# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2023

####################################################################### 
# 
# 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_f9
_database_code_depnum_ccdc_archive 'CCDC 2268648'
loop_
_audit_author_name
_audit_author_address
Wang
;North University of China
China
;
_audit_update_record             
;
2023-06-09 deposited with the CCDC.	2023-08-28 downloaded from the CCDC.
;
_audit_creation_date             2023-06-01
_audit_creation_method           
;
Olex2 1.5-alpha
(compiled 2021.06.01 svn.r985b505f for OlexSys, GUI svn.r6335)
;
_shelx_SHELXL_version_number     2016/6
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C45.474 H32 Eu5.053 O32'
_chemical_formula_sum            'C42.95 H32 Eu5.05 O32'
_chemical_formula_weight         1827.85
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C H O Eu'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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 -8.9294 11.1857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      trigonal
_space_group_IT_number           167
_space_group_name_H-M_alt        'R -3 c'
_space_group_name_Hall           '-R 3 2"c'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'y, x, -z+1/2'
'-x+y, -x, z'
'x-y, -y, -z+1/2'
'-x, -x+y, -z+1/2'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'y+2/3, x+1/3, -z+5/6'
'-x+y+2/3, -x+1/3, z+1/3'
'x-y+2/3, -y+1/3, -z+5/6'
'-x+2/3, -x+y+1/3, -z+5/6'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'y+1/3, x+2/3, -z+7/6'
'-x+y+1/3, -x+2/3, z+2/3'
'x-y+1/3, -y+2/3, -z+7/6'
'-x+1/3, -x+y+2/3, -z+7/6'
'-x, -y, -z'
'y, -x+y, -z'
'-y, -x, z-1/2'
'x-y, x, -z'
'-x+y, y, z-1/2'
'x, x-y, z-1/2'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'-y+2/3, -x+1/3, z-1/6'
'x-y+2/3, x+1/3, -z+1/3'
'-x+y+2/3, y+1/3, z-1/6'
'x+2/3, x-y+1/3, z-1/6'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'-y+1/3, -x+2/3, z+1/6'
'x-y+1/3, x+2/3, -z+2/3'
'-x+y+1/3, y+2/3, z+1/6'
'x+1/3, x-y+2/3, z+1/6'

_cell_length_a                   17.6167(6)
_cell_length_b                   17.6167(6)
_cell_length_c                   49.2103(14)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     13226.3(9)
_cell_formula_units_Z            7.125
_cell_measurement_reflns_used    4007
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      70.6240
_cell_measurement_theta_min      4.6100
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    30.674
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.49532
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.53 (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.635
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             6156
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.10
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0470
_diffrn_reflns_av_unetI/netI     0.0366
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       58
_diffrn_reflns_limit_l_min       -47
_diffrn_reflns_number            9306
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        67.080
_diffrn_reflns_theta_max         67.080
_diffrn_reflns_theta_min         3.409
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.0450
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -24.00  33.00   1.00    5.42    --    0.00 -80.00-156.00   57
  2  ω    -57.00   0.00   1.00    5.42    --    0.00 123.00 -20.00   57
  3  ω      1.00  97.00   1.00   15.00    --   53.63 -99.00 150.00   96
  4  ω     32.00 123.00   1.00   15.00    --   53.63  57.00  90.00   91
  5  ω    102.00 165.00   1.00   17.50    --  107.26 100.00 -22.00   63
  6  ω    103.00 161.00   1.00   17.50    --  107.26 111.00 -60.00   58
  7  ω    103.00 171.00   1.00   17.50    --  107.26 111.00 -90.00   68
  8  ω    126.00 176.00   1.00   17.50    --  107.26 111.00-180.00   50
  9  ω    105.00 168.00   1.00   17.50    --  107.26 111.00 150.00   63
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0330484000
_diffrn_orient_matrix_UB_12      0.0496114000
_diffrn_orient_matrix_UB_13      -0.0177451000
_diffrn_orient_matrix_UB_21      -0.0701265000
_diffrn_orient_matrix_UB_22      -0.0873871000
_diffrn_orient_matrix_UB_23      -0.0125335000
_diffrn_orient_matrix_UB_31      -0.0647417000
_diffrn_orient_matrix_UB_32      -0.0094007000
_diffrn_orient_matrix_UB_33      0.0225532000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2436
_reflns_number_total             2628
_reflns_odcompleteness_completeness 99.73
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 1.5-alpha (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-alpha (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    ?
_refine_diff_density_max         2.555
_refine_diff_density_min         -5.695
_refine_diff_density_rms         0.245
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     144
_refine_ls_number_reflns         2628
_refine_ls_number_restraints     120
_refine_ls_R_factor_all          0.0671
_refine_ls_R_factor_gt           0.0634
_refine_ls_restrained_S_all      1.069
_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)+(0.0760P)²+1188.2347P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1632
_refine_ls_wR_factor_ref         0.1662
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H) groups, All O(H,H) groups
2. Uiso/Uaniso restraints and constraints
Eu1 \\sim O4 \\sim O5 \\sim O6 \\sim O7 \\sim O2 \\sim O1 \\sim O3: within 4.8A
with sigma of 0.001 and sigma for terminal atoms of 0.002 within 4.8A
Uanis(O2) \\sim Ueq, Uanis(O1) \\sim Ueq: with sigma of 0.001 and sigma for
terminal atoms of 0.002
Uanis(C6) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(C5) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C2) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C8) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C9) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
3.a Riding coordinates:
 O2(H2), O1(H1)
3.b Rotating group:
 O3(H3A,H3B)
3.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C7(H7)
;
_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 0.11754(3) 0.13918(3) 0.46666(2) 0.0081(2) Uani 1 1 d . U . . .
O4 O 0.1493(4) 0.2777(4) 0.48417(12) 0.0098(5) Uani 1 1 d . U . . .
O5 O 0.0744(4) 0.2687(4) 0.52165(13) 0.0102(6) Uani 1 1 d . U . . .
C3 C 0.2264(7) 0.4015(7) 0.5470(2) 0.023(2) Uani 1 1 d . . . . .
H3 H 0.174025 0.383162 0.556193 0.028 Uiso 1 1 calc R U . . .
C5 C 0.3065(9) 0.3971(10) 0.5077(3) 0.047(4) Uani 1 1 d . U . . .
H5 H 0.307076 0.374816 0.490633 0.056 Uiso 1 1 calc R U . . .
C2 C 0.3070(8) 0.4637(8) 0.5588(2) 0.031(3) Uani 1 1 d . U . . .
C1 C 0.3070(8) 0.5026(7) 0.5863(2) 0.024(2) Uani 1 1 d . . . . .
C4 C 0.2263(7) 0.3675(8) 0.5210(2) 0.026(3) Uani 1 1 d . . . . .
C9 C 0.1432(7) 0.3001(7) 0.50810(19) 0.017(2) Uani 1 1 d . U . . .
C6 C 0.3837(12) 0.4577(12) 0.5192(4) 0.058(4) Uani 1 1 d . U . . .
C7 C 0.3831(9) 0.4926(12) 0.5451(3) 0.058(5) Uani 1 1 d . . . . .
H7 H 0.435372 0.535824 0.552628 0.070 Uiso 1 1 calc R U . . .
C8 C 0.4669(11) 0.4853(14) 0.5066(3) 0.068(5) Uani 1 1 d . U . . .
O6 O 0.2368(5) 0.4938(5) 0.59499(15) 0.0227(13) Uani 1 1 d . U . . .
O7 O 0.3809(5) 0.5436(5) 0.59763(15) 0.0229(13) Uani 1 1 d . U . . .
O2 O 0.000000 0.000000 0.4542(2) 0.0092(4) Uani 1 3 d S TU P . .
H2 H 0.000000 0.000000 0.436952 0.014 Uiso 1 3 d R U P . .
O1 O 0.1261(4) 0.0197(4) 0.48503(12) 0.0083(5) Uani 1 1 d . U . . .
H1 H 0.175194 0.027372 0.479536 0.012 Uiso 1 1 d R U . . .
O3 O 0.2273(4) 0.2688(4) 0.43567(13) 0.0143(6) Uiso 1 1 d . U . . .
H3A H 0.283334 0.302618 0.438023 0.021 Uiso 1 1 d R U . . .
H3B H 0.215759 0.287455 0.420746 0.021 Uiso 1 1 d R U . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Eu1 Eu1 3.9990(9) 20_556 ?
Eu1 Eu1 3.9581(9) 2 ?
Eu1 Eu1 3.9581(9) 4 ?
Eu1 O4 2.376(6) . ?
Eu1 O5 2.404(6) 20_556 ?
Eu1 O6 2.409(7) 27 ?
Eu1 O7 2.365(7) 30_455 ?
Eu1 O2 2.366(3) . ?
Eu1 H2 2.7127 . ?
Eu1 O1 2.364(6) . ?
Eu1 O1 2.387(6) 22_556 ?
Eu1 O1 2.367(6) 2 ?
Eu1 H1 2.7044 . ?
Eu1 O3 2.619(7) . ?
O4 C9 1.263(11) . ?
O5 C9 1.245(12) . ?
C3 H3 0.9300 . ?
C3 C2 1.415(16) . ?
C3 C4 1.409(15) . ?
C5 H5 0.9300 . ?
C5 C4 1.400(17) . ?
C5 C6 1.36(2) . ?
C2 C1 1.516(15) . ?
C2 C7 1.354(18) . ?
C1 O6 1.242(14) . ?
C1 O7 1.261(14) . ?
C4 C9 1.491(15) . ?
C6 C7 1.42(2) . ?
C6 C8 1.43(2) . ?
C7 H7 0.9300 . ?
C8 C8 1.20(3) 19_666 ?
O2 H2 0.8504 . ?
O1 H1 0.8495 . ?
O3 H3A 0.8690 . ?
O3 H3B 0.8693 . ?

