 0.9800 . ?
C28 H28B 0.9800 . ?
C28 H28C 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O8 Gd4 Gd4 114.43(16) . 7_666 ?
O8 Gd4 O2 91.5(2) . . ?
O8 Gd4 O7 133.41(19) . 2_656 ?
O8 Gd4 O6 75.60(19) . 8_565 ?
O8 Gd4 O5 148.93(19) . 3 ?
O8 Gd4 O4 139.36(18) . 3 ?
O8 Gd4 O1 69.14(19) . . ?
O8 Gd4 O9 75.0(2) . . ?
O8 Gd4 C1 79.9(2) . . ?
O8 Gd4 C15 153.14(19) . 3 ?
O2 Gd4 Gd4 146.75(13) . 7_666 ?
O2 Gd4 O6 140.91(17) . 8_565 ?
O2 Gd4 O5 81.78(17) . 3 ?
O2 Gd4 O4 128.30(16) . 3 ?
O2 Gd4 O1 51.93(16) . . ?
O2 Gd4 O9 71.73(18) . . ?
O2 Gd4 C1 26.02(19) . . ?
O2 Gd4 C15 105.02(18) . 3 ?
O7 Gd4 Gd4 67.34(11) 2_656 7_666 ?
O7 Gd4 O2 79.81(17) 2_656 . ?
O7 Gd4 O6 135.21(16) 2_656 8_565 ?
O7 Gd4 O5 75.42(16) 2_656 3 ?
O7 Gd4 O4 70.37(15) 2_656 3 ?
O7 Gd4 O1 69.75(17) 2_656 . ?
O7 Gd4 O9 140.59(18) 2_656 . ?
O7 Gd4 C1 72.57(18) 2_656 . ?
O7 Gd4 C15 71.42(17) 2_656 3 ?
O6 Gd4 Gd4 69.25(11) 8_565 7_666 ?
O6 Gd4 O5 90.58(17) 8_565 3 ?
O6 Gd4 O4 68.04(15) 8_565 3 ?
O6 Gd4 O1 143.26(17) 8_565 . ?
O6 Gd4 O9 69.31(17) 8_565 . ?
O6 Gd4 C1 151.83(18) 8_565 . ?
O6 Gd4 C15 78.27(17) 8_565 3 ?
O5 Gd4 Gd4 85.08(11) 3 7_666 ?
O5 Gd4 O4 50.75(14) 3 3 ?
O5 Gd4 O1 125.31(16) 3 . ?
O5 Gd4 O9 74.05(19) 3 . ?
O5 Gd4 C1 103.77(18) 3 . ?
O5 Gd4 C15 24.93(17) 3 3 ?
O4 Gd4 Gd4 35.18(10) 3 7_666 ?
O4 Gd4 Gd4 40.39(11) 5_666 7_666 ?
O4 Gd4 O8 80.89(19) 5_666 . ?
O4 Gd4 O2 135.13(16) 5_666 . ?
O4 Gd4 O7 74.35(15) 5_666 2_656 ?
O4 Gd4 O6 79.91(16) 5_666 8_565 ?
O4 Gd4 O5 124.56(16) 5_666 3 ?
O4 Gd4 O4 75.57(16) 5_666 3 ?
O4 Gd4 O1 84.58(16) 5_666 . ?
O4 Gd4 O9 144.62(17) 5_666 . ?
O4 Gd4 C1 109.81(18) 5_666 . ?
O4 Gd4 C1 139.30(17) 3 . ?
O4 Gd4 C15 25.83(16) 3 3 ?
O4 Gd4 C15 100.66(17) 5_666 3 ?
O1 Gd4 Gd4 116.62(13) . 7_666 ?
O1 Gd4 O4 138.90(17) . 3 ?
O1 Gd4 C1 25.92(18) . . ?
O1 Gd4 C15 137.66(17) . 3 ?
O9 Gd4 Gd4 132.94(14) . 7_666 ?
O9 Gd4 O4 107.05(18) . 3 ?
O9 Gd4 O1 109.8(2) . . ?
O9 Gd4 C1 91.2(2) . . ?
O9 Gd4 C15 90.0(2) . 3 ?
C1 Gd4 Gd4 135.15(15) . 7_666 ?
C1 Gd4 C15 123.37(18) . 3 ?
C15 Gd4 Gd4 60.51(13) 3 7_666 ?
C17 O8 Gd4 139.8(8) . . ?
C20 O8 Gd4 129.8(17) . . ?
C1 O2 Gd4 97.8(4) . . ?
C16 O7 Gd4 135.5(4) . 2_656 ?
C16 O6 Gd4 134.6(4) . 8_466 ?
C15 O5 Gd4 99.4(4) . 3_445 ?
C9 O3 C8 115.5(5) . . ?
Gd4 O4 Gd4 104.43(16) 5_666 3_445 ?
C15 O4 Gd4 89.2(4) . 3_445 ?
C15 O4 Gd4 160.5(4) . 5_666 ?
C1 O1 Gd4 87.9(4) . . ?
C3 C4 H4 119.9 . . ?
C3 C4 C5 120.2(8) . . ?
C5 C4 H4 119.9 . . ?
C23 O9 Gd4 128.9(7) . . ?
C27 O9 Gd4 118.8(14) . . ?
C4 C3 H3 119.6 . . ?
C4 C3 C2 120.9(8) . . ?
C2 C3 H3 119.6 . . ?
O3 C9 C10 123.0(6) . . ?
C14 C9 O3 115.8(6) . . ?
C14 C9 C10 121.1(6) . . ?
C12 C11 C16 121.8(6) . . ?
C10 C11 C16 118.0(6) . . ?
C10 C11 C12 120.2(6) . . ?
O2 C1 Gd4 56.2(3) . . ?
O2 C1 C2 117.5(6) . . ?
O1 C1 Gd4 66.1(4) . . ?
O1 C1 O2 122.3(6) . . ?
O1 C1 C2 120.2(6) . . ?
C2 C1 Gd4 172.6(5) . . ?
O5 C15 Gd4 55.7(3) . 3_445 ?
O5 C15 O4 120.6(6) . . ?
O5 C15 C13 120.3(6) . . ?
O4 C15 Gd4 65.0(3) . 3_445 ?
O4 C15 C13 119.0(6) . . ?
C13 C15 Gd4 175.8(5) . 3_445 ?
O7 C16 O6 126.0(6) . . ?
O7 C16 C11 117.2(6) . . ?
O6 C16 C11 116.8(6) . . ?
C3 C2 C1 119.1(7) . . ?
C7 C2 C3 118.9(7) . . ?
C7 C2 C1 122.0(7) . . ?
C11 C12 H12 120.0 . . ?
C13 C12 C11 120.1(6) . . ?
C13 C12 H12 120.0 . . ?
O3 C8 H8A 109.9 . . ?
O3 C8 H8B 109.9 . . ?
O3 C8 C5 109.0(6) . . ?
H8A C8 H8B 108.3 . . ?
C5 C8 H8A 109.9 . . ?
C5 C8 H8B 109.9 . . ?
C9 C14 H14 120.2 . . ?
C9 C14 C13 119.5(6) . . ?
C13 C14 H14 120.2 . . ?
C12 C13 C15 120.3(6) . . ?
C12 C13 C14 120.0(6) . . ?
C14 C13 C15 119.6(6) . . ?
C9 C10 H10 120.5 . . ?
C11 C10 C9 119.0(6) . . ?
C11 C10 H10 120.5 . . ?
C4 C5 C8 116.7(7) . . ?
C6 C5 C4 119.5(7) . . ?
C6 C5 C8 123.6(8) . . ?
C23 N3 C24 123.8(11) . . ?
C23 N3 C25 121.6(12) . . ?
C25 N3 C24 114.4(11) . . ?
C5 C6 H6 120.0 . . ?
C5 C6 C7 120.1(8) . . ?
C7 C6 H6 120.0 . . ?
C2 C7 C6 120.5(7) . . ?
C2 C7 H7 119.8 . . ?
C6 C7 H7 119.8 . . ?
C18 N1 C19 116.2(11) . . ?
C17 N1 C18 121.5(11) . . ?
C17 N1 C19 120.9(11) . . ?
O9 C23 N3 135.2(13) . . ?
O9 C23 H23 112.4 . . ?
N3 C23 H23 112.4 . . ?
N1 C18 H18A 109.5 . . ?
N1 C18 H18B 109.5 . . ?
N1 C18 H18C 109.5 . . ?
H18A C18 H18B 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
O8 C17 N1 125.0(12) . . ?
O8 C17 H17 117.5 . . ?
N1 C17 H17 117.5 . . ?
N1 C19 H19A 109.5 . . ?
N1 C19 H19B 109.5 . . ?
N1 C19 H19C 109.5 . . ?
H19A C19 H19B 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
N3 C24 H24A 109.5 . . ?
N3 C24 H24B 109.5 . . ?
N3 C24 H24C 109.5 . . ?
H24A C24 H24B 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
N3 C25 H25A 109.5 . . ?
N3 C25 H25B 109.5 . . ?
N3 C25 H25C 109.5 . . ?
H25A C25 H25B 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
C29 N5 C30 121(2) . . ?
C29 N5 C31 122.8(16) . . ?
C31 N5 C30 116(2) . . ?
O10 C29 N5 126.1(17) . . ?
O10 C29 H29 117.0 . . ?
N5 C29 H29 117.0 . . ?
N5 C30 H30A 109.5 . . ?
N5 C30 H30B 109.5 . . ?
N5 C30 H30C 109.5 . . ?
H30A C30 H30B 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
N5 C31 H31A 109.5 . . ?
N5 C31 H31B 109.5 . . ?
N5 C31 H31C 109.5 . . ?
H31A C31 H31B 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
C22 N2 C21 122(3) . . ?
C20 N2 C22 123(3) . . ?
C20 N2 C21 110(3) . . ?
N2 C22 H22A 109.9 . . ?
N2 C22 H22B 109.0 . . ?
N2 C22 H22C 109.5 . . ?
H22A C22 H22B 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
O8 C20 N2 131(3) . . ?
O8 C20 H20 114.3 . . ?
N2 C20 H20 114.3 . . ?
N2 C21 H21A 109.5 . . ?
N2 C21 H21B 109.5 . . ?
N2 C21 H21C 109.5 . . ?
H21A C21 H21B 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C26 N4 C28 116(3) . . ?
C27 N4 C26 127(3) . . ?
C27 N4 C28 110(3) . . ?
N4 C26 H26A 109.5 . . ?
N4 C26 H26B 109.5 . . ?
N4 C26 H26C 109.5 . . ?
H26A C26 H26B 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
O9 C27 N4 119(3) . . ?
O9 C27 H27 120.5 . . ?
N4 C27 H27 120.5 . . ?
N4 C28 H28A 109.5 . . ?
N4 C28 H28B 109.5 . . ?
N4 C28 H28C 109.5 . . ?
H28A C28 H28B 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Gd4 O8 C17 N1 163.8(9) . . . . ?
Gd4 O8 C20 N2 174(4) . . . . ?
Gd4 O2 C1 O1 -2.3(8) . . . . ?
Gd4 O2 C1 C2 175.6(5) . . . . ?
Gd4 O7 C16 O6 37.3(10) 2_656 . . . ?
Gd4 O7 C16 C11 -142.8(5) 2_656 . . . ?
Gd4 O6 C16 O7 -10.0(11) 8_466 . . . ?
Gd4 O6 C16 C11 170.1(4) 8_466 . . . ?
Gd4 O5 C15 O4 -1.6(7) 3_445 . . . ?
Gd4 O5 C15 C13 178.3(5) 3_445 . . . ?
Gd4 O4 C15 Gd4 -135.2(12) 5_666 . . 3_445 ?
Gd4 O4 C15 O5 1.4(6) 3_445 . . . ?
Gd4 O4 C15 O5 -133.7(11) 5_666 . . . ?
Gd4 O4 C15 C13 46.4(15) 5_666 . . . ?
Gd4 O4 C15 C13 -178.5(5) 3_445 . . . ?
Gd4 O1 C1 O2 2.1(7) . . . . ?
Gd4 O1 C1 C2 -175.8(6) . . . . ?
Gd4 O9 C23 N3 -166.6(12) . . . . ?
Gd4 O9 C27 N4 164(3) . . . . ?
O2 C1 C2 C3 -0.2(11) . . . . ?
O2 C1 C2 C7 -177.4(8) . . . . ?
O5 C15 C13 C12 25.5(9) . . . . ?
O5 C15 C13 C14 -151.9(6) . . . . ?
O3 C9 C14 C13 -178.0(6) . . . . ?
O3 C9 C10 C11 178.9(6) . . . . ?
O3 C8 C5 C4 155.0(9) . . . . ?
O3 C8 C5 C6 -29.2(14) . . . . ?
O4 C15 C13 C12 -154.6(6) . . . . ?
O4 C15 C13 C14 28.0(9) . . . . ?
O1 C1 C2 C3 177.8(8) . . . . ?
O1 C1 C2 C7 0.5(12) . . . . ?
C4 C3 C2 C1 -175.5(9) . . . . ?
C4 C3 C2 C7 1.8(14) . . . . ?
C4 C5 C6 C7 -1.6(15) . . . . ?
C3 C4 C5 C8 176.9(10) . . . . ?
C3 C4 C5 C6 0.9(16) . . . . ?
C3 C2 C7 C6 -2.5(14) . . . . ?
C9 O3 C8 C5 -166.7(7) . . . . ?
C9 C14 C13 C15 176.7(6) . . . . ?
C9 C14 C13 C12 -0.7(10) . . . . ?
C11 C12 C13 C15 -179.8(6) . . . . ?
C11 C12 C13 C14 -2.4(10) . . . . ?
C1 C2 C7 C6 174.7(8) . . . . ?
C16 C11 C12 C13 -176.1(6) . . . . ?
C16 C11 C10 C9 178.4(6) . . . . ?
C12 C11 C16 O7 177.2(6) . . . . ?
C12 C11 C16 O6 -2.9(9) . . . . ?
C12 C11 C10 C9 -0.9(10) . . . . ?
C8 O3 C9 C14 164.2(7) . . . . ?
C8 O3 C9 C10 -16.9(10) . . . . ?
C8 C5 C6 C7 -177.3(9) . . . . ?
C14 C9 C10 C11 -2.3(10) . . . . ?
C10 C9 C14 C13 3.1(10) . . . . ?
C10 C11 C16 O7 -2.1(9) . . . . ?
C10 C11 C16 O6 177.8(6) . . . . ?
C10 C11 C12 C13 3.2(10) . . . . ?
C5 C4 C3 C2 -1.0(16) . . . . ?
C5 C6 C7 C2 2.5(15) . . . . ?
C18 N1 C17 O8 -10(2) . . . . ?
C19 N1 C17 O8 -175.6(14) . . . . ?
C24 N3 C23 O9 -174.4(14) . . . . ?
C25 N3 C23 O9 10(3) . . . . ?
C30 N5 C29 O10 -2(3) . . . . ?
C31 N5 C29 O10 -179.8(18) . . . . ?
C22 N2 C20 O8 168(4) . . . . ?
C21 N2 C20 O8 10(7) . . . . ?
C26 N4 C27 O9 33(6) . . . . ?
C28 N4 C27 O9 -178(3) . . . . ?

