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

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

data_l71-sm
_database_code_depnum_ccdc_archive 'CCDC 2117146'
loop_
_audit_author_name
_audit_author_address
'SHANG '
; Luoyang Normal University, 
China
;
_audit_update_record             
;
2021-10-21 deposited with the CCDC.	2022-06-01 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT602_l71-sm              
;
PROBLEM: Solvent Accessible VOID(S) in Structure ........          ! Check
RESPONSE: This is due to large void in crystal.
;
_vrf_PLAT971_l71-sm              
;
PROBLEM: Check Calcd Resid. Dens.  2.80A   From O12             4.13 eA-3
RESPONSE: The disordered O and   large void in crystal.
;
# Added during the CSD deposition process: Thursday 21 October 2021 02:21 AM
# end Validation Reply Form

_audit_creation_date             2019-02-26
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2014/7
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C34 H23 N3 O18.5 Sm2'
_chemical_formula_sum            'C34 H31 N3 O22.50 Sm2'
_chemical_formula_weight         1142.32
_chemical_melting_point          ?
_chemical_oxdiff_usercomment     'C H O N Sm'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Sm Sm -0.1638 3.4418 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           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                   17.4522(5)
_cell_length_b                   31.6114(7)
_cell_length_c                   18.0196(3)
_cell_angle_alpha                90
_cell_angle_beta                 107.351(2)
_cell_angle_gamma                90
_cell_volume                     9488.8(4)
_cell_formula_units_Z            8
_cell_measurement_reflns_used    14803
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.7140
_cell_measurement_theta_min      3.7980
_shelx_estimated_absorpt_T_max   0.619
_shelx_estimated_absorpt_T_min   0.548
_exptl_absorpt_coefficient_mu    2.529
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.85464
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            pink
_exptl_crystal_colour_primary    pink
_exptl_crystal_density_diffrn    1.599
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             4480
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.21
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0279
_diffrn_reflns_av_unetI/netI     0.0456
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.826
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       41
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            21589
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.826
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.466
_diffrn_reflns_theta_min         3.447
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0584
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.826
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -16.00  24.00   1.00   12.50    --  -13.80 -99.00  90.00   40
  2  ω    -40.00  29.00   1.00   12.50    --   14.82 -57.00 -30.00   69
  3  ω    -25.00  22.00   1.00   12.50    --   14.82 -57.00  90.00   47
  4  ω      7.00  62.00   1.00   12.50    --   14.82  38.00 -90.00   55
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Single source at offset/far, EosS2'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0276832000
_diffrn_orient_matrix_UB_12      0.0156973000
_diffrn_orient_matrix_UB_13      0.0196412000
_diffrn_orient_matrix_UB_21      -0.0264369000
_diffrn_orient_matrix_UB_22      0.0160764000
_diffrn_orient_matrix_UB_23      -0.0203362000
_diffrn_orient_matrix_UB_31      -0.0185767000
_diffrn_orient_matrix_UB_32      0.0005900000
_diffrn_orient_matrix_UB_33      0.0300196000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                8226
_reflns_number_total             9917
_reflns_odcompleteness_completeness 99.57
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     25.30
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         3.318
_refine_diff_density_min         -0.651
_refine_diff_density_rms         0.223
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     531
_refine_ls_number_reflns         9917
_refine_ls_number_restraints     10
_refine_ls_R_factor_all          0.0681
_refine_ls_R_factor_gt           0.0564
_refine_ls_restrained_S_all      1.063
_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)+(0.1061P)²+150.0892P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1809
_refine_ls_wR_factor_ref         0.1913
_refine_special_details          SQUEEZE
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H,H) groups
2. Restrained distances
 Sm1-O17 \\sim Sm1-O17A \\sim Sm1-O16 \\sim Sm1-O15 \\sim Sm1-O15A
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(O17A) = Uanis(O17)
Uanis(O15A) = Uanis(O15)
4. Others
 Sof(O17A)=Sof(H17C)=Sof(H17D)=1-FVAR(1)
 Sof(O17)=Sof(H17A)=Sof(H17B)=FVAR(1)
 Sof(O15A)=Sof(H15C)=Sof(H15D)=1-FVAR(2)
 Sof(O15)=Sof(H15A)=Sof(H15B)=FVAR(2)
 Fixed Sof: O16(0.5) H16A(0.5) H16B(0.5)
5.a Riding coordinates:
 O15(H15A,H15B), O16(H16A,H16B), O17(H17A,H17B), O18(H18A,H18B), O19(H19A,
 H19B), O17A(H17C,H17D), O15A(H15C,H15D)
5.b Aromatic/amide H refined with riding coordinates:
 C4(H4), C6(H6), C11(H11), C13(H13), C15(H15), C16(H16), C18(H18), C19(H19),
 C20(H20), C21(H21), C23(H23), C24(H24), C28(H28), C30(H30)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Sm1 Sm 0.71431(2) 0.60769(2) 0.62690(2) 0.02738(14) Uani 1 1 d D . . . .
Sm2 Sm 0.94752(2) 0.87427(2) 0.58909(2) 0.02280(13) Uani 1 1 d . . . . .
O1 O 0.3182(5) 0.5603(2) 0.7798(4) 0.055(2) Uani 1 1 d . . . . .
O2 O 0.3650(4) 0.62395(17) 0.7779(3) 0.0324(13) Uani 1 1 d . . . . .
O3 O 0.4510(3) 0.62468(18) 0.4855(3) 0.0301(12) Uani 1 1 d . . . . .
O4 O 0.5722(3) 0.60490(17) 0.5517(3) 0.0277(12) Uani 1 1 d . . . . .
O5 O 0.4775(4) 0.45007(18) 0.5767(3) 0.0421(16) Uani 1 1 d . . . . .
O6 O 0.4136(4) 0.43895(19) 0.6626(4) 0.0411(15) Uani 1 1 d . . . . .
O7 O 0.8393(6) 0.7989(3) 0.7364(4) 0.091(4) Uani 1 1 d . . . . .
O8 O 0.8699(4) 0.84994(19) 0.6686(3) 0.0335(13) Uani 1 1 d . . . . .
O9 O 0.8080(3) 0.88686(17) 0.5170(3) 0.0298(12) Uani 1 1 d . . . . .
O10 O 0.7151(5) 0.9032(2) 0.5739(5) 0.057(2) Uani 1 1 d . . . . .
O11 O 0.6632(4) 0.8735(2) 0.3979(4) 0.0425(15) Uani 1 1 d . . . . .
O12 O 0.5497(5) 0.8398(4) 0.3827(7) 0.116(5) Uani 1 1 d . . . . .
O13 O 0.6839(4) 0.67955(19) 0.6002(3) 0.0363(13) Uani 1 1 d . . . . .
O14 O 0.5929(4) 0.68981(19) 0.4847(3) 0.0409(15) Uani 1 1 d . . . . .
O15 O 0.8017(7) 0.6415(6) 0.7456(6) 0.078(5) Uani 0.742(18) 1 d D . P A 1
H15A H 0.7733 0.6576 0.7770 0.117 Uiso 0.742(18) 1 d R . P A 1
H15B H 0.8363 0.6647 0.7365 0.117 Uiso 0.742(18) 1 d R . P A 1
O16 O 0.8280(9) 0.5577(6) 0.6840(13) 0.093(7) Uani 0.5 1 d D . P A .
H16A H 0.8484 0.5500 0.7333 0.140 Uiso 0.5 1 d R . P . .
H16B H 0.8568 0.5438 0.6590 0.140 Uiso 0.5 1 d R . P . .
O17 O 0.6861(14) 0.5377(4) 0.5661(9) 0.071(5) Uani 0.61(2) 1 d D . P A 1
H17A H 0.7196 0.5314 0.5386 0.107 Uiso 0.61(2) 1 d R . P A 1
H17B H 0.6381 0.5370 0.5299 0.107 Uiso 0.61(2) 1 d R . P A 1
O18 O 1.0202(5) 0.8125(2) 0.6521(4) 0.0538(18) Uani 1 1 d . . . . .
H18A H 1.0256 0.8135 0.7006 0.081 Uiso 1 1 d R . . . .
H18B H 1.0680 0.8133 0.6493 0.081 Uiso 1 1 d R . . . .
O19 O 1.0687(5) 0.8934(2) 0.6945(4) 0.0539(19) Uani 1 1 d . . . . .
H19A H 1.0632 0.9187 0.7137 0.081 Uiso 1 1 d R . . . .
H19B H 1.1105 0.8971 0.6767 0.081 Uiso 1 1 d R . . . .
N1 N 0.3706(4) 0.7311(2) 0.6181(4) 0.0346(15) Uani 1 1 d . . . . .
N2 N 0.6199(8) 0.8157(4) 0.7042(7) 0.076(3) Uani 1 1 d . . . . .
N3 N 0.0772(6) 0.7568(4) 0.5592(7) 0.077(3) Uani 1 1 d . . . . .
C1 C 0.3940(4) 0.5712(2) 0.6921(4) 0.0228(14) Uani 1 1 d . . . . .
C2 C 0.4216(4) 0.5988(2) 0.6447(4) 0.0241(15) Uani 1 1 d . . . . .
C3 C 0.4648(4) 0.5812(2) 0.5973(4) 0.0218(14) Uani 1 1 d . . . . .
C4 C 0.4742(5) 0.5376(2) 0.5945(4) 0.0244(15) Uani 1 1 d . . . . .
H4 H 0.5030 0.5265 0.5631 0.029 Uiso 1 1 calc R . . . .
C5 C 0.4417(5) 0.5103(2) 0.6374(4) 0.0240(15) Uani 1 1 d . . . . .
C6 C 0.4021(5) 0.5278(2) 0.6861(4) 0.0249(15) Uani 1 1 d . . . . .
H6 H 0.3803 0.5099 0.7155 0.030 Uiso 1 1 calc R . . . .
C7 C 0.3565(5) 0.5868(3) 0.7528(4) 0.0269(16) Uani 1 1 d . . . . .
C8 C 0.4979(5) 0.6062(2) 0.5431(4) 0.0233(15) Uani 1 1 d . . . . .
C9 C 0.4441(5) 0.4639(2) 0.6252(4) 0.0250(15) Uani 1 1 d . . . . .
C10 C 0.4465(5) 0.7174(3) 0.6392(4) 0.0301(17) Uani 1 1 d . . . . .
C11 C 0.4662(5) 0.6749(2) 0.6496(4) 0.0270(16) Uani 1 1 d . . . . .
H11 H 0.5196 0.6663 0.6640 0.032 Uiso 1 1 calc R . . . .
C12 C 0.4044(4) 0.6452(2) 0.6381(4) 0.0236(14) Uani 1 1 d . . . . .
C13 C 0.3270(5) 0.6597(3) 0.6169(5) 0.0310(17) Uani 1 1 d . . . . .
H13 H 0.2848 0.6406 0.6093 0.037 Uiso 1 1 calc R . . . .
C14 C 0.3111(5) 0.7026(3) 0.6066(5) 0.0342(18) Uani 1 1 d . . . . .
C15 C 0.6412(7) 0.7763(4) 0.7205(6) 0.058(3) Uani 1 1 d . . . . .
H15 H 0.6940 0.7704 0.7486 0.070 Uiso 1 1 calc R . . . .
C16 C 0.5874(6) 0.7433(3) 0.6973(5) 0.042(2) Uani 1 1 d . . . . .
H16 H 0.6047 0.7156 0.7085 0.050 Uiso 1 1 calc R . . . .
C17 C 0.5089(6) 0.7514(3) 0.6578(5) 0.039(2) Uani 1 1 d . . . . .
C18 C 0.4861(8) 0.7931(4) 0.6413(8) 0.067(3) Uani 1 1 d . . . . .
H18 H 0.4332 0.8000 0.6149 0.080 Uiso 1 1 calc R . . . .
C19 C 0.5433(12) 0.8241(5) 0.6648(10) 0.098(5) Uani 1 1 d . . . . .
H19 H 0.5283 0.8521 0.6529 0.117 Uiso 1 1 calc R . . . .
C20 C 0.0877(9) 0.7138(5) 0.5639(11) 0.092(5) Uani 1 1 d . . . . .
H20 H 0.0440 0.6963 0.5603 0.111 Uiso 1 1 calc R . . . .
C21 C 0.1630(7) 0.6963(4) 0.5740(9) 0.072(4) Uani 1 1 d . . . . .
H21 H 0.1680 0.6671 0.5719 0.086 Uiso 1 1 calc R . . . .
C22 C 0.2288(6) 0.7205(3) 0.5866(5) 0.040(2) Uani 1 1 d . . . . .
C23 C 0.2165(6) 0.7629(4) 0.5809(6) 0.052(3) Uani 1 1 d . . . . .
H23 H 0.2604 0.7807 0.5870 0.062 Uiso 1 1 calc R . . . .
C24 C 0.1411(8) 0.7805(4) 0.5664(7) 0.064(3) Uani 1 1 d . . . . .
H24 H 0.1353 0.8098 0.5617 0.077 Uiso 1 1 calc R . . . .
C25 C 0.7628(5) 0.8039(3) 0.6064(4) 0.0273(16) Uani 1 1 d . . . . .
C26 C 0.7265(4) 0.8312(3) 0.5448(4) 0.0270(16) Uani 1 1 d . . . . .
C27 C 0.6626(5) 0.8166(3) 0.4840(5) 0.0305(17) Uani 1 1 d . . . . .
C28 C 0.6359(5) 0.7754(3) 0.4843(4) 0.0304(17) Uani 1 1 d . . . . .
H28 H 0.5923 0.7661 0.4439 0.037 Uiso 1 1 calc R . . . .
C29 C 0.6730(5) 0.7476(2) 0.5439(4) 0.0260(16) Uani 1 1 d . . . . .
C30 C 0.7363(5) 0.7625(3) 0.6044(4) 0.0290(16) Uani 1 1 d . . . . .
H30 H 0.7617 0.7443 0.6448 0.035 Uiso 1 1 calc R . . . .
C31 C 0.8289(6) 0.8183(3) 0.6756(4) 0.037(2) Uani 1 1 d . . . . .
C32 C 0.7514(5) 0.8773(3) 0.5465(5) 0.0306(17) Uani 1 1 d . . . . .
C33 C 0.6227(5) 0.8446(3) 0.4162(6) 0.046(2) Uani 1 1 d . . . . .
C34 C 0.6478(5) 0.7020(3) 0.5433(4) 0.0287(17) Uani 1 1 d . . . . .
O17A O 0.738(2) 0.5355(5) 0.5911(16) 0.071(5) Uani 0.39(2) 1 d D . P A 2
H17C H 0.7835 0.5198 0.6289 0.107 Uiso 0.39(2) 1 d R . P A 2
H17D H 0.7569 0.5328 0.5439 0.107 Uiso 0.39(2) 1 d R . P A 2
O15A O 0.8220(16) 0.6042(17) 0.7509(13) 0.078(5) Uani 0.258(18) 1 d D . P A 2
H15C H 0.8126 0.5841 0.7948 0.117 Uiso 0.258(18) 1 d R . P A 2
H15D H 0.8349 0.6319 0.7864 0.117 Uiso 0.258(18) 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
Sm1 O1 2.441(6) 2_656 ?
Sm1 O2 2.558(6) 2_656 ?
Sm1 O4 2.448(6) . ?
Sm1 O9 2.510(5) 7_666 ?
Sm1 O11 2.386(6) 7_666 ?
Sm1 O13 2.350(6) . ?
Sm1 O15 2.469(9) . ?
Sm1 O16 2.505(11) . ?
Sm1 O17 2.451(11) . ?
Sm1 C7 2.873(7) 2_656 ?
Sm1 O17A 2.441(14) . ?
Sm1 O15A 2.455(15) . ?
Sm2 O3 2.522(5) 7_666 ?
Sm2 O4 2.544(5) 7_666 ?
Sm2 O5 2.477(6) 3 ?
Sm2 O6 2.598(6) 3 ?
Sm2 O8 2.373(5) . ?
Sm2 O9 2.427(6) . ?
Sm2 O14 2.411(6) 7_666 ?
Sm2 O18 2.420(7) . ?
Sm2 O19 2.460(7) . ?
Sm2 C8 2.883(7) 7_666 ?
Sm2 C9 2.912(7) 3 ?
O1 Sm1 2.442(6) 2_656 ?
O1 C7 1.257(10) . ?
O2 Sm1 2.558(6) 2_656 ?
O2 C7 1.251(10) . ?
O3 Sm2 2.522(5) 7_666 ?
O3 C8 1.258(9) . ?
O4 Sm2 2.544(5) 7_666 ?
O4 C8 1.259(9) . ?
O5 Sm2 2.477(6) 3_445 ?
O5 C9 1.264(9) . ?
O6 Sm2 2.598(6) 3_445 ?
O6 C9 1.254(9) . ?
O7 C31 1.221(11) . ?
O8 C31 1.259(10) . ?
O9 Sm1 2.510(5) 7_666 ?
O9 C32 1.289(10) . ?
O10 C32 1.227(10) . ?
O11 Sm1 2.386(6) 7_666 ?
O11 C33 1.257(11) . ?
O12 C33 1.245(12) . ?
O13 C34 1.252(10) . ?
O14 Sm2 2.410(6) 7_666 ?
O14 C34 1.256(10) . ?
O15 H15A 0.9956 . ?
O15 H15B 0.9956 . ?
O16 H16A 0.8856 . ?
O16 H16B 0.8856 . ?
O17 H17A 0.8953 . ?
O17 H17B 0.8964 . ?
O18 H18A 0.8509 . ?
O18 H18B 0.8510 . ?
O19 H19A 0.8870 . ?
O19 H19B 0.8869 . ?
N1 C10 1.336(11) . ?
N1 C14 1.343(11) . ?
N2 C15 1.306(18) . ?
N2 C19 1.34(2) . ?
N3 C20 1.371(18) . ?
N3 C24 1.317(17) . ?
C1 C2 1.402(10) . ?
C1 C6 1.389(10) . ?
C1 C7 1.516(10) . ?
C2 C3 1.410(10) . ?
C2 C12 1.494(11) . ?
C3 C4 1.389(10) . ?
C3 C8 1.500(10) . ?
C4 H4 0.9300 . ?
C4 C5 1.388(10) . ?
C5 C6 1.382(10) . ?
C5 C9 1.487(10) . ?
C6 H6 0.9300 . ?
C7 Sm1 2.873(7) 2_656 ?
C8 Sm2 2.884(7) 7_666 ?
C9 Sm2 2.912(7) 3_445 ?
C10 C11 1.385(11) . ?
C10 C17 1.498(11) . ?
C11 H11 0.9300 . ?
C11 C12 1.399(11) . ?
C12 C13 1.368(11) . ?
C13 H13 0.9300 . ?
C13 C14 1.388(12) . ?
C14 C22 1.485(12) . ?
C15 H15 0.9300 . ?
C15 C16 1.382(14) . ?
C16 H16 0.9300 . ?
C16 C17 1.367(14) . ?
C17 C18 1.382(15) . ?
C18 H18 0.9300 . ?
C18 C19 1.372(18) . ?
C19 H19 0.9300 . ?
C20 H20 0.9300 . ?
C20 C21 1.387(17) . ?
C21 H21 0.9300 . ?
C21 C22 1.340(16) . ?
C22 C23 1.356(15) . ?
C23 H23 0.9300 . ?
C23 C24 1.380(15) . ?
C24 H24 0.9300 . ?
C25 C26 1.400(11) . ?
C25 C30 1.383(11) . ?
C25 C31 1.496(11) . ?
C26 C27 1.390(11) . ?
C26 C32 1.518(11) . ?
C27 C28 1.385(12) . ?
C27 C33 1.502(12) . ?
C28 H28 0.9300 . ?
C28 C29 1.388(11) . ?
C29 C30 1.384(11) . ?
C29 C34 1.506(10) . ?
C30 H30 0.9300 . ?
O17A H17C 1.0091 . ?
O17A H17D 1.0039 . ?
O15A H15C 1.0671 . ?
O15A H15D 1.0662 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Sm1 O2 51.55(19) 2_656 2_656 ?
O1 Sm1 O4 87.3(2) 2_656 . ?
O1 Sm1 O9 139.2(2) 2_656 7_666 ?
O1 Sm1 O15 83.1(4) 2_656 . ?
O1 Sm1 O16 69.4(4) 2_656 . ?
O1 Sm1 O17 72.3(4) 2_656 . ?
O1 Sm1 C7 25.8(2) 2_656 2_656 ?
O1 Sm1 O15A 67.6(9) 2_656 . ?
O2 Sm1 C7 25.8(2) 2_656 2_656 ?
O4 Sm1 O2 73.53(19) . 2_656 ?
O4 Sm1 O9 67.14(18) . 7_666 ?
O4 Sm1 O15 139.2(4) . . ?
O4 Sm1 O16 138.8(6) . . ?
O4 Sm1 O17 71.6(6) . . ?
O4 Sm1 C7 79.43(19) . 2_656 ?
O4 Sm1 O15A 151.2(8) . . ?
O9 Sm1 O2 136.96(19) 7_666 2_656 ?
O9 Sm1 C7 145.7(2) 7_666 2_656 ?
O11 Sm1 O1 133.4(2) 7_666 2_656 ?
O11 Sm1 O2 140.4(2) 7_666 2_656 ?
O11 Sm1 O4 136.20(19) 7_666 . ?
O11 Sm1 O9 70.2(2) 7_666 7_666 ?
O11 Sm1 O15 72.5(3) 7_666 . ?
O11 Sm1 O16 65.8(4) 7_666 . ?
O11 Sm1 O17 102.3(5) 7_666 . ?
O11 Sm1 C7 144.0(2) 7_666 2_656 ?
O11 Sm1 O17A 87.3(8) 7_666 . ?
O11 Sm1 O15A 72.3(8) 7_666 . ?
O13 Sm1 O1 130.5(2) . 2_656 ?
O13 Sm1 O2 78.98(19) . 2_656 ?
O13 Sm1 O4 78.0(2) . . ?
O13 Sm1 O9 76.46(19) . 7_666 ?
O13 Sm1 O11 83.1(2) . 7_666 ?
O13 Sm1 O15 78.6(5) . . ?
O13 Sm1 O16 142.9(5) . . ?
O13 Sm1 O17 141.0(5) . . ?
O13 Sm1 C7 104.8(2) . 2_656 ?
O13 Sm1 O17A 153.6(6) . . ?
O13 Sm1 O15A 107.1(13) . . ?
O15 Sm1 O2 69.5(3) . 2_656 ?
O15 Sm1 O9 137.0(3) . 7_666 ?
O15 Sm1 O16 73.0(7) . . ?
O15 Sm1 C7 74.9(3) . 2_656 ?
O16 Sm1 O2 111.8(5) . 2_656 ?
O16 Sm1 O9 109.1(5) . 7_666 ?
O16 Sm1 C7 90.6(4) . 2_656 ?
O17 Sm1 O2 113.8(4) . 2_656 ?
O17 Sm1 O9 69.6(4) . 7_666 ?
O17 Sm1 O15 140.1(6) . . ?
O17 Sm1 O16 69.1(8) . . ?
O17 Sm1 C7 93.2(4) . 2_656 ?
O17A Sm1 O1 72.6(6) . 2_656 ?
O17A Sm1 O2 122.2(7) . 2_656 ?
O17A Sm1 O4 92.5(9) . . ?
O17A Sm1 O9 77.1(6) . 7_666 ?
O17A Sm1 O16 48.9(10) . . ?
O17A Sm1 C7 97.4(7) . 2_656 ?
O17A Sm1 O15A 93.2(15) . . ?
O15A Sm1 O2 79.6(9) . 2_656 ?
O15A Sm1 O9 141.6(8) . 7_666 ?
O15A Sm1 O16 45.6(13) . . ?
O15A Sm1 C7 71.8(8) . 2_656 ?
O3 Sm2 O4 51.13(18) 7_666 7_666 ?
O3 Sm2 O6 124.32(18) 7_666 3 ?
O3 Sm2 C8 25.8(2) 7_666 7_666 ?
O3 Sm2 C9 99.82(19) 7_666 3 ?
O4 Sm2 O6 108.73(19) 7_666 3 ?
O4 Sm2 C8 25.9(2) 7_666 7_666 ?
O4 Sm2 C9 88.00(19) 7_666 3 ?
O5 Sm2 O3 74.84(19) 3 7_666 ?
O5 Sm2 O4 68.21(18) 3 7_666 ?
O5 Sm2 O6 51.02(18) 3 3 ?
O5 Sm2 C8 65.62(19) 3 7_666 ?
O5 Sm2 C9 25.54(19) 3 3 ?
O6 Sm2 C8 115.69(19) 3 7_666 ?
O6 Sm2 C9 25.50(19) 3 3 ?
O8 Sm2 O3 160.6(2) . 7_666 ?
O8 Sm2 O4 138.96(18) . 7_666 ?
O8 Sm2 O5 122.8(2) . 3 ?
O8 Sm2 O6 71.95(19) . 3 ?
O8 Sm2 O9 73.41(19) . . ?
O8 Sm2 O14 86.3(2) . 7_666 ?
O8 Sm2 O18 76.6(2) . . ?
O8 Sm2 O19 97.3(2) . . ?
O8 Sm2 C8 163.0(2) . 7_666 ?
O8 Sm2 C9 97.3(2) . 3 ?
O9 Sm2 O3 117.65(18) . 7_666 ?
O9 Sm2 O4 66.91(18) . 7_666 ?
O9 Sm2 O5 89.9(2) . 3 ?
O9 Sm2 O6 78.4(2) . 3 ?
O9 Sm2 O19 150.2(2) . . ?
O9 Sm2 C8 92.8(2) . 7_666 ?
O9 Sm2 C9 82.9(2) . 3 ?
O14 Sm2 O3 81.6(2) 7_666 7_666 ?
O14 Sm2 O4 74.74(18) 7_666 7_666 ?
O14 Sm2 O5 142.94(19) 7_666 3 ?
O14 Sm2 O6 150.3(2) 7_666 3 ?
O14 Sm2 O9 76.1(2) 7_666 . ?
O14 Sm2 O18 66.8(2) 7_666 . ?
O14 Sm2 O19 132.5(2) 7_666 . ?
O14 Sm2 C8 80.7(2) 7_666 7_666 ?
O14 Sm2 C9 156.8(2) 7_666 3 ?
O18 Sm2 O3 84.7(2) . 7_666 ?
O18 Sm2 O4 125.0(2) . 7_666 ?
O18 Sm2 O5 136.7(3) . 3 ?
O18 Sm2 O6 124.3(2) . 3 ?
O18 Sm2 O9 133.3(2) . . ?
O18 Sm2 O19 68.1(2) . . ?
O18 Sm2 C8 107.7(2) . 7_666 ?
O18 Sm2 C9 136.4(2) . 3 ?
O19 Sm2 O3 80.2(2) . 7_666 ?
O19 Sm2 O4 122.4(2) . 7_666 ?
O19 Sm2 O5 71.0(2) . 3 ?
O19 Sm2 O6 71.7(2) . 3 ?
O19 Sm2 C8 99.5(3) . 7_666 ?
O19 Sm2 C9 70.0(2) . 3 ?
C8 Sm2 C9 90.5(2) 7_666 3 ?
C7 O1 Sm1 96.7(5) . 2_656 ?
C7 O2 Sm1 91.3(4) . 2_656 ?
C8 O3 Sm2 93.4(4) . 7_666 ?
Sm1 O4 Sm2 110.84(19) . 7_666 ?
C8 O4 Sm1 154.6(5) . . ?
C8 O4 Sm2 92.3(4) . 7_666 ?
C9 O5 Sm2 96.8(4) . 3_445 ?
C9 O6 Sm2 91.4(5) . 3_445 ?
C31 O8 Sm2 139.7(5) . . ?
Sm2 O9 Sm1 112.7(2) . 7_666 ?
C32 O9 Sm1 122.7(5) . 7_666 ?
C32 O9 Sm2 120.7(5) . . ?
C33 O11 Sm1 146.7(7) . 7_666 ?
C34 O13 Sm1 138.1(5) . . ?
C34 O14 Sm2 138.3(6) . 7_666 ?
Sm1 O15 H15A 115.5 . . ?
Sm1 O15 H15B 115.0 . . ?
H15A O15 H15B 98.3 . . ?
Sm1 O16 H16A 128.0 . . ?
Sm1 O16 H16B 127.2 . . ?
H16A O16 H16B 104.8 . . ?
Sm1 O17 H17A 111.9 . . ?
Sm1 O17 H17B 111.6 . . ?
H17A O17 H17B 102.4 . . ?
Sm2 O18 H18A 109.5 . . ?
Sm2 O18 H18B 109.6 . . ?
H18A O18 H18B 104.4 . . ?
Sm2 O19 H19A 110.7 . . ?
Sm2 O19 H19B 111.3 . . ?
H19A O19 H19B 102.7 . . ?
C14 N1 C10 118.7(7) . . ?
C15 N2 C19 118.6(11) . . ?
C24 N3 C20 117.7(11) . . ?
C2 C1 C7 122.6(7) . . ?
C6 C1 C2 120.4(7) . . ?
C6 C1 C7 117.0(6) . . ?
C1 C2 C3 117.8(7) . . ?
C1 C2 C12 124.1(6) . . ?
C3 C2 C12 118.1(6) . . ?
C2 C3 C8 124.5(7) . . ?
C4 C3 C2 120.3(7) . . ?
C4 C3 C8 115.1(6) . . ?
C3 C4 H4 119.3 . . ?
C5 C4 C3 121.5(7) . . ?
C5 C4 H4 119.3 . . ?
C4 C5 C9 119.8(6) . . ?
C6 C5 C4 118.1(7) . . ?
C6 C5 C9 121.9(7) . . ?
C1 C6 H6 119.1 . . ?
C5 C6 C1 121.7(7) . . ?
C5 C6 H6 119.1 . . ?
O1 C7 Sm1 57.6(4) . 2_656 ?
O1 C7 O2 120.5(7) . . ?
O1 C7 C1 117.2(7) . . ?
O2 C7 Sm1 62.9(4) . 2_656 ?
O2 C7 C1 122.3(7) . . ?
C1 C7 Sm1 174.3(5) . 2_656 ?
O3 C8 Sm2 60.8(4) . 7_666 ?
O3 C8 O4 120.6(7) . . ?
O3 C8 C3 120.0(7) . . ?
O4 C8 Sm2 61.8(4) . 7_666 ?
O4 C8 C3 119.1(7) . . ?
C3 C8 Sm2 159.6(5) . 7_666 ?
O5 C9 Sm2 57.6(4) . 3_445 ?
O5 C9 C5 118.9(7) . . ?
O6 C9 Sm2 63.1(4) . 3_445 ?
O6 C9 O5 120.7(7) . . ?
O6 C9 C5 120.4(7) . . ?
C5 C9 Sm2 175.7(5) . 3_445 ?
N1 C10 C11 122.7(7) . . ?
N1 C10 C17 115.0(8) . . ?
C11 C10 C17 122.1(8) . . ?
C10 C11 H11 120.6 . . ?
C10 C11 C12 118.8(7) . . ?
C12 C11 H11 120.6 . . ?
C11 C12 C2 121.3(7) . . ?
C13 C12 C2 120.7(7) . . ?
C13 C12 C11 118.0(7) . . ?
C12 C13 H13 119.8 . . ?
C12 C13 C14 120.5(8) . . ?
C14 C13 H13 119.8 . . ?
N1 C14 C13 121.4(8) . . ?
N1 C14 C22 115.5(8) . . ?
C13 C14 C22 123.0(8) . . ?
N2 C15 H15 119.0 . . ?
N2 C15 C16 122.0(12) . . ?
C16 C15 H15 119.0 . . ?
C15 C16 H16 120.0 . . ?
C17 C16 C15 120.0(11) . . ?
C17 C16 H16 120.0 . . ?
C16 C17 C10 122.1(8) . . ?
C16 C17 C18 118.1(9) . . ?
C18 C17 C10 119.6(9) . . ?
C17 C18 H18 120.8 . . ?
C19 C18 C17 118.4(13) . . ?
C19 C18 H18 120.8 . . ?
N2 C19 C18 122.9(14) . . ?
N2 C19 H19 118.6 . . ?
C18 C19 H19 118.6 . . ?
N3 C20 H20 119.8 . . ?
N3 C20 C21 120.5(13) . . ?
C21 C20 H20 119.8 . . ?
C20 C21 H21 119.2 . . ?
C22 C21 C20 121.6(12) . . ?
C22 C21 H21 119.2 . . ?
C21 C22 C14 122.8(9) . . ?
C21 C22 C23 116.3(10) . . ?
C23 C22 C14 120.9(9) . . ?
C22 C23 H23 118.9 . . ?
C22 C23 C24 122.2(11) . . ?
C24 C23 H23 118.9 . . ?
N3 C24 C23 121.3(12) . . ?
N3 C24 H24 119.3 . . ?
C23 C24 H24 119.3 . . ?
C26 C25 C31 121.7(7) . . ?
C30 C25 C26 119.7(7) . . ?
C30 C25 C31 118.6(7) . . ?
C25 C26 C32 121.2(7) . . ?
C27 C26 C25 119.0(7) . . ?
C27 C26 C32 119.5(7) . . ?
C26 C27 C33 120.9(8) . . ?
C28 C27 C26 120.2(8) . . ?
C28 C27 C33 118.9(8) . . ?
C27 C28 H28 119.4 . . ?
C27 C28 C29 121.2(7) . . ?
C29 C28 H28 119.4 . . ?
C28 C29 C30 118.2(7) . . ?
C28 C29 C34 122.1(7) . . ?
C30 C29 C34 119.6(7) . . ?
C25 C30 C29 121.6(8) . . ?
C25 C30 H30 119.2 . . ?
C29 C30 H30 119.2 . . ?
O7 C31 O8 123.6(8) . . ?
O7 C31 C25 117.8(8) . . ?
O8 C31 C25 118.6(7) . . ?
O9 C32 C26 117.8(7) . . ?
O10 C32 O9 124.2(8) . . ?
O10 C32 C26 118.0(7) . . ?
O11 C33 C27 118.7(8) . . ?
O12 C33 O11 122.4(9) . . ?
O12 C33 C27 118.8(9) . . ?
O13 C34 C29 117.5(7) . . ?
O14 C34 O13 125.8(7) . . ?
O14 C34 C29 116.6(7) . . ?
Sm1 O17A H17C 116.1 . . ?
Sm1 O17A H17D 115.3 . . ?
H17C O17A H17D 97.9 . . ?
Sm1 O15A H15C 117.2 . . ?
Sm1 O15A H15D 118.5 . . ?
H15C O15A H15D 95.5 . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.266
_oxdiff_exptl_absorpt_empirical_full_min 0.840
_exptl_crystal_preparation       Luminescent
####################################################################### 
# 
# 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_sypl71-gd-porous_sq_s
_database_code_depnum_ccdc_archive 'CCDC 2117148'
loop_
_audit_author_name
_audit_author_address
'SHANG '
; Luoyang Normal University, 
China
;
_audit_update_record             
;
2021-10-21 deposited with the CCDC.	2022-06-01 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT417_sypl71-gd-porous_sq_s 
;
PROBLEM: Short Inter D-H..H-D       H3A      ..H16A     .       1.79 Ang.
RESPONSE: This is due to  the disordered O atoms, large number water molecules. 
;
# Added during the CSD deposition process: Thursday 21 October 2021 02:21 AM
# end Validation Reply Form