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
Eu1 Eu1 Eu1 60.0 4 2 ?
Eu1 Eu1 Eu1 60.339(8) 4 20_556 ?
Eu1 Eu1 Eu1 90.0 2 20_556 ?
Eu1 Eu1 H2 43.2 2 . ?
Eu1 Eu1 H2 101.6 20_556 . ?
Eu1 Eu1 H2 43.2 4 . ?
Eu1 Eu1 H1 100.9 2 . ?
Eu1 Eu1 H1 43.0 4 . ?
Eu1 Eu1 H1 42.5 20_556 . ?
O4 Eu1 Eu1 101.52(14) . 20_556 ?
O4 Eu1 Eu1 156.96(15) . 4 ?
O4 Eu1 Eu1 109.45(15) . 2 ?
O4 Eu1 O5 81.6(2) . 20_556 ?
O4 Eu1 O6 132.9(2) . 27 ?
O4 Eu1 H2 143.6 . . ?
O4 Eu1 O1 72.8(2) . 22_556 ?
O4 Eu1 H1 133.0 . . ?
O4 Eu1 O3 67.9(2) . . ?
O5 Eu1 Eu1 158.06(15) 20_556 2 ?
O5 Eu1 Eu1 102.44(15) 20_556 4 ?
O5 Eu1 Eu1 68.88(15) 20_556 20_556 ?
O5 Eu1 O6 77.0(2) 20_556 27 ?
O5 Eu1 H2 133.2 20_556 . ?
O5 Eu1 H1 59.6 20_556 . ?
O5 Eu1 O3 66.5(2) 20_556 . ?
O6 Eu1 Eu1 108.84(19) 27 20_556 ?
O6 Eu1 Eu1 69.62(18) 27 4 ?
O6 Eu1 Eu1 105.81(18) 27 2 ?
O6 Eu1 H2 62.7 27 . ?
O6 Eu1 H1 66.3 27 . ?
O6 Eu1 O3 65.1(2) 27 . ?
O7 Eu1 Eu1 67.99(19) 30_455 2 ?
O7 Eu1 Eu1 107.1(2) 30_455 4 ?
O7 Eu1 Eu1 157.91(19) 30_455 20_556 ?
O7 Eu1 O4 84.9(2) 30_455 . ?
O7 Eu1 O5 133.2(2) 30_455 20_556 ?
O7 Eu1 O6 80.3(3) 30_455 27 ?
O7 Eu1 H2 63.9 30_455 . ?
O7 Eu1 O1 75.7(2) 30_455 2 ?
O7 Eu1 O1 137.3(2) 30_455 22_556 ?
O7 Eu1 H1 140.7 30_455 . ?
O7 Eu1 O3 66.9(2) 30_455 . ?
O2 Eu1 Eu1 33.22(10) . 4 ?
O2 Eu1 Eu1 86.3(2) . 20_556 ?
O2 Eu1 Eu1 33.22(10) . 2 ?
O2 Eu1 O4 142.44(17) . . ?
O2 Eu1 O5 134.38(15) . 20_556 ?
O2 Eu1 O6 75.8(3) . 27 ?
O2 Eu1 O7 76.3(3) . 30_455 ?
O2 Eu1 H2 17.6 . . ?
O2 Eu1 O1 99.8(3) . 22_556 ?
O2 Eu1 O1 65.7(2) . 2 ?
O2 Eu1 H1 76.0 . . ?
O2 Eu1 O3 129.4(3) . . ?
H2 Eu1 H1 82.1 . . ?
O1 Eu1 Eu1 33.22(15) . 4 ?
O1 Eu1 Eu1 85.47(15) 2 4 ?
O1 Eu1 Eu1 85.51(15) 22_556 2 ?
O1 Eu1 Eu1 85.55(15) 22_556 4 ?
O1 Eu1 Eu1 85.50(15) . 2 ?
O1 Eu1 Eu1 32.87(15) . 20_556 ?
O1 Eu1 Eu1 33.19(15) 2 2 ?
O1 Eu1 Eu1 32.57(15) 22_556 20_556 ?
O1 Eu1 Eu1 84.86(15) 2 20_556 ?
O1 Eu1 O4 78.4(2) 2 . ?
O1 Eu1 O4 133.5(2) . . ?
O1 Eu1 O5 142.9(2) 2 20_556 ?
O1 Eu1 O5 73.6(2) . 20_556 ?
O1 Eu1 O5 79.7(2) 22_556 20_556 ?
O1 Eu1 O6 140.9(2) 22_556 27 ?
O1 Eu1 O6 138.3(2) 2 27 ?
O1 Eu1 O6 78.8(2) . 27 ?
O1 Eu1 O7 140.0(3) . 30_455 ?
O1 Eu1 O2 65.7(2) . . ?
O1 Eu1 H2 76.2 . . ?
O1 Eu1 H2 76.1 2 . ?
O1 Eu1 H2 117.4 22_556 . ?
O1 Eu1 O1 64.7(2) . 22_556 ?
O1 Eu1 O1 98.6(3) . 2 ?
O1 Eu1 O1 64.6(2) 2 22_556 ?
O1 Eu1 H1 116.3 2 . ?
O1 Eu1 H1 17.7 . . ?
O1 Eu1 H1 74.9 22_556 . ?
O1 Eu1 O3 130.6(2) . . ?
O1 Eu1 O3 130.8(2) 2 . ?
O1 Eu1 O3 130.8(2) 22_556 . ?
O3 Eu1 Eu1 134.69(15) . 4 ?
O3 Eu1 Eu1 135.16(15) . 20_556 ?
O3 Eu1 Eu1 134.84(15) . 2 ?
O3 Eu1 H2 111.8 . . ?
O3 Eu1 H1 112.9 . . ?
C9 O4 Eu1 130.2(6) . . ?
C9 O5 Eu1 127.6(6) . 22_556 ?
C2 C3 H3 120.3 . . ?
C4 C3 H3 120.3 . . ?
C4 C3 C2 119.4(10) . . ?
C4 C5 H5 119.2 . . ?
C6 C5 H5 119.2 . . ?
C6 C5 C4 121.6(13) . . ?
C3 C2 C1 119.4(10) . . ?
C7 C2 C3 120.4(11) . . ?
C7 C2 C1 120.0(11) . . ?
O6 C1 C2 118.4(11) . . ?
O6 C1 O7 126.8(10) . . ?
O7 C1 C2 114.8(10) . . ?
C3 C4 C9 121.1(9) . . ?
C5 C4 C3 118.6(10) . . ?
C5 C4 C9 120.2(10) . . ?
O4 C9 C4 116.4(9) . . ?
O5 C9 O4 125.2(9) . . ?
O5 C9 C4 118.4(9) . . ?
C5 C6 C7 119.4(15) . . ?
C5 C6 C8 122.5(16) . . ?
C7 C6 C8 118.0(15) . . ?
C2 C7 C6 120.5(13) . . ?
C2 C7 H7 119.7 . . ?
C6 C7 H7 119.7 . . ?
C8 C8 C6 170(3) 19_666 . ?
C1 O6 Eu1 135.3(7) . 33 ?
C1 O7 Eu1 139.4(7) . 36 ?
Eu1 O2 Eu1 113.6(2) . 2 ?
Eu1 O2 Eu1 113.6(2) . 4 ?
Eu1 O2 Eu1 113.6(2) 2 4 ?
Eu1 O2 H2 105.0 . . ?
Eu1 O2 H2 105.0 4 . ?
Eu1 O2 H2 105.0 2 . ?
Eu1 O1 Eu1 113.6(3) . 4 ?
Eu1 O1 Eu1 114.6(2) . 20_556 ?
Eu1 O1 Eu1 114.5(2) 4 20_556 ?
Eu1 O1 H1 104.5 . . ?
Eu1 O1 H1 103.4 20_556 . ?
Eu1 O1 H1 104.5 4 . ?
Eu1 O3 H3A 127.6 . . ?
Eu1 O3 H3B 127.7 . . ?
H3A O3 H3B 104.7 . . ?