_platon_squeeze_details          ?
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.500 0.870 0.250 116 47 ' '
2 1.000 0.370 0.250 116 47 ' '
3 0.500 0.130 0.750 117 47 ' '
4 1.000 0.630 0.750 117 47 ' '

_platon_squeeze_void_probe_radius 1.20
_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_111_sq
_database_code_depnum_ccdc_archive 'CCDC 2071649'
loop_
_audit_author_name
_audit_author_address
'Yun-Shan Xue' 'Yancheng Teachers University'
_audit_update_record             
;
2021-03-19 deposited with the CCDC.	2021-04-20 downloaded from the CCDC.
;
_audit_creation_date             2019-06-26
_audit_creation_method           
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C22 H23 Eu N2 O9'
_chemical_formula_sum            'C22 H23 Eu N2 O9'
_chemical_formula_weight         611.38
_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      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 1 2/c 1'
_space_group_name_Hall           '-C 2yc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'

_cell_length_a                   28.698(4)
_cell_length_b                   14.307(2)
_cell_length_c                   13.8772(19)
_cell_angle_alpha                90
_cell_angle_beta                 99.521(4)
_cell_angle_gamma                90
_cell_volume                     5619.2(13)
_cell_formula_units_Z            8
_cell_measurement_reflns_used    6947
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.067
_cell_measurement_theta_min      2.977
_shelx_estimated_absorpt_T_max   0.804
_shelx_estimated_absorpt_T_min   0.726
_exptl_absorpt_coefficient_mu    2.278
_exptl_absorpt_correction_T_max  0.804
_exptl_absorpt_correction_T_min  0.726
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1419 before and 0.0691 after correction.
The Ratio of minimum to maximum transmission is 0.4159.
The λ/2 correction factor is Not present.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.445
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             2432
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.1
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0654
_diffrn_reflns_av_unetI/netI     0.0740
_diffrn_reflns_Laue_measured_fraction_full 0.983
_diffrn_reflns_Laue_measured_fraction_max 0.983
_diffrn_reflns_limit_h_max       34
_diffrn_reflns_limit_h_min       -34
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            16142
_diffrn_reflns_point_group_measured_fraction_full 0.983
_diffrn_reflns_point_group_measured_fraction_max 0.983
_diffrn_reflns_theta_full        25.005
_diffrn_reflns_theta_max         25.005
_diffrn_reflns_theta_min         2.977
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_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                3397
_reflns_number_total             4863
_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       'SAINT V8.38A (?, 2016)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    ?
_refine_diff_density_max         2.495
_refine_diff_density_min         -1.340
_refine_diff_density_rms         0.162
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.094
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     321
_refine_ls_number_reflns         4863
_refine_ls_number_restraints     185
_refine_ls_R_factor_all          0.0886
_refine_ls_R_factor_gt           0.0554
_refine_ls_restrained_S_all      1.133
_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)+(0.1000P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1552
_refine_ls_wR_factor_ref         0.1687
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 O9-C17
 1.2 with sigma of 0.01
 N1-C17
 1.3 with sigma of 0.01
 C22-C20
 2.45 with sigma of 0.01
 C13-C16
 1.5 with sigma of 0.01
 C10-C15
 1.39 with sigma of 0.01
 N1-C18 = N1-C19 = N2-C22 = N2-C21
 1.49 with sigma of 0.01
 O6-O4_$1
 3 with sigma of 0.01
 C2-C1
 1.51 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
O8 \\sim O9 \\sim N1 \\sim N2 \\sim C17 \\sim C18 \\sim C19 \\sim C20 \\sim C21
\\sim C22: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.01
Eu1 \\sim Eu2 \\sim O1 \\sim O2 \\sim O8 \\sim O9: within 3A with sigma of 0.02
and sigma for terminal atoms of 0.02
Uanis(C17) \\sim Ueq, Uanis(N1) \\sim Ueq, Uanis(C19) \\sim Ueq, Uanis(C18)
\\sim Ueq, Uanis(C21) \\sim Ueq, Uanis(N2) \\sim Ueq, Uanis(C22) \\sim Ueq,
Uanis(C20) \\sim Ueq, Uanis(O9) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C22) \\sim Ueq, Uanis(C20) \\sim Ueq, Uanis(N2) \\sim Ueq, Uanis(C21)
\\sim Ueq, Uanis(C22) \\sim Ueq, Uanis(C17) \\sim Ueq, Uanis(N1) \\sim Ueq,
Uanis(C18) \\sim Ueq, Uanis(C19) \\sim Ueq: with sigma of 0.0001 and sigma for
terminal atoms of 0.0002
4. Others
 Sof(Eu2)=1-FVAR(1)
 Sof(Eu1)=FVAR(1)
5.a Secondary CH2 refined with riding coordinates:
 C9(H9A,H9B)
5.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C7(H7), C11(H11), C12(H12), C14(H14), C15(H15), C17(H17),
 C20(H20)
5.c Idealised Me refined as rotating group:
 C18(H18A,H18B,H18C), C19(H19A,H19B,H19C), C21(H21A,H21B,H21C), C22(H22A,H22B,
 H22C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_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 0.18218(9) -0.21400(15) 0.45953(16) 0.0226(13) Uani 0.62(6) 1 d . U P A
1
Eu2 Eu 0.18243(17) -0.2123(4) 0.4613(4) 0.049(3) Uani 0.38(6) 1 d . U P A 2
O1 O 0.2062(2) -0.0730(4) 0.5589(5) 0.0517(16) Uani 1 1 d . U . . .
O2 O 0.26866(19) -0.1536(3) 0.5455(4) 0.0366(13) Uani 1 1 d . U . . .
O3 O 0.2297(2) 0.1605(4) 0.8405(4) 0.0470(16) Uani 1 1 d . . . . .
O4 O 0.3003(2) 0.2298(4) 0.8747(4) 0.0413(15) Uani 1 1 d D . . . .
O5 O 0.3984(2) 0.0872(4) 0.6412(4) 0.0527(17) Uani 1 1 d . . . . .
O6 O 0.6182(2) 0.1653(4) 0.4870(5) 0.0585(18) Uani 1 1 d D . . . .
O7 O 0.6077(2) 0.3143(4) 0.5134(6) 0.061(2) Uani 1 1 d . . . . .
O8 O 0.1432(3) -0.0797(6) 0.3651(6) 0.085(2) Uani 1 1 d . U . . .
O9 O 0.1437(3) -0.2805(5) 0.3059(6) 0.080(2) Uani 1 1 d D U . . .
N1 N 0.1208(6) -0.3709(11) 0.1724(12) 0.163(2) Uani 1 1 d D U . . .
N2 N 0.1144(7) -0.0055(12) 0.1986(12) 0.183(2) Uani 1 1 d D U . . .
C1 C 0.2491(3) -0.0818(5) 0.5738(5) 0.035(2) Uani 1 1 d D . . . .
C2 C 0.2792(3) -0.0076(5) 0.6297(6) 0.035(2) Uani 1 1 d D . . . .
C3 C 0.2610(3) 0.0482(5) 0.6984(6) 0.040(2) Uani 1 1 d . . . . .
H3 H 0.229981 0.040367 0.708222 0.048 Uiso 1 1 calc R . . . .
C4 C 0.2898(3) 0.1153(5) 0.7515(6) 0.039(2) Uani 1 1 d . . . . .
C5 C 0.3357(3) 0.1303(5) 0.7349(6) 0.041(2) Uani 1 1 d . . . . .
H5 H 0.354818 0.175393 0.769846 0.049 Uiso 1 1 calc R . . . .
C6 C 0.3523(3) 0.0754(6) 0.6642(7) 0.044(2) Uani 1 1 d . . . . .
C7 C 0.3246(3) 0.0047(5) 0.6127(6) 0.041(2) Uani 1 1 d . . . . .
H7 H 0.336726 -0.032881 0.568123 0.050 Uiso 1 1 calc R . . . .
C8 C 0.2724(3) 0.1723(6) 0.8284(6) 0.034(2) Uani 1 1 d . . . . .
C9 C 0.4217(4) 0.1687(8) 0.6729(8) 0.069(3) Uani 1 1 d . . . . .
H9A H 0.430933 0.166944 0.743384 0.083 Uiso 1 1 calc R . . . .
H9B H 0.400859 0.221714 0.656463 0.083 Uiso 1 1 calc R . . . .
C10 C 0.4647(4) 0.1794(6) 0.6256(8) 0.060(3) Uani 1 1 d D . . . .
C11 C 0.4907(4) 0.1076(7) 0.5961(9) 0.078(4) Uani 1 1 d . . . . .
H11 H 0.480119 0.046550 0.600434 0.094 Uiso 1 1 calc R . . . .
C12 C 0.5324(4) 0.1229(7) 0.5599(9) 0.074(4) Uani 1 1 d . . . . .
H12 H 0.549433 0.072167 0.542392 0.089 Uiso 1 1 calc R . . . .
C13 C 0.5485(3) 0.2106(6) 0.5499(7) 0.047(2) Uani 1 1 d D . . . .
C14 C 0.5220(4) 0.2844(7) 0.5782(9) 0.067(3) Uani 1 1 d . . . . .
H14 H 0.532547 0.345277 0.572019 0.080 Uiso 1 1 calc R . . . .
C15 C 0.4805(4) 0.2701(6) 0.6152(10) 0.077(4) Uani 1 1 d D . . . .
H15 H 0.463426 0.320746 0.632833 0.093 Uiso 1 1 calc R . . . .
C16 C 0.5946(3) 0.2308(6) 0.5146(7) 0.046(2) Uani 1 1 d D . . . .
C17 C 0.1509(7) -0.3224(12) 0.2362(10) 0.137(2) Uani 1 1 d D U . . .
H17 H 0.181899 -0.321254 0.224714 0.164 Uiso 1 1 calc R . . . .
C18 C 0.1454(7) -0.4188(13) 0.1025(13) 0.172(4) Uani 1 1 d D U . . .
H18A H 0.158542 -0.373449 0.063628 0.258 Uiso 1 1 calc GR . . . .
H18B H 0.123543 -0.457913 0.060803 0.258 Uiso 1 1 calc GR . . . .
H18C H 0.170340 -0.456568 0.137229 0.258 Uiso 1 1 calc GR . . . .
C19 C 0.0745(6) -0.3943(14) 0.1981(15) 0.181(4) Uani 1 1 d D U . . .
H19A H 0.071903 -0.460829 0.204204 0.271 Uiso 1 1 calc GR . . . .
H19B H 0.049898 -0.372103 0.147890 0.271 Uiso 1 1 calc GR . . . .
H19C H 0.071434 -0.365148 0.259089 0.271 Uiso 1 1 calc GR . . . .
C20 C 0.1319(7) -0.0894(11) 0.2641(14) 0.154(2) Uani 1 1 d D U . . .
H20 H 0.135043 -0.147459 0.235810 0.185 Uiso 1 1 calc R . . . .
C21 C 0.0994(8) -0.0311(15) 0.0923(13) 0.199(4) Uani 1 1 d D U . . .
H21A H 0.065504 -0.029720 0.076437 0.298 Uiso 1 1 calc GR . . . .
H21B H 0.110523 -0.092668 0.080880 0.298 Uiso 1 1 calc GR . . . .
H21C H 0.112481 0.013022 0.052005 0.298 Uiso 1 1 calc GR . . . .
C22 C 0.1286(9) 0.0805(10) 0.2599(14) 0.204(4) Uani 1 1 d D U . . .
H22A H 0.141455 0.126302 0.221203 0.306 Uiso 1 1 calc GR . . . .
H22B H 0.151888 0.063793 0.315081 0.306 Uiso 1 1 calc GR . . . .
H22C H 0.101308 0.105890 0.282399 0.306 Uiso 1 1 calc GR . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Eu1 Eu1 4.004(5) 7_546 ?
Eu1 O1 2.475(6) . ?
Eu1 O2 2.370(5) 7_546 ?
Eu1 O2 2.711(6) . ?
Eu1 O3 2.433(5) 6 ?
Eu1 O4 2.410(6) 4_546 ?
Eu1 O6 2.594(6) 3_445 ?
Eu1 O7 2.412(7) 3_445 ?
Eu1 O8 2.485(8) . ?
Eu1 O9 2.427(9) . ?
Eu1 C1 2.961(8) . ?
Eu1 C16 2.857(8) 3_445 ?
Eu2 O1 2.442(8) . ?
Eu2 O2 2.690(8) . ?
Eu2 O2 2.388(7) 7_546 ?
Eu2 O3 2.439(7) 6 ?
Eu2 O4 2.396(7) 4_546 ?
Eu2 O6 2.610(7) 3_445 ?
Eu2 O7 2.404(8) 3_445 ?
Eu2 O8 2.480(9) . ?
Eu2 O9 2.458(11) . ?
Eu2 C1 2.931(9) . ?
Eu2 C16 2.861(9) 3_445 ?
O1 C1 1.221(10) . ?
O2 C1 1.264(9) . ?
O3 C8 1.276(9) . ?
O4 C8 1.250(10) . ?
O5 C6 1.422(10) . ?
O5 C9 1.380(11) . ?
O6 C16 1.254(10) . ?
O7 C16 1.253(10) . ?
O8 C20 1.392(18) . ?
O9 C17 1.184(9) . ?
N1 C17 1.327(9) . ?
N1 C18 1.462(9) . ?
N1 C19 1.470(9) . ?
N2 C20 1.54(2) . ?
N2 C21 1.512(9) . ?
N2 C22 1.513(9) . ?
C1 C2 1.502(7) . ?
C2 C3 1.409(10) . ?
C2 C7 1.372(11) . ?
C3 C4 1.394(11) . ?
C4 C5 1.392(11) . ?
C4 C8 1.492(11) . ?
C5 C6 1.399(10) . ?
C6 C7 1.407(11) . ?
C9 C10 1.498(13) . ?
C10 C11 1.373(13) . ?
C10 C15 1.390(8) . ?
C11 C12 1.387(14) . ?
C12 C13 1.353(12) . ?
C13 C14 1.394(12) . ?
C13 C16 1.513(8) . ?
C14 C15 1.389(14) . ?

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 Eu1 83.43(18) . 7_546 ?
O1 Eu1 O2 49.10(19) . . ?
O1 Eu1 O6 126.8(2) . 3_445 ?
O1 Eu1 O8 73.9(3) . . ?
O1 Eu1 C1 23.9(2) . . ?
O1 Eu1 C16 104.6(3) . 3_445 ?
O2 Eu1 Eu1 41.12(14) 7_546 7_546 ?
O2 Eu1 Eu1 35.09(11) . 7_546 ?
O2 Eu1 O1 123.7(2) 7_546 . ?
O2 Eu1 O2 76.21(19) 7_546 . ?
O2 Eu1 O3 80.12(19) 7_546 6 ?
O2 Eu1 O4 74.35(19) 7_546 4_546 ?
O2 Eu1 O6 84.9(2) 7_546 3_445 ?
O2 Eu1 O7 134.9(2) 7_546 3_445 ?
O2 Eu1 O8 145.2(2) 7_546 . ?
O2 Eu1 O9 81.2(2) 7_546 . ?
O2 Eu1 C1 100.9(2) 7_546 . ?
O2 Eu1 C1 25.26(18) . . ?
O2 Eu1 C16 110.0(2) 7_546 3_445 ?
O2 Eu1 C16 138.8(2) . 3_445 ?
O3 Eu1 Eu1 69.12(15) 6 7_546 ?
O3 Eu1 O1 89.2(2) 6 . ?
O3 Eu1 O2 67.89(19) 6 . ?
O3 Eu1 O6 143.0(2) 6 3_445 ?
O3 Eu1 O8 69.7(2) 6 . ?
O3 Eu1 C1 77.1(2) 6 . ?
O3 Eu1 C16 152.3(3) 6 3_445 ?
O4 Eu1 Eu1 66.84(15) 4_546 7_546 ?
O4 Eu1 O1 75.2(2) 4_546 . ?
O4 Eu1 O2 69.81(19) 4_546 . ?
O4 Eu1 O3 134.5(2) 4_546 6 ?
O4 Eu1 O6 71.25(18) 4_546 3_445 ?
O4 Eu1 O7 79.4(2) 4_546 3_445 ?
O4 Eu1 O8 140.0(2) 4_546 . ?
O4 Eu1 O9 134.5(2) 4_546 . ?
O4 Eu1 C1 71.8(2) 4_546 . ?
O4 Eu1 C16 72.9(2) 4_546 3_445 ?
O6 Eu1 Eu1 117.79(18) 3_445 7_546 ?
O6 Eu1 O2 140.0(2) 3_445 . ?
O6 Eu1 C1 139.3(2) 3_445 . ?
O6 Eu1 C16 26.0(2) 3_445 3_445 ?
O7 Eu1 Eu1 145.7(2) 3_445 7_546 ?
O7 Eu1 O1 82.5(2) 3_445 . ?
O7 Eu1 O2 127.1(2) 3_445 . ?
O7 Eu1 O3 141.5(2) 3_445 6 ?
O7 Eu1 O6 51.8(2) 3_445 3_445 ?
O7 Eu1 O8 71.9(2) 3_445 . ?
O7 Eu1 O9 92.3(3) 3_445 . ?
O7 Eu1 C1 104.8(2) 3_445 . ?
O7 Eu1 C16 25.8(2) 3_445 3_445 ?
O8 Eu1 Eu1 132.8(2) . 7_546 ?
O8 Eu1 O2 106.6(2) . . ?
O8 Eu1 O6 108.9(3) . 3_445 ?
O8 Eu1 C1 89.1(3) . . ?
O8 Eu1 C16 90.9(3) . 3_445 ?
O9 Eu1 Eu1 115.2(2) . 7_546 ?
O9 Eu1 O1 148.5(3) . . ?
O9 Eu1 O2 139.6(2) . . ?
O9 Eu1 O3 75.6(3) . 6 ?
O9 Eu1 O6 68.8(2) . 3_445 ?
O9 Eu1 O8 75.0(3) . . ?
O9 Eu1 C1 151.8(2) . . ?
O9 Eu1 C16 80.5(3) . 3_445 ?
C1 Eu1 Eu1 60.00(18) . 7_546 ?
C16 Eu1 Eu1 135.4(2) 3_445 7_546 ?
C16 Eu1 C1 123.7(3) 3_445 . ?
O1 Eu2 O2 49.6(2) . . ?
O1 Eu2 O6 127.6(3) . 3_445 ?
O1 Eu2 O8 74.6(3) . . ?
O1 Eu2 O9 148.7(3) . . ?
O1 Eu2 C1 24.1(2) . . ?
O1 Eu2 C16 105.4(3) . 3_445 ?
O2 Eu2 O1 124.4(3) 7_546 . ?
O2 Eu2 O2 76.3(2) 7_546 . ?
O2 Eu2 O3 79.6(2) 7_546 6 ?
O2 Eu2 O4 74.3(2) 7_546 4_546 ?
O2 Eu2 O6 84.2(3) 7_546 3_445 ?
O2 Eu2 O7 134.3(3) 7_546 3_445 ?
O2 Eu2 O8 144.2(3) 7_546 . ?
O2 Eu2 O9 80.2(3) 7_546 . ?
O2 Eu2 C1 101.3(3) 7_546 . ?
O2 Eu2 C1 25.53(19) . . ?
O2 Eu2 C16 139.7(3) . 3_445 ?
O2 Eu2 C16 109.3(3) 7_546 3_445 ?
O3 Eu2 O1 89.9(3) 6 . ?
O3 Eu2 O2 68.2(2) 6 . ?
O3 Eu2 O6 141.6(3) 6 3_445 ?
O3 Eu2 O8 69.7(3) 6 . ?
O3 Eu2 O9 74.9(3) 6 . ?
O3 Eu2 C1 77.6(2) 6 . ?
O3 Eu2 C16 151.4(3) 6 3_445 ?
O4 Eu2 O1 76.1(3) 4_546 . ?
O4 Eu2 O2 70.4(2) 4_546 . ?
O4 Eu2 O3 135.0(3) 4_546 6 ?
O4 Eu2 O6 71.2(2) 4_546 3_445 ?
O4 Eu2 O7 79.8(3) 4_546 3_445 ?
O4 Eu2 O8 141.2(3) 4_546 . ?
O4 Eu2 O9 133.5(3) 4_546 . ?
O4 Eu2 C1 72.5(3) 4_546 . ?
O4 Eu2 C16 73.1(3) 4_546 3_445 ?
O6 Eu2 O2 140.3(3) 3_445 . ?
O6 Eu2 C1 140.2(3) 3_445 . ?
O6 Eu2 C16 26.0(2) 3_445 3_445 ?
O7 Eu2 O1 83.4(3) 3_445 . ?
O7 Eu2 O2 128.5(3) 3_445 . ?
O7 Eu2 O3 141.6(3) 3_445 6 ?
O7 Eu2 O6 51.7(2) 3_445 3_445 ?
O7 Eu2 O8 72.1(3) 3_445 . ?
O7 Eu2 O9 91.7(3) 3_445 . ?
O7 Eu2 C1 106.0(3) 3_445 . ?
O7 Eu2 C16 25.7(2) 3_445 3_445 ?
O8 Eu2 O2 107.4(3) . . ?
O8 Eu2 O6 108.6(3) . 3_445 ?
O8 Eu2 C1 89.9(3) . . ?
O8 Eu2 C16 90.9(3) . 3_445 ?
O9 Eu2 O2 139.0(3) . . ?
O9 Eu2 O6 68.1(3) . 3_445 ?
O9 Eu2 O8 74.5(3) . . ?
O9 Eu2 C1 151.7(3) . . ?
O9 Eu2 C16 79.9(3) . 3_445 ?
C16 Eu2 C1 124.6(3) 3_445 . ?
C1 O1 Eu1 101.0(5) . . ?
C1 O1 Eu2 101.0(5) . . ?
Eu1 O2 Eu1 103.79(19) 7_546 . ?
C1 O2 Eu1 163.0(5) . 7_546 ?
C1 O2 Eu1 88.5(5) . . ?
C1 O2 Eu2 87.9(5) . . ?
C8 O3 Eu1 134.9(5) . 6_556 ?
C8 O4 Eu1 136.5(5) . 4_556 ?
C9 O5 C6 116.7(6) . . ?
C16 O6 Eu1 88.8(5) . 3 ?
C16 O7 Eu1 97.4(5) . 3 ?
C20 O8 Eu1 117.6(8) . . ?
C20 O8 Eu2 118.3(8) . . ?
C17 O9 Eu1 143.2(11) . . ?
C17 O9 Eu2 143.4(11) . . ?
C17 N1 C18 110.8(14) . . ?
C17 N1 C19 118.1(17) . . ?
C18 N1 C19 127.6(17) . . ?
C21 N2 C20 113.6(16) . . ?
C21 N2 C22 138.8(18) . . ?
C22 N2 C20 105.7(11) . . ?
O1 C1 Eu1 55.2(4) . . ?
O1 C1 Eu2 54.9(4) . . ?
O1 C1 O2 121.3(7) . . ?
O1 C1 C2 119.6(7) . . ?
O2 C1 Eu1 66.2(4) . . ?
O2 C1 Eu2 66.5(4) . . ?
O2 C1 C2 119.1(7) . . ?
C2 C1 Eu1 174.3(6) . . ?
C2 C1 Eu2 174.1(6) . . ?
C3 C2 C1 120.3(7) . . ?
C7 C2 C1 118.9(7) . . ?
C7 C2 C3 120.8(7) . . ?
C4 C3 C2 119.7(7) . . ?
C3 C4 C8 121.1(8) . . ?
C5 C4 C3 120.8(7) . . ?
C5 C4 C8 118.1(8) . . ?
C4 C5 C6 118.1(8) . . ?
C5 C6 O5 121.9(7) . . ?
C5 C6 C7 122.1(7) . . ?
C7 C6 O5 116.1(7) . . ?
C2 C7 C6 118.5(7) . . ?
O3 C8 C4 117.6(8) . . ?
O4 C8 O3 124.6(7) . . ?
O4 C8 C4 117.8(7) . . ?
O5 C9 C10 109.8(8) . . ?
C11 C10 C9 125.6(8) . . ?
C11 C10 C15 117.7(9) . . ?
C15 C10 C9 116.6(9) . . ?
C10 C11 C12 122.2(9) . . ?
C13 C12 C11 120.9(9) . . ?
C12 C13 C14 117.6(8) . . ?
C12 C13 C16 122.8(8) . . ?
C14 C13 C16 119.5(8) . . ?
C15 C14 C13 122.2(9) . . ?
C14 C15 C10 119.4(9) . . ?
O6 C16 Eu1 65.2(4) . 3 ?
O6 C16 C13 120.1(8) . . ?
O7 C16 Eu1 56.9(4) . 3 ?
O7 C16 O6 122.0(7) . . ?
O7 C16 C13 117.9(8) . . ?
C13 C16 Eu1 174.2(7) . 3 ?
O9 C17 N1 128.9(18) . . ?
O8 C20 N2 121.1(12) . . ?