_audit_creation_date             2021-08-26
_audit_creation_method           
;
Olex2 1.2
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5335)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C34 H23 Gd2 N3 O18'
_chemical_formula_sum            'C34 H22 Gd2 N3 O18'
_chemical_formula_weight         1075.04
_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                   17.5877(12)
_cell_length_b                   31.5073(11)
_cell_length_c                   17.9802(7)
_cell_angle_alpha                90
_cell_angle_beta                 107.005(5)
_cell_angle_gamma                90
_cell_volume                     9527.9(9)
_cell_formula_units_Z            8
_cell_measurement_reflns_used    4232
_cell_measurement_temperature    293.7(3)
_cell_measurement_theta_max      22.2950
_cell_measurement_theta_min      3.5100
_shelx_estimated_absorpt_T_max   0.827
_shelx_estimated_absorpt_T_min   0.728
_exptl_absorpt_coefficient_mu    2.825
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.81396
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.499
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             4152
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.07
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0893
_diffrn_reflns_av_unetI/netI     0.1680
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.970
_diffrn_reflns_limit_h_max       ?
_diffrn_reflns_limit_h_min       ?
_diffrn_reflns_limit_k_max       ?
_diffrn_reflns_limit_k_min       ?
_diffrn_reflns_limit_l_max       ?
_diffrn_reflns_limit_l_min       ?
_diffrn_reflns_number            9462
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.970
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.372
_diffrn_reflns_theta_min         3.453
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      293.7(3)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0584
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.970
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -28.00  45.00   1.00   17.50    --  -13.80  57.00 -90.00   73
  2  ω    -18.00  52.00   1.00   17.50    --  -13.80  57.00 150.00   70
  3  ω    -20.00  14.00   1.00   17.50    --  -13.80 -99.00 -60.00   34
  4  ω     25.00  70.00   1.00   17.50    --   14.74  38.00-120.00   45
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Single source at offset/far, EosS2'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0344144000
_diffrn_orient_matrix_UB_12      0.0112048000
_diffrn_orient_matrix_UB_13      0.0016356000
_diffrn_orient_matrix_UB_21      0.0223613000
_diffrn_orient_matrix_UB_22      0.0190803000
_diffrn_orient_matrix_UB_23      0.0079182000
_diffrn_orient_matrix_UB_31      -0.0095814000
_diffrn_orient_matrix_UB_32      0.0041893000
_diffrn_orient_matrix_UB_33      -0.0404657000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                5586
_reflns_number_total             9462
_reflns_odcompleteness_completeness 99.65
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     25.30
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    ?
_refine_diff_density_max         1.971
_refine_diff_density_min         -0.741
_refine_diff_density_rms         0.179
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.965
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     518
_refine_ls_number_reflns         9462
_refine_ls_number_restraints     12
_refine_ls_R_factor_all          0.1224
_refine_ls_R_factor_gt           0.0703
_refine_ls_restrained_S_all      0.965
_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)+(0.0419P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1224
_refine_ls_wR_factor_ref         0.1423
_refine_special_details          Twin,SQUEEZE
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
 At 1.5 times of:
  All O(H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C11) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C7) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
3.a Rotating group:
 O15(H15A,H15B), O16(H16A,H16B), O17(H17A,H17B), O18(H18A,H18B)
3.b Aromatic/amide H refined with riding coordinates:
 C13(H13), C15(H15), C5(H5), C3(H3), C20(H20), C23(H23), C30(H30), C28(H28),
 N3(H3A), C25(H25), C31(H31), C27(H27), C26(H26), C33(H33), C32(H32)
;
_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
Gd1 Gd 0.05238(3) 0.12654(2) 0.41185(3) 0.02230(15) Uani 1 1 d . . . . .
Gd2 Gd 0.28897(3) 0.39189(2) 0.37462(3) 0.02861(16) Uani 1 1 d . . . . .
O9 O 0.4275(4) 0.3952(2) 0.4483(3) 0.0269(16) Uani 1 1 d . . . . .
O1 O 0.1887(4) 0.1129(2) 0.4821(3) 0.0292(17) Uani 1 1 d . . . . .
O10 O 0.5481(4) 0.3753(2) 0.5142(3) 0.0262(16) Uani 1 1 d . . . . .
O8 O 0.4065(4) 0.3100(2) 0.5153(4) 0.0366(19) Uani 1 1 d . . . . .
O7 O 0.3176(4) 0.3206(2) 0.3999(4) 0.0351(19) Uani 1 1 d . . . . .
O5 O 0.1263(4) 0.1511(2) 0.3315(3) 0.0323(18) Uani 1 1 d . . . . .
O11 O 0.5226(5) 0.5511(2) 0.4223(4) 0.039(2) Uani 1 1 d . . . . .
O12 O 0.5871(5) 0.5620(2) 0.3377(4) 0.040(2) Uani 1 1 d . . . . .
O14 O 0.6331(4) 0.3763(2) 0.2214(3) 0.0311(18) Uani 1 1 d . . . . .
O15 O -0.0653(5) 0.1078(2) 0.3063(4) 0.049(2) Uani 1 1 d . . . . .
H15A H -0.055950 0.086347 0.277349 0.074 Uiso 1 1 d GR . . . .
H15B H -0.078811 0.128894 0.271548 0.074 Uiso 1 1 d GR . . . .
O3 O 0.3322(4) 0.1248(2) 0.5996(4) 0.044(2) Uani 1 1 d . . . . .
C11 C 0.5010(6) 0.3934(3) 0.4575(5) 0.018(2) Uani 1 1 d . U . . .
O16 O -0.0209(5) 0.1890(2) 0.3521(4) 0.056(2) Uani 1 1 d . . . . .
H16A H -0.063902 0.194730 0.369975 0.084 Uiso 1 1 d GR . . . .
H16B H -0.045443 0.184963 0.299999 0.084 Uiso 1 1 d GR . . . .
C12 C 0.5342(5) 0.4196(3) 0.4024(5) 0.021(2) Uani 1 1 d . . . . .
C18 C 0.5561(6) 0.5373(3) 0.3745(5) 0.025(2) Uani 1 1 d . . . . .
O13 O 0.6805(5) 0.4399(2) 0.2184(4) 0.058(3) Uani 1 1 d . . . . .
O2 O 0.2803(5) 0.0964(2) 0.4235(4) 0.052(2) Uani 1 1 d . . . . .
C00K C 0.6425(6) 0.4135(3) 0.2447(5) 0.026(2) Uani 1 1 d . . . . .
C10 C 0.3515(6) 0.2977(3) 0.4581(6) 0.029(3) Uani 1 1 d . . . . .
C13 C 0.5251(6) 0.4629(3) 0.4046(5) 0.023(2) Uani 1 1 d . . . . .
H13 H 0.495375 0.474338 0.434819 0.028 Uiso 1 1 calc R . . . .
C14 C 0.5595(5) 0.4897(3) 0.3628(5) 0.019(2) Uani 1 1 d . . . . .
C15 C 0.5973(6) 0.4723(3) 0.3130(5) 0.024(2) Uani 1 1 d . . . . .
H15 H 0.617636 0.490128 0.282297 0.029 Uiso 1 1 calc R . . . .
N2 N 0.6278(6) 0.2686(3) 0.3811(5) 0.036(2) Uani 1 1 d . . . . .
C4 C 0.3263(6) 0.2515(3) 0.4561(5) 0.028(3) Uani 1 1 d . . . . .
C5 C 0.2627(6) 0.2378(3) 0.3964(5) 0.028(3) Uani 1 1 d . . . . .
H5 H 0.237291 0.256564 0.357091 0.033 Uiso 1 1 calc R . . . .
C2 C 0.3363(6) 0.1827(3) 0.5151(5) 0.023(2) Uani 1 1 d . . . . .
O6 O 0.1556(6) 0.2034(3) 0.2651(4) 0.085(4) Uani 1 1 d . . . . .
C16 C 0.6057(6) 0.4287(3) 0.3075(5) 0.024(2) Uani 1 1 d . . . . .
C8 C 0.2460(7) 0.1221(3) 0.4523(6) 0.034(3) Uani 1 1 d . . . . .
O17 O 0.1996(6) 0.3649(4) 0.2566(4) 0.132(6) Uani 1 1 d . . . . .
H17A H 0.173607 0.340449 0.252177 0.198 Uiso 1 1 d GR . . . .
H17B H 0.187390 0.377522 0.210554 0.198 Uiso 1 1 d GR . . . .
C7 C 0.1669(7) 0.1830(4) 0.3248(5) 0.036(3) Uani 1 1 d . U . . .
C6 C 0.2357(6) 0.1963(3) 0.3939(5) 0.028(3) Uani 1 1 d . . . . .
C17 C 0.5780(6) 0.4016(3) 0.3548(5) 0.024(2) Uani 1 1 d . . . . .
C3 C 0.3628(6) 0.2241(3) 0.5138(5) 0.028(3) Uani 1 1 d . . . . .
H3 H 0.406713 0.233263 0.553386 0.034 Uiso 1 1 calc R . . . .
C20 C 0.6716(6) 0.3410(3) 0.3827(5) 0.026(2) Uani 1 1 d . . . . .
H20 H 0.713540 0.360036 0.390282 0.031 Uiso 1 1 calc R . . . .
O18 O 0.2924(9) 0.4611(3) 0.4218(6) 0.162(7) Uani 1 1 d . . . . .
H18A H 0.333846 0.483853 0.421357 0.242 Uiso 1 1 d GR . . . .
H18B H 0.252890 0.474578 0.447032 0.242 Uiso 1 1 d GR . . . .
C23 C 0.5352(6) 0.3254(3) 0.3507(5) 0.025(2) Uani 1 1 d . . . . .
H23 H 0.482440 0.334248 0.337277 0.029 Uiso 1 1 calc R . . . .
C19 C 0.5946(6) 0.3546(3) 0.3622(5) 0.029(3) Uani 1 1 d . . . . .
C22 C 0.5532(7) 0.2828(3) 0.3590(5) 0.031(3) Uani 1 1 d . . . . .
C1 C 0.2721(6) 0.1676(3) 0.4546(5) 0.026(2) Uani 1 1 d . . . . .
O4 O 0.4467(5) 0.1579(3) 0.6138(6) 0.098(4) Uani 1 1 d . . . . .
C9 C 0.3746(7) 0.1543(4) 0.5809(6) 0.044(3) Uani 1 1 d . . . . .
C30 C 0.4141(7) 0.2574(4) 0.3050(6) 0.039(3) Uani 1 1 d . . . . .
H30 H 0.396118 0.285169 0.295584 0.047 Uiso 1 1 calc R . . . .
C24 C 0.7680(8) 0.2796(4) 0.4122(7) 0.046(3) Uani 1 1 d . . . . .
C21 C 0.6850(8) 0.2973(4) 0.3920(6) 0.044(3) Uani 1 1 d . . . . .
N1 N 0.3826(10) 0.1825(4) 0.2981(8) 0.087(4) Uani 1 1 d . . . . .
C29 C 0.4917(8) 0.2482(4) 0.3423(6) 0.045(3) Uani 1 1 d . . . . .
C28 C 0.7832(8) 0.2381(5) 0.4183(7) 0.070(5) Uani 1 1 d . . . . .
H28 H 0.739319 0.220523 0.412619 0.084 Uiso 1 1 calc R . . . .
N3 N 0.9182(9) 0.2442(5) 0.4396(7) 0.097(5) Uani 1 1 d . . . . .
H3A H 0.964241 0.232747 0.447386 0.117 Uiso 1 1 calc R . . . .
C25 C 0.8315(9) 0.3040(5) 0.4245(10) 0.093(6) Uani 1 1 d . . . . .
H25 H 0.825475 0.333269 0.426182 0.112 Uiso 1 1 calc R . . . .
C31 C 0.3623(9) 0.2223(6) 0.2812(7) 0.074(5) Uani 1 1 d . . . . .
H31 H 0.310322 0.227807 0.251670 0.088 Uiso 1 1 calc R . . . .
C27 C 0.8525(10) 0.2185(6) 0.4313(9) 0.097(6) Uani 1 1 d . . . . .
H27 H 0.856741 0.189103 0.434615 0.116 Uiso 1 1 calc R . . . .
C26 C 0.9115(11) 0.2864(6) 0.4357(10) 0.110(7) Uani 1 1 d . . . . .
H26 H 0.955318 0.303749 0.439880 0.132 Uiso 1 1 calc R . . . .
C33 C 0.5114(9) 0.2069(4) 0.3611(8) 0.077(5) Uani 1 1 d . . . . .
H33 H 0.561892 0.200364 0.393298 0.092 Uiso 1 1 calc R . . . .
C32 C 0.4587(12) 0.1752(5) 0.3336(10) 0.098(6) Uani 1 1 d . . . . .
H32 H 0.476655 0.147326 0.339896 0.118 Uiso 1 1 calc R . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Gd1 Gd2 4.0739(7) 7_556 ?
Gd1 O9 2.528(6) 7_556 ?
Gd1 O1 2.399(7) . ?
Gd1 O10 2.504(6) 7_556 ?
Gd1 O8 2.384(6) 7_556 ?
Gd1 O5 2.339(6) . ?
Gd1 O11 2.454(7) 3_445 ?
Gd1 O12 2.601(7) 3_445 ?
Gd1 O15 2.437(7) . ?
Gd1 C11 2.843(9) 7_556 ?
Gd1 O16 2.424(7) . ?
Gd1 C18 2.897(10) 3_445 ?
Gd2 O9 2.411(6) . ?
Gd2 O1 2.495(6) 7_556 ?
Gd2 O7 2.316(7) . ?
Gd2 O14 2.547(6) 2_655 ?
Gd2 O3 2.368(8) 7_556 ?
Gd2 O13 2.430(7) 2_655 ?
Gd2 C00K 2.834(10) 2_655 ?
Gd2 O17 2.397(8) . ?
Gd2 O18 2.334(10) . ?
O9 C11 1.256(11) . ?
O1 C8 1.306(12) . ?
O10 C11 1.248(10) . ?
O8 C10 1.250(11) . ?
O7 C10 1.269(11) . ?
O5 C7 1.258(11) . ?
O11 C18 1.254(11) . ?
O12 C18 1.246(11) . ?
O14 C00K 1.241(11) . ?
O15 H15A 0.8980 . ?
O15 H15B 0.8953 . ?
O3 C9 1.296(12) . ?
C11 C12 1.530(12) . ?
O16 H16A 0.9212 . ?
O16 H16B 0.9189 . ?
C12 C13 1.375(12) . ?
C12 C17 1.427(12) . ?
C18 C14 1.518(12) . ?
O13 C00K 1.243(11) . ?
O2 C8 1.212(12) . ?
C00K C16 1.534(13) . ?
C10 C4 1.517(13) . ?
C13 H13 0.9300 . ?
C13 C14 1.382(11) . ?
C14 C15 1.375(12) . ?
C15 H15 0.9300 . ?
C15 C16 1.387(12) . ?
N2 C22 1.332(13) . ?
N2 C21 1.323(14) . ?
C4 C5 1.375(12) . ?
C4 C3 1.358(13) . ?
C5 H5 0.9300 . ?
C5 C6 1.387(13) . ?
C2 C3 1.387(12) . ?
C2 C1 1.402(12) . ?
C2 C9 1.480(14) . ?
O6 C7 1.217(11) . ?
C16 C17 1.390(12) . ?
C8 C1 1.501(13) . ?
O17 H17A 0.8866 . ?
O17 H17B 0.8868 . ?
C7 C6 1.519(13) . ?
C6 C1 1.417(13) . ?
C17 C19 1.507(13) . ?
C3 H3 0.9300 . ?
C20 H20 0.9300 . ?
C20 C19 1.363(13) . ?
C20 C21 1.399(13) . ?
O18 H18A 1.0247 . ?
O18 H18B 1.0264 . ?
C23 H23 0.9300 . ?
C23 C19 1.362(13) . ?
C23 C22 1.378(13) . ?
C22 C29 1.503(15) . ?
O4 C9 1.238(12) . ?
C30 H30 0.9300 . ?
C30 C29 1.365(15) . ?
C30 C31 1.415(16) . ?
C24 C21 1.505(16) . ?
C24 C28 1.332(16) . ?
C24 C25 1.321(17) . ?
N1 C31 1.314(17) . ?
N1 C32 1.324(18) . ?
C29 C33 1.364(16) . ?
C28 H28 0.9300 . ?
C28 C27 1.324(18) . ?
N3 H3A 0.8600 . ?
N3 C27 1.382(18) . ?
N3 C26 1.334(17) . ?
C25 H25 0.9300 . ?
C25 C26 1.47(2) . ?
C31 H31 0.9300 . ?
C27 H27 0.9300 . ?
C26 H26 0.9300 . ?
C33 H33 0.9300 . ?
C33 C32 1.352(18) . ?
C32 H32 0.9300 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O9 Gd1 Gd2 33.52(15) 7_556 7_556 ?
O9 Gd1 O12 108.2(2) 7_556 3_445 ?
O9 Gd1 C11 26.2(2) 7_556 7_556 ?
O9 Gd1 C18 87.8(2) 7_556 3_445 ?
O1 Gd1 Gd2 34.40(14) . 7_556 ?
O1 Gd1 O9 66.4(2) . 7_556 ?
O1 Gd1 O10 117.9(2) . 7_556 ?
O1 Gd1 O11 89.4(2) . 3_445 ?
O1 Gd1 O12 77.3(2) . 3_445 ?
O1 Gd1 O15 149.0(2) . . ?
O1 Gd1 C11 92.6(2) . 7_556 ?
O1 Gd1 O16 134.3(2) . . ?
O1 Gd1 C18 82.0(2) . 3_445 ?
O10 Gd1 Gd2 83.79(14) 7_556 7_556 ?
O10 Gd1 O9 51.8(2) 7_556 7_556 ?
O10 Gd1 O12 124.2(2) 7_556 3_445 ?
O10 Gd1 C11 26.0(2) 7_556 7_556 ?
O10 Gd1 C18 99.6(3) 7_556 3_445 ?
O8 Gd1 Gd2 65.64(16) 7_556 7_556 ?
O8 Gd1 O9 75.5(2) 7_556 7_556 ?
O8 Gd1 O1 76.4(2) 7_556 . ?
O8 Gd1 O10 82.9(2) 7_556 7_556 ?
O8 Gd1 O11 143.9(2) 7_556 3_445 ?
O8 Gd1 O12 149.2(2) 7_556 3_445 ?
O8 Gd1 O15 133.1(3) 7_556 . ?
O8 Gd1 C11 81.5(2) 7_556 7_556 ?
O8 Gd1 O16 66.4(2) 7_556 . ?
O8 Gd1 C18 156.6(2) 7_556 3_445 ?
O5 Gd1 Gd2 106.14(15) . 7_556 ?
O5 Gd1 O9 139.6(2) . 7_556 ?
O5 Gd1 O1 74.6(2) . . ?
O5 Gd1 O10 160.3(2) . 7_556 ?
O5 Gd1 O8 85.8(2) . 7_556 ?
O5 Gd1 O11 122.5(2) . 3_445 ?
O5 Gd1 O12 71.7(2) . 3_445 ?
O5 Gd1 O15 95.6(2) . . ?
O5 Gd1 C11 163.8(2) . 7_556 ?
O5 Gd1 O16 77.1(3) . . ?
O5 Gd1 C18 97.1(3) . 3_445 ?
O11 Gd1 Gd2 83.83(16) 3_445 7_556 ?
O11 Gd1 O9 68.4(2) 3_445 7_556 ?
O11 Gd1 O10 74.7(2) 3_445 7_556 ?
O11 Gd1 O12 50.9(2) 3_445 3_445 ?
O11 Gd1 C11 66.0(2) 3_445 7_556 ?
O11 Gd1 C18 25.4(2) 3_445 3_445 ?
O12 Gd1 Gd2 99.94(16) 3_445 7_556 ?
O12 Gd1 C11 115.7(2) 3_445 7_556 ?
O12 Gd1 C18 25.5(2) 3_445 3_445 ?
O15 Gd1 Gd2 153.03(18) . 7_556 ?
O15 Gd1 O9 123.3(2) . 7_556 ?
O15 Gd1 O10 80.6(2) . 7_556 ?
O15 Gd1 O11 70.9(2) . 3_445 ?
O15 Gd1 O12 71.6(2) . 3_445 ?
O15 Gd1 C11 100.3(3) . 7_556 ?
O15 Gd1 C18 69.9(3) . 3_445 ?
C11 Gd1 Gd2 59.4(2) 7_556 7_556 ?
C11 Gd1 C18 90.7(3) 7_556 3_445 ?
O16 Gd1 Gd2 131.45(18) . 7_556 ?
O16 Gd1 O9 124.2(2) . 7_556 ?
O16 Gd1 O10 83.5(2) . 7_556 ?
O16 Gd1 O11 136.3(3) . 3_445 ?
O16 Gd1 O12 125.6(2) . 3_445 ?
O16 Gd1 O15 68.3(2) . . ?
O16 Gd1 C11 106.5(3) . 7_556 ?
O16 Gd1 C18 136.9(3) . 3_445 ?
C18 Gd1 Gd2 91.41(18) 3_445 7_556 ?
O9 Gd2 Gd1 35.38(14) . 7_556 ?
O9 Gd2 O1 66.8(2) . 7_556 ?
O9 Gd2 O14 73.9(2) . 2_655 ?
O9 Gd2 O13 87.7(3) . 2_655 ?
O9 Gd2 C00K 79.7(2) . 2_655 ?
O1 Gd2 Gd1 32.90(16) 7_556 7_556 ?
O1 Gd2 O14 137.3(2) 7_556 2_655 ?
O1 Gd2 C00K 145.3(2) 7_556 2_655 ?
O7 Gd2 Gd1 68.13(16) . 7_556 ?
O7 Gd2 O9 78.9(2) . . ?
O7 Gd2 O1 77.3(2) . 7_556 ?
O7 Gd2 O14 79.4(2) . 2_655 ?
O7 Gd2 O3 84.4(3) . 7_556 ?
O7 Gd2 O13 131.3(2) . 2_655 ?
O7 Gd2 C00K 105.4(3) . 2_655 ?
O7 Gd2 O17 83.0(4) . . ?
O7 Gd2 O18 148.5(3) . . ?
O14 Gd2 Gd1 104.79(15) 2_655 7_556 ?
O14 Gd2 C00K 26.0(2) 2_655 2_655 ?
O3 Gd2 Gd1 101.03(16) 7_556 7_556 ?
O3 Gd2 O9 136.4(2) 7_556 . ?
O3 Gd2 O1 70.3(2) 7_556 7_556 ?
O3 Gd2 O14 141.6(2) 7_556 2_655 ?
O3 Gd2 O13 131.7(3) 7_556 2_655 ?
O3 Gd2 C00K 143.9(2) 7_556 2_655 ?
O3 Gd2 O17 72.5(3) 7_556 . ?
O13 Gd2 Gd1 120.6(2) 2_655 7_556 ?
O13 Gd2 O1 138.5(2) 2_655 7_556 ?
O13 Gd2 O14 51.9(2) 2_655 2_655 ?
O13 Gd2 C00K 25.9(2) 2_655 2_655 ?
C00K Gd2 Gd1 114.94(19) 2_655 7_556 ?
O17 Gd2 Gd1 151.0(3) . 7_556 ?
O17 Gd2 O9 142.9(3) . . ?
O17 Gd2 O1 139.2(3) . 7_556 ?
O17 Gd2 O14 71.0(3) . 2_655 ?
O17 Gd2 O13 80.3(3) . 2_655 ?
O17 Gd2 C00K 74.3(3) . 2_655 ?
O18 Gd2 Gd1 81.5(3) . 7_556 ?
O18 Gd2 O9 81.1(4) . . ?
O18 Gd2 O1 72.6(3) . 7_556 ?
O18 Gd2 O14 117.7(3) . 2_655 ?
O18 Gd2 O3 93.7(4) . 7_556 ?
O18 Gd2 O13 71.4(3) . 2_655 ?
O18 Gd2 C00K 94.5(3) . 2_655 ?
O18 Gd2 O17 126.4(5) . . ?
Gd2 O9 Gd1 111.1(2) . 7_556 ?
C11 O9 Gd1 91.0(5) . 7_556 ?
C11 O9 Gd2 155.0(6) . . ?
Gd1 O1 Gd2 112.7(3) . 7_556 ?
C8 O1 Gd1 121.1(6) . . ?
C8 O1 Gd2 122.0(6) . 7_556 ?
C11 O10 Gd1 92.4(6) . 7_556 ?
C10 O8 Gd1 138.6(7) . 7_556 ?
C10 O7 Gd2 137.5(6) . . ?
C7 O5 Gd1 139.2(7) . . ?
C18 O11 Gd1 97.4(6) . 3 ?
C18 O12 Gd1 90.7(6) . 3 ?
C00K O14 Gd2 90.0(6) . 2_655 ?
Gd1 O15 H15A 112.1 . . ?
Gd1 O15 H15B 110.8 . . ?
H15A O15 H15B 102.1 . . ?
C9 O3 Gd2 145.9(8) . 7_556 ?
O9 C11 Gd1 62.8(5) . 7_556 ?
O9 C11 C12 117.6(8) . . ?
O10 C11 Gd1 61.6(5) . 7_556 ?
O10 C11 O9 122.7(9) . . ?
O10 C11 C12 119.2(9) . . ?
C12 C11 Gd1 159.2(6) . 7_556 ?
Gd1 O16 H16A 112.9 . . ?
Gd1 O16 H16B 111.7 . . ?
H16A O16 H16B 101.2 . . ?
C13 C12 C11 116.6(8) . . ?
C13 C12 C17 119.9(9) . . ?
C17 C12 C11 123.3(8) . . ?
O11 C18 Gd1 57.2(5) . 3 ?
O11 C18 C14 118.9(9) . . ?
O12 C18 Gd1 63.9(5) . 3 ?
O12 C18 O11 120.9(9) . . ?
O12 C18 C14 120.2(9) . . ?
C14 C18 Gd1 174.8(6) . 3 ?
C00K O13 Gd2 95.5(6) . 2_655 ?
O14 C00K Gd2 64.0(5) . 2_655 ?
O14 C00K O13 122.6(9) . . ?
O14 C00K C16 120.0(9) . . ?
O13 C00K Gd2 58.6(5) . 2_655 ?
O13 C00K C16 117.4(9) . . ?
C16 C00K Gd2 175.7(7) . 2_655 ?
O8 C10 O7 124.4(10) . . ?
O8 C10 C4 117.9(9) . . ?
O7 C10 C4 117.6(9) . . ?
C12 C13 H13 119.4 . . ?
C12 C13 C14 121.2(9) . . ?
C14 C13 H13 119.4 . . ?
C13 C14 C18 119.1(8) . . ?
C15 C14 C18 122.0(8) . . ?
C15 C14 C13 118.9(9) . . ?
C14 C15 H15 119.3 . . ?
C14 C15 C16 121.5(9) . . ?
C16 C15 H15 119.3 . . ?
C21 N2 C22 117.1(9) . . ?
C5 C4 C10 119.0(9) . . ?
C3 C4 C10 121.5(9) . . ?
C3 C4 C5 119.4(9) . . ?
C4 C5 H5 119.5 . . ?
C4 C5 C6 120.9(9) . . ?
C6 C5 H5 119.5 . . ?
C3 C2 C1 120.3(9) . . ?
C3 C2 C9 120.4(9) . . ?
C1 C2 C9 119.3(9) . . ?
C15 C16 C00K 116.0(8) . . ?
C15 C16 C17 120.1(9) . . ?
C17 C16 C00K 123.8(9) . . ?
O1 C8 C1 117.9(9) . . ?
O2 C8 O1 124.5(10) . . ?
O2 C8 C1 117.6(11) . . ?
Gd2 O17 H17A 125.1 . . ?
Gd2 O17 H17B 125.7 . . ?
H17A O17 H17B 109.2 . . ?
O5 C7 C6 118.7(9) . . ?
O6 C7 O5 123.8(10) . . ?
O6 C7 C6 117.5(10) . . ?
C5 C6 C7 118.0(9) . . ?
C5 C6 C1 120.2(9) . . ?
C1 C6 C7 121.8(9) . . ?
C12 C17 C19 117.6(8) . . ?
C16 C17 C12 118.0(9) . . ?
C16 C17 C19 124.4(9) . . ?
C4 C3 C2 121.7(9) . . ?
C4 C3 H3 119.2 . . ?
C2 C3 H3 119.2 . . ?
C19 C20 H20 121.3 . . ?
C19 C20 C21 117.5(10) . . ?
C21 C20 H20 121.3 . . ?
Gd2 O18 H18A 126.4 . . ?
Gd2 O18 H18B 126.8 . . ?
H18A O18 H18B 106.8 . . ?
C19 C23 H23 120.0 . . ?
C19 C23 C22 119.9(10) . . ?
C22 C23 H23 120.0 . . ?
C20 C19 C17 119.0(9) . . ?
C23 C19 C17 121.9(10) . . ?
C23 C19 C20 119.1(10) . . ?
N2 C22 C23 122.3(9) . . ?
N2 C22 C29 113.9(11) . . ?
C23 C22 C29 123.7(11) . . ?
C2 C1 C8 121.1(9) . . ?
C2 C1 C6 117.4(9) . . ?
C6 C1 C8 121.4(9) . . ?
O3 C9 C2 118.6(10) . . ?
O4 C9 O3 121.9(11) . . ?
O4 C9 C2 119.3(10) . . ?
C29 C30 H30 121.8 . . ?
C29 C30 C31 116.5(13) . . ?
C31 C30 H30 121.8 . . ?
C28 C24 C21 122.7(13) . . ?
C25 C24 C21 122.5(13) . . ?
C25 C24 C28 114.7(13) . . ?
N2 C21 C20 124.0(11) . . ?
N2 C21 C24 115.1(11) . . ?
C20 C21 C24 120.8(12) . . ?
C31 N1 C32 116.4(15) . . ?
C30 C29 C22 120.2(11) . . ?
C33 C29 C22 121.8(12) . . ?
C33 C29 C30 118.0(12) . . ?
C24 C28 H28 115.7 . . ?
C27 C28 C24 128.5(16) . . ?
C27 C28 H28 115.7 . . ?
C27 N3 H3A 119.3 . . ?
C26 N3 H3A 119.3 . . ?
C26 N3 C27 121.3(16) . . ?
C24 C25 H25 119.0 . . ?
C24 C25 C26 122.1(15) . . ?
C26 C25 H25 119.0 . . ?
C30 C31 H31 117.7 . . ?
N1 C31 C30 124.6(16) . . ?
N1 C31 H31 117.7 . . ?
C28 C27 N3 116.3(18) . . ?
C28 C27 H27 121.8 . . ?
N3 C27 H27 121.8 . . ?
N3 C26 C25 116.7(16) . . ?
N3 C26 H26 121.7 . . ?
C25 C26 H26 121.7 . . ?
C29 C33 H33 119.5 . . ?
C32 C33 C29 121.0(16) . . ?
C32 C33 H33 119.5 . . ?
N1 C32 C33 122.5(16) . . ?
N1 C32 H32 118.8 . . ?
C33 C32 H32 118.8 . . ?