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
Eu1 O4 C9 O5 -60.2(13) . . . . ?
Eu1 O4 C9 C4 117.9(9) . . . . ?
Eu1 O5 C9 O4 57.2(13) 22_556 . . . ?
Eu1 O5 C9 C4 -120.8(9) 22_556 . . . ?
C3 C2 C1 O6 -15.3(18) . . . . ?
C3 C2 C1 O7 166.8(12) . . . . ?
C3 C2 C7 C6 -3(3) . . . . ?
C3 C4 C9 O4 175.8(11) . . . . ?
C3 C4 C9 O5 -6.0(18) . . . . ?
C5 C4 C9 O4 -5.6(18) . . . . ?
C5 C4 C9 O5 172.6(12) . . . . ?
C5 C6 C7 C2 3(3) . . . . ?
C2 C3 C4 C5 0(2) . . . . ?
C2 C3 C4 C9 178.3(12) . . . . ?
C2 C1 O6 Eu1 -172.8(8) . . . 33 ?
C2 C1 O7 Eu1 164.0(8) . . . 36 ?
C1 C2 C7 C6 -179.1(16) . . . . ?
C4 C3 C2 C1 177.9(12) . . . . ?
C4 C3 C2 C7 2(2) . . . . ?
C4 C5 C6 C7 -1(3) . . . . ?
C4 C5 C6 C8 176.5(18) . . . . ?
C6 C5 C4 C3 0(2) . . . . ?
C6 C5 C4 C9 -179.0(15) . . . . ?
C7 C2 C1 O6 160.4(15) . . . . ?
C7 C2 C1 O7 -18(2) . . . . ?
C8 C6 C7 C2 -174.7(19) . . . . ?
O6 C1 O7 Eu1 -14(2) . . . 36 ?
O7 C1 O6 Eu1 4.9(19) . . . 33 ?