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

data_1
_database_code_depnum_ccdc_archive 'CCDC 2071651'
loop_
_audit_author_name
_audit_author_address
'Yun-Shan Xue' 'Yancheng Teachers University'
_audit_update_record             
;
2021-03-19 deposited with the CCDC.	2021-04-20 downloaded from the CCDC.
;
_audit_creation_date             2020-07-30
_audit_creation_method           
;
Olex2 1.2-beta
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         '0.11(C288 H207 Dy18 O148.5)'
_chemical_formula_sum            'C32 H23 Dy2 O16.50'
_chemical_formula_weight         996.50
_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'
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      trigonal
_space_group_IT_number           148
_space_group_name_H-M_alt        'R -3'
_space_group_name_Hall           '-R 3'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'

_cell_length_a                   19.6983(10)
_cell_length_b                   19.6983(10)
_cell_length_c                   45.340(2)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     15235.8(17)
_cell_formula_units_Z            9
_cell_measurement_reflns_used    9993
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      26.36
_cell_measurement_theta_min      2.47
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    2.228
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.6064
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0970 before and 0.0485 after correction.
The Ratio of minimum to maximum transmission is 0.8135.
The λ/2 correction factor is Not present.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    0.977
_exptl_crystal_density_meas      .
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             4311
_exptl_crystal_size_max          ?
_exptl_crystal_size_mid          ?
_exptl_crystal_size_min          ?
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0248
_diffrn_reflns_av_unetI/netI     0.0228
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       56
_diffrn_reflns_limit_l_min       -54
_diffrn_reflns_number            33351
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.420
_diffrn_reflns_theta_min         2.157
_diffrn_ambient_temperature      150.01
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                5998
_reflns_number_total             6948
_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       'SAINT v8.37A (Bruker, 2015)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         1.925
_refine_diff_density_min         -1.491
_refine_diff_density_rms         0.113
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     257
_refine_ls_number_reflns         6948
_refine_ls_number_restraints     47
_refine_ls_R_factor_all          0.0436
_refine_ls_R_factor_gt           0.0371
_refine_ls_restrained_S_all      1.075
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0501P)²+159.9902P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1042
_refine_ls_wR_factor_ref         0.1087
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All O(H,H) groups
2. Restrained distances
 O3B-C9 = O3A-C9
 1.45 with sigma of 0.01
 O3B-C1AA = O3A-C1AA
 1.4 with sigma of 0.02
 O1AA-Dy1
 2.45 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
Uanis(O3A) \\sim Ueq, Uanis(C1AA) \\sim Ueq, Uanis(C9) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
Uanis(O3B) \\sim Ueq, Uanis(O3A) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(O1AA) \\sim Ueq, Uanis(O2AA) \\sim Ueq: with sigma of 0.001 and sigma for
terminal atoms of 0.002
Uanis(O2AA) \\sim Ueq, Uanis(O0AA) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
4. Others
 Sof(H9BC)=Sof(H9BD)=Sof(O3B)=1-FVAR(1)
 Sof(O1AA)=Sof(H1AA)=Sof(H1AB)=0.75*(1-FVAR(2))
 Sof(O2AA)=Sof(H2AA)=Sof(H2AB)=0.75*FVAR(2)
 Sof(O3A)=Sof(H9AA)=Sof(H9AB)=FVAR(1)
 Fixed Sof: O0AA(0.5) H0AA(0.5) H0AB(0.5)
5.a Rotating group:
 O0AA(H0AA,H0AB), O2AA(H2AA,H2AB), O1AA(H1AA,H1AB)
5.b Secondary CH2 refined with riding coordinates:
 C9(H9AA,H9AB), C9(H9BC,H9BD)
5.c Aromatic/amide H refined with riding coordinates:
 C7(H7), C3(H3), C5(H5), C12(H12), C14(H14), C11(H11), C15(H15)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     ?
_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 0.62118(2) 0.80571(2) 0.87441(2) 0.02766(8) Uani 1 1 d D . . . .
O7 O 0.2485(2) 0.3880(2) 0.81747(7) 0.0458(9) Uani 1 1 d . . . . .
O6 O 0.3097(2) 0.4647(2) 0.85546(7) 0.0470(9) Uani 1 1 d . . . . .
O5 O 0.4717(2) 0.4068(2) 0.58528(7) 0.0476(9) Uani 1 1 d . . . . .
O2 O 0.6234(2) 0.7285(2) 0.79828(7) 0.0555(11) Uani 1 1 d . . . . .
O1 O 0.5561(2) 0.7074(2) 0.84038(7) 0.0590(12) Uani 1 1 d . . . . .
O4 O 0.4921(3) 0.5268(2) 0.58447(8) 0.0640(12) Uani 1 1 d . . . . .
C16 C 0.4699(3) 0.4627(3) 0.59753(9) 0.0433(12) Uani 1 1 d . . . . .
O3A O 0.4546(7) 0.4963(8) 0.7353(3) 0.032(3) Uani 0.317(15) 1 d D U P A 1
C8 C 0.3076(3) 0.4469(3) 0.82866(10) 0.0461(13) Uani 1 1 d . . . . .
C7 C 0.4365(3) 0.5643(3) 0.82067(10) 0.0465(13) Uani 1 1 d . . . . .
H7 H 0.435603 0.577780 0.840729 0.056 Uiso 1 1 calc R . . . .
C6 C 0.3760(3) 0.4972(3) 0.80928(10) 0.0532(16) Uani 1 1 d . . . . .
C1 C 0.5652(3) 0.6895(3) 0.81451(11) 0.0513(15) Uani 1 1 d . . . . .
C13 C 0.4423(3) 0.4538(4) 0.62873(11) 0.0568(16) Uani 1 1 d . . . . .
C2 C 0.4999(3) 0.6133(3) 0.80254(11) 0.0549(16) Uani 1 1 d . . . . .
C3 C 0.5011(4) 0.5924(4) 0.77352(12) 0.077(2) Uani 1 1 d . . . . .
H3 H 0.543640 0.625930 0.761091 0.092 Uiso 1 1 calc R . . . .
C10 C 0.4003(4) 0.4410(4) 0.68821(13) 0.076(2) Uani 1 1 d . . . . .
C1AA C 0.4404(4) 0.5226(4) 0.76243(12) 0.078(2) Uani 1 1 d D U . . .
C5 C 0.3761(4) 0.4751(4) 0.78007(12) 0.082(3) Uani 1 1 d . . . . .
H5 H 0.333195 0.428556 0.772383 0.099 Uiso 1 1 calc R . . . .
C12 C 0.4214(5) 0.5044(5) 0.64047(15) 0.081(2) Uani 1 1 d . . . . .
H12 H 0.421278 0.543881 0.628520 0.098 Uiso 1 1 calc R . . . .
C14 C 0.4391(5) 0.3950(4) 0.64622(12) 0.073(2) Uani 1 1 d . . . . .
H14 H 0.450473 0.357449 0.637975 0.088 Uiso 1 1 calc R . . . .
C11 C 0.3998(5) 0.4977(5) 0.67092(17) 0.091(3) Uani 1 1 d . . . . .
H11 H 0.385043 0.532760 0.679165 0.109 Uiso 1 1 calc R . . . .
C9 C 0.3822(4) 0.4390(4) 0.72082(13) 0.090(3) Uani 1 1 d D U . . .
H9AA H 0.340694 0.452629 0.723925 0.108 Uiso 0.317(15) 1 calc R . P A 1
H9AB H 0.363976 0.386050 0.728968 0.108 Uiso 0.317(15) 1 calc R . P A 1
H9BC H 0.328521 0.429903 0.723825 0.108 Uiso 0.683(15) 1 calc R . P A 2
H9BD H 0.387019 0.397123 0.730965 0.108 Uiso 0.683(15) 1 calc R . P A 2
C15 C 0.4193(5) 0.3905(5) 0.67621(14) 0.092(3) Uani 1 1 d . . . . .
H15 H 0.419304 0.350959 0.688193 0.110 Uiso 1 1 calc R . . . .
O3B O 0.4405(6) 0.5161(6) 0.73188(19) 0.093(4) Uani 0.683(15) 1 d D U P A 2
O0AA O 0.4921(4) 0.7207(4) 0.89617(14) 0.0478(19) Uani 0.5 1 d . U P A .
H0AA H 0.474933 0.684730 0.919839 0.072 Uiso 0.5 1 d GR . P . .
H0AB H 0.426244 0.701521 0.886482 0.072 Uiso 0.5 1 d GR . P . .
O2AA O 0.5732(8) 0.6989(7) 0.9021(3) 0.033(4) Uani 0.238(11) 1 d . U P A 1
H2AA H 0.563424 0.687689 0.930463 0.049 Uiso 0.238(11) 1 d GR . P A 1
H2AB H 0.546681 0.625009 0.895353 0.049 Uiso 0.238(11) 1 d GR . P A 1
O1AA O 0.6124(5) 0.6858(4) 0.89396(16) 0.050(2) Uani 0.512(11) 1 d D U P A 2
H1AA H 0.559408 0.624476 0.896184 0.075 Uiso 0.512(11) 1 d GR . P A 2
H1AB H 0.662017 0.677799 0.902799 0.075 Uiso 0.512(11) 1 d GR . P A 2