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
Gd1 O9 C11 O10 15.1(9) 7_556 . . . ?
Gd1 O9 C11 C12 -156.5(7) 7_556 . . . ?
Gd1 O1 C8 O2 -102.1(11) . . . . ?
Gd1 O1 C8 C1 78.7(10) . . . . ?
Gd1 O10 C11 O9 -15.3(9) 7_556 . . . ?
Gd1 O10 C11 C12 156.2(7) 7_556 . . . ?
Gd1 O8 C10 O7 33.5(16) 7_556 . . . ?
Gd1 O8 C10 C4 -149.8(7) 7_556 . . . ?
Gd1 O5 C7 O6 -126.3(11) . . . . ?
Gd1 O5 C7 C6 55.6(16) . . . . ?
Gd1 O11 C18 O12 -3.0(10) 3 . . . ?
Gd1 O11 C18 C14 176.0(7) 3 . . . ?
Gd1 O12 C18 O11 2.8(10) 3 . . . ?
Gd1 O12 C18 C14 -176.2(8) 3 . . . ?
Gd1 C11 C12 C13 -23(2) 7_556 . . . ?
Gd1 C11 C12 C17 151.7(15) 7_556 . . . ?
Gd2 O9 C11 Gd1 -152.8(15) . . . 7_556 ?
Gd2 O9 C11 O10 -137.6(11) . . . . ?
Gd2 O9 C11 C12 50.7(18) . . . . ?
Gd2 O1 C8 O2 102.7(10) 7_556 . . . ?
Gd2 O1 C8 C1 -76.6(10) 7_556 . . . ?
Gd2 O7 C10 O8 -29.5(16) . . . . ?
Gd2 O7 C10 C4 153.8(7) . . . . ?
Gd2 O14 C00K O13 -1.0(10) 2_655 . . . ?
Gd2 O14 C00K C16 178.3(8) 2_655 . . . ?
Gd2 O3 C9 C2 -47.5(18) 7_556 . . . ?
Gd2 O3 C9 O4 136.3(12) 7_556 . . . ?
Gd2 O13 C00K O14 1.1(11) 2_655 . . . ?
Gd2 O13 C00K C16 -178.3(7) 2_655 . . . ?
O9 C11 C12 C13 62.1(11) . . . . ?
O9 C11 C12 C17 -122.8(10) . . . . ?
O1 C8 C1 C2 94.6(12) . . . . ?
O1 C8 C1 C6 -89.0(12) . . . . ?
O10 C11 C12 C13 -109.9(10) . . . . ?
O10 C11 C12 C17 65.3(12) . . . . ?
O8 C10 C4 C5 176.0(9) . . . . ?
O8 C10 C4 C3 -1.0(15) . . . . ?
O7 C10 C4 C5 -7.1(14) . . . . ?
O7 C10 C4 C3 176.0(10) . . . . ?
O5 C7 C6 C5 -158.7(10) . . . . ?
O5 C7 C6 C1 21.2(16) . . . . ?
O11 C18 C14 C13 0.5(13) . . . . ?
O11 C18 C14 C15 -178.1(9) . . . . ?
O12 C18 C14 C13 179.5(9) . . . . ?
O12 C18 C14 C15 1.0(14) . . . . ?
O14 C00K C16 C15 -160.7(9) . . . . ?
O14 C00K C16 C17 16.2(14) . . . . ?
C11 C12 C13 C14 173.8(8) . . . . ?
C11 C12 C17 C16 -179.5(8) . . . . ?
C11 C12 C17 C19 -2.5(13) . . . . ?
C12 C13 C14 C18 -172.8(8) . . . . ?
C12 C13 C14 C15 5.8(14) . . . . ?
C12 C17 C19 C20 -121.6(10) . . . . ?
C12 C17 C19 C23 56.9(12) . . . . ?
C18 C14 C15 C16 174.6(8) . . . . ?
O13 C00K C16 C15 18.7(13) . . . . ?
O13 C00K C16 C17 -164.4(10) . . . . ?
O2 C8 C1 C2 -84.7(12) . . . . ?
O2 C8 C1 C6 91.7(12) . . . . ?
C00K C16 C17 C12 -170.5(9) . . . . ?
C00K C16 C17 C19 12.7(14) . . . . ?
C10 C4 C5 C6 -177.5(9) . . . . ?
C10 C4 C3 C2 175.2(9) . . . . ?
C13 C12 C17 C16 -4.5(13) . . . . ?
C13 C12 C17 C19 172.6(8) . . . . ?
C13 C14 C15 C16 -3.9(14) . . . . ?
C14 C15 C16 C00K 174.8(9) . . . . ?
C14 C15 C16 C17 -2.2(15) . . . . ?
C15 C16 C17 C12 6.3(13) . . . . ?
C15 C16 C17 C19 -170.5(9) . . . . ?
N2 C22 C29 C30 -167.2(10) . . . . ?
N2 C22 C29 C33 10.4(16) . . . . ?
C4 C5 C6 C7 -178.0(9) . . . . ?
C4 C5 C6 C1 2.1(15) . . . . ?
C5 C4 C3 C2 -1.7(16) . . . . ?
C5 C6 C1 C2 -1.3(14) . . . . ?
C5 C6 C1 C8 -178.0(10) . . . . ?
O6 C7 C6 C5 23.1(16) . . . . ?
O6 C7 C6 C1 -157.0(11) . . . . ?
C16 C17 C19 C20 55.2(13) . . . . ?
C16 C17 C19 C23 -126.3(11) . . . . ?
C7 C6 C1 C2 178.7(9) . . . . ?
C7 C6 C1 C8 2.1(15) . . . . ?
C17 C12 C13 C14 -1.6(14) . . . . ?
C3 C4 C5 C6 -0.5(15) . . . . ?
C3 C2 C1 C8 175.8(10) . . . . ?
C3 C2 C1 C6 -0.8(14) . . . . ?
C3 C2 C9 O3 150.4(10) . . . . ?
C3 C2 C9 O4 -33.3(17) . . . . ?
C23 C22 C29 C30 11.3(15) . . . . ?
C23 C22 C29 C33 -171.0(11) . . . . ?
C19 C20 C21 N2 0.9(16) . . . . ?
C19 C20 C21 C24 178.1(9) . . . . ?
C19 C23 C22 N2 2.7(15) . . . . ?
C19 C23 C22 C29 -175.7(9) . . . . ?
C22 N2 C21 C20 0.9(17) . . . . ?
C22 N2 C21 C24 -176.5(9) . . . . ?
C22 C23 C19 C17 -179.3(8) . . . . ?
C22 C23 C19 C20 -0.7(14) . . . . ?
C22 C29 C33 C32 -167.9(14) . . . . ?
C1 C2 C3 C4 2.4(15) . . . . ?
C1 C2 C9 O3 -28.7(15) . . . . ?
C1 C2 C9 O4 147.6(12) . . . . ?
C9 C2 C3 C4 -176.7(10) . . . . ?
C9 C2 C1 C8 -5.1(14) . . . . ?
C9 C2 C1 C6 178.3(9) . . . . ?
C30 C29 C33 C32 10(2) . . . . ?
C24 C28 C27 N3 0(3) . . . . ?
C24 C25 C26 N3 -6(3) . . . . ?
C21 N2 C22 C23 -2.7(15) . . . . ?
C21 N2 C22 C29 175.9(9) . . . . ?
C21 C20 C19 C17 177.6(8) . . . . ?
C21 C20 C19 C23 -0.9(14) . . . . ?
C21 C24 C28 C27 175.9(14) . . . . ?
C21 C24 C25 C26 -173.1(14) . . . . ?
C29 C30 C31 N1 5.6(18) . . . . ?
C29 C33 C32 N1 -11(3) . . . . ?
C28 C24 C21 N2 0.4(18) . . . . ?
C28 C24 C21 C20 -177.0(11) . . . . ?
C28 C24 C25 C26 6(2) . . . . ?
C25 C24 C21 N2 179.7(13) . . . . ?
C25 C24 C21 C20 2(2) . . . . ?
C25 C24 C28 C27 -3(2) . . . . ?
C31 C30 C29 C22 170.9(9) . . . . ?
C31 C30 C29 C33 -6.9(16) . . . . ?
C31 N1 C32 C33 9(3) . . . . ?
C27 N3 C26 C25 2(3) . . . . ?
C26 N3 C27 C28 1(3) . . . . ?
C32 N1 C31 C30 -6(2) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.369
_oxdiff_exptl_absorpt_empirical_full_min 0.722