_platon_squeeze_details          
;
TITL CF solution in R-3c
CELL   17.6167   17.6167   49.2104     90.00     90.00    120.00
SPGR R-3c
# Solvent Accessible Volume =      5148
# Electrons Found in S.A.V. =      1641
# Note: Atoms in Void are Labelled as Cxxx and Qxxx for all Others
C101 0.637 0.047 0.453 !       2.37 eA-3
C102 1.001 0.995 0.379 !       2.32 eA-3
C103 0.951 0.708 0.270 !       2.03 eA-3
C104 0.037 0.623 0.893 !       2.01 eA-3
C105 0.660 0.328 0.180 !       1.84 eA-3
C106 1.001 1.005 0.761 !       1.80 eA-3
C107 0.923 0.017 0.336 !       1.80 eA-3
Q108 0.909 0.621 0.192 !       1.64 eA-3
Q109 0.282 0.438 0.321 !       1.57 eA-3
C110 0.860 0.749 0.780 !       1.51 eA-3
C111 0.438 0.517 0.887 !       1.50 eA-3
C112 0.079 0.564 0.886 !       1.49 eA-3
Q113 0.473 0.689 0.612 !       1.44 eA-3
C114 0.759 0.923 0.771 !       1.44 eA-3
C115 0.686 0.918 0.242 !       1.42 eA-3
C116 0.409 0.902 0.937 !       1.40 eA-3
Q117 1.000 0.264 0.250 !       1.33 eA-3
C118 0.643 0.419 0.141 !       1.29 eA-3
C119 0.910 0.033 0.304 !       1.28 eA-3
C120 0.863 0.109 0.778 !       1.25 eA-3
C121 0.455 0.527 0.898 !       1.23 eA-3
C122 0.315 0.623 0.410 !       1.20 eA-3
Q123 0.762 0.261 0.322 !       1.19 eA-3
Q124 0.171 0.889 0.262 !       1.17 eA-3
Q125 0.495 0.551 0.928 !       1.17 eA-3
C126 0.260 0.031 0.743 !       1.15 eA-3
Q127 0.842 0.838 0.989 !       1.13 eA-3
Q128 1.000 0.999 0.598 !       1.13 eA-3
Q129 0.827 0.578 0.084 !       1.12 eA-3
Q130 0.901 0.128 0.211 !       1.09 eA-3
Q131 0.372 0.786 0.613 !       1.08 eA-3
C132 0.713 0.386 0.707 !       1.07 eA-3
C133 0.669 0.501 0.992 !       1.06 eA-3
Q134 0.628 0.747 0.660 !       1.04 eA-3
Q135 0.218 0.567 0.653 !       1.03 eA-3
C136 0.216 0.044 0.220 !       1.01 eA-3
C137 0.829 0.828 0.250 !       1.01 eA-3
C138 0.990 0.032 0.272 !       1.01 eA-3
Q139 0.673 0.351 0.733 !       1.00 eA-3
C140 0.101 0.237 0.762 !       0.98 eA-3
C141 0.767 0.875 0.760 !       0.97 eA-3
C142 0.235 0.438 0.901 !       0.97 eA-3
C143 0.702 0.313 0.644 !       0.96 eA-3
C144 0.720 0.134 0.099 !       0.94 eA-3
Q145 0.514 0.392 0.360 !       0.94 eA-3
Q146 0.996 0.033 0.465 !       0.94 eA-3
C147 0.208 0.565 0.977 !       0.93 eA-3
Q148 0.779 0.639 0.040 !       0.92 eA-3
Q149 0.828 0.232 0.128 !       0.91 eA-3
Q150 0.013 0.094 0.414 !       0.91 eA-3
C151 0.162 0.029 0.231 !       0.89 eA-3
C152 0.424 0.518 0.934 !       0.89 eA-3
Q153 0.187 0.389 0.644 !       0.89 eA-3
C154 0.342 0.754 0.488 !       0.89 eA-3
C155 0.658 0.246 0.512 !       0.89 eA-3
Q156 0.152 0.467 0.341 !       0.88 eA-3
C157 0.860 0.984 0.231 !       0.88 eA-3
C158 0.140 0.016 0.769 !       0.88 eA-3
Q159 0.574 0.690 0.024 !       0.88 eA-3
Q160 0.060 0.297 0.489 !       0.88 eA-3
C161 0.079 0.869 0.281 !       0.88 eA-3
Q162 0.783 0.065 0.222 !       0.88 eA-3
Q163 0.860 0.731 0.169 !       0.87 eA-3
Q164 0.094 0.109 0.527 !       0.87 eA-3
C165 0.771 0.246 0.573 !       0.87 eA-3
Q166 0.719 0.923 0.785 !       0.87 eA-3
Q167 0.505 0.439 0.538 !       0.87 eA-3
Q168 0.482 0.796 0.191 !       0.86 eA-3
C169 0.581 0.890 0.891 !       0.86 eA-3
C170 0.613 0.268 0.066 !       0.85 eA-3
C171 1.001 0.083 0.820 !       0.85 eA-3
C172 0.074 1.004 0.821 !       0.85 eA-3
C173 0.416 0.737 0.412 !       0.85 eA-3
Q174 0.684 0.060 0.066 !       0.84 eA-3
Q175 0.134 0.709 0.781 !       0.84 eA-3
C176 0.733 0.216 0.106 !       0.84 eA-3
C177 0.481 0.796 0.985 !       0.84 eA-3
C178 0.671 0.468 0.126 !       0.83 eA-3
C179 0.965 0.872 0.197 !       0.83 eA-3
C180 0.198 0.116 0.273 !       0.83 eA-3
Q181 0.437 0.894 0.601 !       0.83 eA-3
C182 0.654 0.424 0.117 !       0.83 eA-3
Q183 0.482 0.704 0.259 !       0.83 eA-3
C184 0.059 0.139 0.675 !       0.83 eA-3
C185 0.319 0.530 0.937 !       0.82 eA-3
C186 0.136 0.064 0.823 !       0.82 eA-3
C187 0.403 0.566 0.436 !       0.82 eA-3
C188 0.273 0.654 0.850 !       0.81 eA-3
C189 0.812 0.562 0.581 !       0.81 eA-3
Q190 0.160 0.892 0.795 !       0.81 eA-3
Q191 0.324 0.754 0.309 !       0.80 eA-3
C192 0.690 0.640 0.081 !       0.79 eA-3
Q193 0.578 0.395 0.273 !       0.79 eA-3
Q194 0.171 0.733 0.460 !       0.79 eA-3
Q195 0.080 0.988 0.855 !       0.79 eA-3
Q196 0.353 0.078 0.778 !       0.79 eA-3
C197 0.137 0.391 0.407 !       0.79 eA-3
Q198 0.987 0.658 0.261 !       0.78 eA-3
Q199 0.498 0.608 0.874 !       0.77 eA-3
;
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 -0.333 0.333 0.083 820 259 ' '
2 0.000 0.000 0.250 805 256 ' '
3 0.333 0.667 0.417 821 259 ' '
4 -0.333 0.333 0.583 820 259 ' '
5 0.000 0.000 0.750 805 256 ' '
6 0.333 0.667 0.917 821 259 ' '
7 0.020 0.744 0.373 8 3 ' '
8 0.020 0.276 0.873 8 3 ' '
9 0.057 0.647 0.039 7 3 ' '
10 0.057 0.410 0.539 7 2 ' '
11 0.077 0.390 0.294 7 3 ' '
12 0.077 0.686 0.794 7 3 ' '
13 0.256 0.276 0.373 8 3 ' '
14 0.256 0.980 0.873 8 3 ' '
15 0.276 0.256 0.127 8 3 ' '
16 0.276 0.020 0.627 8 3 ' '
17 0.313 0.923 0.294 7 3 ' '
18 0.313 0.390 0.794 7 3 ' '
19 0.353 0.410 0.039 7 2 ' '
20 0.353 0.943 0.539 7 3 ' '
21 0.390 0.077 0.206 7 3 ' '
22 0.390 0.313 0.706 7 3 ' '
23 0.410 0.353 0.461 7 2 ' '
24 0.410 0.057 0.961 7 2 ' '
25 0.590 0.943 0.039 7 3 ' '
26 0.590 0.647 0.539 7 3 ' '
27 0.609 0.686 0.294 7 3 ' '
28 0.609 0.923 0.794 7 3 ' '
29 0.647 0.057 0.460 7 3 ' '
30 0.647 0.590 0.961 7 3 ' '
31 0.686 0.610 0.206 7 3 ' '
32 0.686 0.077 0.706 7 3 ' '
33 0.724 0.980 0.373 8 3 ' '
34 0.724 0.744 0.873 8 3 ' '
35 0.743 0.020 0.127 8 3 ' '
36 0.743 0.724 0.627 8 3 ' '
37 0.923 0.313 0.206 7 3 ' '
38 0.923 0.610 0.706 7 3 ' '
39 0.943 0.590 0.461 7 3 ' '
40 0.943 0.353 0.961 7 3 ' '
41 0.980 0.724 0.127 8 3 ' '
42 0.980 0.256 0.627 8 3 ' '

_platon_squeeze_void_probe_radius 1.20

_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 1.774
_oxdiff_exptl_absorpt_empirical_full_min 0.700
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_210717f_auto
_database_code_depnum_ccdc_archive 'CCDC 2268650'
loop_
_audit_author_name
_audit_author_address
Wang
;North University of China
China
;
_audit_update_record             
;
2023-06-09 deposited with the CCDC.	2023-08-28 downloaded from the CCDC.
;
_audit_creation_date             2023-06-01
_audit_creation_method           
;
Olex2 1.5-alpha
(compiled 2021.06.01 svn.r985b505f for OlexSys, GUI svn.r6335)
;
_shelx_SHELXL_version_number     2016/6
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C27 H19 O19 Tb3'
_chemical_formula_sum            'C27 H19 O19 Tb3'
_chemical_formula_weight         1124.18
_chemical_melting_point          ?
_chemical_oxdiff_formula         TbC
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Tb Tb -9.1472 9.1891 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      trigonal
_space_group_IT_number           167
_space_group_name_H-M_alt        'R -3 c'
_space_group_name_Hall           '-R 3 2"c'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x-y, -y, -z+1/2'
'-x, -x+y, -z+1/2'
'y, x, -z+1/2'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'x-y+2/3, -y+1/3, -z+5/6'
'-x+2/3, -x+y+1/3, -z+5/6'
'y+2/3, x+1/3, -z+5/6'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'x-y+1/3, -y+2/3, -z+7/6'
'-x+1/3, -x+y+2/3, -z+7/6'
'y+1/3, x+2/3, -z+7/6'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-x+y, y, z-1/2'
'x, x-y, z-1/2'
'-y, -x, z-1/2'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-x+y+2/3, y+1/3, z-1/6'
'x+2/3, x-y+1/3, z-1/6'
'-y+2/3, -x+1/3, z-1/6'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'
'-x+y+1/3, y+2/3, z+1/6'
'x+1/3, x-y+2/3, z+1/6'
'-y+1/3, -x+2/3, z+1/6'