_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 O7 2.276(3) 17_556 ?
Dy1 O7 2.839(3) 2_665 ?
Dy1 O6 2.346(3) 2_665 ?
Dy1 O5 2.408(3) 6_565 ?
Dy1 O2 2.318(4) 16_666 ?
Dy1 O1 2.300(3) . ?
Dy1 O4 2.399(3) 6_565 ?
Dy1 C16 2.749(4) 6_565 ?
Dy1 C8 2.954(5) 2_665 ?
Dy1 O0AA 2.447(6) . ?
Dy1 O2AA 2.215(12) . ?
Dy1 O1AA 2.447(6) . ?
O7 C8 1.268(6) . ?
O6 C8 1.259(5) . ?
O5 C16 1.249(6) . ?
O2 C1 1.251(6) . ?
O1 C1 1.264(6) . ?
O4 C16 1.260(7) . ?
C16 C13 1.494(6) . ?
O3A C1AA 1.415(13) . ?
O3A C9 1.459(9) . ?
C8 C6 1.495(6) . ?
C7 C6 1.364(7) . ?
C7 C2 1.401(7) . ?
C6 C5 1.394(7) . ?
C1 C2 1.507(7) . ?
C13 C12 1.362(10) . ?
C13 C14 1.379(10) . ?
C2 C3 1.383(7) . ?
C3 C1AA 1.389(8) . ?
C10 C11 1.369(12) . ?
C10 C9 1.517(8) . ?
C10 C15 1.340(12) . ?
C1AA C5 1.391(8) . ?
C1AA O3B 1.391(10) . ?
C12 C11 1.431(9) . ?
C14 C15 1.405(8) . ?
C9 O3B 1.459(8) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O7 Dy1 O7 76.21(11) 17_556 2_665 ?
O7 Dy1 O6 125.52(11) 17_556 2_665 ?
O7 Dy1 O5 138.75(13) 17_556 6_565 ?
O7 Dy1 O2 76.83(15) 17_556 16_666 ?
O7 Dy1 O1 77.50(14) 17_556 . ?
O7 Dy1 O4 88.13(13) 17_556 6_565 ?
O7 Dy1 C16 114.09(15) 17_556 6_565 ?
O7 Dy1 C8 101.39(12) 17_556 2_665 ?
O7 Dy1 C8 25.19(11) 2_665 2_665 ?
O7 Dy1 O0AA 143.8(2) 17_556 . ?
O7 Dy1 O1AA 80.1(2) 17_556 . ?
O6 Dy1 O7 49.32(10) 2_665 2_665 ?
O6 Dy1 O5 81.29(12) 2_665 6_565 ?
O6 Dy1 O4 133.05(14) 2_665 6_565 ?
O6 Dy1 C16 107.36(15) 2_665 6_565 ?
O6 Dy1 C8 24.19(12) 2_665 2_665 ?
O6 Dy1 O0AA 72.5(2) 2_665 . ?
O6 Dy1 O1AA 137.4(2) 2_665 . ?
O5 Dy1 O7 121.88(12) 6_565 2_665 ?
O5 Dy1 C16 27.01(15) 6_565 6_565 ?
O5 Dy1 C8 102.23(13) 6_565 2_665 ?
O5 Dy1 O0AA 68.23(18) 6_565 . ?
O5 Dy1 O1AA 100.9(2) 6_565 . ?
O2 Dy1 O7 67.69(13) 16_666 2_665 ?
O2 Dy1 O6 81.26(16) 16_666 2_665 ?
O2 Dy1 O5 77.66(13) 16_666 6_565 ?
O2 Dy1 O4 75.65(16) 16_666 6_565 ?
O2 Dy1 C16 75.39(14) 16_666 6_565 ?
O2 Dy1 C8 74.32(16) 16_666 2_665 ?
O2 Dy1 O0AA 139.3(2) 16_666 . ?
O2 Dy1 O1AA 141.1(2) 16_666 . ?
O1 Dy1 O7 66.12(13) . 2_665 ?
O1 Dy1 O6 80.88(16) . 2_665 ?
O1 Dy1 O5 142.59(13) . 6_565 ?
O1 Dy1 O2 131.09(12) . 16_666 ?
O1 Dy1 O4 143.58(17) . 6_565 ?
O1 Dy1 C16 153.52(14) . 6_565 ?
O1 Dy1 C8 70.93(17) . 2_665 ?
O1 Dy1 O0AA 75.12(17) . . ?
O1 Dy1 O1AA 71.9(2) . . ?
O4 Dy1 O7 142.46(15) 6_565 2_665 ?
O4 Dy1 O5 54.26(13) 6_565 6_565 ?
O4 Dy1 C16 27.26(15) 6_565 6_565 ?
O4 Dy1 C8 145.36(17) 6_565 2_665 ?
O4 Dy1 O0AA 100.2(2) 6_565 . ?
O4 Dy1 O1AA 72.7(2) 6_565 . ?
C16 Dy1 O7 138.24(14) 6_565 2_665 ?
C16 Dy1 C8 125.67(16) 6_565 2_665 ?
O0AA Dy1 O7 112.6(2) . 2_665 ?
O0AA Dy1 C16 83.33(19) . 6_565 ?
O0AA Dy1 C8 91.6(2) . 2_665 ?
O0AA Dy1 O1AA 69.2(3) . . ?
O2AA Dy1 O7 143.0(3) . 2_665 ?
O2AA Dy1 O7 104.2(4) . 17_556 ?
O2AA Dy1 O6 119.0(4) . 2_665 ?
O2AA Dy1 O5 82.7(4) . 6_565 ?
O2AA Dy1 O2 149.2(3) . 16_666 ?
O2AA Dy1 O1 77.7(3) . . ?
O2AA Dy1 O4 73.6(4) . 6_565 ?
O2AA Dy1 C16 76.3(4) . 6_565 ?
O2AA Dy1 C8 133.6(4) . 2_665 ?
O2AA Dy1 O0AA 46.9(4) . . ?
O1AA Dy1 C8 141.5(2) . 2_665 ?
Dy1 O7 Dy1 103.79(11) 18_546 3_565 ?
C8 O7 Dy1 173.4(3) . 18_546 ?
C8 O7 Dy1 82.5(3) . 3_565 ?
C8 O6 Dy1 106.1(3) . 3_565 ?
C16 O5 Dy1 91.9(3) . 8_654 ?
C1 O2 Dy1 134.8(4) . 16_666 ?
C1 O1 Dy1 139.6(3) . . ?
C16 O4 Dy1 92.0(3) . 8_654 ?
O5 C16 Dy1 61.1(2) . 8_654 ?
O5 C16 O4 121.8(4) . . ?
O5 C16 C13 119.1(5) . . ?
O4 C16 Dy1 60.7(2) . 8_654 ?
O4 C16 C13 119.1(5) . . ?
C13 C16 Dy1 177.4(4) . 8_654 ?
C1AA O3A C9 112.2(9) . . ?
O7 C8 Dy1 72.3(3) . 3_565 ?
O7 C8 C6 118.8(4) . . ?
O6 C8 Dy1 49.8(2) . 3_565 ?
O6 C8 O7 121.9(4) . . ?
O6 C8 C6 119.3(4) . . ?
C6 C8 Dy1 167.7(4) . 3_565 ?
C6 C7 C2 119.5(4) . . ?
C7 C6 C8 118.8(4) . . ?
C7 C6 C5 121.7(5) . . ?
C5 C6 C8 119.6(4) . . ?
O2 C1 O1 126.0(5) . . ?
O2 C1 C2 117.6(4) . . ?
O1 C1 C2 116.3(4) . . ?
C12 C13 C16 120.6(6) . . ?
C12 C13 C14 119.1(6) . . ?
C14 C13 C16 120.3(6) . . ?
C7 C2 C1 119.9(4) . . ?
C3 C2 C7 119.7(5) . . ?
C3 C2 C1 120.4(4) . . ?
C2 C3 C1AA 120.4(5) . . ?
C11 C10 C9 118.8(8) . . ?
C15 C10 C11 119.4(6) . . ?
C15 C10 C9 121.7(8) . . ?
C3 C1AA O3A 116.5(7) . . ?
C3 C1AA C5 120.1(5) . . ?
C3 C1AA O3B 114.3(6) . . ?
C5 C1AA O3A 122.3(7) . . ?
C5 C1AA O3B 123.6(6) . . ?
C1AA C5 C6 118.7(5) . . ?
C13 C12 C11 119.7(8) . . ?
C13 C14 C15 120.3(8) . . ?
C10 C11 C12 120.3(8) . . ?
O3A C9 C10 107.0(7) . . ?
O3B C9 C10 104.8(6) . . ?
C10 C15 C14 121.2(8) . . ?
C1AA O3B C9 113.7(7) . . ?

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

data_mo_1210_1_0m_sq
_database_code_depnum_ccdc_archive 'CCDC 2071647'
loop_
_audit_author_name
_audit_author_address
'Yun-Shan Xue' 'Yancheng Teachers University'
_audit_update_record             
;
2021-03-19 deposited with the CCDC.	2021-04-20 downloaded from the CCDC.
;
_audit_creation_date             2020-07-30
_audit_creation_method           
;
Olex2 1.2-beta
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         '0.25(C176 H184 N16 O72 Pr8), C3 H7 N O'
_chemical_formula_sum            'C47 H53 N5 O19 Pr2'
_chemical_formula_weight         1273.76
_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'
Pr Pr -0.2180 2.8214 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 1 2/c 1'
_space_group_name_Hall           '-C 2yc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'

_cell_length_a                   28.5809(12)
_cell_length_b                   14.1925(6)
_cell_length_c                   14.1130(5)
_cell_angle_alpha                90
_cell_angle_beta                 99.9937(13)
_cell_angle_gamma                90
_cell_volume                     5637.9(4)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    9852
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      26.40
_cell_measurement_theta_min      2.26
_shelx_estimated_absorpt_T_max   0.802
_shelx_estimated_absorpt_T_min   0.665
_exptl_absorpt_coefficient_mu    1.780
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.6185
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0803 before and 0.0522 after correction.
The Ratio of minimum to maximum transmission is 0.8298.
The λ/2 correction factor is Not present.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            ?
_exptl_crystal_density_diffrn    1.501
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             2560
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.13
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0324
_diffrn_reflns_av_unetI/netI     0.0196
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       35
_diffrn_reflns_limit_h_min       -35
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            38021
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.418
_diffrn_reflns_theta_min         2.602
_diffrn_ambient_temperature      150.0
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                5398
_reflns_number_total             5762
_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       'SAINT v8.37A (Bruker, 2015)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    ?
_refine_diff_density_max         2.634
_refine_diff_density_min         -0.931
_refine_diff_density_rms         0.149
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.169
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     436
_refine_ls_number_reflns         5762
_refine_ls_number_restraints     375
_refine_ls_R_factor_all          0.0466
_refine_ls_R_factor_gt           0.0437
_refine_ls_restrained_S_all      1.160
_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)+(0.0133P)²+122.0564P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1029
_refine_ls_wR_factor_ref         0.1042
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 O10-C23 = O9-C20A = O9-C20B
 1.2 with sigma of 0.01
 N3-C23 = N2A-C20A = N2B-C20B
 1.3 with sigma of 0.01
 N3-C25 = N3-C24 = N2A-C22A = N2A-C21A
 1.49 with sigma of 0.01
 C20A-C22A
 2.4 with sigma of 0.01
 N2B-C22B = N2B-C21B = N1A-C18A = N1A-C19A
 1.49 with sigma of 0.01
 O8-C17A = O8-C17B
 1.2 with sigma of 0.01
 N1A-C17A = N1B-C17B
 1.3 with sigma of 0.01
 N1B-C19B = N1B-C18B
 1.49 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
O10 \\sim N3 \\sim C24: within 2A with sigma of 0.01 and sigma for terminal
atoms of 0.01
O10 \\sim N3 \\sim C23 \\sim C24 \\sim C25: within 2A with sigma of 0.01 and
sigma for terminal atoms of 0.01
O9 \\sim N2A \\sim C20A \\sim C21A \\sim C22A: within 2A with sigma of 0.01 and
sigma for terminal atoms of 0.01
N2A \\sim N2B \\sim C20A \\sim C20B \\sim C21A \\sim C21B \\sim C22A \\sim
C22B: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.01
N1A \\sim N1B \\sim C17A \\sim C17B \\sim C18A \\sim C18B \\sim C19A \\sim
C19B: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.01
Uanis(C3) \\sim Ueq, Uanis(C4) \\sim Ueq, Uanis(C8) \\sim Ueq, Uanis(C5) \\sim
Ueq, Uanis(N3) \\sim Ueq, Uanis(O10) \\sim Ueq, Uanis(C24) \\sim Ueq: with
sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C24) \\sim Ueq, Uanis(N3) \\sim Ueq, Uanis(C23) \\sim Ueq, Uanis(C25)
\\sim Ueq, Uanis(O10) \\sim Ueq: with sigma of 0.001 and sigma for terminal
atoms of 0.002
Uanis(C20A) \\sim Ueq, Uanis(N2A) \\sim Ueq, Uanis(C22A) \\sim Ueq, Uanis(C21A)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(N2B) \\sim Ueq, Uanis(C20B) \\sim Ueq, Uanis(C22B) \\sim Ueq, Uanis(C21B)
\\sim Ueq, Uanis(C18A) \\sim Ueq, Uanis(C19A) \\sim Ueq: with sigma of 0.01 and
sigma for terminal atoms of 0.02
Uanis(C17A) \\sim Ueq, Uanis(N1A) \\sim Ueq, Uanis(C17B) \\sim Ueq, Uanis(N1B)
\\sim Ueq, Uanis(C19B) \\sim Ueq, Uanis(C18B) \\sim Ueq: with sigma of 0.01 and
sigma for terminal atoms of 0.02
4. Others
 Sof(N2B)=Sof(C20B)=Sof(H20B)=Sof(C21B)=Sof(H21D)=Sof(H21E)=Sof(H21F)=
 Sof(C22B)=Sof(H22D)=Sof(H22E)=Sof(H22F)=1-FVAR(1)
 Sof(N2A)=Sof(C20A)=Sof(H20A)=Sof(C21A)=Sof(H21A)=Sof(H21B)=Sof(H21C)=
 Sof(C22A)=Sof(H22A)=Sof(H22B)=Sof(H22C)=FVAR(1)
 Sof(N1B)=Sof(C17B)=Sof(H17B)=Sof(C18B)=Sof(H18D)=Sof(H18E)=Sof(H18F)=
 Sof(C19B)=Sof(H19D)=Sof(H19E)=Sof(H19F)=1-FVAR(2)
 Sof(N1A)=Sof(C17A)=Sof(H17A)=Sof(C18A)=Sof(H18A)=Sof(H18B)=Sof(H18C)=
 Sof(C19A)=Sof(H19A)=Sof(H19B)=Sof(H19C)=FVAR(2)
 Fixed Sof: O10(0.5) N3(0.5) C23(0.5) H23(0.5) C24(0.5) H24A(0.5) H24B(0.5)
 H24C(0.5) C25(0.5) H25A(0.5) H25B(0.5) H25C(0.5)
5.a Secondary CH2 refined with riding coordinates:
 C8(H8A,H8B)
5.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C6(H6), C7(H7), C10(H10), C12(H12), C14(H14), C17A(H17A),
 C17B(H17B), C20A(H20A), C20B(H20B), C23(H23)
5.c Idealised Me refined as rotating group:
 C18A(H18A,H18B,H18C), C18B(H18D,H18E,H18F), C19A(H19A,H19B,H19C), C19B(H19D,
 H19E,H19F), C21A(H21A,H21B,H21C), C21B(H21D,H21E,H21F), C22A(H22A,H22B,H22C),
 C22B(H22D,H22E,H22F), C24(H24A,H24B,H24C), C25(H25A,H25B,H25C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_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
Pr1 Pr 0.31921(2) 0.28516(2) 0.54299(2) 0.00912(9) Uani 1 1 d . . . . .
O1 O 0.39730(14) 0.3141(3) 0.4983(3) 0.0279(10) Uani 1 1 d . . . . .
O2 O 0.38456(14) 0.1616(3) 0.5123(3) 0.0241(9) Uani 1 1 d . . . . .
O3 O 0.60202(13) 0.0821(3) 0.3536(3) 0.0213(8) Uani 1 1 d . . . . .
O4 O 0.69816(12) 0.2294(3) 0.1232(3) 0.0167(8) Uani 1 1 d . . . . .
O5 O 0.77087(13) 0.1667(3) 0.1635(3) 0.0223(9) Uani 1 1 d . . . . .
O6 O 0.79734(12) -0.0687(3) 0.4396(3) 0.0204(8) Uani 1 1 d . . . . .
O7 O 0.73380(12) -0.1499(2) 0.4591(2) 0.0140(7) Uani 1 1 d . . . . .
O8 O 0.35705(18) 0.2138(4) 0.6950(3) 0.0393(12) Uani 1 1 d D . . . .
O9 O 0.35835(18) 0.4194(4) 0.6431(4) 0.0446(13) Uani 1 1 d D U . . .
O10 O 0.3360(4) 0.7030(8) 0.4495(8) 0.051(2) Uani 0.5 1 d D U P A -1
N1A N 0.3741(3) 0.1229(8) 0.8268(6) 0.049(2) Uani 0.698(10) 1 d D U P B 1
N1B N 0.3803(9) 0.1731(18) 0.8455(14) 0.054(3) Uani 0.302(10) 1 d D U P B 2
N2A N 0.3855(4) 0.4881(6) 0.7939(6) 0.0413(19) Uani 0.624(8) 1 d D U P C 1
N2B N 0.3551(6) 0.5564(10) 0.7166(11) 0.046(3) Uani 0.376(8) 1 d D U P C 2
N3 N 0.2816(4) 0.6673(7) 0.5426(8) 0.036(2) Uani 0.5 1 d D U P A -1
C1 C 0.40947(18) 0.2284(4) 0.4913(4) 0.0192(11) Uani 1 1 d . . . . .
C2 C 0.45430(19) 0.2092(4) 0.4529(4) 0.0230(12) Uani 1 1 d . . . . .
C3 C 0.4801(2) 0.2841(5) 0.4255(6) 0.0403(17) Uani 1 1 d . U . . .
H3 H 0.470247 0.346722 0.435408 0.048 Uiso 1 1 calc R . . . .
C4 C 0.5199(3) 0.2690(5) 0.3840(6) 0.045(2) Uani 1 1 d . U . . .
H4 H 0.536584 0.321052 0.363840 0.054 Uiso 1 1 calc R . . . .
C5 C 0.5353(2) 0.1780(5) 0.3718(5) 0.0333(15) Uani 1 1 d . U . . .
C6 C 0.5102(2) 0.1029(5) 0.3992(5) 0.0314(15) Uani 1 1 d . . . . .
H6 H 0.520207 0.040247 0.389848 0.038 Uiso 1 1 calc R . . . .
C7 C 0.4699(2) 0.1188(4) 0.4408(5) 0.0257(13) Uani 1 1 d . . . . .
H7 H 0.453158 0.066832 0.461029 0.031 Uiso 1 1 calc R . . . .
C8 C 0.5776(2) 0.1671(5) 0.3216(5) 0.0340(16) Uani 1 1 d . U . . .
H8A H 0.566835 0.164843 0.251085 0.041 Uiso 1 1 calc R . . . .
H8B H 0.599222 0.221639 0.336609 0.041 Uiso 1 1 calc R . . . .
C9 C 0.64696(18) 0.0732(4) 0.3316(4) 0.0143(10) Uani 1 1 d . . . . .
C10 C 0.66422(18) 0.1282(4) 0.2635(4) 0.0149(10) Uani 1 1 d . . . . .
H10 H 0.644366 0.174080 0.227613 0.018 Uiso 1 1 calc R . . . .
C11 C 0.71081(17) 0.1157(4) 0.2481(4) 0.0135(10) Uani 1 1 d . . . . .
C12 C 0.74011(17) 0.0502(4) 0.3018(4) 0.0131(10) Uani 1 1 d . . . . .
H12 H 0.772382 0.044339 0.294351 0.016 Uiso 1 1 calc R . . . .
C13 C 0.72183(17) -0.0072(3) 0.3672(3) 0.0119(9) Uani 1 1 d . . . . .
C14 C 0.67532(17) 0.0036(4) 0.3824(3) 0.0130(9) Uani 1 1 d . . . . .
H14 H 0.663065 -0.035786 0.426681 0.016 Uiso 1 1 calc R . . . .
C15 C 0.72822(17) 0.1756(4) 0.1724(4) 0.0136(10) Uani 1 1 d . . . . .
C16 C 0.75298(17) -0.0795(4) 0.4247(3) 0.0130(10) Uani 1 1 d . . . . .
C17A C 0.3455(4) 0.1748(8) 0.7647(7) 0.045(2) Uani 0.698(10) 1 d D U P B 1
H17A H 0.313668 0.182535 0.774763 0.054 Uiso 0.698(10) 1 calc R . P B 1
C17B C 0.3572(9) 0.2276(18) 0.7791(7) 0.045(3) Uani 0.302(10) 1 d D U P B 2
H17B H 0.340030 0.279817 0.797656 0.053 Uiso 0.302(10) 1 calc R . P B 2
C18A C 0.4215(4) 0.1006(12) 0.8039(10) 0.054(3) Uani 0.698(10) 1 d D U P B 1
H18A H 0.423112 0.033414 0.788927 0.082 Uiso 0.698(10) 1 calc GR . P B 1
H18B H 0.446039 0.115893 0.859337 0.082 Uiso 0.698(10) 1 calc GR . P B 1
H18C H 0.426754 0.137904 0.748209 0.082 Uiso 0.698(10) 1 calc GR . P B 1
C18B C 0.4155(13) 0.099(2) 0.835(2) 0.056(4) Uani 0.302(10) 1 d D U P B 2
H18D H 0.420819 0.059023 0.892292 0.083 Uiso 0.302(10) 1 calc GR . P B 2
H18E H 0.445456 0.128118 0.826011 0.083 Uiso 0.302(10) 1 calc GR . P B 2
H18F H 0.403313 0.059883 0.778258 0.083 Uiso 0.302(10) 1 calc GR . P B 2
C19A C 0.3566(5) 0.0748(10) 0.9068(8) 0.059(3) Uani 0.698(10) 1 d D U P B 1
H19A H 0.322837 0.089180 0.903948 0.089 Uiso 0.698(10) 1 calc GR . P B 1
H19B H 0.374629 0.096724 0.968312 0.089 Uiso 0.698(10) 1 calc GR . P B 1
H19C H 0.360689 0.006559 0.901253 0.089 Uiso 0.698(10) 1 calc GR . P B 1
C19B C 0.3739(12) 0.196(2) 0.9455(16) 0.063(4) Uani 0.302(10) 1 d D U P B 2
H19D H 0.353458 0.251281 0.944687 0.094 Uiso 0.302(10) 1 calc GR . P B 2
H19E H 0.404894 0.208673 0.985098 0.094 Uiso 0.302(10) 1 calc GR . P B 2
H19F H 0.359055 0.142056 0.972513 0.094 Uiso 0.302(10) 1 calc GR . P B 2
C20A C 0.3717(4) 0.4193(7) 0.7324(6) 0.036(2) Uani 0.624(8) 1 d D U P C 1
H20A H 0.372051 0.358757 0.761131 0.043 Uiso 0.624(8) 1 calc R . P C 1
C20B C 0.3700(7) 0.4731(11) 0.7049(12) 0.048(3) Uani 0.376(8) 1 d D U P C 2
H20B H 0.394474 0.451605 0.754504 0.058 Uiso 0.376(8) 1 calc R . P C 2
C21A C 0.4029(4) 0.4745(8) 0.8981(7) 0.043(3) Uani 0.624(8) 1 d D U P C 1
H21A H 0.437539 0.467582 0.909690 0.065 Uiso 0.624(8) 1 calc GR . P C 1
H21B H 0.388481 0.417611 0.920014 0.065 Uiso 0.624(8) 1 calc GR . P C 1
H21C H 0.394174 0.529204 0.933665 0.065 Uiso 0.624(8) 1 calc GR . P C 1
C21B C 0.3811(8) 0.6010(17) 0.8061(14) 0.051(3) Uani 0.376(8) 1 d D U P C 2
H21D H 0.389583 0.552701 0.855697 0.076 Uiso 0.376(8) 1 calc GR . P C 2
H21E H 0.360685 0.648392 0.828919 0.076 Uiso 0.376(8) 1 calc GR . P C 2
H21F H 0.410000 0.631300 0.792498 0.076 Uiso 0.376(8) 1 calc GR . P C 2
C22A C 0.3859(5) 0.5847(6) 0.7570(10) 0.052(3) Uani 0.624(8) 1 d D U P C 1
H22A H 0.365559 0.624626 0.789529 0.078 Uiso 0.624(8) 1 calc GR . P C 1
H22B H 0.373872 0.584854 0.687647 0.078 Uiso 0.624(8) 1 calc GR . P C 1
H22C H 0.418424 0.609187 0.769367 0.078 Uiso 0.624(8) 1 calc GR . P C 1
C22B C 0.3175(8) 0.6203(17) 0.668(2) 0.073(5) Uani 0.376(8) 1 d D U P C 2
H22D H 0.331733 0.668673 0.632813 0.110 Uiso 0.376(8) 1 calc GR . P C 2
H22E H 0.301753 0.650444 0.716866 0.110 Uiso 0.376(8) 1 calc GR . P C 2
H22F H 0.294186 0.584100 0.623768 0.110 Uiso 0.376(8) 1 calc GR . P C 2
C23 C 0.3195(4) 0.6518(9) 0.5039(9) 0.036(2) Uani 0.5 1 d D U P A -1
H23 H 0.335794 0.594191 0.520513 0.043 Uiso 0.5 1 calc R . P A -1
C24 C 0.2640(6) 0.5977(10) 0.6069(10) 0.044(3) Uani 0.5 1 d D U P A -1
H24A H 0.265421 0.625305 0.670941 0.066 Uiso 0.5 1 calc GR . P A -1
H24B H 0.283894 0.541079 0.611658 0.066 Uiso 0.5 1 calc GR . P A -1
H24C H 0.231071 0.580821 0.580359 0.066 Uiso 0.5 1 calc GR . P A -1
C25 C 0.2517(7) 0.7529(11) 0.5201(11) 0.046(3) Uani 0.5 1 d D U P A -1
H25A H 0.222476 0.736231 0.476079 0.069 Uiso 0.5 1 calc GR . P A -1
H25B H 0.269325 0.800053 0.489615 0.069 Uiso 0.5 1 calc GR . P A -1
H25C H 0.243758 0.778755 0.579621 0.069 Uiso 0.5 1 calc GR . P A -1