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 0.000 0.277 0.250 45 18 ' '
2 0.000 0.500 0.509 1520 519 ' '
3 0.000 0.723 0.750 45 18 ' '
4 0.500 0.000 0.274 1520 519 ' '
5 0.500 0.223 0.750 45 18 ' '
6 0.500 0.777 0.250 45 18 ' '
_platon_squeeze_details          ?
_exptl_crystal_preparation       Luminescent
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_l71-eu
_database_code_depnum_ccdc_archive 'CCDC 2117147'
loop_
_audit_author_name
_audit_author_address
'SHANG '
; Luoyang Normal University, 
China
;
_audit_update_record             
;
2021-10-21 deposited with the CCDC.	2022-06-01 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_SHFSU01_l71-eu              
;
PROBLEM: The absolute value of parameter shift to su ratio > 0.20
RESPONSE: This is due to large void in crystal, and the disordered O and C atoms
;
_vrf_PLAT080_l71-eu              
;
PROBLEM: Maximum Shift/Error ............................       0.39 Why ?
RESPONSE: Thisthis is due to  the disordered O and C atoms, it can be solvated by more refinement.
;
_vrf_PLAT211_l71-eu              
;
PROBLEM: ADP of Atom C25       is N.P.D. or (nearly) 2D .     Please Check
RESPONSE: this is due to  the disordered  C atoms.
;
_vrf_PLAT305_l71-eu              
;
PROBLEM: Isolated Hydrogen Atom   (Outside Bond Range ??)       H1WA Check
RESPONSE: this is due to large number water molecules.
;
_vrf_PLAT355_l71-eu              
;
PROBLEM: Long   O-H (X0.82,N0.98A)  O5W      - H5WA     .       1.22 Ang.
RESPONSE: this is due to large number water molecules. 
;
_vrf_PLAT602_l71-eu              
;
PROBLEM: Solvent Accessible VOID(S) in Structure ........          ! Check
RESPONSE: This is due to large void in crystal, 
;
# Added during the CSD deposition process: Thursday 21 October 2021 02:21 AM
# end Validation Reply Form