_cell_length_a                   17.6231(8)
_cell_length_b                   17.6231(8)
_cell_length_c                   48.762(2)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     13115.3(13)
_cell_formula_units_Z            12
_cell_measurement_reflns_used    2649
_cell_measurement_temperature    297(2)
_cell_measurement_theta_max      75.2620
_cell_measurement_theta_min      6.0540
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    24.001
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.75334
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.41.112a (Rigaku Oxford Diffraction, 2021)
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    1.708
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             6336
_exptl_crystal_size_max          ?
_exptl_crystal_size_mid          ?
_exptl_crystal_size_min          ?
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.1194
_diffrn_reflns_av_unetI/netI     0.0897
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.967
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       58
_diffrn_reflns_limit_l_min       -59
_diffrn_reflns_number            14436
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.967
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.464
_diffrn_reflns_theta_min         3.416
_diffrn_ambient_temperature      297.00
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.967
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     97.00 126.00   1.00    0.44    --  106.49  57.00 -60.00   29
  2  ω    141.00 178.00   1.00    0.44    --  106.49  57.00 -60.00   37
  3  ω    142.00 177.00   1.00    0.44    --  106.49  38.00  30.00   35
  4  ω     93.00 138.00   1.00    0.44    --  106.49  38.00  30.00   45
  5  ω     92.00 178.00   1.00    0.44    --  106.49  60.00  99.00   86
  6  ω     36.00  70.00   1.00    0.44    --  106.49 -60.00 -39.00   34
  7  ω     34.00  98.00   1.00    0.44    --  106.49 -77.00  60.00   64
  8  ω     17.00  81.00   1.00    0.28    --   48.45-103.00-112.00   64
  9  ω    -22.00  27.00   1.00    0.28    --  -48.45  19.00-120.00   49
 10  ω    -91.00 -65.00   1.00    0.44    --  -86.25  72.00 122.00   26
 11  ω    -51.00 -16.00   1.00    0.44    --  -86.25  72.00 122.00   35
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0236727000
_diffrn_orient_matrix_UB_12      -0.0705052000
_diffrn_orient_matrix_UB_13      -0.0222421000
_diffrn_orient_matrix_UB_21      -0.0878689000
_diffrn_orient_matrix_UB_22      -0.0031471000
_diffrn_orient_matrix_UB_23      -0.0049257000
_diffrn_orient_matrix_UB_31      0.0436737000
_diffrn_orient_matrix_UB_32      0.0721879000
_diffrn_orient_matrix_UB_33      -0.0218930000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2243
_reflns_number_total             2975
_reflns_odcompleteness_completeness 99.17
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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 1.171.41.112a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.112a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.112a (Rigaku OD, 2021)'
_computing_molecular_graphics    'Olex2 1.5-alpha (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-alpha (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'olex2.solve 1.5-alpha (Bourhis et al., 2015)'
_refine_diff_density_max         1.211
_refine_diff_density_min         -1.065
_refine_diff_density_rms         0.192
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.880
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     149
_refine_ls_number_reflns         2975
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0711
_refine_ls_R_factor_gt           0.0559
_refine_ls_restrained_S_all      0.880
_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)+(0.1073P)²+206.7078P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1533
_refine_ls_wR_factor_ref         0.1630
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H) groups, All O(H,H) groups
2.a Rotating group:
 O6(H6A,H6B)
2.b Ternary CH refined with riding coordinates:
 O2(H2), O3(H3)
2.c Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5), C1(H1)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Tb1 Tb 0.88351(3) 0.86227(3) 0.53326(2) 0.0222(2) Uani 1 1 d . . . . .
O2 O 0.8932(3) 0.8744(3) 0.48513(9) 0.0125(9) Uani 1 1 d . . . . .
H2 H 0.845598 0.818118 0.478502 0.019 Uiso 1 1 calc R U . . .
O4 O 0.7340(4) 0.8085(4) 0.52202(13) 0.0300(13) Uani 1 1 d . . . . .
O3 O 1.000000 1.000000 0.54561(16) 0.0099(15) Uani 1 3 d S T P . .
H3 H 1.000002 1.000003 0.565704 0.015 Uiso 1 3 calc R U P . .
O1 O 0.7240(4) 0.8723(4) 0.48389(12) 0.0338(14) Uani 1 1 d . . . . .
C7 C 0.7026(5) 0.8453(6) 0.50818(18) 0.0291(18) Uani 1 1 d . . . . .
C3 C 0.6319(6) 0.8586(6) 0.5210(2) 0.035(2) Uani 1 1 d . . . . .
C4 C 0.5975(6) 0.8236(7) 0.54614(19) 0.035(2) Uani 1 1 d . . . . .
H4 H 0.615049 0.787953 0.554847 0.041 Uiso 1 1 calc R U . . .
C5 C 0.6039(9) 0.9090(9) 0.5073(2) 0.053(3) Uani 1 1 d . . . . .
H5 H 0.627014 0.932607 0.490178 0.063 Uiso 1 1 calc R U . . .
C8 C 0.5402(9) 0.9242(10) 0.5194(3) 0.060(4) Uani 1 1 d . . . . .
C2 C 0.5359(6) 0.8407(7) 0.5591(2) 0.039(2) Uani 1 1 d . . . . .
C1 C 0.5069(8) 0.8903(9) 0.5446(2) 0.051(3) Uani 1 1 d . . . . .
H1 H 0.464417 0.900296 0.552302 0.061 Uiso 1 1 calc R U . . .
C6 C 0.5141(10) 0.9802(11) 0.5056(3) 0.072(5) Uani 1 1 d . . . . .
O6 O 0.7724(15) 0.7275(11) 0.5646(4) 0.157(7) Uani 1 1 d . . . . .
H6A H 0.751741 0.730241 0.584189 0.236 Uiso 1 1 d R U . . .
H6B H 0.741704 0.661628 0.559682 0.236 Uiso 1 1 d R U . . .
O5 O 0.5039(4) 0.7413(4) 0.59524(13) 0.0345(15) Uani 1 1 d . . . . .
O7 O 0.4552(4) 0.8350(5) 0.59793(13) 0.0372(15) Uani 1 1 d . . . . .
C9 C 0.4953(6) 0.8019(6) 0.58626(16) 0.0281(18) 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
Tb1 Tb1 3.9203(8) 3_675 ?
Tb1 Tb1 3.9203(8) 2_765 ?
Tb1 Tb1 3.9548(8) 21_656 ?
Tb1 O2 2.355(4) . ?
Tb1 O2 2.343(5) 21_656 ?
Tb1 O2 2.357(5) 20_566 ?
Tb1 O4 2.376(6) . ?
Tb1 O3 2.342(2) . ?
Tb1 O1 2.364(6) 21_656 ?
Tb1 O6 2.67(2) . ?
Tb1 O5 2.370(6) 17_655 ?
Tb1 O7 2.339(6) 16_665 ?
O2 H2 0.9800 . ?
O4 C7 1.242(11) . ?
O3 H3 0.9800 . ?
O1 C7 1.262(11) . ?
C7 C3 1.512(13) . ?
C3 C4 1.370(13) . ?
C3 C5 1.385(14) . ?
C4 H4 0.9300 . ?
C4 C2 1.413(14) . ?
C5 H5 0.9300 . ?
C5 C8 1.409(16) . ?
C8 C1 1.362(15) . ?
C8 C6 1.448(16) . ?
C2 C1 1.404(14) . ?
C2 C9 1.499(12) . ?
C1 H1 0.9300 . ?
C6 C6 1.17(2) 19_676 ?
O6 H6A 1.0341 . ?
O6 H6B 1.0338 . ?
O5 C9 1.231(11) . ?
O7 C9 1.255(11) . ?