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Pr1 Pr1 4.0566(5) 7_556 ?
Pr1 O1 2.457(4) . ?
Pr1 O2 2.652(4) . ?
Pr1 O4 2.444(3) 2_655 ?
Pr1 O5 2.466(3) 8_456 ?
Pr1 O6 2.550(4) 3_455 ?
Pr1 O7 2.442(3) 5_656 ?
Pr1 O7 2.684(3) 3_455 ?
Pr1 O8 2.447(4) . ?
Pr1 O9 2.516(5) . ?
Pr1 C1 2.913(5) . ?
Pr1 C16 2.994(5) 3_455 ?
O1 C1 1.273(7) . ?
O2 C1 1.252(7) . ?
O3 C8 1.427(7) . ?
O3 C9 1.379(6) . ?
O4 C15 1.263(6) . ?
O5 C15 1.253(6) . ?
O6 C16 1.258(6) . ?
O7 C16 1.276(6) . ?
O8 C17A 1.225(8) . ?
O8 C17B 1.203(10) . ?
O9 C20A 1.252(8) . ?
O9 C20B 1.162(9) . ?
O10 C23 1.211(9) . ?
N1A C17A 1.316(8) . ?
N1A C18A 1.480(9) . ?
N1A C19A 1.480(9) . ?
N1B C17B 1.304(10) . ?
N1B C18B 1.484(10) . ?
N1B C19B 1.489(10) . ?
N2A C20A 1.320(8) . ?
N2A C21A 1.482(9) . ?
N2A C22A 1.467(8) . ?
N2B C20B 1.277(10) . ?
N2B C21B 1.491(10) . ?
N2B C22B 1.478(10) . ?
N3 C23 1.314(9) . ?
N3 C24 1.486(9) . ?
N3 C25 1.486(10) . ?
C1 C2 1.500(7) . ?
C2 C3 1.385(9) . ?
C2 C7 1.379(8) . ?
C3 H3 0.9500 . ?
C3 C4 1.384(8) . ?
C4 H4 0.9500 . ?
C4 C5 1.385(9) . ?
C5 C6 1.379(9) . ?
C5 C8 1.511(7) . ?
C6 H6 0.9500 . ?
C6 C7 1.398(7) . ?
C7 H7 0.9500 . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C9 C10 1.393(7) . ?
C9 C14 1.395(7) . ?
C10 H10 0.9500 . ?
C10 C11 1.397(7) . ?
C11 C12 1.386(7) . ?
C11 C15 1.515(7) . ?
C12 H12 0.9500 . ?
C12 C13 1.398(7) . ?
C13 C14 1.391(7) . ?
C13 C16 1.501(7) . ?
C14 H14 0.9500 . ?
C17A H17A 0.9500 . ?
C17B H17B 0.9500 . ?
C18A H18A 0.9800 . ?
C18A H18B 0.9800 . ?
C18A H18C 0.9800 . ?
C18B H18D 0.9800 . ?
C18B H18E 0.9800 . ?
C18B H18F 0.9800 . ?
C19A H19A 0.9800 . ?
C19A H19B 0.9800 . ?
C19A H19C 0.9800 . ?
C19B H19D 0.9800 . ?
C19B H19E 0.9800 . ?
C19B H19F 0.9800 . ?
C20A H20A 0.9500 . ?
C20B H20B 0.9500 . ?
C21A H21A 0.9800 . ?
C21A H21B 0.9800 . ?
C21A H21C 0.9800 . ?
C21B H21D 0.9800 . ?
C21B H21E 0.9800 . ?
C21B H21F 0.9800 . ?
C22A H22A 0.9800 . ?
C22A H22B 0.9800 . ?
C22A H22C 0.9800 . ?
C22B H22D 0.9800 . ?
C22B H22E 0.9800 . ?
C22B H22F 0.9800 . ?
C23 H23 0.9500 . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?
C25 H25A 0.9800 . ?
C25 H25B 0.9800 . ?
C25 H25C 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Pr1 Pr1 147.85(11) . 7_556 ?
O1 Pr1 O2 51.09(12) . . ?
O1 Pr1 O5 140.62(14) . 8_456 ?
O1 Pr1 O6 81.98(13) . 3_455 ?
O1 Pr1 O7 128.78(13) . 3_455 ?
O1 Pr1 O9 71.48(15) . . ?
O1 Pr1 C1 25.67(15) . . ?
O1 Pr1 C16 105.32(14) . 3_455 ?
O2 Pr1 Pr1 117.80(9) . 7_556 ?
O2 Pr1 O7 140.11(12) . 3_455 ?
O2 Pr1 C1 25.46(14) . . ?
O2 Pr1 C16 136.75(13) . 3_455 ?
O4 Pr1 Pr1 66.92(8) 2_655 7_556 ?
O4 Pr1 O1 81.38(14) 2_655 . ?
O4 Pr1 O2 70.14(13) 2_655 . ?
O4 Pr1 O5 134.98(12) 2_655 8_456 ?
O4 Pr1 O6 74.08(13) 2_655 3_455 ?
O4 Pr1 O7 70.74(11) 2_655 3_455 ?
O4 Pr1 O8 133.82(15) 2_655 . ?
O4 Pr1 O9 141.36(14) 2_655 . ?
O4 Pr1 C1 73.22(14) 2_655 . ?
O4 Pr1 C16 70.69(13) 2_655 3_455 ?
O5 Pr1 Pr1 68.93(9) 8_456 7_556 ?
O5 Pr1 O2 142.24(13) 8_456 . ?
O5 Pr1 O6 93.32(14) 8_456 3_455 ?
O5 Pr1 O7 68.51(12) 8_456 3_455 ?
O5 Pr1 O9 69.53(14) 8_456 . ?
O5 Pr1 C1 151.10(14) 8_456 . ?
O5 Pr1 C16 80.26(13) 8_456 3_455 ?
O6 Pr1 Pr1 84.22(8) 3_455 7_556 ?
O6 Pr1 O2 123.65(12) 3_455 . ?
O6 Pr1 O7 49.81(11) 3_455 3_455 ?
O6 Pr1 C1 102.78(14) 3_455 . ?
O6 Pr1 C16 24.60(12) 3_455 3_455 ?
O7 Pr1 Pr1 39.84(8) 5_656 7_556 ?
O7 Pr1 Pr1 35.66(7) 3_455 7_556 ?
O7 Pr1 O1 135.87(12) 5_656 . ?
O7 Pr1 O2 86.06(12) 5_656 . ?
O7 Pr1 O4 73.23(12) 5_656 2_655 ?
O7 Pr1 O5 78.80(12) 5_656 8_456 ?
O7 Pr1 O6 122.83(12) 5_656 3_455 ?
O7 Pr1 O7 75.50(12) 5_656 3_455 ?
O7 Pr1 O8 82.21(15) 5_656 . ?
O7 Pr1 O9 144.72(13) 5_656 . ?
O7 Pr1 C1 139.58(13) 3_455 . ?
O7 Pr1 C1 110.75(14) 5_656 . ?
O7 Pr1 C16 99.59(13) 5_656 3_455 ?
O7 Pr1 C16 25.22(12) 3_455 3_455 ?
O8 Pr1 Pr1 114.84(13) . 7_556 ?
O8 Pr1 O1 90.64(16) . . ?
O8 Pr1 O2 69.69(14) . . ?
O8 Pr1 O5 74.08(15) . 8_456 ?
O8 Pr1 O6 149.87(16) . 3_455 ?
O8 Pr1 O7 139.30(14) . 3_455 ?
O8 Pr1 O9 74.65(18) . . ?
O8 Pr1 C1 80.17(15) . . ?
O8 Pr1 C16 153.45(14) . 3_455 ?
O9 Pr1 Pr1 132.05(12) . 7_556 ?
O9 Pr1 O2 109.61(16) . . ?
O9 Pr1 O6 75.31(16) . 3_455 ?
O9 Pr1 O7 105.63(16) . 3_455 ?
O9 Pr1 C1 91.33(16) . . ?
O9 Pr1 C16 90.21(17) . 3_455 ?
C1 Pr1 Pr1 135.82(11) . 7_556 ?
C1 Pr1 C16 122.64(14) . 3_455 ?
C16 Pr1 Pr1 60.10(10) 3_455 7_556 ?
C1 O1 Pr1 97.6(3) . . ?
C1 O2 Pr1 89.0(3) . . ?
C9 O3 C8 115.4(4) . . ?
C15 O4 Pr1 136.8(3) . 2_655 ?
C15 O5 Pr1 135.4(3) . 8 ?
C16 O6 Pr1 97.9(3) . 3_545 ?
Pr1 O7 Pr1 104.50(12) 5_656 3_545 ?
C16 O7 Pr1 156.6(3) . 5_656 ?
C16 O7 Pr1 91.1(3) . 3_545 ?
C17A O8 Pr1 138.8(6) . . ?
C17B O8 Pr1 136.3(11) . . ?
C20A O9 Pr1 126.4(5) . . ?
C20B O9 Pr1 163.6(11) . . ?
C17A N1A C18A 117.5(9) . . ?
C17A N1A C19A 120.8(9) . . ?
C19A N1A C18A 120.8(10) . . ?
C17B N1B C18B 128(2) . . ?
C17B N1B C19B 115.1(19) . . ?
C18B N1B C19B 117(2) . . ?
C20A N2A C21A 124.5(8) . . ?
C20A N2A C22A 118.5(8) . . ?
C22A N2A C21A 116.9(9) . . ?
C20B N2B C21B 112.0(15) . . ?
C20B N2B C22B 137.8(19) . . ?
C22B N2B C21B 110.1(18) . . ?
C23 N3 C24 122.2(11) . . ?
C23 N3 C25 122.1(12) . . ?
C24 N3 C25 115.5(12) . . ?
O1 C1 Pr1 56.7(3) . . ?
O1 C1 C2 117.6(5) . . ?
O2 C1 Pr1 65.5(3) . . ?
O2 C1 O1 122.1(5) . . ?
O2 C1 C2 120.2(5) . . ?
C2 C1 Pr1 171.7(4) . . ?
C3 C2 C1 119.3(5) . . ?
C7 C2 C1 122.0(5) . . ?
C7 C2 C3 118.7(5) . . ?
C2 C3 H3 119.5 . . ?
C4 C3 C2 121.0(6) . . ?
C4 C3 H3 119.5 . . ?
C3 C4 H4 120.0 . . ?
C3 C4 C5 120.0(6) . . ?
C5 C4 H4 120.0 . . ?
C4 C5 C8 116.9(6) . . ?
C6 C5 C4 119.6(5) . . ?
C6 C5 C8 123.4(6) . . ?
C5 C6 H6 120.0 . . ?
C5 C6 C7 120.0(6) . . ?
C7 C6 H6 120.0 . . ?
C2 C7 C6 120.7(5) . . ?
C2 C7 H7 119.6 . . ?
C6 C7 H7 119.6 . . ?
O3 C8 C5 109.0(5) . . ?
O3 C8 H8A 109.9 . . ?
O3 C8 H8B 109.9 . . ?
C5 C8 H8A 109.9 . . ?
C5 C8 H8B 109.9 . . ?
H8A C8 H8B 108.3 . . ?
O3 C9 C10 124.0(4) . . ?
O3 C9 C14 115.4(4) . . ?
C10 C9 C14 120.5(4) . . ?
C9 C10 H10 120.1 . . ?
C9 C10 C11 119.8(5) . . ?
C11 C10 H10 120.1 . . ?
C10 C11 C15 118.5(4) . . ?
C12 C11 C10 120.1(4) . . ?
C12 C11 C15 121.4(4) . . ?
C11 C12 H12 120.2 . . ?
C11 C12 C13 119.5(4) . . ?
C13 C12 H12 120.2 . . ?
C12 C13 C16 120.0(4) . . ?
C14 C13 C12 120.9(4) . . ?
C14 C13 C16 119.0(4) . . ?
C9 C14 H14 120.5 . . ?
C13 C14 C9 119.0(4) . . ?
C13 C14 H14 120.5 . . ?
O4 C15 C11 116.8(4) . . ?
O5 C15 O4 125.9(5) . . ?
O5 C15 C11 117.3(4) . . ?
O6 C16 Pr1 57.5(3) . 3_545 ?
O6 C16 O7 121.3(4) . . ?
O6 C16 C13 119.6(4) . . ?
O7 C16 Pr1 63.7(3) . 3_545 ?
O7 C16 C13 119.2(4) . . ?
C13 C16 Pr1 176.7(4) . 3_545 ?
O8 C17A N1A 124.4(9) . . ?
O8 C17A H17A 117.8 . . ?
N1A C17A H17A 117.8 . . ?
O8 C17B N1B 121.9(18) . . ?
O8 C17B H17B 119.1 . . ?
N1B C17B H17B 119.1 . . ?
N1A C18A H18A 109.5 . . ?
N1A C18A H18B 109.5 . . ?
N1A C18A H18C 109.5 . . ?
H18A C18A H18B 109.5 . . ?
H18A C18A H18C 109.5 . . ?
H18B C18A H18C 109.5 . . ?
N1B C18B H18D 109.5 . . ?
N1B C18B H18E 109.5 . . ?
N1B C18B H18F 109.5 . . ?
H18D C18B H18E 109.5 . . ?
H18D C18B H18F 109.5 . . ?
H18E C18B H18F 109.5 . . ?
N1A C19A H19A 109.5 . . ?
N1A C19A H19B 109.5 . . ?
N1A C19A H19C 109.5 . . ?
H19A C19A H19B 109.5 . . ?
H19A C19A H19C 109.5 . . ?
H19B C19A H19C 109.5 . . ?
N1B C19B H19D 109.5 . . ?
N1B C19B H19E 109.5 . . ?
N1B C19B H19F 109.5 . . ?
H19D C19B H19E 109.5 . . ?
H19D C19B H19F 109.5 . . ?
H19E C19B H19F 109.5 . . ?
O9 C20A N2A 131.7(9) . . ?
O9 C20A H20A 114.1 . . ?
N2A C20A H20A 114.1 . . ?
O9 C20B N2B 130.2(18) . . ?
O9 C20B H20B 114.9 . . ?
N2B C20B H20B 114.9 . . ?
N2A C21A H21A 109.5 . . ?
N2A C21A H21B 109.5 . . ?
N2A C21A H21C 109.5 . . ?
H21A C21A H21B 109.5 . . ?
H21A C21A H21C 109.5 . . ?
H21B C21A H21C 109.5 . . ?
N2B C21B H21D 109.5 . . ?
N2B C21B H21E 109.5 . . ?
N2B C21B H21F 109.5 . . ?
H21D C21B H21E 109.5 . . ?
H21D C21B H21F 109.5 . . ?
H21E C21B H21F 109.5 . . ?
N2A C22A H22A 109.5 . . ?
N2A C22A H22B 109.5 . . ?
N2A C22A H22C 109.5 . . ?
H22A C22A H22B 109.5 . . ?
H22A C22A H22C 109.5 . . ?
H22B C22A H22C 109.5 . . ?
N2B C22B H22D 109.5 . . ?
N2B C22B H22E 109.5 . . ?
N2B C22B H22F 109.5 . . ?
H22D C22B H22E 109.5 . . ?
H22D C22B H22F 109.5 . . ?
H22E C22B H22F 109.5 . . ?
O10 C23 N3 127.1(13) . . ?
O10 C23 H23 116.4 . . ?
N3 C23 H23 116.4 . . ?
N3 C24 H24A 109.5 . . ?
N3 C24 H24B 109.5 . . ?
N3 C24 H24C 109.5 . . ?
H24A C24 H24B 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
N3 C25 H25A 109.5 . . ?
N3 C25 H25B 109.5 . . ?
N3 C25 H25C 109.5 . . ?
H25A C25 H25B 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Pr1 O1 C1 O2 -4.7(6) . . . . ?
Pr1 O1 C1 C2 173.0(4) . . . . ?
Pr1 O2 C1 O1 4.3(6) . . . . ?
Pr1 O2 C1 C2 -173.3(5) . . . . ?
Pr1 O4 C15 O5 35.4(9) 2_655 . . . ?
Pr1 O4 C15 C11 -143.7(4) 2_655 . . . ?
Pr1 O5 C15 O4 -12.5(9) 8 . . . ?
Pr1 O5 C15 C11 166.6(4) 8 . . . ?
Pr1 O6 C16 O7 -0.6(5) 3_545 . . . ?
Pr1 O6 C16 C13 178.1(4) 3_545 . . . ?
Pr1 O7 C16 Pr1 -132.4(8) 5_656 . . 3_545 ?
Pr1 O7 C16 O6 -131.9(7) 5_656 . . . ?
Pr1 O7 C16 O6 0.5(5) 3_545 . . . ?
Pr1 O7 C16 C13 49.5(10) 5_656 . . . ?
Pr1 O7 C16 C13 -178.2(4) 3_545 . . . ?
Pr1 O8 C17A N1A 162.7(8) . . . . ?
Pr1 O8 C17B N1B 177.0(17) . . . . ?
Pr1 O9 C20A N2A -167.8(9) . . . . ?
Pr1 O9 C20B N2B -98(4) . . . . ?
O1 C1 C2 C3 -1.0(9) . . . . ?
O1 C1 C2 C7 -178.7(6) . . . . ?
O2 C1 C2 C3 176.7(6) . . . . ?
O2 C1 C2 C7 -1.0(9) . . . . ?
O3 C9 C10 C11 178.2(5) . . . . ?
O3 C9 C14 C13 -177.3(5) . . . . ?
C1 C2 C3 C4 -175.8(7) . . . . ?
C1 C2 C7 C6 175.9(6) . . . . ?
C2 C3 C4 C5 -1.9(13) . . . . ?
C3 C2 C7 C6 -1.8(10) . . . . ?
C3 C4 C5 C6 1.5(13) . . . . ?
C3 C4 C5 C8 177.2(8) . . . . ?
C4 C5 C6 C7 -1.3(11) . . . . ?
C4 C5 C8 O3 152.8(7) . . . . ?
C5 C6 C7 C2 1.5(11) . . . . ?
C6 C5 C8 O3 -31.6(10) . . . . ?
C7 C2 C3 C4 2.0(12) . . . . ?
C8 O3 C9 C10 -15.8(8) . . . . ?
C8 O3 C9 C14 164.4(5) . . . . ?
C8 C5 C6 C7 -176.7(7) . . . . ?
C9 O3 C8 C5 -165.7(5) . . . . ?
C9 C10 C11 C12 -1.4(8) . . . . ?
C9 C10 C11 C15 179.1(5) . . . . ?
C10 C9 C14 C13 2.9(8) . . . . ?
C10 C11 C12 C13 4.0(8) . . . . ?
C10 C11 C15 O4 -4.5(7) . . . . ?
C10 C11 C15 O5 176.3(5) . . . . ?
C11 C12 C13 C14 -3.1(8) . . . . ?
C11 C12 C13 C16 179.0(5) . . . . ?
C12 C11 C15 O4 176.0(5) . . . . ?
C12 C11 C15 O5 -3.2(8) . . . . ?
C12 C13 C14 C9 -0.3(8) . . . . ?
C12 C13 C16 O6 23.9(7) . . . . ?
C12 C13 C16 O7 -157.4(5) . . . . ?
C14 C9 C10 C11 -2.0(8) . . . . ?
C14 C13 C16 O6 -154.0(5) . . . . ?
C14 C13 C16 O7 24.7(7) . . . . ?
C15 C11 C12 C13 -176.6(5) . . . . ?
C16 C13 C14 C9 177.6(5) . . . . ?
C18A N1A C17A O8 -8(2) . . . . ?
C18B N1B C17B O8 11(5) . . . . ?
C19A N1A C17A O8 -177.3(12) . . . . ?
C19B N1B C17B O8 -176(3) . . . . ?
C21A N2A C20A O9 -176.5(11) . . . . ?
C21B N2B C20B O9 -179(2) . . . . ?
C22A N2A C20A O9 0.6(19) . . . . ?
C22B N2B C20B O9 5(5) . . . . ?
C24 N3 C23 O10 178.5(14) . . . . ?
C25 N3 C23 O10 2(2) . . . . ?