_audit_creation_date             2021-10-16
_audit_creation_method           
;
Olex2 1.5
(compiled 2021.08.20 svn.r13c46975 for OlexSys, GUI svn.r6405)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C34 H25 Eu2 N3 O19'
_chemical_formula_sum            'C34 H25 Eu2 N3 O19'
_chemical_formula_weight         1083.49
_chemical_melting_point          ?
_chemical_oxdiff_formula         C1H1O1N1Eu1
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                   17.5969(12)
_cell_length_b                   31.6237(15)
_cell_length_c                   18.0245(15)
_cell_angle_alpha                90
_cell_angle_beta                 107.037(8)
_cell_angle_gamma                90
_cell_volume                     9590.1(12)
_cell_formula_units_Z            8
_cell_measurement_reflns_used    3377
_cell_measurement_temperature    291.07(10)
_cell_measurement_theta_max      21.5940
_cell_measurement_theta_min      3.5230
_shelx_estimated_absorpt_T_max   0.741
_shelx_estimated_absorpt_T_min   0.691
_exptl_absorpt_coefficient_mu    2.660
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.81098
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.501
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             4224
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.12
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.1112
_diffrn_reflns_av_unetI/netI     0.1907
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       37
_diffrn_reflns_limit_k_min       -36
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            20658
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_min         3.441
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      291.07(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0584
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -78.00 -41.00   1.00   22.08    --  -13.80 178.00 -30.00   37
  2  ω    -86.00 -42.00   1.00   22.08    --  -13.80 178.00-120.00   44
  3  ω    -16.00  20.00   1.00   22.08    --  -13.80 -99.00  60.00   36
  4  ω     -1.00  68.00   1.00   22.08    --   14.74  19.00 -60.00   69
  5  ω      8.00  44.00   1.00   22.08    --   14.74  57.00-120.00   36
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Single source at offset/far, EosS2'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0005708000
_diffrn_orient_matrix_UB_12      -0.0028836000
_diffrn_orient_matrix_UB_13      0.0388572000
_diffrn_orient_matrix_UB_21      0.0117842000
_diffrn_orient_matrix_UB_22      0.0213486000
_diffrn_orient_matrix_UB_23      0.0083856000
_diffrn_orient_matrix_UB_31      -0.0404666000
_diffrn_orient_matrix_UB_32      0.0062589000
_diffrn_orient_matrix_UB_33      -0.0106641000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4794
_reflns_number_total             8434
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_refine_diff_density_max         3.136
_refine_diff_density_min         -1.018
_refine_diff_density_rms         0.271
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.330
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     528
_refine_ls_number_reflns         8434
_refine_ls_number_restraints     6
_refine_ls_R_factor_all          0.1698
_refine_ls_R_factor_gt           0.0938
_refine_ls_restrained_S_all      1.330
_refine_ls_shift/su_max          0.394
_refine_ls_shift/su_mean         0.005
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0700P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2230
_refine_ls_wR_factor_ref         0.2420
_refine_special_details          Twin,SQUEEZE
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
 At 1.5 times of:
  All O(H,H) groups
2. Restrained distances
 C10-C13 = C13-C18 = C18-C17 = C17-C11 = C11-N3 = N3-C10
 1.38 with sigma of 0.02
3.a Rotating group:
 O1W(H1WA,H1WB), O2W(H2WA,H2WB), O3W(H3WA,H3WB), O4W(H4WA,H4WB), O5W(H5WA,H5WB)
3.b Aromatic/amide H refined with riding coordinates:
 N3(H3), C4(H4), C7(H7), C8(H8), C9(H9), C10(H10), C11(H11), C13(H13),
 C14(H14), C15(H15), C16(H16), C17(H17), C25(H25), C26(H26), C27(H27)
;
_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
Eu1 Eu 0.94746(5) 0.12670(3) 0.58774(5) 0.0189(3) Uani 1 1 d . . . . .
Eu2 Eu 0.71270(5) 0.39219(3) 0.62643(5) 0.0253(3) Uani 1 1 d . . . . .
O1W O 0.8262(13) 0.4425(9) 0.6833(18) 0.186(15) Uani 1 1 d . . . . .
H1WA H 0.832628 0.474924 0.734175 0.279 Uiso 1 1 d R U . . .
H1WB H 0.898718 0.445383 0.671686 0.279 Uiso 1 1 d R U . . .
O1 O 0.8100(7) 0.1132(4) 0.5172(6) 0.029(3) Uani 1 1 d . . . . .
O2 O 0.7194(7) 0.0974(4) 0.5760(8) 0.045(4) Uani 1 1 d . . . . .
O2W O 0.7982(8) 0.3620(7) 0.7435(9) 0.092(7) Uani 1 1 d . . . . .
H2WA H 0.838214 0.376664 0.786122 0.138 Uiso 1 1 d R U . . .
H2WB H 0.801605 0.332024 0.760322 0.138 Uiso 1 1 d R U . . .
O3 O 0.6671(7) 0.1265(4) 0.3990(8) 0.038(3) Uani 1 1 d . . . . .
O3W O 1.0226(8) 0.1890(4) 0.6468(9) 0.048(4) Uani 1 1 d . . . . .
H3WA H 1.036286 0.186476 0.696590 0.072 Uiso 1 1 d R U . . .
H3WB H 1.067324 0.189901 0.636213 0.072 Uiso 1 1 d R U . . .
O4W O 1.0650(8) 0.1092(4) 0.6950(8) 0.050(4) Uani 1 1 d . . . . .
H4WA H 1.084854 0.131869 0.719379 0.076 Uiso 1 1 d R U . . .
H4WB H 1.051362 0.094479 0.729241 0.076 Uiso 1 1 d R U . . .
O4 O 0.5527(8) 0.1593(5) 0.3862(11) 0.084(6) Uani 1 1 d . . . . .
O5 O 0.8724(6) 0.1510(4) 0.6675(7) 0.026(3) Uani 1 1 d . . . . .
O6 O 0.8449(9) 0.2039(5) 0.7356(9) 0.070(5) Uani 1 1 d . . . . .
O7 O 0.5941(7) 0.3102(4) 0.4853(7) 0.030(3) Uani 1 1 d . . . . .
O8 O 0.6845(7) 0.3214(4) 0.6014(7) 0.029(3) Uani 1 1 d . . . . .
O9 O 0.5717(6) 0.3961(3) 0.5523(7) 0.021(3) Uani 1 1 d . . . . .
O10 O 0.4513(7) 0.3764(4) 0.4856(7) 0.030(3) Uani 1 1 d . . . . .
O11 O 0.3682(7) 0.3766(4) 0.7787(7) 0.027(3) Uani 1 1 d . . . . .
O12 O 0.3176(8) 0.4395(4) 0.7784(8) 0.043(4) Uani 1 1 d . . . . .
O13 O 0.4766(8) 0.5514(4) 0.5769(8) 0.042(4) Uani 1 1 d . . . . .
O14 O 0.4136(7) 0.5616(4) 0.6604(8) 0.036(4) Uani 1 1 d . . . . .
N1 N 0.6219(16) 0.1859(9) 0.7054(17) 0.077(8) Uani 1 1 d . . . . .
N2 N 0.3711(9) 0.2692(5) 0.6181(9) 0.031(4) Uani 1 1 d . . . . .
N3 N 0.0818(14) 0.2454(8) 0.5613(15) 0.099(9) Uani 1 1 d D . . . .
H3 H 0.036236 0.234523 0.558631 0.119 Uiso 1 1 calc R U . . .
C1 C 0.4061(10) 0.3556(6) 0.6388(10) 0.025(5) Uani 1 1 d . . . . .
C2 C 0.6254(12) 0.1553(7) 0.4189(12) 0.040(6) Uani 1 1 d . . . . .
C3 C 0.4455(11) 0.2833(6) 0.6374(11) 0.032(5) Uani 1 1 d . . . . .
C4 C 0.3256(10) 0.3412(6) 0.6159(11) 0.027(5) Uani 1 1 d . . . . .
H4 H 0.283453 0.360104 0.607400 0.033 Uiso 1 1 calc R U . . .
C5 C 0.6641(10) 0.1839(6) 0.4846(11) 0.026(4) Uani 1 1 d . . . . .
C6 C 0.4425(9) 0.4896(5) 0.6367(10) 0.017(4) Uani 1 1 d . . . . .
C7 C 0.5866(11) 0.2574(6) 0.6955(11) 0.029(5) Uani 1 1 d . . . . .
H7 H 0.604007 0.285045 0.706793 0.034 Uiso 1 1 calc R U . . .
C8 C 0.4644(11) 0.3260(6) 0.6484(10) 0.026(5) Uani 1 1 d . . . . .
H8 H 0.517391 0.334342 0.662560 0.031 Uiso 1 1 calc R U . . .
C9 C 0.6358(9) 0.2242(6) 0.4873(10) 0.022(4) Uani 1 1 d . . . . .
H9 H 0.591012 0.232843 0.448391 0.027 Uiso 1 1 calc R U . . .
C10 C 0.0922(19) 0.2884(9) 0.565(3) 0.19(2) Uani 1 1 d D . . . .
H10 H 0.048624 0.306217 0.558131 0.225 Uiso 1 1 calc R U . . .
C11 C 0.1460(15) 0.2197(9) 0.5620(18) 0.102(11) Uani 1 1 d D . . . .
H11 H 0.139873 0.190979 0.550677 0.122 Uiso 1 1 calc R U . . .
O5W O 0.6956(15) 0.4622(5) 0.5697(11) 0.125(10) Uani 1 1 d . . . . .
H5WA H 0.732662 0.479880 0.531025 0.188 Uiso 1 1 d R U . . .
H5WB H 0.647301 0.489539 0.571704 0.188 Uiso 1 1 d R U . . .
C13 C 0.1677(15) 0.3052(8) 0.579(2) 0.107(14) Uani 1 1 d D . . . .
H13 H 0.173811 0.334438 0.583796 0.128 Uiso 1 1 calc R U . . .
C14 C 0.547(3) 0.1801(10) 0.663(2) 0.113(13) Uani 1 1 d . . . . .
H14 H 0.531501 0.152610 0.647111 0.136 Uiso 1 1 calc R U . . .
C15 C 0.4913(15) 0.2100(8) 0.6402(18) 0.075(9) Uani 1 1 d . . . . .
H15 H 0.439287 0.202902 0.612953 0.090 Uiso 1 1 calc R U . . .
C16 C 0.6398(15) 0.2239(11) 0.7191(15) 0.065(8) Uani 1 1 d . . . . .
H16 H 0.691938 0.230360 0.746801 0.078 Uiso 1 1 calc R U . . .
C17 C 0.2183(12) 0.2388(8) 0.5800(15) 0.073(9) Uani 1 1 d D . . . .
H17 H 0.262231 0.221129 0.588239 0.088 Uiso 1 1 calc R U . . .
C18 C 0.2331(12) 0.2811(7) 0.5872(14) 0.049(6) Uani 1 1 d D . . . .
C19 C 0.3120(10) 0.2967(6) 0.6065(12) 0.033(5) Uani 1 1 d . . . . .
C20 C 0.5115(13) 0.2498(6) 0.6572(13) 0.039(6) Uani 1 1 d . . . . .
C21 C 0.4232(9) 0.4019(6) 0.6445(9) 0.017(4) Uani 1 1 d . . . . .
C22 C 0.3943(9) 0.4290(5) 0.6926(10) 0.017(4) Uani 1 1 d . . . . .
C23 C 0.7656(10) 0.1965(6) 0.6074(10) 0.022(4) Uani 1 1 d . . . . .
C24 C 0.7301(9) 0.1691(5) 0.5451(10) 0.019(4) Uani 1 1 d . . . . .
C25 C 0.7394(10) 0.2376(5) 0.6074(10) 0.020(4) Uani 1 1 d . . . . .
H25 H 0.765395 0.255893 0.647152 0.024 Uiso 1 1 calc R U . . .
C26 C 0.4033(9) 0.4721(5) 0.6875(9) 0.020(4) Uani 1 1 d . . . . .
H26 H 0.383130 0.489927 0.718182 0.024 Uiso 1 1 calc R U . . .
C27 C 0.4741(10) 0.4634(5) 0.5961(10) 0.020(4) Uani 1 1 d . . . . .
H27 H 0.502179 0.474831 0.564489 0.024 Uiso 1 1 calc R U . . .
C28 C 0.4447(11) 0.5373(6) 0.6238(11) 0.030(5) Uani 1 1 d . . . . .
C29 C 0.6483(11) 0.2972(6) 0.5420(12) 0.029(5) Uani 1 1 d . . . . .
C30 C 0.8313(12) 0.1832(7) 0.6748(11) 0.037(5) Uani 1 1 d . . . . .
C31 C 0.4671(9) 0.4197(6) 0.5986(9) 0.018(4) Uani 1 1 d . . . . .
C32 C 0.7535(10) 0.1226(5) 0.5472(9) 0.019(4) Uani 1 1 d . . . . .
C33 C 0.6716(9) 0.2525(6) 0.5460(9) 0.020(4) Uani 1 1 d . . . . .
C34 C 0.3570(10) 0.4138(6) 0.7537(9) 0.021(4) Uani 1 1 d . . . . .
C35 C 0.4979(10) 0.3941(6) 0.5424(11) 0.024(4) Uani 1 1 d . . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Eu1 Eu2 4.1021(14) 7_656 ?
Eu1 O1 2.418(12) . ?
Eu1 O3W 2.436(13) . ?
Eu1 O4W 2.445(13) . ?
Eu1 O5 2.348(10) . ?
Eu1 O7 2.384(12) 7_656 ?
Eu1 O9 2.550(11) 7_656 ?
Eu1 O10 2.513(10) 7_656 ?
Eu1 O13 2.455(12) 3_545 ?
Eu1 O14 2.601(12) 3_545 ?
Eu1 C28 2.905(19) 3_545 ?
Eu1 C35 2.862(17) 7_656 ?
Eu2 O1W 2.52(2) . ?
Eu2 O1 2.506(11) 7_656 ?
Eu2 O2W 2.401(16) . ?
Eu2 O3 2.366(12) 7_656 ?
Eu2 O8 2.308(13) . ?
Eu2 O9 2.452(11) . ?
Eu2 O11 2.573(10) 2_656 ?
Eu2 O12 2.450(11) 2_656 ?
Eu2 O5W 2.420(18) . ?
Eu2 C34 2.862(15) 2_656 ?
O1W H1WA 1.3576 . ?
O1W H1WB 1.3551 . ?
O1 C32 1.299(18) . ?
O2 C32 1.204(18) . ?
O2W H2WA 0.9911 . ?
O2W H2WB 0.9929 . ?
O3 C2 1.29(2) . ?
O3W H3WA 0.8619 . ?
O3W H3WB 0.8623 . ?
O4W H4WA 0.8600 . ?
O4W H4WB 0.8604 . ?
O4 C2 1.25(2) . ?
O5 C30 1.28(2) . ?
O6 C30 1.24(2) . ?
O7 C29 1.25(2) . ?
O8 C29 1.32(2) . ?
O9 C35 1.261(18) . ?
O10 C35 1.24(2) . ?
O11 C34 1.255(19) . ?
O12 C34 1.235(19) . ?
O13 C28 1.229(19) . ?
O14 C28 1.24(2) . ?
N1 C14 1.33(4) . ?
N1 C16 1.25(3) . ?
N2 C3 1.33(2) . ?
N2 C19 1.32(2) . ?
N3 H3 0.8600 . ?
N3 C10 1.371(18) . ?
N3 C11 1.390(17) . ?
C1 C4 1.43(2) . ?
C1 C8 1.36(2) . ?
C1 C21 1.49(2) . ?
C2 C5 1.49(3) . ?
C3 C8 1.39(2) . ?
C3 C20 1.53(3) . ?
C4 H4 0.9300 . ?
C4 C19 1.43(2) . ?
C5 C9 1.37(2) . ?
C5 C24 1.42(2) . ?
C6 C26 1.41(2) . ?
C6 C27 1.33(2) . ?
C6 C28 1.53(2) . ?
C7 H7 0.9300 . ?
C7 C16 1.39(3) . ?
C7 C20 1.32(3) . ?
C8 H8 0.9300 . ?
C9 H9 0.9300 . ?
C9 C33 1.39(2) . ?
C10 H10 0.9300 . ?
C10 C13 1.384(19) . ?
C11 H11 0.9300 . ?
C11 C17 1.358(17) . ?
O5W H5WA 1.2209 . ?
O5W H5WB 1.2202 . ?
C13 H13 0.9300 . ?
C13 C18 1.354(17) . ?
C14 H14 0.9300 . ?
C14 C15 1.33(4) . ?
C15 H15 0.9300 . ?
C15 C20 1.32(3) . ?
C16 H16 0.9300 . ?
C17 H17 0.9300 . ?
C17 C18 1.361(17) . ?
C18 C19 1.42(2) . ?
C21 C22 1.42(2) . ?
C21 C31 1.41(2) . ?
C22 C26 1.38(2) . ?
C22 C34 1.51(2) . ?
C23 C24 1.41(2) . ?
C23 C25 1.38(2) . ?
C23 C30 1.47(3) . ?
C24 C32 1.52(2) . ?
C25 H25 0.9300 . ?
C25 C33 1.45(2) . ?
C26 H26 0.9300 . ?
C27 H27 0.9300 . ?
C27 C31 1.39(2) . ?
C29 C33 1.47(2) . ?
C31 C35 1.52(2) . ?