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
Tb1 Tb1 Tb1 60.286(8) 2_765 21_656 ?
Tb1 Tb1 Tb1 60.0 2_765 3_675 ?
Tb1 Tb1 Tb1 90.0 3_675 21_656 ?
O2 Tb1 Tb1 85.14(12) 20_566 21_656 ?
O2 Tb1 Tb1 85.95(12) 21_656 3_675 ?
O2 Tb1 Tb1 33.36(12) 20_566 3_675 ?
O2 Tb1 Tb1 32.94(12) . 21_656 ?
O2 Tb1 Tb1 85.76(12) . 3_675 ?
O2 Tb1 Tb1 85.97(13) . 2_765 ?
O2 Tb1 Tb1 32.75(11) 21_656 21_656 ?
O2 Tb1 Tb1 85.77(12) 20_566 2_765 ?
O2 Tb1 Tb1 33.59(12) 21_656 2_765 ?
O2 Tb1 O2 65.03(16) 21_656 . ?
O2 Tb1 O2 99.3(2) 21_656 20_566 ?
O2 Tb1 O2 64.82(15) . 20_566 ?
O2 Tb1 O4 79.77(19) . . ?
O2 Tb1 O4 143.27(19) 21_656 . ?
O2 Tb1 O4 73.27(19) 20_566 . ?
O2 Tb1 O1 73.15(19) . 21_656 ?
O2 Tb1 O1 78.1(2) 21_656 21_656 ?
O2 Tb1 O1 134.07(19) 20_566 21_656 ?
O2 Tb1 O6 129.3(5) 21_656 . ?
O2 Tb1 O6 131.4(5) 20_566 . ?
O2 Tb1 O6 129.6(4) . . ?
O2 Tb1 O5 138.5(2) 21_656 17_655 ?
O2 Tb1 O5 141.0(2) . 17_655 ?
O2 Tb1 O5 78.8(2) 20_566 17_655 ?
O2 Tb1 O7 75.2(2) 21_656 16_665 ?
O4 Tb1 Tb1 102.23(15) . 3_675 ?
O4 Tb1 Tb1 110.76(16) . 21_656 ?
O4 Tb1 Tb1 158.18(15) . 2_765 ?
O4 Tb1 O6 66.7(5) . . ?
O3 Tb1 Tb1 33.19(8) . 2_765 ?
O3 Tb1 Tb1 86.24(16) . 21_656 ?
O3 Tb1 Tb1 33.19(8) . 3_675 ?
O3 Tb1 O2 66.06(16) . 21_656 ?
O3 Tb1 O2 65.84(16) . 20_566 ?
O3 Tb1 O2 100.1(2) . . ?
O3 Tb1 O4 134.07(15) . . ?
O3 Tb1 O1 142.44(17) . 21_656 ?
O3 Tb1 O6 130.3(4) . . ?
O3 Tb1 O5 75.9(2) . 17_655 ?
O3 Tb1 O7 76.0(2) . 16_665 ?
O1 Tb1 Tb1 109.51(16) 21_656 2_765 ?
O1 Tb1 Tb1 157.47(15) 21_656 3_675 ?
O1 Tb1 Tb1 68.01(16) 21_656 21_656 ?
O1 Tb1 O4 82.1(2) 21_656 . ?
O1 Tb1 O6 66.1(4) 21_656 . ?
O1 Tb1 O5 132.3(2) 21_656 17_655 ?
O6 Tb1 Tb1 136.0(4) . 3_675 ?
O6 Tb1 Tb1 134.6(4) . 2_765 ?
O6 Tb1 Tb1 134.0(4) . 21_656 ?
O5 Tb1 Tb1 69.72(15) 17_655 3_675 ?
O5 Tb1 Tb1 159.64(15) 17_655 21_656 ?
O5 Tb1 Tb1 105.73(17) 17_655 2_765 ?
O5 Tb1 O4 76.5(2) 17_655 . ?
O5 Tb1 O6 66.3(4) 17_655 . ?
O7 Tb1 Tb1 104.99(17) 16_665 21_656 ?
O7 Tb1 Tb1 106.85(18) 16_665 3_675 ?
O7 Tb1 Tb1 67.59(17) 16_665 2_765 ?
O7 Tb1 O2 139.9(2) 16_665 20_566 ?
O7 Tb1 O2 137.3(2) 16_665 . ?
O7 Tb1 O4 133.3(2) 16_665 . ?
O7 Tb1 O1 84.5(2) 16_665 21_656 ?
O7 Tb1 O6 67.0(5) 16_665 . ?
O7 Tb1 O5 80.3(2) 16_665 17_655 ?
Tb1 O2 Tb1 113.1(2) 20_566 21_656 ?
Tb1 O2 Tb1 114.68(19) 20_566 . ?
Tb1 O2 Tb1 114.15(19) . 21_656 ?
Tb1 O2 H2 104.5 20_566 . ?
Tb1 O2 H2 104.5 . . ?
Tb1 O2 H2 104.5 21_656 . ?
C7 O4 Tb1 127.7(5) . . ?
Tb1 O3 Tb1 113.63(15) 2_765 3_675 ?
Tb1 O3 Tb1 113.63(15) . 2_765 ?
Tb1 O3 Tb1 113.63(15) . 3_675 ?
Tb1 O3 H3 104.9 . . ?
Tb1 O3 H3 104.9 2_765 . ?
Tb1 O3 H3 104.9 3_675 . ?
C7 O1 Tb1 128.8(6) . 20_566 ?
O4 C7 O1 125.5(8) . . ?
O4 C7 C3 118.2(8) . . ?
O1 C7 C3 116.3(8) . . ?
C4 C3 C7 120.9(9) . . ?
C4 C3 C5 120.1(9) . . ?
C5 C3 C7 119.0(9) . . ?
C3 C4 H4 119.4 . . ?
C3 C4 C2 121.2(9) . . ?
C2 C4 H4 119.4 . . ?
C3 C5 H5 120.2 . . ?
C8 C5 C3 119.5(9) . . ?
C8 C5 H5 120.2 . . ?
C5 C8 C6 119.3(10) . . ?
C1 C8 C5 120.3(10) . . ?
C1 C8 C6 120.3(11) . . ?
C4 C2 C9 122.7(8) . . ?
C1 C2 C4 117.8(8) . . ?
C1 C2 C9 119.3(8) . . ?
C8 C1 H1 119.5 . . ?
C2 C1 C8 121.0(10) . . ?
C2 C1 H1 119.5 . . ?
C6 C6 C8 174(2) 19_676 . ?
Tb1 O6 H6A 127.3 . . ?
Tb1 O6 H6B 127.3 . . ?
H6A O6 H6B 105.4 . . ?
C9 O5 Tb1 135.9(6) . 17_655 ?
C9 O7 Tb1 140.0(6) . 16_565 ?
O5 C9 C2 118.2(8) . . ?
O5 C9 O7 125.7(8) . . ?
O7 C9 C2 116.1(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
Tb1 O4 C7 O1 57.0(12) . . . . ?
Tb1 O4 C7 C3 -123.9(7) . . . . ?
Tb1 O1 C7 O4 -61.0(12) 20_566 . . . ?
Tb1 O1 C7 C3 119.9(8) 20_566 . . . ?
Tb1 O5 C9 C2 -174.1(7) 17_655 . . . ?
Tb1 O5 C9 O7 6.0(16) 17_655 . . . ?
Tb1 O7 C9 C2 164.4(7) 16_565 . . . ?
Tb1 O7 C9 O5 -15.8(16) 16_565 . . . ?
O4 C7 C3 C4 -6.1(14) . . . . ?
O4 C7 C3 C5 172.0(10) . . . . ?
O1 C7 C3 C4 173.1(9) . . . . ?
O1 C7 C3 C5 -8.8(14) . . . . ?
C7 C3 C4 C2 175.6(10) . . . . ?
C7 C3 C5 C8 -177.9(12) . . . . ?
C3 C4 C2 C1 3.8(17) . . . . ?
C3 C4 C2 C9 178.5(10) . . . . ?
C3 C5 C8 C1 1(2) . . . . ?
C3 C5 C8 C6 177.2(14) . . . . ?
C4 C3 C5 C8 0(2) . . . . ?
C4 C2 C1 C8 -3(2) . . . . ?
C4 C2 C9 O5 -13.2(15) . . . . ?
C4 C2 C9 O7 166.6(10) . . . . ?
C5 C3 C4 C2 -2.5(17) . . . . ?
C5 C8 C1 C2 1(2) . . . . ?
C1 C2 C9 O5 161.4(11) . . . . ?
C1 C2 C9 O7 -18.7(16) . . . . ?
C6 C8 C1 C2 -175.8(15) . . . . ?
C9 C2 C1 C8 -177.8(13) . . . . ?

_smtbx_masks_special_details     ?
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 -0.125 -0.765 -0.421 5130.1 832.4 ?