_platon_squeeze_details          ?
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.500 0.605 0.250 130 44 ' '
2 1.000 0.105 0.250 130 44 ' '
3 0.500 0.395 0.750 130 44 ' '
4 1.000 0.895 0.750 130 44 ' '

_platon_squeeze_void_probe_radius 1.20
_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_222_sq_CCDC1
_database_code_depnum_ccdc_archive 'CCDC 2071648'
loop_
_audit_author_name
_audit_author_address
'Yun-Shan Xue' 'Yancheng Teachers University'
_audit_update_record             
;
2021-03-19 deposited with the CCDC.	2021-04-20 downloaded from the CCDC.
;
_audit_creation_date             2020-07-30
_audit_creation_method           
;
Olex2 1.2-beta
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         '0.25(C176 H184 N16 O72 Sm8), C3 H7 N O'
_chemical_formula_sum            'C47 H53 N5 O19 Sm2'
_chemical_formula_weight         1292.64
_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      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 1 2/c 1'
_space_group_name_Hall           '-C 2yc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'

_cell_length_a                   28.531(2)
_cell_length_b                   14.3021(9)
_cell_length_c                   13.7731(9)
_cell_angle_alpha                90
_cell_angle_beta                 100.718(2)
_cell_angle_gamma                90
_cell_volume                     5522.1(6)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    9951
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      26.47
_cell_measurement_theta_min      2.29
_shelx_estimated_absorpt_T_max   0.796
_shelx_estimated_absorpt_T_min   0.561
_exptl_absorpt_coefficient_mu    2.180
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.5151
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0987 before and 0.0615 after correction.
The Ratio of minimum to maximum transmission is 0.6910.
The λ/2 correction factor is Not present.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            yellowish
_exptl_crystal_density_diffrn    1.555
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             2584
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.11
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0503
_diffrn_reflns_av_unetI/netI     0.0432
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_h_min       -33
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            19960
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        25.048
_diffrn_reflns_theta_max         25.048
_diffrn_reflns_theta_min         2.604
_diffrn_ambient_temperature      149.99
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3976
_reflns_number_total             4849
_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       'SAINT v8.37A (Bruker, 2015)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    ?
_refine_diff_density_max         2.352
_refine_diff_density_min         -0.835
_refine_diff_density_rms         0.149
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     397
_refine_ls_number_reflns         4849
_refine_ls_number_restraints     182
_refine_ls_R_factor_all          0.0566
_refine_ls_R_factor_gt           0.0428
_refine_ls_restrained_S_all      1.051
_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)+(0.0546P)²+53.2209P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1071
_refine_ls_wR_factor_ref         0.1125
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 O9-C23 = O9-C20
 1.2 with sigma of 0.01
 N2-C20 = N3-C23
 1.3 with sigma of 0.01
 N2-C21 = N2-C22 = N3-C25 = N3-C24
 1.49 with sigma of 0.01
 C23-C25
 2.5 with sigma of 0.01
 C25-C24
 2.5 with sigma of 0.01
 N4-C28 = N4-C27
 1.49 with sigma of 0.01
 N4-C26
 1.3 with sigma of 0.01
 H19A_$1-H28B
 2.2 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
C23 \\sim N3 \\sim C25 \\sim C22 \\sim N2 \\sim C20 \\sim C21 \\sim C24: within
2A with sigma of 0.01 and sigma for terminal atoms of 0.01
Uanis(N1) \\sim Ueq, Uanis(C11) \\sim Ueq, Uanis(C17) \\sim Ueq, Uanis(C18)
\\sim Ueq, Uanis(C19) \\sim Ueq, Uanis(C22) \\sim Ueq, Uanis(C23) \\sim Ueq,
Uanis(C25) \\sim Ueq, Uanis(C24) \\sim Ueq, Uanis(N4) \\sim Ueq, Uanis(C26)
\\sim Ueq, Uanis(C27) \\sim Ueq, Uanis(C28) \\sim Ueq: with sigma of 0.01 and
sigma for terminal atoms of 0.02
4. Others
 Sof(N3)=Sof(C23)=Sof(H23)=Sof(C25)=Sof(H25A)=Sof(H25B)=Sof(H25C)=Sof(C24)=
 Sof(H24A)=Sof(H24B)=Sof(H24C)=1-FVAR(1)
 Sof(N2)=Sof(C20)=Sof(H20)=Sof(C21)=Sof(H21A)=Sof(H21B)=Sof(H21C)=Sof(C22)=
 Sof(H22A)=Sof(H22B)=Sof(H22C)=FVAR(1)
 Fixed Sof: O10(0.5) N4(0.5) C26(0.5) H26(0.5) C28(0.5) H28A(0.5) H28B(0.5)
 H28C(0.5) C27(0.5) H27A(0.5) H27B(0.5) H27C(0.5)
5.a Secondary CH2 refined with riding coordinates:
 C9(H9A,H9B)
5.b Aromatic/amide H refined with riding coordinates:
 C15(H15), C14(H14), C2(H2), C4(H4), C6(H6), C11(H11), C12(H12), C20(H20),
 C17(H17), C26(H26), C23(H23)
5.c Idealised Me refined as rotating group:
 C21(H21A,H21B,H21C), C22(H22A,H22B,H22C), C19(H19A,H19B,H19C), C18(H18A,H18B,
 H18C), C28(H28A,H28B,H28C), C27(H27A,H27B,H27C), C25(H25A,H25B,H25C), C24(H24A,
 H24B,H24C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_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
Sm4 Sm 0.31848(2) 0.21437(2) 0.54319(2) 0.01595(12) Uani 1 1 d . . . . .
O2 O 0.30056(14) 0.2664(3) 0.3745(3) 0.0214(9) Uani 1 1 d . . . . .
O7 O 0.60484(16) 0.1867(3) 0.0028(4) 0.0356(12) Uani 1 1 d . . . . .
O1 O 0.22814(14) 0.3323(3) 0.3339(3) 0.0306(11) Uani 1 1 d . . . . .
O3 O 0.20387(14) 0.5708(3) 0.0552(3) 0.0280(10) Uani 1 1 d . . . . .
O5 O 0.39869(14) 0.4144(3) 0.1458(3) 0.0265(10) Uani 1 1 d . . . . .
O8 O 0.3581(2) 0.2837(3) 0.6956(3) 0.0435(13) Uani 1 1 d . . . . .
O4 O 0.26792(14) 0.6519(3) 0.0417(3) 0.0223(9) Uani 1 1 d . . . . .
O9 O 0.35765(18) 0.0826(4) 0.6462(4) 0.0445(13) Uani 1 1 d D . . . .
O6 O 0.61747(15) 0.3374(3) -0.0121(3) 0.0304(10) Uani 1 1 d . . . . .
C15 C 0.4799(2) 0.2282(5) 0.1103(6) 0.0397(18) Uani 1 1 d . . . . .
H15 H 0.462451 0.176225 0.127744 0.048 Uiso 1 1 calc R . . . .
C14 C 0.5209(2) 0.2134(5) 0.0709(6) 0.0381(18) Uani 1 1 d . . . . .
H14 H 0.531185 0.151411 0.061403 0.046 Uiso 1 1 calc R . . . .
C3 C 0.27880(19) 0.5076(4) 0.1306(4) 0.0182(12) Uani 1 1 d . . . . .
C1 C 0.2889(2) 0.3815(4) 0.2492(4) 0.0189(12) Uani 1 1 d . . . . .
C7 C 0.2712(2) 0.3214(4) 0.3255(4) 0.0204(13) Uani 1 1 d . . . . .
C2 C 0.26012(19) 0.4498(4) 0.1958(4) 0.0180(12) Uani 1 1 d . . . . .
H2 H 0.227950 0.457052 0.203710 0.022 Uiso 1 1 calc R . . . .
C4 C 0.3258(2) 0.4960(4) 0.1173(4) 0.0200(12) Uani 1 1 d . . . . .
H4 H 0.338873 0.536593 0.074587 0.024 Uiso 1 1 calc R . . . .
C9 C 0.4217(2) 0.3284(5) 0.1734(5) 0.0328(16) Uani 1 1 d . . . . .
H9A H 0.399257 0.276140 0.153213 0.039 Uiso 1 1 calc R . . . .
H9B H 0.432021 0.325981 0.246061 0.039 Uiso 1 1 calc R . . . .
C6 C 0.33544(19) 0.3686(4) 0.2345(4) 0.0193(12) Uani 1 1 d . . . . .
H6 H 0.355038 0.321725 0.270331 0.023 Uiso 1 1 calc R . . . .
C5 C 0.35309(19) 0.4247(4) 0.1670(4) 0.0202(12) Uani 1 1 d . . . . .
C13 C 0.5469(2) 0.2892(4) 0.0454(4) 0.0214(13) Uani 1 1 d . . . . .
N2 N 0.3847(7) 0.0148(6) 0.8018(8) 0.063(2) Uani 0.771(8) 1 d D U P A 1
C16 C 0.5928(2) 0.2709(4) 0.0095(4) 0.0216(13) Uani 1 1 d . . . . .
C8 C 0.2482(2) 0.5811(4) 0.0726(4) 0.0219(13) Uani 1 1 d . . . . .
C10 C 0.4645(2) 0.3183(5) 0.1243(5) 0.0288(14) Uani 1 1 d . . . . .
C11 C 0.4900(2) 0.3936(5) 0.0980(5) 0.0362(17) Uani 1 1 d . U . . .
H11 H 0.479797 0.455649 0.107431 0.043 Uiso 1 1 calc R . . . .
N1 N 0.3790(3) 0.3803(6) 0.8278(6) 0.066(2) Uani 1 1 d . U . . .
C12 C 0.5308(2) 0.3780(5) 0.0575(5) 0.0353(17) Uani 1 1 d . . . . .
H12 H 0.547684 0.429840 0.038042 0.042 Uiso 1 1 calc R . . . .
C20 C 0.3695(4) 0.0807(7) 0.7374(6) 0.055(2) Uani 0.771(8) 1 d D U P A 1
H20 H 0.367054 0.139998 0.767228 0.066 Uiso 0.771(8) 1 calc R . P A 1
C17 C 0.3495(4) 0.3236(8) 0.7641(7) 0.071(3) Uani 1 1 d . U . . .
H17 H 0.318182 0.315687 0.777110 0.085 Uiso 1 1 calc R . . . .
C21 C 0.4014(4) 0.0253(8) 0.9101(7) 0.065(3) Uani 0.771(8) 1 d D U P A 1
H21A H 0.436019 0.016484 0.926112 0.097 Uiso 0.771(8) 1 calc GR . P A 1
H21B H 0.385760 -0.021672 0.945044 0.097 Uiso 0.771(8) 1 calc GR . P A 1
H21C H 0.393328 0.087974 0.930638 0.097 Uiso 0.771(8) 1 calc GR . P A 1
C22 C 0.3851(5) -0.0835(7) 0.7644(10) 0.075(3) Uani 0.771(8) 1 d D U P A 1
H22A H 0.369860 -0.085415 0.694493 0.112 Uiso 0.771(8) 1 calc GR . P A 1
H22B H 0.367652 -0.124083 0.802584 0.112 Uiso 0.771(8) 1 calc GR . P A 1
H22C H 0.418156 -0.105316 0.771500 0.112 Uiso 0.771(8) 1 calc GR . P A 1
C19 C 0.3622(5) 0.4289(9) 0.9050(8) 0.098(4) Uani 1 1 d . U . . .
H19A H 0.328013 0.416621 0.900397 0.146 Uiso 1 1 calc DGR . . . .
H19B H 0.367292 0.496147 0.898501 0.146 Uiso 1 1 calc GR . . . .
H19C H 0.379581 0.407193 0.969135 0.146 Uiso 1 1 calc GR . . . .
C18 C 0.4259(4) 0.3990(9) 0.8095(9) 0.096(4) Uani 1 1 d . U . . .
H18A H 0.449459 0.366131 0.858539 0.144 Uiso 1 1 calc GR . . . .
H18B H 0.432041 0.466394 0.814354 0.144 Uiso 1 1 calc GR . . . .
H18C H 0.428251 0.377236 0.743110 0.144 Uiso 1 1 calc GR . . . .
O10 O 0.3369(5) 0.2069(9) -0.0484(10) 0.069(4) Uani 0.5 1 d . . P B -1
N4 N 0.2826(5) 0.1696(9) 0.0475(10) 0.054(4) Uani 0.5 1 d D U P B -1
C26 C 0.3200(5) 0.1538(12) 0.0074(12) 0.052(4) Uani 0.5 1 d D U P B -1
H26 H 0.335709 0.095567 0.022410 0.062 Uiso 0.5 1 calc R . P B -1
C28 C 0.2688(7) 0.1017(13) 0.1191(13) 0.070(5) Uani 0.5 1 d D U P B -1
H28A H 0.297292 0.068682 0.153089 0.105 Uiso 0.5 1 calc GR . P B -1
H28B H 0.246049 0.056497 0.083722 0.105 Uiso 0.5 1 calc DGR . P B -1
H28C H 0.254054 0.135232 0.167743 0.105 Uiso 0.5 1 calc GR . P B -1
C27 C 0.2471(16) 0.245(3) 0.016(3) 0.077(9) Uani 0.5 1 d D U P B -1
H27A H 0.243922 0.283494 0.073610 0.115 Uiso 0.5 1 calc GR . P B -1
H27B H 0.216173 0.217203 -0.011728 0.115 Uiso 0.5 1 calc GR . P B -1
H27C H 0.257864 0.284301 -0.033690 0.115 Uiso 0.5 1 calc GR . P B -1
N3 N 0.3533(11) -0.0463(17) 0.7135(19) 0.065(3) Uani 0.229(8) 1 d D U P A 2
C23 C 0.3393(12) 0.0073(13) 0.637(2) 0.065(4) Uani 0.229(8) 1 d D U P A 2
H23 H 0.317030 -0.011470 0.580255 0.078 Uiso 0.229(8) 1 calc R . P A 2
C25 C 0.3352(15) -0.1420(17) 0.728(3) 0.076(5) Uani 0.229(8) 1 d D U P A 2
H25A H 0.303893 -0.137541 0.747217 0.114 Uiso 0.229(8) 1 calc GR . P A 2
H25B H 0.357543 -0.173824 0.780432 0.114 Uiso 0.229(8) 1 calc GR . P A 2
H25C H 0.332412 -0.177479 0.666490 0.114 Uiso 0.229(8) 1 calc GR . P A 2
C24 C 0.383(3) -0.005(3) 0.804(3) 0.065(3) Uani 0.229(8) 1 d D U P A 2
H24A H 0.416370 -0.019659 0.806479 0.097 Uiso 0.229(8) 1 calc GR . P A 2
H24B H 0.372397 -0.030168 0.862828 0.097 Uiso 0.229(8) 1 calc GR . P A 2
H24C H 0.378532 0.063465 0.802811 0.097 Uiso 0.229(8) 1 calc GR . P A 2