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 Eu2 34.3(2) . 7_656 ?
O1 Eu1 O3W 134.7(4) . . ?
O1 Eu1 O4W 149.3(4) . . ?
O1 Eu1 O9 66.9(3) . 7_656 ?
O1 Eu1 O10 118.1(4) . 7_656 ?
O1 Eu1 O13 89.3(4) . 3_545 ?
O1 Eu1 O14 77.5(4) . 3_545 ?
O1 Eu1 C28 82.3(5) . 3_545 ?
O1 Eu1 C35 93.0(5) . 7_656 ?
O3W Eu1 Eu2 131.6(3) . 7_656 ?
O3W Eu1 O4W 67.2(5) . . ?
O3W Eu1 O9 123.9(4) . 7_656 ?
O3W Eu1 O10 83.3(5) . 7_656 ?
O3W Eu1 O13 136.0(5) . 3_545 ?
O3W Eu1 O14 126.5(5) . 3_545 ?
O3W Eu1 C28 137.0(5) . 3_545 ?
O3W Eu1 C35 105.9(5) . 7_656 ?
O4W Eu1 Eu2 154.1(3) . 7_656 ?
O4W Eu1 O9 123.7(4) . 7_656 ?
O4W Eu1 O10 80.9(4) . 7_656 ?
O4W Eu1 O13 72.3(5) . 3_545 ?
O4W Eu1 O14 71.8(4) . 3_545 ?
O4W Eu1 C28 70.6(5) . 3_545 ?
O4W Eu1 C35 100.8(5) . 7_656 ?
O5 Eu1 Eu2 105.6(3) . 7_656 ?
O5 Eu1 O1 74.0(4) . . ?
O5 Eu1 O3W 78.4(5) . . ?
O5 Eu1 O4W 95.0(4) . . ?
O5 Eu1 O7 85.9(4) . 7_656 ?
O5 Eu1 O9 139.7(4) . 7_656 ?
O5 Eu1 O10 161.4(4) . 7_656 ?
O5 Eu1 O13 122.3(4) . 3_545 ?
O5 Eu1 O14 72.4(4) . 3_545 ?
O5 Eu1 C28 97.6(4) . 3_545 ?
O5 Eu1 C35 164.1(4) . 7_656 ?
O7 Eu1 Eu2 65.6(3) 7_656 7_656 ?
O7 Eu1 O1 76.0(4) 7_656 . ?
O7 Eu1 O3W 66.7(4) 7_656 . ?
O7 Eu1 O4W 132.7(4) 7_656 . ?
O7 Eu1 O9 76.1(4) 7_656 7_656 ?
O7 Eu1 O10 83.8(4) 7_656 7_656 ?
O7 Eu1 O13 143.6(4) 7_656 3_545 ?
O7 Eu1 O14 149.5(4) 7_656 3_545 ?
O7 Eu1 C28 156.3(5) 7_656 3_545 ?
O7 Eu1 C35 82.1(4) 7_656 7_656 ?
O9 Eu1 Eu2 34.1(2) 7_656 7_656 ?
O9 Eu1 O14 106.9(4) 7_656 3_545 ?
O9 Eu1 C28 86.6(4) 7_656 3_545 ?
O9 Eu1 C35 26.1(4) 7_656 7_656 ?
O10 Eu1 Eu2 84.1(3) 7_656 7_656 ?
O10 Eu1 O9 51.5(4) 7_656 7_656 ?
O10 Eu1 O14 122.4(4) 7_656 3_545 ?
O10 Eu1 C28 98.1(4) 7_656 3_545 ?
O10 Eu1 C35 25.7(4) 7_656 7_656 ?
O13 Eu1 Eu2 83.4(3) 3_545 7_656 ?
O13 Eu1 O9 67.5(4) 3_545 7_656 ?
O13 Eu1 O10 73.9(4) 3_545 7_656 ?
O13 Eu1 O14 50.0(4) 3_545 3_545 ?
O13 Eu1 C28 24.7(4) 3_545 3_545 ?
O13 Eu1 C35 65.4(4) 3_545 7_656 ?
O14 Eu1 Eu2 99.4(3) 3_545 7_656 ?
O14 Eu1 C28 25.3(4) 3_545 3_545 ?
O14 Eu1 C35 114.4(4) 3_545 7_656 ?
C28 Eu1 Eu2 91.0(4) 3_545 7_656 ?
C35 Eu1 Eu2 59.9(4) 7_656 7_656 ?
C35 Eu1 C28 89.5(5) 7_656 3_545 ?
O1W Eu2 Eu1 135.8(8) . 7_656 ?
O1W Eu2 O11 112.2(6) . 2_656 ?
O1W Eu2 C34 90.4(6) . 2_656 ?
O1 Eu2 Eu1 32.9(3) 7_656 7_656 ?
O1 Eu2 O1W 109.3(7) 7_656 . ?
O1 Eu2 O11 136.2(4) 7_656 2_656 ?
O1 Eu2 C34 145.3(4) 7_656 2_656 ?
O2W Eu2 Eu1 148.2(5) . 7_656 ?
O2W Eu2 O1W 71.1(10) . . ?
O2W Eu2 O1 138.6(5) . 7_656 ?
O2W Eu2 O9 140.5(5) . . ?
O2W Eu2 O11 70.5(4) . 2_656 ?
O2W Eu2 O12 80.6(6) . 2_656 ?
O2W Eu2 O5W 134.7(8) . . ?
O2W Eu2 C34 74.2(5) . 2_656 ?
O3 Eu2 Eu1 100.8(3) 7_656 7_656 ?
O3 Eu2 O1W 65.8(6) 7_656 . ?
O3 Eu2 O1 70.4(4) 7_656 7_656 ?
O3 Eu2 O2W 72.9(5) 7_656 . ?
O3 Eu2 O9 136.5(4) 7_656 . ?
O3 Eu2 O11 141.3(4) 7_656 2_656 ?
O3 Eu2 O12 132.7(4) 7_656 2_656 ?
O3 Eu2 O5W 98.9(6) 7_656 . ?
O3 Eu2 C34 144.2(5) 7_656 2_656 ?
O8 Eu2 Eu1 68.0(3) . 7_656 ?
O8 Eu2 O1W 142.2(7) . . ?
O8 Eu2 O1 76.8(4) . 7_656 ?
O8 Eu2 O2W 80.2(6) . . ?
O8 Eu2 O3 82.7(4) . 7_656 ?
O8 Eu2 O9 79.5(4) . . ?
O8 Eu2 O11 79.3(4) . 2_656 ?
O8 Eu2 O12 130.6(4) . 2_656 ?
O8 Eu2 O5W 144.2(6) . . ?
O8 Eu2 C34 105.3(5) . 2_656 ?
O9 Eu2 Eu1 35.7(2) . 7_656 ?
O9 Eu2 O1W 138.0(8) . . ?
O9 Eu2 O1 67.1(4) . 7_656 ?
O9 Eu2 O11 72.8(4) . 2_656 ?
O9 Eu2 C34 79.1(4) . 2_656 ?
O11 Eu2 Eu1 103.7(3) 2_656 7_656 ?
O11 Eu2 C34 26.0(4) 2_656 2_656 ?
O12 Eu2 Eu1 121.2(3) 2_656 7_656 ?
O12 Eu2 O1W 68.8(5) 2_656 . ?
O12 Eu2 O1 139.8(4) 2_656 7_656 ?
O12 Eu2 O9 87.6(4) 2_656 . ?
O12 Eu2 O11 51.4(4) 2_656 2_656 ?
O12 Eu2 C34 25.4(4) 2_656 2_656 ?
O5W Eu2 Eu1 76.7(5) . 7_656 ?
O5W Eu2 O1W 65.2(10) . . ?
O5W Eu2 O1 70.4(5) . 7_656 ?
O5W Eu2 O9 75.1(7) . . ?
O5W Eu2 O11 115.6(5) . 2_656 ?
O5W Eu2 O12 73.2(5) . 2_656 ?
O5W Eu2 C34 94.2(5) . 2_656 ?
C34 Eu2 Eu1 114.6(3) 2_656 7_656 ?
Eu2 O1W H1WA 130.5 . . ?
Eu2 O1W H1WB 130.4 . . ?
H1WA O1W H1WB 99.1 . . ?
Eu1 O1 Eu2 112.8(4) . 7_656 ?
C32 O1 Eu1 120.7(10) . . ?
C32 O1 Eu2 122.5(10) . 7_656 ?
Eu2 O2W H2WA 128.0 . . ?
Eu2 O2W H2WB 127.9 . . ?
H2WA O2W H2WB 104.1 . . ?
C2 O3 Eu2 147.9(13) . 7_656 ?
Eu1 O3W H3WA 109.3 . . ?
Eu1 O3W H3WB 110.2 . . ?
H3WA O3W H3WB 103.9 . . ?
Eu1 O4W H4WA 109.8 . . ?
Eu1 O4W H4WB 109.9 . . ?
H4WA O4W H4WB 104.0 . . ?
C30 O5 Eu1 139.5(11) . . ?
C29 O7 Eu1 140.1(13) . 7_656 ?
C29 O8 Eu2 138.3(12) . . ?
Eu2 O9 Eu1 110.2(4) . 7_656 ?
C35 O9 Eu1 90.8(10) . 7_656 ?
C35 O9 Eu2 155.6(11) . . ?
C35 O10 Eu1 93.0(9) . 7_656 ?
C34 O11 Eu2 90.0(9) . 2_656 ?
C34 O12 Eu2 96.3(11) . 2_656 ?
C28 O13 Eu1 98.7(11) . 3_455 ?
C28 O14 Eu1 91.2(11) . 3_455 ?
C16 N1 C14 113(3) . . ?
C19 N2 C3 119.3(16) . . ?
C10 N3 H3 120.6 . . ?
C10 N3 C11 119(2) . . ?
C11 N3 H3 120.6 . . ?
C4 C1 C21 119.8(15) . . ?
C8 C1 C4 117.6(18) . . ?
C8 C1 C21 122.5(15) . . ?
O3 C2 C5 119.2(18) . . ?
O4 C2 O3 122(2) . . ?
O4 C2 C5 118.8(18) . . ?
N2 C3 C8 122.6(18) . . ?
N2 C3 C20 116.8(18) . . ?
C8 C3 C20 120.2(18) . . ?
C1 C4 H4 121.1 . . ?
C19 C4 C1 117.8(16) . . ?
C19 C4 H4 121.1 . . ?
C9 C5 C2 120.4(17) . . ?
C9 C5 C24 120.0(17) . . ?
C24 C5 C2 119.6(17) . . ?
C26 C6 C28 121.7(14) . . ?
C27 C6 C26 118.2(16) . . ?
C27 C6 C28 119.9(14) . . ?
C16 C7 H7 119.9 . . ?
C20 C7 H7 119.9 . . ?
C20 C7 C16 120(2) . . ?
C1 C8 C3 120.6(18) . . ?
C1 C8 H8 119.7 . . ?
C3 C8 H8 119.7 . . ?
C5 C9 H9 118.7 . . ?
C5 C9 C33 122.5(17) . . ?
C33 C9 H9 118.7 . . ?
N3 C10 H10 120.1 . . ?
N3 C10 C13 120(3) . . ?
C13 C10 H10 120.1 . . ?
N3 C11 H11 121.8 . . ?
C17 C11 N3 116(2) . . ?
C17 C11 H11 121.8 . . ?
Eu2 O5W H5WA 129.7 . . ?
Eu2 O5W H5WB 129.6 . . ?
H5WA O5W H5WB 100.7 . . ?
C10 C13 H13 118.6 . . ?
C18 C13 C10 123(2) . . ?
C18 C13 H13 118.6 . . ?
N1 C14 H14 116.8 . . ?
C15 C14 N1 126(3) . . ?
C15 C14 H14 116.8 . . ?
C14 C15 H15 120.6 . . ?
C20 C15 C14 119(3) . . ?
C20 C15 H15 120.6 . . ?
N1 C16 C7 124(3) . . ?
N1 C16 H16 117.9 . . ?
C7 C16 H16 117.9 . . ?
C11 C17 H17 116.6 . . ?
C11 C17 C18 127(2) . . ?
C18 C17 H17 116.6 . . ?
C13 C18 C17 114(2) . . ?
C13 C18 C19 125(2) . . ?
C17 C18 C19 121(2) . . ?
N2 C19 C4 122.1(16) . . ?
N2 C19 C18 118.5(18) . . ?
C18 C19 C4 119.4(17) . . ?
C7 C20 C3 124.8(19) . . ?
C15 C20 C3 118(2) . . ?
C15 C20 C7 117(2) . . ?
C22 C21 C1 122.3(13) . . ?
C31 C21 C1 119.2(14) . . ?
C31 C21 C22 118.4(16) . . ?
C21 C22 C34 124.3(15) . . ?
C26 C22 C21 119.2(14) . . ?
C26 C22 C34 116.4(14) . . ?
C24 C23 C30 122.6(17) . . ?
C25 C23 C24 120.6(16) . . ?
C25 C23 C30 116.8(17) . . ?
C5 C24 C32 119.4(16) . . ?
C23 C24 C5 118.8(16) . . ?
C23 C24 C32 121.2(16) . . ?
C23 C25 H25 119.8 . . ?
C23 C25 C33 120.5(16) . . ?
C33 C25 H25 119.8 . . ?
C6 C26 H26 119.3 . . ?
C22 C26 C6 121.3(15) . . ?
C22 C26 H26 119.3 . . ?
C6 C27 H27 118.4 . . ?
C6 C27 C31 123.2(14) . . ?
C31 C27 H27 118.4 . . ?
O13 C28 Eu1 56.6(9) . 3_455 ?
O13 C28 O14 120.1(18) . . ?
O13 C28 C6 120.1(16) . . ?
O14 C28 Eu1 63.5(10) . 3_455 ?
O14 C28 C6 119.8(15) . . ?
C6 C28 Eu1 176.0(12) . 3_455 ?
O7 C29 O8 123.0(18) . . ?
O7 C29 C33 119.7(19) . . ?
O8 C29 C33 117.2(17) . . ?
O5 C30 C23 118.3(17) . . ?
O6 C30 O5 122.9(19) . . ?
O6 C30 C23 118.8(19) . . ?
C21 C31 C35 122.9(16) . . ?
C27 C31 C21 119.2(14) . . ?
C27 C31 C35 117.2(13) . . ?
O1 C32 C24 116.4(14) . . ?
O2 C32 O1 124.6(16) . . ?
O2 C32 C24 119.0(15) . . ?
C9 C33 C25 117.5(16) . . ?
C9 C33 C29 121.7(16) . . ?
C25 C33 C29 120.4(17) . . ?
O11 C34 Eu2 64.0(8) . 2_656 ?
O11 C34 C22 120.2(14) . . ?
O12 C34 Eu2 58.3(8) . 2_656 ?
O12 C34 O11 122.3(15) . . ?
O12 C34 C22 117.5(16) . . ?
C22 C34 Eu2 175.2(13) . 2_656 ?
O9 C35 Eu1 63.0(9) . 7_656 ?
O9 C35 C31 115.8(17) . . ?
O10 C35 Eu1 61.3(9) . 7_656 ?
O10 C35 O9 122.8(16) . . ?
O10 C35 C31 120.9(15) . . ?
C31 C35 Eu1 160.5(12) . 7_656 ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Eu1 O1 C32 O2 -102.2(19) . . . . ?
Eu1 O1 C32 C24 77.9(16) . . . . ?
Eu1 O5 C30 O6 -123.9(19) . . . . ?
Eu1 O5 C30 C23 55(3) . . . . ?
Eu1 O7 C29 O8 32(3) 7_656 . . . ?
Eu1 O7 C29 C33 -151.4(13) 7_656 . . . ?
Eu1 O9 C35 O10 13.9(18) 7_656 . . . ?
Eu1 O9 C35 C31 -158.3(13) 7_656 . . . ?
Eu1 O10 C35 O9 -14.1(18) 7_656 . . . ?
Eu1 O10 C35 C31 157.7(14) 7_656 . . . ?
Eu1 O13 C28 O14 -2(2) 3_455 . . . ?
Eu1 O13 C28 C6 177.2(14) 3_455 . . . ?
Eu1 O14 C28 O13 2(2) 3_455 . . . ?
Eu1 O14 C28 C6 -177.3(15) 3_455 . . . ?
Eu2 O1 C32 O2 102.0(18) 7_656 . . . ?
Eu2 O1 C32 C24 -77.9(17) 7_656 . . . ?
Eu2 O3 C2 O4 138(2) 7_656 . . . ?
Eu2 O3 C2 C5 -44(3) 7_656 . . . ?
Eu2 O8 C29 O7 -27(2) . . . . ?
Eu2 O8 C29 C33 156.4(11) . . . . ?
Eu2 O9 C35 Eu1 -150(3) . . . 7_656 ?
Eu2 O9 C35 O10 -136(2) . . . . ?
Eu2 O9 C35 C31 51(3) . . . . ?
Eu2 O11 C34 O12 -0.9(18) 2_656 . . . ?
Eu2 O11 C34 C22 177.4(15) 2_656 . . . ?
Eu2 O12 C34 O11 0.9(19) 2_656 . . . ?
Eu2 O12 C34 C22 -177.4(13) 2_656 . . . ?
O3 C2 C5 C9 151.6(17) . . . . ?
O3 C2 C5 C24 -29(3) . . . . ?
O4 C2 C5 C9 -30(3) . . . . ?
O4 C2 C5 C24 149(2) . . . . ?
O7 C29 C33 C9 1(2) . . . . ?
O7 C29 C33 C25 174.0(14) . . . . ?
O8 C29 C33 C9 178.5(14) . . . . ?
O8 C29 C33 C25 -9(2) . . . . ?
N1 C14 C15 C20 4(5) . . . . ?
N2 C3 C8 C1 -1(3) . . . . ?
N2 C3 C20 C7 -162.2(19) . . . . ?
N2 C3 C20 C15 12(3) . . . . ?
N3 C10 C13 C18 3(7) . . . . ?
N3 C11 C17 C18 -10(4) . . . . ?
C1 C4 C19 N2 0(3) . . . . ?
C1 C4 C19 C18 177.3(18) . . . . ?
C1 C21 C22 C26 -171.5(15) . . . . ?
C1 C21 C22 C34 12(3) . . . . ?
C1 C21 C31 C27 171.5(16) . . . . ?
C1 C21 C31 C35 0(2) . . . . ?
C2 C5 C9 C33 -177.7(16) . . . . ?
C2 C5 C24 C23 -179.3(15) . . . . ?
C2 C5 C24 C32 -8(2) . . . . ?
C3 N2 C19 C4 -2(3) . . . . ?
C3 N2 C19 C18 -179.0(19) . . . . ?
C4 C1 C8 C3 -1(2) . . . . ?
C4 C1 C21 C22 57(2) . . . . ?
C4 C1 C21 C31 -120.6(17) . . . . ?
C5 C9 C33 C25 -2(2) . . . . ?
C5 C9 C33 C29 170.6(15) . . . . ?
C5 C24 C32 O1 96.6(18) . . . . ?
C5 C24 C32 O2 -83(2) . . . . ?
C6 C27 C31 C21 2(3) . . . . ?
C6 C27 C31 C35 173.1(17) . . . . ?
C8 C1 C4 C19 1(2) . . . . ?
C8 C1 C21 C22 -128.5(18) . . . . ?
C8 C1 C21 C31 54(2) . . . . ?
C8 C3 C20 C7 11(3) . . . . ?
C8 C3 C20 C15 -175(2) . . . . ?
C9 C5 C24 C23 0(2) . . . . ?
C9 C5 C24 C32 171.5(15) . . . . ?
C10 N3 C11 C17 11(5) . . . . ?
C10 C13 C18 C17 0(5) . . . . ?
C10 C13 C18 C19 -176(4) . . . . ?
C11 N3 C10 C13 -8(6) . . . . ?
C11 C17 C18 C13 4(4) . . . . ?
C11 C17 C18 C19 180(3) . . . . ?
C13 C18 C19 N2 175(3) . . . . ?
C13 C18 C19 C4 -3(4) . . . . ?
C14 N1 C16 C7 3(4) . . . . ?
C14 C15 C20 C3 -175(3) . . . . ?
C14 C15 C20 C7 0(4) . . . . ?
C16 N1 C14 C15 -5(5) . . . . ?
C16 C7 C20 C3 171.9(18) . . . . ?
C16 C7 C20 C15 -3(3) . . . . ?
C17 C18 C19 N2 -1(3) . . . . ?
C17 C18 C19 C4 -178(2) . . . . ?
C19 N2 C3 C8 2(3) . . . . ?
C19 N2 C3 C20 174.6(17) . . . . ?
C20 C3 C8 C1 -173.1(16) . . . . ?
C20 C7 C16 N1 1(4) . . . . ?
C21 C1 C4 C19 176.2(15) . . . . ?
C21 C1 C8 C3 -175.6(15) . . . . ?
C21 C22 C26 C6 -2(3) . . . . ?
C21 C22 C34 O11 19(3) . . . . ?
C21 C22 C34 O12 -163.1(17) . . . . ?
C21 C31 C35 Eu1 154(3) . . . 7_656 ?
C21 C31 C35 O9 -124.0(17) . . . . ?
C21 C31 C35 O10 64(2) . . . . ?
C22 C21 C31 C27 -6(2) . . . . ?
C22 C21 C31 C35 -177.2(16) . . . . ?
C23 C24 C32 O1 -92.1(18) . . . . ?
C23 C24 C32 O2 88(2) . . . . ?
C23 C25 C33 C9 -1(2) . . . . ?
C23 C25 C33 C29 -174.2(14) . . . . ?
C24 C5 C9 C33 3(2) . . . . ?
C24 C23 C25 C33 4(2) . . . . ?
C24 C23 C30 O5 20(3) . . . . ?
C24 C23 C30 O6 -160.3(18) . . . . ?
C25 C23 C24 C5 -3(2) . . . . ?
C25 C23 C24 C32 -174.8(14) . . . . ?
C25 C23 C30 O5 -159.6(16) . . . . ?
C25 C23 C30 O6 20(3) . . . . ?
C26 C6 C27 C31 3(3) . . . . ?
C26 C6 C28 O13 -177.1(17) . . . . ?
C26 C6 C28 O14 2(3) . . . . ?
C26 C22 C34 O11 -158.2(16) . . . . ?
C26 C22 C34 O12 20(2) . . . . ?
C27 C6 C26 C22 -3(3) . . . . ?
C27 C6 C28 O13 -1(3) . . . . ?
C27 C6 C28 O14 178.3(17) . . . . ?
C27 C31 C35 Eu1 -17(5) . . . 7_656 ?
C27 C31 C35 O9 65(2) . . . . ?
C27 C31 C35 O10 -107(2) . . . . ?
C28 C6 C26 C22 173.0(16) . . . . ?
C28 C6 C27 C31 -173.0(16) . . . . ?
C30 C23 C24 C5 176.5(15) . . . . ?
C30 C23 C24 C32 5(2) . . . . ?
C30 C23 C25 C33 -175.9(15) . . . . ?
C31 C21 C22 C26 6(2) . . . . ?
C31 C21 C22 C34 -170.5(15) . . . . ?
C34 C22 C26 C6 175.3(15) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.371
_oxdiff_exptl_absorpt_empirical_full_min 0.756
_exptl_crystal_preparation       Luminescent
####################################################################### 
# 
# 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_a
_database_code_depnum_ccdc_archive 'CCDC 2117149'
loop_
_audit_author_name
_audit_author_address
'Feng YQ'
;luoyang university
China
;
_audit_update_record             
;
2021-12-19 deposited with the CCDC.	2022-06-01 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C34 H18 N3 O28 Tb2'
_chemical_formula_weight         1234.35

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

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   C2/c

loop_
_symmetry_equiv_pos_as_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                   17.6182(12)
_cell_length_b                   31.3835(12)
_cell_length_c                   17.8680(13)
_cell_angle_alpha                90.00
_cell_angle_beta                 106.722(8)
_cell_angle_gamma                90.00
_cell_volume                     9461.8(10)
_cell_formula_units_Z            8
_cell_measurement_temperature    292(2)
_cell_measurement_theta_max      23.0830
_cell_measurement_theta_min      3.5410
_cell_measurement_reflns_used    3996