_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2

_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 1.283
_oxdiff_exptl_absorpt_empirical_full_min 0.817
####################################################################### 
# 
# 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 2268649'
loop_
_audit_author_name
_audit_author_address
Wang
;North University of China
China
;
_audit_update_record             
;
2023-06-09 deposited with the CCDC.	2023-08-28 downloaded from the CCDC.
;
_audit_creation_date             2023-06-05
_audit_creation_method           
;
Olex2 1.5-alpha
(compiled 2021.06.01 svn.r985b505f for OlexSys, GUI svn.r6335)
;
_shelx_SHELXL_version_number     2016/6
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C9 H6.333 Ce O6.333'
_chemical_formula_sum            'C8.53 H6.10 Ce O6.33'
_chemical_formula_weight         350.05
_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 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ce Ce -1.8482 9.6596 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      trigonal
_space_group_IT_number           167
_space_group_name_H-M_alt        'R -3 c'
_space_group_name_Hall           '-R 3 2"c'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x-y, -y, -z+1/2'
'-x, -x+y, -z+1/2'
'y, x, -z+1/2'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'x-y+2/3, -y+1/3, -z+5/6'
'-x+2/3, -x+y+1/3, -z+5/6'
'y+2/3, x+1/3, -z+5/6'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'x-y+1/3, -y+2/3, -z+7/6'
'-x+1/3, -x+y+2/3, -z+7/6'
'y+1/3, x+2/3, -z+7/6'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-x+y, y, z-1/2'
'x, x-y, z-1/2'
'-y, -x, z-1/2'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-x+y+2/3, y+1/3, z-1/6'
'x+2/3, x-y+1/3, z-1/6'
'-y+2/3, -x+1/3, z-1/6'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'
'-x+y+1/3, y+2/3, z+1/6'
'x+1/3, x-y+2/3, z+1/6'
'-y+1/3, -x+2/3, z+1/6'

_cell_length_a                   17.9267(4)
_cell_length_b                   17.9267(4)
_cell_length_c                   49.8631(16)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     13877.5(8)
_cell_formula_units_Z            36
_cell_measurement_reflns_used    2649
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      75.2620
_cell_measurement_theta_min      6.0540
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    22.931
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.508
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             5974
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.10
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.1817
_diffrn_reflns_av_unetI/netI     0.1130
_diffrn_reflns_Laue_measured_fraction_full 0.986
_diffrn_reflns_Laue_measured_fraction_max 0.952
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       57
_diffrn_reflns_limit_l_min       -60
_diffrn_reflns_number            15818
_diffrn_reflns_point_group_measured_fraction_full 0.986
_diffrn_reflns_point_group_measured_fraction_max 0.952
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         76.562
_diffrn_reflns_theta_min         3.353
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.952
_diffrn_measurement_device_type  'multiwire proportional'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_source                   ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2449
_reflns_number_total             3105
_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       ?
_computing_data_collection       ?
_computing_data_reduction        ?
_computing_molecular_graphics    'Olex2 1.5-alpha (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-alpha (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'olex2.solve 1.5-alpha (Bourhis et al., 2015)'
_refine_diff_density_max         2.388
_refine_diff_density_min         -1.437
_refine_diff_density_rms         0.325
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.084
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     149
_refine_ls_number_reflns         3105
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1129
_refine_ls_R_factor_gt           0.0980
_refine_ls_restrained_S_all      1.084
_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)+(0.1633P)²+262.0013P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2499
_refine_ls_wR_factor_ref         0.2629
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H) groups, All O(H,H) groups
2.a Rotating group:
 O1(H1A,H1B)
2.b Ternary CH refined with riding coordinates:
 O2(H2), O3(H3)
2.c Aromatic/amide H refined with riding coordinates:
 C7(H7), C5(H5), C3(H3A)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ce1 Ce 0.85964(4) 0.87871(4) 0.46598(2) 0.0251(3) Uani 1 1 d . . . . .
O2 O 0.9822(5) 0.8732(5) 0.48496(15) 0.0186(15) Uani 1 1 d . . . . .
H2 H 0.974636 0.818264 0.478485 0.028 Uiso 1 1 calc R U . . .
O3 O 1.000000 1.000000 0.4540(3) 0.019(3) Uani 1 3 d S T P . .
H3 H 1.000000 1.000000 0.434344 0.029 Uiso 1 3 calc R U P . .
O4 O 0.7190(6) 0.8450(6) 0.48473(18) 0.035(2) Uani 1 1 d . . . . .
O1 O 0.7307(10) 0.7680(9) 0.4356(3) 0.071(4) Uani 1 1 d . . . . .
H1A H 0.689449 0.718366 0.440074 0.107 Uiso 1 1 d R U . . .
H1B H 0.720684 0.773760 0.419174 0.107 Uiso 1 1 d R U . . .
O5 O 0.7257(6) 0.9189(6) 0.5215(2) 0.036(2) Uani 1 1 d . . . . .
C7 C 0.5984(11) 0.7670(10) 0.5454(3) 0.046(4) Uani 1 1 d . . . . .
H7 H 0.617949 0.819791 0.553891 0.055 Uiso 1 1 calc R U . . .
C6 C 0.6284(10) 0.7660(10) 0.5208(3) 0.047(4) Uani 1 1 d . . . . .
C9 C 0.6965(9) 0.8509(9) 0.5078(3) 0.036(3) Uani 1 1 d . . . . .
C4 C 0.5413(19) 0.6154(13) 0.5201(4) 0.085(9) Uani 1 1 d . . . . .
C5 C 0.6018(14) 0.6915(11) 0.5081(4) 0.066(6) Uani 1 1 d . . . . .
H5 H 0.623854 0.690594 0.491273 0.079 Uiso 1 1 calc R U . . .
C1 C 0.4979(10) 0.6901(9) 0.5848(3) 0.036(3) Uani 1 1 d . . . . .
C2 C 0.5380(11) 0.6907(10) 0.5591(3) 0.049(4) Uani 1 1 d . . . . .
C3 C 0.5077(15) 0.6157(11) 0.5446(3) 0.071(7) Uani 1 1 d . . . . .
H3A H 0.463606 0.564519 0.551671 0.085 Uiso 1 1 calc R U . . .
C8 C 0.510(2) 0.5305(13) 0.5067(6) 0.108(12) Uani 1 1 d . . . . .
O6 O 0.5084(7) 0.7594(7) 0.59398(19) 0.040(2) Uani 1 1 d . . . . .
O7 O 0.4558(7) 0.6181(7) 0.5959(2) 0.044(2) 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
Ce1 Ce1 4.0942(12) 2_765 ?
Ce1 Ce1 4.1352(11) 21_656 ?
Ce1 Ce1 4.0943(12) 3_675 ?
Ce1 O2 2.455(8) 3_675 ?
Ce1 O2 2.439(8) . ?
Ce1 O2 2.457(8) 20_566 ?
Ce1 O3 2.438(4) . ?
Ce1 O4 2.464(9) . ?
Ce1 O1 2.644(12) . ?
Ce1 O5 2.493(10) 21_656 ?
Ce1 O6 2.489(9) 30_665 ?
Ce1 O7 2.466(10) 28 ?
O2 H2 0.9800 . ?
O3 H3 0.9800 . ?
O4 C9 1.243(17) . ?
O1 H1A 0.8546 . ?
O1 H1B 0.8554 . ?
O5 C9 1.258(17) . ?
C7 H7 0.9300 . ?
C7 C6 1.35(2) . ?
C7 C2 1.42(2) . ?
C6 C9 1.54(2) . ?
C6 C5 1.33(2) . ?
C4 C5 1.38(3) . ?
C4 C3 1.37(2) . ?
C4 C8 1.49(3) . ?
C5 H5 0.9300 . ?
C1 C2 1.47(2) . ?
C1 O6 1.248(18) . ?
C1 O7 1.252(18) . ?
C2 C3 1.37(2) . ?
C3 H3A 0.9300 . ?
C8 C8 1.18(4) 19_666 ?