_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
Sm4 Sm4 3.9995(6) 7_556 ?
Sm4 O2 2.402(4) . ?
Sm4 O7 2.421(4) 2_655 ?
Sm4 O1 2.432(4) 7_556 ?
Sm4 O3 2.477(4) 4_545 ?
Sm4 O8 2.405(5) . ?
Sm4 O4 2.393(4) 6_566 ?
Sm4 O4 2.678(4) 4_545 ?
Sm4 O9 2.494(5) . ?
Sm4 O6 2.629(4) 2_655 ?
Sm4 C16 2.875(6) 2_655 ?
Sm4 C8 2.943(6) 4_545 ?
O2 C7 1.252(7) . ?
O7 C16 1.261(8) . ?
O1 C7 1.265(7) . ?
O3 C8 1.251(7) . ?
O5 C9 1.413(7) . ?
O5 C5 1.393(6) . ?
O8 C17 1.168(11) . ?
O4 C8 1.270(7) . ?
O9 C20 1.239(8) . ?
O9 C23 1.193(10) . ?
O6 C16 1.251(7) . ?
C15 C14 1.394(9) . ?
C15 C10 1.387(9) . ?
C14 C13 1.395(9) . ?
C3 C2 1.396(8) . ?
C3 C4 1.397(8) . ?
C3 C8 1.499(8) . ?
C1 C7 1.515(8) . ?
C1 C2 1.396(8) . ?
C1 C6 1.391(8) . ?
C4 C5 1.385(8) . ?
C9 C10 1.508(8) . ?
C6 C5 1.392(8) . ?
C13 C16 1.508(8) . ?
C13 C12 1.370(9) . ?
N2 C20 1.312(8) . ?
N2 C21 1.487(9) . ?
N2 C22 1.498(9) . ?
C10 C11 1.385(9) . ?
C11 C12 1.400(9) . ?
N1 C17 1.363(12) . ?
N1 C19 1.427(13) . ?
N1 C18 1.432(14) . ?
O10 C26 1.240(19) . ?
N4 C26 1.310(9) . ?
N4 C28 1.488(9) . ?
N4 C27 1.487(10) . ?
N3 C23 1.304(10) . ?
N3 C25 1.490(10) . ?
N3 C24 1.493(10) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O2 Sm4 Sm4 67.23(9) . 7_556 ?
O2 Sm4 O7 80.66(15) . 2_655 ?
O2 Sm4 O1 135.41(13) . 7_556 ?
O2 Sm4 O3 74.97(15) . 4_545 ?
O2 Sm4 O8 134.24(16) . . ?
O2 Sm4 O4 70.60(13) . 4_545 ?
O2 Sm4 O9 140.90(15) . . ?
O2 Sm4 O6 70.42(14) . 2_655 ?
O2 Sm4 C16 73.02(15) . 2_655 ?
O2 Sm4 C8 71.11(15) . 4_545 ?
O7 Sm4 Sm4 147.61(12) 2_655 7_556 ?
O7 Sm4 O1 140.81(15) 2_655 7_556 ?
O7 Sm4 O3 82.79(15) 2_655 4_545 ?
O7 Sm4 O4 129.39(15) 2_655 4_545 ?
O7 Sm4 O9 72.19(16) 2_655 . ?
O7 Sm4 O6 51.51(14) 2_655 2_655 ?
O7 Sm4 C16 25.77(16) 2_655 2_655 ?
O7 Sm4 C8 106.04(16) 2_655 4_545 ?
O1 Sm4 Sm4 69.29(9) 7_556 7_556 ?
O1 Sm4 O3 91.99(15) 7_556 4_545 ?
O1 Sm4 O4 68.53(13) 7_556 4_545 ?
O1 Sm4 O9 69.04(15) 7_556 . ?
O1 Sm4 O6 141.58(15) 7_556 2_655 ?
O1 Sm4 C16 150.89(15) 7_556 2_655 ?
O1 Sm4 C8 79.50(16) 7_556 4_545 ?
O3 Sm4 Sm4 84.87(9) 4_545 7_556 ?
O3 Sm4 O4 50.38(12) 4_545 4_545 ?
O3 Sm4 O9 74.18(17) 4_545 . ?
O3 Sm4 O6 125.59(13) 4_545 2_655 ?
O3 Sm4 C16 104.15(15) 4_545 2_655 ?
O3 Sm4 C8 24.81(15) 4_545 4_545 ?
O8 Sm4 Sm4 115.41(14) . 7_556 ?
O8 Sm4 O7 89.72(19) . 2_655 ?
O8 Sm4 O1 74.62(17) . 7_556 ?
O8 Sm4 O3 148.25(16) . 4_545 ?
O8 Sm4 O4 139.78(16) . 4_545 ?
O8 Sm4 O9 74.15(17) . . ?
O8 Sm4 O6 68.78(16) . 2_655 ?
O8 Sm4 C16 79.14(18) . 2_655 ?
O8 Sm4 C8 153.03(17) . 4_545 ?
O4 Sm4 Sm4 40.51(9) 6_566 7_556 ?
O4 Sm4 Sm4 35.50(8) 4_545 7_556 ?
O4 Sm4 O2 74.02(14) 6_566 . ?
O4 Sm4 O7 134.52(14) 6_566 2_655 ?
O4 Sm4 O1 79.54(14) 6_566 7_556 ?
O4 Sm4 O3 124.34(14) 6_566 4_545 ?
O4 Sm4 O8 82.12(16) 6_566 . ?
O4 Sm4 O4 76.01(14) 6_566 4_545 ?
O4 Sm4 O9 144.51(15) 6_566 . ?
O4 Sm4 O6 84.24(13) 6_566 2_655 ?
O4 Sm4 C16 109.29(15) 6_566 2_655 ?
O4 Sm4 C16 139.97(14) 4_545 2_655 ?
O4 Sm4 C8 100.66(15) 6_566 4_545 ?
O4 Sm4 C8 25.56(14) 4_545 4_545 ?
O9 Sm4 Sm4 132.17(12) . 7_556 ?
O9 Sm4 O4 105.96(15) . 4_545 ?
O9 Sm4 O6 110.29(16) . 2_655 ?
O9 Sm4 C16 91.94(17) . 2_655 ?
O9 Sm4 C8 89.72(18) . 4_545 ?
O6 Sm4 Sm4 116.83(10) 2_655 7_556 ?
O6 Sm4 O4 139.79(14) 2_655 4_545 ?
O6 Sm4 C16 25.78(15) 2_655 2_655 ?
O6 Sm4 C8 138.06(15) 2_655 4_545 ?
C16 Sm4 Sm4 135.26(12) 2_655 7_556 ?
C16 Sm4 C8 123.75(16) 2_655 4_545 ?
C8 Sm4 Sm4 60.45(12) 4_545 7_556 ?
C7 O2 Sm4 135.8(4) . . ?
C16 O7 Sm4 97.7(4) . 2_655 ?
C7 O1 Sm4 134.2(4) . 7_556 ?
C8 O3 Sm4 99.0(3) . 4 ?
C5 O5 C9 116.2(5) . . ?
C17 O8 Sm4 140.5(7) . . ?
Sm4 O4 Sm4 103.99(14) 6_565 4 ?
C8 O4 Sm4 89.0(3) . 4 ?
C8 O4 Sm4 159.8(4) . 6_565 ?
C20 O9 Sm4 127.0(6) . . ?
C23 O9 Sm4 118.7(14) . . ?
C16 O6 Sm4 88.2(3) . 2_655 ?
C10 C15 C14 120.4(6) . . ?
C15 C14 C13 120.2(6) . . ?
C2 C3 C4 120.3(5) . . ?
C2 C3 C8 120.2(5) . . ?
C4 C3 C8 119.4(5) . . ?
C2 C1 C7 121.5(5) . . ?
C6 C1 C7 118.5(5) . . ?
C6 C1 C2 120.0(5) . . ?
O2 C7 O1 126.3(5) . . ?
O2 C7 C1 117.0(5) . . ?
O1 C7 C1 116.7(5) . . ?
C1 C2 C3 119.7(5) . . ?
C5 C4 C3 119.2(5) . . ?
O5 C9 C10 109.7(5) . . ?
C1 C6 C5 119.6(5) . . ?
C4 C5 O5 115.8(5) . . ?
C4 C5 C6 121.0(5) . . ?
C6 C5 O5 123.2(5) . . ?
C14 C13 C16 118.9(5) . . ?
C12 C13 C14 119.0(6) . . ?
C12 C13 C16 122.1(6) . . ?
C20 N2 C21 127.5(10) . . ?
C20 N2 C22 117.7(10) . . ?
C21 N2 C22 114.7(9) . . ?
O7 C16 Sm4 56.6(3) . 2_655 ?
O7 C16 C13 117.0(5) . . ?
O6 C16 Sm4 66.0(3) . 2_655 ?
O6 C16 O7 122.5(5) . . ?
O6 C16 C13 120.5(5) . . ?
C13 C16 Sm4 172.5(4) . 2_655 ?
O3 C8 Sm4 56.2(3) . 4 ?
O3 C8 O4 121.7(5) . . ?
O3 C8 C3 119.2(5) . . ?
O4 C8 Sm4 65.4(3) . 4 ?
O4 C8 C3 119.1(5) . . ?
C3 C8 Sm4 175.3(4) . 4 ?
C15 C10 C9 117.1(6) . . ?
C11 C10 C15 119.4(6) . . ?
C11 C10 C9 123.4(6) . . ?
C10 C11 C12 119.8(6) . . ?
C17 N1 C19 121.0(10) . . ?
C17 N1 C18 118.9(9) . . ?
C19 N1 C18 119.7(9) . . ?
C13 C12 C11 121.2(6) . . ?
O9 C20 N2 134.0(11) . . ?
O8 C17 N1 127.8(11) . . ?
C26 N4 C28 120.2(14) . . ?
C26 N4 C27 125(2) . . ?
C27 N4 C28 115(2) . . ?
O10 C26 N4 126.7(16) . . ?
C23 N3 C25 126.0(13) . . ?
C23 N3 C24 119(2) . . ?
C25 N3 C24 114.1(10) . . ?
O9 C23 N3 112(2) . . ?

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
Sm4 O2 C7 O1 -38.5(10) . . . . ?
Sm4 O2 C7 C1 140.9(4) . . . . ?
Sm4 O7 C16 O6 4.4(7) 2_655 . . . ?
Sm4 O7 C16 C13 -175.5(4) 2_655 . . . ?
Sm4 O1 C7 O2 13.7(10) 7_556 . . . ?
Sm4 O1 C7 C1 -165.8(4) 7_556 . . . ?
Sm4 O3 C8 O4 0.7(6) 4 . . . ?
Sm4 O3 C8 C3 -178.6(4) 4 . . . ?
Sm4 O8 C17 N1 -158.3(7) . . . . ?
Sm4 O4 C8 Sm4 130.6(10) 6_565 . . 4 ?
Sm4 O4 C8 O3 130.0(9) 6_565 . . . ?
Sm4 O4 C8 O3 -0.6(6) 4 . . . ?
Sm4 O4 C8 C3 178.7(5) 4 . . . ?
Sm4 O4 C8 C3 -50.7(13) 6_565 . . . ?
Sm4 O9 C20 N2 170.3(14) . . . . ?
Sm4 O9 C23 N3 -159(2) . . . . ?
Sm4 O6 C16 O7 -4.0(6) 2_655 . . . ?
Sm4 O6 C16 C13 175.9(5) 2_655 . . . ?
O5 C9 C10 C15 -155.4(6) . . . . ?
O5 C9 C10 C11 28.2(9) . . . . ?
C15 C14 C13 C16 175.8(7) . . . . ?
C15 C14 C13 C12 -1.5(11) . . . . ?
C15 C10 C11 C12 0.2(11) . . . . ?
C14 C15 C10 C9 -176.1(7) . . . . ?
C14 C15 C10 C11 0.5(12) . . . . ?
C14 C13 C16 O7 1.3(9) . . . . ?
C14 C13 C16 O6 -178.6(6) . . . . ?
C14 C13 C12 C11 2.2(11) . . . . ?
C3 C4 C5 O5 176.7(5) . . . . ?
C3 C4 C5 C6 -4.1(9) . . . . ?
C1 C6 C5 O5 -178.0(5) . . . . ?
C1 C6 C5 C4 2.9(9) . . . . ?
C7 C1 C2 C3 176.0(5) . . . . ?
C7 C1 C6 C5 -178.1(5) . . . . ?
C2 C3 C4 C5 2.1(9) . . . . ?
C2 C3 C8 O3 -24.9(8) . . . . ?
C2 C3 C8 O4 155.8(5) . . . . ?
C2 C1 C7 O2 -175.2(5) . . . . ?
C2 C1 C7 O1 4.2(9) . . . . ?
C2 C1 C6 C5 0.5(9) . . . . ?
C4 C3 C2 C1 1.3(9) . . . . ?
C4 C3 C8 O3 153.7(6) . . . . ?
C4 C3 C8 O4 -25.6(8) . . . . ?
C9 O5 C5 C4 -163.0(6) . . . . ?
C9 O5 C5 C6 17.8(8) . . . . ?
C9 C10 C11 C12 176.6(7) . . . . ?
C6 C1 C7 O2 3.4(8) . . . . ?
C6 C1 C7 O1 -177.1(6) . . . . ?
C6 C1 C2 C3 -2.6(9) . . . . ?
C5 O5 C9 C10 166.1(5) . . . . ?
C16 C13 C12 C11 -175.1(6) . . . . ?
C8 C3 C2 C1 179.8(5) . . . . ?
C8 C3 C4 C5 -176.5(5) . . . . ?
C10 C15 C14 C13 0.2(12) . . . . ?
C10 C11 C12 C13 -1.6(11) . . . . ?
C12 C13 C16 O7 178.6(6) . . . . ?
C12 C13 C16 O6 -1.3(9) . . . . ?
C21 N2 C20 O9 174.7(13) . . . . ?
C22 N2 C20 O9 -6(3) . . . . ?
C19 N1 C17 O8 176.1(10) . . . . ?
C18 N1 C17 O8 3.1(17) . . . . ?
C28 N4 C26 O10 -175.3(17) . . . . ?
C27 N4 C26 O10 14(4) . . . . ?
C25 N3 C23 O9 176(3) . . . . ?
C24 N3 C23 O9 9(6) . . . . ?