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.18
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.733
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             4776
_exptl_absorpt_coefficient_mu    3.058
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.456
_exptl_absorpt_correction_T_max  0.577
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      292(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            22705
_diffrn_reflns_av_R_equivalents  0.1092
_diffrn_reflns_av_sigmaI/netI    0.1883
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_k_min       -39
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         3.25
_diffrn_reflns_theta_max         26.37
_reflns_number_total             9442
_reflns_number_gt                5555
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0237P)²+5.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         9442
_refine_ls_number_parameters     556
_refine_ls_number_restraints     144
_refine_ls_R_factor_all          0.1537
_refine_ls_R_factor_gt           0.0852
_refine_ls_wR_factor_ref         0.1493
_refine_ls_wR_factor_gt          0.1298
_refine_ls_goodness_of_fit_ref   1.156
_refine_ls_restrained_S_all      1.152
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Tb1 Tb 0.55241(4) 0.626619(16) 0.41116(3) 0.01882(17) Uani 1 1 d . . .
Tb2 Tb 0.70854(4) 0.608854(18) 0.62372(4) 0.02491(19) Uani 1 1 d . . .
O8 O 0.6871(5) 0.6126(2) 0.4813(5) 0.026(2) Uani 1 1 d . . .
O13 O 0.4278(5) 0.6044(2) 0.9483(4) 0.023(2) Uani 1 1 d . . .
O14 O 0.5470(5) 0.6252(2) 1.0145(5) 0.025(2) Uani 1 1 d . . .
O2 O 0.6264(5) 0.6504(2) 0.3311(4) 0.025(2) Uani 1 1 d . . .
O3 O 0.8182(5) 0.8202(2) 0.4007(5) 0.031(2) Uani 1 1 d . . .
O9 O 0.6324(5) 0.6250(2) 0.7206(5) 0.029(2) Uani 1 1 d . . .
O12 O 0.5202(5) 0.4494(2) 0.9215(5) 0.036(2) Uani 1 1 d . . .
O6 O 0.8301(5) 0.6233(3) 0.5996(5) 0.039(2) Uani 1 1 d . . .
O11 O 0.5871(5) 0.4379(2) 0.8378(5) 0.029(2) Uani 1 1 d . . .
O4 O 0.9061(5) 0.8096(2) 0.5167(5) 0.034(2) Uani 1 1 d . . .
O16 O 0.4803(5) 0.6884(2) 0.3521(5) 0.048(3) Uani 1 1 d . . .
H16A H 0.4290 0.6833 0.3365 0.072 Uiso 1 1 d R . .
H16B H 0.4846 0.7088 0.3867 0.072 Uiso 1 1 d R . .
O15 O 0.4357(5) 0.6086(2) 0.3068(5) 0.046(3) Uani 1 1 d . . .
H15A H 0.4301 0.6252 0.2630 0.069 Uiso 1 1 d R . .
H15B H 0.4392 0.5819 0.2875 0.069 Uiso 1 1 d R . .
C19 C 0.5020(7) 0.6064(3) 0.9589(7) 0.017(3) Uani 1 1 d U . .
C18 C 0.5557(8) 0.4630(4) 0.8717(7) 0.023(3) Uani 1 1 d U . .
O7 O 0.7780(6) 0.5955(3) 0.4216(6) 0.049(3) Uani 1 1 d . . .
C16 C 0.5349(7) 0.5809(3) 0.9028(7) 0.021(3) Uani 1 1 d . . .
C11 C 0.6423(7) 0.5873(4) 0.7464(8) 0.031(3) Uani 1 1 d . . .
O10 O 0.6794(6) 0.5616(3) 0.7171(6) 0.054(3) Uani 1 1 d . . .
C15 C 0.5242(7) 0.5372(3) 0.9054(6) 0.017(3) Uani 1 1 d U . .
H15 H 0.4941 0.5258 0.9356 0.021 Uiso 1 1 calc R . .
C8 C 0.8538(7) 0.7968(4) 0.4586(7) 0.023(3) Uani 1 1 d U . .
C12 C 0.6055(7) 0.5717(3) 0.8085(7) 0.019(3) Uani 1 1 d U . .
C4 C 0.8264(7) 0.7520(3) 0.4566(7) 0.022(3) Uani 1 1 d . . .
C13 C 0.5969(7) 0.5274(3) 0.8136(6) 0.019(3) Uani 1 1 d U . .
H13 H 0.6176 0.5094 0.7830 0.023 Uiso 1 1 calc R . .
O5 O 0.9443(6) 0.6556(3) 0.6120(7) 0.088(5) Uani 1 1 d . . .
O1 O 0.6526(7) 0.7050(3) 0.2646(6) 0.079(4) Uani 1 1 d . . .
C7 C 0.7712(7) 0.6676(3) 0.4542(7) 0.023(3) Uani 1 1 d U . .
C6 C 0.8362(7) 0.6810(3) 0.5147(7) 0.022(3) Uani 1 1 d . . .
C3 C 0.7646(8) 0.7375(3) 0.3965(7) 0.026(3) Uani 1 1 d . . .
H3 H 0.7406 0.7563 0.3565 0.031 Uiso 1 1 calc R . .
C17 C 0.5771(7) 0.5992(3) 0.8552(7) 0.018(3) Uani 1 1 d . . .
C10 C 0.7449(8) 0.6216(4) 0.4506(8) 0.034(4) Uani 1 1 d . . .
C14 C 0.5587(6) 0.5105(3) 0.8626(7) 0.018(3) Uani 1 1 d . . .
C5 C 0.8625(7) 0.7223(3) 0.5140(7) 0.026(3) Uani 1 1 d U . .
H5 H 0.9067 0.7308 0.5538 0.031 Uiso 1 1 calc R . .
N2 N 0.6279(7) 0.7323(3) 0.8799(6) 0.033(3) Uani 1 1 d . . .
C1 C 0.6655(8) 0.6832(4) 0.3246(8) 0.037(4) Uani 1 1 d . . .
C9 C 0.8725(9) 0.6514(4) 0.5790(9) 0.047(4) Uani 1 1 d . . .
C2 C 0.7362(7) 0.6965(3) 0.3923(7) 0.021(3) Uani 1 1 d . . .
C20 C 0.5941(7) 0.6457(3) 0.8622(7) 0.019(3) Uani 1 1 d . . .
C24 C 0.6716(7) 0.6588(3) 0.8813(7) 0.024(3) Uani 1 1 d . . .
H24 H 0.7124 0.6391 0.8881 0.029 Uiso 1 1 calc R . .
C21 C 0.5331(7) 0.6741(3) 0.8516(7) 0.023(3) Uani 1 1 d . . .
H21 H 0.4806 0.6651 0.8390 0.028 Uiso 1 1 calc R . .
C32 C 0.4925(8) 0.7525(3) 0.8412(8) 0.031(3) Uani 1 1 d . . .
C31 C 0.5127(9) 0.7939(4) 0.8613(10) 0.064(6) Uani 1 1 d . . .
H31 H 0.5639 0.8009 0.8906 0.077 Uiso 1 1 calc R . .
C23 C 0.6887(8) 0.7033(4) 0.8905(7) 0.029(3) Uani 1 1 d . . .
C26 C 0.7820(9) 0.7620(4) 0.9176(8) 0.049(4) Uani 1 1 d U . .
H26 H 0.7396 0.7804 0.9132 0.058 Uiso 1 1 calc R . .
N1 N 0.9209(8) 0.7546(5) 0.9406(8) 0.079(5) Uani 1 1 d . . .
C25 C 0.7673(8) 0.7208(4) 0.9090(8) 0.035(4) Uani 1 1 d . . .
C33 C 0.4154(9) 0.7449(4) 0.8043(8) 0.043(4) Uani 1 1 d U . .
H33 H 0.3980 0.7170 0.7930 0.052 Uiso 1 1 calc R . .
N3 N 0.3804(11) 0.8172(4) 0.7980(10) 0.075(5) Uani 1 1 d . . .
C22 C 0.5532(8) 0.7183(4) 0.8606(8) 0.034(4) Uani 1 1 d U . .
O18 O 0.8010(8) 0.6316(4) 0.7433(8) 0.119(5) Uani 1 1 d U . .
C34 C 0.3618(9) 0.7782(6) 0.7832(9) 0.055(5) Uani 1 1 d . . .
H34 H 0.3094 0.7718 0.7568 0.066 Uiso 1 1 calc R . .
C30 C 0.4569(12) 0.8246(5) 0.8378(13) 0.083(7) Uani 1 1 d . . .
H30 H 0.4722 0.8527 0.8499 0.100 Uiso 1 1 calc R . .
C29 C 0.8336(10) 0.6958(5) 0.9198(10) 0.067(5) Uani 1 1 d U . .
H29 H 0.8276 0.6663 0.9172 0.080 Uiso 1 1 calc R . .
C27 C 0.8578(11) 0.7794(5) 0.9329(9) 0.064(5) Uani 1 1 d U . .
H27 H 0.8643 0.8087 0.9378 0.076 Uiso 1 1 calc R . .
C28 C 0.9097(11) 0.7130(5) 0.9344(12) 0.103(9) Uani 1 1 d . . .
H28 H 0.9529 0.6949 0.9398 0.124 Uiso 1 1 calc R . .
O17 O 0.7181(10) 0.5382(3) 0.5825(7) 0.120(6) Uani 1 1 d . . .
O4W O 0.6510(8) 0.4671(4) 0.6238(8) 0.116(5) Uiso 1 1 d . . .
O3W O 0.2802(11) 0.8779(5) 0.7404(11) 0.187(8) Uiso 1 1 d . . .
O2W O 0.2777(13) 0.5497(7) 0.2255(13) 0.237(10) Uiso 1 1 d . . .
O1W O 0.7770(12) 0.5116(6) 0.4607(12) 0.214(9) Uiso 1 1 d . . .
O8W O 0.7149(13) 0.3949(6) 0.5741(13) 0.234(9) Uiso 1 1 d . . .
O7W O 0.9063(15) 0.7055(7) 0.7506(15) 0.271(11) Uiso 1 1 d . . .
O6W O 0.8183(18) 0.5768(8) 0.8888(17) 0.322(14) Uiso 1 1 d . . .
O5W O 1.033(2) 0.6155(9) 0.733(2) 0.379(18) Uiso 1 1 d . . .
O10W O 0.419(2) 0.9265(11) 0.916(2) 0.44(2) Uiso 1 1 d . . .
O9W O 0.542(3) 0.8939(13) 1.029(3) 0.50(3) Uiso 1 1 d . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Tb1 O2 2.318(8) . ?
Tb1 O4 2.379(7) 7_666 ?
Tb1 O8 2.385(8) . ?
Tb1 O16 2.391(7) . ?
Tb1 O15 2.412(8) . ?
Tb1 O12 2.472(7) 6_565 ?
Tb1 O14 2.485(8) 2_656 ?
Tb1 O13 2.532(7) 2_656 ?
Tb1 O11 2.579(8) 6_565 ?
Tb1 C19 2.826(12) 2_656 ?
Tb1 C18 2.905(11) 6_565 ?
Tb2 O3 2.293(7) 7_666 ?
Tb2 O6 2.347(9) . ?
Tb2 O17 2.357(9) . ?
Tb2 O13 2.380(8) 2_656 ?
Tb2 O18 2.393(13) . ?
Tb2 O10 2.397(9) . ?
Tb2 O8 2.465(8) . ?
Tb2 O9 2.528(8) . ?
Tb2 C11 2.845(15) . ?
O8 C10 1.319(16) . ?
O13 C19 1.267(12) . ?
O13 Tb2 2.380(7) 2_656 ?
O13 Tb1 2.532(7) 2_656 ?
O14 C19 1.228(12) . ?
O14 Tb1 2.485(8) 2_656 ?
O2 C1 1.264(13) . ?
O3 C8 1.275(12) . ?
O3 Tb2 2.293(7) 7_666 ?
O9 C11 1.264(13) . ?
O12 C18 1.297(15) . ?
O12 Tb1 2.472(7) 6_566 ?
O6 C9 1.276(16) . ?
O11 C18 1.219(14) . ?
O11 Tb1 2.579(8) 6_566 ?
O4 C8 1.240(12) . ?
O4 Tb1 2.379(7) 7_666 ?
O16 H16A 0.8795 . ?
O16 H16B 0.8796 . ?
O15 H15A 0.9221 . ?
O15 H15B 0.9162 . ?
C19 C16 1.524(16) . ?
C19 Tb1 2.826(12) 2_656 ?
C18 C14 1.501(14) . ?
C18 Tb1 2.905(11) 6_566 ?
O7 C10 1.205(15) . ?
C16 C15 1.387(13) . ?
C16 C17 1.403(15) . ?
C11 O10 1.245(14) . ?
C11 C12 1.519(17) . ?
C15 C14 1.386(15) . ?
C15 H15 0.9300 . ?
C8 C4 1.484(14) . ?
C12 C17 1.389(15) . ?
C12 C13 1.405(13) . ?
C4 C3 1.368(15) . ?
C4 C5 1.396(14) . ?
C13 C14 1.355(15) . ?
C13 H13 0.9300 . ?
O5 C9 1.240(15) . ?
O1 C1 1.236(14) . ?
C7 C6 1.394(14) . ?
C7 C2 1.426(14) . ?
C7 C10 1.511(15) . ?
C6 C5 1.377(14) . ?
C6 C9 1.473(16) . ?
C3 C2 1.373(14) . ?
C3 H3 0.9300 . ?
C17 C20 1.488(14) . ?
C5 H5 0.9300 . ?
N2 C22 1.335(15) . ?
N2 C23 1.377(15) . ?
C1 C2 1.523(15) . ?
C20 C21 1.368(14) . ?
C20 C24 1.373(14) . ?
C24 C23 1.427(15) . ?
C24 H24 0.9300 . ?
C21 C22 1.429(14) . ?
C21 H21 0.9300 . ?
C32 C33 1.349(17) . ?
C32 C31 1.368(15) . ?
C32 C22 1.485(16) . ?
C31 C30 1.353(19) . ?
C31 H31 0.9300 . ?
C23 C25 1.439(17) . ?
C26 C25 1.318(15) . ?
C26 C27 1.39(2) . ?
C26 H26 0.9300 . ?
N1 C28 1.322(17) . ?
N1 C27 1.331(19) . ?
C25 C29 1.376(19) . ?
C33 C34 1.386(17) . ?
C33 H33 0.9300 . ?
N3 C34 1.275(17) . ?
N3 C30 1.35(2) . ?
C34 H34 0.9300 . ?
C30 H30 0.9300 . ?
C29 C28 1.40(2) . ?
C29 H29 0.9300 . ?
C27 H27 0.9300 . ?
C28 H28 0.9300 . ?
O5W O5W 1.44(7) 2_756 ?

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 Tb1 O4 85.6(3) . 7_666 ?
O2 Tb1 O8 74.5(3) . . ?
O4 Tb1 O8 76.5(3) 7_666 . ?
O2 Tb1 O16 77.8(3) . . ?
O4 Tb1 O16 66.3(3) 7_666 . ?
O8 Tb1 O16 134.7(3) . . ?
O2 Tb1 O15 96.0(3) . . ?
O4 Tb1 O15 132.6(3) 7_666 . ?
O8 Tb1 O15 149.5(3) . . ?
O16 Tb1 O15 67.8(3) . . ?
O2 Tb1 O12 122.6(3) . 6_565 ?
O4 Tb1 O12 144.4(3) 7_666 6_565 ?
O8 Tb1 O12 89.9(3) . 6_565 ?
O16 Tb1 O12 135.4(3) . 6_565 ?
O15 Tb1 O12 70.7(3) . 6_565 ?
O2 Tb1 O14 160.7(2) . 2_656 ?
O4 Tb1 O14 83.1(3) 7_666 2_656 ?
O8 Tb1 O14 117.6(3) . 2_656 ?
O16 Tb1 O14 83.4(3) . 2_656 ?
O15 Tb1 O14 80.4(3) . 2_656 ?
O12 Tb1 O14 74.4(3) 6_565 2_656 ?
O2 Tb1 O13 139.4(3) . 2_656 ?
O4 Tb1 O13 76.2(3) 7_666 2_656 ?
O8 Tb1 O13 66.1(3) . 2_656 ?
O16 Tb1 O13 124.4(3) . 2_656 ?
O15 Tb1 O13 123.1(3) . 2_656 ?
O12 Tb1 O13 68.3(3) 6_565 2_656 ?
O14 Tb1 O13 51.8(2) 2_656 2_656 ?
O2 Tb1 O11 71.4(2) . 6_565 ?
O4 Tb1 O11 148.8(3) 7_666 6_565 ?
O8 Tb1 O11 77.1(3) . 6_565 ?
O16 Tb1 O11 125.8(3) . 6_565 ?
O15 Tb1 O11 72.4(3) . 6_565 ?
O12 Tb1 O11 51.2(3) 6_565 6_565 ?
O14 Tb1 O11 124.3(2) 2_656 6_565 ?
O13 Tb1 O11 107.6(2) 2_656 6_565 ?
O2 Tb1 C19 164.3(3) . 2_656 ?
O4 Tb1 C19 82.4(3) 7_666 2_656 ?
O8 Tb1 C19 92.8(3) . 2_656 ?
O16 Tb1 C19 106.4(3) . 2_656 ?
O15 Tb1 C19 99.6(3) . 2_656 ?
O12 Tb1 C19 65.4(3) 6_565 2_656 ?
O14 Tb1 C19 25.7(2) 2_656 2_656 ?
O13 Tb1 C19 26.6(3) 2_656 2_656 ?
O11 Tb1 C19 115.3(3) 6_565 2_656 ?
O2 Tb1 C18 96.2(3) . 6_565 ?
O4 Tb1 C18 157.2(3) 7_666 6_565 ?
O8 Tb1 C18 82.1(3) . 6_565 ?
O16 Tb1 C18 136.3(3) . 6_565 ?
O15 Tb1 C18 70.0(3) . 6_565 ?
O12 Tb1 C18 26.4(3) 6_565 6_565 ?
O14 Tb1 C18 100.3(3) 2_656 6_565 ?
O13 Tb1 C18 88.1(3) 2_656 6_565 ?
O11 Tb1 C18 24.8(3) 6_565 6_565 ?
C19 Tb1 C18 91.0(4) 2_656 6_565 ?
O3 Tb2 O6 85.7(3) 7_666 . ?
O3 Tb2 O17 152.0(4) 7_666 . ?
O6 Tb2 O17 88.5(4) . . ?
O3 Tb2 O13 80.4(3) 7_666 2_656 ?
O6 Tb2 O13 138.1(3) . 2_656 ?
O17 Tb2 O13 85.9(4) . 2_656 ?
O3 Tb2 O18 86.0(4) 7_666 . ?
O6 Tb2 O18 71.5(4) . . ?
O17 Tb2 O18 117.9(5) . . ?
O13 Tb2 O18 145.3(4) 2_656 . ?
O3 Tb2 O10 131.4(3) 7_666 . ?
O6 Tb2 O10 129.6(3) . . ?
O17 Tb2 O10 71.6(3) . . ?
O13 Tb2 O10 87.4(3) 2_656 . ?
O18 Tb2 O10 77.9(4) . . ?
O3 Tb2 O8 78.2(3) 7_666 . ?
O6 Tb2 O8 71.2(3) . . ?
O17 Tb2 O8 74.1(3) . . ?
O13 Tb2 O8 67.3(3) 2_656 . ?
O18 Tb2 O8 140.3(4) . . ?
O10 Tb2 O8 138.4(3) . . ?
O3 Tb2 O9 79.3(3) 7_666 . ?
O6 Tb2 O9 141.2(3) . . ?
O17 Tb2 O9 120.2(3) . . ?
O13 Tb2 O9 74.3(3) 2_656 . ?
O18 Tb2 O9 71.8(4) . . ?
O10 Tb2 O9 52.1(3) . . ?
O8 Tb2 O9 138.0(3) . . ?
O3 Tb2 C11 105.7(3) 7_666 . ?
O6 Tb2 C11 141.8(3) . . ?
O17 Tb2 C11 95.7(4) . . ?
O13 Tb2 C11 80.1(3) 2_656 . ?
O18 Tb2 C11 73.0(4) . . ?
O10 Tb2 C11 25.7(3) . . ?
O8 Tb2 C11 146.3(3) . . ?
O9 Tb2 C11 26.4(3) . . ?
C10 O8 Tb1 120.8(7) . . ?
C10 O8 Tb2 122.2(7) . . ?
Tb1 O8 Tb2 112.6(3) . . ?
C19 O13 Tb2 156.3(7) . 2_656 ?
C19 O13 Tb1 89.7(7) . 2_656 ?
Tb2 O13 Tb1 110.5(3) 2_656 2_656 ?
C19 O14 Tb1 92.8(7) . 2_656 ?
C1 O2 Tb1 137.5(9) . . ?
C8 O3 Tb2 137.7(7) . 7_666 ?
C11 O9 Tb2 90.9(8) . . ?
C18 O12 Tb1 95.8(7) . 6_566 ?
C9 O6 Tb2 145.9(9) . . ?
C18 O11 Tb1 92.7(8) . 6_566 ?
C8 O4 Tb1 139.9(8) . 7_666 ?
Tb1 O16 H16A 111.1 . . ?
Tb1 O16 H16B 110.7 . . ?
H16A O16 H16B 103.2 . . ?
Tb1 O15 H15A 112.5 . . ?
Tb1 O15 H15B 111.7 . . ?
H15A O15 H15B 101.5 . . ?
O14 C19 O13 123.0(12) . . ?
O14 C19 C16 120.2(11) . . ?
O13 C19 C16 116.5(10) . . ?
O14 C19 Tb1 61.5(7) . 2_656 ?
O13 C19 Tb1 63.7(6) . 2_656 ?
C16 C19 Tb1 160.4(7) . 2_656 ?
O11 C18 O12 120.3(10) . . ?
O11 C18 C14 123.5(12) . . ?
O12 C18 C14 116.1(11) . . ?
O11 C18 Tb1 62.5(6) . 6_566 ?
O12 C18 Tb1 57.8(5) . 6_566 ?
C14 C18 Tb1 172.4(9) . 6_566 ?
C15 C16 C17 121.7(11) . . ?
C15 C16 C19 114.7(11) . . ?
C17 C16 C19 123.5(9) . . ?
O10 C11 O9 119.3(13) . . ?
O10 C11 C12 118.9(11) . . ?
O9 C11 C12 121.7(12) . . ?
O10 C11 Tb2 56.6(7) . . ?
O9 C11 Tb2 62.7(7) . . ?
C12 C11 Tb2 174.7(9) . . ?
C11 O10 Tb2 97.7(8) . . ?
C14 C15 C16 119.5(11) . . ?
C14 C15 H15 120.2 . . ?
C16 C15 H15 120.2 . . ?
O4 C8 O3 124.4(10) . . ?
O4 C8 C4 119.0(11) . . ?
O3 C8 C4 116.4(10) . . ?
C17 C12 C13 120.8(11) . . ?
C17 C12 C11 122.8(10) . . ?
C13 C12 C11 116.3(11) . . ?
C3 C4 C5 116.4(10) . . ?
C3 C4 C8 120.9(11) . . ?
C5 C4 C8 122.7(10) . . ?
C14 C13 C12 120.7(11) . . ?
C14 C13 H13 119.6 . . ?
C12 C13 H13 119.6 . . ?
C6 C7 C2 119.0(9) . . ?
C6 C7 C10 119.6(10) . . ?
C2 C7 C10 121.0(10) . . ?
C5 C6 C7 118.6(10) . . ?
C5 C6 C9 121.9(11) . . ?
C7 C6 C9 119.4(10) . . ?
C4 C3 C2 123.3(11) . . ?
C4 C3 H3 118.3 . . ?
C2 C3 H3 118.3 . . ?
C12 C17 C16 117.0(10) . . ?
C12 C17 C20 124.1(11) . . ?
C16 C17 C20 118.7(10) . . ?
O7 C10 O8 124.0(11) . . ?
O7 C10 C7 119.2(14) . . ?
O8 C10 C7 116.8(12) . . ?
C13 C14 C15 119.9(10) . . ?
C13 C14 C18 119.8(11) . . ?
C15 C14 C18 120.3(11) . . ?
C6 C5 C4 123.5(11) . . ?
C6 C5 H5 118.2 . . ?
C4 C5 H5 118.2 . . ?
C22 N2 C23 119.1(10) . . ?
O1 C1 O2 124.1(12) . . ?
O1 C1 C2 116.2(11) . . ?
O2 C1 C2 119.5(11) . . ?
O5 C9 O6 122.6(13) . . ?
O5 C9 C6 117.3(13) . . ?
O6 C9 C6 120.1(12) . . ?
C3 C2 C7 118.9(10) . . ?
C3 C2 C1 120.1(10) . . ?
C7 C2 C1 120.9(10) . . ?
C21 C20 C24 121.6(10) . . ?
C21 C20 C17 119.9(10) . . ?
C24 C20 C17 118.5(10) . . ?
C20 C24 C23 118.9(11) . . ?
C20 C24 H24 120.5 . . ?
C23 C24 H24 120.5 . . ?
C20 C21 C22 117.3(11) . . ?
C20 C21 H21 121.4 . . ?
C22 C21 H21 121.4 . . ?
C33 C32 C31 116.5(12) . . ?
C33 C32 C22 122.9(11) . . ?
C31 C32 C22 120.7(13) . . ?
C30 C31 C32 118.8(15) . . ?
C30 C31 H31 120.6 . . ?
C32 C31 H31 120.6 . . ?
N2 C23 C24 120.1(11) . . ?
N2 C23 C25 115.9(11) . . ?
C24 C23 C25 123.9(12) . . ?
C25 C26 C27 123.4(15) . . ?
C25 C26 H26 118.3 . . ?
C27 C26 H26 118.3 . . ?
C28 N1 C27 117.9(16) . . ?
C26 C25 C29 114.5(14) . . ?
C26 C25 C23 123.1(13) . . ?
C29 C25 C23 122.4(13) . . ?
C32 C33 C34 120.7(14) . . ?
C32 C33 H33 119.6 . . ?
C34 C33 H33 119.6 . . ?
C34 N3 C30 115.6(14) . . ?
N2 C22 C21 122.9(11) . . ?
N2 C22 C32 114.3(11) . . ?
C21 C22 C32 122.5(12) . . ?
N3 C34 C33 123.5(16) . . ?
N3 C34 H34 118.2 . . ?
C33 C34 H34 118.2 . . ?
N3 C30 C31 124.7(16) . . ?
N3 C30 H30 117.7 . . ?
C31 C30 H30 117.7 . . ?
C25 C29 C28 122.4(15) . . ?
C25 C29 H29 118.8 . . ?
C28 C29 H29 118.8 . . ?
N1 C27 C26 121.1(15) . . ?
N1 C27 H27 119.4 . . ?
C26 C27 H27 119.4 . . ?
N1 C28 C29 120.6(17) . . ?
N1 C28 H28 119.7 . . ?
C29 C28 H28 119.7 . . ?