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
Ce1 Ce1 Ce1 89.999(1) 3_675 21_656 ?
Ce1 Ce1 Ce1 60.0 2_765 3_675 ?
Ce1 Ce1 Ce1 60.327(10) 2_765 21_656 ?
O2 Ce1 Ce1 85.37(19) . 3_675 ?
O2 Ce1 Ce1 32.51(17) . 21_656 ?
O2 Ce1 Ce1 85.17(18) 20_566 3_675 ?
O2 Ce1 Ce1 33.09(18) 3_675 3_675 ?
O2 Ce1 Ce1 33.34(19) . 2_765 ?
O2 Ce1 Ce1 84.52(18) 3_675 21_656 ?
O2 Ce1 Ce1 85.17(18) 3_675 2_765 ?
O2 Ce1 Ce1 85.41(19) 20_566 2_765 ?
O2 Ce1 Ce1 32.66(18) 20_566 21_656 ?
O2 Ce1 O2 97.9(4) . 3_675 ?
O2 Ce1 O2 64.1(2) 3_675 20_566 ?
O2 Ce1 O2 64.3(2) . 20_566 ?
O2 Ce1 O4 77.9(3) 3_675 . ?
O2 Ce1 O4 132.4(3) . . ?
O2 Ce1 O4 71.8(3) 20_566 . ?
O2 Ce1 O1 130.8(4) 3_675 . ?
O2 Ce1 O1 130.4(4) 20_566 . ?
O2 Ce1 O1 131.2(4) . . ?
O2 Ce1 O5 79.4(3) 20_566 21_656 ?
O2 Ce1 O5 142.1(3) 3_675 21_656 ?
O2 Ce1 O5 73.3(3) . 21_656 ?
O2 Ce1 O6 138.0(3) 3_675 30_665 ?
O2 Ce1 O6 140.2(3) 20_566 30_665 ?
O2 Ce1 O6 78.2(3) . 30_665 ?
O2 Ce1 O7 75.4(3) 3_675 28 ?
O2 Ce1 O7 138.9(3) . 28 ?
O2 Ce1 O7 137.0(3) 20_566 28 ?
O3 Ce1 Ce1 32.90(12) . 3_675 ?
O3 Ce1 Ce1 85.6(3) . 21_656 ?
O3 Ce1 Ce1 32.90(12) . 2_765 ?
O3 Ce1 O2 65.3(3) . . ?
O3 Ce1 O2 98.7(4) . 20_566 ?
O3 Ce1 O2 65.1(3) . 3_675 ?
O3 Ce1 O4 141.7(3) . . ?
O3 Ce1 O1 130.9(5) . . ?
O3 Ce1 O5 134.2(2) . 21_656 ?
O3 Ce1 O6 75.8(3) . 30_665 ?
O3 Ce1 O7 75.5(4) . 28 ?
O4 Ce1 Ce1 100.6(2) . 21_656 ?
O4 Ce1 Ce1 155.8(2) . 2_765 ?
O4 Ce1 Ce1 108.9(2) . 3_675 ?
O4 Ce1 O1 68.3(4) . . ?
O4 Ce1 O5 81.7(3) . 21_656 ?
O4 Ce1 O6 134.9(3) . 30_665 ?
O4 Ce1 O7 86.6(4) . 28 ?
O1 Ce1 Ce1 135.4(4) . 2_765 ?
O1 Ce1 Ce1 135.0(3) . 21_656 ?
O1 Ce1 Ce1 135.0(3) . 3_675 ?
O5 Ce1 Ce1 157.5(2) 21_656 3_675 ?
O5 Ce1 Ce1 68.2(2) 21_656 21_656 ?
O5 Ce1 Ce1 102.3(2) 21_656 2_765 ?
O5 Ce1 O1 67.0(4) 21_656 . ?
O6 Ce1 Ce1 107.9(3) 30_665 21_656 ?
O6 Ce1 Ce1 68.6(3) 30_665 2_765 ?
O6 Ce1 Ce1 105.4(2) 30_665 3_675 ?
O6 Ce1 O1 66.8(5) 30_665 . ?
O6 Ce1 O5 77.5(3) 30_665 21_656 ?
O7 Ce1 Ce1 66.9(3) 28 3_675 ?
O7 Ce1 Ce1 156.8(3) 28 21_656 ?
O7 Ce1 Ce1 105.8(3) 28 2_765 ?
O7 Ce1 O1 68.2(4) 28 . ?
O7 Ce1 O5 134.9(4) 28 21_656 ?
O7 Ce1 O6 80.7(4) 28 30_665 ?
Ce1 O2 Ce1 113.6(3) . 2_765 ?
Ce1 O2 Ce1 115.3(3) . 21_656 ?
Ce1 O2 Ce1 114.6(3) 2_765 21_656 ?
Ce1 O2 H2 103.8 2_765 . ?
Ce1 O2 H2 103.8 21_656 . ?
Ce1 O2 H2 103.8 . . ?
Ce1 O3 Ce1 114.2(2) 3_675 2_765 ?
Ce1 O3 Ce1 114.2(2) 2_765 . ?
Ce1 O3 Ce1 114.2(2) 3_675 . ?
Ce1 O3 H3 104.2 3_675 . ?
Ce1 O3 H3 104.2 2_765 . ?
Ce1 O3 H3 104.2 . . ?
C9 O4 Ce1 131.8(9) . . ?
Ce1 O1 H1A 127.5 . . ?
Ce1 O1 H1B 128.0 . . ?
H1A O1 H1B 104.6 . . ?
C9 O5 Ce1 127.5(9) . 20_566 ?
C6 C7 H7 118.6 . . ?
C6 C7 C2 122.7(15) . . ?
C2 C7 H7 118.6 . . ?
C7 C6 C9 119.6(14) . . ?
C5 C6 C7 120.1(15) . . ?
C5 C6 C9 120.2(15) . . ?
O4 C9 O5 126.0(13) . . ?
O4 C9 C6 115.8(13) . . ?
O5 C9 C6 118.2(13) . . ?
C5 C4 C8 121.5(17) . . ?
C3 C4 C5 120.9(17) . . ?
C3 C4 C8 117.6(18) . . ?
C6 C5 C4 119.7(16) . . ?
C6 C5 H5 120.2 . . ?
C4 C5 H5 120.2 . . ?
O6 C1 C2 119.0(13) . . ?
O6 C1 O7 125.3(13) . . ?
O7 C1 C2 115.7(13) . . ?
C7 C2 C1 124.0(14) . . ?
C3 C2 C7 115.4(15) . . ?
C3 C2 C1 119.8(15) . . ?
C4 C3 C2 120.9(17) . . ?
C4 C3 H3A 119.5 . . ?
C2 C3 H3A 119.5 . . ?
C8 C8 C4 171(3) 19_666 . ?
C1 O6 Ce1 137.3(9) . 36_665 ?
C1 O7 Ce1 141.2(10) . 34_545 ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Ce1 O4 C9 O5 60(2) . . . . ?
Ce1 O4 C9 C6 -118.5(13) . . . . ?
Ce1 O5 C9 O4 -56.9(19) 20_566 . . . ?
Ce1 O5 C9 C6 121.3(13) 20_566 . . . ?
C7 C6 C9 O4 -177.8(16) . . . . ?
C7 C6 C9 O5 4(2) . . . . ?
C7 C6 C5 C4 2(4) . . . . ?
C7 C2 C3 C4 7(4) . . . . ?
C6 C7 C2 C1 -173.9(18) . . . . ?
C6 C7 C2 C3 -4(3) . . . . ?
C9 C6 C5 C4 179(2) . . . . ?
C5 C6 C9 O4 5(3) . . . . ?
C5 C6 C9 O5 -173.5(19) . . . . ?
C5 C4 C3 C2 -5(5) . . . . ?
C1 C2 C3 C4 177(2) . . . . ?
C2 C7 C6 C9 -177.4(17) . . . . ?
C2 C7 C6 C5 0(3) . . . . ?
C2 C1 O6 Ce1 174.4(11) . . . 36_665 ?
C2 C1 O7 Ce1 -167.8(12) . . . 34_545 ?
C3 C4 C5 C6 1(5) . . . . ?
C8 C4 C5 C6 -180(3) . . . . ?
C8 C4 C3 C2 175(3) . . . . ?
O6 C1 C2 C7 9(3) . . . . ?
O6 C1 C2 C3 -160(2) . . . . ?
O6 C1 O7 Ce1 13(3) . . . 34_545 ?
O7 C1 C2 C7 -170.3(17) . . . . ?
O7 C1 C2 C3 20(3) . . . . ?
O7 C1 O6 Ce1 -6(3) . . . 36_665 ?

_smtbx_masks_special_details     ?
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 -0.778 -0.800 -0.042 5739.8 160.3 ?

_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2

_olex2_submission_special_instructions 'No special instructions were received'