_platon_squeeze_details          ?
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.500 0.885 0.250 128 45 ' '
2 1.000 0.385 0.250 128 45 ' '
3 0.500 0.115 0.750 128 45 ' '
4 1.000 0.615 0.750 128 45 ' '

_platon_squeeze_void_probe_radius 1.20
_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_2
_database_code_depnum_ccdc_archive 'CCDC 2071652'
loop_
_audit_author_name
_audit_author_address
'Yun-Shan Xue' 'Yancheng Teachers University'
_audit_update_record             
;
2021-03-19 deposited with the CCDC.	2021-04-20 downloaded from the CCDC.
;
_audit_creation_date             2020-07-30
_audit_creation_method           
;
Olex2 1.2-beta
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         '0.11(C288 H207 Ho18 O148.5)'
_chemical_formula_sum            'C32 H23 Ho2 O16.50'
_chemical_formula_weight         1001.36
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ho Ho -0.2175 4.6783 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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      trigonal
_space_group_IT_number           148
_space_group_name_H-M_alt        'R -3'
_space_group_name_Hall           '-R 3'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'

_cell_length_a                   19.6548(11)
_cell_length_b                   19.6548(11)
_cell_length_c                   45.295(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     15153.5(19)
_cell_formula_units_Z            9
_cell_measurement_reflns_used    9886
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      26.36
_cell_measurement_theta_min      2.47
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    2.371
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.6544
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0876 before and 0.0555 after correction.
The Ratio of minimum to maximum transmission is 0.8779.
The λ/2 correction factor is Not present.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    0.988
_exptl_crystal_density_meas      .
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             4329
_exptl_crystal_size_max          ?
_exptl_crystal_size_mid          ?
_exptl_crystal_size_min          ?
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0397
_diffrn_reflns_av_unetI/netI     0.0300
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       56
_diffrn_reflns_limit_l_min       -56
_diffrn_reflns_number            50520
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.443
_diffrn_reflns_theta_min         2.160
_diffrn_ambient_temperature      150.01
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                5624
_reflns_number_total             6930
_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       'SAINT v8.37A (Bruker, 2015)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         2.779
_refine_diff_density_min         -1.319
_refine_diff_density_rms         0.131
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.086
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     245
_refine_ls_number_reflns         6930
_refine_ls_number_restraints     32
_refine_ls_R_factor_all          0.0533
_refine_ls_R_factor_gt           0.0424
_refine_ls_restrained_S_all      1.117
_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)+(0.0697P)²+113.8379P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1246
_refine_ls_wR_factor_ref         0.1305
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All O(H,H) groups
2. Restrained distances
 Ho01-O10 = Ho01-O8
 2.4 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
O8 \\sim O10: within 2A with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(O8) \\sim Ueq, Uanis(O9) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(O8) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O8) \\sim Ueq, Uanis(O10) \\sim Ueq: with sigma of 0.005 and sigma for
terminal atoms of 0.01
Uanis(O10) \\sim Ueq, Uanis(O8) \\sim Ueq: with sigma of 0.005 and sigma for
terminal atoms of 0.01
Uanis(O7) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
4. Rigid body (RIGU) restrains
 O8, O10
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.005
5. Others
 Sof(O10)=Sof(H10A)=Sof(H10B)=0.75*(1-FVAR(2))
 Sof(O8)=Sof(H8A)=Sof(H8B)=0.75*FVAR(2)
 Fixed Sof: O9(0.5) H9A(0.5) H9B(0.5)
6.a Riding coordinates:
 O8(H8A,H8B), O9(H9A,H9B), O10(H10A,H10B)
6.b Secondary CH2 refined with riding coordinates:
 C15(H15A,H15B)
6.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C6(H6), C10(H10), C11(H11), C13(H13), C14(H14), C16(H16)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     ?
_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
Ho01 Ho 0.19414(2) 0.37891(2) 0.37430(2) 0.02957(10) Uani 1 1 d D . . . .
O1 O 0.1949(3) 0.2796(2) 0.34931(8) 0.0479(10) Uani 1 1 d . . . . .
O2 O 0.3992(2) 0.2603(3) 0.58172(8) 0.0486(10) Uani 1 1 d . . . . .
O3 O 0.1785(3) 0.2023(2) 0.31141(8) 0.0478(11) Uani 1 1 d . . . . .
O4 O 0.1813(3) -0.0414(2) 0.32648(9) 0.0610(14) Uani 1 1 d . . . . .
O5 O 0.2281(3) -0.0626(2) 0.36830(8) 0.0572(13) Uani 1 1 d . . . . .
O6 O 0.2999(3) 0.1399(3) 0.58232(10) 0.0641(14) Uani 1 1 d . . . . .
O7 O 0.2754(4) 0.1602(3) 0.43315(11) 0.0800(16) Uani 1 1 d . U . . .
C1 C 0.3413(4) 0.2042(4) 0.56928(11) 0.0428(14) Uani 1 1 d . . . . .
C2 C 0.1948(4) 0.2205(4) 0.33805(12) 0.0469(15) Uani 1 1 d . . . . .
C3 C 0.2055(4) 0.1025(3) 0.34597(12) 0.0462(15) Uani 1 1 d . . . . .
H3 H 0.190190 0.088475 0.325992 0.055 Uiso 1 1 calc R . . . .
C4 C 0.2203(5) 0.0539(4) 0.36426(12) 0.059(2) Uani 1 1 d . . . . .
C5 C 0.2137(5) 0.1705(4) 0.35741(12) 0.0537(18) Uani 1 1 d . . . . .
C6 C 0.2412(6) 0.0740(5) 0.39324(13) 0.078(3) Uani 1 1 d . . . . .
H6 H 0.249332 0.039844 0.405750 0.094 Uiso 1 1 calc R . . . .
C7 C 0.2506(7) 0.1439(5) 0.40428(14) 0.085(3) Uani 1 1 d . . . . .
C8 C 0.2085(5) -0.0234(4) 0.35211(12) 0.0536(17) Uani 1 1 d . . . . .
C9 C 0.3234(5) 0.2137(4) 0.53805(12) 0.0550(17) Uani 1 1 d . . . . .
C10 C 0.2355(6) 0.1919(4) 0.38658(13) 0.075(3) Uani 1 1 d . . . . .
H10 H 0.239890 0.238962 0.394238 0.090 Uiso 1 1 calc R . . . .
C11 C 0.3775(6) 0.2712(5) 0.52064(14) 0.077(2) Uani 1 1 d . . . . .
H11 H 0.426528 0.308383 0.528983 0.092 Uiso 1 1 calc R . . . .
O8 O 0.3122(4) 0.3858(6) 0.39343(19) 0.056(3) Uani 0.509(12) 1 d D U P A 1
H8A H 0.311754 0.389370 0.415003 0.085 Uiso 0.509(12) 1 d R . P A 1
H8B H 0.358054 0.432730 0.385533 0.085 Uiso 0.509(12) 1 d R . P A 1
C12 C 0.2942(6) 0.2262(5) 0.47870(15) 0.073(2) Uani 1 1 d . . . . .
C13 C 0.2510(5) 0.1620(5) 0.52620(16) 0.079(2) Uani 1 1 d . . . . .
H13 H 0.211821 0.121806 0.538158 0.095 Uiso 1 1 calc R . . . .
O9 O 0.2799(5) 0.5085(4) 0.39608(17) 0.054(2) Uani 0.5 1 d . U P A .
H9A H 0.256377 0.513199 0.414489 0.080 Uiso 0.5 1 d R . P . .
H9B H 0.285207 0.549039 0.382179 0.080 Uiso 0.5 1 d R . P . .
C14 C 0.3637(7) 0.2777(6) 0.49067(15) 0.088(3) Uani 1 1 d . . . . .
H14 H 0.403174 0.318358 0.478936 0.105 Uiso 1 1 calc R . . . .
C15 C 0.2781(7) 0.2290(5) 0.44612(15) 0.100(4) Uani 1 1 d . . . . .
H15A H 0.227461 0.227526 0.443248 0.120 Uiso 1 1 calc R . . . .
H15B H 0.320433 0.277575 0.436989 0.120 Uiso 1 1 calc R . . . .
C16 C 0.2353(7) 0.1687(6) 0.49638(19) 0.091(3) Uani 1 1 d . . . . .
H16 H 0.184877 0.134375 0.488316 0.109 Uiso 1 1 calc R . . . .
O10 O 0.3082(7) 0.4327(12) 0.4028(3) 0.048(4) Uani 0.241(12) 1 d D U P A 2
H10A H 0.295505 0.410558 0.422774 0.072 Uiso 0.241(12) 1 d R . P A 2
H10B H 0.345905 0.420208 0.393724 0.072 Uiso 0.241(12) 1 d R . P A 2


_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
Ho01 O1 2.263(4) . ?
Ho01 O1 2.837(4) 16 ?
Ho01 O2 2.396(4) 12_556 ?
Ho01 O3 2.336(4) 16 ?
Ho01 O4 2.294(4) 17 ?
Ho01 O5 2.298(4) 2 ?
Ho01 O6 2.384(4) 12_556 ?
Ho01 C1 2.740(5) 12_556 ?
Ho01 C2 2.944(5) 16 ?
Ho01 O8 2.416(6) . ?
Ho01 O9 2.451(7) . ?
Ho01 O10 2.333(9) . ?
O1 C2 1.268(7) . ?
O2 C1 1.255(7) . ?
O3 C2 1.254(6) . ?
O4 C8 1.253(7) . ?
O5 C8 1.255(7) . ?
O6 C1 1.257(7) . ?
O7 C7 1.376(8) . ?
O7 C15 1.450(8) . ?
C1 C9 1.491(7) . ?
C2 C5 1.495(8) . ?
C3 C4 1.401(7) . ?
C3 C5 1.366(8) . ?
C4 C6 1.373(8) . ?
C4 C8 1.521(8) . ?
C5 C10 1.388(8) . ?
C6 C7 1.387(9) . ?
C7 C10 1.379(9) . ?
C9 C11 1.352(11) . ?
C9 C13 1.378(11) . ?
C11 C14 1.403(9) . ?
C12 C14 1.342(13) . ?
C12 C15 1.516(9) . ?
C12 C16 1.396(13) . ?
C13 C16 1.407(10) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Ho01 O1 76.30(13) . 16 ?
O1 Ho01 O2 139.33(15) . 12_556 ?
O1 Ho01 O3 125.63(13) . 16 ?
O1 Ho01 O4 77.26(16) . 17 ?
O1 Ho01 O5 77.29(17) . 2 ?
O1 Ho01 O6 88.37(15) . 12_556 ?
O1 Ho01 C1 114.32(17) . 12_556 ?
O1 Ho01 C2 25.25(13) 16 16 ?
O1 Ho01 C2 101.52(15) . 16 ?
O1 Ho01 O8 78.9(3) . . ?
O1 Ho01 O9 143.1(3) . . ?
O1 Ho01 O10 104.4(6) . . ?
O2 Ho01 O1 121.79(14) 12_556 16 ?
O2 Ho01 C1 27.24(16) 12_556 12_556 ?
O2 Ho01 C2 102.05(15) 12_556 16 ?
O2 Ho01 O8 101.2(3) 12_556 . ?
O2 Ho01 O9 68.0(2) 12_556 . ?
O3 Ho01 O1 49.33(11) 16 16 ?
O3 Ho01 O2 81.20(14) 16 12_556 ?
O3 Ho01 O6 133.32(15) 16 12_556 ?
O3 Ho01 C1 107.48(17) 16 12_556 ?
O3 Ho01 C2 24.13(14) 16 16 ?
O3 Ho01 O8 138.2(3) 16 . ?
O3 Ho01 O9 72.8(3) 16 . ?
O4 Ho01 O1 66.14(15) 17 16 ?
O4 Ho01 O2 142.21(15) 17 12_556 ?
O4 Ho01 O3 80.59(18) 17 16 ?
O4 Ho01 O5 130.86(14) 17 2 ?
O4 Ho01 O6 143.44(19) 17 12_556 ?
O4 Ho01 C1 153.48(16) 17 12_556 ?
O4 Ho01 C2 70.84(19) 17 16 ?
O4 Ho01 O8 72.4(2) 17 . ?
O4 Ho01 O9 75.1(2) 17 . ?
O4 Ho01 O10 76.9(4) 17 . ?
O5 Ho01 O1 67.35(14) 2 16 ?
O5 Ho01 O2 77.97(14) 2 12_556 ?
O5 Ho01 O3 81.18(17) 2 16 ?
O5 Ho01 O6 76.25(18) 2 12_556 ?
O5 Ho01 C1 75.66(15) 2 12_556 ?
O5 Ho01 C2 74.05(18) 2 16 ?
O5 Ho01 O8 140.5(3) 2 . ?
O5 Ho01 O9 139.6(2) 2 . ?
O5 Ho01 O10 150.6(4) 2 . ?
O6 Ho01 O1 142.70(17) 12_556 16 ?
O6 Ho01 O2 54.52(15) 12_556 12_556 ?
O6 Ho01 C1 27.28(17) 12_556 12_556 ?
O6 Ho01 C2 145.61(18) 12_556 16 ?
O6 Ho01 O8 72.0(2) 12_556 . ?
O6 Ho01 O9 99.7(2) 12_556 . ?
C1 Ho01 O1 138.22(16) 12_556 16 ?
C1 Ho01 C2 125.65(18) 12_556 16 ?
O8 Ho01 O1 135.2(2) . 16 ?
O8 Ho01 C1 86.1(2) . 12_556 ?
O8 Ho01 C2 142.1(3) . 16 ?
O8 Ho01 O9 69.8(4) . . ?
O9 Ho01 O1 113.0(2) . 16 ?
O9 Ho01 C1 83.2(2) . 12_556 ?
O9 Ho01 C2 91.9(3) . 16 ?
O10 Ho01 O1 142.0(4) . 16 ?
O10 Ho01 O6 74.5(4) . 12_556 ?
O10 Ho01 C2 132.4(5) . 16 ?
O10 Ho01 O9 45.6(6) . . ?
Ho01 O1 Ho01 103.70(13) . 16 ?
C2 O1 Ho01 173.7(4) . . ?
C2 O1 Ho01 82.1(3) . 16 ?
C1 O2 Ho01 91.9(3) . 11_556 ?
C2 O3 Ho01 106.2(3) . 16 ?
C8 O4 Ho01 139.6(4) . 18_545 ?
C8 O5 Ho01 134.8(4) . 3 ?
C1 O6 Ho01 92.4(3) . 11_556 ?
C7 O7 C15 116.4(5) . . ?
O2 C1 Ho01 60.9(3) . 11_556 ?
O2 C1 O6 121.3(5) . . ?
O2 C1 C9 118.9(6) . . ?
O6 C1 Ho01 60.4(3) . 11_556 ?
O6 C1 C9 119.8(6) . . ?
C9 C1 Ho01 177.3(4) . 11_556 ?
O1 C2 Ho01 72.6(3) . 16 ?
O1 C2 C5 118.6(5) . . ?
O3 C2 Ho01 49.6(3) . 16 ?
O3 C2 O1 122.1(5) . . ?
O3 C2 C5 119.3(5) . . ?
C5 C2 Ho01 167.6(4) . 16 ?
C5 C3 C4 118.7(5) . . ?
C3 C4 C8 119.2(5) . . ?
C6 C4 C3 120.3(5) . . ?
C6 C4 C8 120.5(5) . . ?
C3 C5 C2 118.3(5) . . ?
C3 C5 C10 121.7(5) . . ?
C10 C5 C2 119.9(5) . . ?
C4 C6 C7 120.1(6) . . ?
O7 C7 C6 115.4(6) . . ?
O7 C7 C10 124.5(6) . . ?
C10 C7 C6 120.1(6) . . ?
O4 C8 O5 126.0(5) . . ?
O4 C8 C4 116.5(5) . . ?
O5 C8 C4 117.5(5) . . ?
C11 C9 C1 121.5(7) . . ?
C11 C9 C13 118.6(6) . . ?
C13 C9 C1 119.9(7) . . ?
C7 C10 C5 119.0(6) . . ?
C9 C11 C14 122.3(9) . . ?
C14 C12 C15 121.2(9) . . ?
C14 C12 C16 119.9(7) . . ?
C16 C12 C15 118.9(9) . . ?
C9 C13 C16 119.9(9) . . ?
C12 C14 C11 119.4(9) . . ?
O7 C15 C12 105.7(6) . . ?
C12 C16 C13 119.6(9) . . ?

_olex2_submission_special_instructions 'No special instructions were received'