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
O2 Tb1 O8 C10 -1.6(8) . . . . ?
O4 Tb1 O8 C10 -90.8(9) 7_666 . . . ?
O16 Tb1 O8 C10 -55.8(10) . . . . ?
O15 Tb1 O8 C10 73.5(10) . . . . ?
O12 Tb1 O8 C10 122.5(9) 6_565 . . . ?
O14 Tb1 O8 C10 -165.3(8) 2_656 . . . ?
O13 Tb1 O8 C10 -171.4(9) 2_656 . . . ?
O11 Tb1 O8 C10 72.5(8) 6_565 . . . ?
C19 Tb1 O8 C10 -172.2(8) 2_656 . . . ?
C18 Tb1 O8 C10 97.2(9) 6_565 . . . ?
O2 Tb1 O8 Tb2 155.4(3) . . . . ?
O4 Tb1 O8 Tb2 66.2(3) 7_666 . . . ?
O16 Tb1 O8 Tb2 101.2(4) . . . . ?
O15 Tb1 O8 Tb2 -129.5(5) . . . . ?
O12 Tb1 O8 Tb2 -80.5(3) 6_565 . . . ?
O14 Tb1 O8 Tb2 -8.3(4) 2_656 . . . ?
O13 Tb1 O8 Tb2 -14.4(2) 2_656 . . . ?
O11 Tb1 O8 Tb2 -130.5(3) 6_565 . . . ?
C19 Tb1 O8 Tb2 -15.2(3) 2_656 . . . ?
C18 Tb1 O8 Tb2 -105.8(4) 6_565 . . . ?
O3 Tb2 O8 C10 87.3(9) 7_666 . . . ?
O6 Tb2 O8 C10 -2.1(8) . . . . ?
O17 Tb2 O8 C10 -96.0(9) . . . . ?
O13 Tb2 O8 C10 171.8(9) 2_656 . . . ?
O18 Tb2 O8 C10 18.8(11) . . . . ?
O10 Tb2 O8 C10 -131.3(8) . . . . ?
O9 Tb2 O8 C10 146.3(8) . . . . ?
C11 Tb2 O8 C10 -172.1(8) . . . . ?
O3 Tb2 O8 Tb1 -69.3(3) 7_666 . . . ?
O6 Tb2 O8 Tb1 -158.7(4) . . . . ?
O17 Tb2 O8 Tb1 107.4(5) . . . . ?
O13 Tb2 O8 Tb1 15.2(3) 2_656 . . . ?
O18 Tb2 O8 Tb1 -137.9(6) . . . . ?
O10 Tb2 O8 Tb1 72.1(5) . . . . ?
O9 Tb2 O8 Tb1 -10.3(5) . . . . ?
C11 Tb2 O8 Tb1 31.3(7) . . . . ?
O4 Tb1 O2 C1 -4.8(12) 7_666 . . . ?
O8 Tb1 O2 C1 -82.0(12) . . . . ?
O16 Tb1 O2 C1 61.9(12) . . . . ?
O15 Tb1 O2 C1 127.6(12) . . . . ?
O12 Tb1 O2 C1 -161.6(11) 6_565 . . . ?
O14 Tb1 O2 C1 49.5(16) 2_656 . . . ?
O13 Tb1 O2 C1 -67.6(13) 2_656 . . . ?
O11 Tb1 O2 C1 -163.3(12) 6_565 . . . ?
C19 Tb1 O2 C1 -45.2(18) 2_656 . . . ?
C18 Tb1 O2 C1 -162.0(12) 6_565 . . . ?
O3 Tb2 O9 C11 -177.5(7) 7_666 . . . ?
O6 Tb2 O9 C11 -108.4(7) . . . . ?
O17 Tb2 O9 C11 24.0(8) . . . . ?
O13 Tb2 O9 C11 99.5(7) 2_656 . . . ?
O18 Tb2 O9 C11 -88.3(7) . . . . ?
O10 Tb2 O9 C11 0.3(7) . . . . ?
O8 Tb2 O9 C11 123.9(7) . . . . ?
O3 Tb2 O6 C9 -3.8(16) 7_666 . . . ?
O17 Tb2 O6 C9 148.9(17) . . . . ?
O13 Tb2 O6 C9 66.8(17) 2_656 . . . ?
O18 Tb2 O6 C9 -90.9(17) . . . . ?
O10 Tb2 O6 C9 -146.7(15) . . . . ?
O8 Tb2 O6 C9 75.2(16) . . . . ?
O9 Tb2 O6 C9 -70.8(17) . . . . ?
C11 Tb2 O6 C9 -113.8(16) . . . . ?
Tb1 O14 C19 O13 17.0(11) 2_656 . . . ?
Tb1 O14 C19 C16 -157.6(8) 2_656 . . . ?
Tb2 O13 C19 O14 132.3(15) 2_656 . . . ?
Tb1 O13 C19 O14 -16.7(10) 2_656 . . . ?
Tb2 O13 C19 C16 -53(2) 2_656 . . . ?
Tb1 O13 C19 C16 158.1(8) 2_656 . . . ?
Tb2 O13 C19 Tb1 149.0(17) 2_656 . . 2_656 ?
Tb1 O11 C18 O12 -2.2(12) 6_566 . . . ?
Tb1 O11 C18 C14 174.6(10) 6_566 . . . ?
Tb1 O12 C18 O11 2.3(13) 6_566 . . . ?
Tb1 O12 C18 C14 -174.7(8) 6_566 . . . ?
O14 C19 C16 C15 112.4(12) . . . . ?
O13 C19 C16 C15 -62.5(13) . . . . ?
Tb1 C19 C16 C15 23(3) 2_656 . . . ?
O14 C19 C16 C17 -63.9(15) . . . . ?
O13 C19 C16 C17 121.2(12) . . . . ?
Tb1 C19 C16 C17 -153.2(19) 2_656 . . . ?
Tb2 O9 C11 O10 -0.6(12) . . . . ?
Tb2 O9 C11 C12 -176.5(10) . . . . ?
O3 Tb2 C11 O10 -178.1(8) 7_666 . . . ?
O6 Tb2 C11 O10 -74.8(10) . . . . ?
O17 Tb2 C11 O10 20.1(9) . . . . ?
O13 Tb2 C11 O10 104.8(9) 2_656 . . . ?
O18 Tb2 C11 O10 -97.4(9) . . . . ?
O8 Tb2 C11 O10 89.8(10) . . . . ?
O9 Tb2 C11 O10 179.4(13) . . . . ?
O3 Tb2 C11 O9 2.5(7) 7_666 . . . ?
O6 Tb2 C11 O9 105.8(7) . . . . ?
O17 Tb2 C11 O9 -159.3(7) . . . . ?
O13 Tb2 C11 O9 -74.6(6) 2_656 . . . ?
O18 Tb2 C11 O9 83.2(7) . . . . ?
O10 Tb2 C11 O9 -179.4(13) . . . . ?
O8 Tb2 C11 O9 -89.6(8) . . . . ?
O3 Tb2 C11 C12 148(9) 7_666 . . . ?
O6 Tb2 C11 C12 -108(9) . . . . ?
O17 Tb2 C11 C12 -13(9) . . . . ?
O13 Tb2 C11 C12 71(9) 2_656 . . . ?
O18 Tb2 C11 C12 -131(9) . . . . ?
O10 Tb2 C11 C12 -34(9) . . . . ?
O8 Tb2 C11 C12 56(9) . . . . ?
O9 Tb2 C11 C12 146(9) . . . . ?
O9 C11 O10 Tb2 0.6(13) . . . . ?
C12 C11 O10 Tb2 176.6(9) . . . . ?
O3 Tb2 O10 C11 2.4(10) 7_666 . . . ?
O6 Tb2 O10 C11 129.2(8) . . . . ?
O17 Tb2 O10 C11 -158.9(10) . . . . ?
O13 Tb2 O10 C11 -72.4(8) 2_656 . . . ?
O18 Tb2 O10 C11 75.9(9) . . . . ?
O8 Tb2 O10 C11 -123.1(8) . . . . ?
O9 Tb2 O10 C11 -0.3(7) . . . . ?
C17 C16 C15 C14 2.7(17) . . . . ?
C19 C16 C15 C14 -173.6(10) . . . . ?
Tb1 O4 C8 O3 27(2) 7_666 . . . ?
Tb1 O4 C8 C4 -149.6(9) 7_666 . . . ?
Tb2 O3 C8 O4 -23(2) 7_666 . . . ?
Tb2 O3 C8 C4 153.5(9) 7_666 . . . ?
O10 C11 C12 C17 166.8(12) . . . . ?
O9 C11 C12 C17 -17.3(18) . . . . ?
Tb2 C11 C12 C17 -161(8) . . . . ?
O10 C11 C12 C13 -17.0(17) . . . . ?
O9 C11 C12 C13 158.9(10) . . . . ?
Tb2 C11 C12 C13 15(10) . . . . ?
O4 C8 C4 C3 174.9(13) . . . . ?
O3 C8 C4 C3 -1.9(18) . . . . ?
O4 C8 C4 C5 -6.6(19) . . . . ?
O3 C8 C4 C5 176.7(12) . . . . ?
C17 C12 C13 C14 1.8(17) . . . . ?
C11 C12 C13 C14 -174.4(10) . . . . ?
C2 C7 C6 C5 2.4(19) . . . . ?
C10 C7 C6 C5 175.6(12) . . . . ?
C2 C7 C6 C9 179.8(12) . . . . ?
C10 C7 C6 C9 -7(2) . . . . ?
C5 C4 C3 C2 2(2) . . . . ?
C8 C4 C3 C2 -179.1(12) . . . . ?
C13 C12 C17 C16 -4.5(17) . . . . ?
C11 C12 C17 C16 171.5(10) . . . . ?
C13 C12 C17 C20 170.6(10) . . . . ?
C11 C12 C17 C20 -13.4(18) . . . . ?
C15 C16 C17 C12 2.2(17) . . . . ?
C19 C16 C17 C12 178.2(10) . . . . ?
C15 C16 C17 C20 -173.1(10) . . . . ?
C19 C16 C17 C20 2.9(17) . . . . ?
Tb1 O8 C10 O7 -101.8(13) . . . . ?
Tb2 O8 C10 O7 103.5(13) . . . . ?
Tb1 O8 C10 C7 79.6(12) . . . . ?
Tb2 O8 C10 C7 -75.1(12) . . . . ?
C6 C7 C10 O7 -82.8(17) . . . . ?
C2 C7 C10 O7 90.2(16) . . . . ?
C6 C7 C10 O8 95.9(15) . . . . ?
C2 C7 C10 O8 -91.1(15) . . . . ?
C12 C13 C14 C15 3.3(17) . . . . ?
C12 C13 C14 C18 -175.2(10) . . . . ?
C16 C15 C14 C13 -5.5(16) . . . . ?
C16 C15 C14 C18 173.0(10) . . . . ?
O11 C18 C14 C13 1.0(18) . . . . ?
O12 C18 C14 C13 177.9(11) . . . . ?
Tb1 C18 C14 C13 142(6) 6_566 . . . ?
O11 C18 C14 C15 -177.5(11) . . . . ?
O12 C18 C14 C15 -0.6(16) . . . . ?
Tb1 C18 C14 C15 -37(7) 6_566 . . . ?
C7 C6 C5 C4 2(2) . . . . ?
C9 C6 C5 C4 -175.8(13) . . . . ?
C3 C4 C5 C6 -4(2) . . . . ?
C8 C4 C5 C6 177.6(12) . . . . ?
Tb1 O2 C1 O1 -122.8(14) . . . . ?
Tb1 O2 C1 C2 60.5(19) . . . . ?
Tb2 O6 C9 O5 137.4(14) . . . . ?
Tb2 O6 C9 C6 -41(2) . . . . ?
C5 C6 C9 O5 -32(2) . . . . ?
C7 C6 C9 O5 150.6(15) . . . . ?
C5 C6 C9 O6 146.7(14) . . . . ?
C7 C6 C9 O6 -31(2) . . . . ?
C4 C3 C2 C7 1(2) . . . . ?
C4 C3 C2 C1 178.2(13) . . . . ?
C6 C7 C2 C3 -3.9(19) . . . . ?
C10 C7 C2 C3 -176.9(13) . . . . ?
C6 C7 C2 C1 179.4(12) . . . . ?
C10 C7 C2 C1 6.4(19) . . . . ?
O1 C1 C2 C3 22(2) . . . . ?
O2 C1 C2 C3 -160.8(12) . . . . ?
O1 C1 C2 C7 -161.1(13) . . . . ?
O2 C1 C2 C7 16(2) . . . . ?
C12 C17 C20 C21 128.5(13) . . . . ?
C16 C17 C20 C21 -56.5(16) . . . . ?
C12 C17 C20 C24 -53.2(16) . . . . ?
C16 C17 C20 C24 121.8(12) . . . . ?
C21 C20 C24 C23 0.2(18) . . . . ?
C17 C20 C24 C23 -178.1(11) . . . . ?
C24 C20 C21 C22 0.5(18) . . . . ?
C17 C20 C21 C22 178.8(11) . . . . ?
C33 C32 C31 C30 -5(2) . . . . ?
C22 C32 C31 C30 175.4(16) . . . . ?
C22 N2 C23 C24 -0.3(19) . . . . ?
C22 N2 C23 C25 178.3(12) . . . . ?
C20 C24 C23 N2 -0.4(18) . . . . ?
C20 C24 C23 C25 -178.8(12) . . . . ?
C27 C26 C25 C29 3(2) . . . . ?
C27 C26 C25 C23 -177.8(15) . . . . ?
N2 C23 C25 C26 2(2) . . . . ?
C24 C23 C25 C26 -179.7(13) . . . . ?
N2 C23 C25 C29 -178.8(14) . . . . ?
C24 C23 C25 C29 0(2) . . . . ?
C31 C32 C33 C34 5(2) . . . . ?
C22 C32 C33 C34 -176.0(13) . . . . ?
C23 N2 C22 C21 1(2) . . . . ?
C23 N2 C22 C32 -172.9(11) . . . . ?
C20 C21 C22 N2 -1.2(19) . . . . ?
C20 C21 C22 C32 172.3(12) . . . . ?
C33 C32 C22 N2 165.1(14) . . . . ?
C31 C32 C22 N2 -16(2) . . . . ?
C33 C32 C22 C21 -9(2) . . . . ?
C31 C32 C22 C21 170.2(14) . . . . ?
C30 N3 C34 C33 -1(3) . . . . ?
C32 C33 C34 N3 -2(3) . . . . ?
C34 N3 C30 C31 1(3) . . . . ?
C32 C31 C30 N3 3(3) . . . . ?
C26 C25 C29 C28 -3(3) . . . . ?
C23 C25 C29 C28 177.2(17) . . . . ?
C28 N1 C27 C26 -1(3) . . . . ?
C25 C26 C27 N1 -1(3) . . . . ?
C27 N1 C28 C29 0(3) . . . . ?
C25 C29 C28 N1 2(3) . . . . ?

_diffrn_measured_fraction_theta_max 0.974
_diffrn_reflns_theta_full        26.37
_diffrn_measured_fraction_theta_full 0.974
_refine_diff_density_max         1.313
_refine_diff_density_min         -1.004
_refine_diff_density_rms         0.223
